TY - JOUR A1 - Völzke, Holger A1 - Nieslony, Gregor A1 - Noack, Volker A1 - Hagenow, Peter A1 - Kovacs, Oliver T1 - Current developments in container design testing for the Konrad repository N2 - At present BAM works on numerous applications for Container design testing for the Konrad repository. Some licensing procedures were successfully finished in the past and BfS certified several Container types like Steel sheet, concrete until cast iron containers which are now available for waste packaging for final disposal. However, large quantities of radioactive wastes had been placed into interim storage using containers which are not already approved for the Konrad repository. Safety assessment of these so-called “old” containers is a big challenge for all parties because documentation sheets about container design testing and fabrication often contain gaps or have not yet been completed. Appropriate solution strategies are currently under development and discussion. Furthermore, BAM has successfully initiated and established an Information forum, called “ERFA QM Konrad Containers”, which facilitates discussions on various issues of common interest with respect to Konrad container licensing procedures as well as the interpretation of disposal requirements under consideration of operational needs. Thus, it provides additional, valuable supports for container licensing procedures. T2 - KONTEC 2011 - 10. Internationales Symposium "Konditionierung radioaktiver Betriebs- und Stilllegungsabfälle" CY - Dresden, Germany DA - 06.04.2011 KW - Radioactive waste KW - Container KW - Testing KW - Konrad repository PY - 2012 SN - 1431-5254 VL - 57 IS - 5 SP - 343 EP - 346 PB - Inforum CY - Berlin AN - OPUS4-25988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja T1 - Combined impact of UV radiation and nitric acid (HNO3) on HDPE jerrycans – comparison of outdoor and lab test N2 - A damaging action of HNO3-55% only occurs in combination with its decomposition into nitrous gases, which can be caused by UV radiation. In a laboratory test, transparent HDPE jerrycans have been exposed to both UV radiation and 55 wt-% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The respective damages are compared with FTIR spectroscopy in ATR and HT-gel permeation chromatography (GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. The gradual increase in oxidative damage shows the good reproducibility of the lab exposure. The decomposition of nitric acid into nitrous gases by UV radiation – as well as the jerrycan oxidation – is also observed at lower HNO3 concentration (28 wt- %). Similar results are obtained after outdoor tests. Again, the damage occurs only after combined exposure, in contrast to the exposures to UV only and to HNO3 only, which were conducted in parallel. Outdoor exposures are most readily accepted as they represent possible end-use conditions. However, the reproducibility of these exposures is poor due to the large temporal variations in weather. There are also several safety risks, which is why the number of replicates remains limited. Since the outdoor and lab exposure tests show the same qualitative results, it is appropriate to conduct systematic studies in the laboratory. After 6 days of lab exposure, the oxidation damage is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. It should be noted that this amount can also occur in two sunny weeks. T2 - 24th iapri World Packaging Conference CY - Valencia, Spain DA - 17.06.2024 KW - UV exposure KW - Nitric acid KW - Polyethylene KW - Oxidation PY - 2024 AN - OPUS4-60416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolkoori, Sanjeevareddy A1 - Rahman, Mehbub-Ur A1 - Prager, Jens T1 - Effect of columnar grain orientation on ultrasonic plane wave energy reflection and transmission behaviour in anisotropic austenitic weld materials N2 - This article describes a comprehensive quantitative analysis on effect of columnar grain orientation on ultrasonic plane wave energy reflection and transmission behaviour in acoustically anisotropic austenitic weld materials. The quantitative results are presented for following general interfaces (a) Isotropic-Anisotropic, (b) Anisotropic-Isotropic, (c) Fluid-Anisotropic, (d) Anisotropic-Fluid, (e) Anisotropic-Anisotropic, (f) Anisotropic-Free surface occur during the ultrasonic non destructive evaluation of austenitic weld materials. Explicit analytical expressions are presented for energy reflection and transmission coefficients at an interface between two arbitrarily oriented transversely isotropic materials. By applying explicit analytical expressions for energy reflection and transmission coefficients, numerical results are presented for several columnar grain orientations of the transverse isotropic austenitic weld material including both real and complex domain of the reflected and transmitted normal component of slowness vectors. Valid domains of incident wave vector angles, angular dependency of energy reflection and transmission coefficients and critical angles for reflected and transmitted waves are discussed. The existence of a reflected (or) transmitted second branch of quasi shear vertical waves and its consequence to the ultrasonic non destructive testing of austenitic weld materials are investigated. The presented comprehensive quantitative evaluation provides an overview on the effect of anisotropic properties on energy reflection and transmission coefficients in columnar grained austenitic weld materials. KW - Anisotropy KW - Inhomogeneous waves KW - Austenitic weld material KW - Polarization vector KW - Energy skewing KW - Critical angle KW - Energy flux vector KW - Evanescent waves PY - 2012 DO - https://doi.org/10.1007/s10921-012-0140-1 SN - 0195-9298 SN - 1573-4862 VL - 31 IS - 3 SP - 253 EP - 269 PB - Plenum Press CY - New York, NY AN - OPUS4-27792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Geburtig, Anja T1 - Alterungseffekte bei Polymerwerkstoffen messen N2 - Bei der Auswahl von Werkstoffen spielt deren Alterung oft eine untergeordnete Rolle, stattdessen wird häufig der ungealterte Ausgangszustand optimiert. Materialien altern aber unterschiedlich. Der Effekt der molekularen Alterung spiegelt sich in den Eigenschaften mehr oder weniger stark und in unterschiedlichem zeitlichen Verlauf wider. Da es kein physikalisch-chemisches Modell dafür gibt, sind Alterungseffekte empirisch zu bestimmen. KW - Alterung KW - Polymerwerkstoff KW - Eigenschaftsänderung PY - 2012 DO - https://doi.org/10.1002/nadc.201290356 SN - 1439-9598 SN - 1521-3854 VL - 60 IS - 10 SP - 1018 EP - 1022 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26666 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Schulz, Ulrich A1 - Geburtig, Anja A1 - Stephan, Ina T1 - Mildew growth on automotive coatings influencing the results of outdoor weathering N2 - As the results of a 14 weeks outdoor exposure of a series of automotive coatings in South Florida, the panels were found to be overgrown with an almost closed layer of mildew. Pinholes remained as permanent surface damage after removing the mildew mycelium. The extent of the damage differed in dependence of the kind of the coating. By tracing the images and profiles of the coating surfaces systematically over all phases of weathering and the subsequent cleaning procedure, a connection between formation of pinholes and mildew growth could be found. Outdoor weathering tests in other regions of Florida as well as in Europe and Australia showed that pinholes caused by mildew attack could also be found in all other locations, but always to a lower extent than in South Florida. The standardised mildew tests EN ISO 846 and MIL-STD 810F for laboratory exposure failed to reproduce the formation of pinholes. KW - Coatings KW - Mildew KW - Weathering KW - South Florida PY - 2012 DO - https://doi.org/10.1002/maco.201005784 SN - 0947-5117 SN - 1521-4176 VL - 63 IS - 2 SP - 140 EP - 147 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-25467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - PE-Rezyklat Einsatz in Gefahrgutbehältern? N2 - In diesem Vortrag geht es darum zu beschreiben, ob Rezyklat für PE Behälter gefüllt mit Gefahrgut Anwendung finden darf. Kanister aus Neuware und Rezyklat wurden verschiedenen Untersuchungen unterzogen. Es wurde der Feststoff und Leachable getestet. Methoden sind TED-GC/MS und GC-HRMS. Proben der Leachable wurden nach 1 und 4 Wochen genommen und die Peakanzahl vergleichen dargestellt. Als Lösemittel wurden Wasser, Ethanol, EtOAc, Ammoniak und HNO3 verwendet. T2 - Fachaustausch Projekt GeSKAR CY - Dessau, Germany DA - 10.01.2025 KW - Gefahrgutbehälter KW - Rezyklat PY - 2025 AN - OPUS4-62396 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - What can thermoanalytical methods do for you ? N2 - This presentation summarizes outcomes of the CUSP projects POLYRISK and PlasticsFatE according to thermoanalytical methods.It highlights the importants of analytical methods to measure physical and chemical properties of the test materials. These informations are neccessary for interpretation of the toxicological test results. T2 - CUSP conference CY - Utrecht, Netherlands DA - 14.09.2023 KW - Microplastics KW - TED-GC/MS KW - CUSP KW - Polymer 3R KW - Thermoanalytical methods PY - 2023 AN - OPUS4-58312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallstabe, Ronald T1 - Laser-assisted surface modification of alumina and its tribological behavior N2 - High performance friction systems, e.g., dry clutches and brakes, require a good wear resistance and a friction coefficient that is nearly independent from sliding velocity and environmental conditions. Organic-based friction materials have reached their limitations regarding higher power densities. Engineering ceramics such as alumina (Al2O3) or silicon carbide (SiC) offer a great potential since remarkably higher thermal and mechanical loading is possible. However, the tribological performance of these monolithic ceramics is still insufficient. The aim of the present study was to assess the potential of a laser-assisted surface modification process in order to improve the tribological performance with regard to the application in dry friction systems. Therefore, commercially available alumina was modified using a newly developed laser-assisted preheating process and subsequent melting of the ceramic’s surface using a CO2-laser and modification by additives such as TiC, TiN, B4C, WC, ZrB2, Cr, Ni, Cu, and Ti. A systematic variation of additives and process parameters led to different multiphase microstructures. Subsequently, these were characterized using scanning electron microscopy and surface analysis methods (wavelength dispersive X-ray spectroscopy, energy dispersive X-ray spectroscopy). Finally, the tribological properties were investigated using a laboratory tribometer. The surface-modified ceramics were tested in unidirectional sliding motion against steel disks. The tribological results of the surface-modified ceramics were compared to those of monolithic Al2O3 and SiC ceramics and showed a reduced dependence of friction coefficient on sliding velocity. Moreover, the multi-phase ceramics possessed a higher wear resistance than the monolithic ones. KW - Alumina KW - Ceramics KW - Ceramic matrix composites KW - Dry sliding KW - Laser-assisted surface modification KW - Steel KW - Tribology KW - Wear resistance PY - 2013 DO - https://doi.org/10.1007/s11665-012-0215-2 SN - 1059-9495 SN - 1544-1024 VL - 22 IS - 1 SP - 223 EP - 235 PB - ASM International CY - Materials Park, Ohio AN - OPUS4-25842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Komann, Steffen A1 - Kiyak, Yusuf A1 - Wille, Frank A1 - Zerbst, Uwe A1 - Weber, Mike A1 - Klingbeil, Dietmar T1 - Assessment of ductile cast iron fracture mechanics analysis within licensing of German transport packages N2 - In recent years BAM was involved in several licensing procedures of new package designs for the transport of radioactive material, where the cask body was made of Ductile Cast Iron (DCI). According to IAEA regulations type B(U) packages must withstand the defined accident conditions of transport. For the cask material DCI, it is necessary to determine the brittle fracture behaviour. Due to the complex structure of the cask body and the dynamic loading a fracture mechanical assessment in an analytical way is not always possible. Numerical calculations are necessary to determine the fracture mechanical load in the component. At the first step a numerical analysis has to be done to identify the loading state at the cask body. Secondly an analysis of a detail of the cask body is made considering the boundary conditions of the global model. An artificial flaw is considered in this detailed model to calculate the fracture mechanical loading state. The size of the artificial flaw is characterized by the ultrasonic inspection used for the quality assurance of the package. The applicant developed additional analysis tools for calculation of stress intensity factor and/or J-Integral. The paper describes the authority assessment approach for the DCI fracture mechanics analysis. T2 - ASME 2012 Pressure vessels & piping division conference CY - Toronto, Ontario, Canada DA - 15.07.2012 PY - 2012 SP - PVP2012-78213, 1-7 PB - American Society of Mechanical Engineers CY - New York AN - OPUS4-26363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachtendorf, Volker A1 - Wägner, Yannick A1 - Geburtig, Anja T1 - Gedanken, Tipps & Tricks zu künstlichen Bewitterungsprüfungen N2 - Die Fragestellung kann nur exemplarisch dargestellt werden, aber ist hoffentlich auch für langjährige Praktiker in den ausgewählten Punkten interessant. Es sollen für folgende Bereiche Beispiele gegeben werden: Probenvorbereitung, Testvorbereitung, Testdurchführung und Auswertung. T2 - 53. Jahrestagung der GUS 2025 CY - Stutensee-Blankenloch bei Karlsruhe, Germany DA - 26.03.2025 KW - Wechseltemperaturen KW - Künstliche Bewitterung KW - Prüfung KW - UV KW - Feuchte KW - Beregnung PY - 2025 SN - 978-3-9826129-2-8 VL - 53 SP - 253 EP - 257 PB - Gesellschaft für Umweltsimulation e.V. CY - 76327 Pfinztal (Berghausen) AN - OPUS4-62861 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rouquerol, J. A1 - Baron, G. A1 - Denoyel, R. A1 - Giesche, H. A1 - Groen, J. A1 - Klobes, Peter A1 - Levitz, P. A1 - Neimark, A.V. A1 - Rigby, S. A1 - Skudas, R. A1 - Sing, K. A1 - Thommes, M. A1 - Unger, K. T1 - Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC technical report) N2 - This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 µm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion–extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed and evaluated. The reliability of mercury porosimetry is discussed in the first part of the report along with the conditions required for its safe use. Other procedures for macropore size analysis, which are critically examined, include the intrusion of other non-wetting liquids and certain wetting liquids, capillary condensation, liquid permeation, imaging, and image analysis. The statistical reconstruction of porous materials and the use of macroporous reference materials (RMs) are also examined. Finally, the future of macropore analysis is discussed. KW - Capillary condensation KW - Image analysis KW - IUPAC physical and biophysical chemistry division KW - Liquid intrusion KW - Macroporous materials KW - Mercury prorsimetry KW - Permeation KW - Pore size characterization KW - Reference porous materials KW - Statistical reconstruction of porous solids PY - 2012 DO - https://doi.org/10.1351/PAC-REP-10-11-19 SN - 0033-4545 SN - 1365-3075 VL - 84 IS - 1 SP - 107 EP - 136 PB - Union CY - Research Triangle Park, NC AN - OPUS4-26109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jagenbrein, A. A1 - Tscheliesnig, P. A1 - Wachsmuth, Janne A1 - Bohse, Jürgen T1 - Detection of corrosion processes and fatigue cracks by means of acoustic emission monitoring N2 - Fatigue crack growth and active corrosion processes are the main causes for structural failures of transport products like road tankers, railway tank cars, and ships. Within the 7th EC framework programme the aim of project CORFAT is to develop a new monitoring technology based on acoustic emission testing (AT) of the structural integrity in terms of proceeding degradation. Differentiation of acoustic emission (AE) signals of real degradation processes by fatigue crack growth or active corrosion from operational or environmental background noise requires the signal classification using also pattern recognition. Therefore, a data base of AE signals related to the different source mechanisms was built up experimentally. In this article selected results of corrosion and fatigue tests in the laboratory as well as results of monitoring background noise during moving of a road tanker are described. KW - Acoustic emission monitoring KW - Corrosion processes KW - Fatigue cracks KW - Background noise KW - Signal classification KW - Transport products PY - 2012 DO - https://doi.org/10.3139/120.110391 SN - 0025-5300 VL - 54 IS - 11-12 SP - 769 EP - 778 PB - Hanser CY - München AN - OPUS4-27061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Gorbushina, Anna A1 - Plarre, Rüdiger A1 - Stephan, Ina T1 - Umweltsimulation an der BAM – Grundlegende Ansätze mit Beispielen aus der natürlichen Umwelt N2 - Drei grundlegend verschiedene Ansätze für Umweltsimulation werden an Beispielen illustriert: (i) Ganzheitlicher Ansatz - Nachstellen von Umweltmilieus im Labor Ziel ist hier das Nachstellen von (kombinierten) Umweltbedingungen im Labor; die Umweltparameter werden mit all ihren Wechselwirkungen aufgebracht. Hauptnutzen ist eine gegenüber der natürlichen Beanspruchung erhöhte Reproduzierbarkeit der Umweltbedingungen. Hat man sein Laborsetup entwickelt, ist es auf verschiedene Materialien anwendbar. Unter solchen Laborbedingungen ermittelte Lebensdauern sind dabei nicht auf die typischerweise sehr variablen Real-Umweltbedingungen übertragbar. (ii) Parametrisierter Ansatz - Ermittlung einzelner Materialempfindlichkeiten Hierbei werden im Labor die Wirkungen separater Umweltparameter auf Materialien nachgestellt. Für eine solche Separation der Einflussfaktoren ist insbesondere die Aufschlüsselung möglicher Wechselwirkungen der Umwelt-parameter (z.B. Mikroklima an bestrahlten Oberflächen) erforderlich. Einzelne (meist Alterungs-) Empfindlichkeiten können qualitativ nachgewiesen werden oder sogar – als Beanspruchungs-Wirkungs-Funktionen – quantifiziert werden, was einen wesentlichen Schritt in Richtung der Digitalisierung der Material¬prüfung darstellt. Insbesondere ist dann auch eine Lebensdauer-vorhersage für vorgegebene Zeitreihen der Beanspruchungs¬parameter umsetzbar. (iii) Rückwirkungen auf die Umwelt Umweltbeanspruchungen können zur Freisetzung von Schadstoffen in die Umwelt führen. Durch die Nachstellung kritischer, aber realitätsnaher Einsatzszenarien kann die Menge an freigesetzten Substanzen abgeschätzt werden. Egal, welcher Ansatz verfolgt wird – ein Vergleich mit der oder einer Real-beanspruchung ist unerlässlich, ebenso wie die Messdatenaufzeichnung (data logging) aller potenziell relevanten Beanspruchungsparameter während dieser Realbeanspruchung. Obwohl die naturnahe Umwelt – sowohl in der BAM als auch bei der GUS – gegenüber der technischen Umwelt eher untergeordnet auftritt, werden zur Illustration Beispiele aus der naturnahen Umwelt verwendet. T2 - 50. Jahrestagung der GUS CY - Online meeting DA - 23.03.2022 KW - Umweltsimulation PY - 2022 SN - 978-3-9818507-7-2 SP - 79 EP - 89 AN - OPUS4-55015 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kempel, Florian A1 - Schartel, Bernhard A1 - Linteris, G.T. A1 - Stoliarov, S.I. A1 - Lyon, R.E. A1 - Walters, R.N. A1 - Hofmann-Böllinghaus, Anja T1 - Prediction of the mass loss rate of polymer materials: Impact of residue formation N2 - Two different numerical simulation tools, Fire Dynamic Simulator (FDS) and ThermaKin, are investigated with respect to their capability to predict the mass loss rate of polymer materials exposed to different fires. For validation, gasification apparatus and cone calorimeter tests are conducted. The main focus is on the influence of residue formation. Therefore, poly (butylene terephthalate) (PBT) and PBT reinforced with glass fibres (PBT-GF) are investigated and compared. PBT decomposes almost completely, while PBT-GF forms residue. The materials are characterised in order to provide suitable input parameters. Additionally the total incident heat flux to the sample is measured. With accurate input parameters, FDS and ThermaKin predicted the pyrolysis behaviour of PBT very well. Only some limitations are identified regarding the residue-forming PBT-GF. Both numerical simulation tools demonstrate a high value regarding the assessment of parameters' relative impacts and thus the evaluation of optimisation routes in polymer and composite development. KW - Polymer KW - Pyrolysis simulation KW - Residue formation KW - Fire dynamics simulator (FDS) KW - ThermKin PY - 2012 DO - https://doi.org/10.1016/j.combustflame.2012.03.012 SN - 0010-2180 SN - 1556-2921 VL - 159 IS - 9 SP - 2974 EP - 2984 PB - Elsevier CY - New York, NY AN - OPUS4-26382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Riedel, Juliane A1 - Proske, Matthias A1 - Drzymala, Sarah A1 - Rasenko, Tatjana A1 - Durmaz, V. A1 - Weber, M. A1 - Koch, Matthias T1 - Photochemical trans-/cis-isomerization and quantitation of zearalenone in edible oils N2 - The emphasis of the present work was to investigate the photochemical conversion of trans- to cis-zearalenone in edible oils under real-life conditions. For quantitation purposes a cis-zearalenone standard was synthesized and characterized for its identity and purity (≥95%) by 1H NMR, X-ray crystallography, HPLC fluorescence and mass spectrometric detection. In a sample survey of 12 edible oils (9 corn oils, 3 hempseed oils) from local supermarkets all corn oils contained trans-zearalenone (median 194 µg/kg), but no cis-zearalenone was detected. For alteration studies trans-zearalenone contaminated corn oils were exposed to sunlight over 4 and 30 weeks, revealing an obvious shift toward cis-zearalenone up to a cis/trans ratio of 9:1 by storage in colorless glass bottles. Irradiation experiments of trans-zearalenone in different organic solvents confirmed the preferred formation of cis-zearalenone possibly caused by entropic effects rather than by enthalpic entities as investigated by quantum chemical and classical force field simulations. KW - Fusarium mycotoxins KW - Food KW - Analysis KW - Occurrence PY - 2012 DO - https://doi.org/10.1021/jf3037775 SN - 0021-8561 SN - 1520-5118 VL - 60 IS - 47 SP - 11733 EP - 11740 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-27375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hennig, C. A1 - Takao, S. A1 - Takao, K. A1 - Weiss, S. A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Scheinost, A.C. T1 - Structure and stability range of a hexanuclear Th(IV)-glycine complex N2 - A hexanuclear Th(IV)–glycine complex was observed by Th L3-edge EXAFS measurements in an aqueous solution. Within the stability range of this complex the positively charged hexanuclear species [Th6(µ3-O)4(µ3-OH)4(H2O)6(Gly)6(HGly)6]6+ was preserved in a crystal with the composition [Th6(µ3-O)4(µ3-OH)4(H2O)6(Gly)6(HGly)6]·(NO3)3(ClO4)3(H2O)3. This complex appears as a result of a competing reaction between hydrolysis and ligation by glycine. At a pH value below the stability range of the hexanuclear complex, crystals with the composition [Th(H2O)3(HGly)3]·(ClO4)4H2O were obtained from the solution. Three water molecules in the thorium coordination sphere indicate that this complex occurs prior to the onset of Th(IV) hydrolysis. PY - 2012 DO - https://doi.org/10.1039/c2dt31367g SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 41 SP - 12818 EP - 12823 PB - RSC CY - Cambridge AN - OPUS4-27265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kovalev, Alexander A1 - Sturm, Heinz T1 - In situ direct observation of adsorption and desorption on a single crystal of 2,4,6-trinitrophenol (TNP) N2 - For the first time, we report the direct observation of the nanoscale adsorption and desorption of 2,4,6-trinitrophenol (TNP) molecules on the crystal surface during atomic force microscopy scanning. Our results reveal the position instability of TNP molecules at the border of molecular layers under normal ambient conditions. The observed phenomena are of great interest for exploring the origin of hot-spot generation on the surface of energetic materials. On the basis of the explored properties of TNP crystal, a plausible mechanism of hot-spot formation upon weak initiation at the nanoscale is proposed. KW - Nanoscale adsorption and desorption KW - 2,4,6-trinitrophenol (TNP) KW - Instability of TNP KW - Mechanism of hot-spot formation PY - 2012 DO - https://doi.org/10.1021/cg300366m SN - 1528-7483 VL - 12 IS - 7 SP - 3557 EP - 3564 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-26734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittler, Katrin A1 - Schreiner, M. A1 - Krumbein, A. A1 - Manzei, S. A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, Ronald T1 - Uptake of the cyanobacterial toxin cylindrospermopsin in brassica vegetables N2 - Toxin-producing cyanobacterial species are increasingly being found in freshwater systems. However, literature on the impact of many cyanobacterial toxins on plants is scarce. Cylindrospermosin (CYN), a secondary metabolite of cyanobacteria such as Cylindrospermopsis and Aphanizomenon species, is a potent hepatotoxin and protein synthesis inhibitor. Worryingly, CYN is increasingly found in surface and drinking water worldwide causing human and animal intoxications. Further, exposure of crop plants to CYN by irrigation with contaminated water has already been shown. Therefore, in this study, horticulturally important and highly consumed Brassica species were investigated to determine the level of CYN in the leaves after exposure of the roots to the toxin. Treatment of Brassica oleracea var. sabellica, Brassica juncea, and Sinapis alba under varying experimental conditions showed significant CYN uptake, with CYN levels ranging from 10% to 21% in the leaves compared to the CYN concentration applied to the roots (18–35 µg/l). In seedlings, CYN concentrations of up to 49 µg/g fresh weight were observed. Thus, crop plants irrigated with CYN-containing water may represent a significant source of this toxin within the food chain. KW - Cylindrospermopsin KW - Plant systemic availability KW - Cyanobacterial toxin KW - Brassicaceae KW - Exposure source PY - 2012 DO - https://doi.org/10.1016/j.foodchem.2012.01.107 SN - 0308-8146 VL - 133 IS - 3 SP - 875 EP - 879 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-25730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klimakow, Maria A1 - Klobes, Peter A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Characterization of mechanochemically synthesized MOFs N2 - The compound MOF-14 (Cu3(BTB)2, BTB = 4,4',4''-benzenetribenzoate) was synthesized by ball milling and characterized by powder X-ray diffraction (XRD). The raw material was activated using an efficient single washing step to ensure a free pore access. Nitrogen adsorption measurements were carried out to determine the specific areas of the samples before and after activation. To interpret the activation process in terms of blocking effects in the micropore channels, NLDFT evaluations (Nonlocal Density Functional Theory) of the MOF-14 nitrogen isotherms were carried out. In connection with the appearance of additional hysteresis loops in the nitrogen isotherms, calculations of the mesopore size distribution were performed using the method of Barret, Joyner, and Halenda (BJH). The results are compared to those of a structurally analogue MOF, namely HKUST-1 (Cu3(BTC)2, BTC = 1,3,5-benzenetricarboxylate). This comparison showed notable differences regarding the impact of the activation step on the formation of mesopores and their size distribution. KW - Metal-organic frameworks KW - Mechanochemistry KW - Gas adsorption KW - Specific surface area KW - MOF-14 PY - 2012 DO - https://doi.org/10.1016/j.micromeso.2011.11.039 SN - 1387-1811 SN - 1873-3093 VL - 154 SP - 113 EP - 118 PB - Elsevier CY - Amsterdam AN - OPUS4-25597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Correia, A.M. A1 - Rodrigues, J.P.C. A1 - Korzen, Manfred T1 - Experimental research on the load-bearing capacity of partially encased steel columns under fire conditons N2 - The composite steel and concrete columns are known to have enhanced fire behaviour when compared with bare steel columns. However there are still aspects that must be clarified, as the influence of the building surrounding structure on the fire resistance of the columns. In this paper, the results of fire resistance tests on partially encased steel columns carried out with two different experimental systems are compared. In one of the experimental systems, the building surrounding structure is materialised by a steel restraining frame, and in the other is performed by the so-called substructuring method. Due to the concept of hybrid substructuring, the entire building is decomposed in two parts: one is represented by the building element under test, whereas the remaining building is simulated numerically in a computer. The main conclusion drawn from this work was that the surrounding structure has a major influence in the development of axial forces in the test columns. Moreover, it was observed that the higher the non-dimensional axial restraint ratio the lower the critical time of the columns. KW - Fire resistance KW - Thermal restraint KW - Composite steel-concrete columns KW - Substructuring method KW - Restraining frame PY - 2012 DO - https://doi.org/10.1260/2040-2317.3.1.81 SN - 2040-2317 VL - 3 IS - 1 SP - 81 EP - 94 PB - Multi-Science Publ. Co. CY - Brentwood AN - OPUS4-25632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kolkoori, Sanjeevareddy A1 - Rahman, Mehbub-Ur A1 - Chinta, P.K. A1 - Kreutzbruck, Marc A1 - Prager, Jens ED - Thompson, D. O. ED - Chimenti, D. E. T1 - Quantitative evaluation of ultrasonic sound fields in anisotropic austenitic welds using 2D ray tracing model N2 - Ultrasonic investigation of inhomogeneous anisotropic materials such as austenitic welds is complicated because its columnar grain structure leads to curved energy paths, beam splitting and asymmetrical beam profiles. A ray tracing model has potential advantage in analyzing the ultrasonic sound field propagation and there with optimizing the inspection parameters. In this contribution we present a 2D ray tracing model to predict energy ray paths, ray amplitudes and travel times for the three wave modes quasi longitudinal, quasi shear vertical, and shear horizontal waves in austenitic weld materials. Inhomogenity in the austenitic weld material is represented by discretizing the inhomogeneous region into several homogeneous layers. At each interface between the layers the reflection and transmission problem is computed and yields energy direction, amplitude and energy coefficients. The ray amplitudes are computed accurately by taking into account directivity, divergence and density of rays, phase relations as well as transmission coefficients. Ultrasonic sound fields obtained from the ray tracing model are compared quantitatively with the 2D Elastodynamic Finite Integration Technique (EFIT). The excellent agreement between both models confirms the validity of the presented ray tracing results. Experiments are conducted on austenitic weld samples with longitudinal beam transducer as transmitting probe and amplitudes at the rear surface are scanned by means of electrodynamical probes. Finally, the ray tracing model results are also validated through the experiments. T2 - 38th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Burlington, VT, USA DA - 17.07.2011 KW - Ultrasonic sound field KW - Ray tracing KW - Ray directivity KW - Austenitic weld PY - 2012 SN - 978-0-7354-1013-8 DO - https://doi.org/10.1063/1.4716359 SN - 0743-0760 SN - 0094-243X N1 - Serientitel: AIP conference proceedings – Series title: AIP conference proceedings IS - 1430 SP - 1227 EP - 1234 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-26205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane ED - Cardone, G. T1 - Determination of the spatial energy distribution generated by means of a flash lamp N2 - In order to carry out a quantitative analysis of thermographic data the heating energy and its spatial distribution have to be known. Especially in the case of flash lamp excitation the correct determination of these parameters is complicated due to very short excitation times combined with high power densities. The paper describes a procedure for the characterization of such lamps using a simple calorimetric sensor and a plane reference area. The presented results illustrate the performance and the suitability of the method in the field of thermography. T2 - QIRT 11 - 11th International conference on Quantitative InfraRed Thermography CY - Naples, Italy DA - 11.06.2012 KW - Thermography KW - Flash lamp KW - Heat pulse KW - Calorimetric sensor KW - Energy meter KW - Energy distribution PY - 2012 SP - 1 EP - 10(?) AN - OPUS4-26378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, Daniel A1 - Müller, Christina A1 - Pitkänen, J. A1 - Ewert, Uwe T1 - Bayesian approach for the evaluation of the reliability of non-destructive testing methods: combination of data from artificial and real defects N2 - The Probability of Detection (POD) is used to evaluate the detectability of non-destructive testing (NDT) systems. The POD is highly dependent on the amount of available data. The Bayesian approach provides a solution to compute POD-curves in case of a small amount of real defects without losing the necessary information. The result contains the needed information for the computation of POD-curves for real defects with an acceptable amount of information, even for sparse amount of data. In this paper is shown limitations of the Bayesian approach and how it can be applied to NDT. The Bayesian approach is applied in this case to the evaluation of radiographic testing. Bayesian approach is applied to determine POD-curves for the inspection techniques of nuclear fuel disposal canisters. The reason for using Bayesian approach is the high safety demands and also the low amount of real defects due to the high quality of the reliable production techniques. T2 - 18th WCNDT - World conference on nondestructive testing CY - Durban, South Africa DA - 16.04.2012 KW - Reliability KW - Probability of Detection KW - Real defect testing KW - Bayesian statistics KW - Radiographic testing PY - 2012 SN - 978-0-620-52872-6 SP - 1 EP - 6 (Paper 196) AN - OPUS4-27582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wenzel, B. A1 - Li, Y. A1 - Kraus, Werner A1 - Sorger, D. A1 - Sabri, O. A1 - Brust, P. A1 - Steinbach, J. T1 - Pyrrolovesamicols - synthesis, structure and VAChT binding of two 4-fluorobenzoyl regioisomers N2 - This Letter describes the synthesis of two regioisomers of a new class of vesamicol analogs as possible ligands for imaging the vesicular acetylcholine transporter in future PET studies. The two pyrrolovesamicols (±)-6a and (±)-6b were synthesized by nucleophilic ring opening reaction of a tetrahydroindole epoxide precursor with 4-phenylpiperidine. The reaction mechanism of the synthesis was studied by HPLC and the molecular structures were determined by X-ray structure analysis. Unexpected low binding affinities to VAChT (Κi = 312 ± 73 nM for (±)-6a and Κi = 7320 ± 1840 nM for (±)-6b) were determined by competitive binding analysis using a cell line stably transfected with ratVAChT and (–)-[3H]vesamicol. KW - Pyrrolovesamicol KW - Vesamicol KW - VAChT KW - Pyrrole PY - 2012 DO - https://doi.org/10.1016/j.bmcl.2012.01.127 SN - 0960-894X SN - 1464-3405 VL - 22 IS - 6 SP - 2163 EP - 2166 PB - Pergamon, Elsevier Science CY - New York, NY [u.a.] AN - OPUS4-25574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Fedelich, Bernard T1 - Simulation of non-isothermal mechanical tests on a single crystal nickel-basis superalloy N2 - An extension of the constitutive viscoplastic model of Meric and Cailletaud is presented. The new model accounts for coupling of plasticity and viscoplasticity to describe the rate dependence at low and moderate temperatures. The model contains two boundaries: an elastic one and a viscoplastic one. Between the boundaries, the only contribution to yielding is the rate dependent viscoplastic mechanism. Once the viscoplastic boundary is reached, an additional rate independent flow mechanism becomes active. However, the extended model is not able to predict properly both creep and long-term relaxation tests simultaneously. Therefore, a deformation-induced softening is assumed, which is supposed to mainly affect static recovery. The model has been calibrated with the mechanical tests on a single crystal nickel-basis superalloy. The uniaxial tests have been carried out in the temperature interval 600°C – 1100°C in [001], [011] and [111] specimens. The predicted creep, relaxation and non-isothermal cyclic tests exhibit reasonable agreement with the experimental observations. KW - Non-isothermal mechanical tests KW - Superalloys KW - Constitutive modeling PY - 2012 SN - 0232-3869 VL - 32 IS - 2-5 SP - 321 EP - 332 PB - Institut für Mechanik CY - Magdeburg AN - OPUS4-25925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kind, Thomas A1 - Wöstmann, Jens T1 - Kombinierte Radar- und Ultraschalluntersuchungen zum schadfreien Kernbohren im Zuge einer Verstärkung N2 - Im Rahmen von Ertüchtigungsmaßnahmen an Spannbetonbrücken werden häufig Kernbohrungen durchgeführt, die die vorhandenen Spannbewehrungen nicht beschädigen dürfen. Die Zerstörungsfreie Prüfung (ZfP) kann einen wesentlichen Beitrag leisten, das Risiko einer Beschädigung zu minimieren und somit eine bessere Planungssicherheit für die Ertüchtigungsmaßnahmen zu schaffen. Typische ZfP-Verfahren für das Auffinden von vorgespannter Bewehrung sind das Radar- und das Ultraschallverfahren. Am Beispiel der Ertüchtigung einer Brücke in Bremen wird die Vorgehensweise beschrieben, und es werden die Grenzen der Verfahren aufgezeigt. KW - Zerstörungsfreie Prüfung KW - Radar KW - Ultraschall KW - Spanngliedortung KW - Ertüchtigung KW - Bauwerkserhaltung/Sanierung KW - Bewehrung KW - Brückenbau PY - 2012 DO - https://doi.org/10.1002/best.201200003 SN - 0005-9900 SN - 1437-1006 VL - 107 IS - 4 SP - 255 EP - 261 PB - Ernst CY - Berlin AN - OPUS4-25755 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kolkoori, Sanjeevareddy A1 - Rahman, Mehbub-Ur A1 - Chinta, P.K. A1 - Boehm, Rainer A1 - Prager, Jens ED - Linde, B. B. J. ED - Paczkowski, J. ED - Ponikwicki, N. T1 - Simulation of ultrasonic fields in anisotropic materials using 2D ray tracing method N2 - Ultrasound propagation in inhomogeneous anisotropic materials is difficult to examine because of the directional dependency of elastic properties. Simulation tools play an important role in developing advanced reliable ultrasonic testing techniques for the inspection of anisotropic materials particularly austenitic cladded materials and dissimilar welds. A 2-D Ray tracing method is developed for evaluating ray path, amplitude and travel time for three wave modes namely quasi longitudinal wave (qP), quasi shear vertical wave (qSV) and shear horizontal waves (SH) in anisotropic materials such as austenitic cladded materials. The inhomogenity in the anisotropic material is represented by discretizing the anisotropic region into several homogeneous layers. The ray paths are traced during its propagation through the various interfaces between those layers. At each interface the problem of reflection and refraction is solved. The ray amplitudes are computed by taking into account the directivity and phase relations. Ray divergence variation and ray transmission coefficients at each refraction boundary are considered. The Ray tracing results for ultrasonic field profiles in austenitic cladded materials are validated quantitatively by 2-D Elastodynamic Finite Integration Technique (EFIT) results and by the experiments. T2 - International congress on ultrasonics CY - Gdansk, Poland DA - 05.09.2011 KW - Ray path KW - Energy vector KW - Austenitic cladded material KW - Ultrasonic beam profile PY - 2012 SN - 978-0-7354-1019-0 DO - https://doi.org/10.1063/1.3703288 SN - 0094-243X N1 - Serientitel: AIP conference proceedings – Series title: AIP conference proceedings IS - 1433 SP - 743 EP - 746 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-26207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giesen, C. A1 - Müller, Larissa A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - History of inductively coupled plasma mass spectrometry-based immunoassays N2 - The analysis of biomolecules requires highly sensitive and selective detection methods capable of tolerating a complex, biological matrix. First applications of biomolecule detection by ICP-MS relied on the use of heteroelements as a label for quantification. However, the combination of immunoassays and ICP-MS facilitates multiparametric analyses through elemental tagging, and provides a powerful alternative to common bioanalytical methods. This approach extends the detection of biomarkers in clinical diagnosis, and has the potential to provide a deeper understanding of the investigated biological system. The results might lead to the detection of diseases at an early stage, or guide treatment plans. Immunoassays are well accepted and established for diagnostic purposes, albeit ICP-MS is scarcely applied for the detection of immune-based assays. However, the screening of biomarkers demands high throughput and multiplex/multiparametric techniques, considering the variety of analytes to be queried. Finally, quantitative information on the expression level of biomarkers is highly desirable to identify abnormalities in a given organism. Thus, it is the aim of this review to introduce the fundamentals, and to discuss the enormous strength of ICP-MS for the detection of different immunoassays on the basis of selected applications, with a special focus on LA-ICP-MS. KW - ICP-MS KW - LA-ICP-MS KW - Immunoassay KW - Elemental tagging KW - Multiplexing PY - 2012 DO - https://doi.org/10.1016/j.sab.2012.06.009 SN - 0584-8547 SN - 0038-6987 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. VL - 76 SP - 27 EP - 39 PB - Elsevier CY - Amsterdam AN - OPUS4-27686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, M.E.H. A1 - Steier, I. A1 - Köppen, Robert A1 - Proske, Matthias A1 - Korn, U. A1 - Koch, Matthias A1 - Siegel, David T1 - Cocultivation of phytopathogenic Fusarium and Alternaria strains affects fungal growth and mycotoxin production N2 - Aims: A laboratory study was conducted to evaluate the influence of cocultivation of toxigenic Fusarium (F.) and Alternaria (A.) fungi with respect to growth and mycotoxin production. Methods and Results: Fusarium culmorum Fc13, Fusarium graminearum Fg23 and two Alternaria tenuissima isolates (At18 and At220) were simultaneously or consecutively co-incubated on wheat kernels in an in vitro test system. Fungal biomass was quantified by determining ergosterol content. Three Fusarium toxins (DON, NIV and ZON) and three Alternaria toxins (AOH, AME and ALT) were analysed by a newly developed HPLC/MS/MS method. In simultaneous cocultures, the fungal biomass was enhanced up to 460% compared with individual cultures; Alternaria toxins were considerably depressed down to <5%. Combining At18 and At220 with Fg23 inhibited the toxin production of both fungal partners. In contrast, Fc13 increased its DON and ZON production in competitive interaction with both A. strains. Conclusions: The interfungal competitive effects aid the understanding of the processes of competition of both fungi in natural environments and the involvement of mycotoxins as antifungal factors. Significance and Impact of Study: Cocultivation significantly affects fungal growth and mycotoxin production of phytopathogenic Alternaria and Fusarium strains. The impact of mycotoxins on the interfungal competition is highlighted. KW - Alternaria KW - Cocultivation KW - Ergosterol KW - Fusarium KW - Interfungal competition KW - Multimycotoxin analysis PY - 2012 DO - https://doi.org/10.1111/j.1365-2672.2012.05388.x SN - 1364-5072 VL - 113 IS - 4 SP - 874 EP - 887 PB - Wiley-Blackwell CY - Malden, Mass., USA AN - OPUS4-26932 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Varga, E. A1 - Glauner, T. A1 - Köppen, Robert A1 - Mayer, K. A1 - Sulyok, M. A1 - Schuhmacher, R. A1 - Krska, R. A1 - Berthiller, F. T1 - Stable isotope dilution assay for the accurate determination of mycotoxins in maize by UHPLC-MS/MS N2 - A fast, easy-to-handle and cost-effective analytical method for 11 mycotoxins currently regulated in maize and other cereal-based food products in Europe was developed and validated for maize. The method is based on two extraction steps using different acidified acetonitrile–water mixtures. Separation is achieved using ultrahigh-performance liquid chromatography (UHPLC) by a linear water–methanol gradient. After electrospray ionisation, tandem mass spectrometric detection is performed in dynamic multiple reaction monitoring mode. Since accurate mass spectrometric quantification is hampered by matrix effects, uniformly [13C]-labelled mycotoxins for each of the 11 compounds were added to the sample extracts prior to UHPLC-MS/MS analysis. Method performance parameters were obtained by spiking blank maize samples with mycotoxins before as well as after extraction on six levels in triplicates. The twofold extraction led to total recoveries of the extraction steps between 97% and 111% for all target analytes, including fumonisins. The [13C]-labelled internal standards efficiently compensated all matrix effects in electrospray ionisation, leading to apparent recoveries between 88% and 105% with reasonable additional costs. The relative standard deviations of the whole method were between 4% and 11% for all analytes. The trueness of the method was verified by the measurement of several maize test materials with well-characterized concentrations. In conclusion, the developed method is capable of determining all regulated mycotoxins in maize and presuming similar matrix effects and extraction recovery also in other cerealbased foods. KW - Mycotoxins KW - Stable isotope dilution assay KW - Multi-target analysis KW - Ultrahigh-performance liquid chromatography KW - Tandem mass spectrometry KW - Maize PY - 2012 DO - https://doi.org/10.1007/s00216-012-5757-5 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 9 SP - 2675 EP - 2686 PB - Springer CY - Berlin AN - OPUS4-25640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kasper, J. A1 - Hermanns, M.I. A1 - Bantz, C. A1 - Koshkina, Olga A1 - Lang, Thomas A1 - Maskos, Michael A1 - Pohl, C. A1 - Unger, R. E. A1 - Kirkpatrick, C.J. T1 - Interactions of silica nanoparticles with lung epithelial cells and the association to flotillins N2 - Amorphous silica nanoparticles (aSNPs) gain increasing popularity for industrial and therapeutic claims. The lung with its surface area of 1006#8211;140 m² displays an ideal target for therapeutic approaches, but it represents also a serious area of attack for harmful nanomaterials. The exact nature of the cytotoxic effects of NPs is still unknown. Furthermore, cellular pathways and the destiny of internalized NPs are still poorly understood. Therefore, we examined the cytotoxicity (MTS, LDH) and inflammatory responses (IL-8) for different-sized aSNPs (30, 70, 300 nm) on our lung epithelial cells line NCI H441 and endothelial cell line ISO-HAS-1. Additionally, colocalization studies have been conducted via immunofluorescence staining for flotillin-1- and flotillin-2-bearing endocytic vesicles. Subsequently, the relevance of flotillins concerning the viability of aSNP-exposed epithelial cells has been evaluated using flotillin-1/2 depleted cells (siRNA). This study reveals the relevance of the nanoparticle size regarding cytotoxicity (MTS, LDH) and inflammatory responses (IL-8), whereat the smaller the size of the nanoparticle is, the more harmful are the effects. All different aSNP sizes have been incorporated in flotillin-1- and flotillin-2-labelled vesicles in lung epithelial and endothelial cells, which display a marker for late endosomal or lysosomal structures and appear to exhibit a clathrin- or caveolae-independent mode of endocytosis. Flotillin-depleted H441 showed a clearly decreased uptake of aSNPs. Additionally, the viability of aSNP-exposed cells was reduced in these cells. These findings indicate a contribution of flotillins in as yet unknown (clathrin or caveolae-independent) endocytosis mechanisms and (or) endosomal storage. KW - Silica nanoparticles KW - Alveolar-capillary barrier KW - Lung epithelial cells KW - Endothelial cells KW - Endocytosis KW - Flotillin-1 KW - Flotillin-2 KW - Cytotoxicity KW - Inflammatory response PY - 2012 DO - https://doi.org/10.1007/s00204-012-0876-5 SN - 0340-5761 SN - 1432-0738 SP - 1 EP - 13 PB - Springer CY - Berlin ; Heidelberg [u.a.] AN - OPUS4-26195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Prager, Jens T1 - Device concept for the generation of guided waves for early damage detection N2 - In this study a method for early damage detection is investigated based on the directed excitation and measuring of Lamb waves (guided waves). The objective is to make a statement about the practicability of a Lamb wave generator (LWG) and about the application relevant parameters (specimen materials and dimensions, wave characteristics, excitation, transmission und reflection). Guided waves enable an effective differentiation of structural and defective indications as well as a classification of different defect types. For the investigations, a LWG was developed which combines the advantages of the single excitation of a piezoelectric actuator and the possibility of a group excitation. Algorithms were developed to identify and analyze damage patterns (cracks, wholes, weakening). T2 - Eurosensors XXVI CY - Kraków, Poland DA - 09.09.2012 KW - Lamb wave KW - Guided wave KW - DDS KW - SHM KW - Early damage detection PY - 2012 DO - https://doi.org/10.1016/j.proeng.2012.09.363 SN - 1877-7058 VL - 47 SP - 1185 EP - 1188 PB - Elsevier AN - OPUS4-27552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liehr, Sascha A1 - Krebber, Katerina T1 - Application of quasi-distributed and dynamic length and power change measurement using optical frequency domain reflectometry N2 - Application results of a dynamic technique for simultaneous measurement of length changes and optical power changes between multiple reflection points in an optical fiber are presented. The technique is based on incoherent optical frequency domain reflectometry (I-OFDR) and allows for measuring for example length changes and optical power changes quasi-distributed at repetition rates up to 2 kHz. Precise measurement with length change resolutions in the µm-range can be conducted using standard single-mode or multi-mode fibers. Previous results of dynamic refractive index change measurement and the use of polymer optical fibers for high-strain measurement are concluded and possible sources of measurement inaccuracies are discussed. Field test results with sensors installed on a masonry building during a seismic shake test are presented. The versatility and simplicity of this technique makes it potentially interesting for application in the structural health monitoring sector and chemical process control. KW - Distributed strain sensor KW - Dynamic measurement KW - Optical fiber sensor KW - Refractive index sensors KW - Structural health monitoring PY - 2012 DO - https://doi.org/10.1109/JSEN.2011.2157126 SN - 1530-437X SN - 1558-1748 VL - 12 IS - 1 SP - 237 EP - 245 CY - New York, NY, USA AN - OPUS4-25565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krebber, Katerina A1 - Liehr, Sascha A1 - Witt, Jens ED - Liao, Y. ED - Jin, W. ED - Sampson, D.D. ED - Yamauchi, R. ED - Chung, Y. ED - Nakamura, K. ED - Rao, Y. T1 - Smart technical textiles based on fiber optic sensors N2 - Smart technical textiles containing fiber optic sensors have been developed and successfully demonstrated for the purposes of the structural health monitoring in geotechnical and civil engineering as well as for healthcare monitoring in the medical sector. The paper highlights the results achieved in this innovative field in the framework of several German and European projects and shows selected examples of using such fiber-sensor-based technical textiles in different geotechnical and medical applications. T2 - OFS2012 - 22nd International conference on optical fiber sensors CY - Beijing, China DA - 15.10.2012 KW - Fiber optic sensor KW - Distributed fiber optic sensor KW - Polymer optical fibers (POF) KW - POF sensor KW - POF OTDR KW - Technical textiles KW - Geotextiles KW - Medical textiles PY - 2012 DO - https://doi.org/10.1117/12.981342 SN - 0277-786X SN - 1996-756X N1 - Serientitel: Proceedings of SPIE – Series title: Proceedings of SPIE IS - 8421 SP - 84212A-1 EP - 84212A-10 PB - SPIE, the International Society for Optical Engineering CY - Bellingham, Wash. AN - OPUS4-26915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kromm, Arne ED - Lexow, J. ED - Kishi, T. ED - Kitagawa, M. ED - Böllinghaus, Thomas T1 - Controlling welding residual stresses by means of alloy design N2 - Residual stresses are a major consequence of many manufacturing processes. In particular, welding residual stresses can affect the processing properties and durability of a component. Especially when welding high strength steels in complex structures, showing high restraint intensities, tensile residual stresses can easily reach the level of the yield strength and cause cracking. Therefore, in this study approaches have been evaluated to control the level and distribution of residual stresses already during the welding process using suitable alloy concepts with reduced phase transformation temperatures. This issue affects primarily the mechanisms between transformation temperature, transformation kinetics and resulting residual stresses. The present work includes discussion and approaches, how these phenomena can be evaluated using an appropriate in-situ monitoring. For that purpose, investigations using high energy synchrotron diffraction have been carried out. Initially, diffraction analyses have been made during simple thermal cycles, focusing on the observation of phase transformation kinetics, i.e. transformation temperatures and temperature dependent phase formation and contents. Furthermore, welding experiments incorporating an external shrinkage restraint show how the stress formation during cooling is influenced by superimposed mechanical and thermal impacts compared to conventional filler material. The results demonstrate that residual stresses can be effectively controlled by means of an adjusted alloy design. Prior to experimental results a review is presented including the mechanisms of stress reduction due to phase transformation during welding. Beside this the progress in designing special alloys for controlling residual stresses is reflected. KW - Residual stress KW - Martensite KW - Phase transformation KW - Welding PY - 2012 SN - 978-3-642-23347-0 SN - 978-3-642-23348-7 DO - https://doi.org/10.1007/978-3-642-23348-7 SP - 23 EP - 33 PB - Springer CY - Berlin Heidelberg AN - OPUS4-25520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaltzakorta, O. A1 - Wäsche, Rolf A1 - Hartelt, Manfred A1 - Aginagalde, A. A1 - Tato, W. T1 - Influence of polymer filler on tribological properties of thermoplastic polyurethane under oscillating sliding conditions against cast iron N2 - The tribological behaviour of unfilled thermoplastic polyurethane (TPU) and a polymer sphere filled (TPUG) thermoplastic polyurethane have been studied under oscillating sliding condition against cast iron as a counterpart. In the case of unfilled TPU, the wear mechanisms are dominated by particle detachment and roll formation. In principle, TPUG also showed a similar wear mechanism as that of unfilled TPU; in addition, particle pull-out and delamination are also observed. Wear volume of TPUG was significantly higher than that for the unfilled TPU and this is attributed to the different material removal processes taking place in the material during sliding. The polymer spheres as a filler material deteriorated the wear resistance of TPU because of improper adhesion and bonding of filler in the TPU matrix and therefore it contributed to more wear. In case of TPU the friction behaviour was strongly dependant on the temperature and surface roughness of the counter body. The results showed that below the glass transition temperature higher friction values are observed with higher counter body surface roughness. However, above the glass transition temperature, higher friction values are observed with a smoother surface roughness of the counter body. In case of TPUG, the friction behaviour was not significantly dependent on surface roughness of the counter body. KW - Dry sliding KW - Polymers KW - Cast iron KW - Temperature PY - 2012 DO - https://doi.org/10.1007/s11249-012-0017-6 SN - 1023-8883 SN - 1573-2711 VL - 48 IS - 2 SP - 209 EP - 216 PB - Springer Science Business Media B.V. CY - Dordrecht AN - OPUS4-27272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bismarck, A. A1 - Carreyette, S. A1 - Fontana, Q.P.V. A1 - Greenhalgh, E.S. A1 - Jacobsson, P. A1 - Johansson, P. A1 - Marczewski, M.J. A1 - Kalinka, Gerhard A1 - Kucernak, A. A1 - Shaffer, M.S. A1 - Shirshova, N. A1 - Steinke, J.H.G. A1 - Wienrich, Malte T1 - Multifunctional epoxy resin for structural supercapacitors N2 - Polymer-based electrolytes based on commercially available epoxy resins were prepared through the addition of a liquid electrolyte, a solution of a lithium salt in an ionic liquid. The polymer monoliths were characterized using impedance spectroscopy, 3-point bending test, scanning electron microscopy (SEM) and nitrogen adsorption (BET). The balance of ionic conductivity and flexural modulus is crucially dependent on the relative proportions of epoxy resin to electrolyte. Also the effect of the liquid electrolyte on curing kinetics and processing was assessed by complex viscosity measurements and differential scanning calorimetry (DSC). Only one out of the three resins investigated exhibited a significant acceleration effect. T2 - ECCM15 - 15th European conference on composite materials CY - Venice, Italy DA - 24.06.2012 KW - Multifunctional epoxy KW - Polymer electrolyte KW - Morphology KW - Ionic liquid PY - 2012 SN - 978-88-88785-33-2 SP - 1 EP - 8 AN - OPUS4-28694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hjelmar, O. A1 - Wahlström, M. A1 - Comans, R. A1 - Kalbe, Ute A1 - Grathwohl, P. A1 - Mehu, J. A1 - Schiopu, N. A1 - Hyks, J. A1 - Laine-Ylijoki, J. A1 - Van Zomeren, A. A1 - Krüger, Oliver A1 - Schoknecht, Ute A1 - Wendel, T. A1 - Abdelghafour, M. A1 - Borho, N. ED - Arm, M. ED - Vandecasteele, C. ED - Heynen, J. ED - Suer, P. ED - Lind, B. T1 - Robustness validation of two harmonized European leaching tests for assessment ot the leaching of construction products, including waste-based construction materials N2 - Two leaching tests, a tank leaching test (TS-2) and a percolation test (TS-3), developed by CEN/TC 351 for use in assessing environmental properties in relation to CE marking of construction products, are undergoing robustness validation as part of the standardisation procedure. This paper provides an overview of the activities included in the robustness validation programme. T2 - WASCON 2012 CY - Gothenburg, Sweden DA - 30.05.2012 KW - Tank leaching test KW - Percolation test KW - Robustness validation KW - Construction products PY - 2012 SP - 1 EP - 5 PB - ISCOWA and SGI AN - OPUS4-26966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias A1 - Stark, Wolfgang A1 - Wolff, Dietmar T1 - Comparison of low temperature properties of different elastomer materials investigated by a new method for compression set measurement N2 - The method for the determination of compression set values with a Dynamic Mechanical Analysis (DMA) setup at low temperatures, which was presented previously, allows a much faster and readily automated procedure than the standardized compression set test according to ISO 815-2. This method is applied to a series of different elastomeric materials that are commonly used for sealing applications. The results of the compression set test are compared with results from thermal analysis to allow an in depth comparison of the material behaviour at low temperatures. Furthermore, a comparison between two EPDM materials is presented. These materials show very similar properties determined by thermo analytical methods such as Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) but differ clearly in their compression set behaviour. This comparison shows the importance and value of information of the compression set test in addition to thermal analysis to judge the behaviour of sealing materials and confirms the relevance of the new compression set test method for the investigation of low temperature properties of elastomers. KW - Sealing material KW - Elastomer KW - Compression set KW - Dynamic mechanical analysis KW - Low temperature behaviour PY - 2012 DO - https://doi.org/10.1016/j.polymertesting.2012.07.016 SN - 0142-9418 VL - 31 IS - 8 SP - 987 EP - 992 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-26538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Godehardt, M. A1 - Krebs, Holger A1 - Ohser, J. A1 - Staude, Andreas T1 - Analyse der Porengrößenverteilung in einer myCT-Aufnahme eines Sprengstoffes N2 - An der BAMIine von BESSY II wurden durch Mikro-Computertomographie (pCT) 3D-Bilder der Mikrostruktur von drei verschiedenen Explosivstoffen aufgenommen (Probennummern 2075, 2076, 2077), von denen zunächst nur der 3DDatensatz von Probe 2075, eines mit Mikrohohlkugeln sensibilisierten Emulsionssprengstoffes, analysiert wurde. Für die anderen Proben erschien der Aufwand zur Charakterisierung der Mikrostruktur zu hoch bzw. muss die Zielstellung der Analyse noch klarer formuliert werden. PY - 2012 SN - 0941-4584 VL - 34 IS - 1 SP - 3 EP - 4 PB - Deutscher Sprengverband CY - Siegen AN - OPUS4-27976 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kalbe, Ute A1 - Krüger, Oliver A1 - Wachtendorf, Volker A1 - Berger, Wolfgang T1 - Umweltverträglichkeit von Kunststoff- und Kunststoffrasenbelägen auf Sportfreianlagen N2 - Auf vielen Sportfreianlagen werden aktuell Sportböden aus Kunststoffen verwendet. Kunstrasenkomponenten und Verbundmaterialien wie Sportbeläge aus Kunststoff können gezielt für die Anforderungen der jeweiligen Sportart optimiert werden und werden daher immer beliebter. Auf modernen Hockeyanlagen kommen beispielsweise ausschließlich Kunststoffrasenbeläge zur Anwendung. Bei Laufbahnen hat der Kunststoff schon seit längerem die Tennenbeläge abgelöst und auch auf Fußballplätzen finden Kunststoffrasenbeläge mehr und mehr Akzeptanz. KW - Sportboden KW - Sportbodenbelag KW - Kunststoffbelag KW - Kunststoffrasenbelag KW - Kunstrasen KW - Schadstoff KW - Umweltverträglichkeit KW - Ökotoxizität PY - 2012 SN - 978-3-86884-522-8 IS - 2 SP - 1 EP - 261 PB - Sportverlag Strauß CY - Bonn AN - OPUS4-26997 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kannengießer, Thomas A1 - Lausch, Thomas T1 - Diffusible hydrogen content depending on welding and cooling parameters N2 - Safety of welded components made from high-strength materials is assured above all by the avoidance of hydrogen-assisted cold cracking which occurs during fabrication and may have effects during service. In this context, continuous advancement of the procedures and standards for hydrogen analysis is required. Exact determination of the weld metal diffusible hydrogen according to ISO DIS 3690 is therefore highly relevant as regards the welding and cooling parameters to be maintained. In the investigations presented in this paper, the influence of the welding process parameters and of the cooling parameters on the diffusible hydrogen content was examined and the procedures and parameters specified in ISO DIS 3690 for the weld specimen preparation were checked. The influence of cooling conditions, arc length and contact tube distance (CTD) on the weld metal hydrogen concentration was studied for a high-strength flux cored wire electrode and a high-strength solid wire electrode. Measurement of the diffusible hydrogen was carried out by means of carrier gas hot extraction using a sensitive and long-term stable thermal conductivity detector (TCD). KW - MAG welding KW - Hydrogen KW - Measurement KW - Cold cracking KW - Hydrogen embrittlement KW - Cooling rate PY - 2012 SN - 0043-2288 SN - 1878-6669 VL - 56 IS - 11/12 SP - 26 EP - 33 PB - Springer CY - Oxford AN - OPUS4-27677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Seefeldt, Henrik A1 - Karrasch, Andrea A1 - Jäger, Christian T1 - What reacts with what in bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate) during pyrolysis and fire behavior? N2 - The pyrolysis and flame retardancy of a bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate) (PC/SiR/BDP) blend were investigated and compared to those of PC/BDP and PC/SiR. The impact modifier SiR consists mainly of poly(dimethylsiloxane) (PDMS > 80 wt %). The pyrolysis of PC/SiR/BDP was studied by thermogravimetry (TG), TG–FTIR to analyze the evolved gases, and a Linkam hot stage cell within FTIR as well as 29Si NMR and 31P NMR to analyze the solid residue. The fire performance was determined by PCFC, LOI, UL 94, and a cone calorimeter under different external irradiations. The fire residues were studied by using ATR-FTIR as well as the additional binary systems PC + PDMS, PC + BDP, and BDP + PDMS, focusing on the specific chemical interactions. The decomposition pathways are revealed, focusing on the competing interaction between the components. Fire retardancy in PC/SiR/BDP is caused by both flame inhibition in the gas phase and inorganic-carbonaceous residue formation in the condensed phase. The PC/SiR/BDP does not work as well superimposing the PC/SiR and PC/BDP performances. PDMS reacts with PC and BDP, decreasing BDP's mode of action. Nevertheless, the flammability (LOI > 37%, UL 94 V-0) of PC/SiR/BDP equals the high level of PC/BDP. Indeed, SiR in PC/SiR/BDP is underlined as a promising impact modifier in flame-retarded PC/impact modifier blends as an alternative to highly flammable impact modifiers such as acrylonitrile–butadiene–styrene (ABS), taking into account that the chosen SiR leads to PC blends with a similar mechanical performance. KW - PC KW - BDP KW - PDMS KW - Flame retardancy KW - Flammability KW - Decomposition KW - Pyrolysis PY - 2012 DO - https://doi.org/10.1021/ie201908s SN - 0888-5885 SN - 1520-5045 VL - 51 IS - 3 SP - 1244 EP - 1255 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Ciesielski, M. A1 - Kretzschmar, B. A1 - Braun, Ulrike A1 - Döring, M. T1 - Are novel aryl phosphates competitors for bisphenol A bis(diphenyl phosphate) in halogen-free flame-retarded polycarbonate/acrylonitrile-butadiene-styrene blends? N2 - The reactivity of the flame retardant and its decomposition temperature control the condensed-phase action in bisphenol A polycarbonate/acrylonitrile–butadiene–styrene/polytetrafluoroethylene (PC/ABSPTFE) blends. Thus, to increase charring in the condensed phase of PC/ABSPTFE + aryl phosphate, two halogen-free flame retardants were synthesized: 3,3,5-trimethylcyclohexylbisphenol bis(diphenyl phosphate) (TMC-BDP) and bisphenol A bis(diethyl phosphate) (BEP). Their performance is compared to bisphenol A bis(diphenyl phosphate) (BDP) in PC/ABSPTFE blend. The comprehensive study was carried out using thermogravimetry (TG); TG coupled with Fourier transform infrared spectrometer (TG-FTIR); the Underwriters Laboratory burning chamber (UL 94); limiting oxygen index (LOI); cone calorimeter at different irradiations; tensile, bending and heat distortion temperature tests; as well as rheological studies and differential scanning calorimeter (DSC). With respect to pyrolysis, TMC-BDP works as well as BDP in the PC/ABSPTFE blend by enhancing the cross-linking of PC, whereas BEP shows worse performance because it prefers cross-linking with itself rather than with PC. As to its fire behavior, PC/ABSPTFE + TMC-BDP presents results very similar to PC/ABSPTFE + BDP; the blend PC/ABSPTFE + BEP shows lower flame inhibition and higher total heat evolved (THE). The UL 94 for the materials with TMC-BDP and BDP improved from HB to V0 for specimens of 3.2 mm thickness compared to PC/ABSPTFE and PC/ABSPTFE + BEP; the LOI increased from around 24% up to around 28%, respectively. BEP works as the strongest plasticizer in PC/ABSPTFE, whereas the blends with TMC-BDP and BDP present the same rheological properties. PC/ABSPTFE + TMC-BDP exhibits the best mechanical properties among all flame-retarded blends. KW - Polycarbonate (PC) KW - Aryl phosphate KW - Flame retardancy KW - Pyrolysis KW - PC/ABS PY - 2012 DO - https://doi.org/10.1016/j.eurpolymj.2012.06.015 SN - 0014-3057 SN - 1873-1945 VL - 48 IS - 9 SP - 1561 EP - 1574 PB - Elsevier CY - Oxford AN - OPUS4-26292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Larissa A1 - Jakubowski, Norbert A1 - Hösl, Simone A1 - Scheler, C. A1 - Roos, P. H. A1 - Linscheid, M. W. T1 - Comparison of different chelates for lanthanide labeling of antibodies and application in a Western blot immunoassay combined with detection by laser ablation (LA-)ICP-MS N2 - We have developed lanthanide labeling strategies for antibodies to adapt conventional biochemical workflows like Western blot immunoassays for detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis with a special interest to apply the multi-element capabilities of ICP-MS for the design of multiplexed immunoassays. In this paper the lanthanide labeling of antibodies with MeCAT was investigated and the reaction conditions were optimized for application in a Western blot immunoassay analyzed by LA-ICP-MS. Furthermore, the MeCAT labeling strategy was compared with two other commercially available labeling reagents, MAXPAR™ and SCN-DOTA. As a proof-of-principle experiment chemically induced alterations of cytochrome P450 protein expression were investigated and the suitability of the differentially labeled antibodies for Western blot immunoassays of a complex liver microsomal protein fraction was tested. Limits of detection (LODs) in the lower fmol range were reached in the Western blot application using MeCAT and MAXPAR™ as element labeling reagents, whereas even sub-fmol LODs can be achieved in a dot blot experiment for the pure antibodies. PY - 2012 DO - https://doi.org/10.1039/c2ja30068k SN - 0267-9477 SN - 1364-5544 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. N1 - Geburtsname von Hösl, Simone: Hardt, S. - Birth name of Hösl, Simone: Hardt, S. VL - 27 IS - 8 SP - 1311 EP - 1320 PB - Royal Society of Chemistry CY - London AN - OPUS4-26256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trubiroha, P. A1 - Geburtig, Anja A1 - Wachtendorf, Volker T1 - 40 Years of Global-UV-Test weathering device: with fluorescent UV lamps and a precise microclimatical control into the future N2 - On the basis of a lot of investigation on the spectral sensitivity of photo degradation of plastics and on the underestimated influence of temperature and relative humidity on degradation processes a new type of weathering device was presented at the end of the seventies: It was a combination of a radiation source with fluorescent UV lamps and a precise climatic cabinet. The radiation emission from a combination of four different types of fluorescent UV lamps was superimposed on the specimen surfaces in the climatic cabinet to match the UV part of solar radiation as closely as possible. Air temperature was controlled to within ± 1 °C, and relative humidity to within ± 5 %RH. As the lamps’ emission is focussed on the UV range almost no radiation heating of the sample occurs. Therefore, the temperature of the sample, which is the quantity of consideration for the degradation, is nearly identical with the chamber’s air temperature, which is the quantity to be controlled. Also, therefore, high humidity can be obtained on the sample surface. The limitation of the emission to the UV range is sufficient for the study of the polymer matrix. This type of weathering device offers an exactness of microclimatic control of the sample’s surface, which should be a standard for weathering devices. Even now it is the only weathering device which generates pure relative humidity (without aerosol). T2 - 9th European Weathering Symposium CY - Basel, Switzerland DA - 18.09.2019 KW - Weathering KW - Irradiation PY - 2019 SN - 978-3-9818507-5-8 SP - 37 EP - 47 PB - Thomas Würtz Grafik-Design CY - Karlsruhe, Germany AN - OPUS4-49151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, P. T1 - Evaluation of outdoor exposures by means of exposure response functions N2 - Outdoor exposure tests are a common tool to evaluate the weathering resistance of a polymeric material or component. However, they have only a limited validity, mainly due to the limited reproducibility of the weather as well as of the bad adaptability to other exposure sites. Typically, an outdoor exposure is characterized by the measured radiant exposure; sometimes averaged temperature data are added. These can be – separately – related to long-term annual means, to get an idea on the severity of the exposure. However, as for polymeric ageing, irradiance and temperature act simultaneously, such severity of an outdoor exposure could be better described by a computed property change of a similar material, which is calculated from the hourly irradiance and temperature values on the base of established exposure response functions. In this way, various outdoor exposures are evaluated. For several exposure sites, annual deviations of the ageing amount are related to annual mean values, to evaluate the weathering reproducibility at the exposure site. Additionally, correlations to relevant weather parameters are illuminated. Also some specific exposure conditions, such as tilt angle, are tested. Compared to the use of weathering reference materials, this procedure unfavourably depends on the availability of a suited control as well as on the quality of the established exposure response function. In contrast, it enables a later exposure evaluation, on the base of documented weather data, if for instance no reference material was exposed. T2 - 8th European Weathering Symposium CY - Vienna, Austria DA - 20.09.2017 KW - Weathering KW - Service life prediction KW - Photodegradation PY - 2017 SN - 978-3-9818507-1-0 VL - 18 SP - 127 EP - 135 PB - Thomas Würtz Grafik Design CY - Karlsruhe AN - OPUS4-42126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachtendorf, Volker T1 - „Test Tailoring“ eines künstlichen Bewitterungstests am Beispiel der Entwicklung des „Acid Dew and Fog“ Testes N2 - Häufig ist es wünschenswert, für neue Materialien oder Anwendungen künstliche Bewitterungsverfahren zu benutzen, die auf die spezifischen Anforderungen besser zugeschnitten sind, als es bei bestehenden standardisierten Verfahren der Fall ist. Nachdem man die spezifischen Parameter der Beanspruchung unter Anwendungsbedingungen und die spezifische Empfindlichkeit des Materials erfasst hat, beginnt ein Prozess, der als „Test Tailoring“ häufig abstrakt verwendet, auf den aber nur selten näher eingegangen wird. Genau dieser Prozess soll hier am Beispiel der Entwicklung eines künstlichen Bewitterungstests unter saurer Beaufschlagung, dem in der BAM entwickelten Acid Dew and Fog Test, beispielhaft erläutert werden. T2 - 47. Jahrestagung der Gesellschaft für Umweltsimulation (GUS) 2018 CY - Pfinztal (Berghausen), Germany DA - 21.03.2018 KW - Test Tailoring KW - Bewitterung KW - Acid Dew and Fog KW - Umweltsimulation PY - 2018 AN - OPUS4-46542 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Karrasch, Andrea A1 - Jäger, Christian T1 - Flame-retarded bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate): Adding inorganic additives N2 - Various inorganic additives belonging to four different groups: layered materials, metal hydroxides, metal oxides/carbonate and metal borates are investigated in bisphenol A polycarbonate/silicon rubber/bisphenol A bis(diphenyl phosphate) (PC/SiR/BDP) to improve flame retardancy. The pyrolysis, reaction to small flame and fire behaviour of the blends are characterised and structure–property relationships discussed. Among the added layered materials, talc functions as an inert filler with potential for commercialisation, whereas organically modified montmorillonite (LS) enhances decomposition. PC/SiR/BDP + talc and PC/SiR/BDP + LS reinforce the char and induce a flow limit. The different dispersion and location of boehmite (AlO(OH)) nano-particles and Mg(OH)2 micro-particles determine the impact on performance. PC/SiR/BDP + Mg(OH)2 shows additional hydrolysis and thus reduced flame retardancy. AlO(OH) is embedded in SiR and thus behaves as an inert filler. Both additives worked as smoke suppressants. Using selective filling with nano-particles is proposed as an interesting route for flame retardancy in PC/SiR blends. Adding metal oxides and carbonate (MgO, CaCO3 and SiO2) changes the decomposition pathways of PC/SiR/BDP, worsening the fire performance of PC/SiR/BDP. CaCO3 harbours the potential to intumescence, even though an early collapse of the char structure occurred. Adding hydrated metal borates, CaB, MgB and ZnB, changes the pyrolysis and flame retardancy action. Smoke suppression occurs; LOI is improved as well as UL 94 classification. ZnB performs better than MgB and CaB. The comprehensive study, also based on systematic material variation, delivers valuable guidelines for future development of flame-retarded multi-component PC blends. KW - Flame retardancy KW - Polycarbonate blends KW - Aryl phosphate KW - Inorganic fillers PY - 2014 DO - https://doi.org/10.1016/j.polymdegradstab.2013.08.006 SN - 0141-3910 SN - 1873-2321 VL - 106 SP - 74 EP - 87 PB - Applied Science Publ. CY - London AN - OPUS4-30952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karrasch, Andrea A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Jäger, Christian T1 - Solid-state NMR on thermal and fire residues of bisphenol A polycarbonate/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate)/(PC(SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) - Part 1: PC charring and the impact of BDP and ZnB N2 - Structural changes in the condensed phase of bisphenol A polycarbonate (containing 0.45 wt% poly (tetrafluoroethylene))/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate) (PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) during thermal treatment in nitrogen atmosphere and in fire residues were investigated by solid-state NMR. H-1, B-11, C-13 and P-31 NMR experiments using direct excitation with a single pulse and H-1-P-31 cross-polarization (CP) were carried out including 31P(1 H) and C-13{P-31}double-resonance techniques (REDOR: Rotational Echo Double Resonance) on a series of heat-treated samples (580 K-850 K). Because many amorphous phases occur in the solid residues, and solid-state NMR spectroscopy addresses the most important sites carbon, phosphorus and boron, this paper is the key analytical approach for understanding the pyrolysis and flame retarding phenomenon in the condensed phase of PC/SiR/BDP and PC/SiR/BDP/ZnB. For the system PC/SiR/BDP it is shown that (i) at temperatures around 750-770 K (main decomposition step) carbonaceous charring of PC occurs and arylphosphate structures are still present, reacted in part with the decomposing PC; (ii) for higher temperatures from 770 K the phosphorus remaining in the solid phase increasingly converts to amorphous phosphonates and inorganic orthophosphates with a minor amount of crystalline orthophosphates; and (iii) H-1-P-31{H-1} CP REDOR and H-1-C-13{P-31} CP REDOR NMR experiments suggest that the phosphates and phosphonates are bound via oxygen to aromatic carbons, indicating the interaction with the carbonaceous char. When ZnB is added to the system PC/SiR/BDP, (i) ZnB leads to a slightly enhanced PC decomposition for temperatures below 750 K; (ii) alpha-Zn-3(PO4)(2) and borophosphate (BPO4) are formed in small amounts at high temperatures suggesting a reaction between BDP and ZnB during thermal decomposition; and (iii) most of the borate remains in the solid residues, forming an amorphous pure borate network, with the BO3/BO4 ratio increasing with higher temperatures. The NMR data of thermal and fire residues are highly correlated, underlining the importance of this work for understanding the pyrolysis and flame retardancy mechanisms in the condensed phase during the burning of the PC/SiR blends. (C) 2010 Elsevier Ltd. All rights reserved. KW - Flame retardance KW - NMR KW - Polycarbonate (PC) blends KW - Bisphenol-A bis(diphenyl)phosphate (BDP) KW - Zinc borate PY - 2010 DO - https://doi.org/10.1016/j.polymdegradstab.2010.07.034 SN - 0141-3910 SN - 1873-2321 VL - 95 IS - 12 SP - 2525 EP - 2533 PB - Applied Science Publ. CY - London AN - OPUS4-22647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Schmidt, Anita A1 - Goedecke, Thomas T1 - Combined impact of UV radiation and nitric acid on HDPE containers during outdoor exposure T1 - Kombinierte Einwirkung von UV-Strahlung und Salpetersäure auf HDPE-Behälter bei der Freibewitterung N2 - Unpigmented HDPE jerrycans filled with nitric acid (55%) and water respectively had been exposed to outdoor conditions for one Berlin summer season. As both liquids underwent equal temperature progression, exposure effects of UV radiation and nitric acid as well as of their combination can be separated and compared. On the basis of various property changes after these exposures, synergistic action is evaluated and compared to a damaged Intermediate Bulk Container (IBC) from a transport accident. It is found that carbonyl formation goes along with lightness increase in color measurement due to microcracking and with a worsening in mechanical behavior, all of them showing synergistic effects of UV and nitric acid exposure. In contrast, embedding nitrogen compounds goes along with yellowing of the material but cannot be correlated to oxidation. The reason for intensified damaging is the decomposition of the 55-percent nitric acid and formation of nitrogen oxides even at ambient temperatures, caused by UV radiation. Thus, damaging effects become similar to those caused by fuming nitric acid exposure at temperatures above 60 °C, with the result of strong oxidative degradation of the polyethylene. In contrast, exclusive exposure to the 55-percent nitric acid at 40 °C does not cause any failure. It can therefore be assumed that also the damaged IBC had been exposed to both UV radiation and nitric acid, probably outdoors. KW - Polyethylene KW - Nitric acid KW - UV radiation KW - Outdoor weathering KW - Resistance PY - 2018 DO - https://doi.org/10.3139/120.111148 SN - 0025-5300 VL - 60 IS - 3 SP - 257 EP - 264 PB - Carl Hanser Verlag CY - München AN - OPUS4-44567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karrasch, Andrea A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Jäger, Christian T1 - Solid-state NMR on thermal and fire residues of bisphenol A polycarbonate/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate)/(PC(SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) - Part II: The influence of SiR N2 - Solid residues of bisphenol A polycarbonate (containing 0.45 wt% poly(tetrafluoroethylene))/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate) (PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) after thermal treatment were investigated by solid-state and liquid-state NMR, focusing on the role and interaction of SiR with the other components of the polymer blend. In PC/SiR/BDP, part of the SiR reacts to an amorphous silicate network rather than being completely released in the gas phase. The silicate network consists of Q4 and Q3 groups formed via intermediate D and T groups. The D groups are formed by a reaction of SiR with bisphenol-A units as well as phenyl groups of PC and BDP. In addition a small amount of silicon diphosphate was observed after thermal treatment at temperatures higher than 810 K. The same decomposition products (without SiP2O7) occur in the solid residues of PC/SiR/BDP/ZnB samples. The formation of intermediate D and T groups occurs earlier, at slightly lower temperatures. Any formation of a borosilicate network was excluded. The results also apply for the fire residues of PC/SiR/BDP and PC/SiR/BDP/ZnB and are thus valuable for understanding the impact of SiR on pyrolysis and flame retardancy mechanisms in the condensed phase during the burning of PC/SiR/BDP blends. SiR was found to influence the pyrolysis and the char formed. Beyond the replacement of highly combustible mechanical modifiers, SiR harbours the potential to enhance flame retardancy. KW - Flame retardance KW - 29Si NMR KW - Polycarbonate (PC) blends KW - Bisphenol A bis(diphenyl)phosphate (BDP) KW - Silicone rubber PY - 2010 DO - https://doi.org/10.1016/j.polymdegradstab.2010.07.030 SN - 0141-3910 SN - 1873-2321 VL - 95 IS - 12 SP - 2534 EP - 2540 PB - Applied Science Publ. CY - London AN - OPUS4-22648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachtendorf, Volker A1 - Geburtig, Anja T1 - Digitale Umweltsimulation am Beispiel der Photooxidation von Polymeren N2 - Die Umweltwirkungen auf ein Material werden als Überlapp der Funktionskurven von Materialempfindlichkeit und einwirkenden Umweltparametern betrachtet. Wenn entweder die Empfindlichkeit oder die Beanspruchungen Null sind, ergibt sich auch keine Umweltwirkung und bei beidseitig Werten größer Null das jeweilige Produkt der beiden. Die Akkumulation der nicht-reversiblen Effekte über die Zeit und allen Eigenschaftsänderungen entspricht der Alterung des Materials für den jeweiligen Expositionszeitraum. Die digitale Umweltsimulation gliedert sich hier in drei Teilaspekte. Ein erster, rein materialwissenschaftlicher Teil hat die Aufgabe, alle relevanten Materialempfindlichkeiten experimentell zu quantifizieren. Ein zweiter – unter Umständen numerischer Teil – hat die Aufgabe, das Bauteil und seine Einbaulage zu digitalisieren und aus den makroskopischen Umgebungsbedingungen die relevanten mikroklimatischen Umweltparameter für alle Oberflächen- oder Volumenelemente zu bestimmen. In einem dritten Teil werden die Einwirkungen über den betrachteten Zeitraum berechnet und kumuliert. Dieses Konzept, das auf den so genannten Expositions-Reaktions-Funktionen (ERF) basiert, wird an Beispielen der Photoxidation erläutert. Dieses Vorgehen wurde schon beim ViPQuali-Projekt als Numerische Umweltsimulation umgesetzt. Überprüft werden muss das Modell unbedingt an einer realitätsnahen Validierungsbeanspruchung. Hier werden die ermittelten ERFs mit über den kompletten Beanspruchungszeitraum geloggten Umweltparametern gekoppelt, um die berechnete mit der experimentell erfahrenen Alterungswirkung zu vergleichen. Nur so kann sichergestellt sein, dass alle für die Anwendungsumgebung relevanten Materialempfindlichkeiten einbezogen wurden. T2 - 52. Jahrestagung der GUS CY - Stutensee-Blankenloch, Germany DA - 26.03.2024 KW - UV KW - Polymer 3R KW - Bewitterung KW - Bestrahlung PY - 2024 SN - 978-3-9826129-0-4 SP - 31 EP - 40 PB - Gesellschaft für Umweltsimulation e.V. CY - Pfinztal (Berghausen) AN - OPUS4-59830 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Schulz, Ulrich A1 - Trubiroha, Peter T1 - „Test Tailoring“ eines künstlichen Bewitterungstests am Beispiel der Entwicklung des „Acid Dew and Fog“ Testes N2 - Häufig ist es wünschenswert, für neue Materialien oder Anwendungen künstliche Bewitterungsverfahren zu benutzen, die auf die spezifischen Anforderungen besser zugeschnitten sind, als es bei bestehenden standardisierten Verfahren der Fall ist. Nachdem man die spezifischen Parameter der Beanspruchung unter Anwendungsbedingungen und die spezifische Empfindlichkeit des Materials erfasst hat, beginnt ein Prozess, der als „Test Tailoring“ häufig abstrakt verwendet, auf den aber nur selten näher eingegangen wird. Genau dieser Prozess soll hier am Beispiel der Entwicklung eines künstlichen Bewitterungstests unter saurer Beaufschlagung, dem in der BAM entwickelten Acid Dew and Fog Test, beispielhaft erläutert werden. T2 - 47. Jahrestagung der GUS 2018, Umwelteinflüsse erfassen, simulieren, bewerten CY - Pfinztal (Berghausen), Germany DA - 21.03.2018 KW - Test Tailoring KW - Bewitterung KW - Acid Dew and Fog KW - Umweltsimulation PY - 2018 VL - 47 SP - Vortrag V4, 45 EP - 54 PB - Gesellschaft für Umweltsimulation e.V. CY - Pfinztal AN - OPUS4-45412 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, P. T1 - Exposure response function for a quantitative prediction of weathering caused aging of polyethylene N2 - The exposure response function of the carbonyl formation over the bulk has been determined for a high-density polyethylene of a thickness of 200 μm, which was used as a weathering reference material according to ISO TR 19032. To this end, spectral sensitivity was studied by local measurement of the effect of spectrally dispersed irradiation. Both the exposure device and the methodology of determination are described. The temperature dependency of photooxidation was determined by UV exposure at various temperatures between 23 and 80 °C. Deviations from linearity and thus reciprocity below 40 °C are discussed and assumed to be related to diffusion limitations. An Arrhenius approach –based on data of linear carbonyl formation – has been incorporated into the exposure response function. Using this exposure response function, aging in terms of the distribution of a quantitative property change over a plastic component can be predicted for a specific outdoor location with real chronologic weather data as input for the exposure. Thus, artificial and natural weathering can be linked and compared. The established exposure response function has been validated by outdoor exposure results from the literature. If an estimated diffusion limitation is taken into consideration, calculations and published data are in good agreement. KW - Irradiation KW - Weathering KW - Spectral sensitivity KW - Temperature dependency KW - Spectral irradiation PY - 2019 DO - https://doi.org/10.3139/120.111348 SN - 0025-5300 VL - 61 IS - 6 SP - 517 EP - 526 PB - Carl Hanser Verlag GmbH & Co. KG AN - OPUS4-48295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, P. ED - Ziegahn, K.-F. T1 - Quantitative Auswertemöglichkeiten bei der spektralen Bestrahlung – Berechnung des Wirkungsspektrums N2 - Für die Bewertung des Wellenlängeneinflusses auf die Alterungsvorgänge bei der Bestrahlung UV- oder lichtempfindlicher Materialien kann die Methode der spektralen Bestrahlung angewendet werden. Im Prinzip wird dabei das linear dispergierte Spektrum einer Strahlenquelle mit kontinuierlichem Spektrum (z.B. Xe-Lampe) auf eine Probenoberfläche abgebildet, so dass Ort einer Materialänderung und Wellenlänge der Bestrahlung einander zugeordnet werden können. Nachfolgende lokal-auflösende Analysemethoden ermitteln eine Eigenschaftsänderung an einem spezifischen Ort der Probe, aus dem sich dann die Bestrahlungswellenlänge ergibt. Der verwendete Aufbau wird beschrieben. Es wird an einem ausgewählten Beispiel gezeigt, wie durch geeignete Anbindung eines Messsystems zur Bestimmung der spektralen Bestrahlungsstärke und ortsaufgelöste Messungen der Eigenschaftsänderungen eine quantitative Auswertung realisiert werden kann. Der Einfluss nichtlinearer Alterungsverläufe wird diskutiert. Grenzen der Methode werden aufgezeigt und Erweiterungsmöglichkeiten dargestellt. T2 - 46. Jahrestagung der GUS CY - Stutensee-Blankenloch, Germany DA - 22.03.2017 KW - UV-Bestrahlung PY - 2017 SN - 978-3-9816286-9-2 SP - V 8, 91 EP - 99 AN - OPUS4-42578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Kömmling, Anja A1 - Wachtendorf, Volker ED - Reichert, T. T1 - UV-LEDs - a new tool to determine the spectral response N2 - To determine a polymer’s spectral response of photo degradation, two main methods have been established. The so-called “filter technique” uses polychromatic radiation, which is filtered by a set of various sharp cut-on filters. This procedure provides separated reading points of an activation spectrum of the investigated material. With the "spectrographic technique” a specimen is irradiated with pectrally dispersed radiation, locally quasi monochromatically, and the local property changes.are related to the radiant exposure at the respective wavelengths. A third method, the irradiation of specimens with quasi monochromatic radiation behind interference filters, is rarely used. These methods have advantages and disadvantages and therefore, there are limits for conclusions from these spectral data. Concerning the quasi monochromatic Irradiation of specimens the development of new UV radiation sources looks promising. With the rapid development of inexpensive UV Light-emitting diodes (LEDs), new : sources of nearly monochromatic radiation in the UV ränge are available, even down to about 250 nm. To determine the spectral response, the use of such UV-LEDs in TO-18 ) and TO-39 metal cases combines the advantages of low cost and energy efficiency, stable spectral irradiance, temperature.and humidity control, larger specimen areas, and an easy and stable analysis. Combinations of different UV LEDs are also discussed as replacement for xenon arc ' radiation sources, see patent application EP01528388A1. T2 - 5th European weathering symposium - Natural and artificial ageing of polymers CY - Lisbon, Portugal DA - 21.09.2011 KW - UV resistance KW - Weathering KW - Spectral sensitivity KW - Action spectrum KW - UV-LEDs PY - 2011 SN - 978-3-9813136-2-8 N1 - Serientitel: CEEES Publication – Series title: CEEES Publication IS - 15 SP - 77 EP - 86 PB - GUS (Gesellschaft für Umweltsimulation) CY - Pfinztal AN - OPUS4-24396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meurer, Maren T1 - Is olypropylene relevant for microplastic analytics? N2 - Nowadays, in every terrestrial and aquatic ecosystem, even in the remotest areas, small residues of plastics, the so called microplastic (MP) can be found. MPs are particles with a size of 1-1000 µm (ISO/TR 21960:2020), mainly containing synthetic polymers like polyethylene (PE), polypropylene (PP), polystyrene (PS) or polyethylene terephthalate (PET). Even styrene-butadiene rubber (SBR) as an indication for tire wear is included due to similar particle formation. To understand the MPs consequences to the environment, it is of high priority to capture its extent of contamination. It is surprising that in the analysis of polymer masses in environmental samples, PE, PS and SBR are often detected, but only small amounts of PP, although this is the second most commonly produced standard plastic and many MP particles originate from carelessly disposed packaging materials. This presentation provides hypotheses about the reasons of rare PP identification and mass quantification in environmental samples. Different investigations of pristine PP and representative environmental samples, including the pre-treatment by Accelerated Solvent Extraction (ASE) or with density separation followed by the thermal extraction / desorption gas chromatography-mass spectrometry (TED-GC/MS) are presented. The results are discussed according to the material properties and a possible degradation mechanism under different weathering conditions which indicate less stability under relevant storage conditions. T2 - Society of Environmental Toxicology and Chemistry CY - Dublin, Ireland DA - 30.04.2023 KW - Sample preparation KW - Polypropylene KW - Microplastic KW - Degradation PY - 2023 AN - OPUS4-57474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Völzke, Holger A1 - Wolff, Dietmar A1 - Barnabas, I. A1 - Ordogh, M. A1 - Shirai, K. A1 - Saegusa, T. A1 - Cho, C.-H. A1 - Kook, D. A1 - Lopez, J. F. A1 - Conde, J. M. A1 - Alejano, C. A1 - Lloret, M. A1 - Quecedo, M. A1 - Shea, J. A1 - Ross, P. J. A1 - White, N. A1 - Rossiter, G. A1 - Hodgson, Z. A1 - Sorenson, K. A1 - McConnell, P. A1 - Hanson, B. ED - Sorenson, K. ED - Shirai, K. ED - Völzke, Holger T1 - Extended storage collaboration program - International subcommittee report - International perspectives on technical data gaps associated with extended storage and transportation of used nuclear fuel N2 - The US Electric Power Research Institute (EPRI) chartered a volunteer committee in November 2009 to share information and data related to extended storage and subsequent transportation of used nuclear fuel. This committee is named the Extended Storage Collaboration Program (ESCP) and was initially comprised of representatives from industry (fuel and cask vendors, utilities, the Nuclear Energy Institute, and EPRI), as well as government (e.g., US Department of Energy) and the US Nuclear Regulatory Commission. The primary motivation for establishing this committee was the recognition that used fuel will need to be stored past the regulatory licensing timeframe. In the US, this is mainly a result of the cessation of licensing activities for the planned Yucca Mountain repository. Recognizing that there is a global interest in extended storage and transportation, the International Subcommittee was established in December 2010 to extend the reach of ESCP internationally in order to fully address extended storage and transportation issues, as they apply to different systems, national policies, and regulations around the world. This Subcommittee serves to deepen the overall understanding of degradation mechanisms associated with storage and transportation systems, expand the access to data and programs related to extended storage and transportation, and strengthen the overall technical basis for programmatic decisions. The International Subcommittee established three basic objectives: 1. Conduct a technical data gap survey 2. Assess opportunities to leverage specific research to benefit the larger international group 3. Integrate our work with relevant International Atomic Energy Agency (IAEA) committee work This report constitutes completion of Objective #1. The International Subcommittee worked to identify and prioritize technical gaps that need to be addressed to support licensing activities within their own countries. Because there are varying types of storage and transportation system designs, national policies and regulations, there are identified commonalities as well as differences that stress the importance of this work on an international scale. Section 5 of this report identifies and prioritizes all of the identified data gaps for each participating organization. However, important data gaps were identified that had a consensus of opinion of being a high priority. These technical gaps, as a function of storage system component are: 1. Fuel – hydride effects on fuel cladding and retrievability of fuel after storage 2. Canister – general canister corrosion and stress corrosion cracking of canister closure welds, particularly in marine environments 3. Closure – degradation of bolts and seals (metallic and organic) 4. Overpack – concrete degradation Dry storage systems were originally designed for limited periods. With extended dry storage, it is generally believed that used fuel can be stored safely and securely past the regulatory time period. However, the technical arguments need to be made to justify extended licensing periods. Addressing the data gaps will provide the necessary arguments to justify license extensions. In the development of this report, the International Subcommittee met five times over a period of 18 months to work through the issues of identifying and prioritizing the data gaps, and discussing of technical issues as they pertain to the safety of used fuel storage and transportation. The meeting locations and dates were: 1. Vienna June 2010 2. London October 2010 3. Charlotte December 2010 4. Berlin June 2011 5. Charlotte December 2011 This report is not meant to be a technical document. Rather, it is an overview of country regulatory policy, a review of in-country operational status and used fuel inventory, followed by a role-up of identification and prioritization of technical data gaps. Technical documents that were used in the data gap assessments are referenced. It is important to note that this document represents only the opinions of the contributors. This document in no way represents any official country position. The organizations providing support to the writing of this report are: Germany: - Bundesanstalt für Materialforschung und -prüfung Hungary: - Radioaktiv Julladekokat Kezelo Kozhasznu - Som System Kft. Japan: - Central Research Institute of Electric Power Industry South Korea: - Korea Atomic Energy Research Institute - Korea Radioactive Waste Management Corporation Spain: - Consejo de Seguridad Nuclear - ENRESA Empresa Nacional de Residuos Radiactivos - ENUSA Industrias Avanzadas United Kingdom: - EDF Energy - National Nuclear Laboratory Ltd. United States: - Pacific Northwest National Laboratory - Sandia National Laboratories KW - Used/spent fuel dry storage KW - Used/spent fuel transportation KW - Extended used/spent nuclear fuel storage KW - High burnup spent fuel storage and transportation KW - Spent fuel storage and transportation KW - Extended Storage Collaboration Program (ESCP) KW - ESCP International Subcommittee PY - 2012 UR - https://www.epri.com/research/products/1026481 N1 - This final report was prepared as part of the volunteer Extended Storage Collaboration Program (ESCP). VL - 1026481 SP - 1 EP - 132 PB - Electric Power Research Institute (EPRI) CY - Palo Alto, CA, USA AN - OPUS4-27405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trubiroha, P. A1 - Geburtig, Anja A1 - Wachtendorf, Volker T1 - Natural versus artificial weathering of polymers – main differences in climatic conditions N2 - Different climatic conditions and weather variables during natural and artificial exposure of polymers may be reasons for an unsatisfying correlation between the ageing results. Here the main differences are discussed for: - Global solar radiation In weathering devices there is a constant spectral irradiance which is 5 times higher than the averaged spectral irradiance outdoors, which is strongly varying in its diurnal course. Intensified weathering using Fresnel reflectors concentrates only the direct solar radiation with a relatively low UV proportion. Problems of reciprocity may arise from the different mean of irradiance levels. - Temperatures at specimen surfaces. Because of the high irradiance levels mentioned above, artificial exposures may lead to high surface temperatures and large temperature differences between differently coloured specimen surfaces, if the artificial radiation source emits much VIS- and IR-radiation. Outdoors the surface temperature and temperature differences of exposed specimens are influenced by considerably lower irradiance levels and additionally by an effective radiation loss in the night. - Relative humidity at specimen surfaces In weathering devices the relative humidity at specimen surfaces is very low if it is uncontrolled. If controlled by ultrasonic humidifiers or spray nozzles, the additional exposure to water droplets is quite likely. - Wetness on specimen surfaces All usual spray programs prescribed in weathering standards recommend frequently changing of short spray/dry periods and result in total times of wetness (TOW) of the exposed specimen surfaces which is only about 30 % of the outdoor TOW. - Acidic precipitation and bio films Acidic precipitation and bio films are usual outdoor conditions which are only considered in special weathering tests. T2 - 8th European Weathering Symposium CY - Vienna, Austria DA - 20.09.2017 KW - Artificial weathering KW - Natural weathering KW - Weathering parameters PY - 2017 SN - 978-3-9818507-1-0 VL - 18 SP - 63 EP - 75 CY - Karlsruhe AN - OPUS4-42127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Purohit, Purv A1 - Huacuja Sánchez, Jesús A1 - Wang, D.-Y. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Heinrich, G. A1 - Schönhals, Andreas T1 - Structure - property relationships of nanocomposites based on polypropylene and layered double hydroxides N2 - Nanocomposites based on polypropylene (PP) and organically modified ZnAl layered double hydroxides (ZnAl-LDH) were prepared by melt blending and investigated by a combination of differential scanning calorimetry (DSC), small- and wide-angle X-ray scattering (SAXS and WAXS), and dielectric relaxation spectroscopy (DRS). An average number of stack size of LDH layers is calculated by analyzing the SAXS data which is close to that of pure organically modified ZnAl-LDH. Scanning microfocus SAXS investigations show that the ZnAl-LDH is homogeneously distributed in the PP matrix as stacks of 4–5 layers with an intercalated morphology. DSC and WAXS results show that the degree of crystallinity decreases linearly with the increasing content of LDH. The extrapolation of this dependence to zero estimates a limiting concentration of ca. 40% LDH where the crystallization of PP is completely suppressed by the nanofiller. The dielectric spectra of the nanocomposites show several relaxation processes which are discussed in detail. The intensity of the dynamic glass transition (β-relaxation) increases with the concentration of LDH. This is attributed to the increasing concentration of the exchanged anion dodecylbenzenesulfonate (SDBS) which is adsorbed at the LDH layers. Therefore, a detailed analysis of the β-relaxation provides information about the structure and the molecular dynamics in the interfacial region between the LDH layers and the polypropylene matrix which is otherwise dielectrically invisible (low dipole moment). As a main result, it is found that the glass transition temperature in this interfacial region is by 30 K lower than that of pure polypropylene. This is accompanied by a drastic change of the fragility parameter deduced from the relaxation map. KW - Nanocomposites KW - Layered double hydroxide KW - Dielectric spectroscopy KW - X-ray scattering KW - Polypropylene PY - 2011 DO - https://doi.org/10.1021/ma200323k SN - 0024-9297 SN - 1520-5835 VL - 44 IS - 11 SP - 4342 EP - 4354 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leiterer, Jork T1 - In Droplet Monitoring of Catalytic Precursors Preparation T2 - 27 th Bessy User's Meeting CY - Berlin, Germany DA - 2008-12-06 PY - 2008 AN - OPUS4-18516 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leiterer, Jork T1 - In situ Studies of Caffeine Polymorph Crystal Formation by Droplet Evaporation T2 - 27h Bessy Users´ Meeting CY - Berlin, Germany DA - 2008-12-06 PY - 2008 AN - OPUS4-18520 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Kraus, Werner A1 - Bischoff, F. A. A1 - Emmerling, Franziska A1 - Resch-Genger, Ute A1 - Tschiche, Harald T1 - Temperature- and Structure-Dependent Optical Properties and Photophysics of BODIPY Dyes N2 - We report on the temperature- and structural-dependent optical properties and photophysics of a set of boron dipyrromethene (BODIPY) dyes with different substitution patterns of their meso-aryl subunit. Single-crystal Xray diffraction analysis of the compounds enabled a classification of the dyes into a sterically hindered and a unhindered group. The steric hindrance refers to a blocked rotational motion of the aryl subunit around the bond connecting this moiety to the meso-position of the BODIPY core. The energy barriers related to this rotation were simulated by DFT calculations. As follows from the relatively low rotational barrier calculated to about 17 kcal/mol, a free rotation is only possible for sterically unhindered compounds. Rotational barriers of more than 40 kcal/mol determined for the sterically hindered compounds suggest an effective freezing of the rotational motion in These molecules. With the aid of temperature-dependent spectroscopic measurements, we could show that the ability to rotate directly affects the optical properties of our set of BODIPY dyes. This accounts for the strong temperature dependence of the fluorescence of the sterically unhindered compounds which show a drastic decrease in fluorescence quantum yield and a significant shortening in fluorescence lifetime upon heating. The optical properties of the sterically hindered compounds, however, are barely affected by temperature. Our results suggest a nonradiative deactivation of the first excited singlet state of the sterically unhindered compounds caused by a conical intersection of the potential energy surfaces of the Ground and first excited state which is accessible by rotation of the meso-subunit. This is in good agreement with previously reported deactivation mechanisms. In addition, our results suggest the presence of a second nonradiative depopulation pathway of the first excited singlet state which is particularly relevant for the sterically hindered compounds. KW - Fluorescence KW - Sensor KW - Switch KW - pH KW - BODIPY KW - Dye KW - Probe KW - Synthesis KW - Photophysics KW - Mechanism PY - 2020 DO - https://doi.org/10.1021/acs.jpca.9b11859 SN - 1089-5639 VL - 124 IS - 9 SP - 1787 EP - 1797 PB - American Chemical Society AN - OPUS4-50639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Olivera, Paulo A1 - Michalchuk, Adam A1 - Marquardt, Julien A1 - Feiler, Torvid A1 - Prinz, Carsten A1 - Torresi, R. A1 - Camargo, P. A1 - Emmerling, Franziska T1 - Investigating the role of reducing agents on mechanosynthesis of Au nanoparticles N2 - Control over the bottom up synthesis of metal nanoparticles (NP) depends on many experimental factors, including the choice of stabilising and reducing agents. By selectively manipulating these species, it is possible to control NP characteristics through solution-phase synthesis strategies. It is not known, however, whether NPs produced from mechanochemical syntheses are governed by the same rules. Using the Au NPs mechanosynthesis as a model system, we investigate how a series of common reducing agents affect both the reduction kinetics and size of Au NPs. It is shown that the relative effects of reducing agents on mechanochemical NP synthesis differ significantly from their role in analogous solution-phase reactions. Hence, strategies developed for control over NP growth in solution are not directly transferrable to environmentally benign mechanochemical approaches. This work demonstrates a clear need for dedicated, systematic studies on NP mechanosynthesis. KW - Mechanochemistry KW - Metal nanoparicels PY - 2020 DO - https://doi.org/10.1039/d0ce00826e VL - 22 IS - 38 SP - 6261 EP - 6267 PB - Royal Society of Chemistry AN - OPUS4-51757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Haferkamp, Sebastian A1 - Akhmetova, Irina A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical one-pot syntheses N2 - We present an in situ triple coupling of synchrotron X-ray diffraction with Raman spectroscopy, and thermography to study milling reactions in real time. This combination of methods allows a correlation of the structural evolution with temperature information. The temperature information is crucial for understanding both the thermodynamics and reaction kinetics. The reaction mechanisms of three prototypical mechanochemical syntheses, a cocrystal formation, a C@C bond formation (Knoevenagel condensation), and the formation of a manganese-phosphonate, were elucidated. Trends in the temperature development during milling are identified. The heat of reaction and latent heat of crystallization of the product contribute to the overall temperature increase. A decrease in temperature occurs via release of, for example, water as a byproduct. Solid and liquid intermediates are detected. The influence of the mechanical impact could be separated from temperature effects caused by the reaction. KW - In situ studies KW - Mechanochemistry KW - Raman spectroscopy KW - Thermography KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1002/anie.201800147 SN - 1433-7851 SN - 1521-3773 VL - 57 IS - 20 SP - 5930 EP - 5933 PB - Wiley-VCH CY - Weinheim AN - OPUS4-44946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - First seconds in a building's life - In situ synchrotron X-ray diffraction study of cement hydration on the millisecond timescale N2 - Setting cement: Highly dynamic hydration processes that occur during the first seconds of cement hydration were studied by time-resolved synchrotron X-ray diffraction. Polycarboxylate ether additives were found to influence the formation of the initial crystalline hydration products on a molecular level. KW - Cement hydration KW - Colloidal suspensions KW - In situ analysis KW - X-ray diffraction KW - SyXRD KW - High resolution KW - In-situ PY - 2012 DO - https://doi.org/10.1002/anie.201200993 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 51 IS - 20 SP - 4993 EP - 4996 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kittner, Maria T1 - Bewertung der Freisetzung von Mikroplastik aus Sportböden auf Kunststoffbasis N2 - Es handelt sich hierbei um die Abschluss-Präsentation des Projektes "Bewertung der Freisetzung von Mikroplastik aus Sportböden auf Kunststoffbasis", die am 28.11.24 vor dem Drittmittelgeber Zukunft Bau Forschungsförderung im Rahmen der 28. Projekttage der Bauforschung präsentiert wurde. Der 30-minütige Vortrag gliederte sich in die Kapitel Forschungsbedarf, Konzept, Ergebnisse und Take Home-Messages des Projektes. T2 - 28. Projekttage der Zukunft Bau Forschungsförderung CY - Online meeting DA - 26.11.2024 KW - Mikroplastik KW - TED-GC/MS KW - Kunststoffrasen KW - PAK KW - Schwermetalle KW - Mikroplastik Eluat Lysimeter PY - 2024 AN - OPUS4-61815 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska T1 - Insights into the mechanochemical Knoevenagel condensation N2 - Mechanochemistry paves the way to simple, fast, and green syntheses, but there is a lack in understanding of the underlying mechanisms. Here, we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. T2 - Bessy User Meeting 2019 CY - Berlin, Germany DA - 05.12.2019 KW - Mechanochemistry PY - 2019 AN - OPUS4-50122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - May, Anastasia T1 - Thermomechanochemical Synthesis of Pimelic Acid Cocrystals N2 - Milling temperature is a critical factor in mechanochemistry, affecting the kinetics and outcomes of reactions. In the context of cocrystallization, the influence of milling temperature on the process has been investigated for cocrystal systems pyrazinamide:pimelic acid (PZA:PA) and 4,4'-bipyridine:pimelic acid (BPY:PA). By means of temperature-controlled milling, stabilization of metastable polymorph of PZA:PA was achieved, thereby decelerating the aging process of the polymorph. This was accomplished through controlled heated milling of PZA and PA. Furthermore, we have successfully synthesized all three BPY:PA polymorphs by mechanochemistry involving controlled cooled and heated milling. In previous studies, only the most stable polymorph was obtained by mechanochemistry. T2 - 10th European Crystallography School CY - Ohrid, North Macedonia DA - 23.06.2025 KW - Mechanochemistry KW - Cocrystal PY - 2025 AN - OPUS4-63797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Bannick, C.G. A1 - Szewzyk, R. A1 - Ricking, M. A1 - Schniegler, S. A1 - Obermaier, N. A1 - Barthel, A. K. A1 - Altmann, Korinna A1 - Eisentraut, Paul T1 - Development and testing of a fractionated filtration for sampling of microplastics in water N2 - A harmonization of sampling, sample preparation and detection is pivotal in order to obtain comparable data on microplastics (MP) in the environment. This paper develops and proposes a suitable sampling concept for waterbodies that considers different plastic specific properties and influencing factors in the environment. Both artificial water including defined MP fractions and the discharge of a wastewater treatment plant were used to verify the derived sampling procedure, sample preparation and the subsequent analysis of MP using thermal extraction-desorption gas chromatography - mass spectrometry (TED-GC-MS). A major finding of this paper is that an application of various particle size classes greatly improves the practical handling of the sampling equipment. Size classes also enable the TED-GC-MS to provide any data on the MP size distribution, a substantial sampling property affecting both the necessary sampling volume and the optimal sampling depth. In the artificial water with defined MP fractions, the recovery rates ranged from 80 to 110%, depending on the different MP types and MP size classes. In the treated wastewater, we found both Polyethylene and polystyrene in different size classes and quantities. KW - Microplastics KW - Sampling KW - Sampling techniques KW - Water PY - 2019 DO - https://doi.org/10.1016/j.watres.2018.10.045 SN - 0043-1354 VL - 149 SP - 650 EP - 658 PB - Elsevier AN - OPUS4-47200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Polte, J. A1 - Bernsmeier, D. A1 - Eckhardt, B. A1 - Paul, B. A1 - Bergmann, A. A1 - Strasser, P. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Pd/TiO2 coatings with template-controlled mesopore structure as highly active hydrogenation catalyst N2 - Micro-structured reactors offer excellent mass and heat transport capabilities and can therefore sustain very high reaction rates and space–time-yields also for highly exothermic catalytic reactions. However, such high rates cannot be reached when the reactors are coated or filled with conventional catalysts powders. We present a strategy for the direct synthesis of highly active wall-coated supported catalysts via co-deposition of a pore template (here micelles formed from PEO-b-PPO-b-PEO) and a precursors for the metal oxide (TiCl4) along with a compatible precursor for the active metal (PdCl2). The obtained catalytic coatings possess a template-controlled open pore structure and excellent mechanical stability. Moreover, the active metal is highly dispersed and well-distributed across the coating also at high Pd loadings. The corresponding high activity along with rapid mass transfer enabled by the open pore system results in the best space–time-yields in the gas-phase hydrogenation of butadiene reported so far in literature for a supported catalyst. KW - Titanium oxide films KW - Palladium nanoparticle KW - Wall-coated supported catalysts KW - Template-controlled mesoporous materials KW - Hydrogenation of 1,3-butadiene PY - 2015 DO - https://doi.org/10.1016/j.apcata.2014.12.044 SN - 0926-860X SN - 1873-3875 VL - 493 SP - 25 EP - 32 PB - Elsevier CY - Amsterdam AN - OPUS4-32465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Tuaev, X. A1 - Wuithschick, M. A1 - Fischer, A. A1 - Thünemann, Andreas A1 - Rademann, K. A1 - Kraehnert, R. A1 - Emmerling, Franziska T1 - Formation mechanism of colloidal silver nanoparticles: analogies and differences to the growth of gold nanoparticles N2 - The formation mechanisms of silver nanoparticles using aqueous silver perchlorate solutions as precursors and sodium borohydride as reducing agent were investigated based on time-resolved in situ experiments. This contribution addresses two important issues in colloidal science: (i) differences and analogies between growth processes of different metals such as gold and silver and (ii) the influence of a steric stabilizing agent on the growth process. The results reveal that a growth due to coalescence is a fundamental growth principle if the monomer-supplying chemical reaction is faster than the actual particle formation. KW - Silver nanoparticle growth KW - Formation mechanisms KW - Nucleation KW - SAXS PY - 2012 DO - https://doi.org/10.1021/nn301724z SN - 1936-0851 VL - 6 IS - 7 SP - 5791 EP - 5802 PB - ACS Publ. CY - Washington, DC, USA AN - OPUS4-26427 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 - Strontium-coordination polymers based on tetrafluorophthalic and phthalic acids: mechanochemical synthesis, ab initio structures determination, and spectroscopic characterization N2 - Two strontium-based dicarboxylate systems [Sr(oBDC-F4)(H2O)2] (1) and [{Sr(oBDC)(H2O)2)·H2O] (2) were synthesized mechanochemically via milling of Sr(OH)2·8H2O with tetrafluorophthalic acid (H2oBDC-F4) or phthalic acid (H2oBDC), respectively. The new structures were determined ab initio from the powder X-ray diffraction (PXRD) data. Both compounds 1 and 2 crystallize in the monoclinic space group P21 /c as two-dimensional coordination polymers (2D-CPs). The determined structures were validated by extended X-ray absorption (EXAFS) data. Compounds 1 and 2 show different thermal stabilities. The fluorinated CP 1 is decomposed at 300 °C while the nonfluorinated CP 2 transforms into a new phase after thermal treatment at 400 °C. The two hydrated CPs exhibit small surface areas which increase after the thermal posttreatment for 1 but remains unchanged for the dehydrated sample of 2. Dynamic vapor sorption (DVS) experiments indicate that both the dehydrated and hydrated samples of 2 depict no significant differences in their adsorption isotherms. The DVS of water indicates that the phase transition after thermal posttreatment of 2 is irreversible. KW - Mechanochemistry KW - XRD KW - NMR PY - 2017 DO - https://doi.org/10.1039/c7dt02564e SN - 1477-9226 SN - 1477-9234 VL - 46 IS - 37 SP - 12574 EP - 12587 PB - The Royal Society of Chemistry CY - Cambridge AN - OPUS4-42261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manoharan, D. A1 - Ahmad, S. A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit A1 - Ghosh, S. T1 - Stress and light sensitive dual-mechanical property of acylhydrazone crystal N2 - Mechanically dual-responsive molecular crystals have gained ubstantial interest among researchers due to their significant applications in various fields. However, incorporation of disparate mechanical responses in the same crystalline material is still a challenging issue and is continuously being explored. Here, we report long acicular crystals derived from 4-bromobenzhydrazide and 9-anthraldehyde exhibit both stressinduced mechanical bending and blue-light induced photomechanical bending. Furthermore, the crystals show thermal back isomerization upon gradual heating. These two distinct mechanical responses in the crystalline phase have been studied and their structure–property correlation have been established. KW - Light sensitive crystal KW - Mechanical flexibility KW - Organic crystal PY - 2023 DO - https://doi.org/10.1039/d3ce00296a VL - 25 IS - 21 SP - 3237 EP - 3244 PB - Royal Society of Chemisty (RSC) CY - London/Cambridge AN - OPUS4-57593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Identification and Quantification of Microplastic in Sewage systems by TED-GC-MS N2 - The number of publications reporting the amount of microplastic (MP) all over the world increased rapidly. Methods used so far are very time consuming and not able to provide information on total contents. As harmonised sampling, sample preparation and analysis strategies are missing different studies can hardly be compared and quantitative data, including identification and mass contents of the polymers found, are missing. This leads to a lack of comprehensive understanding of MP occurrence, source and entry pathways into the environment. We developed a method, Thermal Extraction/Desorption-Gaschromatography-Massspectrometry, as a fast screening method for MP analysis. Solid residues of water samples are heated up to 600 C under a N2 atmosphere without any sample preparation. The collected decomposition gases are separated in a gas chromatography system and detected in a mass spectrometer. Mass contents of the identified polymers can be calculated. In this presentation we will show first results from the influent of the wastewater treatment plant Kaiserslautern (Germany) and its combined sewage system as possibly entry pathway. In order to determine the relevance of wastewater split streams analysis of grey water will be conducted. Samples are fractionally filtered by a sieve cascade with mesh sizes of 500, 100, 50 µm. T2 - CEST2019 CY - Rhodos, Greece DA - 04.09.2019 KW - Microplastic KW - TED-GC-MS KW - Microplastic analysis KW - Grey water KW - Waste water treatment plant PY - 2019 AN - OPUS4-48933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gugin, Nikita A1 - Villajos Collado, José Antonio A1 - Dautain, O. A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy N2 - We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production. KW - Mechanochemistry KW - In situ Raman KW - Large-scale processing KW - Metal−organic frameworks KW - Twin-screw extrusion (TSE) PY - 2023 DO - https://doi.org/10.1021/acssuschemeng.2c07509 SN - 2168-0485 VL - 11 IS - 13 SP - 5175 EP - 5183 PB - ACS Publications AN - OPUS4-57366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leiterer, Jork T1 - Characterisation of levitated samples for modelling of condensed matter N2 - Many of today’s analytical problems are characterized by small sample volumes and can only be solved through a corresponding miniaturisation of the analytical instrumentation. Handling of small-sample volumes is inherently difficult due to contamination and sorption processes on the walls of containers. Acoustic levitation is a powerful tool for contact-free sample handling of solid, liquid, and selected gaseous samples. In addition, levitation permits a chemical pre-treatment such as enrichment, extraction, and derivatisation as well as combination with other analytical techniques such as optical spectroscopy. Acoustically levitated liquid and solid samples are typically in a range between 0.005-5 µl (diameter 0.2-2 mm respectively) and are suspended in a gaseous environment by a stationary ultrasonic field. Acoustic levitation avoids sample contamination and sorption processes by container walls, but suffers from evaporation and loss of solvents. Nonetheless, it is of great impact for the characterization of small samples. Exact determination of volume is inherently important to find out the resultant concentration in evaporating droplets. Levitation is a possibility to characterise the starting conditions of crystallisation and polymerisation. Even for spectroscopic methods the correct information on shape, size and concentration of samples are indispensable. To determine the size and volume of levitated samples, different methods of contactless droplet size monitoring were developed and compared in detail. They give the initial values for modelling of evaporation effects. In addition, for balancing evaporation and condensation on levitated drops during the experiments, non-contact techniques of solvent and reagent supply have been tested. Here, the advantages of acoustic levitation are demonstrated for on line analysis of crystallisation in a levitated droplet. The evaporation and formation of crystals is observed via time-resolved X-ray diffraction using synchrotron radiation at BESSY. Wall-free crystallisation in an acoustic levitator gives a tool to prove existing models concerning crystallisation processes. Furthermore the occurrence of polymorphic modifications depending on different conditions can be detected in situ under different and adjustable conditions. T2 - 13. Vortragstagung "Modellierung in der Festkörper- und Materialchemie" der GDCh-Fachgruppe Analytische Chemie, Rheinisch-Westfälische Technische Hochschule Aachen CY - Aachen, Germany DA - 2006-09-20 PY - 2006 AN - OPUS4-13805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Božičević, Lucija A1 - Altmann, Korinna A1 - Hildebrandt, Jana A1 - Knigge, Xenia A1 - Vrček, Valerije A1 - Peranić, Nikolina A1 - Kalcec, Nikolina A1 - Vinkovic Vrcek, Ivana T1 - Estrogenic activity of plastic nanoparticles mixture under in vitro settings N2 - The plastic value chain, central part of modern living, caused environmental pollution and bioaccumulation of plastic nanoparticles (PNPs). Their ubiquitous presence in different environmental and biological compartments has become a serious threat to human health and ecosystems. Frequently used plastic materials such as polypropylene (PP), polystyrene (PS) and polyethylene (PE) have been detected in the form of PNPs in the food chain, soil, water and air, as well as in human feces and blood. In this study, we aimed to provide novel insights in endocrine disrupting properties of PNPs using in vitro estrogen receptor (ER) transactivation assay. The effects of PP-NPs, PE-NPs and PS-NPs and their mixture on T47D-KBluc cell line stably transfected with luciferase as reporter enzyme was evaluated by means of cytotoxicity, cellular uptake and ER activation. Tested dose range for PNPs was 0.001 – 10 mg/L. Both cellular uptake and cytotoxicity for all PNPs was found to be dose-dependent. Only the highest dose of PP-NPs and PE-NPs induced apoptosis and cell death, while PS-NPs were not cytotoxic in tested dose range. For tested concentrations, PP-NPs and PE-NPs showed significant agonistic activity on ER, while PS-NPs cannot be considered ER active. When, applied as mixture, PNP demonstrated additive toxicity effects compared to the effect of each individual PNPs. Additivity was also observed for ER agonistic effect of PNPs mixture according to the benchmark dose-addition modelling approach. This study provides missing science-based evidence on endocrine disrupting effects of PE-NPs, PP-NPs, PS-NPs and their mixtures and highlights the importance of considering unintentional, aggregate and combined exposure to different PNPs in risk management. KW - Risk assessment KW - Nanoplastics KW - Estrogenic activity of plastic nanoparticles PY - 2024 DO - https://doi.org/10.1039/D3EN00883E SN - 2051-8153 VL - 11 IS - 5 SP - 2112 EP - 2126 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lee, P.-W. A1 - Kaynak, T. A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Schalley, C. T1 - Effect of Perfluorinated Side-Chain Length on the Morphology, Hydrophobicity, and Stability of Xerogel Coatings N2 - Superhydrophobic surfaces can be quickly formed with supramolecular materials. Incorporating low-molecular-weight gelators (LMWGs) with perfluorinated chains generates xerogel coatings with low surface energies and high roughness. Here, we examine and compare the properties of the xerogel coatings formed with eight different LMWGs. These LMWGs all have a trans-1,2-diamidocyclohexane core and two perfluorinated ponytails, whose lengths vary from three to ten carbon atoms (CF3 to CF10). Investigation of the xerogels aims to provide in-depth information on the chain length effect. LMWGs with a higher degree of fluorination (CF7 to CF10) form superhydrophobic xerogel coatings with very low surface energies. Scanning electron microscopy images of the coatings show that the aggregates of CF5 and CF7 are fibrous, while the others are crystal-like. Aggregates of CF10 are particularly small and further assemble into a porous structure on the micrometer scale. To test their stabilities, the xerogel coatings were flushed multiple times with a standardized water flush test. The removal of material from the surface in these flushes was monitored by a combination of the water contact angle, contact angle hysteresis, and coating thickness measurements. A new method based on image processing techniques was developed to reliably determine the change of the coating thickness. The CF7, CF9, and CF10 surfaces show consistent hydrophobicity and coating durability after repetitive flushing tests. The length of the perfluorinated side chains thus has a significant effect on the morphology of the deposited xerogel coatings, their roughness, and, in consequence, their hydrophobicity and mechanical durability. KW - Coating materials KW - Amorphous materials KW - Hydrophobicity KW - Materials Stability PY - 2021 DO - https://doi.org/10.1021/acs.langmuir.1c02341 SN - 1520-5827 VL - 37 IS - 49 SP - 14390 EP - 14397 PB - ACS Publications AN - OPUS4-54071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmitt, M. A1 - Altmann, Korinna A1 - Fengler, Petra A1 - Gehde, M. T1 - Air-based polyethylene fragmentation with high yield to form microplastic particles as reference material candidates N2 - Microplastic particles with sizes between 1 to 1000 μm are widely distributed worldwide. Origin, transport pathways and fate are poorly known, as sampling, sample preparation and detection methods are major challenges. In addition, reference materials that mimic environmental particles are lacking. Most challenging is the yield of MP particle production and the need for resource-intensive grinding with liquid nitrogen. In this paper, a machine is designed to produce aged microplastic particles as reference material candidates with high yield. The machine is based on ultraviolet aging of a thin foil and mechanical fragmentation using clean air. An example of aging and fragmentation of high density polyethylene with additional physical and chemical characterization of shape, size, aging state by carbonyl index and density is presented. KW - Microplastics KW - Degradation of polyethylene KW - Air fragmentation KW - Microplastics reference material PY - 2023 DO - https://doi.org/10.1002/appl.202200121 SP - 1 EP - 18 PB - Wiley online library AN - OPUS4-57203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline T1 - Detection of microplastic and tire wear particles in road run-off samples using TED-GC-MS N2 - Plastics and rubber are used in many applications, such as packaging, building, construction and mobility. Due to their favourable properties like light weight, flexible processing and low costs their production and consequently their input into the environment has increased significantly over the last decades. In the environment, oxidation processes and mechanical abrasion lead to the decomposition of these plastics into small fragments, called microplastic (< 5 mm). By definition, microplastics only involve thermoplastics and duroplastics but elastomers made out of synthetic polymers (e. g. styrene butadiene rubber), modified natural polymers (e. g. natural rubber) and products of synthetic polymers (e. g. tires) are also part of the current microplastic discussion. The main entry pathway of rubber into the environment is the wear of used tire treads in road traffic. Lassen et al. showed that 60 % of the microplastic emissions in Denmark into the environment come from secondary microplastics generated by tires. Rain events can cause microplastic and rubber to get from the street into the street inlets. Depending on the sewage system, these waters are sometimes not cleaned in the sewage treatment plants and reach the surface waters untreated. To analyse microplastic particles in samples, mainly FTIR or Raman spectroscopic methods are applied at present. Rubber or tire particles in environmental samples cannot be analysed by these methods, because the added carbon black leads to annoying absorption and fluorescent effects. We developed a thermoanalytical method, the so-called TED-GC-MS (thermal extraction desorption gas chromatography mass spectrometry), which allows the simultaneous detection of microplastic and tire wear with almost no sample preparation in about 2.5 h. The TED-GC-MS is a two-step analytical method which consists of a thermobalance and a GC-MS system. Up to 50 mg of an environmental sample is heated up to 600 °C in a nitrogen atmosphere. During pyrolysis, between 300 and 600 °C polymer-specific decomposition products are produced and collected on a solid phase. Afterwards the substances are desorbed, separated and analysed using the GC-MS. The aim of the present work is to present the TED-GC-MS as a time efficient screening method to quantify the industrial most relevant polymers in street run-off samples. Analytical challenges in the determination of polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA), polymethyl methacrylate (PMMA) and styrene-butadiene-rubber (SBR) as a component of tire wear are honestly discussed. The study area is a 200 m long section of the Clayallee in Berlin, a representative typical urban catchment area. The road run-off in this section flows through the gullies directly into a sample chamber, which directs the runoff in an open channel to the rainwater sewer of this area. The sample chamber allows a sample to be taken directly from the road run-off without mixing with the run-off from other areas. The sample chamber is equipped with an automatic sampler. The automatic sampler is controlled by a conductivity sensor to detect the storm event at an early stage. The sensor gives the sampler a signal to start the sampling program when it gets in contact with water and reaches a certain conductivity threshold. The capacity of the sample container is 100 l and the maximum delivery of the automatic sampler is 2.8 l/min. Afterwards, the water was pumped through various stainless-steel sieves with a diameter of approximately 20 cm and mesh widths of 500, 100, 50 μm. The obtained solids were steam sterilized, freeze-dried and measured with the TED-GC-MS. The results of the TED-GC-MS-measurements are summarized in Figure 1. It shows the polymers which were detected in 1 mg of the dry masses of various street run off samples obtained during a period of 1.5 years. We detected PMMA, PS, PP, PE and SBR, as a component of tire wear in the samples. The quantification of the polymers leads to amounts of PS, PP, PE and SBR between 0 µg and 10 µg. PMMA was only detected in traces. T2 - ICCE 2019 CY - Thessaloniki, Greece DA - 16.06.2019 KW - Microplastics KW - TED-GC-MS KW - Road run-off KW - Chromatography PY - 2019 AN - OPUS4-48301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Simone T1 - Influence of the pH Value to the Degradation of Ester-Based Thermoplastic Polyurethanes N2 - Microplastics are solid polymeric particles with a size of 1-1000 μm (ISO/TR21960:2020), which can be emitted from mismanaged waste into the environment, where microplastic is now ubiquitous. What happens to the microplastics after ending up in the environment, which risks entail and what effects it has are not sufficiently clarified up to now. The most certain issue is that the plastic particles in the environment are exposed to natural ageing, are fragmenting and degrading, such that the potential risk to ecosystems and humans is increasing due to the formation of smaller and smaller particles, potentially even including nanoplastics, if these are ingested before their further degradation. Therefore, and in view of a possible registration of polymers under REACH in the future, it is necessary to investigate the degradation of thermoplastic polyurethanes (TPU) regarding hydrolysis stability to evaluate possible risks and effects to the environment. In the present studies, one thermoplastic polyurethane – with and without hydrolysis stabilizer – is exposed to different pH buffers at 50°C for 14 days to investigate hydrolysis depending to different pH values (acid, alkali and neutral) based on OECD guideline TG111. The hydrolysis behavior of the TPUs is characterized by surface sensitive techniques and on bulk properties. First degradation effects can be detected by SEC. Hydrolysis, especially under acidic and basic conditions, leads to chain scissions to lower molecular masses. Furthermore, the degradation products which indicate the structure of the bulk material were detected by thermo-analytical methods like TGA-FTIR for the small degradation products and the thermo extraction/desorption-gaschromatography/mass spectrometry (TED-GC/MS) for bigger degradation products. Acidic and basic hydrolysis shows the same degradation behavior which is caused by a preferred scission of the ester and urethane functionalities. Surface-sensitive techniques such as XPS demonstrate less carboxylic acid formation at acidic than at alkaline pH value in the TPU without stabilator, where as the TPU with stabilator ages to the same extent in both pH ranges. Altogether, the hydrolysis of TPUs – independently of added stabilizer or not – in acid and alkali environment is accelerated compared to the neutral hydrolysis. T2 - SETAC CY - Dubin, Ireland DA - 30.04.2023 KW - Degradation KW - Thermoplastic Polyurethane KW - Microplastic KW - Polymer Hydrolysis KW - Polymer 3R KW - REACH PY - 2023 AN - OPUS4-58906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wiesner, Yosri T1 - Erfassung von Degradationsprodukten und Additiven sowie temperaturspezifische Pyrolyseprodukte mittels TED-GC/MS N2 - Im der Präsentation werden, neben der Möglichkeit der Mikroplastikquantifizierung, auf weitere Anwendungsfelder der Methode TED-GC/MS eigegangen. Dies beinhaltet die Erfassung von Degradationsprodukten UV/O2 geschädigter Polymere und die Detektion von Additiven. Die Optimierung der Methode betreffend Messzeit und materialspezifischer Messanforderung sind ebenfalls Gegenstand. T2 - Kolloquium Massenspektrometrie von Polymeren CY - Berlin, Germany DA - 09.05.2023 KW - TED-GC/MS KW - Polymere KW - Degradation KW - Additive PY - 2023 AN - OPUS4-57480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moss, Caitlin T1 - Mechanochemistry as a Green Synthetic Route N2 - Mechanochemistry has emerged as a transformative approach in sustainable chemistry, offering a solvent-free and energy-efficient pathway for chemical synthesis. By utilizing mechanical force—typically through ball milling, grinding, or other shear-driven methods, reactions can proceed without the extensive use of harmful solvents, reducing waste and environmental impact. This poster explores the principles, methodologies, and applications of mechanochemistry in developing greener synthetic routes, with a focus on pharmaceutical and materials science applications. Key advantages, including reduced reaction times, enhanced selectivity, and improved atom economy, will be highlighted alongside challenges such as scalability. By presenting mechanochemistry as a frontier technology at the intersection of chemistry, materials science, and environmental stewardship, this work invites dialogue among students and academics about its future in sustainable innovation. T2 - Furture WINS 2024 CY - Berlin, Germany DA - 21.11.2024 KW - Mechanochemistry KW - Green chemistry PY - 2024 AN - OPUS4-62123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinekamp, Christian T1 - Synthesis of zirconiumfluorides using a sol-gel/postfluorination approach and their application in C-F bond activation N2 - ZrF4 species have shown to exhibit hard Lewis acidity in homogeneous systems. In order to study solid state Lewis acidic ZrF4 a sol-gel synthesis was adapted following previous approaches for AlF3 and a necessary post fluorination is being optimised to obtain a Lewis acidic heterogeneous catalyst for C-F bond activation. The influence of different Zr precursors was also studied while the local coordination sphere of a active species was found to be similar to β-ZrF4 using EXAFS of the Zr K-edge. T2 - RSC Twitter Poster Conference 2023 CY - Online meeting DA - 28.02.2023 KW - ZrF4 KW - Heterogeneous catalysis PY - 2023 AN - OPUS4-57227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, Gudrun A1 - Emmerling, Franziska A1 - Kemnitz, Erhard T1 - Barium coordination polymers based on fluorinated and fluorine-free benzene-dicarboxylates: Mechanochemical synthesis and spectroscopic characterization N2 - A series of new Ba-based coordination polymers (CPs) were mechanochemically synthesized by milling Ba-hydroxide samples with perfluorinated and fluorine-free benzene-dicarboxylic acids, including tetrafluoroisophthalic acid (H2mBDC-F4), tetrafluorophthalic acid (H2oBDC-F4), isophthalic acid (H2mBDC) and phthalic acid (H2oBDC). The new fluorinated CPs: [Ba(mBDC-F4)$0.5H2O] (1) and [Ba(oBDC-F4)·1.5H2O] (2) are compared to their nonfluorinated counterparts: [Ba(mBDC)·2.5H2O] (3), and [Ba(oBDC)·1H2O] (4). These materials are thoroughly characterized using powder X-ray diffraction. The products obtained by milling are all hydrated but vary in their water contents. Compositions and local structures are investigated by elemental analysis, thermal analysis, MAS NMR and attenuated total reflectioninfrared spectroscopy. These materials exhibit high thermal stabilities but small surface areas that remain unchanged even after thermal treatments. KW - Mechanochemical synthesis KW - Barium KW - Fluorine KW - Coordination polymers KW - PXRD KW - MAS NMR spectroscopy PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S1293255817310798 DO - https://doi.org/10.1016/j.solidstatesciences.2018.03.013 SN - 1293-2558 SN - 1873-3085 VL - 79 SP - 99 EP - 108 PB - Elsevier AN - OPUS4-44880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eitzen, L. A1 - Paul, S. A1 - Braun, Ulrike A1 - Altmann, Korinna A1 - Jekel, M. A1 - Ruhl, A. T1 - The challenge in preparing particle suspensions for aquatic microplastic research N2 - The occurrence of small particles consisting of organic polymers, so-called microplastic (MP), in aquatic Environments attracts increasing interest in both public and science. Recent sampling campaigns in surface Waters revealed substantial numbers of particles in the size range from a few micrometers to a few millimeters. In order to validate sample preparation, identification and quantification and to investigate the behavior of MP particles and potential toxic effects on organisms, defined MP model particles are needed. Many studies use spherical compounds that probably behave differently compared to irregularly shaped MP found in environmental samples. However, preparation and handling of MP particles are challenging tasks and have been systematically investigated in the present study. Polystyrene (PS) as a commonly found polymer with a density slightly above that of water was selected as polymer type for milling and fractionation studies. A cryogenic ball mill proved to be practical and effective to produce particles in the size range from 1 to 200 μm. The yield of small particles increased with increasing pre-cooling and milling durations. Depending on the concentration and the size, PS particles do not completely disperse in water and particles partly creep vertically up along glass walls. Stabilized MP suspensions without use of surfactants that might harm organisms are needed for toxicological studies. The stabilization of PS particle suspensions with ozone treatment reduced the wall effect and increased the number of dispersed PS particles but increased the dissolved organic carbon concentration and changed the size Distribution of the particles. KW - Reference material KW - Microplastic PY - 2018 DO - https://doi.org/10.1016/j.envres.2018.09.008 SN - 0013-9351 SN - 1096-0953 VL - 168 SP - 490 EP - 495 PB - Elsevier AN - OPUS4-46462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanochemical Syntheses of Metal Phosphonates N2 - Mechanochemistry is a suitable method for synthesizing a variety of metal phosphonates. By varying the ratio of the reactants, it is possible to control the reaction pathway. With this approach targeted synthesis of a certain composition is possible. Several new metal phosphonate structures were solved from the powder X-ray diffraction data including molecular metal phosphonates. The results demonstrate a new fast, facile, and environmental friendly alternative for the preparation of metal phosphonates. In situ investigations of the milling processes provided insights into the formation process of metal phosphonates. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. T2 - 1st European Workshop on Metalphophantes CY - Swanse, UK DA - 18.09.2018 KW - Mechanochemistry PY - 2018 AN - OPUS4-46382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zauer, M. A1 - Prinz, Carsten A1 - Adolphs, J. A1 - Emmerling, Franziska A1 - Wagenführ, A. T1 - Sorption surfaces and energies of untreated and thermally modified wood evaluated by means of excess surface work (ESW) N2 - Water vapor sorption surface areas and sorption energies of untreated and thermally modified Norway spruce [Picea abies (L.) Karst.], sycamore maple (Acer pseudoplatanus L.) and European ash (Fraxinus excelcior L.) were investigated by means of dynamic vapor sorption (DVS) measurements and excess surface work (ESW) evaluation method, respectively. Adsorption and desorption experiments in the hygroscopic range and desorption tests from water saturation were conducted. Thermodynamically, ESW is the sum of the surface free energy and the isothermal isobaric work of sorption. From the amount adsorbed in the first Minimum a specific surface area similar to the BET surface area can be obtained. The results show that untreated spruce has a significantly higher specific water vapor Sorption surface and sorption energy compared to both hardwoods maple and ash. Thermal modification of the woods leads to a significant reduction of water vapor Sorption surface and sorption energy. The determined surface area and energy are higher in desorption direction than in adsorption direction, whereby the highest values in Desorption direction from water saturation, especially for maple and ash, were obtained. The surface areas calculated by means of the ESW method are similar to the surface areas calculated by means of the BET method, particularly in adsorption direction. KW - Excess surface work KW - Dynamic vapor sorption KW - Wood KW - BET PY - 2018 DO - https://doi.org/10.1007/s00226-018-1021-2 SN - 1432-5225 SN - 0043-7719 VL - 52 IS - 4 SP - 957 EP - 969 PB - Springer CY - Berlin Heidelberg AN - OPUS4-44975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline T1 - Optimierte Materialien und Verfahren zur Entfernung von Mikroplastik aus dem Wasserkreislauf N2 - Das Ziel dieses Projektes ist die Entwicklung neuer Materialien, um den Rückhalt von Mikroplastik-Partikeln (MP) aus verschiedenen urbanen Eintragspfaden (Kläranlagenablauf, Mischwasserüberlauf und Straßenabfluss)zu optimieren. Die im Rahmen des Projekts entwickelten Materialien sollten auf ihre Rückhaltefähigkeit von MP aus dem Kläranlagenklarlauf getestet werden. Für die Probenahme sowie für die Analytik wurden die entwickelten und optimierten Probenahme- sowie Analysetechniken angewendet. T2 - Konferenz der BMBF-Fördermaßnahme "MachWas-Materialien für die nachhaltige Wasserwirtschaft" CY - Frankfurt am Main, Germany DA - 29.05.2018 KW - Mikroplastik KW - TED-GC-MS KW - Mischwasser KW - Straßenablauf PY - 2018 AN - OPUS4-45043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Tagging reagents for imaging mass cytometry N2 - In der klinischen Diagnostik werden für zytometrische Messverfahren bereits eine Reihe von Reagenzien eingesetzt zur Markierung von Antikörper eingesetzt, um die Detektion von Biomarkern mittels Fluoreszenz- oder Flugzeitmassenspektrometrie zu ermöglichen. Seit kurzem ist auch eine Imaging Mass Cytometry Kombination direkt erhältlich, wodurch der Nachweis von Biomarkern in Gewebeschnitten erreicht werden kann. Dazu wird eine Kopplung von Laser Ablation und induktiv gekoppeltem Plasma Massenspektrometrie eingesetzt, wobei ähnlich der Massenzytometrie, zuvor Antikörper mit Metallen markiert, und im Anschluss mit dem Gewebeschnitt inkubiert werden. Durch die hohe Ortsauflösung können die Biomarker lokalisiert, und zukünftig vielleicht auch quantifiziert werden. Insbesondere Lanthanide eignen sich als Markierungsmetalle, da sie einen niedrigen Untergrund und chemisch ähnliches Verhalten zueinander aufweisen. Allein durch diese Elemente können bereits etwa 15 Parameter unterschieden werden, was durch isotopenreine Standards weiter gesteigert werden kann. Vom Markierungsgrad abhängig werden unterschiedlich viele Metalle am Antikörper gebunden, und beeinflussen so die Sichtbarkeit im ICP-MS. Nanopartikel könnten daher eine deutliche Steigerung der Sensitivität bewirken. GdVO4 Nanokristalle scheinen bisher sehr vielversprechend und bieten neben multiparametrischen Anwendungen auch Multimodalität. Die Synthese der Nanokristalle zeigte hohe Homogenität und Reproduzierbarkeit in Partikelgröße in der Zusammensetzung. Ein erstes Experiment mit einer Zellkultur konnte bereits die effiziente Markierung der Zellen unter Beweis stellen, wobei durch hohe Signalstärke auch subzelluläre Auflösung in der LA-ICP-MS erreicht werden konnte. T2 - ICPMS Anwendertreffen 2018 CY - Berlin, Germany DA - 03.09.2018 KW - LA-ICP-MS KW - Immuno assay KW - Bioimaging KW - Nanocrystal KW - Lanthanide KW - Metal-tag PY - 2018 AN - OPUS4-45866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - Mechanochemical Knoevenagel condensations of benzaldehyde derivates investigated in situ N2 - Mechanochemistry is widely applicable for the synthesis of inorganic, metal-organic, and organic compounds. It is known for short reaction times, nearly quantitative conversions, and decreasing amount of solvents, which opens the field to more environmentally friendly syntheses routes. Among organic syntheses, the Knoevenagel condensation is an important C-C bond forming reaction leading to α,β-unsaturated compounds. To gain more information on the underlying processes, we investigated the syntheses by a combination of different in situ investigation techniques, including synchrotron X-ray diffraction, Raman spectroscopy and thermography. This combination provides information on the structural changes and temperature influences during milling. Benzaldehyde derivates (nitro- and fluoro-derivates) reacted with malononitrile to the respective benzylidenemalononitriles. The in situ investigations show direct and quantitative conversions. In the case of the fluorinated benzaldehyde derivates we showed the possibility of using liquid substrates in mechanochemical organic synthesis. Surprisingly, after crystallization from a viscous state, the material was suitable for single-crystal X-ray analysis. T2 - Powder Diffraction School 2018 CY - Villigen, Switzerland DA - 24.09.2018 KW - C-C coupling KW - Mechanochemistry KW - In situ KW - Knoevenagel PY - 2018 AN - OPUS4-46320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Analyse von Reifenabrieb in Umweltproben mit der TED-GC-MS N2 - Im Vortrag wird erstmals präsentiert, dass die von der BAM entwickelte Methode TED-GC-MS sich auch zur Analyse von Reifenabrieb in Umweltproben eignet. T2 - Wassertagung der GdCh CY - Papenburg, Germany DA - 07.05.2018 KW - TED-GC-MS KW - Mikroplastik KW - Analytik KW - Reifenabrieb PY - 2018 AN - OPUS4-45200 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Detektion von Polymeren im Abwasser eines Klärwerks mittels TED-GC_MS N2 - In den Umweltmedien Wasser, Boden und Luft wird Mikroplastik (MP) gefunden. Mögliche Eintragspfade, besonders Einträge über den Klarlauf kommunaler Klärwerke, sind unklar. Dazu wurde das Klärwerk Ruhleben in Berlin an jeweils vier Tagen im Sommer- und Winterbetrieb beprobt. Es wurde jeweils 1 m3 Klarlauf fraktioniert filtriert (500, 100 und 50 µm Siebe). Weiterhin wurde Rohabwasser exemplarisch untersucht. Als Analyse-methoden wurden die TED-GC-MS und die FTIR Mikroskopie verwendet. Bei der TED-GC-MS wird die Probe zunächst thermisch extrahiert, bevor die charakteristischen Zersetzungsgase mittels einer GC-Säule getrennt und im MS detektiert werden [1,2]. Es ist hier erstmals gelungen, nicht nur das MP zu identi-fizieren, sondern auch eine Massenbilanz zu erstellen und so eine quantitative Auswertung vorzunehmen. Es wurde PE, PS ganzjährig und PP im Sommer gefunden. Das Klärwerk Ruhleben hat einen Rückhalt an MP von 99%. T2 - Wasser 2018 CY - Papenburg, Germany DA - 07.05.2018 KW - Mikroplastik KW - Abwasser KW - TED-GC-MS KW - Bilanzierung PY - 2018 AN - OPUS4-44889 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ investigations of a mechanochemical cocrystal formation by X-ray diffraction in two different milling jars N2 - We present an in situ PXRD investigation of the mechanochemical cocrystal formation of pyrazinamide with pimelic acid in two milling jar materials. DFT calculations of the two synthesized polymorphs suggest that the relative stability is based on a conformation change of pyrazinamide in the cocrystal. T2 - 3. BAM-BfR Workshop CY - Berlin, Adlershof, Germany DA - 15.02.2018 KW - Mechanochemistry KW - Cocrystal KW - Polymorph KW - In situ XRD KW - DFT PY - 2018 AN - OPUS4-44315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ monitoring of a mechanochemical Knoevenagel condensation N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Mechanochemistry KW - In situ KW - Knoevenagel condensation KW - C-C coupling PY - 2017 AN - OPUS4-44142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roy, Arkendu A1 - Kumar, Sourabh A1 - de Oliveira Guilherme Buzanich, Ana A1 - Prinz, Carsten A1 - Götz, Emilia A1 - Retzmann, Anika A1 - Hickel, Tilmann A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska T1 - Synergistic Catalytic Sites in High‐Entropy Metal Hydroxide Organic Framework for Oxygen Evolution Reaction N2 - AbstractThe integration of multiple elements in a high‐entropy state is crucial in the design of high‐performance, durable electrocatalysts. High‐entropy metal hydroxide organic frameworks (HE‐MHOFs) are synthesized under mild solvothermal conditions. This novel crystalline metal–organic framework (MOF) features a random, homogeneous distribution of cations within high‐entropy hydroxide layers. HE‐MHOF exhibits excellent electrocatalytic performance for the oxygen evolution reaction (OER), reaching a current density of 100 mA cm−2 at ≈1.64 VRHE, and demonstrates remarkable durability, maintaining a current density of 10 mA cm−2 for over 100 h. Notably, HE‐MHOF outperforms precious metal‐based electrocatalysts despite containing only ≈60% OER active metals. Ab initio calculations and operando X‐ray absorption spectroscopy (XAS) demonstrate that the high‐entropy catalyst contains active sites that facilitate a multifaceted OER mechanism. This study highlights the benefits of high‐entropy MOFs in developing noble metal‐free electrocatalysts, reducing reliance on precious metals, lowering metal loading (especially for Ni, Co, and Mn), and ultimately reducing costs for sustainable water electrolysis technologies. KW - Electrocatalysis KW - Green Hydrogen PY - 2024 DO - https://doi.org/10.1002/adma.202408114 SP - 1 EP - 14 PB - Wiley AN - OPUS4-61739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nag, Sayak A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska A1 - Ghosh, Soumyajit T1 - Stress and Light-Induced Dual Mechanical Properties of Two 1,3-Dicyanostilbene Derivative Crystals N2 - Dynamic molecular crystals with multistimuli responses hold immense potential for applications as actuators and smart materials. Here, we report two new 1,3-dicyanostilbene derivative crystals (crystals 1 and 2), which exhibit dual mechanical responses. Both crystals 1 and 2 demonstrate stress-induced mechanical flexibility and light-induced photomechanical bending upon exposure to a 375 nm UV LED. These two distinct mechanical responses are associated with different underlying phenomena and are independent of each other. Mechanical flexibility is attributed to the absence of slip planes and a criss-cross packing arrangement in an isotropic structure, while photomechanical bending is ascribed to the formation of a heterogeneous phase distribution due to Z → E photoisomerization. However, they show thermal reversibility, pointing toward a reversible E → Z back isomerization. This study demonstrates that single molecular crystals combining mechanical flexibility and photomechanical bending can be designed and fabricated for developing multistimuli responsive actuators. KW - Photoisomerization KW - Crystal structure KW - Crystals KW - Flexibility KW - Molecules PY - 2025 DO - https://doi.org/10.1021/acs.cgd.5c00097 SN - 1528-7483 SP - 1 EP - 11 PB - American Chemical Society (ACS) AN - OPUS4-63267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cirkovic Velickovic, T. A1 - Altmann, Korinna A1 - Dailey, L T1 - CUSP Conference WG1 & WG3: MATERIALS AND METHODS N2 - This talk is a presentation about the main results of the CUSP cluster on micro- and nanoplastics human health that work from 2021 to 2025 in Horizon Europe programme according to the WG1 and 3. These groups combined the analytics and the materials with interlaboratory comparisons (ILC). The talk reflects the need of realistic test materials with defined properties for micro- and nanoplastic research. Some were developed are now available. The talk also highlights the need for harmonisation and the results of different ILCs that were performed. T2 - CUSP conference CY - Brussels, Belgium DA - 25.02.2025 KW - Microplastics KW - Reference materials KW - Interlaboratory comparison (ILC) PY - 2025 AN - OPUS4-62703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -