TY - CONF A1 - Resch-Genger, Ute T1 - Standardization of Flourescence Measurements in the UV/VIS/NIR/IR at BAM N2 - Photoluminescence techniques are amongst the most widely used tools in the life sciences, with new and exciting applications in medical diagnostics and molecular imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are also time-dependent due to aging of instrument-components, and difficulties to measure absolute fluorescence intensities. Moreover, scattering systems require special measurement geometries and the interest in new optical reporters with emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material performance and the rational design of new fluorophores with improved properties. Here, we present strategies to versatile method-adaptable liquid and solid fluorescence standards for different fluorescence parameters. Examples are multi-emitter glasses, spectral fluorescence standards, and quantum yield standards for the UV/vis/NIR. T2 - Konsortiumtreffen Mikroskopie CY - Universität Münster, Germany DA - 20.01.2020 KW - Fluorescence standard KW - Instrument calibration KW - Integrating sphere spectroscopy KW - Fluorescence quantum yield KW - Fluorescent glasses KW - Fluorescence microscopy KW - Particle, imaging PY - 2020 AN - OPUS4-50308 LA - eng 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 - Lörchner, Dominique A1 - Tang, Ductri A1 - Mauch, Tatjana A1 - Jung, Christian A1 - Hofmann, Andrea A1 - Kroh, L.W. T1 - Development and validation of a liquid chromatography-mass spectrometry method for simultaneous analysis of triazine-based brominated flame retardants in environmental samples N2 - In the present study, a novel and reliable analytical method was developed and validated for the simultaneous determination of 1,3,5-tris(2,3-dibromopropyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (TDBP-TAZTO) and 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5-triazine (TTBP-TAZ) in environmental samples using high-performance liquid chromatography coupled to a tandem mass spectrometer. Firstly, for optimization of the liquid chromatography separation, mobile phases, oven temperatures, modifiers, and buffers were varied. Afterwards, the extraction efficiency of sediment and fish samples was tested with different techniques (pressurized liquid, solid-liquid, ultrasound-assisted, and Soxhlet extraction). Additionally, cleanup using modified multilayer silica gel (sediment) and gel permeation chromatography as well as Florisil® columns (fish) with several solvent mixtures were performed. The best results were obtained with the pressurized liquid extraction (optimal conditions: extraction solvent 100% toluene, extraction time 20 min, cycles two, extraction temperature 100 °C, and flushing volume 60%) compared to other solvent extraction methods. On the basis of this optimized analytical procedure, the method was validated with satisfactory values of correlation coefficient (R2) between 0.998 and 0.999 for both matrices in the calibration range of 2.0–502.0 μg kg−1 for TDBP-TAZTO and 16.6–770.6 μg kg−1 for TTBP-TAZ in sediment samples as well as 4.8–303.5 μg kg−1 and 47.4–742.5 μg kg−1 in fish samples (bream), respectively.Mean recoveries (n=5) were calculated for both analytes with spiked matrices at one concentration level (100 μg kg−1) between 98 and 114% with intra-day relative standard deviations less than 11%. The inter-day precision (n = 15) was also acceptable for both compounds < 11%. It was found that the limit of detection and limit of quantification were in the range of 0.4–1.3 μg kg−1 for TDBP-TAZTO and 10–28 μg kg−1 for TTBP-TAZ in surface sediment samples and 7–25 μg kg−1 and 22–80 μg kg−1 in fish samples (bream), respectively. The results indicated that these analytical methods could provide reliable and efficient approaches for quantification of TDBP-TAZTO and TTBPTAZ in sediment and fish samples. KW - Brominated flame retardants KW - Pressurized liquid extraction KW - TDBP-TAZTO KW - TTBP-TAZ KW - Sediment and fish samples PY - 2020 DO - https://doi.org/10.1007/s00216-020-03057-x VL - 413 IS - 4 SP - 987 EP - 998 PB - Springer AN - OPUS4-51685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Transport von defekten Lithiumbatterien: Umsetzungspraxis der neuen Rechtsvorschriften, Wo besteht Forschungsbedarf? N2 - Transport von defekten Lithiumbatterien - die BAM setzt die Vorschriften des internationalen Gefahrguttransportrechts für defekte Lithiumbatterien um. Um die Kompetenz hierfür sicherzustellen, bedarf es eigener Forschungstätigkeit. Auch im zuständigen UN Gremium werden Untersuchungen durchgeführt, an denen die BAM beteiligt ist. T2 - Fachkonferenz Lithiumbatterien CY - Göttingen, Germany DA - 22.01.2020 KW - Lithiumbatterien KW - Gefahrguttransport KW - ADR PY - 2020 AN - OPUS4-50806 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Mirtsch, Mona A1 - Koch, Claudia A1 - Dudek, Gabriele A1 - Blind, K. T1 - Die Nutzung und Wirkung genormter Managementsysteme N2 - Das Ziel der Initiative QI-FoKuS ist es, eine Datenbasis für neue wissenschaftliche Erkenntnisse zu Einflussfaktoren und Effekten in der Konformitätsbewertung und Akkreditierung zu schaffen. Ende 2019 wurden in einer ersten Online-Erhebung Unternehmen verschiedener Branchen und Größenklassen in Deutschland zur Nutzung von Managementsystemen und ihren Wirkungen befragt. Diese umfasste weit verbreitete genormte Managementsysteme wie ISO 9001 und ISO 14001 genauso wie bisher wenig untersuchte Systeme wie die ISO 50001 oder ISO/IEC 27001. Es konnten 180 Fragebögen für die vorliegende Studie ausgewertet werden. KW - QI-FoKuS KW - Managementsysteme KW - ISO 9001 KW - ISO/IEC 27001 KW - ISO 50001 KW - ISO 14001 KW - Zertifizierung KW - Konformitätsbewertung KW - Akkreditierung PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510831 SN - 978-3-9818564-3-9 DO - https://doi.org/10.26272/opus4-51083 VL - 1 SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51083 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Marc Benjamin T1 - Temperature effects in the Object Oriented Micromagnetic Framework (OOMMF) - OOMMF input parameter files for Tc determination N2 - To simulate the movement of the macroscopic magnetic moment in ferromagnetic systems under the influence of elevated temperatures, the stochastic version of the Landau-Lifshitz (LL) or the Landau-Lifshitz-Gilbert equation with a spin density of one per unit cell has to be used. To apply the stochastic LL to micromagnetic simulations, where the spin density per unit cell is generally higher, a conversion has to be performed. OOMMF sample files MIF) are provided which can be used to determine the Curie temperature for the classical bulk magnets, iron, nickel and cobalt. KW - OOMMF KW - Temperature KW - Micromagnetism KW - Thetaevolve KW - Ferromagnetism KW - Exchange interaction KW - LLG KW - Landau Lifshitz equation KW - Magnetic moment KW - Magnetic nanoparticles KW - Object oriented micromagnetic framework KW - Stochastic Landau Lifshitz Gilbert equation KW - Temperature scaling PY - 2020 DO - https://doi.org/10.26272/opus4-51169 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Marc Benjamin T1 - TOPAS cell model with nanoparticles N2 - These files contain cell models for TOPAS/Geant4 and the inclusion of nano particles in particle scattering simulations. A simple spherical cell with nanoparticles can be generated in a fast manner. The user has the option to include the following organelles: nucleus, mitochondria, cell membrane. Additionally nanoparticles can be included in the cytosol and at the surface of the nucleus and/or the mitochondria. The C++ classes in this repository extend the functionality of the TOPAS (http://www.topasmc.org/) Monte-Carlo program, which is itself a wrapper of the Geant4 MCS Toolkit (http://geant4.org). The sourcecode together with examples and scorers are provided. "If you use this extension please cite the following literature: Hahn, M.B., Zutta Villate, J.M. "Combined cell and nanoparticle models for TOPAS to study radiation dose enhancement in cell organelles." Sci Rep 11, 6721 (2021). https://doi.org/10.1038/s41598-021-85964-2 " KW - Monte-Carlo simulation KW - MCS KW - Geant4 KW - TOPAS KW - TOPAS-nBio KW - Dosimetry KW - Nanoparticles KW - Nanoparticle KW - AuNP KW - Gold KW - Microdosimetry KW - Targeted nanoparticle KW - Simulation KW - Particle scattering KW - Cell KW - Nucleus KW - Mitochondria KW - Cancer therapy KW - Radiation therapy PY - 2020 UR - https://github.com/BAMresearch/TOPAS-CellModels UR - https://github.com/MarcBHahn/TOPAS-CellModels DO - https://doi.org/10.26272/opus4-51150 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Mirtsch, Mona A1 - Koch, Claudia A1 - Dudek, Gabriele A1 - Blind, K. T1 - Die Nutzung und Wirkung der Norm ISO/IEC 27001 für Informationssicherheit in Unternehmen in Deutschland N2 - Das Ziel der Initiative QI-FoKuS ist es, eine Datenbasis für neue wissenschaftliche Erkenntnisse zu Einflussfaktoren und Effekten in der Konformitätsbewertung und Akkreditierung zu schaffen und hierbei insbesondere auch auf aktuelle Trends und Entwicklungen einzugehen. Von Januar bis März 2020 wurden in einer Online-Erhebung Unternehmen verschiedener Branchen und Größenklassen in Deutschland zur Nutzung und den Wirkungen ihres zertifizierten Managementsystems für Informationssicherheit nach ISO/IEC 27001 befragt. Es konnten 125 vollständig ausgefüllte Fragebögen für die vorliegende Studie ausgewertet werden. KW - Managementsysteme KW - ISO/IEC 27001 KW - Informationssicherheit KW - Zertifizierung KW - Konformitätsbewertung KW - Akkreditierung KW - QI-FoKuS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517922 DO - https://doi.org/10.26272/opus4-51792 VL - 2 SP - 1 EP - 28 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51792 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Mirtsch, Mona A1 - Blind, K. T1 - CORONA-MONITOR - Auswirkungen der Corona-Pandemie auf Konformitätsbewertung und Konformitätsbewertungsstellen in Deutschland N2 - Die Studie fasst Ergebnisse einer Befragung von Konformitätsbewertungsstellen zu deren Lage und den Aussichten während der Corona-Pandemie zusammen. Besondere Schwerpunkte wurden auf die wirtschaftlichen Auswirkungen und die Arbeitsfähigkeit, aber auch auf die Resilienz und die Wirkungen auf die Digitalisierung gelegt. KW - Corona KW - COVID-19 KW - Resilienz KW - Qualitätsinfrastruktur KW - Prüfung KW - Zertifizierung KW - Kalibrierung KW - Inspektion KW - Labor KW - Laboratorium KW - Studie KW - Befragung KW - Digitalisierung PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518276 UR - www.qi-fokus.de DO - https://doi.org/10.26272/opus4-51827 VL - 3 SP - 1 EP - 26 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51827 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Voss, L. A1 - Hsiao, I-L. A1 - Ebisch, Maximilian A1 - Vidmar, J. A1 - Dreiack, N. A1 - Böhmert, L. A1 - Stock, V. A1 - Braeuning, A. A1 - Loeschner, K. A1 - Laux, P. A1 - Thünemann, Andreas A1 - Lampen, A. A1 - Sieg, H. T1 - The presence of iron oxide nanoparticles in the food pigment E172 N2 - Iron oxides used as food colorants are listed in the European Union with the number E172. However, there are no specifications concerning the fraction of nanoparticles in these pigments. Here, seven E172 products were thoroughly characterized. Samples of all colors were analyzed with a Broad spectrum of methods to assess their physico-chemical properties. Small-Angle X-ray Scattering (SAXS), Dynamic Light Scattering (DLS), Transmission Electron Microscopy (TEM), zeta-potential, Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), X-ray diffraction (XRD), Brunauer-Emmett-Teller analysis (BET), Asymmetric Flow Field-Flow Fractionation (AF4) and in vitro cell viability measurements were used. Nanoparticles were detected in all E172 samples by TEM or SAXS measurements. Quantitative results from both methods were comparable. Five pigments were evaluated by TEM, of which four had a size median below 100 nm, while SAXS showed a size median below 100 nm for six evaluated pigments. Therefore, consumers May be exposed to iron oxide nanoparticles through the consumption of food pigments. KW - SAXS KW - Small-angle X-ray scattering KW - Nanoparticle PY - 2020 DO - https://doi.org/10.1016/j.foodchem.2020.127000 VL - 327 SP - 127000 PB - Elsevier Ltd. AN - OPUS4-50810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thöns, Sebastian A1 - Stewart, M. G. T1 - On the cost-efficiency, significance and effectiveness of terrorism risk reduction strategies for buildings N2 - We analyse the performance of risk reduction strategies for Terrorist attacks with Improvised Explosive Devices (IEDs) for large governmental building structures in terms of cost-efficiency, significance and effectiveness Accounting for life safety in conjunction with societal preferences and capabilities. The approach builds upon an extended Bayesian pre-posterior decision analysis and the principles of the marginal lifesaving costs based on the Life Quality Index (LQI). The decision scenario is formulated for a decision maker responsible for the safety of governmental or large commercial buildings and consequently the direct risks, the indirect risks due to fatalities and economical importance of the building beside the expected cost for the individual risk reduction strategies are modelled, aggregated and optimised. The considered risk reduction strategies encompass an explicit consideration and distinction of information and actions such as (i) threat surveillance may trigger the temporary evacuation of the building, (ii) the implementation of protection provisions provided by codes and guidelines, (iii) a detailed progressive collapse assessment and specific protection measures and (iv) the combination of protection and surveillance. All considered strategies are found to contribute to risk reduction and can be costefficient, especially for higher threat probabilities. The risk reduction strategies comply with societal macroeconomic and demographical characteristics and societal preferences according to the LQI. The progressive collapse assessment with targeted protection measures is found to be the most cost-efficient, significant and effective counter-terrorism strategy. This finding points to the necessity for a comprehensive utilisation of scientific methods and sophisticated engineering for progressive collapse assessment to determine targeted protection measures. KW - Significance and effectiveness KW - Risk mitigation strategies KW - Terrorist attacks KW - Value of information KW - Bayesian probability KW - Reliability KW - Risk and decision analysis KW - Decision optimality PY - 2020 DO - https://doi.org/10.1016/j.strusafe.2020.101957 VL - 85 SP - 10195 PB - Elsevier Ltd. AN - OPUS4-50794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Voss, L. A1 - Saloga, Patrick E. J. A1 - Stock, V. A1 - Böhmert, L. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Lampen, A. A1 - Sieg, H. T1 - Correction to "Environmental impact of ZnO nanoparticles evaluated by in vitro simulated digestion" N2 - This is a corrigendum to the original article "Environmental impact of ZnO nanoparticles evaluated by in vitro simulated digestion" that was published in the journal "ACS Applied Nano Materials", vol. 3 (2020), no. 1, pp. 724-733. PY - 2020 DO - https://doi.org/10.1021/acsanm.0c01054 VL - 3 IS - 5 SP - 4914 EP - 4914 PB - American Chemical Society CY - Washington, D.C., USA AN - OPUS4-50812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieg, H. A1 - Krause, B.-C. A1 - Kästner, Claudia A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Tentschert, J. A1 - Jungnickel, H. A1 - Laux, P. A1 - Braeuning, A. A1 - Fessard, V. A1 - Thünemann, Andreas A1 - Luch, A. A1 - Lampen, A. T1 - Cellular Effects of In Vitro-Digested Aluminum Nanomaterials on Human Intestinal Cells N2 - Aluminum (Al) can be taken up from food, packaging, or the environment and thus reaches the human gastrointestinal tract. Its toxic potential after oral uptake is still discussed. The fate of different solid and ionic Al species during the passage through the digestive tract is the focus of this research, as well as the cellular effects caused by these different Al species. The present study combines the physicochemical processing of three recently studied Al species (metallic Al0, mineral Al2O3, and soluble AlCl3) in artificial digestion fluids with in vitro cell systems for the human intestinal barrier. Inductively coupled plasma mass spectrometry (ICP-MS) and small-angle X-ray scattering (SAXS) methods were used to characterize the Al species in the artificial digestion fluids and in cell culture medium for proliferating and differentiated intestinal Caco-2 cells. Cytotoxicity testing and cellular impedance measurements were applied to address the effects of digested Al species on cell viability and cell proliferation. Microarray-based transcriptome analyses and quantitative real-time PCR were conducted to obtain a deeper insight into cellular mechanisms of action and generated indications for cellular oxidative stress and an influence on xenobiotic metabolism, connected with alterations in associated signaling pathways. These cellular responses, which were predominantly caused by formerly ionic Al species and only at very high concentrations, were not impacted by artificial digestion. A two-directional conversion of Al between ionic species and solid particles occurred throughout all segments of the gastrointestinal tract, as evidenced by the presence of nanoscaled particles. Nevertheless, this presence did not increase the toxicity of the respective Al species. KW - SAXS KW - Small-angle X-ray scattering KW - Nanoparticle PY - 2020 DO - https://doi.org/10.1021/acsanm.9b02354 VL - 3 IS - 3 SP - 2246 EP - 2256 PB - American Chemical Society AN - OPUS4-50632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Voss, L. A1 - Saloga, Patrick E. J. A1 - Stock, V. A1 - Böhmert, L. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Lampen, A. A1 - Sieg, H. T1 - Environmental impact of ZnO nanoparticles evaluated by in vitro simulated digestion N2 - ZnO nanoparticles are found in different food and consumer products, and their toxicological effects are still under investigation. It is therefore important to understand their behavior in the gastrointestinal tract. Here, we used an in vitro model to assess the physicochemical fate of ZnO nanoparticles during the digestive process in artificial saliva, stomach juice, and intestinal juice. Atomic absorption spectrometry and small-angle X-ray scattering were employed to investigate two ZnO nanomaterials, one intensively characterized reference material and soluble ZnCl2 in a broad range of concentrations between 25 and 1000 μg/mL in the intestinal fluid. Because food components may influence the behavior of nanomaterials in the gastrointestinal tract, starch, milk powder, and olive oil were used to mimic carbohydrates, protein, and fat, respectively. Additionally, ion release of all Zn species was assessed in cell culture media and compared to artificial intestinal juice to investigate relevance of typical cell culture conditions in ZnO nanotoxicology. ZnCl2 as well as the ZnO species were present as particles in artificial saliva but were solubilized completely in the acidic stomach juice. Interestingly, in the intestinal fluid a concentration-independent de novo formation of particles in the nanoscale range was shown. This was the case for all particles as well as for ZnCl2, regardless of the concentration used. Neither of the food components affected the behavior of any Zn species. On the contrary, all Zn species showed a Zn-concentration-dependent ion release in common cell culture medium. This questions the suitability of cell culture studies to investigate the effect of ZnO nanoparticles on intestinal cells. Our results show that Zn-containing nanoparticles reach the intestine. This underlines the importance of determining the influence of the test environment on nanoparticle fate. KW - SAXS KW - Digestion KW - Zinc oxide KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acsanm.9b02236 VL - 3 IS - 1 SP - 724 EP - 733 AN - OPUS4-50288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, W.-H. A1 - Qin, J. A1 - Lu, D.-G. A1 - Thöns, Sebastian A1 - Havbro Faber, M. T1 - Vol-informed decision-making for SHM system arrangement N2 - Structural health monitoring systems have been widely implemented to provide real-time continuous data support and to ensure structural safety in the context of structural integrity management. However, the quantification of the potential benefits of structural health monitoring systems has not yet attracted widespread attention. At the same time, there is an urgent need to develop strategies, such as optimizing the monitoring period, monitoring variables, and other factors, to maximize the potential benefits of structural health monitoring systems. Considering the continuity of structural health monitoring information, a framework is developed in this article to support decision-making for structural Health monitoring systems arrangement in the context of structural integrity management, which integrates the concepts of value of information and risk-based inspection planning based on an approach which utilizes a conjugate prior probability distribution for updating of the probabilistic models of structural performances based on structural health Monitoring information. An example considering fatigue degradation of steel structures is investigated to illustrate the application of the proposed framework. The considered example shows that the choice of monitoring variables, the Monitoring period, and the monitoring quality may be consistently optimized by the application of the proposed framework and approach. Finally, discussions and conclusions are provided to clarify the potential benefits of the proposed Framework with a special view to practical applications of structural health monitoring systems. KW - Value of information KW - Structural health monitoring systems arrangement strategy KW - Structural integrity management KW - Rskbased inspection KW - Structural health monitoring information model PY - 2020 DO - https://doi.org/10.1177/1475921720962736 SN - 1475-9217 VL - 21 IS - 1 SP - 37 EP - 58 PB - SAGE Journals CY - USA AN - OPUS4-53064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Lapalus, Antoin A1 - Tiebe, Carlo A1 - Bartholmai, Matthias T1 - Design and Implementation of Smart Multisensor Monitoring System for Safe Workplaces with LoRaWAN N2 - This project addresses the application of safe workplaces in offices and chemical laboratories where indoor air quality plays an important role. The LoRaWAN (Long Range Wide Area Network) is used as a communication interface to make important sensor data globally accessible. The goal of the development is to create a sensor node and an online and offline solution that collects the data from the sensor nodes and stores it on a local server or in a cloud. In cooperation with the companies WISTA GmbH and IONOS, a test sensor network is going to be established in the Berlin-Adlershof area. T2 - SMSI 2020 CY - Meeting was canceled DA - 22.06.2020 KW - Smart sensors KW - Air quality monitoring KW - LoRaWAN KW - VOC KW - Multisensor system PY - 2020 DO - https://doi.org/10.5162/SMSI2020/E5.4 SP - 388 EP - 389 AN - OPUS4-50878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eberwein, Robert T1 - Untersuchung der Gefährdung von Personen und Bauwerken in Folge des Versagens von LNG-Kraftstoffspeichern für Fahrzeuge in Tunneln N2 - Der Markt von LNG als Transportgut und als Kraftstoff ist seit Jahrzehnten kontinuierlich am Wachsen, wobei das Hauptanwendungsgebiet im Schiffsverkehr lag. LNG ist verflüssigtes Erdgas mit Hauptbestandteil Methan, das neben fossilen, aus erneuerbaren Quellen, wie synthetischen Methan oder Biogas, gewonnen werden kann. LNG hat als Kraftstoff sehr gute Eigenschaften dessen Potenzial als alternativer Kraftstoff zu Diesel im Schwerlast- und Fernverkehr gesehen wird. Dabei weist LNG gegenüber Diesel geringere Emissionen von CO2, Feinstaub, Stickoxiden und Lärm auf und hat gegenüber anderen erneuerbaren Energiespeichern wie CNG, Elektrobatterien oder Wasserstoff die höchste volumetrische und zweitgrößte gravimetrische Energiedichte. Neben seinen Vorteilen zu anderen erneuerbaren Energieträgern birgt LNG durch seine sehr niedrige Temperatur von bis zu 160°C und seiner Brennbarkeit aber auch neue Gefahren für Personen und Infrastrukturen. Zur Bewertung von Gefahren und zur späteren Durchführung von Risikobewertungen bedarf es Methoden und Modellen deren Untersuchung Ziel des Forschungsprojekts war. Schwerpunkt der Untersuchung stellt die Freisetzung von LNG in Tunnel, mit sich anschließender Stoffausbreitung und verzögerter Zündung des Kraftstoff-Luftgemisches dar. Unfallszenarien mit Brandereignissen in Tunnel haben gezeigt, dass diese meist mit hohen Personen, Bauwerks und volkswirtschaftlichen Schäden verbunden sind. Des Weiteren zeigten Untersuchungen das von Gasexplosionen in Umschließungen wie sie ein Tunnel darstellt, mehr Gefahren ausgehen als von Gasexplosionen im Freifeld. Im Vortrag werden die untersuchten Modelle und die aus dem Projekt gewonnenen Erkenntnisse für die Stoffausbreitung und Verbrennung der Gasphase von LNG in Umschließungen vorgestellt. T2 - Abteilungs-Vortragsseminar-Doktoranden CY - BAM Berlin, Germany DA - 08.12.2020 KW - LNG KW - Erdgas KW - Störfall KW - CFD KW - Schwergas PY - 2020 AN - OPUS4-51959 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza T1 - A model for grain boundary thermodynamics N2 - Systematic microstructure design requires reliable thermodynamic descriptions of each and all microstructure elements. While such descriptions are well established for most bulk phases, thermodynamic assessment of microstructure defects is challenging because of their individualistic nature. In this paper, a model is devised for assessing grain boundary thermodynamics based on available bulk thermodynamic data. We propose a continuous relative atomic density field and its spatial gradients to describe the grain boundary region with reference to the homogeneous bulk and derive the grain boundary Gibbs free energy functional. The grain boundary segregation isotherm and phase diagram are computed for a regular binary solid solution, and qualitatively benchmarked for the Pt–Au system. The relationships between the grain boundary's atomic density, excess free volume, and misorientation angle are discussed. Combining the current density-based model with available bulk thermodynamic databases enables constructing databases, phase diagrams, and segregation isotherms for grain boundaries, opening possibilities for studying and designing heterogeneous microstructures. KW - Phase Diagram KW - Thermodynamics KW - Grain boundary PY - 2020 VL - 10 IS - 45 SP - 26728 EP - 26741 AN - OPUS4-51268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fedelich, Bernard T1 - Untersuchung des Kriechverhaltens einer Nickelbasis-Superlegierung bei ultrahohen homologen Temperaturen und Anwendung auf das heiß-isostatische Pressen (HIP) N2 - Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird. Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert. T2 - Langzeitverhalten warmfester Stähle und Hochtemperaturwerkstoffe CY - Online meeting DA - 27.11.2020 KW - HIP KW - Superlegierung KW - Kriechen PY - 2020 AN - OPUS4-51795 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Mechanical behaviour of AM metals: Creep of LPBF 316L and low-cycle-fatigue of LMD Ti-6Al-4V N2 - Additively manufactured metallic materials have already started to find application in safety-relevant components. However, this has only happened for certain materials and specific applications and loading conditions, since there is still an extensive lack of knowledge as well as of historical data regarding their mechanical behaviour. This contribution aims to address this lack of understanding and historical data concerning the creep behaviour of the austenitic stainless steel 316L manufactured by Laser-Powder-Bed-Fusion (L-PBF) and the low-cycle-fatigue behaviour of the titanium alloy Ti-6Al-4V manufactured by Laser-Metal-Deposition (LMD). Furthermore, it aims to assess their mechanical behaviour against their conventional counterparts. With that in mind, specimens from conventional and additive materials are tested and their mechanical behaviour analysed based on characteristic curves. To understand the damage behaviours the materials are characterized by destructive and non-destructive techniques before and after failure. T2 - 1st Workshop on In-situ Monitoring and Microstructure Development in Additive Manufacturing CY - Online Meeting DA - 10.12.2020 KW - Ti-6Al-4V KW - 316L KW - Additive manufacturing KW - Creep behaviour KW - Low-cycle-fatigue behaviour PY - 2020 AN - OPUS4-51879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mair, Georg W. T1 - BAM - Bundesanstalt für Materialforschung und -prüfung: Hydrogen - Safety in Technology and Chemistry N2 - The presentation starts with some key figures about BAM. Then it introduces BAM's competence centre H2Safety@BAM and shows aspects of special competence of the centre. It closes with information about the engagement of BAM in European research projects on hydrogen and a reference to our bilingual paper about our hydrogen strategy. T2 - 27th Hydrogen Europe Research General Assembly CY - Online meeting DA - 02.07.2020 KW - Material properties and compatibility KW - Component testing KW - Safety assessment KW - Approval KW - Sensors KW - Inspection KW - Gas behaviour KW - Safe handling PY - 2020 AN - OPUS4-53155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holtappels, Kai T1 - Hydrogen - Trust through safety N2 - In den Virtual Talks der DECHEMA wurden allgemeine Aspekte der Sicherheit und Akzeptanz von Wasserstofftechnologien vorgestellt. Wie kann Vertrauen in neue Technologien geschaffen werden, wenn Unfälle aus der Vergangenheit zu Mythen und Märchen führten? Der Vortrag räumt mit allgemeinen Vorurteilen auf und zeigt, dass der Umgang mit Wasserstoff weder unsicherer, noch sicherer ist als der Umgang mit anderen Brenngasen. Basis für den sicheren Umgang mit Wasserstoff ist immer eine Risikoanalyse. N2 - In the DECHEMA Virtual Talks, general aspects of the safety and acceptance of hydrogen technologies were presented. How can trust in new technologies be built when past accidents led to myths and fairy tales? The presentation does away with general prejudices and shows that handling hydrogen is neither more unsafe nor safer than handling other fuel gases. The basis for the safe handling of hydrogen is always a risk analysis. T2 - DECHEMA Virtual Talks CY - Online meeting DA - 23.11.2020 KW - Hydrogen KW - Wasserstoff KW - Safety KW - Sicherer Umgang KW - Sicherheit PY - 2020 AN - OPUS4-52082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Richter, Tim A1 - Mayr, P. A1 - Nitsche, A. A1 - Mente, Tobias A1 - Böllinghaus, Thomas T1 - Hydrogen diffusion in creep-resistant 9% Cr P91 multi-layer weld metal N2 - Welded components of P91 9% Cr steel demand for careful welding fabrication with necessary post weld heat treatment (PWHT). Before the PWHT, a hydrogen removal heat treatment is necessary for avoidance of hydrogen assisted cracking (HAC). In this context, the microstructure and temperature-dependent hydrogen diffusion is important, and reliable diffusion coefficients of P91 weld metal are rare. For that reason, the diffusion behavior of P91 multi-layer weld metal was investigated for as-welded (AW) and PWHT condition by electrochemical permeation experiments at room temperature and carrier gas hot extraction (CGHE) from 100 to 400 °C. Hydrogen diffusion coefficients were calculated, and the corresponding hydrogen concentration was measured. It was ascertained that both heat treatment conditions show significant differences. At room temperature the AW condition showed significant hydrogen trapping expressed by to seven times lower diffusion coefficients. A preferred diffusion direction was found in perpendicular direction expressed by high permeability. The CGHE experiments revealed lower diffusion coefficients for the AW condition up to 400 °C. In this context, a hydrogen concentration of approximately 21 ml/100 g was still trapped at 100 °C. For that reason, a certain HAC susceptibility of as-welded P91 weld metal cannot be excluded, and hydrogen removal should be done before PWHT. KW - Creep resisting materials KW - Diffusion KW - Hydrogen KW - Weld metal KW - Post weld heat treatment KW - Microstructure PY - 2020 DO - https://doi.org/10.1007/s40194-019-00828-8 SN - 0043-2288 VL - 64 IS - 2 SP - 267 EP - 281 PB - Springer AN - OPUS4-50471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kauffeld, M. A1 - Maurath, T. A1 - Germanus, J. A1 - Askar, Enis T1 - N2O/CO2-Gemische als Kältemittel für Temperaturen unter -50 °C N2 - Die F-Gas-Verordnung der EU gewährt Ausnahmen vom GWPbezogenen Verbot des Inverkehrbringens für stationäre Kühlgeräte für Anwendungen unter -50 °C. Brennbare Alternativen auf der Basis von Methan, Ethan und Ethylen stehen zur Verfügung, sind aber aufgrund ihrer Entzündbarkeit nicht für alle Anwendungen einsetzbar. Distickstoffmonoxid (N2O) mit einem Tripelpunkt bei -92 °C scheint aber eine Alternative zu sein. Die mögliche exotherme Zersetzung von N2O erfordert jedoch zusätzliche Maßnahmen, um solche Systeme sicher betreiben zu können. Am ILK und an der Hochschule Karlsruhe wurden zwei Tieftemperatursysteme mit Gemischen aus N2O und CO2 und verschiedenen Schmierstoffen entwickelt, gebaut und bei Verdampfungstemperaturen bis -80 °C erfolgreich betrieben. VORSICHT: Reines N2O sowie Mischungen von N2O und CO2 mit Schmiermitteln auf Kohlenwasserstoffbasis können explosionsartig reagieren. KW - Kohlendioxid KW - Gefriertrocknung KW - Distickstoffmonoxid KW - Sicherheitsmaßnahmen PY - 2020 VL - 56 IS - 11 SP - 41 EP - 46 PB - Hüthig GmbH CY - Heidelberg AN - OPUS4-51748 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - Wasserstoffsicherheitsfragen - Sicherheitstechnische Kenngrößen von Wasserstoff und Gemischen von Wasserstoff mit Erdgas N2 - Wasserstoff unterscheidet sich hinsichtlich der sicherheitstechnischen Eigenschaften von anderen brennbaren Gassen, v.a. durch die sehr niedrige Mindestzündenergie und die sehr hohe Flammengeschwindigkeit. Durch Beimischung von Wasserstoff zum Erdgas ändern sich die sicherheitstechnischen Eigenschaften zum Teil in kritischer Richtung. Bis zu einem Wasserstoffanteil von 10 Mol-% im Erdgas ist aber keine wesentliche Anpassung der Maßnahmen für den Explosionsschutz erforderlich. Synthesgas ist ein weiteres Wasserstoffgemisch das in Zukunft vermutlich zunehmend relevant sein wird. Die beiden Komponenten Wasserstoff und Kohlenmonoxid haben zwar in mancher Hinsicht ähnliche sicherheitstechnische Eigenschaften unterscheiden sich aber auch sehr stark bzgl. der Mindestzündenergie und der Flammengeschwindigkeit. T2 - 9. HYPOS-Dialog: Grüner Wasserstoff, aber sicher! - Sicherheitsaspekte im Umgang mit Wasserstoff CY - Magdeburg, Germany DA - 11.09.2020 KW - Explosionsschutz KW - Zündenergie KW - Explosionsgrenzen KW - Zündquellen KW - Synthesegas PY - 2020 AN - OPUS4-51264 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Askar, Enis A1 - Aksam, A. A1 - Brandes, E. A1 - Markus, D. A1 - Stolz, T. T1 - Berechnung der Explosionsbereiche von Alkoholen, Ketonen und halogenierten Kohlenwasserstoffen im Gemisch mit Inertgasen N2 - Die Explosionsbereiche für Dreistoffsysteme aus Brennstoff Inertgas und Luft wurden nach dem Modell der konstanten adiabatischen Flammentemperaturprofile berechnet. Für die Parametrisierung des halbempirischen Modells muss der Explosionsbereich für ein bestimmtes Dreistoffsystem aus Brennstoff, Inertgas und Luft bekannt sein. Dann lassen sich Explosionsbereiche desselben Brennstoffs mit einem beliebigen Inertgas und bei einer beliebigen Temperatur berechnen. Ergänzend zu früheren Arbeiten, in denen die Explosionsbereiche für Brenngase aus der homologen Reihe der Alkane und Alkene berechnet worden sind, wurden nun die Berechnungen für 1-Propanol, Aceton und Difluormethan durchgeführt. Als Inertgase wurden neben Stickstoff und Kohlendioxid auch die Edelgase Argon und Helium berücksichtigt. Für die Berechnung der Explosionsbereiche in Systemen mit Helium, ist das Modell erweitert worden, so dass auch die Transporteigenschaften (d.h. Wärmeleitfähigkeit, Diffusionskoeffizient) der Komponenten berücksichtigt werden. Weiterhin ist eine Möglichkeit zur praxisnahen Berechnung der Spitze des Explosionsbereichs implementiert worden. Die Ergebnisse zeigen insgesamt, dass die Berechnung der Explosionsbereiche für Alkohole, Ketone und halogenierte Kohlenwasserstoffe mit ähnlicher Genauigkeit wie für Alkane und Alkene möglich ist. Die vorgenommenen Modifikationen sind geeignet, um auch eine Berechnung für Gasgemische mit Helium durchzuführen, dessen starke inertisierende Wirkung im Vergleich zu den Inertgasen Argon oder Stickstoff vor allem auf den stark unterschiedlichen Transporteigenschaften beruht. KW - Explosionsgrenzen KW - Inertisierung KW - Modell der konstanten Flammentemperaturen KW - Explosionsschutz PY - 2020 DO - https://doi.org/10.7795/310.20200199 SN - 0030-834X VL - 130 IS - 1 SP - 25 EP - 29 AN - OPUS4-50945 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Askar, Enis A1 - Kauffeld, M. A1 - Maurath, T. A1 - Germanus, J. T1 - N2O/CO2-mixtures as refrigerants for temperatures below -50 °C N2 - The EU F-Gas Regulation grants exceptions from the GWP-related placing on the market prohibition for stationary refrigeration equipment for applications below -50 °C. Nonetheless, non-flammable refrigerants, which can be used for that temperature range, become increasingly expensive and rare inside the EU due to the phase down of HFCs under the regulation. Flammable alternatives based on methane, ethane and ethylene are available, but are not viable for all applications due to their flammability. Carbon dioxide cannot be used for applications below -50 °C due to CO 2 ’s triple point at -56 °C. Nitrous oxide with a triple point at -92 °C seems to be an alternative. However, possible exothermal decomposition of N 2 O calls for additional measures in order to be able to operate such systems safely. Two low-temperature systems have been developed, built and successfully operated at evaporation temperatures down to - 80 °C with mixtures of N 2 O and CO 2 and different lubricants at ILK and Karlsruhe University of Applied Sciences. The units achieved similar energy efficiency as the standard HFC-equipment used for freeze drying. Possible decomposition of N 2 O could successfully be supressed by various measures. KW - Carbon dioxide KW - Freeze-dryer KW - Low temperature KW - Nitrous oxide KW - Safety measures PY - 2020 DO - https://doi.org/10.1016/j.ijrefrig.2020.04.026 SN - 0140-7007 VL - 117 SP - 316 EP - 327 PB - Elsevier Ltd. AN - OPUS4-50946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Michaelis, Matthias A1 - Prinz, Carsten A1 - Würth, Christian T1 - Time-resolved luminescence spectroscopy for monitoring the stability and dissolution behaviour of upconverting nanocrystals with different surface coatings† N2 - We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs. KW - Fluorescence KW - Lifetime KW - Method KW - Quantification KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Fluoride KW - Electrochemistry KW - ICP-OES KW - Upconversion KW - Nano KW - Particle KW - Aging KW - Quality assurance KW - TEM PY - 2020 DO - https://doi.org/10.1039/d0nr02931a VL - 12 IS - 23 SP - 12589 EP - 12601 PB - Royal Society od Chemistry AN - OPUS4-52088 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 - CONF A1 - Stuff, Maria A1 - Rübner, Katrin A1 - Prinz, Carsten A1 - Rische, N. A1 - Chronz, M. A1 - Kühne, Hans-Carsten ED - Siegesmund, S. ED - Middendorf, B. T1 - Towards a better understanding of tuff stone deterioration N2 - Stone deterioration is the result of a complex interaction of external physical, chemical and biological forces with the mineralogical-petrophysical properties of the stone. With a better understanding of how these properties are linked to material behavior and durability, more effective measures for stone conservation can be developed. Studying these interactions in tuff is particularly complex due to the naturally high heterogeneity of tuff rocks. The first aim of a current research project is to combine the results of recent and older studies on tuff deterioration. Furthermore, the literature overview is complemented by our own investigation of Weibern and Ettringen tuff, with a focus on pore structure characteristics. T2 - STONE - 14th international congress on the deterioration and conservation of stone CY - Meeting was canceled DA - 07.09.2020 KW - Pore structure KW - Weathering KW - Weibern tuff KW - Ettringen tuff PY - 2020 SN - 978-3-96311-172-3 SP - 805 EP - 810 PB - Mitteldeutscher Verlag CY - Halle (Saale) AN - OPUS4-51549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fedelich, Bernard A1 - Feldmann, Titus A1 - Haftaoglu, Cetin A1 - Nolze, Gert A1 - Schriever, Sina A1 - Epishin, A. A1 - Camin, B. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. T1 - Untersuchung des Kriechverhaltens einer Nickelbasis-Superlegierung bei ultrahohen homologen Temperaturen und Anwendung auf das heiß-isostatische Pressen (HIP) N2 - Mit Hilfe des HIP-Verfahrens („Hot Isostatic Pressing“) werden Poren in der einkristallinen Nickel-Basis Superlegierung CMSX-4 kontinuierlich geschrumpft und dadurch die nach der Erstarrung und der Wärmebehandlung vorhandene Porosität stark reduziert. In diesem Beitrag werden experimentelle und numerische Untersuchungen zu den Mechanismen der Porenschrumpfung zusammengefasst. Es zeigt sich, dass das Verformungsverhalten während Kriechversuchen bei der HIP-Temperatur durch Versetzungsgleitung auf oktaedrischen Ebenen dominiert wird. Dagegen zeigen Messungen der Porositätsabnahme und Simulationen des Porenschließens, dass die Kinetik der Porenschrumpfung durch das Phänomen der Leerstellendiffusion zwischen Poren und Kleinwinkelkorngrenzen („Low Angle Boundary“, LAB) bestimmt wird. Im Gegensatz führt die klassische Kristallviskoplastizität zu einer systematischen Überschätzung dieser Kinetik. Der scheinbare Widerspruch lässt sich auflösen, wenn man bedenkt, dass auf der Skala der Poren Versetzungsquellen nicht gleichmäßig verteilt sind, wie in der konventionellen Kristallplastizität implizit angenommen wird. Stattdessen wird in einem weiterführenden Modell davon ausgegangen, das Kleinwinkelkorngrenzen (LABs) als Versetzungsquellen fungieren, während die Scherspannungen sehr stark in der Nähe der Poren lokalisiert sind, was die Emission von Versetzungen deutlich reduziert. T2 - Langzeitverhalten warmfester Stähle und Hochtemperaturwerkstoffe CY - Online meeting DA - 27.11.2020 KW - HIP KW - Superlegierung KW - Kriechen PY - 2020 SN - 978-3-946885-95-5 VL - 2020 SP - 28 EP - 39 PB - Forschungsvereinigung Warmfeste Stähle und Hochtemperaturwerkstoffe AN - OPUS4-51796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - Safety Related Properties of Hydrogen Mixtures - Laboratory Tests N2 - Wasserstoff unterscheidet sich hinsichtlich der sicherheitstechnischen Eigenschaften von anderen brennbaren Gassen, v.a. durch die sehr niedrige Mindestzündenergie und die sehr hohe Flammengeschwindigkeit. In der Praxis treten Wasserstoffgemische z.B. durch Einspeisung von Wasserstoff in das Erdgasnetz, bei der Herstellung von Synthesegas (CO, H2) und in Biogasanlagen auf. Die sicherheitstechnischen Eigenschaften von Wasserstoffgemischen wurden experimentell untersucht und werden vorgestellt. Darüber hinaus wurde die Genauigkeit von Berechnungsmethoden für sicherheitstechnische Eigenschaften von Wasserstoffgemischen untersucht. N2 - Hydrogen differs from most other flammable gases regarding the safety related properties. Mainly the minimum ignition energy (MIE) is particularly low and the burning velocity is particularly high. Hydrogen mixtures are formed in different hydrogen applications, for example if hydrogen is added to the existing natural gas grid, if synthetic gas (mixture of CO and H2) is produced or in biogas plants. Safety related properties of hydrogen mixtures were determined experimentally and are presented in this presentation. Moreover the accuracy of estimation methods for safety related properties of hydrogen mixtures is evaluated.” T2 - Center for Hydrogen Safety 2020 European Conference CY - Online meeting DA - 20.10.2020 KW - Explosion Protection KW - Explosion Limits KW - Minimum Ignition Energy KW - Ignition Source KW - Synthetic Gas PY - 2020 AN - OPUS4-51530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Butz, Adam T1 - Detection and prediction of high temperature fatigue crack growth around notches in polycrystalline nickel base alloy N2 - Im Rahmen eines Vorhabens wurden Methoden zur Reduktion des Versuchsaufwandes bei der Modellerstellung für LCF-Lebensdauervorhersage untersucht. Einige dieser Methoden sind hier kurz vorgestellt. N2 - Methods for reducing the experimental effort necessary for the development of LCF life time prediction models were investigated. Some of these methods are briefly presented here. T2 - 4th International Symposium for Fatigue Design and Material Defects CY - Online meeting DA - 26.05.2020 KW - LCF KW - Mechanistic Modelling KW - Fatigue KW - Data Fusion PY - 2020 AN - OPUS4-50904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Orellana Pérez, Teresa T1 - Die Wasserstoffstrategie der BAM; Kompetenzzentrum H 2 safety@bam N2 - Das Thema Wasserstoff ist an der BAM seit mehr als hundert Jahren aktuell und steht auch gegenwärtig im Zentrum zahlreicher Forschungs- und Kooperationsaktivitäten. Mit der aktuellen Wasserstoff-Strategie der BAM werden wichtige Voraussetzungen dafür geschaffen, dass der Markthochlauf gelingt und die technische Sicherheit und Überwachung der Infrastrukturen und Anlagen gewährleistet ist – von der Erzeugung, über den Transport bis zur Speicherung und Bereitstellung von Wasserstoff als Energieträger der Zukunft. T2 - 1st Digital AK PostDocs Meeting CY - Online meeting DA - 01.10.2020 KW - Kompetenzzentrum H2Safety@BAM KW - Wasserstoff KW - Wasserstoffstrategie PY - 2020 AN - OPUS4-51371 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Askar, Enis T1 - Explosion Protection for Hydrogen Applications N2 - In the this lecture the safety related properties of hydrogen compared to other fuel gases and the explosion protection measures of avoiding flammable mixtures, avoiding ignition sources and mitigating the consequences of explosions are presented. T2 - Guest Lecture at the University of Birmingham CY - Online meeting DA - 19.10.2020 KW - New energy carriers KW - Explosion limits KW - Ignition energy KW - Ignition source KW - Renewable energy PY - 2020 AN - OPUS4-51531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan A1 - Bertovic, Marija A1 - Radtke, Martin A1 - et al., ED - Wahlster, W. ED - Winterhalter, C. T1 - Deutsche Normungsroadmap künstliche Intelligenz N2 - Rund ein Jahr haben DIN und DKE in einem gemeinsamen Projekt mit dem Bundesministerium für Wirtschaft und Energie und zusammen mit ca. 300 Fachleuten aus Wirtschaft, Wissenschaft, öffentlicher Hand und Zivilgesellschaft an der Normungsroadmap Künstliche Intelligenz gearbeitet. Eine hochrangige Steuerungsgruppe unter dem Vorsitz von Prof. Wolfgang Wahlster hat die Erarbeitung koordiniert und begleitet. Ziel der Roadmap ist die frühzeitige Entwicklung eines Handlungsrahmens für die Normung und Standardisierung, der die internationale Wettbewerbsfähigkeit der deutschen Wirtschaft unterstützt und europäische Wertmaßstäbe auf die internationale Ebene hebt. KW - Künstliche Intelligenz KW - Normung KW - Roadmap PY - 2020 UR - https://www.din.de/resource/blob/772438/ecb20518d982843c3f8b0cd106f13881/normungsroadmap-ki-data.pdf VL - 2020 SP - 1 EP - 232 PB - Deutsches Institut für Normung (DIN) CY - Berlin ET - 1. AN - OPUS4-51733 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - Full field X-ray fluorescence imaging with coded apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energy-dispersive array detector with a coded aperture to obtain high resolution images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @ BESSY II. This method enables the simultaneous detection of multiple elements, which is important e.g. in the field of catalysis. T2 - CONEXS 2020 CY - Newcastle, UK DA - 18.02.2020 KW - X-ray fluorescence spectroscopy KW - Coded apertures KW - Imaging KW - Iterative reconstruction PY - 2020 AN - OPUS4-50461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning: examples from BAMline N2 - Various applications for artificial intelligence in the context of spectroscopy will be presented. in particular, examples from BAMline will be presented. After a short introduction to synchrotron radiation, artificial intelligence algorithms for the quantification of X-ray fluorescence measurement are discussed. In the second example, information retrieval by natural language processing is discussed. T2 - Analytical Academy CY - Online meeting DA - 02.06.2020 KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron PY - 2020 AN - OPUS4-51898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan A1 - Sturm, Patrick A1 - Kühne, Hans-Carsten A1 - Gluth, Gregor ED - Bishnoi, S. T1 - Comparison of brick clays and a kaolinitic clay regarding calcination and performance in blended cement mortars N2 - Two brick clays (rich in 2:1 clay minerals) and a low-grade kaolinitic clay were studied regarding their transformations during calcination and their performance in blended cement mortars. The mortars with calcined clays exhibited decreased workability (slump flow), but this effect could be mitigated by employment of a conventional superplasticizer; however, compressive strength of the hardened mortar was lowered in some cases. While the kaolinitic clay generally yielded the highest strength, the performance of a brick clay could be increased by grinding to higher fineness and by mixing it with the kaolinitic clay. T2 - 3rd International Conference on Calcined Clays for Sustainable Concrete CY - New Delhi, India DA - 15.10.2019 KW - Calcined clays KW - Blended cements KW - Workability KW - Supplementary cementitious materials PY - 2020 SN - 978-981-15-2805-7 DO - https://doi.org/10.1007/978-981-15-2806-4_10 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 25 SP - 85 EP - 93 PB - Springer CY - Singapore AN - OPUS4-50663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, U.E.A. A1 - Streli, C. A1 - Radtke, Martin T1 - Comparison of three reconstruction methods based on deconvolution, iterative algorithm and neural network for X-ray fluorescence imaging with coded apertures N2 - X-ray imaging methods are used in many fields of research, as they allow a non-destructive Investigation of the elemental content of various samples. As for every imaging method, for X-ray imaging the optics are of crucial importance. However, these optics can be very expensive and laborious to build, as the requirements on surface roughness and precision are extremely high. Angles of reflection and refraction are often in the range of a few mrad, making a compact design hard to achieve. In this work we present a possibility to simplify X-ray imaging. We have adapted the coded aperture method, a high energy radiation imaging method that has its origins in astrophysics, to full field X-ray fluorescence imaging. In coded aperture imaging, an object is projected through a known mask, the coded aperture, onto an area sensitive detector. The resulting image consists of overlapping projections of the object and a reconstruction step is necessary to obtain the information from the recorded image. We recorded fluorescence images of different samples with an energy-dispersive 2D detector (pnCCD) and investigated different reconstruction methods. With a small coded aperture with 12 holes we could significantly increase the count rate compared to measurements with a straight polycapillary optic. We show that the reconstruction of two different samples is possible with a deconvolution approach, an iterative algorithm and a neural network. These results demonstrate that X-ray fluorescence imaging with coded apertures has the potential to deliver good results without scanning and with an improved count rate, so that measurement times can be shortened compared to established methods. KW - X-ray fluorescence imaging KW - Coded apertures KW - Imaging KW - Elemental mapping KW - Image reconstruction PY - 2020 DO - https://doi.org/10.1039/d0ja00146e VL - 35 IS - 7 SP - 1423 EP - 1434 PB - Royal Society of Chemistry CY - United Kingdom AN - OPUS4-51518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Ke, X. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. T1 - Evidence for redox reactions during vanadium crossover inside the nanoscopic water-body of Nafion 117 using X-ray absorption near edge structure spectroscopy N2 - A major source of capacity fade of the common vanadium redox flow battery (VRFB) is the vanadium ion transport through the separator. However, different transport models disagree significantly in the diffusion coefficient for the different V species and the influence of different transport mechanisms. The underlying hypothesis of this work is that reactions inside the membrane are partly responsible for these discrepancies. Accordingly, it was investigated if redox reactions inside the nanoscopic water body of Nafion 117 can occur. X-ray absorption near edge structure spectroscopy (XANES) was used to distinguish between the different V species inside hydrated Nafion 117 and novel PVDF-based membranes. It was validated that the speciation of vanadium can be performed using the pre-edge peak energy and intensity. The experiments were performed as follows: strips of the membrane were exposed from one site to a V3+ solution (green) and from the other site to a VO2+ solution (yellow). The ions could diffuse into the membrane from both sides. A change of color of the membrane strip was observed. The blue color in the middle of the strip indicated that VO2+ was formed where V3+ and VO2+ got in contact. Using XANES this reaction inside Nafion was proven. KW - PVDF-Based membrane KW - VRFB KW - Vanadium speciation KW - XANES KW - Nafion 117 PY - 2020 DO - https://doi.org/10.1016/j.jpowsour.2020.229176 VL - 483 SP - 229176 PB - Elsevier B.V. AN - OPUS4-51719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gluth, Gregor T1 - Sulfuric acid resistance of copper-doped and plain metakaolin-based alkali-activated materials studied by 29Si, 27Al and 1H MAS NMR, and Cu K-edge XANES spectroscopy N2 - Alkali-activated materials have been repeatedly reported to exhibit high acid resistance, but no generally accepted hypothesis regarding the underlying mechanisms has emerged yet. To contribute to this issue, K-waterglass-activated metakaolin specimens, with and without the addition of CuSO4·5H2O in the starting mix, were exposed to either a chemically aggressive sewer environment (mortars) or sulfuric acid (pastes). The mode of copper incorporation in the materials and the formation of copper phases in the corroded layers were studied by XANES at the Cu K-edge, and 29Si, 27Al and 1H MAS NMR was employed to understand the processes during acid attack. Copper was found as a spertiniite-like phase in the as-cured materials, while in the deterioration layers of the pastes it was present as copper sulfate. In the corroded regions of the mortars, unequivocal identification of Cu phases was not possible, but the results were reconcilable with the presence of copper carbonate hydroxide. The solid-state NMR results revealed virtually complete dissolution of the K-A-S-H gel and the formation of silica gel, interpreted to be a central mechanism determining the acid resistance. No significant differences between the microstructural alterations of the pastes with and without Cu addition on (chemical) sulfuric acid attack were observed. T2 - 74th RILEM Annual Week & 40th Cement and Concrete Science Conference CY - Online meeting DA - 31.08.2020 KW - Alkali-activated materials KW - Sulfuric acid resistance KW - Sewer structures PY - 2020 AN - OPUS4-51198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - X-Ray fluorescence with synchrotron radiation basics and applications N2 - In this talk, the features of X-ray fluorescence analysis with synchrotron radiation will be presented. First, the basics of the origin of synchrotron radiation and X-ray fluorescence analysis and the experimental setup will be discussed. Then, examples of trace element detection, micrometer resolution, and application of the X-ray color camera will be shown. T2 - HZB Photon school 2020 CY - Berlin, Germany DA - 09.03.2020 KW - Synchrotron KW - BAMline KW - XRF KW - Machine learning PY - 2020 AN - OPUS4-51894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fittschen, U. A1 - Lutz, C. T1 - Element Species Determination in Polymer Electrolyte Membranes N2 - Polymer electrolyte membranes (PEM) are polymers which act as separator in an electrochemical cell and allow ionic charge flow to close the circuit. Widely used membranes are perfluorinated sulfonic-acid (PFSA) ionomers (e.g. Nafion™), a class of ion-conducting polymers with remarkable ion conductivity and chemical-mechanical stability. A nanoscopic water system around the sulfonic acid capped side-chains of the otherwise hydrophobic polymer allows the ion transport. Only approx. 14 molecules of water per sulfonic group are present in the fully hydrated state. In vanadium redox flow batteries (VRFB) ideally only protons are transported. The weak ion selectivity of Nafion™ is the main cause for the transportation of vanadium, briefly vanadium crossover, in VRFBs a system we have investigated more closely, lately. The consequences of crossover are a concentration imbalance and a self-discharge of the battery, which leads to a decrease of the capacity. The development of efficient energy storage systems is crucial for the transformation towards a renewable energy based economy. The VRFB has a great potential as a commercial electrochemical energy storage system due to properties including, but not limited to, no cross-contamination, a long cycle-life and a theoretically unlimited capacity. VRFB consists of two half-cells, which are linked to electrolyte tanks and separated by a membrane. The membrane plays a major role in overall cell performance. So far, vanadium transportation models, which include diffusion, migration, electroosmotic convection and pressure gradients, are inconsistent. There is no agreement in the literature on the diffusion coefficients of vanadium species (e.g. published diffusion coefficients of V2+ are located between 3.13·10-12 m²s-1 and 9.44·10-12 m²s-1) indicate that thevanadium crossover is not well understood and there is a lack on a more fundamental level. Since the membrane transport is the rate-determining step of the crossover as well as of the proton exchange it is extremely important to understand these phenomena on a fundamental level. This will eventually allow us to design better membranes. Alternative materials need to show equivalent performance compared with Nafion™ and ideally be more selective regarding ion cross-membrane transport.There are several options to approach the chemistry i.e. the interaction of dissolved and bound ions inside the confined water body of ionomeric membranes. Vanadium ions are a versatile model as UV/VIS data can be used to distinguish between the 5 species V2+, V3+, VO2+, VO2+ and V2O33+ of the electrolyte. Infrared spectroscopy has been applied to study the interaction of sulfonic groups and the ions. Molecular dynamic modeling is another approach to study the distribution and distances of ions. We now introduce X-ray absorption near edge structure spectroscopy (XANES) to study species and species changes inside Nafion™ and a novel membrane based on poly(1,1-difluoroethylene) (PVDF). We evaluated the methods and investigated the influence of irradiation, temperature and hydration on the measurements. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Batteries KW - BAMline KW - XANES PY - 2020 AN - OPUS4-51910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gluth, Gregor T1 - RILEM TC 281-CCC WG6 - Carbonation of alkali-activated concrete: preliminary results N2 - Preliminary results of RILEM TC 281-CCC Working Group 6 'Carbonation of alkali-activated concrete' are presented. T2 - 74th RILEM Annual Week & 40th Cement and Concrete Science Conference CY - Online meeting DA - 31.08.2020 KW - Alkali-activated materials KW - Carbonation PY - 2020 AN - OPUS4-51199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Melzer, Michael T1 - Seminar about the expression of uncertainty in measurement N2 - The evaluation of measurement uncertainty is essential for testing and calibration laboratories. This paper provides a general process description for the determination of the measurement uncertainty of quantitative data and its application to the conformity assessment with examples, and how to deal with the uncertainty of qualitative (Boolean) results, e. g. when "Alarm" or "No alarm" occours in an instrument display. T2 - GW4SHM - 1st Training Event CY - Online meeting DA - 23.11.2020 KW - Uncertainty KW - Conformity assessment KW - Boolean results PY - 2020 AN - OPUS4-52040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thünemann, Andreas A1 - Gruber, Alexandra A1 - Klinger, Daniel T1 - Amphiphilic Nanogels: Fuzzy Spheres with a Pseudo-Periodic Internal Structure N2 - Amphiphilic polymer nanogels (NGs) are promising drug delivery vehicles that extend the application of conventional hydrophilic NGs to hydrophobic cargoes. By randomly introducing hydrophobic groups into a hydrophilic polymer network, loading and release profiles as well as surface characteristics of these colloids can be tuned. However, very little is known about the underlying internal structure of such complex colloidal architectures. Of special interest is the question how the amphiphilic network composition influences the internal morphology and the “fuzzy” surface structure. To shine light into the influence of varying network amphiphilicity on these structural features, we investigated a small library of water-swollen amphiphilic NGs using small-angle X-ray scattering (SAXS). It was found that overall hydrophilic NGs, consisting of pure poly(N-(2-hydroxypropyl)methacrylamide) (PHPMA), display a disordered internal structure as indicated by the absence of a SAXS peak. In contrast, a SAXS peak is present for amphiphilic NGs with various amounts of incorporated hydrophobic groups such as cholesteryl (CHOLA) or dodecyl (DODA). The internal composition of the NGs is considered structurally homologous to microgels. Application of the Teubner–Strey model reveals that hydrophilic PHPMA NGs have a disordered internal structure (positive amphiphilicity factor) while CHOLA and DODA samples have an ordered internal structure (negative amphiphilicity factor). From the SAXS data it can be derived that the internal structure of the amphiphilic NGs consists of regularly alternating hydrophilic and hydrophobic domains with repeat distances of 3.45–5.83 nm. KW - Polymer KW - Nanoparticle KW - SAXS PY - 2020 DO - https://doi.org/10.1021/acs.langmuir.0c01812 VL - 36 IS - 37 SP - 10979 EP - 10988 PB - American Chemical Society AN - OPUS4-51302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawlitza, Kornelia A1 - Johann, Sergej A1 - Mansurova, M. A1 - Kohlhoff, Harald A1 - Tiebe, Carlo A1 - Bell, Jérémy A1 - Bartholmai, Matthias A1 - Rurack, Knut T1 - Semi-automatic Measurement Device for Long-Term Monitoring of Ammonia in Gas Phase N2 - The present paper describes the development of a sensor material that changes its fluorescence in the presence of gaseous ammonia in a relevant concentration range. The implementation into a semi-automatic gas measurement device enables low-cost, precise, simple and fast monitoring of low con-centrations of harmful gases, like ammonia, and hence can help to improve the climate monitoring in livestock housing, barns or stables. T2 - SMSI 2020 CY - Meeting was canceled KW - Spectroscopy KW - Emmbedded sensor KW - Environment KW - Air quality PY - 2020 DO - https://doi.org/10.5162/SMSI2020/B5.4 SP - 133 EP - 134 AN - OPUS4-50867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stock, V. A1 - Fahrenson, C. A1 - Thünemann, Andreas A1 - Donmez, M. H. A1 - Voss, L. A1 - Bohmert, L. A1 - Braeuning, A. A1 - Lampen, A. A1 - Sieg, H. T1 - Impact of artificial digestion on the sizes and shapes of microplastic particles N2 - Current analyses show a widespread occurrence of microplastic particles in food products and raise the question of potential risks to human health. Plastic particles are widely considered to be inert due to their low chemical reactivity and therefore supposed to pose, if at all only minor hazards. However, variable physicochemical conditions during the passage of the gastrointestinal tract gain strong importance, as they may affect particle characteristics. This study aims to analyze the impact of the gastrointestinal passage on the physicochemical particle characteristics of the five most produced and thus environmentally relevant plastic materials polyethylene, polypropylene, polyvinyl chloride, polyethylene terephthalate and polystyrene. Scanning electron microscopy (SEM) and subsequent image analysis were employed to characterize microplastic particles. Our results demonstrate a high resistance of all plastic particles to the artificial digestive juices. The present results underline that the main stages of the human gastrointestinal tract do not decompose the particles. This allows a direct correlation between the physicochemical particle characteristics before and after digestion. Special attention must be paid to the adsorption of organic compounds like proteins, mucins and lipids on plastic particles since it could lead to misinterpretations of particle sizes and shapes. KW - Artificial digestion KW - Gastrointestinal barrier KW - Microplastic KW - Oral uptake KW - Particle size PY - 2020 DO - https://doi.org/10.1016/j.fct.2019.111010 VL - 135 SP - 111010 PB - Elsevier Ltd. AN - OPUS4-49999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Long, Lijia A1 - Anh Mai, Q. A1 - Morato, P. G. A1 - Dalsgaard Sorensen, J. A1 - Thöns, Sebastian T1 - Information value-based optimization of structural and environmental monitoring for offshore wind turbines support structures N2 - The use of load and structural performance measurement information is vital for efficient structural integrity management and for the cost of energy production with Offshore Wind Turbines (OWTs). OWTs are dynamically sensitive structures subject to an interaction with a control unit exposed to repeated cyclic wind and wave loads causing deterioration and fatigue. This study focuses on the quantification of the value of structural and environmental information on the integrity management of OWT structures, with the focus on fatigue of welded joints. By utilizing decision analysis, structural reliability methods, measurement data, as well as the cost-benefit models, a Value of Information (VoI) analysis can be performed to quantify the most beneficial measurement strategy. The VoI assessment is demonstrated for the integrity management of a butt welded joint of a monopile support structure for a 3 MW OWT with a hub height of approximately 71m. The conditional value of three-year measured oceanographic information and one-year strain monitoring information is quantified posteriori in conjunction with an inspection and repair planning. This paper provides insights on how much benefits can be achieved through structural and environmental information, with practical relevance on reliability-based maintenance of OWT structures. KW - Structural health monitoring KW - Offshore wind turbine KW - Monopile support structure KW - Value of information KW - Weld fatigue KW - Decision tree KW - Dynamic Bayesian Network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514098 DO - https://doi.org/10.1016/j.renene.2020.06.038 VL - 10 IS - 159 SP - 1036 EP - 1046 PB - Elsevier Ltd. AN - OPUS4-51409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee Analyse von Gold mit Synchrotronstrahlung III N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Der Fund von Bernstorf wird ausführlich diskutiert. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 06.11.2020 KW - Synchrotron KW - BAMline KW - XRF KW - Gold KW - Archäometrie PY - 2020 AN - OPUS4-51893 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weimann, Karin T1 - Baustoffrecycling: Kreislaufwirtschaft und Umweltschutz N2 - Aktuelle Zahlen zum Baustoffrecycling Zielkonflikte im Kontext von Abfallwirtschaft, Boden- und Grundwasserschutz sowie rechtlichen Vorgabe mit den Beispielen rezyklierte Gesteinskörnungen und RC-Gips. T2 - IX. Baustoffseminar CY - Weimar, Germany DA - 11.03.2020 KW - Kreislaufwirtschaft KW - Baustoffrecycling KW - Ressourcenschonung PY - 2020 AN - OPUS4-51436 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wahl, S. A1 - El-Refaei, S. M. A1 - Amsalem, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Koch, N. A1 - Pinna, N. T1 - Operando diffuse reflectance UV-vis spectroelectrochemistry for investigating oxygen evolution electrocatalysts N2 - The characterization of the active structure of water-splitting catalysts is crucial to evolve to a sustainable energy future based on hydrogen. Such information can only be obtained by operando methods. We present a diffuse reflectance UV-vis (DRUV) spectroelectrochemical study that allows tracking the changes of solid oxygen evolution catalysts under working conditions. The versatility of our approach is demonstrated on two cobalt-containing catalysts, Zn0.35Co0.65O and CoAl2O4. The changes the catalysts undergo during the oxygen evolution reaction can be tracked by probing the electronic structure using UV-vis spectroscopy. These findings are compared to ex situ analyses, which support the assignments of the structures stabilized under different potentials. Thus, structure–activity correlations can be proposed, and deeper insights into the catalytically active structures can be obtained. KW - EXAFS PY - 2020 DO - https://doi.org/10.1039/c9cy02329a VL - 10 IS - 2 SP - 517 EP - 528 PB - Royal Society of Chemistry AN - OPUS4-50468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reifschneider, O. A1 - Vennemann, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Hogeback, J A1 - Köppen, C. A1 - Großgarten, M. A1 - Sperling, M. A1 - Wiemann, M. A1 - Karst, U. T1 - Revealing Silver Nanoparticle Uptake by Macrophages Using SR-μXRF and LA-ICP-MS N2 - To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed. KW - Synchrotron KW - BAMline KW - XRF KW - Nanoparticle KW - Macrophagen PY - 2020 DO - https://doi.org/10.1021/acs.chemrestox.9b00507 VL - 33 IS - 5 SP - 1250 EP - 1255 PB - American Chemical Society AN - OPUS4-50855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Artificial intelligence for spectroscopy examples from BAMline N2 - Various applications for artificial intelligence in the context of spectroscopy will be presented. in particular, examples from bamline will be featured. After a short introduction to synchrotron radiation, artificial intelligence algorithms for the quantification of X-ray fluorescence measurement are discussed. In the second example, information retrieval by natural language processing is reviewed. As a last example the reconstruction of measurements with the X-ray color camera and coded apertures is presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - ATi Wien, Austria DA - 22.01.2020 KW - Machine learning KW - Natural language processing KW - Neural networks KW - Synchrotron KW - BAMline PY - 2020 AN - OPUS4-51891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weimann, Karin T1 - Gypsum plasterboard recycling - a sustainable approach N2 - Gypsum (calcium sulfate dihydrate) has excellent building material properties and has been widely used in constructions in the last decades in many countries. Accordingly, an increase of waste gypsum in C&D waste is expected in the upcoming years. On one hand, sulfates are unwanted in other secondary building materials (particularly in recycled concrete aggregates) and should be minimized for quality reasons. On the other hand, used gypsum from CDW can also be used in gypsum production if the high quality requirements for the recycled gypsum – especially regarding the sorting accuracy - are met. A large percentage of the gypsum from buildings was installed as gypsum plasterboards in interior fittings so far. Gypsum plasterboards are comparatively simple to remove and to separate during selective dismantling. Therefore, a high sorting purity can be achieved. In addition, techniques for the recycling of gypsum plasterboards already exist and high quality standards can be achieved. Also, the reuse in gypsum production has been improved in the last decade. Furthermore, an environmental evaluation of the whole process of gypsum plasterboard recycling and reuse showed that this approach can be environmentally advantageous. Therefore, a closed-loop recycling of gypsum plasterboards is feasible. This poster will show the development of gypsum consumption in different countries as well as a prognosis for the upcoming of gypsum in CDW in the future decades in Germany. Furthermore, a simplified scheme of the recycling process and selected results from an environmental evaluation will be presented. T2 - Conference on Mining the European Anthroposphere: Poster session CY - Bologna, Italy DA - 20.02.2020 KW - LCA KW - Gypsum recycling PY - 2020 AN - OPUS4-51435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Trace element analysis with synchrotron radiation N2 - Trace elements are chemical elements whose concentration in a material is very low. The exact definition depends on the application and varies for example between 100 micrograms per gram in analytical chemistry and 1000 micrograms per gram in geology. The ability to detect trace elements fast and quantitatively is of great importance in many areas of science and technology. With its high brilliance and flexibility in the excitation conditions, synchrotron radiation is an ideal tool for detecting traces even in small sample quantities. In this contribution I will report about the use of X-ray fluorescence(XRF)for qualitative and quantitative element sensitiveanalysis. In addition to the fundamentals of XRF and its quantification methods, the advantages and problems of different geometries like e.g. microXRF, Total Reflection X-ray Fluorescence (TXRF)or Double Dispersive XRF (D²XRF) will be discussed. Practical examples from BAMline from the research fields of medicine, geology and archaeometry will complete the lecture. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Synchrotron KW - BAMline KW - XRF PY - 2020 AN - OPUS4-51890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lutz, C. T1 - Investigation on Vanadium Crossover in Nafion ™ and Novel PVDF Based Membranes for Vanadium Redox Flow Batteries N2 - Vanadium redoxflow batteries (VRFB)are currently one of the most promising candidates for stationary energys torage.For large scale applications the ion conducting membranes currently in use need to be improved. Ideally,they need to become more cost efficient and selective regarding the vanadium crossover.For a better understanding of the vanadium crossover, the development of reliable analytical methods and procedures, that elucidate uptake and transport of vanadium ions in the membrane, is necessary. First, we present the uptake of V2+,V3+,VO2+, VO2+ and V2O33+ in Nafion™ and in a novel membrane based onpoly(1,1-difluoroethylene)(PVDF). In preliminary discharge/charge experiments the ETFE-based membrane, the precursor of PVDF-based membrane, performed comparable to Nafion™. The methods of choice for speciation are UV/Vis and X-ray absorption near edge structure spectroscopy (XANES). According to the results, V2O33+, formed from VO2+ and VO2+, diffuses also into the membrane. In present models, the diffusion of V2O33+ is neglected. In addition,we study whether reactions could take place inside the membranes’ nanoscopic water body using XANES. Exposing Nafion™ from one site with V3+a nd from the other site with VO2+ realized the experiment. The results verified that VO2+ was formed inside the membrane. However,in present models reactions inside the membrane are neglected, too. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Batteries KW - BAMline KW - XANES KW - VRF PY - 2020 AN - OPUS4-51909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Varadarajan, A. A1 - Allan, R. A1 - Valentin, J. A1 - Castañeda Ocampo, O. A1 - Somerville, V. A1 - Buhmann, M. A1 - West, J. A1 - Skipp, Paul A1 - van der Mei, H. A1 - Ren, Q. A1 - Schreiber, Frank A1 - Webb, J. A1 - Pietsch, Franziska A1 - Ahrens, C. T1 - An integrated model system to gain mechanistic insights into biofilm-associated antimicrobial resistance in Pseudomonas aeruginosa MPAO1 N2 - Pseudomonas aeruginosa MPAO1 is the parental strain of the widely utilized transposon mutant collection for this important clinical pathogen. Here, we validate a model system to identify genes involved in biofilm growth and biofilm-associated antibiotic resistance. Our model employs a genomics-driven workflow to assemble the complete MPAO1 genome, identify unique and conserved genes by comparative genomics with the PAO1 reference strain and genes missed within existing assemblies by proteogenomics. Among over 200 unique MPAO1 genes, we identified six general essential genes that were overlooked when mapping public Tn-seq data sets against PAO1, including an antitoxin. Genomic data were integrated with phenotypic data from an experimental workflow using a user-friendly, soft lithography-based microfluidic flow chamber for biofilm growth and a screen with the Tn-mutant library in microtiter plates. The screen identified hitherto unknown genes involved in biofilm growth and antibiotic resistance. Experiments conducted with the flow chamber across three laboratories delivered reproducible data on P. aeruginosa biofilms and validated the function of both known genes and genes identified in the Tn-mutant screens. Differential Protein abundance data from planktonic cells versus biofilm confirmed the upregulation of candidates known to affect biofilm formation, of structural and secreted proteins of type VI secretion systems, and provided proteogenomic evidence for some missed MPAO1 genes. This integrated, broadly applicable model promises to improve the mechanistic understanding of biofilm formation, antimicrobial tolerance, and resistance evolution in biofilms. KW - Biofilms PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515108 DO - https://doi.org/10.1038/s41522-020-00154-8 VL - 6 IS - 1 SP - Article number: 46 PB - Springer Nature CY - Singapore AN - OPUS4-51510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pietsch, Franziska A1 - O'Neill, A. J. A1 - Ivask, A. A1 - Jenssen, H. A1 - Inkinen, J. A1 - Kahru, A. A1 - Ahonen, M. A1 - Schreiber, Frank T1 - Selection of resistance by antimicrobial coatings in the healthcare setting N2 - Antimicrobial touch surfaces have been introduced in healthcare settings with the aim of supporting existing hygiene procedures, and to help combat the increasing threat of antimicrobial resistance. However, concerns have been raised over the potential selection pressure exerted by such surfaces, which may drive the evolution and spread of antimicrobial resistance. This review highlights studies that indicate risks associated with resistance on antimicrobial surfaces by different processes, including evolution by de-novo mutation and horizontal gene transfer, and species sorting of inherently resistant bacteria dispersed on to antimicrobial surfaces. The review focuses on antimicrobial surfaces made of copper, silver and antimicrobial peptides because of the practical application of copper and silver, and the promising characteristics of antimicrobial peptides. The available data point to a potential for resistance selection and a subsequent increase in resistant strains via cross-resistance and co-resistance conferred by metal and antibiotic resistance traits. However, translational studies describing the development of resistance to antimicrobial touch surfaces in healthcare-related environments are rare, and will be needed to assess whether and how antimicrobial surfaces lead to resistance selection in These settings. Such studies will need to consider numerous variables, including the antimicrobial concentrations present in coatings, the occurrence of biofilms on surfaces, and the humidity relevant to dry-surface environments. On-site tests on the efficacy of antimicrobial Coatings should routinely evaluate the risk of selection associated with their use. KW - Antimicrobial resistance KW - Antimicrobial coating KW - Touch surfaces KW - Healthcare KW - Infections KW - COST action CA15114 AMICI PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510926 DO - https://doi.org/10.1016/j.jhin.2020.06.006 SN - 0195-6701 VL - 106 IS - 1 SP - 115 EP - 125 PB - Elsevier Ltd AN - OPUS4-51092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Selina T1 - Antimicrobial resistance in soil microbes mediated by resistance evolution and horizontal gene transfer (HGT) N2 - Biocides are in contact with soils through direct application and passive leaching from protected materials. Consequently, soil microorganisms are exposed to biocides even though they are not their primary targets. Soil is a large reservoir of microbial diversity and has been hypothesized to be a crucial factor for the evolution and spread of antimicrobial resistance. Currently, there is little knowledge on how biocides used to protect materials affect the evolution and spread of resistance. Thus, our aim is to investigate the risk for the evolution of biocide resistance and cross-resistance to antibiotics. In addition, we aim to elucidate the affect of biocides on the spread of resistance via horizontal gene transfer (HGT). In adaptive laboratory evolution experiments we cultured selected model soil microorganism with representative biocides under selection regimes with increasing and stable biocide concentrations followed by antibiotic and biocide cross-resistance determination. Moreover, we investigate if the selected biocides affect the rates of de novo mutations and HGT of plasmids that carry resistance genes among soil microorganism. Our results show only small increases of biocide resistance during serial transfers under increasing biocide concentrations. One reason for this might be the narrow selective window for biocide resistance due to steep dose-response relationships. Furthermore, our results indicate that a stable low-level biocide regime did not select for high level cross-resistance to antibiotics and other biocides. Moreover, material preservatives affected the rates of HGT via conjugation and the mutation rates at sub-inhibitory concentrations. The results will enable future risk assessment regarding resistance evolution for biocides used as material preservatives. T2 - 4th Evo Eco PhD Meeting CY - Lutherstadt Wittenberg DA - 04.03.2020 KW - Microbiology KW - Biocides KW - Horizontal gene transfer HGT KW - Resistance evolution KW - Antimicrobial resistance PY - 2020 AN - OPUS4-51313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fittschen, U. T1 - Improving surface sensitive XRF using ink jet printing and information from the angle dependent signal N2 - Total Reflection X-ray Fluorescence (TXRF) is a small footprint, ressource efficient micro-analytical tool for trace elemental determination. However, depending on the matrix TXRF is also challenging in several ways: the preparation of a representative aliquot maybe difficult for slurries, shading effects and matrix effects may occur and the applicability of an IS maybe hampered by interferences (fitting may be impaired as well) or inhomogeneities. It is therefore crucial to understand and if applicable mitigate the influence of the before mentioned phenomena. We have used the small volume approach using pL droplets to study shading in TXRF previously.Using this approach thin specimens in a favorable geometry are prepared with a well defined morphology; this way minimizing matrix effects and shading. To be used as standard it is also necessary to determine the delivered elemental amounts. Here we will present on the performance of a commercial ink-jet printer cartridge to deliver defined volumes and elemental amounts. The microscopic specimens obtained have been successfully applied to determine relative sensitivities in TXRF and prepare references to study coded apertures in grazing incidence full field micro-XRF.The homogeneous lateral distribution of analyte and IS may be probed by micro-XRF, to obtain information on alikeness of analyte and IS. To study the alikeness of the in depth distribution (film-like or particle-like) angle scans can deliver valuable data. Here we present first results on angle scans using a prototype GIXRF set up and a commercial TXRF instrument. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - TXRF KW - Coded Aperture PY - 2020 AN - OPUS4-51913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - SRXRF examples from the BAMline N2 - Synchrotron radiation sources with their unique properties in terms of intensity, polarization and adjustability offer a wide range of possibilities in materials research. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods. T2 - Better with Scattering CY - Online meeting DA - 16.03.2020 KW - Synchrotron KW - BAMline KW - XRF PY - 2020 AN - OPUS4-51895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - An, Biwen Annie A1 - Deland, Eric A1 - Sobol, Oded A1 - Yao, Jizheng A1 - Skovhus, T. L. A1 - Koerdt, Andrea T1 - The differences in the corrosion product compositions of Methanogen-induced microbiologically influenced corrosion (Mi-MIC) between static and dynamic growth conditions N2 - Currently, corrosion rates (CR) and/or corrosion products (CP) obtained for methanogen-induced microbiologically influenced corrosion (Mi-MIC) on carbon steel are mainly analyzed from static-incubations. By using a multiport-flow-column, much higher CRs (0.72 mm/yr) were observed, indicating static-incubations are not suitable for determining the corrosive potential of Mi-MIC. With the combination of various analytical methods (ToF-SIMS/SEM-EDS/SEM-FIB) and contrary to previously published data, we observed that CPs contained phosphorus, oxygen, magnesium, calcium and iron but lacked carbon-related species (e.g. siderite). Overall, siderite nucleation is disrupted by methanogens, as they convert aqueous bicarbonate into carbon dioxide for methanogenesis resulting in increased localized corrosion. KW - Carbon steel KW - Modelling studies KW - SIMS KW - SEM KW - Reactor conditions KW - Microbiologically influenced corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517632 DO - https://doi.org/10.1016/j.corsci.2020.109179 SN - 0010-938X VL - 180 SP - 9179 PB - Elsevier AN - OPUS4-51763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geoerg, Paul A1 - Schumann, Jette A1 - Holl, Stefan A1 - Holl, Maik A1 - Hofmann-Böllinghaus, Anja T1 - The influence of individual impairments in crowd dynamics N2 - The importance of empirical relations to quantify the movement of pedestrians through a facility has increased during the last decades since performance-based design methods became more common. Bottlenecks are of special interest because of their importance for egress routes and as they result in a reduced capacity. The empirical relations as the density-dependent movement speed or flow rate were derived by studies under laboratory conditions, which were usually conducted with populations of homogeneous characteristics forbetter control of influencing variables. If individual characteristics of a crowd become more heterogeneous, individuals were forced to adapt their individual movement and control individual manoeuvring. These unintended interactions lead to a different shape of the fundamental empirical relations. Here, we present results from a movement study under well-controlled boundary conditions in which participants with and without different characteristics of disabilities participated. To consider the effect of different heterogeneities on the capacity of a facility, fundamental diagrams are generated using the Voronoi method. If participants with visible disabilities (such as using assistive devices) are part of a crowd, significant differences relating to the shape of the empirical Relations and the capacities are found. This indicates that the heterogeneity of a Population leads to an increased interpersonal interaction which results in influenced movement characteristics. KW - Engineering egress data KW - Heterogeneity KW - Human behaviour KW - Movement characteristics KW - Pedestrian dynamics PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508943 DO - https://doi.org/10.1002/fam.2789 SN - 0308-0501 VL - 45 IS - 4 SP - 529 EP - 542 PB - Wiley Online Libary CY - New Jersey, USA AN - OPUS4-50894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, L. A1 - Darvishi Kamachali, Reza A1 - Li, Z. A1 - Zhang, Z. T1 - Grain boundary energy effect on grain boundary segregation in an equiatomic high-entropy alloy N2 - Grain boundary (GB) Segregation has a substantial effect on the microstructure evolution and properties of polycrystalline alloys. The mechanism of nanoscale segregation at the various GBs in multicomponent alloys is of great challenge to reveal and remains elusive so far. To address this issue, we studied the GB segregation in a representative equiatomic FeMnNiCoCr high-entropy alloy (HEA) aged at 450 °C. By combining transmission Kikuchi diffraction, atom probe tomography analysis and a density-based thermodynamics modeling, we uncover the nanoscale segregation behavior at a series of well-characterized GBs of different characters. No segregation occurs at coherent twin boundaries; only slight nanoscale segregation of Ni takes place at the low-angle GBs and vicinal \Sigma 29b coincidence site lattice GBs. Ni and Mn show cosegregation of high levels at the general high-angle GBs with a strong depletion in Fe, Cr, and Co. Our density-based thermodynamic model reveals that the highly negative energy of mixing Ni and Mn is the main driving force for nanoscale cosegregation to the GBs. This is further assisted by the opposite segregation of Ni and Cr atoms with a positive enthalpy of mixing. It is also found that GBs of higher interfacial energy, possessing lower atomic densities (higher disorder and free volume), show higher segregation levels. By clarifying the origins of GB segregations in the FeMnNiCoCr HEA, the current work provides fundamental ideas on nanoscale segregation at crystal defects in multicomponent alloys. KW - Thermodynamics KW - High-Entropy Alloys KW - Grain Boundary Segregation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508827 DO - https://doi.org/10.1103/PhysRevMaterials.4.053603 VL - 4 IS - 5 SP - 053603 PB - American Physical Society AN - OPUS4-50882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Hänninen, H. A1 - Böllinghaus, Thomas T1 - In-situ ToF-SIMS analyses of deuterium re-distribution in austenitic steel AISI 304L under mechanical load N2 - Hydrocarbons fuel our economy. Furthermore, intermediate goods and consumer products are often hydrocarbon-based. Beside all the progress they made possible, hydrogen-containing substances can have severe detrimental effects on materials exposed to them. Hydrogen-assisted failure of iron alloys has been recognised more than a century ago. The present study aims to providing further insight into the degradation of the austenitic stainless steel AISI 304L (EN 1.4307) exposed to hydrogen. To this end, samples were electrochemically charged with the hydrogen isotope deuterium (2H, D) and analysed by scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). It was found that deuterium caused a phase transformation from the original γ austenite into ε- and α’-martensite. Despite their low solubility for hydrogen, viz. deuterium, the newly formed phases showed high deuterium concentration which was attributed to the increased density of traps. Information about the behaviour of deuterium in the material subjected to external mechanical load was gathered. A four-point-bending device was developed for this purpose. This allowed to analyse in-situ pre-charged samples in the ToF-SIMS during the application of external mechanical load. The results indicate a movement of deuterium towards the regions of highest stress. KW - ToF-SIMS KW - Hydrogen KW - Deuterium KW - AISI 304L KW - EBSD PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505142 DO - https://doi.org/10.1038/s41598-020-60370-2 VL - 10 IS - 1 SP - 3611 PB - Nature AN - OPUS4-50514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schaupp, Thomas A1 - Rhode, Michael A1 - Yahyaoui, Hamza A1 - Kannengießer, Thomas ED - Lippold, J. ED - Böllinghaus, Thomas ED - Norrish, J. ED - Scotti, A. T1 - Hydrogen-assisted cracking in GMA welding of high-strength structural steels using the modified spray arc process N2 - High-strength structural steels are used in machine, steel, and crane construction with yield strength up to 960 MPa. However, welding of these steels requires profound knowledge of three factors in terms of avoidance of hydrogen-assisted cracking (HAC): the interaction of microstructure, local stress/strain, and local hydrogen concentration. In addition to the three main factors, the used arc process is also important for the performance of the welded joint. In the past, the conventional transitional arc process (Conv. A) was mainly used for welding of high-strength steel grades. In the past decade, the so-called modified spray arc process (Mod. SA) has been increasingly used for welding production. This modified process enables reduced seam opening angles with increased deposition rates compared with the Conv. A. Economic benefits of using this arc type are a reduction of necessary weld beads and required filler material. In the present study, the susceptibility to HAC in the heat-affected zone (HAZ) of the high-strength structural steel S960QL was investigated with the externally loaded implant test. For that purpose, both Conv. A and Mod. SA were used with same heat input at different deposition rates. Both conducted test series showed same embrittlement index “EI” of 0.21 at diffusible hydrogen concentrations of 1.3 to 1.6 ml/100 g of arc weld metal. The fracture occurred in the HAZ or in the weld metal (WM). However, the test series withMod. SA showed a significant extension of the time to failure of several hours compared with tests carried out with Conv. A. KW - High-strength steel KW - GMA welding KW - Diffusible hydrogen KW - Implant test KW - Fractography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515330 DO - https://doi.org/10.1007/s40194-020-00978-0 SN - 1878-6669 SN - 0043-2288 VL - 64 IS - 12 SP - 1997 EP - 2009 PB - Springer CY - Berlin Heidelberg AN - OPUS4-51533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza A1 - da Silva, A. A1 - McEniry, E. A1 - Gault, B. A1 - Neugebauer, J. A1 - Raabe, D. T1 - Segregation-assisted spinodal and transient spinodal phase separation at grain boundaries N2 - Segregation to grain boundaries affects their cohesion, corrosion, and embrittlement and plays a critical role in heterogeneous nucleation. In order to quantitatively study segregation and low-dimensional phase separation at grain boundaries, here, we apply a density-based phase-field model. The current model describes the grain-boundary thermodynamic properties based on available bulk thermodynamic data, while the grain-boundary-density profile is obtained using atomistic simulations. To benchmark the performance of the model, Mn grain-boundary segregation in the Fe–Mn system is studied. 3D simulation results are compared against atom probe tomography measurements conducted for three alloy compositions. We show that a continuous increase in the alloy composition results in a discontinuous jump in the segregation isotherm. The jump corresponds to a spinodal Phase separation at grain boundary. For alloy compositions above the jump, we reveal an interfacial transient spinodal phase separation. The transient spinodal phenomenon opens opportunities for knowledge-based microstructure design through the chemical manipulation of grain boundaries. The proposed density-based model provides a powerful tool to study thermodynamics and kinetics of segregation and phase changes at grain boundaries. KW - Grain Boundary Spinodal KW - Densty-based Thermodynamics KW - Microstrucrue Design PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519497 DO - https://doi.org/10.1038/s41524-020-00456-7 VL - 6 IS - 1 SP - 191 PB - Nature AN - OPUS4-51949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Kulla, Hannes A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Advances in Nickel Nanoparticle Synthesis via Oleylamine Route N2 - Nickel nanoparticles are an active research area due to their multiple applications as catalysts in different processes. A variety of preparation techniques have been reported for the synthesis of these nanoparticles, including solvothermal, microwave-assisted, and emulsion techniques. The well-studied solvothermal oleylamine synthesis route comes with the drawback of needing standard air-free techniques and often space-consuming glassware. Here, we present a facile and straightforward synthesis method for size-controlled highly monodisperse nickel nanoparticles avoiding the use of, e.g., Schlenk techniques and space-consuming labware. The nanoparticles produced by this novel synthetic route were investigated using small-angle X-ray scattering, transmission electron microscopy, X-ray diffraction, and X-ray spectroscopy. The nanoparticles were in a size range of 4–16 nm, show high sphericity, no oxidation, and no agglomeration after synthesis. KW - Nanoparticle synthesis KW - Nickel nanoparticles KW - SAXS KW - TEM KW - XAS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507531 DO - https://doi.org/10.3390/nano10040713 VL - 10 IS - 4 SP - 713 PB - MDPI AN - OPUS4-50753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Halisch, M. A1 - Dlugosch, R. A1 - Prinz, Carsten T1 - Toward a better understanding of low-frequency electrical relaxation - An enhanced pore space characterization N2 - Relaxation phenomena observed in the electrical low-frequency range (approximately 1 mHz-10 kHz) of natural porous media like sandstones is often assumed to be directly related to the dominant (modal) pore throat sizes measured, for instance, with mercury intrusion porosimetry. Attempts to establish a universally valid relationship between pore size and peak Spectral Induced Polarization (SIP) relaxation time have failed, considering sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties. In addition working with characteristic relaxation times determined in Cole-Cole or Debye decomposition fits to build the relationship have not been successful. In particular, samples with narrow pore throats are often characterized by long SIP relaxation times corresponding to long “characteristic length scales” in these media, assuming that the diffusion coefficients along the electrical double layer were constant. Based on these observations, three different types of SIP relaxation can be distinguished. We present a new way of assessing complex pore spaces of very different sandstones in a multi-methodical approach to combine the benefits of mercury intrusion porosimetry, micro-computed tomography, and nuclear magnetic resonance. In this way, we achieve much deeper insight into the pore space due to the different resolutions and sensitivities of the applied methods to both pore constrictions (throats) and wide pores (pore bodies). We experimentally quantify pore aspect ratios and volume distributions within the two pore regions. We clearly observe systematic differences between three SIP relaxation types identified previously and can attribute the SIP peak relaxation times to measured characteristic length scales within our materials. We highlight selected results for a total of nine sandstones. It seems that SIP relaxation behavior depends on the size difference of the narrow pore throats to the wide pore bodies, which increases from SIP Type 1 to Type 3. KW - µ-CT KW - Spectral induced polarization KW - Nuclear magnetic resonance KW - Pore space PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509763 DO - https://doi.org/10.1190/GEO2019-0074.1 SN - 0016-8033 VL - 85 IS - 4 SP - MR257 EP - MR270 PB - Society of Exploration Geophysicists AN - OPUS4-50976 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 (NP) have become important materials for a variety of chemical technologies. The enhance surface-area-to-volume ratio of NPs is very high, 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 nanoparticles 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 catalytically active sites are accessible. 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 - Joint Polish-German Crystallographic Meeting CY - Wroclaw, Poland DA - 24.02.2020 KW - Nanoparticles KW - Synthesis KW - Catalysis PY - 2020 AN - OPUS4-51663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baer, Wolfram T1 - Detection and understanding of the chunky graphite degeneration in ferritic spheroidal graphite cast iron materials with respect to fatigue N2 - CHG is very different compared to other graphite degenerations or defects; Filigree, multi-branched string-like, 3d interconnected structure; Morphology and volumetric amount of CHG cannot be accessed by stereological interpretation of 2d section data; Field-tested, technically established method to quantify CHG in components not available; Fatigue: CHG causes substantial reduction in fatigue limit and significant increase in crack growth rate; Therefore: Avoid or exclude CHG! T2 - 4th International Symposium on Fatigue Design and Material Defects CY - Online meeting DA - 26.05.2020 KW - Ductile cast iron KW - Chunky graphite degeneration KW - Fatigue KW - Correlation microstructure to properties PY - 2020 AN - OPUS4-54409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Afantitis, A. A1 - Melagraki, G. A1 - Isigonis, P. A1 - Tsoumanis, A. A1 - Varsou, D. D. A1 - Valsami-Jones, E. A1 - Papadiamantis, A. A1 - Ellis, L.-J. A. A1 - Sarimveis, H. A1 - Doganis, P. A1 - Karatzas, P. A1 - Tsiros, P. A1 - Liampa, I. A1 - Lobaskin, V. A1 - Greco, D. A1 - Serra, A. A1 - Kinaret, P. A. S. A1 - Saarimäki, L. A. A1 - Grafström, R. A1 - Kohonen, P. A1 - Nymark, P. A1 - Willighagen, E. A1 - Puzyn, T. A1 - Rybinska-Fryca, A. A1 - Lyubartsev, A. A1 - Jensen, K. A. A1 - Brandenburg, J. G. A1 - Lofts, S. A1 - Svendsen, C. A1 - Harrison, S. A1 - Maier, D. A1 - Tamm, K. A1 - Jänes, J. A1 - Sikk, L. A1 - Dusinska, M. A1 - Longhin, E. A1 - Rundén-Pran, E. A1 - Mariussen, E. A1 - El Yamani, N. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Tropsha, A. A1 - Cohen, Y. A1 - Lesczynski, J. A1 - Hendren, C. O. A1 - Wiesner, M. A1 - Winkler, D. A1 - Suzuki, N. A1 - Yoon, T. H. A1 - Choi, J.-S. A1 - Sanabria, N. A1 - Gulumian, M. A1 - Lynch, I. T1 - NanoSolveIT Project: Driving nanoinformatics research to develop innovative and integrated tools for in silico nanosafety assessment N2 - Nanotechnology has enabled the discovery of a multitude of novel materials exhibiting unique physicochemical (PChem) properties compared to their bulk analogues. These properties have led to a rapidly increasing range of commercial applications; this, however, may come at a cost, if an association to long-term health and environmental risks is discovered or even just perceived. Many nanomaterials (NMs) have not yet had their potential adverse biological effects fully assessed, due to costs and time constraints associated with the experimental assessment, frequently involving animals. Here, the available NM libraries are analyzed for their suitability for integration with novel nanoinformatics approaches and for the development of NM specific Integrated Approaches to Testing and Assessment (IATA) for human and environmental risk assessment, all within the NanoSolveIT cloud-platform. These established and well-characterized NM libraries (e.g. NanoMILE, NanoSolutions, NANoREG, NanoFASE, caLIBRAte, NanoTEST and the Nanomaterial Registry (>2000 NMs)) contain physicochemical characterization data as well as data for several relevant biological endpoints, assessed in part using harmonized Organisation for Economic Co-operation and Development (OECD) methods and test guidelines. Integration of such extensive NM information sources with the latest nanoinformatics methods will allow NanoSolveIT to model the relationships between NM structure (morphology), properties and their adverse effects and to predict the effects of other NMs for which less data is available. The project specifically addresses the needs of regulatory agencies and industry to effectively and rapidly evaluate the exposure, NM hazard and risk from nanomaterials and nano-enabled products, enabling implementation of computational ‘safe-by-design’ approaches to facilitate NM commercialization. KW - Nanoinformatics KW - Hazard assessment KW - (Quantitative) Structure-Active Relationships KW - Safe-by-design KW - Predictive modelling PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505952 DO - https://doi.org/10.1016/j.csbj.2020.02.023 VL - 18 SP - 583 EP - 602 PB - Elsevier B.V. AN - OPUS4-50595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agostini, G. A1 - Radnik, Jörg T1 - Spectroscopy in Catalysis N2 - Knowledge-based catalyst development is always an interaction between preparation, analysis and catalytic testing. Only if these three factors fit together can success be expected. For the analytic side of this triangle, spectroscopic methods play a crucial role. Whereas with diffraction, scattering and microscopy, decisive insights into the structure and morphology of the catalysts can be obtained, spectroscopy produces new knowledge about the chemical nature of the catalyst, e.g., its bonding and valence states. KW - Spectroscopy KW - Catalysis KW - Operando KW - In situ PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506507 DO - https://doi.org/10.3390/catal10040408 VL - 10 IS - 4 SP - 408 PB - MDPI CY - Basel AN - OPUS4-50650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Analytical and Characterisation Excellence in nanomaterial risk assessment: A tiered approach Task2.5 N2 - The final results of Task 2.5 "Optimization of sample preparation for characterization of ENPs using TOF-SIMS under real-life conditions (a.) UfZ: polymer template; b.) BAM: pressing of pellets)" were presented. T2 - ACEnano General Meeting CY - Amsterdam, The Netherlands DA - 05.03.2020 KW - Nanoparticles KW - ToF-SIMS KW - Preparation PY - 2020 AN - OPUS4-50572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B. P. A1 - Cant, D.J.H. A1 - Spencer, J. A1 - Carmona-Carmona, A. J. A1 - Bushell, A. A1 - Herrara-Gómez, A. A1 - Kurokawa, A. A1 - Thissen, A. A1 - Thomas, A.G. A1 - Britton, A.J. A1 - Bernasik, A. A1 - Fuchs, A. A1 - Baddorf, A. P. A1 - Bock, B. A1 - Thellacker, B. A1 - Cheng, B. A1 - Castner, D.G. A1 - Morgan, D.J. A1 - Valley, D. A1 - Willneff, E.A. A1 - Smith, E.F. A1 - Nolot, E. A1 - Xie, F. A1 - Zorn, G. A1 - Smith, G.C. A1 - Yasukufu, H. A1 - Fenton, J. L. A1 - Chen, J. A1 - Counsell, J..D.P. A1 - Radnik, Jörg A1 - Gaskell, K.J. A1 - Artyushkova, K. A1 - Yang, L. A1 - Zhang, L. A1 - Eguchi, M. A1 - Walker, M. A1 - Hajdyla, M. A1 - Marzec, M.M. A1 - Linford, M.R. A1 - Kubota, N. A1 - Cartazar-Martínez, O. A1 - Dietrich, P. A1 - Satoh, R. A1 - Schroeder, S.L.M. A1 - Avval, T.G. A1 - Nagatomi, T. A1 - Fernandez, V. A1 - Lake, W. A1 - Azuma, Y. A1 - Yoshikawa, Y. A1 - Shard, A.G. T1 - Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene N2 - We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ∼3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ∼5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ∼4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. We also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration. KW - X-ray photoelectron spectroscopy KW - Transmission function KW - Intensity scale calibration KW - Reference spectra KW - Low-density polyethylene (LDPE) PY - 2020 DO - https://doi.org/10.1116/6.0000577 VL - 38 IS - 6 SP - 063208 AN - OPUS4-51655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Analytical & Characterisation Excellence in nanomaterial risk assessment: A tiered approach N2 - The work packages of the EU H2020 project ACEnano are presented and their activities in standardization and guidance for regulators and SMEs. T2 - ISO/TC 229 Strategy meeting CY - Online meeting DA - 10.11.2020 KW - Nanomaterials KW - Standardization KW - Risk assessment PY - 2020 AN - OPUS4-51611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Füllenbach, L.C. A1 - Perez, J. P. H. A1 - Freeman, H.M. A1 - Thomas, A.N. A1 - Mayanna, S. A1 - Parker, J. E. A1 - Göttlicher, J. A1 - Steininger, R. A1 - Radnik, Jörg A1 - Benning, L.G. A1 - Oelkers, E.H. T1 - Nanoanalytical Identification of Siderite Dissolution-Coupled Pb Removal Mechanisms from Oxic and Anoxic Aqueous Solutions N2 - Lead(II) is a toxic pollutant often found in metalcontaminated soils and wastewaters. In acidic aqueous environments, Pb(II) is highly mobile. Chemical treatment strategies of such systems therefore often include neutralization agents and metal sorbents. Since metal solubility and the retention potential of sorbents depend on the redox state of the aqueous system, we tested the efficiency of the naturally occurring redox-sensitive ferrous iron carbonate mineral siderite to remove Pb(II) from acidic aqueous solutions in batch experiments under oxic and anoxic conditions over a total of 1008 h. Siderite dissolution led to an increase in reactive solution pH from 3 to 5.3 and 6.9, while 90 and 100% of the initial aqueous Pb(II) (0.48 × 10−3 mol kg−1) were removed from the oxic and anoxic systems, respectively. Scanning and transmission electron microscopy, combined with X-ray absorption and photoelectron spectroscopy, indicated that under oxic conditions, Pb(II) was consumed by cerussite precipitation and inner-sphere surface complexation to secondary goethite. Under anoxic conditions, Pb(II) was removed by the rapid precipitation of cerussite. This efficient siderite dissolution-coupled sequestration of Pb(II) into more stable solid phases demonstrates this potential method for contaminated water Treatment regardless of the redox environment. KW - Siderite KW - X-ray absorption spectroscopy KW - X-ray photoelectron spectroscopy KW - Wastewater treatment PY - 2020 DO - https://doi.org/10.1021/acsearthspacechem.0c00180 VL - 4 IS - 11 SP - 1966 EP - 1977 PB - ACS Publication AN - OPUS4-51961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Schnack, R. A1 - Kraffert, K. A1 - Radnik, Jörg A1 - Dietrich, P. A1 - Sachse, René A1 - Krähnert, R. T1 - Role of Water in Phase Transformations and Crystallization of Ferrihydrite and Hematite N2 - The oxides, hydroxides, and oxo-hydroxides of iron belong to the most abundant materials on earth. They also feature a wide range of practical applications. In many environments, they can undergo facile phase transformations and crystallization processes. Water appears to play a critical role in many of these processes. Despite numerous attempts, the role of water has not been fully revealed yet. We present a new approach to study the influence of water in the crystallization and phase transformations of iron oxides. The approach employs model-type iron oxide films that comprise a defined homogeneous nanostructure. The films are exposed to air containing different amounts of water reaching up to pressures of 10 bar. Ex situ analysis via scanning electron microscopy, Transmission electron microscopy, selected area electron diffraction, and X-ray diffraction is combined with operando near-ambient pressure X-ray photoelectron spectroscopy to follow water-induced changes in hematite nd ferrihydrite. Water proves to be critical for the nucleation of ematite domains in ferrihydrite, the resulting crystallite orientation, and the underlying crystallization mechanism. KW - Iron oxide KW - Ferrihydrite KW - Hematite KW - Water KW - NAP-XPS KW - High pressure PY - 2020 DO - https://doi.org/10.1021/acsami.0c05253 VL - 12 SP - 38714 EP - 38722 PB - ACS Publication AN - OPUS4-51201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - Reference material for the determination of the field of view of small-area X-ray photoelectron spectrometers N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces. For evaluating the quality of such microstructures, it is crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. The aperture has a major influence on the signal-contribution from the outside. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize the FoV: The signal-contribution from the outside is reduceable down to lower than 50 %, when the aperture is 30 % of the structure dimension for our Kratos AXIS Ultra DLD system. T2 - Kratos User's Meeting 2020 CY - Online meeting DA - 21.09.2020 KW - Small-area XPS KW - Field of View KW - Imaging XPS KW - Reference Material PY - 2020 AN - OPUS4-51412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - New Test Specimen for the Determination of the Field of View of Small-Area XPS N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces. For evaluating the quality of such microstructures, it is crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. The aperture has a major influence on the signal-contribution from the outside. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize the FoV: The signal-contribution from the outside is reduceable down to lower than 50 %, when the aperture is 30 % of the structure dimension for our Kratos AXIS Ultra DLD system. T2 - Kratos User's Meeting 2020 CY - Online meeting DA - 21.09.2020 KW - Small Area XPS KW - Reference Material KW - Imaging XPS KW - Field of View PY - 2020 AN - OPUS4-51413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Surface chemical analysis surface chemical analysis of cells and biofilms N2 - The status of the planned technical report "Surface characterization of biomaterials" will be presented. T2 - ISO TC201 Meeting CY - Online meeting DA - 05.09.2020 KW - X-ray photoelectron spectroscopy KW - X-ray spectroscopy KW - Biomaterials KW - Standardization PY - 2020 AN - OPUS4-51197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Schneider, Ronald T1 - Time-variant reliability of deteriorating structural systems conditional on inspection and monitoring data N2 - The current practice of operating and maintaining deteriorating structural systems ensures acceptable levels of structural reliability, but it is not clear how efficient it is. Changing the current prescriptive approach to a risk-based approach has great potential to enable a more efficient management of such systems. Risk-based optimization of operation and maintenance strategies identifies the strategy that optimally balances the cost for controlling deterioration in a structural system with the achieved risk reduction. Inspections and monitoring are essential parts of operation and maintenance strategies. They are typically performed to reduce the uncertainty in the structural condition and inform decisions on future operation and maintenance actions. In risk-based optimization of operation and maintenance strategies, Bayesian updating is used to include information contained in inspection and monitoring data in the prediction of the structural reliability. All computations need to be repeated many times for different potential inspection and monitoring outcomes. This motivates the development of robust and efficient approaches to this computationally challenging task. The reliability of deteriorating structural systems is time-variant because the loads on them and their capacities change with time. In most practical applications, the reliability analysis of deteriorating structural systems can be approached by dividing their lifetime into discrete time intervals. The time-variant reliability problem can then be represented by a series of time-invariant reliability problems. Using this methodology as a starting point, this thesis proposes a novel approach to compute the time-variant reliability of deteriorating structural systems for which inspection and monitoring data are available. The problem is formulated in a nested way in which the prediction of the structural condition is separated from the computation of the structural reliability conditional on the structural condition. Information on the structural condition provided by inspections and monitoring is included in the reliability assessment through Bayesian updating of the system deterioration model employed to predict the structural condition. The updated system reliability is obtained by coupling the updated deterioration model with a probabilistic structural model utilized to calculate the failure probability conditional on the structural condition. This approach is the first main outcome of this thesis and termed nested reliability analysis (NRA) approach. It is demonstrated in two numerical examples considering inspected and monitored steel structures subject to high-cycle fatigue. An alternative – recently developed – approach, which also follows the strategy of discretizing time, describes deteriorating structural systems with hierarchical dynamic Bayesian networks (DBN). DBN combined with approximate or exact inference algorithms also enable the computation of the time-variant reliability of deteriorating structural systems conditional on information provided by inspection and monitoring data. In this thesis – as a proof of concept – a software prototype is developed based on the DBN approach, which can be used to assess the reliability of a corroding concrete box girder for which half-cell potential measurements are available. This is the second main outcome of this thesis. Both approaches presented in this thesis enable an integral reliability analysis of inspected and monitored structures that accounts for system effects arising from (a) the correlation among deterioration states of different structural elements, (b) the interaction between element deterioration and system failure, and (c) the indirect information gained on the condition of all unobserved structural elements from inspecting or monitoring the condition of some structural elements. Thus, both approaches enable a systemwide risk-based optimization of operation and maintenance strategies for deteriorating structural systems. The NRA approach can be implemented relatively easily with subset simulation, which is a sequential Monte Carlo method suitable for estimating rare event probabilities. Subset simulation is robust and considerably more efficient than crude Monte Carlo simulation. It is, however, still sampling-based and its efficiency is thus a function of the number of inspection and monitoring outcomes, as well as the value of the simulated event probabilities. The current implementation of the NRA approach performs separate subset simulation runs to estimate the reliability at different points in time. The efficiency of the NRA approach with subset simulation can be significantly improved by exploiting the fact that failure events in different years are nested. The lifetime reliability of deteriorating structural systems can thus be computed in reverse chronological order in a single subset simulation run. The implementation of the DBN approach is much more demanding than the implementation of the NRA approach but it has two main advantages. Firstly, the graphical format of the DBN facilitates the presentation of the model and the underlying assumptions to stakeholders who are not experts in reliability analysis. Secondly, it can be combined with exact inference algorithms. In this case, its efficiency neither depends on the number of inspection and monitoring outcomes, nor on the value of the event probabilities to be calculated. However, in contrast to the NRA approach with subset simulation, the DBN approach with exact inference imposes restrictions on the number of random variables and the dependence structure that can be implemented in the model. T3 - BAM Dissertationsreihe - 168 KW - Reliability KW - Structural systems KW - Deterioration KW - Bayesian analysis KW - Inspection KW - Monitoring KW - Zuverlässigkeit KW - Tragstrukturen KW - Schädigungsprozesse KW - Bayes'sche Analyse KW - Inspektion KW - Monitoring PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512977 SN - 1613-4249 VL - 168 SP - 1 EP - 188 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chowdhary, S. A1 - Moschner, J. A1 - Mikolajczak, D. J. A1 - Becker, M. A1 - Thünemann, Andreas A1 - Kästner, Claudia A1 - Klemczak, D. A1 - Stegemann, A.-K. A1 - Böttcher, C. A1 - Metrangolo, P. A1 - Netz, R. R. A1 - Koksch, B. T1 - The Impact of Halogenated Phenylalanine Derivatives on NFGAIL Amyloid Formation N2 - The hexapeptide hIAPP22–27 (NFGAIL) is known as a crucial amyloid core sequence of the human islet amyloid polypeptide (hIAPP) whose aggregates can be used to better understand the wild‐type hIAPP′s toxicity to β‐cell death. In amyloid research, the role of hydrophobic and aromatic‐aromatic interactions as potential driving forces during the aggregation process is controversially discussed not only in case of NFGAIL, but also for amyloidogenic peptides in general. We have used halogenation of the aromatic residue as a strategy to modulate hydrophobic and aromatic‐aromatic interactions and prepared a library of NFGAIL variants containing fluorinated and iodinated phenylalanine analogues. We used thioflavin T staining, transmission electron microscopy (TEM) and small‐angle X‐ray scattering (SAXS) to study the impact of side‐chain halogenation on NFGAIL amyloid formation kinetics. Our data revealed a synergy between aggregation behavior and hydrophobicity of the phenylalanine residue. This study introduces systematic fluorination as a toolbox to further investigate the nature of the amyloid self‐assembly process. KW - Small-angle X-ray scattering KW - SAXS KW - Nanoparticle KW - Nanostructure KW - Peptide KW - Amyloid PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518632 DO - https://doi.org/10.1002/cbic.202000373 VL - 21 IS - 24 SP - 3544 EP - 3554 PB - Wiley CY - Weinheim AN - OPUS4-51863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liebig, F. A1 - Sarhan, R. M. A1 - Schmitt, C. N. Z. A1 - Thünemann, Andreas A1 - Prietzel, C. A1 - Bargheer, M. A1 - Koetz, J. T1 - Gold Nanotriangles with Crumble Topping and their Influence on Catalysis and Surface‐Enhanced Raman Spectroscopy N2 - By adding hyaluronic acid (HA) to dioctyl sodium sulfosuccinate (AOT)‐stabilized gold nanotriangles (AuNTs) with an average thickness of 7.5±1 nm and an edge length of about 175±17 nm, the AOT bilayer is replaced by a polymeric HA‐layer leading to biocompatible nanoplatelets. The subsequent reduction process of tetrachloroauric acid in the HA‐shell surrounding the AuNTs leads to the formation of spherical gold nanoparticles on the platelet surface. With increasing tetrachloroauric acid concentration, the decoration with gold nanoparticles can be tuned. SAXS measurements reveal an increase of the platelet thickness up to around 14.5 nm, twice the initial value of bare AuNTs. HRTEM micrographs show welding phenomena between densely packed particles on the platelet surface, leading to a crumble formation while preserving the original crystal structure. Crumbles crystallized on top of the platelets enhance the Raman signal by a factor of around 20, and intensify the plasmon‐driven dimerization of 4‐nitrothiophenol (4‐NTP) to 4,4′‐dimercaptoazobenzene in a yield of up to 50 %. The resulting crumbled nanotriangles, with a biopolymer shell and the absorption maximum in the second window for in vivo imaging, are promising candidates for biomedical sensing. KW - SAXS KW - Small-angle X-ray scattering KW - Nanoparticle KW - Gold PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503977 DO - https://doi.org/10.1002/cplu.201900745 VL - 85 IS - 3 SP - 519 EP - 526 PB - Wiley-VCH Verlag CY - Weinheim AN - OPUS4-50397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saloga, Patrick E. J. A1 - Smales, Glen Jacob A1 - Clark, Adam H. A1 - Thünemann, Andreas T1 - Zinc Phosphate Nanoparticles Produced in Saliva N2 - This paper reports the formation of zinc phosphate nanoparticles from the artificial digestion of zinc chloride. Initially, the formation of amorphous primary particles with a mean radius of 1.1 nm is observed, alongside the formation of larger, protein stabilized aggregates. These aggregates, with a radius of gyration of 37 nm, are observed after 5 minutes of exposure to artificial saliva and are shown to be colloidally stable for a minimum time of two weeks. The initially formed primary particles are thought to consist of amorphous zinc phosphate, which is then transformed into crystalline Zn3(PO4)2·4H2O over the course of two weeks. Our results demonstrate that the interaction of inorganic salts with bodily fluids can induce the formation of de novo nanoparticles, which in turn, provides insights into how zinc‐enriched foods may also facilitate the formation of nanoparticles upon contact with saliva. As such, this may be considered as an undesirable (bio)mineralization. KW - SAXS KW - Digestion KW - Zinc phosphate PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514239 DO - https://doi.org/10.1002/ejic.202000521 IS - 38 SP - 3654 EP - 3661 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Tiebe, Carlo A1 - Bayat, Mehmet E. A1 - Bartholmai, Matthias T1 - Unsicherheit bei der Probenahme von Sprengstoffspuren und Detektion durch Ionenmobilitätsspektrometrie N2 - IMS trägt zur Luftfrachtsicherheit bei Geltende Luftsicherheitsgesetze verpflichten Luftsicherheitsbehörden, Flughafenbetreiber und Fluggesellschaften umfassende Sicherheitsmaßnahmen auf den Flughäfen zu ergreifen, um die Gefahr möglicher terroristischer Bedrohungen zu erkennen und zu verhindern. Wenn ein verdächtiges Objekt durch Röntgenstrahlen identifiziert wurde, kann die IMS als schnelles Analyseverfahren vor Ort orthogonal zur Radiologie eingesetzt werden, um chemische Informationen über Gefahrstoffe wie Sprengstoffe oder Drogen vor dem Abflug zu erhalten. Vor der Detektion von Sprengstoffen beginnt die Untersuchung eines verdächtigen Objekts mit der Probenahme mittels Wischprobensammlern. Eine Luftsicherheitskontrollkraft wischt dabei Oberflächen des Objekts mit einem Probensammler ab, um Partikel von Gefahrstoffen zu sammeln. Der beladene Probensammler wird anschließend in einen Probeneinlass eingeführt. Nach thermischer Desorption der gesammelten Stoffe erhält der Bediener (z. B. Luftsicherheitskontrollkraft) ein boolesches Ergebnis - "Alarm" oder "Kein Alarm". Verfahren und Ergebnisse In dieser Studie wurden drei Verfahren mit vier ECAC-zertifizierten ETD-Geräten zur Entwicklung eines Unsicherheitskonzeptes bezüglich der Probenahme (PN) angewandt: I) direkte Probenaufnahme durch lösemittelbasierten Auftrag einer bekannten Sprengstoffmenge auf einem Probensammler, II) Auftragung einer bekannten Menge eines gelösten Sprengstoffs auf einem 10 cm × 10 cm Substrat (Aluminium, Papier, Eisen und Polyvinylchlorid) und manuelle PN nach Lösemittelverdampfung, III) lösemittelbasierter Sprengstoffauftrag auf eine PTFE- oder PTFE-beschichtete Glasfaseroberfläche, nach Lösemittelverdunstung trockene Übertragung auf das zu beprobende Substrat zur PN. Nach dem binären Regressionsverfahren wurde die funktionale Abhängigkeit der Detektionswahrscheinlichkeit von einer bekannten Sprengstoffmasse mit einer Logit-Funktion beschrieben: POD=1/(1+e^(-A·(m-B))). Dabei ist POD die Wahrscheinlichkeit der Detektion für eine bekannte Sprengstoff-Masse, die Parameter A (logistische Wachstumsrate der Kurve) und B (m-Wert des Mittelpunktes des Sigmoids) sind geschätzte Parameter nach der Methode der kleinsten Quadrate, und m ist die Sprengstoffmasse. Das entwickelte Messunsicherheitsmodell kombiniert quantitative Ergebnisse aus Wägen, Lösen und Pipettieren sowie qualitative Ergebnisse - "Alarm" oder "Kein Alarm" und die Unsicherheit der PN. Identifizierte Unsicherheitsursachen sind die Durchführung der Wischprobenahme, Staub, Lösemitteleffekte und die Unsicherheit bei der Herstellung von Testlösungen. T2 - 8. IMS-Anwendertreffen CY - Potsdam, Germany DA - Veranstaltung wurde abgesagt - Meeting was cancelled KW - IMS KW - Ionenmobilitätsspektrometrie KW - Wischprobenahme KW - binäres Regressionsverfahren KW - ETD KW - Sprengstoffspurendetektion PY - 2020 VL - 2020 SP - 9 EP - 9 PB - Universität Potsdam CY - Potsdam AN - OPUS4-51136 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eberwein, Robert A1 - Rogge, Andreas A1 - Behrendt, F. A1 - Knaust, Christian T1 - Dispersion Modeling of LNG-Vapor on Land – A CFD-Model Evaluation Study N2 - Based on methane from renewable resources, LNG is an alternative fuel for heavy and long-distance traffic in land transport. Contrary to its positive properties, the fuel contains risks from an explosion and extremely low temperatures for personal and infrastructure safety. CFD-models are suitable for doing risk analyses for arbitrary scenarios. For examining how to model for risk research the dispersion of LNG-vapor, this paper contains a model variant study, with an evaluation by experiments. This paper describes the use of the CFD-code ANSYS Fluent for simulating experiments of the ‘LNG Safety Program Phase II‘. The content of the well-documented experiments was the research of the vaporization rate of LNG on land and the dispersion of LNG-vapor in the air. Based on the comparison to two experiments, overall 12 CFD-model variants with varying thermal and turbulence parameters were examined how they affect the transient LNG-vapor dispersion in air. The definition of turbulence-boundary-condition at the domain borders had the biggest impact on modeling, followed by the turbulence model. The most accurate model variant had been applied for observing the spreading behavior of LNG-vapor in the air after evaporation on land and analyzing the influence of the LNG-composition to the dispersion. The results show that the mixture of LNG-vapor and the air in the free field is cooler than the ambient air and spreads like a heavy gas on the ground. KW - LNG KW - CFD KW - Heavy gas KW - Model evaluation PY - 2020 DO - https://doi.org/10.1016/j.jlp.2020.104116 VL - 65 SP - 104116 PB - Elsevier Ltd. AN - OPUS4-50697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lumpe, H. A1 - Menke, A. A1 - Haisch, C. A1 - Mayer, P. A1 - Kabelitz, Anke A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Block, T. A1 - Pöttgen, R. A1 - Emmerling, Franziska A1 - Daumann, L. J. T1 - The Earlier the Better: Structural Analysis and Separation of Lanthanides with Pyrroloquinoline Quinone N2 - Lanthanides (Ln) are critical raw materials, however, their mining and purification have a considerable negative environmental impact and sustainable recycling and separation strategies for these elements are needed. In this study, the precipitation and solubility behavior of Ln complexes with pyrroloquinoline quinone (PQQ), the cofactor of recently discovered lanthanide (Ln) dependent methanol Dehydrogenase (MDH) enzymes, is presented. In this context, the molecular structure of a biorelevant europium PQQ complex was for the first time elucidated outside a protein environment. The complex crystallizes as an inversion symmetric dimer, Eu2PQQ2, with binding of Eu in the biologically relevant pocket of PQQ. LnPQQ and Ln1Ln2PQQ complexes were characterized by using inductively coupled Plasma mass spectrometry (ICP-MS), infrared (IR) spectroscopy, 151Eu-Mössbauer spectroscopy, X-ray total scattering, and Extended X-ray absorption fine structure (EXAFS). It is shown that a natural enzymatic cofactor is capable to achieve Separation by precipitation of the notoriously similar, and thus difficult to separate, lanthanides to some extent. KW - Lanthanides KW - Structural Analysis KW - Separation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510821 DO - https://doi.org/10.1002/chem.202002653 SN - 0947-6539 VL - 26 SP - 1 EP - 8 PB - WILEY-VCH Verlag GmbH & co. KGaA AN - OPUS4-51082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gluth, Gregor A1 - Ebell, Gino A1 - Hlavacek, Petr A1 - Mietz, Jürgen T1 - Chloride‐induced steel corrosion in alkali‐activated fly ash mortar: Increased propensity for corrosion initiation at defects N2 - Chloride contents at the steel–mortar interface that initiate steel corrosion were determined for carbon steel in alkali‐activated fly ash mortar for three different exposure conditions: exposure to 1 M NaCl solution; leaching in deionized water and then exposure to 1 M NaCl solution; and leaching in deionized water, aging in air at 20°C and natural CO2 concentration, and then exposure to 1 M NaCl solution. For comparison, a Portland cement mortar, exposed to 1 M NaCl solution, was studied. The median values of the corrosion‐initiating chloride contents (average over the full length of the rebar) in the alkali‐activated fly ash mortar varied between 0.35 and 1.05 wt% Cl with respect to binder, consistently lower than what was obtained for the Portland cement mortar, but with no clear trend regarding the exposure conditions. For most of the alkali‐activated fly ash mortar specimens, preferential corrosion at the connection between the working electrode and the external measurement setup was observed, while preferential corrosion did not occur for the Portland cement mortar. Scanning electron microscopy and auxiliary experiments in synthetic solutions indicated that this behavior was caused by inhomogeneities at the steel–mortar interface in the alkali‐activated mortar, likely due to its peculiar rheological properties in the fresh state. KW - Alkali-activated materials KW - Steel corrosion KW - Critical chloride content KW - Steel-concrete interface PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507268 DO - https://doi.org/10.1002/maco.202011541 VL - 71 IS - 5 SP - 749 EP - 758 PB - Wiley-VCH AN - OPUS4-50726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Streli, C. A1 - Radtke, Martin T1 - On the way to full-field X-ray fluorescence spectroscopy imaging with coded apertures N2 - Imaging with X-rays is a challenging field, due to the optical properties of X-rays. The fabrication of appropriate optics is usually expensive and requires an elaborate manufacturing process. One simpler and less expensive possibility of imaging high energy radiation is coded aperture imaging, a technique well established in astrophysics and also used in nuclear medicine or radiation detection, e.g., for nuclear decommissioning. Our aim is to adapt coded aperture imaging for X-ray fluorescence spectroscopy in the nearfield. In this work we show theoretical considerations and preliminary simulations of Image formation through a coded aperture and three different reconstruction methods to prepare the experiments. We used a new mask based on an inverted modified uniformly redundant array (MURA) that could be used for the construction of a decoding mask for all investigated geometrical arrangements. The most commonly used reconstruction method, convoluting the detected image with a Decoding mask, does not always deliver satisfactory results. This is more noticeable for small distances between the object, mask and detector. Hence, we developed two new reconstruction methods, one based on iterative algebraic optimization and another one based on a genetic algorithm. Both show good performance even in those cases where the convolution method fails. This provides a basis for further investigations of the ideal parameters for near field coded aperture imaging and refinements of the algorithms. We performed first measurements with a coded aperture at the BAMline at BESSY II and could successfully reconstruct a test object from the obtained recorded images. KW - X-ray fluorescence spectroscopy KW - Coded aperture KW - Imaging KW - Iterative reconstruction PY - 2020 DO - https://doi.org/10.1039/c9ja00232d VL - 35 IS - 2 SP - 347 EP - 356 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kulow, Anicó A1 - Kabelitz, Anke A1 - Grunewald, C. A1 - Seidel, R. A1 - Chapartegui-Arias, Ander A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Beyer, S. T1 - Observation of early ZIF-8 crystallization stages with X-ray absorption spectroscopy N2 - The present study investigates early stages of ZIF-8 crystallization up to 5 minutes post mixing of precursor solutions. Dispersive X-ray Absorption Spectroscopy (DXAS) provides a refined understanding of the evolution of the coordination environment during ZIF-8 crystallization. Linear Combination Fiting (LCF) suggests tetrakis(1-methylimidazole)zinc2+ to be a suitable and stable mononuclear structure analogue for some early stage ZIF-8 intermediates. Our results pave the way for more detailed studies on physico-chemical aspects of ZIF-8 crystallization to better control tailoring ZIF-8 materials for specific applications. KW - In-situ KW - XANES KW - ZIF-8 KW - Crystallization PY - 2020 DO - https://doi.org/10.1039/D0SM01356K SN - 1744-6848 VL - 17 IS - 2 SP - 331 EP - 334 PB - Royal Scociety of Chemistry AN - OPUS4-51723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunkel, B. A1 - Kabelitz, Anke A1 - de Oliveira Guilherme Buzanich, Ana A1 - Wohlrab, S. T1 - Increasing the Efficiency of Optimized V-SBA-15 Catalysts in the Selective Oxidation of Methane to Formaldehyde by Artificial Neural Network Modelling N2 - The present study investigates the possibility of improving the selective oxidation of methane to formaldehyde over V-SBA-15 catalysts in two different ways. In a classical approach of catalyst optimization, the in situ synthesis of V-SBA-15 catalysts was optimized with regard to the applied pH value. Among the set of catalysts synthesized, a higher amount of incorporated vanadium, a higher content of polymeric VOx species as well as a less ordered structure of the support material were observed by increasing the pH values from 2.0 to 3.0. An optimum in performance during the selective oxidation of methane to formaldehyde with respect to activity and selectivity was found over V-SBA-15 prepared at a pH value of 2.5. With this knowledge, we have now evaluated the possibilities of reaction control using this catalyst. Specifically, artificial neural network modelling was applied after the collection of 232 training samples for obtaining insight into the influence of different reaction parameters (temperature; gas hourly space velocity (GHSV); and concentration of O2, N2 and H2O) onto methane conversion and selectivity towards formaldehyde. This optimization of reaction conditions resulted in an outstanding high space-time yield of 13.6 kgCH2O∙kgcat∙h−1 KW - Artificial neural network modelling KW - Selective oxidation KW - Molecular VOx catalysts KW - Formaldehyde PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517420 DO - https://doi.org/10.3390/catal10121411 VL - 10 IS - 12 SP - 1411 PB - MDPI AN - OPUS4-51742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Olivera, Paulo A1 - Michalchuk, Adam A1 - de Oliveira Guilherme Buzanich, Ana A1 - Bienert, Ralf A1 - Torresi, R. A1 - Camargo, P. A1 - Emmerling, Franziska T1 - Tandem X-ray absorption spectroscopy and scattering for in situ time-resolved monitoring of gold nanoparticle mechanosynthesis N2 - Current time-resolved in situ approaches limit the scope of mechanochemical investigations possible. Here we develop a new, general approach to simultaneously follow the evolution of bulk atomic and electronic structure during a mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based X-ray methods: X-ray absorption spectroscopy (XAS) and X-ray diffraction. We apply this method to investigate the bottom-up mechanosynthesis of technologically important Au micro and nanoparticles in the presence of three different reducing agents, hydroquinone, sodium citrate, and NaBH4. Moreover, we show how XAS offers new insight into the early stage generation of growth species (e.g. monomers and clusters), which lead to the subsequent formation of nanoparticles. These processes are beyond the detection capabilities of diffraction methods. This combined X-ray approach paves the way to new directions in mechanochemical research of advanced electronic materials. KW - Mechanochemistry KW - XANES KW - X-ray diffraction KW - Nano particles PY - 2020 DO - https://doi.org/10.1039/d0cc03862h SN - 1364-548X VL - 56 SP - 10329 EP - 10332 PB - Royal Society of Chemistry AN - OPUS4-51760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winnefeld, F. A1 - Gluth, Gregor A1 - Bernal, S. A. A1 - Bignozzi, M. C. A1 - Carabba, L. A1 - Chithiraputhiran, S. A1 - Dehghan, A. A1 - Dolenec, S. A1 - Dombrowski-Daube, K. A1 - Dubey, A. A1 - Ducman, V. A1 - Yu, J. A1 - Peterson, K. A1 - Stephan, D. A1 - Provis, J. L. T1 - RILEM TC 247-DTA round robin test: sulfate resistance, alkali-silica reaction and freeze–thaw resistance of alkali-activated concretes N2 - The RILEM technical committee TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ conducted a round robin testing programme to determine the validity of various durability testing methods, originally developed for Portland cement based-concretes, for the assessment of the durability of alkali-activated concretes. The outcomes of the round robin tests evaluating sulfate resistance, alkali-silica reaction (ASR) and freeze–thaw resistance are presented in this contribution. Five different alkali-activated concretes, based on ground granulated blast furnace slag, fly ash, or metakaolin were investigated. The extent of sulfate damage to concretes based on slag or fly ash seems to be limited when exposed to an Na2SO4 solution. The mixture based on metakaolin showed an excessive, very early expansion, followed by a dimensionally stable period, which cannot be explained at present. In the slag-based concretes, MgSO4 caused more expansion and visual damage than Na2SO4; however, the expansion limits defined in the respective standards were not exceeded. Both the ASTM C1293 and RILEM AAR-3.1 test methods for the determination of ASR expansion appear to give essentially reliable identification of expansion caused by highly reactive aggregates. Alkali-activated materials in combination with an unreactive or potentially expansive aggregate were in no case seen to cause larger expansions; only the aggregates of known very high reactivity were seen to be problematic. The results of freeze–thaw testing (with/without deicing salts) of alkali-activated concretes suggest an important influence of the curing conditions and experimental conditions on the test outcomes, which need to be understood before the tests can be reliably applied and interpreted. KW - Alkali-activated materials KW - Sulfate attack KW - Alkali silica reaction KW - Alkali aggregate reaction KW - Freeze-thaw attack PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515527 DO - https://doi.org/10.1617/s11527-020-01562-0 VL - 53 IS - 6 SP - 140 PB - Springer Nature AN - OPUS4-51552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gluth, Gregor A1 - Arbi, K. A1 - Bernal, S. A. A1 - Bondar, D. A1 - Castel, A. A1 - Chithiraputhiran, S. A1 - Dehghan, A. A1 - Dombrowski-Daube, K. A1 - Dubey, A. A1 - Ducman, V. A1 - Peterson, K. A1 - Pipilikaki, P. A1 - Valcke, S. L. A. A1 - Ye, G. A1 - Zuo, Y. A1 - Provis, J. L. T1 - RILEM TC 247-DTA round robin test: carbonation and chloride penetration testing of alkali-activated concretes N2 - Many standardised durability testing methods have been developed for Portland cement-based concretes, but require validation to determine whether they are also applicable to alkali-activated materials. To address this question, RILEM TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ carried out round robin testing of carbonation and chloride penetration test methods, applied to five different alkali-activated concretes based on fly ash, blast furnace slag or metakaolin. The methods appeared overall to demonstrate an intrinsic precision comparable to their precision when applied to conventional concretes. The ranking of test outcomes for pairs of concretes of similar binder chemistry was satisfactory, but rankings were not always reliable when comparing alkali-activated concretes based on different precursors. Accelerated carbonation testing gave similar results for fly ash-based and blast furnace slag-based alkali-activated concretes, whereas natural carbonation testing did not. Carbonation of concrete specimens was observed to have occurred already during curing, which has implications for extrapolation of carbonation testing results to longer service life periods. Accelerated chloride penetration testing according to NT BUILD 443 ranked the tested concretes consistently, while this was not the case for the rapid chloride migration test. Both of these chloride penetration testing methods exhibited comparatively low precision when applied to blast furnace slag-based concretes which are more resistant to chloride ingress than the other materials tested. KW - Alkali-activated materials KW - Durability KW - Carbonation KW - Chloride penetration KW - Concrete PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504045 DO - https://doi.org/10.1617/s11527-020-1449-3 SN - 1359-5997 SN - 1871-6873 VL - 53 IS - 1 SP - 21 PB - Springer Nature AN - OPUS4-50404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lumpe, H. A1 - Menke, Annika A1 - Haisch, C. A1 - Mayer, P. A1 - Kabelitz, Anke A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Block, T. A1 - Pöttgen, R. A1 - Emmerling, Franziska A1 - Daumann, L. T1 - The Earlier the Better: Structural Analysis and Separation of Lanthanides with Pyrroloquinoline Quinone N2 - Lanthanides (Ln) are critical raw materials, however, their mining and purification have a considerable negative environmental impact and sustainable recycling and separation strategies for these elements are needed. In this study, the precipitation and solubility behavior of Ln complexes with pyrroloquinoline quinone (PQQ), the cofactor of recently discovered lanthanide (Ln) dependent methanol dehydrogenase (MDH) enzymes, is presented. In this context, the molecular structure of a biorelevant europium PQQ complex was for the first time elucidated outside a protein environment. The complex crystallizes as an inversion symmetric dimer, Eu2PQQ2, with binding of Eu in the biologically relevant pocket of PQQ. LnPQQ and Ln1Ln2PQQ complexes were characterized by using inductively coupled plasma mass spectrometry (ICP‐MS), infrared (IR) spectroscopy, 151Eu‐Mössbauer spectroscopy, X‐ray total scattering, and extended X‐ray absorption fine structure (EXAFS). It is shown that a natural enzymatic cofactor is capable to achieve separation by precipitation of the notoriously similar, and thus difficult to separate, lanthanides to some extent. KW - PQQ KW - Lanthanoide KW - Coordination chemistry KW - Rare earth elements separations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512707 DO - https://doi.org/10.1002/chem.202002653 VL - 26 IS - 44 SP - 10133 EP - 10139 AN - OPUS4-51270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Rakotondrajoa, A. T1 - Machine learning based quantification of synchrotron radiation-induced X-ray fluorescence measurements - a case study N2 - In this work, we describe the use of artificial neural networks for the quantification of X-ray fluorescence measurements. The training data were generated using Monte Carlo simulation, which avoided the use of adapted reference materials. The extension of the available data set by means of an ANN to generate additional data was demonstrated. Particular emphasis was put on the comparability of simulated and experimental data and how the influence of deviations can be reduced. The search for the optimal hyperparameter, manual and automatic, is also described. For the presented case, we were able to train a network with a mean absolute error of 0.1 weight percent for the synthetic data and 0.7 weight percent for a set of experimental data obtained with certified reference materials. KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron KW - Neural network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519008 DO - https://doi.org/10.1088/2632-2153/abc9fb SP - 1 EP - 16 PB - IOP Publishing AN - OPUS4-51900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüsken, Götz A1 - Wagner, L.-C. A1 - Gluth, Gregor A1 - Pirskawetz, Stephan A1 - Kühne, Hans-Carsten T1 - Application of Steel Fibres in Alkali-Activated Mortars N2 - Alkali-activated materials are ideal for the repair of concrete structures in harsh environmental conditions due to their high durability in chemically aggressive environments. However, slag-based mortars, in particular, are prone to shrinkage and associated cracks. In this respect, the application of steel fibres is one solution to reduce the formation of shrinkage induced cracks and to improve post cracking behaviour of these mortars. This study investigated the influence of two different types of steel fibres on the tensile properties of two alkali-activated mortars. Direct tensile tests and single fibre pull-outs were performed to analyse the determining failure modes both on macro and micro scale. Mechanical testing was accompanied by non-destructive testing methods such as digital image correlation and acoustic emission for a detailed analysis of the fracture process. T2 - Local Mechanical Properties - LMP 2019 CY - Prague, Czech Republic DA - 06.11.2019 KW - Alkali-activated materials KW - Fibre pull-out KW - Steel fibres KW - Tensile strength PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509291 UR - https://ojs.cvut.cz/ojs/index.php/APP/article/view/6695 DO - https://doi.org/10.14311/APP.2020.27.0090 VL - 27 SP - 90 EP - 95 CY - Prague, Czech Republic AN - OPUS4-50929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -