TY - CONF A1 - Casperson, Ralf T1 - Datenformate für die zerstörungsfreie Prüfung N2 - Der Vortrag gibt eine Übersicht über die Versuche der Vergangenheit, ein standardisiertes Datenformat für die zerstörungsfreie Prüfung zu etablieren. T2 - 4. Sitzung DGZfP FA ZfP 4.0 UA Schnittstellen CY - Stockelsdorf, Germany DA - 19.02.2020 KW - ZfP KW - Datenformat KW - TRAPPIST KW - STEP KW - NDTML KW - DICONDE KW - HDF5 PY - 2020 AN - OPUS4-50448 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulze-Makuch, D. A1 - Haque, S. A1 - Beckles, D. A1 - Schmitt-Kopplin, P. A1 - Harir, M. A1 - Schneider, Beate A1 - Stumpp, C. A1 - Wagner, D. T1 - A chemical and microbial characterization of selected mud volcanoes in Trinidad reveals pathogens introduced by surface water and rain water N2 - Terrestrial mud volcanoes are unique structures driven by tectonic pressure and fluids from the deep subsurface. These structures are mainly found in active tectonic zones, such as the area near the Los Bajos Fault in Trinidad. Here we report a chemical and microbiological characterization of three mud volcanoes, which included analyses of multiple liquid and solid samples from the mud volcanoes. Our study confirms previous suggestions that at least some of the mud volcano fluids are a mixture of deeper salt-rich water and surficial/precipitation water. No apparent water quality differences were found between sampling sites north and south of a major geological fault line. Microbiological analyses revealed diverse communities, both aerobic and anaerobic, including sulfate reducers, methanogens, carbon dioxide fixing and denitrifying bacteria. Several identified species were halophilic and likely derived from the deeper salt-rich subsurface water, while we also cultivated pathogenic species from the Vibrionaceae, Enterobacteriaceae, Shewanellaceae, and Clostridiaceae. These microorganisms were likely introduced into the mud volcano fluids both from surface water or shallow ground-water, and perhaps to a more minor degree by rain water. The identified pathogens are a major health concern that needs to be addressed. KW - Water stable isotope analysis KW - Mud volcanoe fluids KW - Metabolomics PY - 2020 DO - https://doi.org/10.1016/j.scitotenv.2019.136087 VL - 707 SP - 136087 PB - Elsevier B.V. AN - OPUS4-50499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - On-line hyphenation of CE with multicollector-ICP-MS for species-specific isotopic analysis of sulfur N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a future field could be species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - Capillary electrophoresis KW - Hyphenated techniques KW - Isotopic analysis KW - Multicollector-ICP-MS KW - Speciation analysis PY - 2020 AN - OPUS4-50501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus T1 - HR-CS-GF-MAS as a new screening method for emerging pollutants - per- and polyfluorinated substances in the environment N2 - The introduction of fluorine in organic molecules leads to new chemical/physical properties. Especially in the field of pharmaceuticals, fluorinated organic molecules are becoming more and more popular and at present amount up to 25% of market share, with an upward trend. The main benefits of fluorinated pharmaceuticals are: (i) enhanced fat solubility; (ii) enhanced interaction of catalytic-center of enzymes with fluorine-drugs; (iii) a delayed metabolism within the human body. Highly fluorinated organic substances are also used in technical applications (e.g. coatings, fire-extinguishing agents). Due to the broad variety of fluorinated substances and increasing production volumes numerous and up to date unknown fluorine-species are most likely to be present in the (aquatic) environment. Analytical methods to assess the degree of contamination of surface waters with organically bound fluorine are highly needed and up to now only combustion ion chromatography based method is available, which is relatively laborious. Since a few years’ high resolution-continuum source-graphite furnace atomic absorption spectrometers (HR-CS-GFAAS) are commercially available from Analytik Jena. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled. Thus, fluoride is detectable upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF). Just recently, we applied this technique for total fluorine (mainly dissolved fluoride) analysis in river water samples. In the present work a HR-CS-GFMAS method for extractable organically bound fluorine (EOF) analysis in surface water samples was developed by us. The method is based on SPE extraction of organically bound fluorine even in the presence of high fluoride concentrations followed by HR-CS-GFMAS analysis upon elution. Due to high enrichment factors, LODs in the low ng/L range were achieved. We successfully applied our SPE HR-CS-GFMAS method to Rhine water samples and EOF in the range of about 50-300 ng/L was detectable. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - SPE HR-CS GF MAS PY - 2020 AN - OPUS4-50503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus T1 - HR-CS-GF-MAS as a new screening method for emerging pollutants - per- and polyfluorinated substances in the environment N2 - The introduction of fluorine in organic molecules leads to new chemical/physical properties. Especially in the field of pharmaceuticals, fluorinated organic molecules are becoming more and more popular and at present amount up to 25% of market share, with an upward trend. The main benefits of fluorinated pharmaceuticals are: (i) enhanced fat solubility; (ii) enhanced interaction of catalytic-center of enzymes with fluorine-drugs; (iii) a delayed metabolism within the human body. Highly fluorinated organic substances are also used in technical applications (e.g. coatings, fire-extinguishing agents). Due to the broad variety of fluorinated substances and increasing production volumes numerous and up to date unknown fluorine-species are most likely to be present in the (aquatic) environment. Analytical methods to assess the degree of contamination of surface waters with organically bound fluorine are highly needed and up to now only combustion ion chromatography based method is available, which is relatively laborious. Since a few years’ high resolution-continuum source-graphite furnace atomic absorption spectrometers (HR-CS-GFAAS) are commercially available from Analytik Jena. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled. Thus, fluoride is detectable upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF). Just recently, we applied this technique for total fluorine (mainly dissolved fluoride) analysis in river water samples. In the present work a HR-CS-GFMAS method for extractable organically bound fluorine (EOF) analysis in surface water samples was developed by us. The method is based on SPE extraction of organically bound fluorine even in the presence of high fluoride concentrations followed by HR-CS-GFMAS analysis upon elution. Due to high enrichment factors, LODs in the low ng/L range were achieved. We successfully applied our SPE HR-CS-GFMAS method to Rhine water samples and EOF in the range of about 50-300 ng/L was detectable. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - SPE HR-CS GF MAS PY - 2020 AN - OPUS4-50504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Corrigendum to "Measurement of the radiative energy output of flash lamps by means of thermal thin probes" [Infrared Phys. Technol. 67 (2014) 363-370] N2 - This is a corrigendum to the original article "Measurement of the radiative energy output of flash lamps by means of thermal thin probes" that was published in the journal "Infrared physics & technology", vol. 67 (2014), pp. 363-370. PY - 2018 DO - https://doi.org/10.1016/j.infrared.2017.11.011 SN - 1350-4495 VL - 91 SP - 278 PB - Elsevier CY - Amsterdam AN - OPUS4-50505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora T1 - Sulfur isotope dilution ICP MS for traceable protein quantification N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful method for the matrix-independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms has gained recognition in the last decade, considering that established quantification methods like organic mass spectrometry depend on labelling of the target protein or the existence of matched protein and peptide standards. The need for reliable quantification of proteins is continuously growing, but only a limited number of well-characterized and quantified protein standards are available so far. Accurately quantified, traceable protein standards are necessary to ensure comparability of measurements between laboratories, not only in basic research but also in a clinical context. One example of this is the Alzheimer’s disease biomarker tau protein. However, existing tau standards lack comparability, emphasizing the need for a well-quantified protein standard. Therefore, we developed a method for the quantification of pure proteins via sulfur isotope dilution ICP-MS (IDMS). As sulfur is present in two amino acids, cysteine and methionine, it exists in nearly all proteins and can be used for the quantification of proteins of known stoichiometry. We employed simple offline strategies for the separation of non-protein bound sulfur species. Quantification of these contaminations by IDMS allows for correction of the protein content and enables reliable protein quantification. We report the protein mass fractions of a standard reference material and commercially available proteins determined by sulfur IDMS, including the expanded uncertainties. The developed method can be applied for the reliable and traceable quantification of pure proteins for use as in-house standards. Here, we successfully used this method for the quantification of the tau protein. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - ICP-MS KW - Isotope dilution KW - Protein KW - Quantification KW - Tau protein PY - 2020 AN - OPUS4-50510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hein, Sebastian T1 - Ansätze und Herausforderungen für das QM-System einer Ressortforschungseinrichtung N2 - Die BAM betreibt ein QM-System, das stark an der DIN EN ISO/IEC 17025 orientiert ist und welches in den meisten Fachabteilungen durch Akkreditierungen untersetzt wird. Mit der Zunahme der Forschungsaktivitäten in den letzten Jahren ist der DFG-Kodex zur Sicherstellung der Guten wissenschaftlichen Praxis deutlicher in den Fokus des Qualitätsmanagements gerückt. Der Vortrag zeigt auf, welche QM-Anforderungen an die Leistungen der BAM gestellt werden und mit welchen Instrumenten sie diese umsetzt, so dass Gute wissenschaftliche Praxis und Akkreditierungen gut harmonieren können. T2 - QM-Seminar; Robert-Koch-Institut CY - Berlin, Germany DA - 21.01.2020 KW - Qualitätsmanagement KW - Gute wissenschaftliche Praxis PY - 2020 AN - OPUS4-50311 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Combined Raman and LIBS using Spatial Heterodyne Spectrometer with High Repetition Rate Laser N2 - Spatial heterodyne spectroscopy is used for Raman and laser-induced breakdown spectroscopy of six rocks with various mineral content, using high repetition rate diode-pumped solid state lasers. While LIBS data are obtained for all samples, Raman signal was determined only for half of those. This work shows that it is possible to combine LIBS and Raman spectrometry into a single instrument consisting of a DPSS laser for excitation and SHS for spectral recording. For better results and gain from complementary spectrochemical information that the system provides, it is necessary to optimize light collection. T2 - 2020 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 13.01.2020 KW - Laser-Induced Background Spectroscopy KW - Spatial heterodyne spectroscopy KW - Raman spectroscopy PY - 2020 AN - OPUS4-50265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauschkin, Maik A1 - Bulling, Jannis A1 - Lugovtsova, Yevgeniya A1 - Wasmer, P. A1 - Prager, Jens T1 - Bestimmung von Materialparametern aus dem dispersiven Verhalten geführter Wellen mittels neuronaler Netze N2 - Damit eine Simulationsrechnung, beispielsweise mit einer FEM-Software, eine ausreichend hohe Genauigkeit erreicht, muss vorausgesetzt werden, dass die Modellparameter eine sehr hohe Güte aufweisen. Die genaue Kenntnis der Materialparameter ist dabei von besonderer Bedeutung. Um diese Parameter bestimmen zu können, müssen die verwendeten Werkstoffe messtechnisch charakterisiert werden. Neben anderen Ansätzen sind dafür akustische Verfahren im Ultraschallbereich geeignet. Für dünnwandige und plattenförmige Materialien können aus den sich ausbreitenden geführten Wellen messtechnisch Dispersionskurven bestimmt und aus diesen die Materialparameter abgeleitet werden. Da für die Signalverarbeitung und für Optimierungsaufgaben aktuell zunehmend Machine Learning Tools zum Einsatz kommen, stellt sich die Frage, ob diese Werkzeuge auch für die Ermittlung der Materialparameter aus den gemessenen Dispersionskurven eingesetzt werden können. In der vorgestellten Untersuchung soll ein Convolutional Neural Network aufgestellt werden, welches aus Dispersionsbildern Muster extrahiert und aus diesen eine Schätzung für die Materialparameter ermittelt. Um die Machbarkeit dieses Ansatzes zu prüfen, werden zunächst nur isotrope Materialien betrachtet. Für das Netz werden mit der Scaled-Boundary-Finite-Element-Methode synthetische Daten für das Trainieren und Validieren generiert. Zusätzlich werden die Hyperparameter des neuronalen Netzes variiert, um ein optimales Model für die Schätzung zu finden. Anschließend kann das Netz mit experimentellen Daten getestet und das Ergebnis hinsichtlich der Genauigkeit bewertet werden. T2 - DAGA 2020 - 46. Jahrestagung für Akustik CY - Meeting was canceled DA - 16.03.2020 KW - Machinelles Lernen KW - Geführte Ultraschallwellen KW - Materialcharakterisierung KW - Elastische Konstanten KW - Isotrope Materialien PY - 2020 SN - 978-3-939296-17-1 SP - 571 EP - 574 PB - Deutsche Gesellschaft für Akustik e.V. CY - Berlin AN - OPUS4-50765 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Galbacs, G. A1 - Keri, A. A1 - Kalomista, I. A1 - Kovacs-Szeles, E. A1 - Gornushkin, Igor B. T1 - Deuterium analysis by inductively coupled plasma mass spectrometry using polyatomic species: An experimental study supported by plasma chemistry modeling N2 - based on the use of the signal from hydrogen-containing polyatomic ions formed in the inductively coupled plasma. Prior to analytical experiments, a theoretical study was performed to assess the concentration of polyatomic species present in an equilibrium Ar-O-D-H plasma, as a function of temperature and stoichiometric composition. It was established that the highest sensitivity and linearity measurement of D concentration in a wide range can be achieved by monitoring the ions of D2 and ArD, at masses 4 and 42, respectively. Results of the calculations are in good agreement with the experiments. Signal stability, spectral interferences, as well as the effect of plasma parameters were also assessed. Under optimized conditions, the limit of detection (LOD) was found to be 3 ppm atom fraction for deuterium when measured as ArD (in calcium and potassium free water), or 78 ppm when measured as D2. The achieved LOD values and the 4 to 5 orders of magnitude dynamic range easily allow the measurement of deuterium concentrations at around or above the natural level, up to nearly 100% (or 1 Mio ppm) in a standard quadrupole ICP-MS instrument. An even better performance is expected from the method in high resolution ICP-MS instruments equipped with low dead volume sample introduction systems KW - ICP MS KW - Deuterium KW - Deuterium enriched water PY - 2020 DO - https://doi.org/10.1016/j.aca.2020.01.011 VL - 1104 SP - 28 EP - 37 PB - Elsevier B.V. AN - OPUS4-50777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marquardt, Julien T1 - Investigating the morphology of nanostructured mixed metal oxides (Ir/TiOx) and its impact on the electrocatalytic OER-activity N2 - The electrocatalytic conversion of water into molecular hydrogen and oxygen under the utilization of excess renewable energies, such as wind power, photovoltaics and hydroelectric power is one possible pathway to establish a sustainable hydrogen economy. The obtained hydrogen is either stored and used in a fuel cell or consumed on-site in industrial applications. Water electrolysis systems (WES) are based on two half cell reactions, such as oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) which both proceed simultaneously. The OER suffers from slow reaction kinetics and thus limits the overall performance. The most promising compounds in acidic electrolysis are IrO2 and RuO2. Due to their rare abundance and extremely high price a wide use of acidic WES was prevented. Lowering the catalysts noble metal content by mixing iridium with titanium reduces the production costs. Thin films are produced by dip coating a solution of metal oxide precursors alongside with a polymer template dissolved in ethanol. The obtained samples are subsequently calcined to the remove the template and adjust crystallinity. Finally, an additional iridium deposition step was performed on the outer surface plane area. Understanding the influence of structural and morphological aspects on the OER-activity is beneficial to further optimize WES. The current presentation will thus give detailed insights to structural aspects obtained by Raman spectroscopy, small- and wide-angle X-ray scattering which are then combined with electrochemical parameters to deduce structure-activity relationships. T2 - Joint Polish-German Crystallographic Meeting 2020 CY - Wrocław, Poland DA - 24.02.2020 KW - nanostructured KW - electrocatalysis PY - 2020 AN - OPUS4-50664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baláž, M. A1 - Tešinský, M. A1 - Marquardt, Julien A1 - Škrobian, M. A1 - Daneu, N. A1 - Rajňák, M. A1 - Baláž, P. T1 - Synthesis of copper nanoparticles from refractory sulfides using a semi-industrial mechanochemical approach N2 - The large-scale mechanochemical reduction of binary sulfides chalcocite (Cu2S) and covellite (CuS) by elemental iron was investigated in this work. The reduction of Cu2S was almost complete after 360 min of milling, whereas in the case of CuS, a significant amount of non-reacted elemental iron could still be identified after 480 min. Upon application of more effective laboratory-scale planetary ball milling, it was possible to reach almost complete reduction of CuS. Longer milling leads to the formation of ternary sulfides and oxidation product, namely cuprospinel CuFe2O4. The rate constant calculated from the magnetometry measurements using a diffusion model for Cu2S and CuS reduction by iron in a large-scale mill is 0.056 min−0.5 and 0.037 min−0.5, respectively, whereas for the CuS reduction in a laboratory-scale mill, it is 0.1477 min−1. The nanocrystalline character of the samples was confirmed by TEM and XRD, as the produced Cu exhibited sizes up to 16 nm in all cases. The process can be easily scaled up and thus copper can be obtained much easier from refractory minerals than in traditional metallurgical approaches. KW - Mechanochemistry KW - Copper sulfides KW - Copper nanoparticles KW - Magnetometry KW - Oxidation PY - 2020 DO - https://doi.org/10.1016/j.apt.2019.11.032 VL - 31 IS - 2 SP - 782 EP - 791 PB - Elsevier B.V. AN - OPUS4-50665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias ED - Zemčík, R. ED - Krystek, J. T1 - Influence of rotor downwash on vertically displaced nanobots in flight N2 - One challenge associated with navigating a nano aerial robot swarm indoors in unstructured environments is, i.a., the limited air space. To avoid an over-regulation of the available indoor air space (e.g., prohibit copters to fly above each other), a safety region around each copter must be defined. In this paper, we investigate the impact of the downwash of a nano-drone on the stability of another nearby nano-drone. In the experiments, we found out that this downwash has a negative influence of a second nano-drone in a distance of around 1 m vertically and 0.2 m horizontally. Based on the obtained data, we developed a model describing the above-mentioned safety region to enable a safe operation of the swarm in these environments with fewer constraints. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Mobile Robot Olfaction KW - Nano aerial robot KW - Swarm KW - Collision-free navigation KW - Safety region model PY - 2020 DO - https://doi.org/10.1016/j.matpr.2020.03.047 VL - 32 IS - 2 SP - 108 EP - 111 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brinker, U. A1 - Bērziņš, V. A1 - Ceriņa, A. A1 - Gerhards, G. A1 - Kalniņš, M. A1 - Schmölcke, U. A1 - Meinel, Dietmar A1 - Luebke, H. T1 - Two burials in a unique freshwater shell midden: insights into transformations of Stone Age hunter-fisher daily life in Latvia N2 - The Stone Age site Riņņukalns, Latvia, is the only well-stratified shell midden in the Eastern Baltic. In this paper, we present new interdisciplinary results concerning its dating, stratigraphy, features, and finds to shed light on the daily life of a fisher population prior to the introduction of domesticated animals. The undisturbed part of the midden consists of alternating layers of unburnt mussel shell, burnt mussel shell and fish bone, containing artefacts, some mammal and bird bones, and human burials. Two of them, an adult man and a baby, are discovered recently and date to the calibration plateau between 3350 and 3100 cal BC, and to the later 4th millennium, respectively. Stable isotopes suggest a diet based heavily on freshwater fish, and this is supported not only by ten thousands of identified fish remains, but also by a fish bone concentration nearby the skull of the man, which is interpreted as remain of a grave gift (possible fish soup). Of special interest are the baby’s stable isotope values. It shows that the mother’s diet was atypical (perhaps because she was non-local), and/or that dietary stress during pregnancy increased fractionation between the mother’s diet and her bloodstream KW - Baltic Stone Age KW - Palaeoanthropology PY - 2020 DO - https://doi.org/10.1007/s12520-020-01049-7 VL - 12 IS - 5 SP - Article number: 97 PB - Springer-Verlag GmbH CY - Germany AN - OPUS4-50653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aratsu, K. A1 - Takeya, R. A1 - Pauw, Brian Richard A1 - Hollamby, M.J. A1 - Kitamoto, Y. A1 - Shimizu, N. A1 - Takagi, H. A1 - Haruki, R. A1 - Adachi, S. A1 - Yagai, S. T1 - Supramolecular copolymerization driven by integrative self-sorting of hydrogen-bonded rosettes N2 - Molecular recognition to preorganize noncovalently polymerizable supramolecular complexes is a characteristic process of natural supramolecular polymers, and such recognition processes allow for dynamic self-alteration, yielding complex polymer systems with extraordinarily high efficiency in their targeted function. We herein show an example of such molecular recognition-controlled kinetic assembly/disassembly processes within artificial supramolecular polymer systems using six-membered hydrogen-bonded supramolecular complexes (rosettes). Electron-rich and poor monomers are prepared that kinetically coassemble through a temperature-controlled protocol into amorphous coaggregates comprising a diverse mixture of rosettes. Over days, the electrostatic interaction between two monomers induces an integrative self-sorting of rosettes. While the electron-rich monomer inherently forms toroidal homopolymers, the additional electrostatic interaction that can also guide rosette association allows helicoidal growth of supramolecular copolymers that are comprised of an alternating array of two monomers. Upon heating, the helicoidal copolymers undergo a catastrophic transition into amorphous coaggregates via entropy-driven randomization of the monomers in the rosette. KW - Self-assembly KW - Coaggregation KW - Scattering KW - Simulation KW - AFM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506555 DO - https://doi.org/10.1038/s41467-020-15422-6 VL - 11 IS - 1 SP - Article number: 1623 PB - Springer Nature AN - OPUS4-50655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Bernsmeier, D. A1 - Schmack, R. A1 - Häusler, I. A1 - Hertwig, Andreas A1 - Kraffert, K. A1 - Nissen, J. A1 - Kraehnert, R. T1 - Colloidal bimetallic platinum–ruthenium nanoparticles in ordered mesoporous carbon films as highly active electrocatalysts for the hydrogen evolution reaction N2 - Hydrogen features a very high specific energy density and is therefore a promising candidate for clean fuel from renewable resources. Water electrolysis can convert electrical energy into storable and transportable hydrogen gas. Under acidic conditions, platinum is the most active and stable monometallic catalyst for the hydrogen evolution reaction (HER). Yet, platinum is rare and needs to be used efficiently. Here, we report a synthesis concept for colloidal bimetallic platinum–ruthenium and rhodium–ruthenium nanoparticles (PtRuNP, RhRuNP) and their incorporation into ordered mesoporous carbon (OMC) films. The films exhibit high surface area, good electrical conductivity and well-dispersed nanoparticles inside the mesopores. The nanoparticles retain their size, crystallinity and composition during carbonization. In the hydrogen evolution reaction (HER), PtRuNP/OMC catalyst films show up to five times higher activity per Pt than Pt/C/Nafion® and PtRu/C/Nafion® reference catalysts. KW - Ordered mesoporous carbon KW - Bimetallic noble metal nanoparticles KW - Platinum-ruthenium colloid KW - Electrolysis KW - Hydrogen evolution reaction PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506868 DO - https://doi.org/10.1039/C9CY02285F SN - 2044-4753 VL - 10 IS - 7 SP - 2057 EP - 2068 PB - Royal Society of Chemistry AN - OPUS4-50686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Goedecke, Caroline A1 - Wiesner, Yosri A1 - Jekel, M A1 - Ruhl, A S A1 - Braun, Ulrike T1 - Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine N2 - The adsorption of organic micropollutants onto activated carbon is a favourable solution for the treatment of drinking water and wastewater. However, these adsorption processes are not sufficiently understood to allow for the appropriate prediction of removal processes. In this study, thermogravimetric analysis, alongside evolved gas analysis, is proposed for the characterisation of micropollutants adsorbed on activated carbon. Varying amounts of carbamazepine were adsorbed onto three different activated carbons, which were subsequently dried, and their thermal decomposition mechanisms examined. The discovery of 55 different pyrolysis products allowed differentiations to be made between specific adsorption sites and conditions. However, the same adsorption mechanisms were found for all samples, which were enhanced by inorganic constituents and oxygen containing surface groups. Furthermore, increasing the loadings led to the evolution of more hydrated decomposition products, whilst parts of the carbamazepine molecules were also integrated into the carbon structure. It was also found that the chemical composition, especially the degree of dehydration of the activated carbon, plays an important role in the adsorption of carbamazepine. Hence, it is thought that the adsorption sites may have a higher adsorption energy for specific adsorbates, when the activated carbon can then potentially increase its degree of graphitisation. KW - Aktivkohle KW - TED-GC/MS KW - Adsorption KW - Thermoanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506946 DO - https://doi.org/10.1038/s41598-020-63481-y VL - 10 IS - 1 SP - 6695 PB - Nature Publishing Group AN - OPUS4-50694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zimmermann, T. A1 - von der Au, Marcus A1 - Reese, A. A1 - Klein, O. A1 - Hildebrandt, L. A1 - Pröfrock, D. T1 - Substituting HF by HBF4 – an optimized digestion method for multi-elemental sediment analysis via ICP-MS/MS N2 - Determination of elemental mass fractions in sediments plays a major role in evaluating the environmental status of aquatic ecosystems. Herewith, the optimization of a new total digestion protocol and the subsequent analysis of 48 elements in different sediment reference materials (NIST SRM 2702, GBW 07313, GBW 07311 and JMC-2) based on ICP-MS/MS detection is presented. The developed method applies microwave acid digestion and utilizes HBF4 as fluoride source for silicate decomposition. Similar to established protocols based on HF, HBF4 ensures the dissolution of the silicate matrix, as well as other refractory oxides. As HBF4 is not acutely toxic; no special precautions have to be made and digests can be directly measured via ICP-MS without specific sample inlet systems, evaporation steps or the addition of e.g. H3BO3, in order to mask excess HF. Different acid mixtures with and without HBF4 were evaluated in terms of digestion efficiency based on the trace metal recovery. The optimized protocol (5 mL HNO3, 2 mL HCL, 1 mL HBF4) allows a complete dissolution of the analyzed reference materials, as well as quantitative recoveries for a wide variety of certified analytes. Low recoveries for e.g. Sr, Ba and rare earth elements due to fluoride precipitation of HF-based digestions protocols, can be avoided by the usage of HBF4 instead. Based on the usage of high purity HBF4 all relevant trace, as well as matrix elements can be analyzed with sufficiently low LOQs (0.002 μg L−1 for U up to 6.7 μg L−1 for Al). In total, 34 elements were within a recovery range of 80%–120% for all three analyzed reference materials GBW 07313, GBW 07311 and JMC-2. 14 elements were outside a recovery range of 80%–120% for at least one of the analyzed reference materials. KW - Reference Materials KW - Sediment KW - HF free Digestion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510480 DO - https://doi.org/10.1039/D0AY01049A SP - 1 EP - 10 PB - Royal Society of Chemistry AN - OPUS4-51048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raschpichler, C. A1 - Goroncy, C. A1 - Langer, B. A1 - Antonsson, E. A1 - Wassermann, B. A1 - Graf, C. A1 - Klack, Patrick A1 - Lischke, T. A1 - Rühl, E. T1 - Surface Properties and Porosity of Silica Particles Studied by Wide-Angle Soft X-ray Scattering N2 - Wide-angle soft X-ray scattering on free silica particles of different porosity prepared in a beam is reported. The explored q region is mostly dominated by features due to surface roughness and bulk porosity. A comprehensive experimental and theoretical analysis of silica particles of different porosity is presented for various incident photon energies. A correlation analysis, based on the theory of Porod, is used to test the validity of exact Mie theory in different pore density limits. The ability of the discrete dipole scattering model (DDSCAT) to resolve local effects, caused by various pore distributions, is discussed. Characteristic differences between the soft X-ray scattering patterns of the particle samples of different surface properties and porosity are detected. For all mentioned cases, it was confirmed that the effective radius concept of the Guinier model can be successfully extended to Mie theory and DDSCAT in describing the additive contributions of the primary particles, including a thin inhomogeneous solvent-rich surface shell and empty bulk pores. Close agreement, within ±15%, between the calculated and observed pore sizes and porosity values is reached. The influence of pores is alternatively described either in terms of secondary Mie scattering, which is modulated by the local internal electrical field within the particles, or by an independent Mie scattering process induced by the incident field on isolated pores. It is found that for the typical pore/particle size ratios the latter approach presents the best choice. KW - Wide-Angle Soft X‑ray Scattering KW - Silica KW - Porosity PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c04308 SN - 1932-7447 SN - 1932-7455 VL - 124 SP - 16663 EP - 16674 AN - OPUS4-51089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Schienenprüfung mit Wirbelstrom N2 - Ausgehend von einer Machbarkeitsstudie im Jahr 1999 wurde von der BAM in Zusammenarbeit mit der DB AG und verschiedenen anderen Partnern ein Schienenprüfsystem zur Detektion und Bewertung von Schienenfehlern des Typs Head Checks entwickelt. Dieses Prüfsystem arbeitet nach dem Wirbelstromprinzip. Die Firma Prüftechnik Linke & Rühe GmbH aus Magdeburg fertigt und vertreibt seit geraumer Zeit verschiedene manuelle und zuggestützte Prüfsysteme, die auf dieser Entwicklung basieren. Seit Januar 2013 wird in Deutschland der Qualitätsnachweis nach der Schienenbearbeitung mittels Wirbelstromprüfung gefordert. Im Laufe der Entwicklungsarbeiten wurden verschiedentlich benachbarte Themenfelder rund um die Prüfung auf Head Checks gestreift. Der Schwerpunkt dieses Vortrages liegt auf diesen erweiterten Möglichkeiten der magnetinduktiven Prüfung von verlegten Schienen. Hierbei wird sowohl auf die Verbesserung der Möglichkeiten des bestehenden Systems (z. B. durch Kopplung mit anderen Prüfverfahren) als auch auf mögliche Neuentwicklungen (z. B. durch Einsatz neuer Sensorik) eingegangen. Angestrebte Ziele sind z. B. die Verbesserung der Prüfaussage bei der Head Check Prüfung, Erweiterung der Prüfaussage auf andere Schienenfehlertypen oder die Bestimmung von Schieneneigenschaften wie Härte und Rauigkeit. T2 - ZfP im Eisenbahnwesen CY - Wittenberge DA - 15.03.2016 KW - Schienenprüfung KW - Wirbelstromprüfung KW - Zerstörungsfreie Prüfung PY - 2016 AN - OPUS4-35516 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -