TY - JOUR A1 - Myrach, Philipp A1 - Maierhofer, Christiane A1 - Rahammer, M. A1 - Kreutzbruck, Marc T1 - Parameters in lock-in thermography of CFRP laminates N2 - Active thermography with lock-in excitation is a non-destructive testing method that is also feasible for testing of carbon fiber reinforced polymers (CFRP). For validating the method extensive investigations were done during a research project in order to advance a standardization process. The most important parameters of optical and ultrasonic excitation thermography were investigated. For example, the appropriate selection of spectral sensitivity of the used infrared camera systems is important for recording undisturbed thermal signals. Regarding excitation, influences of excitation power and ultrasonic frequency were studied. Furthermore, material parameters such as CFRP layup are known for strongly affecting the results of measurement. KW - Standardisierung KW - Lock-in thermography KW - Lock-in Thermografie KW - CFRP KW - CFK KW - optical excitation KW - ultrasonic excitation KW - Ultraschall KW - standardization PY - 2016 DO - https://doi.org/10.3139/120.110814 SN - 0025-5300 VL - 58 IS - 1 SP - 31 EP - 35 PB - Carl Hanser Verlag CY - München AN - OPUS4-35479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jonietz, Florian A1 - Myrach, Philipp A1 - Suwala, H. A1 - Ziegler, Mathias T1 - Examination of Spot Welded Joints with Active Thermography N2 - The method described here allows to determine the size of the thermal contact between two metal sheets joined by spot welding. This size is a measure for the size of the weld nugget, i.e. the zone melted during the welding process, and thus the quality of the welded joint. The method applies active thermography in transmission or reflection setup. Especially the reflection setup offers an attractive possibility for non-destructive testing when components can be accessed from one side only. The spot weld region is optically heated by laser or flash light radiation. The weld nugget provides the mechanical joint, but also constitutes a thermal bridge between the two welded sheets. The latter will be exploited in this method. The better thermal contact at the weld Nugget contrasts with the surrounding material, where the heat transfer between the two sheets is comparatively low. A major advantage of the described method is the applicability on sheets without any surface treatment. This is achieved by a proper normalization of the data, allowing for a correction of the varying surface emissivity. KW - Active thermography KW - Spot weld KW - Automotive industry PY - 2016 UR - http://link.springer.com/article/10.1007/s10921-015-0318-4?wt_mc=internal.event.1.SEM.ArticleAuthorIncrementalIssue DO - https://doi.org/10.1007/s10921-015-0318-4 VL - 35:1 SP - 1 EP - 14 PB - Springer CY - New York AN - OPUS4-35480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Helmecke, E. A1 - Fleßner, M. A1 - Kaufmann, M. A1 - Staude, Andreas A1 - Hausotte, T. T1 - Numerical measurement uncertainty determination for dimensional measurements of microparts with CT N2 - Up to now, the only standardized method to determine the measurement uncertainty for computed tomography (CT) is to use calibrated workpieces as specified in the Guideline VDI/VDE 2630 Part 2.1. This paper discusses a promising numerical method for uncertainty determination with help of a virtual metrological CT (VMCT). It gives an explanation of the adjustments, the input parameters and the execution of the simulation. Furthermore, it discusses the first results of uncertainty determination compared to the method of using calibrated workpieces with the aid of two example cases. T2 - 6th Conference on Industrial Computed Tomography (iCT) CY - Wels, Austria DA - 09.02.2016 KW - simulation KW - Simulation KW - Computertomographie KW - Dimensionelle Metrologie KW - Normung KW - numerische Messunsicherheitsbestimmung KW - computed tomography KW - dimensional metrology KW - standardization KW - numerical uncertainty determination PY - 2016 UR - http://www.ndt.net/article/ctc2016/papers/ICT2016_paper_id17.pdf SP - Paper ID17, 1 EP - 7 AN - OPUS4-35481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Burkert, Andreas A1 - Mietz, Jürgen T1 - Investigations proofing the passive layer stability of stainless steels N2 - The presented investigations have proved the principal suitability of the KorroPad method to assess the passive layer stability of stainless steels. The electrochemical mode of action could be described in detail and limitations of the applicability have been demonstrated. The influence of different surface finishes has been investigated and verified by known methods for describing corrosion resistances. As a result, the increased corrosion susceptibility of two ground surfaces has been detected, but also the corrosion resistance of further surface finishes could be confirmed. KW - Stainless steel KW - KorroPad KW - Passive layer PY - 2016 DO - https://doi.org/10.1002/maco.201408202 VL - 1 IS - 67 SP - 84 EP - 91 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-35545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmack, R. A1 - Eckhardt, B. A1 - Koch, G. A1 - Ortel, Erik A1 - Kraehnert, R. T1 - ZnO coatings with controlled pore size, crystallinity and electrical conductivity N2 - Zinc oxide is a wide bandgap semiconductor with unique optical, electrical and catalytic properties. Many of its practical applications rely on the materials pore structure, crystallinity and electrical conductivity. We report a synthesis method for ZnO films with ordered mesopore structure and tuneable crystallinity and electrical conductivity. The synthesis relies on dip-coating of solutions containing micelles of an amphiphilic block copolymer and complexes of Zn2+ ions with aliphatic ligands. A subsequent calcination at 400 °C removes the template and induces crystallization of the pore walls. The pore structure is controlled by the template polymer, whereas the aliphatic ligands control the crystallinity of the pore walls. Complexes with a higher thermal stability result in ZnO films with a higher content of residual carbon, smaller ZnO crystals and therefore lower electrical conductivity. The paper discusses the ability of different types of ligands to assist in the synthesis of mesoporous ZnO and relates the structure and thermal stability of the precursor complexes to the crystallinity and electrical conductivity of the zinc oxide. KW - conductivity KW - EISA KW - pore templating KW - pore size control KW - ligands KW - zinc oxide PY - 2016 DO - https://doi.org/10.5755/j01.ms.22.1.8634 SN - 1392–1320 VL - 22 IS - 1 SP - 74 EP - 81 PB - Kaunas University of Technology, Lithuania AN - OPUS4-35550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Hübert, Thomas A1 - Boon-Brett, L. A1 - Buttner, W. J. T1 - Sensors for Safety and Process Control in Hydrogen Technologies N2 - This book is on sensors which are regularly deployed in technologies and processes related to hydrogen production, storage, distribution, and use. Not all types of sensors are equally suitable for specific hydrogen applications. The information in this book is intended to help the reader understand the basics of sensors, sensing technologies, sensor applications, and to provide guidelines for choosing the right sensors and the use of them correctly. Correct deployment of appropriate sensors demands knowledge of the sensing principle and of the physical or chemical quantities being measured. Because of the properties of hydrogen, the potential for its vastly increased use in a future low-carbon economy and possible hazards associated with its use, special attention is paid to hydrogen sensors. This book will not focus on the details of the hydrogen technologies nor on the many safety-related aspects of these technologies. Many books are already available on these topics. Instead the detection principle of hydrogen sensors and other sensor types used, in the dynamic and rapidly developing field of hydrogen technologies, are treated in detail in this book. In the first chapter a brief overview is presented on basic hydrogen properties and particularly on those properties which are most relevant for safety and for sensing. To illustrate the extensive field of contemporary applications and the exciting possibilities for near future sensor applications, existing and emerging markets using large quantities of hydrogen are mentioned. The role of sensors as devices for monitoring and control of processes and as safety monitoring devices is outlined. The second chapter gives an introduction to sensing technology and provides the Reader with relevant information pertaining to sensor definitions and classification, sensor metrics, and performance arameters, in addition to background information on sensor preparation technologies and techniques. While there are many books available which provide more exhaustive information on each of these topics, e.g., the level of detail provided in this chapter is sufficient to appreciate the salient features of sensing and sensing Technology which are central to hydrogen safety and monitoring of relevant applications. Chapter 3 provides a comprehensive overview of emerging and commercially available hydrogen sensors, an explanation of their sensing principle, and important aspects of their performance. A comprehensive and up-to-date account of the theory (physical or chemical principles), design, and practical implementations of hydrogen sensors for use in hydrogen related applications is presented. Similar information on chemical sensors for other gases, such as oxygen and trace components, which are also highly important in hydrogen technologies because of potential hazards to human health, process safety or facility performance, is provided in Chapter 4. In Chapter 5 descriptions of physical sensors for temperature, pressure, gas flow, and fire indication, which are also germane for the safe use of hydrogen, are provided. Standards, codes, and regulatory documents, which provide practical advice and legislative requirements regarding sensor deployment and performance, are described in Chapter 6. This chapter also makes reference to the main procedures for sensor testing in gas Standards including precise analytical methods and reference methods. The chapter concludes with a discussion on sensor selection and some installation guidelines are provided. In Chapter 7 traditional and emerging processes and technologies involving hydrogen are described. The application of sensors in processes for the production of hydrogen, hydrogen storage, distribution, and the use of hydrogen in stationary and mobile fuel cells is discussed. Furthermore, the use of hydrogen as a coolant and chemical reagent (medium) in various processes is described. The exploitation of sensors for replacing traditional analytical instrumentation is also discussed. Finally supplementary information is provided on hydrogen properties, measuring quantities, and sensor parameters. KW - Hydrogen Technologies KW - Hydrogen Sensors KW - Gas Sensors, Safety KW - Process Control PY - 2016 SN - 978-1-4665-9654-2 SP - 1 EP - 414 PB - CRC Press Taylor & Francis Group CY - Boca Raton, Florida, USA AN - OPUS4-35507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Spatial and temporal control of thermal waves by using DMDs for interference based crack detection N2 - Active Thermography is a well-established non-destructive testing method and used to detect cracks, voids or material inhomogeneities. It is based on applying thermal energy to a samples’ surface whereas inner defects alter the non-stationary heat flow. Conventional excitation of a sample is hereby done spatially, either planar (e.g. using a lamp) or local (e.g. using a focused laser) and temporally, either pulsed or periodical. In this work we combine a high power laser with a Digital Micromirror Device (DMD) allowing us to merge all degrees of freedom to a spatially and temporally controlled heat source. This enables us to exploit the possibilities of coherent thermal wave shaping. Exciting periodically while controlling at the same time phase and amplitude of the illumination source induces – via absorption at the sample’s surface - a defined thermal wave propagation through a sample. That means thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mm-range for modulation frequencies below 10 Hz which is perfectly met by DMD technology. This approach gives us the opportunity to transfer known technologies from wave shaping techniques to thermography methods. We will present experiments on spatial and temporal wave shaping, demonstrating interference based crack detection. T2 - Photonics West 2016, OPTO, 9761 CY - San Francisco, Cal, USA DA - 15.02.2016 KW - Thermal Waves KW - Laser KW - DMD KW - Active Thermography PY - 2016 AN - OPUS4-35586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik A1 - Kreutzbruck, M. A1 - Ziegler, Mathias T1 - Spatial and temporal control of thermal waves by using DMDs for interference based crack detection N2 - Active Thermography is a well-established non-destructive testing method and used to detect cracks, voids or material inhomogeneities. It is based on applying thermal energy to a samples’ surface whereas inner defects alter the nonstationary heat flow. Conventional excitation of a sample is hereby done spatially, either planar (e.g. using a lamp) or local (e.g. using a focused laser) and temporally, either pulsed or periodical. In this work we combine a high power laser with a Digital Micromirror Device (DMD) allowing us to merge all degrees of freedom to a spatially and temporally controlled heat source. This enables us to exploit the possibilities of coherent thermal wave shaping. Exciting periodically while controlling at the same time phase and amplitude of the illumination source induces – via Absorption at the sample’s surface - a defined thermal wave propagation through a sample. That means thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mmrange for modulation frequencies below 10 Hz which is perfectly met by DMD technology. This approach gives us the opportunity to transfer known technologies from wave shaping techniques to thermography methods. We will present experiments on spatial and temporal wave shaping, demonstrating interference based crack detection. T2 - Photonics West 2016, OPTO, 9761 CY - San Francisco, CA, USA DA - 15.02.2016 KW - Active thermography KW - Thermal wave KW - Spatial light modulation KW - Crack detection KW - DMD KW - DMD coupled laser PY - 2016 DO - https://doi.org/10.1117/12.2210918 SN - 0277-786X VL - 9761 SP - 97610N-1 EP - 97610N-13 AN - OPUS4-35587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Real-world examples of how to calculate a KCRV N2 - In this presentation the different ways are presented, which are used to calculate in practice the key comparison reference value. T2 - EURAMET TC Metrology in Chemistry Meeting CY - Geel, Belgium DA - 03.02.2016 KW - key comparison KW - CCQM KW - Degree of equivalence PY - 2016 AN - OPUS4-35573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abali, B. E. A1 - Wu, Cheng-Chieh A1 - Müller, W.H. T1 - An energy-based method to determine material constants in nonlinear rheology with applications N2 - Many polymer-type materials show a rate-dependent and nonlinear rheological behavior. Such a response may be modeled by using a series of spring-dashpot systems. However, in order to cover different time scales the number of systems may become unreasonably large. A more appropriate treatment based on continuum mechanics will be presented herein. This approach uses representation theorems for deriving material equations and allows for a systematic increase in modeling complexity. Moreover, we propose an approach based on energy to determine thematerial parameters.This method results in a simple linear regression problemeven for highly nonlinearmaterial equations. Therefore, the inverse problem leads to a unique solution. The significance of the proposed method is that the stored and dissipated energies necessary for the procedure are measurable quantities. We apply the proposed method to a 'semi-solid' material and measure its material parameters by using a simple-shear rheometer. KW - Material equations KW - Constitutive relations KW - Nonlinear rheology KW - Simple-shear rheometer KW - Inverse analysis PY - 2016 DO - https://doi.org/10.1007/s00161-015-0472-z SN - 0935-1175 SN - 1432-0959 VL - 28 IS - 5 SP - 1221 EP - 1246 PB - Springer CY - Berlin AN - OPUS4-34333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unnikrishnakurup, Sreedhar A1 - Krishnamurthy, C. V. A1 - Balasubramaniam, Krishnan T1 - Monitoring TIG welding using Infrared Thermography - Simulations and Experiments N2 - In the current work a 3D model has been developed to predict the thermal cycles during the Tungsten Inert Gas welding of Aluminum 2219. This paper describes the step by step procedure adopted to get the actual cooling rate during the TIG welding process both experimentally and numerically. The model was developed in the COMSOL Finite Element Package and considered a Gaussian heat distribution. The developed model then validated using the experimental data collected in field experiments on actual large propellant tanks. Temperature measurements were performed using Infrared Camera. Results show a close comparison between model and experiment. KW - Image Analysis KW - Infrared Thermography KW - Online Monitoring KW - Finite Element Method PY - 2016 DO - https://doi.org/10.15199/48.2016.04.02 SN - 0033-2097 IS - 4/2016 SP - 6 EP - 9 AN - OPUS4-35743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartholmai, Matthias A1 - Kammermeier, Michael A1 - Koeppe, Tabea A1 - Werner, Klaus-Dieter ED - Nicoletto, G. ED - Pastrama, S.D. ED - Emri, I. T1 - High dynamic measurement of strain and acceleration using a multichannel measuring system with single cable serial connection N2 - Strain and acceleration measurement during high dynamic drop tests, e.g., of containments for dangerous goods is performed using high speed multichannel measuring systems. So far established and operated systems need a cable connection of every strain gauge and acceleration sensor with the measuring device, often counting up to a number of more than 100 cables, corresponding to the number of applied sensors. The result is a massive cable harness consisting of all single cables, which is difficult to handle and causes a number of practical problems. An innovative approach is proposed by using a single cable measuring system, consisting of measuring modules with data bus connection and local data acquisition. Promising results were presented in a previous study. This paper follows up with additional results from full-scale testing of a further enhanced single cable system for the application in drop tests. T2 - 32nd DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Multichannel measuring KW - Single cable serial connection KW - Dangerous goods container KW - Drop test KW - High impact testing PY - 2016 DO - https://doi.org/10.1016/j.matpr.2016.03.023 SN - 2214-7853 VL - 3 IS - 4 SP - 931 EP - 935 PB - Elsevier Ltd. AN - OPUS4-35689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Levee inspection - geophysics between science, standards, reliability and budgets N2 - Numerous case histories show evidence that geophysical methods are valuable tools for levee inspection and monitoring. National and international standards and recommendations recommend the use of geophysics for a variety of tasks. However, in some cases reported have been flaws missed or false indications given. Due to the larger variety in type, size and construction of levees and the even larger variety of potential tasks and targets the success of geophysical surveys still pretty much depends on the available budget and the experience and capabilities of the clients and contractors involved. It is strongly recommended that all relevant parties agree on the detailed objectives of the survey, required accuracy and reliability of the results and any follow up measures. For the most common tasks more research and practical work using techniques as POD (probability of detection), which are well established in other fields of non-destructive testing, would be of benefit. T2 - SAGEEP 2016 CY - Denver, CO, USA DA - 20.03.2016 KW - Levee KW - Geophysics KW - Inspection PY - 2016 SP - paper levees 07, 1 EP - 4 AN - OPUS4-35705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Bald, Ilko T1 - Decomposition of DNA nucleobases by laser irradiation of gold nanoparticles monitored by surface-enhanced Raman scattering N2 - Different approaches have been proposed to treat cancer cells using gold nanoparticles (AuNPs) in combination with radiation ranging from infrared lasers to high-energy ion beams. Here we study the decomposition of the DNA/RNA nucleobases thymine (T) and uracil (U) and the well-known radiosensitizer 5-bromouracil (BrU) in close vicinity to AuNPs, which are irradiated with a nanosecond pulsed laser (532 nm) matching the surface plasmon resonance of the AuNPs. The induced damage of nucleobases is analyzed by UV−vis Absorption spectroscopy and surface-enhanced Raman scattering (SERS). A clear DNA damage is observed upon laser irradiation. SERS spectra indicate the fragmentation of the aromatic ring system of T and U as the dominant form of damage, whereas with BrU mainly the cleavage of the Br−C bond and formation of Br− ions is observed. This is accompanied by a partial transformation of BrU into U. The observed damage is at least partly ascribed to the intermediate formation of lowenergy electrons from the laser-excited AuNPs and subsequent dissociative electron attachment to T, U, and BrU. These reactions represent basic DNA damage pathways occurring on the one hand in plasmon-assisted cancer therapy and on the other hand in conventional cancer radiation therapy using AuNPs as sensitizing agents. KW - Gold nanoparticles KW - SERS KW - Electrons KW - DNA damage KW - Gold-Nanopartikel KW - Elektronen KW - DNA-Schädigung PY - 2016 DO - https://doi.org/10.1021/acs.jpcc.5b10564 VL - 120 IS - 5 SP - 3001 EP - 3009 PB - AMER CHEMICAL SOC AN - OPUS4-35673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kühn, Julius T1 - Composition and chemistry of Pd-Ni-Co thin film alloys for hydrogen related applications N2 - The discovery and design of high performance Pd-alloys is of great interest for the use of hydrogen as a future energy carrier. Therefore hydrogen has to be detected, separated from other gases and stored. In this respect this thesis presents the combinatorial synthesis and characterization of the ternary Pd-Ni-Co alloy System over a wide composition range based on so-called thin film alloy libraries. Those libraries are model systems to characterize a large number of alloy compositions at the same time. The sputter-deposition process is optimized for the gradient of the Pd concentration on the surface of the alloy library by the use of electron-excited Auger electron spectroscopy. The scientific goal of this work is the experimental Investigation of adsorbate-induced surface segregation phenomena on alloy libraries. The surface and bulk compositions of an alloy library are studied after deposition, H2 exposure and H2S poisoning. The co-segregation of Ni and Co to the surface is observed. The segregation process is influenced by the oxidation of Ni and Co due to the contact with ambient air, by H2 and by H2S poisoning. Also at very high Pd concentrations in the range of 87 at.% to 97 at.%, which is interesting for the detection of very low H2-Concentrations in air, the co-segregation of Ni and Co takes place. The poisoning effects were investigated in detail on a pre-selected Pd-Ni-Co alloy by photoelectron spectroscopy (XPS, HAXPES) in addition to AES and EDX. The composition profile of the alloy on the nm scale is acquired and the surface and bulk chemistry is discussed before and after poisoning. The composition of the alloy only changed within the first 3 nm due to H2S exposure. In the ternary Pd-Ni-Co alloy system Pd is present in its metallic state, while Ni and Co show several oxidation states. The presented concepts of ternary alloy development pave the way for the systematic synthesis and characterization of new ternary transition metal alloy systems. KW - Hydrogen sensor KW - Library of ternary Pd-alloys KW - AES KW - (HAX)PES KW - REM/EDX KW - Wasserstoffsensor KW - Bibliothek ternärer Pd-Legierungen PY - 2016 DO - https://doi.org/10.14279/depositonce-5002 SP - 1 EP - 127 PB - Technische Universität CY - Berlin AN - OPUS4-35680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Petrov, Sergej A1 - Neumann, Patrick P. A1 - Werner, Klaus-Dieter A1 - Wosniok, Aleksander A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Nicoletto, G. ED - Pastrama, S.D. ED - Emri, I. T1 - Concept for investigating mechanical and thermal impacts on distributed subsurface gas monitoring N2 - A multifunctional sensor in line shape was developed and introduced in previous work for measuring of gas concentrations, temperature change, and strain. A current field study focuses on a spatially distributed monitoring of subsurface CO 2 gas storage sites in near real time. Mechanical impacts, e.g., caused by construction work, denudation, and seismic activity, can affect the integrity of underground gas storage sites. Thermal or moisture impacts, e.g., caused by weather conditions, can influence the gas Distribution behavior. In this paper, we briefly describe the setup of a CO 2 injection soil test field. This setup contains actuating elements for the investigation of mechanical and thermal impacts on distributed subsurface gas monitoring. A concept is given for evaluating these impacts and first experimental results are presented. T2 - 32nd DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Linear sensor KW - Distributed sensor KW - Monitoring of CO 2 KW - Subsurface monitoring KW - Gas storage areas KW - Membrane-based gas sensing KW - Fibre optical sensing PY - 2016 DO - https://doi.org/10.1016/j.matpr.2016.03.060 SN - 2214-7853 VL - 3 IS - 4 SP - 1124 EP - 1128 PB - Elsevier Ltd. AN - OPUS4-35688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Development of a laser induced plasma ion source coupled to ambient mass spectrometry N2 - Only a few years after the invention of the laser, the concept of laser microprobe mass spectrometry (LMMS), a technique which employed intense laser radiation for ion generation, was introduced. In these early studies at excessive irradiation microplasma formation could be observed to be an effective channel for ion formation. However, this plasma generation in vacuum led to undesired distortions of the mass analyzers and, thus, was discarded as an analytical ion source. Under ambient conditions, the surrounding air effectively cools the plasma cloud, making the plasma more controllable. The resulting laser induced plasma is nowadays commonly used in laser induced breakdown spectroscopy (LIBS) applications as excitation source for optical emission spectroscopy experiments. However, little effort has been made to introduce a LIBS plasma as a promising ion source for ambient mass spectrometry. The main hindrance is the transient character of laser induced plasmas that typically only has a lifetime on the order of several microseconds. This drastically reduces the duty cycle of these plasma sources. After these microseconds, the generated ions recombinate to uncharged atoms and even newly bound molecules, making them inaccessible to mass-to-charge analyzers. The advent of high repetition lasers together with the ever growing knowledge about manipulation of charged species at atmospheric pressures allow overcoming these obstacles. This presentation will introduce an ionization scheme using a laser induced plasma as the primary ion source. We believe that this novel ionization strategy will pave the way for future applications in ambient mass spectrometry. T2 - 5. Berliner Chemie Symposium CY - Berlin, Germany DA - 12.04.2016 KW - Laser induced plasma KW - Time-of-flight mass spectrometry KW - Ambient mass spectrometry KW - Ionization KW - Laser induziertes Plasma KW - Flugzeitmassenspektrometer KW - Atmosphärendruckmassenspektrometrie KW - Ionisierung PY - 2016 AN - OPUS4-35732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Innovative seismic and resistivity tools for determining the diameter of jet grouting columns N2 - Jet grouting is used for soil improvement, foundation support and groundwater low control all over the world. It is well accepted and subject of standardization in many countries. However, some issues with the method remain. As the grout columns are produced in the subsurface without visual control in an often inhomogeneous soil, the prediction of the column’s diameter is still a challenge. All methods applied so far have their limitations. The approach presented in this study is twofold. At Colorado School of Mines a resistivity probe has been developed, which is pushed into the fresh grout directly after production. ERT sections are measured and inverted. Given some background information is available, the diameter of the columns can be evaluated. At BAM the focus has been on post-production investigations using seismic borehole methods. After hardening of the concrete seismic waves are sent through the column downhole (sensors placed in a casing in the column’s axis, source on top) and crosshole (source and sensor in boreholes on opposite sides of the column). We have developed a scheme to evaluate the diameter of the column based on travel time measurements without calibration. As this method is eventually more time and cost intensive we assume its application mainly for test columns. These are casted and dug out for visual inspection to determine appropriate grouting parameters. Our method would replace the often very cost intensive visual inspection. Both approaches have been tested at three test columns produced at BAM’s test site at Horstwalde, Germany and on an actual constructions site. Both methods have been in good agreement with the diameters predicted by the jet grouting contractors, which were confirmed in one case by mechanical measurements. T2 - SAGEEP 2016 CY - Denver, CO, USA DA - 20.03.2016 KW - Jet grouting KW - Diameter KW - Quality assurance KW - Seismic PY - 2016 AN - OPUS4-35708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoesl, Simone A1 - Neumann, B. A1 - Techritz, Sandra A1 - Sauter, G. A1 - Simon, R. A1 - Schlüter, H. A1 - Linscheid, M. W. A1 - Theruing, F. A1 - Müller, Larissa A1 - Jakubowski, Norbert T1 - Internal standardization of LA-ICP-MS immunoimaging via printing of universal metal spiked inks onto tissue sections N2 - Formalin-fixed paraffin-embedded (FFPE) specimen from biopsy materials are a widespread sample format for pathologists and medical researchers. Pathologists are archiving vast numbers of FFPE samples which can be stored for decades. Conventional immunohistochemical staining (IHC) of biomarkers on FFPE tissue sections is one of the most important analytical techniques for cancer diagnosis and pathology in general. However standardization for IHC samples and quality management is tedious and differs significantly from clinic to clinic. Combining established IHC staining strategies with modern mass spectrometry mediated methods would increase it`s potential and enable access of large FFPE archives for multiplexed quantitation purposes. In this work element mass spectrometry and a new ink-jet printed internal standardization approach was successfully combined with IHC staining to facilitate quantitative multiplex assays for archived FFPE samples. The printing strategy improves elemental image resolution and reproducibility of paraffin embedded breast cancer tissue sections in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) using conventional IHC staining as a model system to investigate the new capabilities of this technique. For the internal standardization we applied a conventional CD-ink-jet printer to print a metal spiked ink onto the top of thin layer tissue sections with constant density. Printing was carried out in a direct comparison to an iodination of the tissue section as previously described as an alternative standardization method. The use of the printed internal standard allowed correction of the fluctuation during the laser ablation process and compensated instrumental drift effects. Mediated by the ink correction approach we achieved better signal-to-background-ratios (SBR) of 74 and better spatial resolution of 30 µm compared to iodination (SBR=23). This improved performance was demonstrated on tumorous areas in FFPE breast cancer tissue sections and allowing detection of Her-2 in tumorous areas of this tissue with significantly improved contrast. KW - Internal standardization KW - LA-ICP-MS KW - Immuno imaging PY - 2016 DO - https://doi.org/10.1039/c5ja00409h SN - 0267-9477 SN - 1364-5544 VL - 31 IS - 3 SP - 801 EP - 808 AN - OPUS4-35711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Ebert, S. A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Nicoletto, G. ED - Dan Pastrama, S. ED - Emri, I. T1 - Inverse calibration routine for linear soil gas sensors N2 - Gas sensors in linear form based on the measuring principle of gas selective permeability through a membrane were developed and introduced for the detection and quantification of gas concentrations. A current field study focuses on measuring CO2 concentrations for a spatially distributed monitoring of subsurface CO2 gas storage sites in near real time. A 400 m² test site and a corresponding laboratory system were built up to characterize, validate, and optimize the sensor. A calibration routine was developed, which can be applied subsequently to underground installation. First measurement results indicate the potential of the method. T2 - 32nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Linear sensor KW - Distributed sensor KW - Subsurface monitoring KW - Gas storage areas KW - Membrane-based gas sensing KW - Calibration PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S221478531600256X DO - https://doi.org/doi:10.1016/j.matpr.2016.03.051 SN - 2214-7853 VL - 3 IS - 4 SP - 1074 EP - 1078 PB - Elsevier Ltd. AN - OPUS4-35633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer A1 - Kreutzbruck, Marc A1 - Commandeur, Colin A1 - Pelkner, Matthias T1 - Development of adapted GMR-probes for automated detection of hidden defects in thin steel sheets N2 - Thin steel sheets with a thickness of 0.3 mm and less are the base materials of many everyday life products (cans, batteries, etc.). Potential inhomogeneities such as non-metallic inclusions inside the steel can lead to a rupture of the sheets when it is formed into a product such as a beverage can. Therefore, there is a need to develop automated NDT techniques to detect hidden defects and inclusions in thin sheets during production. For this purpose Tata Steel Europe and BAM, the Federal Institute for Materials Research and Testing (Germany), collaborate in order to develop an automated NDT-system. Defect detection systems have to be robust against external influences, especially when used in an industrial environment. In addition, such a facility has to achieve a high sensitivity and a high spatial resolution in terms of detecting small inclusions in the μm-regime. In a first step, we carried out a feasibility study to determine which testing method is promising for detecting hidden defects and inclusions inside ferrous thin steel sheets. Therefore, two methods were investigated in more detail – magnetic flux leakage testing (MFL) using giant magneto resistance sensor arrays (GMR) as receivers [1,2] and eddy current testing (ET). The capabilities of both methods were tested with 0.2 mm-thick steel samples containing small defects with depths ranging from 5 μm up to 60 μm. Only in case of GMRMFL-testing, we were able to detect parts of the hidden defects with a depth of 10 μm trustworthily with a SNR better than 10 dB. Here, the lift off between sensor and surface was 250 μm. On this basis, we investigated different testing scenarios including velocity tests and different lift offs. In this contribution we present the results of the feasibility study leading to first prototypes of GMR-probes which are now installed as part of a demonstrator inside a production line. T2 - Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, MN, USA DA - 26.07.2015 KW - GMR KW - NDT PY - 2016 DO - https://doi.org/10.1063/1.4940464 VL - 1706 SP - Article Number: 020018 PB - Amer institute physics CY - Melville, New York, USA AN - OPUS4-36100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moraleja, I. A1 - Esteban-Fernández, Diego A1 - Lázaro, A. A1 - Humanes, B. A1 - Neumann, B. A1 - Tejedor, A. A1 - Mena, M. A1 - Jakubowski, Norbert A1 - Gómez-Gómez, M. T1 - Printing metal-spiked inks for LA-ICP-MS bioimaging internal standardization: comparison of the different nephrotoxic behavior of cisplatin, carboplatin, and oxaliplatin N2 - The study of the distribution of the cytostatic drugs cisplatin, carboplatin, and oxaliplatin along the kidney may help to understand their different nephrotoxic behavior. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) allows the acquisition of trace element images in biological tissues. However, results obtained are affected by several variations concerning the sample matrix and instrumental drifts. In this work, an internal standardization method based on printing an Ir-spiked ink onto the surface of the sample has been developed to evaluate the different distributions and accumulation levels of the aforementioned drugs along the kidney of a rat model. A conventional ink-jet printer was used to print fresh sagittal kidney tissue slices of 4 μm. A reproducible and homogenous deposition of the ink along the tissue was observed. The ink was partially absorbed on top of the tissue. Thus, this approach provides a pseudo-internal standardization, due to the fact that the ablation sample and internal standard take place subsequently and not simultaneously. A satisfactory normalization of LA-ICP-MS bioimages and therefore a reliable comparison of the kidney treated with different Pt-based drugs were achieved even for tissues analyzed on different days. Due to the complete ablation of the sample, the transport of the ablated internal standard and tissue to the inductively coupled plasma-mass spectrometry (ICP-MS) is practically taking place at the same time. Pt accumulation in the kidney was observed in accordance to the dosages administered for each drug. Although the accumulation rate of cisplatin and oxaliplatin is high in both cases, their Pt distributions differ. The strong nephrotoxicity observed for cisplatin and the absence of such side effect in the case of oxaliplatin could explain these distribution differences. The homogeneous distribution of oxaliplatin in the cortical and medullar areas could be related with its higher affinity for cellular transporters such as MATE2-k. KW - Bioimaging KW - LA-ICP-MS KW - Cisplatin KW - Standardization KW - Printed internal standard KW - Pt-based drugs KW - Nephrotoxicity PY - 2016 DO - https://doi.org/10.1007/s00216-016-9327-0 SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 9 SP - 2309 EP - 2318 AN - OPUS4-36110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ryan, T. M. A1 - Xun, Y. A1 - Cowieson, N. P. A1 - Mata, J. P. A1 - Jackson, A. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Kirby, N. A1 - McGillivray, D. T1 - Combined pressure and temperature denaturation of ribonuclease A produces alternate dentatured states N2 - Protein folding, unfolding and misfolding have become critically important to a range of health and industry applications. Increasing high temperature and high pressure are used to control and speed up reactions. A number of studies have indicated that these parameters can have a large effecton protein structure and function. Here we describe the additive effects of these parameters on the small angle scattering behaviour of ribonuclease A. We find that alternate unfolded structures can be obtained with combined high pressure and temperature treatment of the protein. KW - Protein unfolding KW - Small angle scattering KW - Ribonuclease A KW - High pressure PY - 2016 DO - https://doi.org/10.1016/j.bbrc.2016.03.135 SN - 0006-291X IS - 473 SP - 834 EP - 839 PB - Academic Press Inc Elsevier Science CY - San Diego, USA AN - OPUS4-36052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Process analytical technology for resource analytics – The role of reference materials N2 - Resource Analytics with the help of process analytical technology and the use of online methods is becoming increasingly important for mining and processing technologies and for the recovery of raw materials from secondary raw materials. Current online analytical methods like laser-induced breakdown spectroscopy (LIBS), X-ray fluorescence analysis (RFA), or Raman spectroscopy for the characterization of primary and secondary raw materials are increasingly being used in close association with the technologies for exploration and extraction, mechanical and metallurgical processing, as well as for recycling. Because of the complex matrices such methods are a considerable challenge at the same time. The use of reference materials, which are derived from appropriate matrices, can considerably shorten calibration and method development times. As an example, the development of an online process control method for recovery of phosphorus from sewage sludge ashes is discussed. A combination of LIBS and RFA was developed for the determination of element contents in sewage sludge ashes and their products coming from a thermo-chemical reprocessing step, which removes pollutants. T2 - Analytica Conference CY - München, Germany DA - 10.05.2016 KW - Resource Analytics KW - Ressourcenanalytik KW - Prozessanalytik KW - Process Analytical Technology PY - 2016 AN - OPUS4-36043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. T1 - Systematic approach for online spectroscopy in technical systems - Experimental design for Raman Spectroscopy in micro emulsions N2 - Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied for short-chained alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactants, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process. Another promising approach is the processing within a microemulsion by using a suitable surfactant system. This maintains a large interface between catalyst and reactants, as well as the possibility of catalyst recycling via downstream phase separation in a settler. Optimized processing within the three-phase region in accordance with Kahlweit fish leads to an efficient product separation, while the valuable catalyst and surfactant can be recycled into the process. In this work we present reaction monitoring of Rh-catalyzed hydroformylation of 1 dodecene. Experiments were conducted on a specialized laboratory setup, which allows coupling of different online spectroscopic methods (Raman, HR-NMR, LF-NMR, UV/VIS) under process-similar conditions. The focus of this contribution lies on results of high-resolution Online-NMR obtained during calibration experiments for development of a multivariate model for Raman spectroscopy, which will be part of another contribution. T2 - Analytica Conference CY - München, Germany DA - 10.05.2016 KW - Prozess-Sensoren KW - Process Analytical Technology KW - Hydroformylation KW - Design of Experiments PY - 2016 AN - OPUS4-36044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Road-map for purity determination N2 - From several CCQM studies (CCQM-P107, CCQM-K72 and CCQM-P149) conclusions can be drawn for the purity assessment of a pure (metallic) element. These conclusions will be put together in this document in order to assist all NMIs/DIs in performing a purity assessment, whenever needed. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - Purity KW - Metrology KW - Traceability PY - 2016 AN - OPUS4-36063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Applicability of CCQM-P149 to support CMCs N2 - CCQM-P149 is an attempt to obtain a snapshot on actual procedures the NMIs and DIs within CCQM-IAWG applied to the purity characterization of their “fit for purpose” elemental Standards. This presentation describes how the results of CCQM-P149 may be used to underpin calibration and measurement capabilities being claimed in the BIPM database. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - metrology KW - purity KW - traceability PY - 2016 AN - OPUS4-36064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Using information from CC Tables for supporting CMC claims N2 - Core capability tables list the skills and experiences, which at least partially are needed to successfully carry out a specific analytical task within the IAWG. The required skills and experiences, so-called core capabilities (CC), are identified for each analytical procedure. The summarized CC tables are listed in the appendix of each report on the corresponding key comparison or pilot study. These CC tables enable us to demonstrate that we have the analytical procedure we claim under control by means of other Key Comparison, which do not exactly meet the claimed calibration and measurement capability. This is especially important for: a) fields where no Key Comparison is available, b) Revision of CMC claims or c) when a participation in a Key Comparison was not possible. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - metrology KW - traceability PY - 2016 AN - OPUS4-36066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Staude, Andreas T1 - Computed tomography and its potential for cultural heritage studies N2 - Since the advent of industrial computed tomography (CT), this new analysis method has been used also for the investigation of objects of cultural heritage and art. CT provides the possibility to determine the inner and outer surfaces and to investigate the material structure without causing damage to the valuable objects. In this talk I will present examples of measurements performed at BAM, which demonstrate what CT can do for objects of diverse materials and for different objectives. T2 - Italian-German Worshop on "Technology and infrastructures for Cultural Heritage" CY - Bode-Museum, Berlin, Germany DA - 12.04.2016 KW - Computed tomography KW - Computertomographie KW - Cultural heritage KW - Art KW - Archaeology KW - Kulturelles Erbe KW - Kunst KW - Archäologie PY - 2016 AN - OPUS4-36162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - The Analytical centrifuge – an additional tool to optimize ceramic slurries for spray drying N2 - Spray drying is a widely used process step in ceramic technology to convert fine grained raw powders to free-flowing granules. Type and amount of the organic additives (dispersants, binders and plasticizers) define viscosity and stability of the slurry, the granulate structure and the compaction behaviour. Alumina and Zirconia powders were characterized with regard to particle size, shape and specific surface area (BET). Zeta-potential measurements by Stabino® were used to investigate the effect of different dispersants on slurry stability. Unfortunately, this method is restricted to suspensions with less than about 30% by weight of solid content. The multi-sample analytical centrifuge LUMiSizer® overcomes this problem. This device enables analysis of the separation behaviour of suspensions over a wide range of solid content. On the basis of position and time resolved photometric detection of transmitted light, it is possible to determine the instability index, the sedimentation velocity, and the sediment height in dependence of type and amount of organic additives at various centrifugal accelerations. Additional information is obtained from the shape of the transmission profiles. Based on LUMiSizer® measurements, suitable additive concentrations were derived. Thereby, the number of investigations by viscometry and spray drying experiments can be significantly reduced. Finally, it was possible to produce alumina, zirconia and ZTA aqueous slurries with up to 80 weight-% of solid. The optimized suspensions were successfully spray dried and the resulted granules show good compaction behaviour. T2 - Jahrestagung der Deutschen Keramischen Gesellschaft und Symposium Hochleistungskeramik CY - Freiberg, Germany DA - 07.03.2016 KW - Analytical centrifuge KW - Ceramic suspension KW - Slurry KW - Spray drying KW - Granules PY - 2016 AN - OPUS4-36130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zientek, Nicolai A1 - Laurain, C. A1 - Meyer, Klas A1 - Paul, Andrea A1 - Engel, D. A1 - Guthausen, G. A1 - Kraume, M. A1 - Maiwald, Michael T1 - Automated data evaluation and modelling of simultaneous F-19-H-1 medium-resolution NMR spectra for online reaction monitoring N2 - Medium-resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and processmonitoring. In contrast to high-resolution onlineNMR (HR-NMR),MR-NMRcan be operated under rough environmental conditions. A continuous re-circulating stream of reaction mixture fromthe reaction vessel to the NMR spectrometer enables a non-invasive, volume integrating online analysis of reactants and products. Here, we investigate the esterification of 2,2,2-trifluoroethanol with acetic acid to 2,2,2-trifluoroethyl acetate both by 1H HR-NMR (500MHz) and 1H and 19F MRNMR (43MHz) as amodel system. The parallel online measurement is realised by splitting the flow,which allows the adjustment of quantitative and independent flow rates, both in the HR-NMR probe as well as in the MR-NMR probe, in addition to a fast bypass line back to the reactor. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra are treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprise (i) direct integration, (ii) automated line fitting, (iii) indirect hard modelling (IHM) and (iv) partial least squares regression (PLS-R). To assess the potential of these evaluation strategies for MR-NMR, prediction results are compared with the line fitting data derived from the quantitative HR-NMR spectroscopy. Although, superior results are obtained from both IHM and PLS-R for 1H MR-NMR, especially the latter demands for elaborate data pretreatment, whereas IHM models needed no previous alignment. KW - NMR KW - 1H-NMR KW - 19F-NMR KW - Medium-resolution NMR KW - Online NMR KW - Quantitative NMR KW - Reaction monitoring KW - Data processing KW - Automation KW - Process analytical technology KW - IHM KW - Indirect hard modeling KW - Chemometrics KW - PLS-R KW - Partial least squares regression PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/mrc.4216/abstract DO - https://doi.org/doi:10.1002/mrc.4216 VL - 54 SP - 513 EP - 520 PB - John Wiley & Sons, Ltd CY - Hoboken, New Jersey, USA AN - OPUS4-36135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Book review: Freddy Adams and Carlo Barbante - Chemical imaging analysis N2 - In this book many practical hints are given and analytical problems are discussed by the authors from their own experiences. A critical assessment of the methods is given, which is most important for decision makers to select a good combination of complementary methods to solve practical analytical problems. KW - Chemical imaging analysis KW - Surface analysis KW - Interface analysis PY - 2016 DO - https://doi.org/10.1007/s00216-016-9517-9 SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 16 SP - 4199 EP - 4201 PB - Springer AN - OPUS4-36216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Nietzold, Carolin A1 - Weise, Matthias A1 - Unger, Wolfgang A1 - Alnabulsi, Saad A1 - Moulder, John T1 - XPS depth profiling of an ultrathin bioorganic film with an argon gas cluster ion beam N2 - The growing interest in artificial bioorganic Interfaces as a platform for applications in emerging Areas as personalized medicine, clinical diagnostics, biosensing, biofilms, prevention of biofouling, and other fields of bioengineering is the origin of a need for in Detail multitechnique characterizations of such layers and interfaces. The in-depth analysis of biointerfaces is of special interest as the properties of functional bioorganic coatings can be dramatically affected by in-depth variations of composition. In worst cases, the functionality of a device produced using such coatings can be substantially reduced or even fully lost. KW - XPS KW - Ar gas cluster gun KW - Depth profiling KW - Bioorganic film PY - 2016 UR - http://scitation.aip.org/content/avs/journal/bip/11/2/10.1116/1.4948341 DO - https://doi.org/10.1116/1.4948341 SN - 1934-8630 VL - 11 IS - 2 SP - 029603-1 EP - 029603-5 PB - American Vacuum Society CY - New York AN - OPUS4-36218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gemeinert, Marion T1 - Stability assessment of ceramic high dielectric N2 - Resolution of capacitive sensors can be improved enormously by replacement of the dielectric material between the capacitor plates (e.g. air-dielectric) by a dielectric fluid with high permittivity. High dielectric liquid dispersions of ceramic micro and nano powders should be qualified as dielectric fluid with longtime shelf life. For this purpose it was necessary to produce stabilized ceramic suspensions with high particle concentration and to investigate sedimentation processes of the particles. Characterization of particles was done by use of zeta potential measurement, gas adsorption measurements (BET), density measurement with gas pycnometer as well as particle sizing by ultrasound spectroscopy and by use of an optical centrifuge. Shelf life of optimized electrostatic and steric stabilized ceramic suspension was investigated by use of an optical centrifuge, a LUMISizer 651 MW (LUM Ltd.) with STEP technology and front tracking analysis. Two different wave lengths – NIR (865 nm) and blue light (470 nm) were available for examination. Centrifugation measurements with different rotation speed were used to study the rheological behavior and the sedimentation process. By this way it was possible to achieve accelerated stability determination. Measured values could be used to simulate the sedimentation process under gravity acceleration and to predict shelf life for suspensions with different dispersants. T2 - PARTEC 2016 CY - Nürnberg, Germany DA - 19.04.2016 KW - Ceramic dispersion KW - Stability assessment KW - Analytical centrifuge KW - Shelf life prediction PY - 2016 AN - OPUS4-36184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharlach, C. A1 - Müller, Larissa A1 - Wagner, S. A1 - Kobayashi, Y. A1 - Kratz, H. A1 - Ebert, M. A1 - Jakubowski, Norbert A1 - Schellenberger, E. T1 - LA-ICP-MS allows quantitative microscopy of europium-doped iron oxide nanoparticles and is a possible alternative to ambiguous Prussian blue iron staining N2 - The development of iron oxide nanoparticles for biomedical applications requires accurate histological evaluation. Prussian blue iron staining is widely used but may be unspecific when tissues contain substantial endogenous iron. Here we tested whether microscopy by laser ablation coupled to inductively coupled plasma mass spectrometry (LA-ICP-MS) is sensitive enough to analyze accumulation of very small iron oxide particles (VSOP) doped with europium in tissue sections. KW - Atherosclerotic plaques KW - LA-ICP-MS microscopy KW - Quantification KW - Element microscopy KW - Histology PY - 2016 DO - https://doi.org/10.1166/jbn.2016.2230 SN - 1550-7033 SN - 1550-7041 VL - 12 IS - 5 SP - 1001 EP - 1010 AN - OPUS4-36189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heck, Christian T1 - Plasmonic gold nanolenses self-assembled by DNA origami N2 - Surface-enhanced Raman scattering (SERS) exploits the enhancement of electromagnetic fields in close vicinity of plasmonic nanostructures. The nanometer-scale spatial arrangement of plasmonic metal nanoparticles and analyte molecules has a significant effect on the observed signal enhancements and represents a great challenge in this technique. Especially interesting effects are expected for complex gold nanolenses (AuNLs), consisting of three or more differently-sized AuNPs. We use DNA origami to assemble AuNLs with 10, 20 and 60 nm AuNPs, arranged in three different geometries. Using correlated AFM and Raman spectroscopy, and probing single AuNLs, we systematically examined the SERS properties of the three different assemblies. T2 - DNA Nanotechnology 2016 CY - Jena, Germany DA - 19.05.2016 KW - gold nanoparticles KW - DNA origami KW - plasmonics PY - 2016 AN - OPUS4-36205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prinz, J. A1 - Heck, Christian A1 - Ellerik, L. A1 - Merk, V. A1 - Bald, Ilko T1 - DNA origami based Au–Ag-core–shell nanoparticle dimers with single-molecule SERS sensitivity N2 - DNA origami nanostructures are a versatile tool to arrange metal nanostructures and other chemical entities with nanometer precision. In this way gold nanoparticle dimers with defined distance can be constructed, which can be exploited as novel substrates for surface enhanced Raman scattering (SERS). We have optimized the size, composition and arrangement of Au/Ag nanoparticles to create intense SERS hot spots, with Raman enhancement up to 10^10, which is sufficient to detect single molecules by Raman scattering. This is demonstrated using single dye molecules (TAMRA and Cy3) placed into the center of the nanoparticle dimers. In conjunction with the DNA origami nanostructures novel SERS substrates are created, which can in the future be applied to the SERS analysis of more complex biomolecular targets, whose position and conformation within the SERS hot spot can be precisely controlled. KW - single molecule spectroscopy KW - DNA origami KW - SERS KW - gold nanoparticles KW - silver nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-358761 UR - http://pubs.rsc.org/en/content/articlelanding/2016/nr/c5nr08674d#!divAbstract DO - https://doi.org/10.1039/C5NR08674D SP - 5612 EP - 5620 PB - Royal Society of Chemistry CY - Cambridge, England AN - OPUS4-35876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhammad, R. T1 - Influence of the of dealumination and porosity on the acid sites of natural zeolite clinoptilolite N2 - Heavy feedstock from crude and bio oil is a widely available and renewable resource for production of fuel and starting materials for other organic valuables by cracking or hydrocracking. Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Clinoptilolite has a crystalline structure with a defined micropore system of medium size showing unique ion exchange and sorption properties. However, it is catalytically active only in the H-form. Also certain porosity is required for improvement of the accessibility of active sites. This paper deals with the tuning of acid properties and of the mesoporosity of the clinoptilolite by variation of the Si/Al framework ratio, extra-framework aluminum and modification of the porosity by specific acid and water vapor treatment. The preparation of hierarchical pore structures containing interconnected micro-meso-macropores is an important factor influencing the catalytic performance. The obtained materials have been characterized by XRD, TEM, FTIR, Raman, TG/DSC. The chemical composition has been determined by ICP-AES. The porosity have been investigated by nitrogen adsorption desorption measurements. The acidity has been measured by Ammonia-TPD. The extent of dealumination, stability of the clinoptilolite against acid treatment and the change in the nature of acid sites and their local structure has been studied by solid state 29Si and 27Al MAS NMR spectroscopy in detail. The catalytic activity has been investigated in the acetalization of benzaldehyde with 1,3-butanediol. The impact of the porosity, change of the Si/Al ratio as well as present Al species on catalytic properties will be discussed. T2 - 28. Deutsche Zeolith-Tagung CY - Giessen, Germany DA - 02.03.2016 KW - NMR KW - Zeolite KW - Clinoptilolite KW - Catalyst PY - 2016 AN - OPUS4-35886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Mechanochemical synthesis, characterization, and structure determination of new alkaline earth metal-tetrafluoroterephthalate frameworks: Ca(pBDC‑F4 )·4H2O, Sr(pBDC‑F4 )·4H2O, and Ba(pBDC‑F4 ) N2 - New fluorinated alkaline earth metal−organic frameworks were successfully synthesized by milling of metal hydroxides M(OH)2 with tetrafluoroterephthalic acid H2 pBDC-F4. Both calcium- and strontium-tetrafluoroterephthalates are tetrahydrated, while the barium tetrafluoroterephthalate is free of coordinating water molecules. The two isomorphic structures Ca(pBDC-F4)·4H2O and Sr(pBDC-F4)·4H2O were solved from the powder diffraction data by ab initio structure determination and subsequent Rietveld refinement. The products were thoroughly characterized by elemental analysis, thermal analysis, magicangle spinning NMR, Fourier transform infrared spectroscopy, scanning electron microscopy imaging, and Brunauer−Emmett−Teller measurements. Our findings suggest that the mechanochemical synthesis route is a promising approach for the preparation of new fluorinated alkaline earth metal−organic frameworks. KW - Mechanochemistry KW - MOFs KW - XRD PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.cgd.5b01457 DO - https://doi.org/10.1021/acs.cgd.5b01457 SN - 1528-7483 VL - 16/4 SP - 1923 EP - 1933 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-35940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bartusch, Jürgen A1 - Schadow, Florian A1 - Köppe, Enrico A1 - Dohse, Elmar ED - Chimenti, D. E. ED - Bond, L. J. T1 - Focusing of ferroelectret air-coupled ultrasound transducers N2 - Air-coupled ultrasound has been applied increasingly as a non-destructive testing method for lightweight construction in recent years. It is particularly appropriate for composite materials being used in automotive and aviation industry. Air-coupled ultrasound transducers mostly consist of piezoelectric materials and matching layers. However, their fabrication is challenging and their signal-to-noise ratio often not sufficient for many testing requirements. To enhance the efficiency, air-coupled ultrasound transducers made of cellular polypropylene have been developed. Because of its small density and sound velocity, this piezoelectric ferroelectret matches the small acoustic impedance of air much better than matching layers applied in conventional transducers. In our contribution, we present two different methods of spherical focusing of ferroelectret transducers for the further enhancement of their performance in NDT applications. Measurements on carbon-fiber-reinforced polymer (CFRP) samples and on metal adhesive joints performed with commercially available focused air-coupled ultrasound transducers are compared to measurements executed with self-developed focused ferroelectret transducers. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Ferroelectret KW - Transducer KW - Air-coupled KW - Ultrasonic KW - Focusing PY - 2016 SP - 080001 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-35955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaal, Mate A1 - Bovtun, Viktor A1 - Stark, Wolfgang A1 - Erhard, Anton A1 - Yakymenko, Y. A1 - Kreutzbruck, Marc T1 - Viscoelastic properties of cellular polypropylene ferroelectrets N2 - Viscoelastic properties of cellular polypropylene ferroelectrets (PP FEs) were studied at low frequencies (0.3–33 Hz) by dynamic mechanical analysis and at high frequencies (250 kHz) by laser Doppler vibrometry. Relaxation behavior of the in-plane Young’s modulus (Y´ 11~1500 MPa at room temperature) was observed and attributed to the viscoelastic response of polypropylene matrix. The out-of-plane Young’s modulus is very small (Y´33≈0.1 MPa) at low frequencies, frequency- and stress-dependent, evidencing nonlinear viscoelastic response of PP FEs. The highfrequency mechanical response of PP FEs is shown to be linear viscoelastic with Y´33≈0.8 MPa. It is described by thickness vibration mode and modeled as a damped harmonic oscillator with one degree of freedom. Frequency dependence of Y*33 in the large dynamic strain regime is described by the broad Cole-Cole relaxation with a mean frequency in kHz range attributed to the Dynamics of the air flow between partially closed air-filled voids in PP FEs. Switching-off the relaxation contribution causes dynamic crossover from the nonlinear viscoelastic regime at low frequencies to the linear viscoelastic regime at high frequencies. In the small strain regime, contribution of the air flow seems to be insignificant and the power-law response, attributed to the mechanics of polypropylene cell walls and closed air voids, dominates in a broad frequency range. Mechanical Relaxation caused by the air flow mechanism takes place in the sound and ultrasound frequency range (10 Hz–1MHz) and, therefore, should be taken into account in ultrasonic applications of the PP FEs deal with strong exciting or receiving signals. KW - Viscoelastic KW - Cellular polypropylene KW - Ferroelectret PY - 2016 DO - https://doi.org/10.1063/1.4944798 SN - 0021-8979 SN - 1089-7550 SN - 1520-8850 VL - 119 SP - Article Number: 125101 PB - AIP Publishing AN - OPUS4-35956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Myrach, Philipp A1 - Röllig, Mathias A1 - Jonietz, Florian A1 - Illerhaus, Bernhard A1 - Meinel, Dietmar A1 - Richter, U. A1 - Miksche, R. ED - Chimenti, Dale E. ED - Bond, Leonard J. T1 - Characterization of pores in high pressure die cast aluminum using active thermography and computed tomography N2 - Larger high pressure die castings (HPDC) and decreasing wall thicknesses are raising the issue of casting defects like pores in aluminum structures. Properties of components are often strongly influenced by inner porosity. As these products are being established more and more in lightweight construction (e.g. automotive and other transport areas), non-destructive testing methods, which can be applied fast and on-site, are required for quality assurance. In this contribution, the application of active thermography for the direct detection of larger pores is demonstrated. The analysis of limits and accuracy of the method are completed by numerical simulation and the method is validated using computed tomography. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - flash thermography KW - aluminum KW - pores KW - computed tomography PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940580 VL - 1706 SP - 110009-1 EP - 110009-8 PB - AIP Publishing LLC CY - Melville, New York, USA AN - OPUS4-35848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Metrology for spatially resolved chemical analysis at the micro and nanometre scales N2 - CCQM has established a framework of comparisons to demonstrate the international comparability of chemical measurements. The key point is the establishment of comparable measurements, with traceability to internationally or nationally stated references. The Surface Analysis Working Group (SAWG) has been formally founded in 2003. CCQM ratified the group as a full working group of CCQM in April 2003 with these terms of reference: - to develop pilot studies and carry out key comparisons of national measurement standards for surface and micro/nano-analysis; - to assist in identifying and establishing inter-laboratory work to improve the traceability of surface and micro/nano-analysis; - to establish and update a work plan to be adopted by CCQM; - to discuss and review the scope of the working group and to liase with other working groups related to nanotechnology. Following the 2015 meeting of the CCQM, the pilot study CCQM-P130 “WD and ED Electron Probe Micro Analysis on Au-Cu alloys” lead by BAM&NIST has been finalized. The Key Comparison K-129 “Measurement of atomic fractions in Cu(In,Ga)Se2 Films” lead by KRISS has made substantial progress and is about to be finalized. The new Key Comparison K-136 on “BET specific surface of ” lead by UNIIM&BAM has made strong progress in 2015 and will be finished in 2016. T2 - 22nd Meeting of CCQM CY - Sevres, France DA - 21.4.16 KW - Surface chemical analysis KW - Metrology PY - 2016 AN - OPUS4-35865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - 2-D materials standardization N2 - The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed. In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies! T2 - Science-Industry-Workshop 2D Materials CY - EMPA Akademie, Dübendorf, Switzerland DA - 21.3.16 KW - Standardization KW - Graphene PY - 2016 AN - OPUS4-35866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roth, Christina T1 - Incorporating mechanically interlocked molecules into crystalline coordination networks on surfaces: Electro-active SURMOFs to translate molecular switching into macroscopic function and devices N2 - We aim at preparing, characterising, and applying SURMOFs incorporating electro-active and -switchable mechanically interlocked molecules such as rotaxanes as the basis of functional devices. Preparation and Positioning Synthesis, purification and analytical characterization of electro-switchable rotaxanes suitable for SURMOF-formation as well as Layer-by-Layer assembly on surfaces. Controlled deposition of electro-active SURMOFs and Layer-by-Layer self-assembled multilayers based on these switchable rotaxanes. Construction of SURMOFs on micro-patterned surfaces. Structural Characterisation and Physico-Chemical Properties Electrochemical characterization of these rotaxanes in solution with cyclic voltammetry, chronoamperometry and impedance spectroscopy. Surface characterization of SURMOFs and multilayers with XPS, NEXAFS, AFM, contact-angle measurements, transmission UV/Vis, ToF-SIMS and – in cooperation with partners from SPP – XRD. Development of ToF-SIMS (also assisted by Principle Component Analysis of the fragment-ion data) as a method for imaging and depth-profiling. Development of an appropriate electrochemical cell to perform cyclic voltammetry, chronoamperometry and impedance spectroscopy with SURMOFS and multilayers as working electrodes in a three-electrode cell. Comparison of the structural and electrochemical properties of the redox-active unit in solution, multilayers and SURMOF focusing on the advantages of SURMOFs. System Integration and Function Demonstration Examination of the usability of the electroactive SURMOFS as optoelectronic switch or data storage device with a focus on the robustness of the system. Usage of the SURMOFs as functional electrodes for electrochemical application. Selective switching of ordered nanostructures to translate molecular motion to macroscopic property changes. T2 - Colloquium of the priority programme "Coordination networks: building blocks for functional systems” SPP 1928 CY - Garching, Germany DA - 30.3.16 KW - SurfMOF KW - XPS KW - NEXAFS KW - Characterization PY - 2016 AN - OPUS4-35867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roth, C. T1 - Incorporating mechanically interlocked molecules into crystalline coordination networks on surfaces: Electro-active SURMOFs to translate molecular switching into macroscopic function and devices N2 - We aim at preparing, characterising, and applying SURMOFs incorporating electro-active and -switchable mechanically interlocked molecules such as rotaxanes as the basis of functional devices. Preparation and Positioning Synthesis, purification and analytical characterization of electro-switchable rotaxanes suitable for SURMOF-formation as well as Layer-by-Layer assembly on surfaces. Controlled deposition of electro-active SURMOFs and Layer-by-Layer self-assembled multilayers based on these switchable rotaxanes. Construction of SURMOFs on micro-patterned surfaces. Structural Characterisation and Physico-Chemical Properties Electrochemical characterization of these rotaxanes in solution with cyclic voltammetry, chronoamperometry and impedance spectroscopy. Surface characterization of SURMOFs and multilayers with XPS, NEXAFS, AFM, contact-angle measurements, transmission UV/Vis, ToF-SIMS and – in cooperation with partners from SPP – XRD. Development of ToF-SIMS (also assisted by Principle Component Analysis of the fragment-ion data) as a method for imaging and depth-profiling. Development of an appropriate electrochemical cell to perform cyclic voltammetry, chronoamperometry and impedance spectroscopy with SURMOFS and multilayers as working electrodes in a three-electrode cell. Comparison of the structural and electrochemical properties of the redox-active unit in solution, multilayers and SURMOF focusing on the advantages of SURMOFs. System Integration and Function Demonstration Examination of the usability of the electroactive SURMOFS as optoelectronic switch or data storage device with a focus on the robustness of the system. Usage of the SURMOFs as functional electrodes for electrochemical application. Selective switching of ordered nanostructures to translate molecular motion to macroscopic property changes. T2 - Colloquium of the Priority Programme "Coordination Networks: Building Blocks for Functional Systems” SPP 1928 CY - Garching, Germany DA - 30.3.16 KW - SURMOF KW - XPS KW - NEXAFS KW - Characterization PY - 2016 AN - OPUS4-35868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shokouhi, P. A1 - Heideklang, Rene T1 - Fusion of multi-sensory NDT data for reliable detection of surface cracks: Signal-level vs. decision-level N2 - We present and compare two different approaches for NDT multi-sensor data fusion at signal (low) and decision (high) levels. Signal-level fusion is achieved by applying simple algebraic rules to strategically post-processed images. This is done in the original domain or in the domain of a suitable signal transform. The importance of signal normalization for low-level fusion applications is emphasized in regard to heterogeneous NDT data sets. For fusion at decision level, we develop a procedure based on assembling joint kernel density estimation (KDE). The procedure involves calculating KDEs for individual sensor detections and aggregating them by applying certain combination rules. The underlying idea is that if the detections from more than one sensor fall spatially close to one another, they are likely to result from the presence of a defect. On the other hand, single-senor detections are more likely to be structural noise or false alarm indications. To this end, we design the KDE combination rules such that it prevents single-sensor domination and allows data-driven scaling to account for the influence of individual sensors. We apply both fusion rules to a three-sensor dataset consisting in ET, MFL/GMR and TT data collected on a specimen with built-in surface discontinuities. The performance of the fusion rules in defect detection is quantitatively evaluated and compared against those of the individual sensors. Both classes of data fusion rules result in a fused image of fewer false alarms and thus improved defect detection. Finally, we discuss the advantages and disadvantages of low-level and high-level NDT data fusion with reference to our experimental results. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE) CY - Minneapolis, USA DA - 26.07.2015 KW - multi-sensory KW - NDT KW - signal-level KW - decision-level PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940634 SN - 0094-243X VL - 1706 SP - Article Number: 180004 PB - AMER INST PHYSICS CY - Melville, USA AN - OPUS4-35870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Desolvation of indometacin solvates characterized structurally and kinetically N2 - The structure of indometacin solvates and the desolvation process of these compounds are investigated by synchrotron X-ray radiation, Raman spectroscopy and thermal analysis. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Crystallization KW - In situ analysis KW - Indometacin KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair Distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of Paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Paracetamol KW - Crystallization KW - In situ analysis KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ermilov, Eugeny A. A1 - Liu, J.-Y. A1 - Menting, R. A1 - Huang, Y.-S. A1 - Röder, B. A1 - Ng, D. K. P. T1 - An artificial photosynthetic model based on a molecular triad of boron dipyrromethene and phthalocyanine N2 - A boron dipyrromethene (BDP) unit and its monostyryl derivative (MSBDP) were introduced at the axial positions of a silicon(IV) phthalocyanine (SiPc) core. The absorption spectrum of this compound virtually covered the entire visible region (300-700 nm) and could be interpreted as a superposition of the spectra of individual components. The intramolecular photoinduced energy and charge transfer processes of this triad were studied using steady-state and time-resolved spectroscopic methods in polar and nonpolar solvents. Upon BDP-part excitation, a fast and highly efficient excitation energy transfer (EET) occurred resulting in strong quenching of its fluorescence and the formation of the first excited singlet state of SiPc or MSBDP. It was found that both EET and charge transfer (CT) processes competed with each other in the depopulation of the first excited singlet state of the MSBDP moiety. The former strongly superseded CT in nonpolar toluene, whereas the latter was dominant in a polar environment. Direct or indirect (via EET) excitation of the SiPc-part of the triad was followed by CT yielding the charge-separated (CS) species BDP-SiPc center dot--MSBDP center dot+. The energy gap between the CS state and the S-1-state of the SiPc moiety was found to be only 0.06 eV in toluene, which facilitated the back CT process and resulted in the appearance of thermally activated delayed fluorescence. With increasing solvent polarity, the energy of the CS state reduced resulting in the disappearance of the delayed fluorescence in CHCl3, tetrahydrofuran or N,N-dimethylformamide. The charge recombination rate, k(CR), was very fast in polar DMF (3.3 x 10(10) s(-1)), whereas this process was two-orders of magnitude slower in nonpolar toluene (k(CR) = 4.0 x 10(8) s(-1)). KW - Photoinduced electron-transfers KW - Zinc phthalocyanine KW - Solar-energy KW - Charge separation KW - Solvent polarity KW - Porphyrin KW - Excitation KW - Fullerene KW - Recombination KW - Carotenoids PY - 2016 DO - https://doi.org/10.1039/c6cp00920d VL - 18 IS - 16 SP - 10964 EP - 10975 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nagli, L. A1 - Gaft, M. A1 - Gornushkin, Igor B. A1 - Glaus, Reto T1 - Stimulated emission and lasing in laser-induced plasma plume N2 - The lasing effect is demonstrated in laser plasmas induced on various metal targets and pumped by a laser tuned in resonance with a strong optical transition of a metal. The intense, polarized and lowdivergent radiation is emitted from a longitudinally pumped plasma plume in forward and backward directions with respect to the pump beam. Lasing occurs only within duration of the pumping pulse. The effect is found for elements of 13th and 14th groups and for Ca, Ti, Zr, Fe and Ni. The Einstein coefficients for spontaneous emission of all lasing transitions are higher than 10⁷ s⁻¹. For some elements like Al and In, a three-level lasing scheme is realized. For others, like Tl, both three- and four-level lasing schemes are realized. It is found that the longitudinal pump geometry is more efficient than the transversal one. KW - Optically pumped plasma lasers KW - Laser Induced Breakdown Spectroscopy (LIBS) KW - Laser Induced Fluorescence (LIF) PY - 2016 DO - https://doi.org/10.1016/j.optcom.2016.05.071 SN - 0030-4018 VL - 378 SP - 41 EP - 48 PB - Elsevier CY - Amsterdam, Netherlands AN - OPUS4-36320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olejko, Lydia A1 - Cywinski, P. A1 - Bald, Ilko T1 - An ion-controlled four-color fluorescent telomeric switch on DNA origami structures N2 - The folding of single-stranded telomeric DNA into guanine (G) quadruplexes is a conformational change that plays a major role in sensing and drug targeting. The telomeric DNA can be placed on DNA origami nanostructures to make the folding process extremely selective for K+ ions even in the presence of high Na+ concentrations. Here, we demonstrate that the K+-selective G-quadruplex formation is reversible when using a cryptand to remove K+ from the G-quadruplex. We present a full characterization of the reversible switching between single-stranded telomeric DNA and G-quadruplex structures using Förster resonance energy transfer (FRET) between the dyes fluorescein (FAM) and cyanine3 (Cy3). When attached to the DNA origami platform, the G-quadruplex switch can be incorporated into more complex photonic networks, which is demonstrated for a three-color and a four-color FRET cascade from FAM over Cy3 and Cy5 to IRDye700 with G-quadruplex-Cy3 acting as a switchable transmitter. KW - DNA origami KW - FRET KW - Photonic wire KW - G quadruplex PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-362560 DO - https://doi.org/10.1039/C6NR00119J SN - 2040-3364 SN - 2040-3372 VL - 8 IS - 19 SP - 10339 EP - 10347 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias T1 - Tomographic reconstruction of soil gas distribution from multiple gas sources based on sparse sampling N2 - A monitoring method is introduced that creates twodimensional (2D) maps of the soil gas distribution. The method combines linear gas sensing technology for in-situ monitoring of gases in soil with the mapping capabilities of Computed Tomography (CT) to reconstruct spatial and temporal resolved gas distribution maps. A weighted iterative algebraic reconstruction method based on Maximum Likelihood with Expectation Maximization (MLEM) in combination with a source-by-source reconstruction approach is introduced that works with a sparse setup of orthogonally-aligned linear gas sensors. The reconstruction method successfully reduces artifact production, especially when multiple gas sources are present, allowing the discrimination between true and non-existing so-called ghost source locations. Experimental validation by controlled field experiments indicates the high potential of the proposed method for rapid gas leak localization and quantification with respect to Pipeline or underground gas storage issues. KW - Computed tomography KW - Gas distribution mapping and gas source localization KW - Discrimination of multiple gas sources KW - Distributed linear sensor KW - Membrane-based gas sensing KW - Subsurface monitoring KW - Gas storage areas PY - 2016 DO - https://doi.org/10.1109/JSEN.2016.2545103 SN - 1530-437X VL - 16 IS - 11 SP - 4501 EP - 4508 PB - IEEE - Inst. Electrical Electronics Engineers Inc CY - Hoes Lane, NJ, USA AN - OPUS4-36228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Glamsch, Stephan A1 - Ehlert, Christopher A1 - Lippitz, Andreas A1 - Kulak, N. A1 - Unger, Wolfgang T1 - Synchrotron-radiation XPS analysis of ultra-thin silane films: Specifying the organic silicon N2 - The analysis of chemical and elemental in-depth variations in ultra-thin organic layers with thicknesses below 5 nm is very challenging. Energy- and angle-resolved XPS (ER/AR-XPS) opens up the possibility for non-destructive chemical ultra-shallow depth profiling of the outermost surface layer of ultra-thin organic films due to its exceptional surface sensitivity. For common organic materials a reliable chemical in-depth analysis with a lower limit of the XPS information depth z95 of about 1 nm can be performed. As a proof-of-principle example with relevance for industrial applications the ER/AR-XPS analysis of different organic monolayers made of amino- or benzamidosilane molecules on silicon oxide surfaces is presented. It is demonstrated how to use the Si 2p core-level region to non-destructively depth-profile the organic (silane monolayer) – inorganic (SiO2/Si) interface and how to quantify Si species, ranging from elemental silicon over native silicon oxide to the silane itself. The main advantage of the applied ER/AR-XPS method is the improved specification of organic from inorganic silicon components in Si 2p core-level spectra with exceptional low uncertainties compared to conventional laboratory XPS. KW - Synchrotron radiation XPS KW - Depth profiling KW - Silanes KW - Monolayer KW - Amines KW - Amides PY - 2016 DO - https://doi.org/10.1016/j.apsusc.2015.12.052 SN - 0169-4332 SN - 1873-5584 VL - 363 SP - 406 EP - 411 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Field integration of benchtop NMR instruments for online monitoring and process control of a modular industrial reaction step N2 - Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectroscopy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. Within the project CONSENS, the continuous production of high-value products in small production scale is advanced by introducing benchtop NMR spectroscopy. CONSENS is a research and innovation project on integrated control and sensing for sustainable operation of flexible intensified processes. This poster will present the first steps of the process integration of a benchtop NMR instrument for a lithiation process and outlines further fields of activity and potential challenges. Hereby, the following issues are going to be addressed: explosion-proof housing for the spectrometer, automation of signal processing (data pretreatment, evaluation and communication to the control system), flow cells and measuring conditions. Furthermore, first online spectra of the lithiation reaction in batch mode were acquired in lab scale. The reaction was performed in a 25 mL glass reactor with thermal jackets for temperature control of the reaction mixture. The Li-HMDS was dosed stepwise by using a glass syringe. First spectra in the proton and fluorine domain were recorded online using a flowrate of 3.5 mL min–1 and a simple 5 mm polytetrafluoroethylene tube (PTFE) as a flow cell. T2 - 4th Practical Applications of NMR in Industry Conference (PANIC) CY - Houston, Texas, USA DA - 15.02.2016 KW - Reaction monitoring KW - Online NMR spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-354427 AN - OPUS4-35442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Siebler, Daniel T1 - A new generation of elastomeric polymer optical fibers and its potential for sensor applications N2 - This talk reflects recent progress in the detection of partial discharges in cables accessories with polymer optical fibers. T2 - Mahanakorn University of Technology, Bangkok, Thailand CY - Bangkok, Thailand DA - 17.01.2016 KW - fluorescence KW - partial discharge KW - silicone rubber KW - high voltage cable accessories KW - elastomeric polymer optical fiber POF KW - coincidence PY - 2016 AN - OPUS4-35397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online NMR spectroscopy as a reference tool for model developments - Successful approaches in process analytical technology N2 - Quantitative Online NMR spectroscopy as a direct ratio method of analysis represents a perfect reference for calibration of further process analytical techniques, e.g., optical spectroscopic techniques. In this work we present a combined approach including Online NMR and Raman spectroscopy on a laboratory setup for development of suitable models for process monitoring. Therefore we investigated the absorption process of carbon dioxide in solutions of monoethanolamine, as well as the homogeneous catalyzed hydroformylation reaction of 1-dodecene taking place in an emulsion stabilized by a technical surfactant. The models for Raman spectroscopy were tested and approved during several days of operational studies of miniplant-scale setups for both mentioned applications. T2 - 4th Annual Practical Applications of NMR in Industry Conference (PANIC) CY - Houston, Texas, USA DA - 15.02.2016 KW - Online-NMR spectroscopy KW - Online-Raman spectroscopy KW - Process Analytical Technology PY - 2016 AN - OPUS4-35423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - qNMR under pressure - applications on compressed and liquefied gases N2 - During the last years quantitative NMR spectroscopy has become a general method for solving complex problems in science and industry. The opportunity of a calibration-free quantification, related to a simple counting of the nuclear spins in the active volume of the spectrometer represents a key advantage comparing to other analytical techniques. With modern NMR systems detection limits in the lower ppm range on a molar basis are accessible in a reasonable time period, which makes it a promising method for purity assessment, as well as applications in metrological research. First experiments showed that qNMR is suitable for gas analysis with respect to components used for production of primary reference gas mixtures. For this a laboratory setup for high-pressure NMR experiments up to 20 MPa (2900 psi) in fluid and gas phase was built and tested. In this work we show the determination of the composition of high precision mixtures, consisting of liquid and liquefied hydrocarbons commonly supplied in floating piston cylinders. Therefore an experimental setup was developed allowing sampling, as well as circulation of the mixture within a high-pressure NMR tube by using a concentric tubing assembly. Additionally, a piston-cylinder pressure cell was designed and manufactured allowing wide-range volume displacement. Mainly intended for density variation within supercritical fluid experiments, it can also function as a compression element for further increasing of gas-pressure in the system. Equipped with liquid thermostat and a motor-powered screw drive unit it is designed to operate at pressure levels up to 60 MPa (8700 psi) and temperatures up to 130 °C. T2 - 4th Annual practical applications of NMR in industry conference (PANIC) CY - Houston, TX, USA DA - 15.02.2016 KW - Gas-phase NMR KW - High-pressure NMR KW - Liquefied gases PY - 2016 AN - OPUS4-35435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Laser induced plasma ion source for ambient mass spectrometry N2 - Laser microprobe mass analysis (LMMS) employs local ionization by a focused laser and subsequent mass analysis. At excessive irradiation microplasmas led to undesired distortions. Thus, LMMS was discarded as promising ion source. Effective cooling under ambient conditions resulted in more controllable plasmas and development of laser induced breakdown spectroscopy (LIBS). However, little effort has been made to combine LIBS and ambient MS, since these plasmas only provide microsecond lifetimes. After these, recombination yields uncharged and newly bound species, making them inaccessible for MS. The combination of high repetition rate lasers together with growing knowledge about manipulation of charged species at atmospheric pressure allow overcoming these obstacles. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie (DGMS) CY - Hamburg, Germany DA - 28.02.2016 KW - laser induced plasma KW - ion source KW - ambient mass spectrometry KW - emission spectroscopy KW - laser induziertes Plasma KW - Ionenquelle KW - Atmosphärendruck-Massenspektrometrie KW - Emissionsspektroskopie PY - 2016 AN - OPUS4-35454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heideklang, René A1 - Shokouhi, P. T1 - Decision-level fusion of spatially scattered multi-modal data for nondestructive inspection of surface defects N2 - This article focuses on the fusion of flaw indications from multi-sensor nondestructive materials testing. Because each testing method makes use of a different physical principle, a multi-method approach has the potential of effectively differentiating actual defect indications from the many false alarms, thus enhancing detection reliability. In this study, we propose a new technique for aggregating scattered two- or three-dimensional sensory data. Using a density-based approach, the proposed method explicitly addresses localization uncertainties such as registration errors. This feature marks one of the major of advantages of this approach over pixel-based image fusion techniques. We provide guidelines on how to set all the key parameters and demonstrate the technique's robustness. Finally, we apply our fusion approach to experimental data and demonstrate its capability to locate small defects by substantially reducing false alarms under conditions where no single-sensor method is adequate. KW - Multi-sensor data fusion KW - Density estimation KW - Scattered data KW - Defect detection KW - Nondestructive testing KW - Registration errors PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-352977 DO - https://doi.org/10.3390/s16010105 SN - 1424-8220 VL - 16 SP - Article Number: 105 PB - MDPI CY - Basel, Switzerland AN - OPUS4-35297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zerbst, Uwe A1 - Heckel, Thomas A1 - Carboni, M. T1 - Non-destructive testing and fracture mechanics - A short discussion N2 - A discussion is provided on the relation between non-destructive testing (NDT) and fracture mechanics. The basic tasks behind this are to guarantee the safety of a component at a potential hazard loading event, to specify inspection intervals or, alternatively, of demands on NDT for a fixed inspection regime, to plan accompanying measures for cases of temporary continued operation of structures in which cracks have been detected, and, finally, fatigue strength considerations which take into account initial defects. T2 - 42nd Annual review of progress in quantitative nondestructive evaluation conference CY - Minneapolis, Minnesota, USA DA - 2015-07-26 KW - Zerstörungsfreie Prüfung KW - Schwingfestigkeit KW - Schadenstoleranz KW - Bruchmechanik KW - probability KW - damage tolerance KW - railway axles KW - inspection PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940614 SN - 0094-243X VL - 1706 SP - 150002-1 EP - 150002-5 PB - AIP Publishing CY - Melville, New York, USA AN - OPUS4-33866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beckmann, Jörg A1 - Marchetti, B. A1 - von Chrzanowski, Lars S. A1 - Ritter, E. A1 - Puskar, L. A1 - Aziz, E. F. A1 - Schade, U. T1 - Optical constants of harmful and highly energetic liquids for application to THz screening systems N2 - The far-infrared (IR) optical constants of a set of hazardous and flammable liquids have been obtained by means of spectroscopic ellipsometry in attenuated total reflection configuration over a broad spectral range. Such liquids recently became of considerable concern for transportation security measures worldwide. Their optical identification at check-in gates can only become possible if the characteristic spectra are already known. The refractive indices and the extinction coefficients reported here contribute to a spectroscopic data base in the far-IR and terahertz (THz) spectral regions and may support modeling the performance of THz screening systems on liquids for airports and other security sensitive areas. Examples of several container material/liquid systems are discussed. From the measured optical constants typical THz waveforms are calculated and discussed. KW - liquids material characterization KW - Ellipsometry KW - FT-IR spectroscopy KW - THz time-domain spectroscopy (THz-TDS) PY - 2016 DO - https://doi.org/10.1109/TTHZ.2016.2547319 SN - 2156-342X VL - 2016 / Vol. PP IS - 99 SP - 1 EP - 12 PB - IEEE - Inst. Electrical Electronics Engineers Inc CY - New York, NY, USA AN - OPUS4-36366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäferling, Michael T1 - Nanoparticle-based luminescent probes for intracellular sensing and imaging of pH N2 - Fluorescence imaging microscopy is an essential tool in biomedical research. Meanwhile, various fluorescent probes are available for the staining of cells, cell membranes, and organelles. Though, to monitor intracellular processes and dysfunctions, probes that respond to ubiquitous chemical parameters determining the cellular function such as pH, pO2, and Ca2+ are required. This review is focused on the progress in the design, fabrication, and application of photoluminescent nanoprobes for sensing and imaging of pH in living cells. The advantages of using nanoprobes carrying fluorescent pHindicators compared to single molecule probes are discussed as well as their limitations due to the mostly lysosomal uptake by cells. Particular attention is paid to ratiometric dual wavelength nanosensors that enable intrinsic referenced measurements. Referencing and proper calibration procedures are basic prerequisites to carry out reliable quantitative pH determinations in complex samples such as living cells. A variety of examples will be presented that highlight the diverseness of nanocarrier materials (polymers, micelles, silica, quantum dots, carbon dots, gold, photon upconversion nanocrystals, or bacteriophages), fluorescent pH indicators for the weak acidic range, and referenced sensing mechanisms, that have been applied intracellularly up to now. KW - pH sensing KW - Luminescent probes KW - Imaging PY - 2016 DO - https://doi.org/10.1002/wnan.1366 SN - 1939-0041 SN - 1939-5116 VL - 8 IS - 3 SP - 378 EP - 413 PB - Wiley-Blackwell CY - Hoboken, New Jersey, USA AN - OPUS4-36367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR spectroscopy of technical mixtures and gases from elevated to high-pressure N2 - Recent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10 ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer. Technical mixtures can be investigated online directly next to a process setup by using flow probes. This makes it a promising method for process analytical applications, especially during process development in laboratory and pilot plant scale. With the growing market of Benchtop devices based on permanent magnets nowadays an integration of NMR spectroscopy in an industrial environment becomes reasonable. A special application of qNMR in technical mixtures is the observation in the gas phase, which is rarely applied compared to liquid and solid NMR studies. Because of the low density it results in a reduced sensitivity, which can be improved by applying pressure. Therefore a high-pressure NMR setup was developed based on a commercially available NMR tube made of zirconia. This is currently tested up to 20 MPa, but can be extended up to 100 MPa with regard to pressure rating of its components. This work shows results of gas-phase application on natural-gas like reference gas mixtures produced at BAM, as well as investigations on liquefied gas mixtures with high accuracy provided in piston cylinders. Besides that amine gas treatment and hydroformylation in a microemulsion represent two other examples of applications in process analytical technology. These show the potential of combination of online NMR spectroscopy with other spectroscopic methods, especially during model development for data evaluation. T2 - Presentation at Statoil Research Center CY - Trondheim, Norway DA - 27.05.2016 KW - Quantitative NMR spectroscopy KW - Process analytical technology KW - Gas-phase NMR PY - 2016 AN - OPUS4-36330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zientek, Nicolai A1 - Meyer, Klas A1 - Kern, Simon A1 - Maiwald, Michael T1 - Quantitative online NMR spectroscopy in a nutshell N2 - Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced. KW - Prozessanalytik KW - Process analytical technology KW - Online NMR spectroscopy KW - Online monitoring PY - 2016 DO - https://doi.org/10.1002/cite.201500120 SN - 0009-286X VL - 88 IS - 6 SP - 698 EP - 709 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Germany AN - OPUS4-36333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gravenkamp, Hauke T1 - A remark on the computation of shear-horizontal and torsional modes in elastic waveguides N2 - When modeling the propagation of elastic guided waves in plates or cylinders, Finite Element based numerical methods such as the Scaled Boundary Finite Element Method (SBFEM) or the Semi-Analytical Finite Element (SAFE) Method lead to an eigenvalue problem to be solved at each frequency. For the particular case of shear horizontal modes in a homogeneous plate or torsional modes in a homogeneous cylinder, the problem can be drastically simplified. The eigenvalues become simple functions of the frequency, while the eigenvectors are constant. The current contribution discusses how this behavior is represented in the numerical formulation and derives the expressions for the eigenvalues and eigenvectors as well as the dynamic stiffness matrix of infinite elastic waveguides. KW - Guided waves KW - Shear-horizontal modes KW - Torsional modes KW - Scaled Boundary Finite Element Method PY - 2016 DO - https://doi.org/10.1016/j.ultras.2016.03.003 SN - 0041-624X VL - 2016/69 SP - 25 EP - 28 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-36429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sturm, Heinz T1 - Friction-induced explosive reactions N2 - The motivation to examine the influence of friction on surfaces of energetic materials (EM) has diverse backgrounds. On the one hand the very old hot spot theory predicts, that the size of such hot spot could be in the range of a molecule. The initiation of an EM could start by mechanical excitation, i.e. friction, and continues driven by an exothermal chemical reaction. Following such phenomena on the molecular scale with an imaging method such as AFM should enable us to separate several steps of ignition, if there are any. The experiments showed that HMX mainly undergoes a plastic deformation without further consequences. TNP however showed self healing in the wear track after scratching and simultaneously the destruction of a crystal edge outside the wear track. Additionally nanoparticles appear, tribologists call this "third body formation", which are proven to have a different chemical composition as the original TNP. The self healing effect on the surface is verified with experiments on self diffusion of TNP molecules to and fro the free edges of the crystal. The conclusion is that the formation of a hot spot can be shown to consist of several subsequent steps, separated temporally and locally. The goal to excite the thermal decomposition of a whole TNP crystal (nanoexplosion) was yet not reached due to unfavourable conditions related to thermal conductivity and build-up of pressure. T2 - Role of Third Bodies in Tribology, Colloquium of 5.1 CY - BAM, Berlin, Germany DA - 09.06.2016 KW - AFM KW - Energetic material KW - Hot spot KW - Friction PY - 2016 AN - OPUS4-36433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Cluster algorithm for the evaluation of heterogeneous materials by LIBS N2 - The laser-induced breakdown spectroscopy (LIBS) is a fast method to provide multi-elemental analysis of any sample. At the Federal Institute for Materials Research and Testing (BAM) the LIBS technique is applied on building materials to measure ingress profiles of harmful species like chloride and alkalis. The ingress depth and the quantitative amount is important for the evaluation of the potential for damage processes like the alkali-silica reaction or chloride-induced corrosion. Concrete as an example is a highly heterogeneous material with 1/7 cement (major component CaO) and 6/7 aggregates (SiO2) with different grain sizes. Due to a scanning procedure a two dimensional element distribution of a concrete surface can be measured. In order to have an automated Separation method to evaluate heterogeneous materials, different cluster algorithm have been tested. Best results have been achieved with the Expectation-Maximization-Algorithm (EM-Algorithm). T2 - Chemometrics in analytical chemistry CY - Barcelona, Spain DA - 06.06.2016 KW - LIBS KW - Concrete KW - Multivariate analysis PY - 2016 AN - OPUS4-36471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR metrology and "primary" references N2 - qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The development of CRMs addressing qNMR specific measurement issues will give analysts compounds ideally suited for the analytical method and also provide full characterisation of qNMR related parameters to enable more realistic uncertainty budgets. These materials will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden of multiple analytical testing. T2 - First qNMR Foundation Meeting CY - Köln, Germany DA - 10.06.2016 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - purity KW - Referenzmaterialien KW - Reference Material PY - 2016 AN - OPUS4-36450 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Coping with the EU Nano-definition: abilities and limitations of particle sizing with SAXS N2 - Excelling in brevity but lacking in applicability, the 2011 EU nanomaterial definition has become a source of anguish for scientists and industry alike. Repeated pleas and discussions with our own envoy have demonstrated the strength of their resolve: this definition is unlikely to change. Manufacturers of many materials (cosmetics, pigments, foodstuffs, etc.) will have to characterise and label all their products accordingly, a task still impossible for lack of a clear metrological approach towards this goal. Therefore, the onus has fallen on the scientists to come up with a practicable measurement technique allowing inexpensive classification covering large swathes of the material landscape. Small-angle X-ray Scattering (SAXS) probes the size range in question, and can - with due care - deliver a bulk-averaged volume-weighted size distribution. Like any other real-world measurement method, however, it is not (and can never be) a universal solution. This presentation will clarify the SAXS technique, provide several application examples for nanomaterial characterisation, and will detail the limitations and pitfalls that accompany its abilities. At the end of this presentation, you will have the information to judge whether the technique is amenable to your materials or not. T2 - 2016 TechConnect World Innovation Conference CY - National Harbor, MD, USA DA - 23.05.2016 KW - SAXS KW - presentation KW - EU KW - Nanomaterial PY - 2016 AN - OPUS4-36489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Aggregation behavior of UCST-Type Poly(Acrylamide-co-Acrylonitrile) copolymer N2 - Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST) in a relevant temperature range, i.e. phase separate from solution upon cooling, have been reported so far. Moreover, the most studied UCST type polymers namely polybetaines are difficult to use under physiological conditions, which significantly restricts their potential applications. Therefore, UCST polymers with sharp and robust phase transition in physiological conditions (in the presence of salts, ions etc.) are highly needed in order to extend the range of applications of this class of polymers. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied. At temperature below the UCST, the copolymer chains were aggregated together. The aggregate size was found to be larger with increasing AN contents and became smaller upon dilution of the copolymer solutions. While above the UCST, the copolymer chains were expanded and weekly associated in solution. The association between the copolymer chains formed smaller aggregates with increasing the AN contents or the dilution of the solutions. A model is proposed to explain such aggregation-association behavior of the Fig. 1. Figure 1. Schematic illustration of the proposed thermos-induced aggregation behavior of the poly(AAm-co-AN) in aqueous solution. T2 - World Congress on Living Polymerizations and Polymers 2016 CY - Budapest, Hungry DA - 29.05.2016 - 03.06.2016 KW - Polymer KW - UCST PY - 2016 AN - OPUS4-36491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Spranger, Holger T1 - THz-ToF techniques for the detection of inherent discontinuities in dielectric materials based on a SAFT – and an Optical Layer reconstruction algorithm N2 - Electromagnetic waves with frequencies between 0.1 and 10 THz are described as THz-radiation (T-ray). The ability to penetrate dielectric materials makes T-rays attractive to reveal discontinuities in polymer and ceramic materials. THz-Time Domain Spectroscopy Systems (THz-TDS) are available on the market today which operates with THz-pulses transmitted and received by optically pumped semiconductor antennas. In THz-TDS the travelling time (ToF) and shape of the pulse is changed if it interacts with the dielectric material and its inherent disconti-nuities. A tomogram of the object under the test can be reconstructed from time of flight diffraction (ToFD) scans if a synthetic focusing aperture (SAFT) algorithm is applied. Otherwise, planar discontinuities like cracks in plastics or delaminated lay-ers in composites can be abstracted as layers located at any angle in relation to the outer sample surface direction. A tomogram from the scanned sample can then be reconstructed in case the interactions of electromagnetic pulses with the existing in-herent interfaces are detectable and a model is assumed which describes the device under the test as multilayer structure composed of thin layers with different dielec-tric properties. A short description of both the SAFT – and Optical Layer algorithm for the recon-struction of the inherent structure is initially given. Measurements on representative samples with a variety of artificially produced small and large scale. Reconstructed tomograms are presented to discuss and evaluate the benefits and limits of the two different reconstruction approaches. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - Munich, Germany DA - 13.06.2016 KW - SAFT KW - ToF KW - Optical layer reconstruction KW - Dielectric materials KW - THz PY - 2016 AN - OPUS4-36591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Manufacturing of reference defects for NDT using low-energy EDM N2 - For non-destructive testing (NDT) appropriate reference blocks are required in order to verify and calibrate a testing procedure. At BAM a special electric discharge machining (EDM) system has been developed which is able to manufacture artificial defects having a width down to 30 μm. Especially in the case of austenitic materials conventional EDM leads to a transformation of austenite to martensite. The martensite transformation causes a higher sensitivity of electromagnetic NDT methods (e. g. eddy current testing) at the artificial defects compared to natural defects of same size. The EDM system developed at BAM uses very low energy to avoid this material transformation. A side effect of the low-energy EDM is a lower surface roughness compared to conventional EDM. The artificial defects manufactured at BAM are measured optically and delivered with a certificate. A comparison of artificial defects shows the influence of material transformation on NDT and how differently the quality of the artificial defects can be. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Reference defect KW - EDM KW - Electric discharge machining KW - Artificial defect PY - 2016 AN - OPUS4-36600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Antibody-based SAW sensor for the detection of explosives N2 - A robust and sensitive method for the detection of the explosive trinitrotoluene (TNT) was developed. The detection limit was determined to be around 0.5 µg/L. The fast signal response of less than 1 minute shows that this approach is suitable for security and other time-critcal applications. In addition, the very low cross-reactivity highly reduces the number of false-positives in relation to competing techniques, including sniffer dogs. Due to the multianalyte ability of the SAW system, several explosives might be detected in parallel. T2 - BAM Meeting 2016 CY - Berlin, Germany DA - 17.02.2016 KW - TNT KW - Trinitrotoluene KW - Explosives KW - Airport security KW - High-speed biosensor KW - Selectivity KW - Sensitivity KW - Self-assembled monolayer KW - Gold surface KW - Immunosensor KW - Reversibility KW - Inhibition assay KW - Polyethylene glycol KW - PEG PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366265 UR - http://f1000research.com/posters/5-1352 DO - https://doi.org/10.7490/f1000research.1112309.1 AN - OPUS4-36626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Improved quantitative XRF analysis of industrial thin film samples by calibration using thin film RMs certified by reference-free XRF enabling traceability to the SI N2 - Reference-free XRF is a SI traceable technique for the determination of the mass deposition (mass per unit area) of elements in films on the nano- and micro scale. The method is radiometrically calibrated instrumentation (PTB@BESSY II, Germany) and based on reliable knowledge of all relevant atomic fundamental, experimental and instrumental parameters. No calibration sample or reference materials are necessary. The approach had been validated in the CCQM-P140 pilot study and the K129 key comparison by determination of mole fractions in Cu(In,Ga)Se2 thin films. T2 - Annual Meeting of ISO TC 201 SC 10 XRR/XRF CY - Seoul, Korea DA - 12.10.2016 KW - Reference-free XRF KW - CIGS thin films PY - 2016 AN - OPUS4-38265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Testing lateral resolution and field of view in imaging and small area analysis: reference materials and standardization N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1-xAs and InxGa1 xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers a plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. T2 - 7th International Symposium on Practical Surface Analysis(PSA-16) CY - Daejeon, Korea DA - 17.10.2016 KW - BAM L200 KW - SIMS KW - AES KW - XPS PY - 2016 AN - OPUS4-38266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Schwarz, F. A1 - Heinrich, Thomas A1 - Kaufmann, J. O. A1 - Lippitz, Andreas A1 - Puttreddy, R. A1 - Rissanen, K. A1 - Schalley, C. A. T1 - Photocontrolled on-surface pseudorotaxane formation with well-ordered macrocycle multilayers N2 - The photoinduced pseudorotaxane formation between a photoresponsive axle and a tetralactam macrocycle was investigated in solution and on glass surfaces with immobilized multilayers of macrocycles. In the course of this reaction, a novel photoswitchable binding station with azobenzene as the photoswitchable unit and diketopiperazine as the binding station was synthesized and studied by NMR and UV/Vis spectroscopy. Glass surfaces have been functionalized with pyridine-terminated SAMs and subsequently withmultilayers of macrocycles through layer-by-layer self assembly. A preferred orientation of the macrocycles could be confirmed by NEXAFS spectroscopy. The photocontrolled Deposition of the axle into the surface-bound macrocycle-multilayers was monitored by UV/Vis spectroscopy and led to an increase of the molecular order, as indicated by more substantial linear dichroism effects in angle-resolved NEXAFS spectra. KW - Well-ordered macrocycle multilayers KW - XPS KW - NEXAFS PY - 2016 DO - https://doi.org/10.1002/chem.201603156 SN - 0947-6539 SN - 1521-3765 VL - 22 IS - 40 SP - 14383 EP - 14389 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Pelster, A. A1 - Tyler, B.J. A1 - Kösgen, M. A1 - Kassenböhmer, R. A1 - Peterson, R.E. A1 - Stöver, M. A1 - Arlinghaus, H. F. T1 - Improved 3D-imaging of a sirolimus/probucol eluting stent coating using laser postionization secondary neutral mass spectrometry and time-of-flight secondary ion mass spectrometry N2 - Implantable drug delivery systems that provide controlled and sustained release of a therapeutic agent are used in a wide variety of applications. Drug eluting stents, which are used to treat coronary artery disease, are among the most widespread of these devices, with an estimated 3x10⁶ implants annually worldwide. Controlling the rate of drug release from these devices relies on precise control of the three dimensional (3D)-distribution of the drug, so methods for measuring this distribution are of great importance. The aims of this work were to determine how 3D-imaging of polymer-free sirolimus/probucol drug eluting stent coatings could be improved through the use of laser postionization secondary neutral mass spectrometry (Laser- SNMS) and Ar cluster sputtering with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and to optimize conditions for this analysis. In this study, 3D-imaging of a sirolimus/probucol dual drug eluting stent has been investigated using Laser-SNMS and ToF-SIMS. Laser-SNMS studies of pure sirolimus and probucol were undertaken using 30 keV Bi₃⁺ primary Ions and a 157 nm excimer postionization laser. Under optimal conditions, a greater than 100-fold increase in detected ion yield was observed for Laser-SNMS when compared to ToF-SIMS, although ToF-SIMS provided equal or greater yields for higher mass characteristic ions. Although the optimal laser power density for detecting probucol (5x10⁶W/cm²) was significantly lower than the optimum for sirolimus(7x10⁷W/cm²), an intermediate laser power density of 1x10⁷W/cm² was sufficient to allow imaging of both drugs. Using individual selected ion signals, ToF-SIMS and Laser-SNMS produced similar images of the two drug species. When using, however, a multivariate approach (Maximum autocorrelation factors), Laser-SNMS provided significant improvements in image contrast and small area detection when compared to ToF-SIMS. Following optimization of the technique, 3D-images of the dual drug eluting stent coating were obtained using 10 keV Ar₂₀₀₀⁺ cluster ions for sputtering and 30 keV Bi₃⁺ cluster ions for Analysis for both ToF-SIMS and Laser-SNMS. This work demonstrates the advantages of Laser-SNMS for 3D-imaging of pharmaceutical devices, which has not been previously published. Both ToF-SIMS and Laser-SNMS revealed that the outermost surface of the drug eluting coating contained pure sirolimus to a depth of a few tens of nanometers, with a few channels of sirolimus extending to a depth of around 1 lm. Below about 1 lm, the two drugs were uniformly mixed. Using the 10 keV Ar₂₀₀₀⁺ sputter beam, the authors were able to sputter through the complete drug coating (~6 μm) without observing any accumulated damage in the organic layer. The two techniques showed complementary strengths: ToF-SIMS offers faster data collection and better detected ion yield for larger characteristic ions than Laser-SNMS, and Laser-SNMS offers significantly enhanced detected ion yield for smaller fragment ions, allowing for improved Image contrast and Resolution of smaller features. KW - Imaging ToF SIMS KW - Eluting stent PY - 2016 DO - https://doi.org/10.1116/1.4964687 SN - 1934-8630 SN - 1559-4106 VL - 11 IS - 4 SP - 041001-1 EP - 041001-10 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-38272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Kalbe, Henryk A1 - Rades, Steffi T1 - Determining shell thicknesses in stabilised CdSe@ZnS core-shell nanoparticles by quantitative XPS analysis using an infinitesimal columns model N2 - A novel Infinitesimal Columns (IC) simulation model is introduced in this study for the quantitativeanalysis of core-shell nanoparticles (CSNP) by means of XPS, which combines the advantages of exist-ing approaches. The IC model is applied to stabilised Lumidot™CdSe/ZnS 610 CSNP for an extensiveinvestigation of their internal structure, i.e. calculation of the two shell thicknesses (ZnS and stabiliser)and exploration of deviations from the idealised CSNP composition. The observed discrepancies betweendifferent model calculations can be attributed to the presence of excess stabiliser as well as synthesisresidues, demonstrating the necessity of sophisticated purification methods. An excellent agreement isfound in the comparison of the IC model with established models from the existing literature, the Shardmodel and the software SESSA. KW - XPS KW - Quantum dot KW - Core shell nano particle PY - 2016 DO - https://doi.org/10.1016/j.elspec.2016.08.002 SN - 0368-2048 VL - 212 SP - 34 EP - 43 PB - Elsevier B.V. AN - OPUS4-38273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Swaraj, S. A1 - Dietrich, Paul M. T1 - X-ray spectromicroscopy of nanoparticulate iron oxide phases N2 - Soft x-ray spectromicroscopy techniques have seen great amount of development in the recent years, and with the development of new diffraction limited synchrotron source, many new nanoscale and mesoscale characterization opportunities of applied materials are foreseen. In this perspective, the authors present some examples that illustrate the capabilities of spectromicroscopy techniques, namely, 2D and 3D spatially resolved chemical quantification, surface and bulk sensitive measurements, and polarization dependent measurements as applied to iron oxide nanoparticulate materials of biological, geological, and other origins. KW - X-ray spectromicroscopy KW - STXM KW - Iron oxide PY - 2016 DO - https://doi.org/10.1116/1.4966654 SN - 1934-8630 SN - 1559-4106 VL - 11 IS - 4 SP - 04B402-1 EP - 04B402-6 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-38274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Current activities to implement the technology roadmap „Process Sensors 4.0“ N2 - As presented at the NAMUR general meeting 2015, the technology roadmap "Process Sensors 4.0" identifies the necessary requirements as well as the communication abilities of such process sensors. We report on the progress of discussions in trialogue between users, software and device manufacturers as well as the research. An important key is the definition of an appropriate and uniform topology for such smart sensors, which will be driven forward in a new NAMUR AK 3.7 "smart sensors" in mutual exchange with device and software manufacturers and research institutions. T2 - NAMUR General Meeting 2016 CY - Bad Neuenahr, Germany DA - 10.11.2016 KW - Prozess-Sensoren KW - Prozess-Sensoren 4.0 KW - Prozess-Spektroskopie KW - Process analytical technology PY - 2016 AN - OPUS4-38228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönhals, Andreas A1 - Zorn, R. A1 - Frick, B. T1 - Inelastic neutron spectroscopy as a tool to investigate nanoconfined polymer systems N2 - The effect of a nanometer scale confinement (pore sizes 7.5 nm down to 2.5 nm) on the vibrational density of states (VDOS) and on the molecular dynamics of Poly(dimethyl siloxane) (PDMS) and Poly(-methyl phenyl siloxane) (PMPS) is studied by inelastic Neutron scattering. The high penetration depth of neutrons makes neutron scattering a suitable tool for the study of confined systems. Moreover, Neutrons are sensitive to light nuclei therefore the confined polymers can be investigated directly, more or less independently of the confining host. Resulting findings are firstly, a reduction of the low frequency contributions to the VDOS below the Boson Peak frequency for both polymers. Including literature data, this reduction can be regarded as a more general feature for glass-forming systems confined by hard walls. Secondly, clear deviations in the temperature dependence of the mean squared displacement of the confined molecules compared to the bulk were found close to the thermal glass transition temperature, whereas localized methyl group rotations were only weakly influenced. Furthermore, the molecular dynamics is accessed. The combination of neutron Time-of-Flight with neutron backscattering, thus covering a broad dynamical range from sub ps to ns, reveal clear influence from confinement on the intermediate incoherent scattering function S(q,t). The latter was obtained by combining the inverse Fourier transform of the individual dynamical structure factors measured by the both methods. The time and q dependence of S(q,t) are discussed in detail for the local methyl group rotations and the segmental dynamics, considering both the interaction of the segments with the pore walls and possible geometrical confinement effects. KW - Confinement KW - Density of states KW - Dynamic glass transition PY - 2016 DO - https://doi.org/10.1016/j.polymer.2016.06.006 SN - 0032-3861 SN - 1873-2291 VL - 105 SP - 393 EP - 406 PB - Elsevier AN - OPUS4-38256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hetti, M. A1 - Wei, Q. A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Bartusch, M. A1 - Neu, V. A1 - Pospiech, D. A1 - Voit, B. T1 - Magnetite core-shell nanoparticles in nondestructive flaw detection of polymeric materials N2 - Nondestructive flaw detection in polymeric materials is important but difficult to achieve. In this research, the application of magnetite nanoparticles (MNPs) in nondestructive flaw detection is studied and realized, to the best of our knowledge, for the first time. Superparamagnetic and highly magnetic (up to 63 emu/g) magnetite core-shell nanoparticles are prepared by grafting bromo-end group-functionalized poly(glycidyl methacrylate) (Br-PGMA) onto surface-modified Fe3O4 NPs. These Fe3O4-PGMA NPs are blended into bisphenol A diglycidylether (BADGE) based epoxy to form homogeneously distributed magnetic epoxy nanocomposites (MENCs) after curing. The core Fe3O4 of the Fe3O4-PGMA NPs endows the MENCs with magnetic property, which is crucial for nondestructive flaw detection of the materials, while the shell PGMA promotes colloidal stability and prevents NP aggregation during curing. The eddy current testing (ET) technique is firstly applied to detect flaws in the MENCs. Through the brightness contrast of the ET image, surficial and sub-surficial flaws in MENCs can be detected, even for MENCs with low content of Fe3O4-PGMA NPs (1 wt %). The incorporation of Fe3O4-PGMA NPs can be easily extended to other polymer and polymer-based composite systems and opens a new and very promising pathway toward MNP-based nondestructive flaw detection in polymeric materials. KW - Magnetite nanoparticles KW - Poly(glycidyl methacrylate) KW - Atom transfer radical polymerization KW - Magnetic nanocomposites KW - Nondestructive flaw detection PY - 2016 DO - https://doi.org/10.1021/acsami.6b09934 SN - 1944-8244 SN - 1944-8252 VL - 8 IS - 41 SP - 28208 EP - 28215 PB - American Chemical Society CY - Washington, DC AN - OPUS4-38300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ehlert, Christopher T1 - A detailed assignment of NEXAFS resonances of imidazolium based ionic liquids N2 - In Near Edge X-Ray Absorption Fine Structure (NEXAFS) spectroscopy X-Ray photons are used to excite tightly bound core electrons to low-lying unoccupied orbitals of the system. This technique offers insight into the electronic structure of the system as well as useful structural information. In this work, we apply NEXAFS to two kinds of imidazolium based ionic liquids ([CnC1im]+ [NTf2]− and [C4C1im]+ [I]−). A combination of measurements and quantum chemical calculations of C K and N K NEXAFS resonances is presented. The simulations, based on the transition potential density functional theory method (TP-DFT), reproduce all characteristic features observed by the experiment. Further, a detailed assignment of resonance features to excitation centers leads to a consistent interpretation of the spectra. T2 - 52nd Symposium on Theoretical Chemistry (STC2016) CY - Ruhr Universität Bochum, Germany DA - 26.9.2016 KW - NEXAFS KW - Simulation KW - Ionic liquid PY - 2016 AN - OPUS4-38276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph A1 - Kruschwitz, Sabine A1 - Boller, C. A1 - Wiggenhauser, Herbert T1 - Feasibility study on adapting a machine learning based multi-sensor data fusion approach for honeycomb detection in concrete N2 - We present the results of a machine learning (ML)- inspired data fusion approach, applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) measurements collected on large-scale concrete specimens with built–in simulated honeycombing defects. In a previous study we were able to improve the detectability of honeycombs by fusing the information from the three different sensors with the density based clustering algorithm DBSCAN. We demonstrated the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The main objective of this contribution is to investigate the generality, i.e. whether the conclusions from one specimen can be adapted to the other. The effectiveness of the proposed approach on a separate full-scale concrete specimen was evaluated. T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology 2016 CY - Portland, Oregon, USA DA - 29.08.2016 KW - Data fusion KW - Concrete evaluation KW - Honeycombing KW - Machine learning KW - Clustering PY - 2016 SN - 978-1-57117-392-8 SP - 144 EP - 148 PB - The American Society for Nondestructive Testing, Inc CY - Portland, Oregon, USA AN - OPUS4-38288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Feasibility study on adapting a machine learning based multi-sensor data fusion approach for honeycomb detection in concrete N2 - We present the results of a machine learning (ML)- inspired data fusion approach, applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) measurements collected on large-scale concrete specimens with built–in simulated honeycombing defects. In a previous study we were able to improve the detectability of honeycombs by fusing the information from the three different sensors with the density based clustering algorithm DBSCAN. We demonstrated the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The main objective of this contribution is to investigate the generality, i.e. whether the conclusions from one specimen can be adapted to the other. The effectiveness of the proposed approach on a separate full-scale concrete specimen was evaluated. T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology 2016 CY - Portland, Oregon, USA DA - 29.08.2016 KW - Data fusion KW - Concrete evaluation KW - Honeycombing KW - Machine learning KW - Clustering PY - 2016 AN - OPUS4-38289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias T1 - Leak detection with linear soil gas sensors under field conditions - First experiences running a new measurement technique N2 - A 400 m² soil test field with gas injection system was built up, which enables an experimental validation of linear gas sensors for specific applications and gases in an application-relevant scale. Several injection and soil watering experiments with carbon dioxide (CO2) at different days with varying boundary conditions were performed indicating the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Soil test field KW - Membrane-based linear gas sensor KW - Leak detection KW - Field conditions PY - 2016 SN - 978-1-4799-8287-5 SN - 1930-0395 SP - B-3-65, 757 EP - 759 PB - IEEE AN - OPUS4-38244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. T1 - Leak detection with linear soil gas sensors under field conditions - First experiences running a new measurement technique N2 - A 400 m² soil test field with gas injection system was built up, which enables an experimental validation of linear gas sensors for specific applications and gases in an application-relevant scale. Several injection and soil watering experiments with carbon dioxide (CO2) at different days with varying boundary conditions were performed indicating the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Soil test field KW - Membrane-based linear gas sensor KW - Leak detection KW - Field conditions PY - 2016 AN - OPUS4-38247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fretwurst, T. A1 - Buzanich, Günter A1 - Nahles, S. A1 - Woelber, J. P. A1 - Riesemeier, Heinrich A1 - Nelson, K. T1 - Metal elements in tissue with dental peri-implantitis: a pilot study N2 - Objectives: Dental peri-implantitis is characterized by a multifactorial etiology. The role of metal elements as an etiological factor for peri-implantitis is still unclear. The aim of this study was to investigate the incidence of metal elements in bone and mucosal tissues around dental Grade 4 CP titanium implants with signs of peri-implantitis in human patients. Methods: In this prospective pilot study, all patients were enrolled consecutively in two study centers. Bone and soft tissue samples of patients with peri-implantitis with indication for explantation were analyzed for the incidence of different elements (Ca, P, Ti, Fe) by means of synchrotron radiation X-ray fluorescence spectroscopy (SRXRF) and polarized light microscopy (PLM). The existence of macrophages and lymphocytes in the histologic specimens was analyzed. Results: Biopsies of 12 patients (seven bone samples, five mucosal samples) were included and analyzed. In nine of the 12 samples (75%), the SRXRF examination revealed the existence of titanium (Ti) and an associated occurrence with Iron (Fe). Metal particles were detected in peri- implant soft tissue using PLM. In samples with increased titanium concentration, lymphocytes were detected, whereas M1 macrophages were predominantly seen in samples with metal particles. Conclusion: Titanium and Iron elements were found in soft and hard tissue biopsies retrieved from peri-implantitis sites. Further histologic and immunohistochemical studies need to clarify which specific immune reaction metal elements/particles induce in dental peri-implant tissue. KW - Peri-implantitis KW - Metal elements KW - Synchrotron radiation X-ray fluorescence PY - 2016 DO - https://doi.org/10.1111/clr.12718 SN - 0905-7161 VL - 27 IS - 9 SP - 1178 EP - 1186 PB - WILEY-BLACKWELL CY - 111 RIVER ST, HOBOKEN 07030-5774, NJ USA AN - OPUS4-38641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Surfchem - Traceable quantitative surface chemical analysis for industrial applications N2 - The project addresses chemical and topographical metrology at surfaces. The new methodologies of measurements at surfaces will be developed as good practice guides and new work item proposals for industrial ISO standards. The objectives of the Joint research project (JRP) are to provide measurement standards and methods with traceability wherever it is practicable to do so for quantitative surface chemical analysis for industrial applications. KW - Method development KW - Surface chemical analysis KW - Analytical methods KW - Reference material PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386319 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Vivien A1 - Gong, Xin A1 - Hofmann, Detlef A1 - Basedau, Frank A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Westphal, Anja A1 - Sahre, Mario A1 - Beck, Uwe ED - Berghmans, F. ED - Mignani, A. G. T1 - Modelling and simulation of a fibre Bragg grating strain sensor based on a magnetostrictive actuator principle N2 - A new concept for the self-diagnosis of embedded fiber Bragg grating (FBG) strain sensors was developed, simulated and experimentally tested. This concept is based on a magnetostrictive metallic layer directly coated on the fibre cladding over the grating segment of the FBG sensor, so that an on-demand external magnetic field in a millitesla scale can produce a controllable artificial strain as an indication signal for the remote optical interrogator. The relationship between the pre-defined magnetic field and its induced Bragg wavelength shift characterizes this validation concept. Any deviation of the local bonding state of the interfaces from the initial or/and any change of shear strain transferring mechanism from composite matrix to the optical fibre core will result in alterations in this sensitive relationship, and thus triggers an immediate alert for a further inspection. The finite element method is used to simulate the strain of this configuration as result of different values of the magnetic field in order to optimize the geometrical sensor parameters. The simulations are verified by experiments results. © (2016) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE). Downloading of the abstract is permitted for personal use only. T2 - Optical Sensing and Detection IV CY - Brüssel, Belgium DA - 03.04.2016 KW - Fiber Bragg gratings KW - Actuators KW - Modeling and simulation KW - Finite element methods PY - 2016 SN - 9781510601444 DO - https://doi.org/10.1117/12.2224728 SN - 0277-786X SN - 1996-756X VL - 9899 SP - 9899-39 PB - SPIE Digital Library AN - OPUS4-38634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koegler, M. A1 - Paul, Andrea A1 - Alborch, K. P. A1 - Birkholz, M. A1 - Junne, S. A1 - Neubauer, P. T1 - Raman on-line monitoring approach for bioprocess and bio-pharmaceutical manufacturing N2 - There is a high demand of monitoring in the era of QbD in industrial scale require new approaches to gain data rapidly and of sufficient quality in real time. Raman spectroscopy technology has great potential but not yet shown it fully in process on-line monitoring due to limitations such as i) uncomplete separation between cells and growth media alone, ii) general weak Raman signals of analytes in complex solutions and iii) strong background signals such as the auto-fluorescence, cosmic rays and surrounding lights overlapping the weak Raman signals. Here we demonstrate a Proof-of-Concept on an the example lactic acid bacteria process using a Streptococcus thermophiles fermentation. Results from three different Raman approaches are presented: 1) Time-Gated Raman Spectroscopy (TG-Raman), 2) Surface Enhanced Raman Spectroscopy (SERS) and 3) Raman process spectroscopy with NIR excitation combined with multivariate data analysis (MVDA) using Principal Component Analysis (PCA) and Partial Least Squares Regression (PLSR). T2 - 12. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman KW - Chemometrics KW - SERS KW - TimeGate PY - 2016 SP - 91 EP - 93 CY - Berlin AN - OPUS4-38673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Applicability of CCQM-P149 to support CMCs N2 - The presentation describes the limitations of CCQM-P149 to be used for supporting CMCs and it gives possibilities and applications where CCQM-P149 can provide additional Support. T2 - CCQM IAWG Meeting CY - Daejeon, South Korea DA - 04.10.2016 KW - CCQM KW - CMC KW - Purity assessment PY - 2016 AN - OPUS4-38586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - MetVBadBugs - XRF and NAP-XPS characterization of drug uptake in multi-resistant bacteria N2 - Multi-resistant bacteria embedded in infectious biofilms are one of the largest future threats in human healthcare. The mechanism of drug uptake and the origin of resistancy is quantitatively not well characterized and understood. Modern X-ray and synchrotron excited spectroscopic methods like XRF and NAP-XPS under ambient pressure conditions and liquid media will add new insights into this field. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XPS KW - XRF KW - Biofilm PY - 2016 AN - OPUS4-38684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Nele T1 - Nuclease activity of copper(II)phenanthroline complexes immobilized on silicon nitride films N2 - Copper(II)phenanthroline complexes intercalate into DNA and induce DNA cleavage. Here, we investigate the nuclease activity of copper(II)phenanthroline complexes on Silicon nitride films. 1,10-phenanthroline-5-carboxylic acid is immobilized at Si-NHx bonds via amide coupling followed by the formation of copper(II)phenanthroline complexes. XPS and NEXAFS were carried out at the HE-SGM beamline. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XPS KW - NEXAFS KW - Copper(II) - phenanthroline - complexe filmss PY - 2016 AN - OPUS4-38685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Seewald, G. T1 - 2PM FlySCAN: Innovative approach for wide field high resolution imaging of skin tissue volumes N2 - Two Photon Microscopy (2PM) is an innovative Technology for high resolution imaging of human skin in vivo and ex vivo. Up to now the method is limited by its interdependence between the field of view and the attainable resolution. The new FlySCAN Technology overcomes these boundaries and enable images sizes of many millimeters by resolutions in the submicrometer range revealing very specific information on clinically and biologically relevant tissue and cell structures. The advantages of the new approach are demonstrated by excellent in vivo and ex vivo tissue images. T2 - EPIC Biophotonics Workshop “Translating Biophotonics Technologies to Clinical Oncology: Perspectives & Challenges” CY - Paris, France DA - 01.12.2016 KW - Two photon microscopy KW - Wide field KW - Skin tissue PY - 2016 AN - OPUS4-38687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Philipp, Rosemarie T1 - Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC N2 - The European Water Framework Directive (WFD) 2000/60/EC specifies a list of 33 priority water pollutants. For these substances, Environmental Quality Standards (EQS), equivalent to the maximum allowable concentrations, had been defined at very low levels. EQS values refer to the whole water body, i.e. include contaminants which are associated to suspended solids or colloids present in the natural water. For several priority pollutants primary analytical methods capable of measuring the target analytes at EQS level in natural water are still missing. The project has developed and validated such methods for three selected compounds, namely Tributyltin (TBT), Polybrominated Diphenylether (PBDE) and Polycyclic Aromatic Hydrocarbons (PAH). KW - Water polluntants KW - Monitoring KW - Water analysis KW - Tributyltin KW - Polybrominated diphenylether KW - Polycyclic aromatic hydrocarbons PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386230 SP - 1 EP - 3 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Roadmap for purity determination N2 - A Roadmap for the purity Determination of pure metallic elements is presented. The roadmap distinguishes between different approaches for the purity determination and list theindividual steps for each Approach which are necessary to successfully apply These approaches. T2 - CCQM IAWG Meeting CY - Daejeon, South Korea DA - 04.10.2016 KW - Traceability KW - Purity determination PY - 2016 AN - OPUS4-38590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Development of an online-analysis technique for the determina-tion of plant essential nutrients in soils using XRF and LIBS N2 - The main task of BAM in the I4S project is the development of online analytics for reliable monitoring of major and minor nutrients like K, P, Ca in soil using mobile-XRF (X-ray fluorescence spectroscopy) and mobile-LIBS (laser-induced breakdown spectroscopy). Each method provides fast and simultaneous multi-element analyses which are neccessary for mapping agricultural cropland. The first objective was to design a combined measurement setup for XRF and LIBS. The centerpiece is the rotatable sample plate which enables the measurement of moving samples. Current steps are the optimisation of the parameters for the analysis of soils. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - RFA KW - Agricultural KW - LIBS KW - Online KW - Soil KW - Monitoring PY - 2016 AN - OPUS4-38591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Establishment of reference values for sensor based soil analysis N2 - Production of soil reference materials (for project partners) is integrated into the project „X-ray fluorescence, laser-induced breakdown spectroscopy (and Raman spectroscopy) as tools for a site-specific management of soil fertility“. BAM provides good analytics which is necessary for measuring the right values. Why is it important to have reference values? They enable the connection of own measuring results to the SI (international system of units) and the comparison with results from other laboratories. The soil reference materials are also needed for the calibration of the matrix dependent methods laser-induced breakdown spectroscopy (LIBS) and X-ray fluorescence analysis (XRF). For the production of soil reference materials different steps are required, for example drying, sieving and homogenisation. T2 - BonaRes Statusseminar CY - Leipzig, Germany DA - 14.11.2016 KW - LIBS KW - Reference KW - Homogenisation KW - Calibration KW - RFA KW - Soil PY - 2016 AN - OPUS4-38593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -