TY - CONF A1 - Radtke, Martin T1 - Insights into materials with hard x-rays: capabilities of the bamline N2 - This contribution provides an overview of the BAMline synchrotron radiation beamline, which specializes in hard X-ray spectroscopy techniques for materials research. The BAMline offers X-ray absorption spectroscopy (XAS), x-ray fluorescence spectroscopy (XRF), and tomography to study materials' electronic structure, chemical composition, and structure. Key capabilities include standard and dispersive XAS for electronic structure, micro-XRF for elemental mapping, coded aperture imaging, and depth-resolved grazing exit XAS. The BAMline enables in situ characterization during materials synthesis and functions for energy, catalysis, corrosion, biology, and cultural heritage applications. Ongoing developments like the implementation of machine learning techniques for experiment optimization and data analysis will be discussed. For instance, Bayesian optimization is being used to improve beamline alignment and scanning. An outlook to the future, where the BAMline will continue pioneering dynamic and multi-scale characterization, aided by advanced data science methods, to provide unique insights into materials research, will be given. T2 - μ-XRF at Elettra 2.0: challenges and opportunities CY - Trieste, Italy DA - 11.09.2023 KW - Synchrotron KW - XRF KW - XANES KW - Bayes PY - 2023 AN - OPUS4-58607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernández-González, V. T1 - Innovations in Microplastic Measurement: A Pyrolysis Approach for a Polyethylene Terephthalate Reference Material N2 - In the framework of the PlasticTrace project, in which a reference material for PET microplastics will be proposed, a method using pyrolysis and gas chromatography coupled with mass spectrometry detection (Py-GC-MS) is developed to quantify the mass of PET microplastics (10-100 µm) in tablets at two different concentration levels. The overall aim of this project is to develop international metrological capacity that enables the traceable measurement and characterization of SMPs and NPs in environmental and food samples and the production of suitable reference materials, according to the metrological requirements (https://plastictrace.eu/). The proposed method consists of dissolving the tablet containing the PET microplastics in milli-Q water and filtering the solution using a glass microfiber membrane 13 mm filter size, 1.6 µm pore size. After filtering and several washes to ensure complete dissolution of the tablet and recovery of all PET microplastics, the filter is removed, folded, and placed in a capsule of the pyrolyzer for direct Py-GC/MS analysis. Two main markers were selected for PET quantification: vinyl benzoate and benzoic acid, with consistent concentrations found for both at high PET concentrations (≈400 µg) (24% RSD, n=17), but interferences with the matrix and vinyl benzoate were found at low concentrations (≈17 µg PET), with only benzoic acid being valid as a marker in this case (22% RSD, n=10). As an alternative to the quantification of PET microplastics in tablets at low concentrations, derivatization is proposed, for which tetramethylammonium hydroxide solution (TMAH) is added directly into the pyrolysis cap. The PET marker in this case is dimethyl terephthalate, with which good results have also been found (19.6% RSD, n=10 ). The proposed method is robust, simple, with high automation and very little sample handling and treatment, and allows the analysis of PET microplastics (>10 µm) in tablets with excellent accuracy and precision even at very low concentrations. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics KW - GC/MS PY - 2025 AN - OPUS4-63383 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 - Eisentraut, Paul T1 - Improvements in micro- & nanoplastic mass detection by TED-GC/MS N2 - Introduction to microplastics, definition, relevance, analytical approaches & challenges. TED-GC/MS working principle, features & performance. Optimisation in TED-GC/MS methodology, new validation data. Replacement of Internal Standard, outlook towards upcoming publication and application within EU´s revised drinking water directive. T2 - SETAC 2023 CY - Dublin, Ireland DA - 01.05.2023 KW - Microplastics KW - Thermoanalytics KW - Validation KW - Internal Standard PY - 2023 AN - OPUS4-57421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chabbah, T. A1 - Chatti, S. A1 - Jaffrezic-Renault, N. A1 - Weidner, Steffen A1 - Marestin, C. A1 - Mercier, R. T1 - Impedimetric sensors based on diethylphosphonate-containingpoly(arylene ether nitrile)s films for the detection of lead ions N2 - This article describes the elaboration and characterization of diethylphosphonate-containing polymers coated electrodes as sensors for the detection of heavy metalstraces, by electrochemical impedance spectroscopy. Diethylphosphonate groupswere chosen as heavy metals binding sites. Two different series of polymers bearingthese anchoring groups were synthesized. Whereas the diethylphosphonate groupsare directly incorporated in the aromatic macromolecular chain in some polymers, analiphatic spacer is removing the chelating site from the polymer backbone in others.The influence of the macromolecular structure on the sensing response was studied,especially for the detection of Pb2+,Ni2+,Cd2+and Hg2+. Polymer P6, including thehigher amount of diethylphosphonate groups removed from the polymer chain by ashort alkyl spacer gave the higher sensitivity of detection of lead ions, with a detec-tion limit of 50 pM KW - Heavy metals KW - Phosphonate esters KW - Lead ions KW - MALDI TOF MS PY - 2023 DO - https://doi.org/10.1002/pat.6065 SN - 1042-7147 SP - 1 EP - 11 PB - John Wiley & Sons, Ltd AN - OPUS4-57356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Illuminating the Past, Shaping the Future: Advanced Technologies in Gold Analysis and Beamline Control N2 - The presentation explores how synchrotron radiation is used for non-destructive and highly precise analysis of gold artifacts. It explains how synchrotron radiation provides extremely bright and tunable X-rays that can examine very small areas with great accuracy. These features make it ideal for studying cultural heritage objects without damaging them. The presentation highlights case studies such as the Nebra Sky Disk, the Hiddensee gold jewelry, Phoenician ivory, and Egyptian gold from Abydos. These examples show how synchrotron-based techniques reveal details about the origin, composition, and manufacturing of ancient gold. A major focus is the Bernstorf gold discovery in Bavaria. Over several years, different analytical methods, including synchrotron X-ray fluorescence, were applied to test whether the gold was genuinely ancient. The studies found nearly pure gold, sparking debate about whether such purity could be achieved in the Bronze Age. In the final part, the presentation connects this research with modern developments in automation and artificial intelligence. It describes how beamline experiments can be controlled through the EPICS system, Python scripting, and AI tools such as ChatGPT and Whisper, enabling intelligent and voice-assisted operation. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - Wien, Austria DA - 29.01.2025 KW - Synchrotron KW - BAMline KW - AI KW - Gold KW - XRF PY - 2025 AN - OPUS4-64477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.-G. A1 - Abusafia, A. A1 - Scheid, C. A1 - Steinmetz, H. A1 - Paul, Andrea A1 - Beleites, C. A1 - Braun, U. T1 - Identification of microplastic pathways within a typical European urban wastewater system N2 - In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other. KW - Microplastics KW - Microplastic analysis KW - TED-GC/MS KW - Microplastic pathways KW - Mass contents PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568289 DO - https://doi.org/doi.org/10.1002/appl.202200078 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Holistic Experimentation in the HExX-Lab N2 - Through bottom-up, comprehensive digitalisation of all aspects of an experiment, the HEX-lab improves the trustworthiness (traceability, reproducibility, quality) of scientific findings. The five main parts that make up a materials science experiment, i.e. Sample preparation, Measurements, Processing, Analysis, and Interpretation, each have been addressed in thorough and unique ways in this lab, building up a foundation for a wide range of materials science collaborations. Improvements span the spectrum. Hardware developments include new sample environments and stages, such as grazing incidence motion towers, electrochemistry cells and flow-through holders, electronic components such as safety interlocks and multipurpose I/O controllers, and liquid handling systems such as coolant flow cross-over systems. Software developments include: 1) a new comprehensive control system operating on both the RoWaN as well as the MOUSE allowing for full Python control and sequencing of all experimentation, 2) Automated scripts for instrument optimization, sample alignments and measurements, 3) revamped data pipelines and analysis software, standalone or launched as part of operations sequencing dashboards on servers, and 4) meticulously structured archival datafiles, fully documenting sample preparation, measurements, processing and analyses. These allow for holistic databases and dashboards to be constructed to investigate the links between synthesis parameters and resulting morphology. This poster will highlight some of the tools and techniques developed and available in the HEX-lab over the years, from sample environments to overarching experiment and data organisation structures. T2 - Materials Science Core Facility Synergy Forum 2025 CY - Bremen, Germany DA - 26.02.2025 KW - Digitalization KW - Holistic experiments KW - Traceability KW - Data provenance PY - 2025 AN - OPUS4-62675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falqueto, J. B. A1 - Clark, A. H. A1 - Štefančič, A. A1 - Smales, Glen Jacob A1 - Vaz, C. A. F. A1 - Schuler, A. J. A1 - Bocchi, N. A1 - Kazzi, M. E. T1 - High performance doped Li-rich Li1+xMn2–xO4 cathodes nanoparticles synthesized by facile, fast, and efficient microwave-assisted hydrothermal route N2 - Li-rich nanoparticles of Li1+xMn2–xO4 doped with Al, Co, or Ni are successfully synthesized using a facile, fast, and efficient microwave-assisted hydrothermal route. Synchrotron X-ray diffraction confirms the formation of the crystalline cubic spinel phase type. X-ray absorption spectroscopy analysis at the Co and Ni K- and L-edges verifies that the dopants are within the Li1+xMn2–xO4 spinel structure and are inactive during cycling in the bulk and at the surface. Moreover, we demonstrate that nanocrystallinity and cationic doping play an important role in improving the electrochemical performance with respect to LiMn2O4 microparticles. They significantly reduce the charge-transfer resistance, lower the first cycle irreversible capacity loss to 6%, and achieve a capacity retention between 85 and 90% after 380 cycles, with excellent Coulombic efficiency close to 99% without compromising the specific charge at a 5C cycling rate. Furthermore, the Mn K- and L-edges attest that after long cycling, the Mn oxidation state in the bulk differs from that at the surface caused by the Mn disproportion reaction; however, the cationic doping helps mitigate the Mn dissolution with respect to the undoped Li1+xMn2–xO4 nanoparticles, as indicated by inductively coupled plasma atomic emission spectrometry. KW - XAS KW - SAXS KW - Li-ion battery KW - Cathode material KW - Spinel KW - The MOUSE PY - 2022 DO - https://doi.org/10.1021/acsaem.2c00902 SN - 2574-0962 VL - 5 IS - 7 SP - 8357 EP - 8370 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drago, C A1 - Wiesner, Yosri A1 - Braun, U A1 - Giovannozi, A A1 - Fadda, M A1 - Putzu, Mara A1 - Lorenzo, S A1 - Moscoso-Pérez, C A1 - Benismail, N A1 - Palma, C A1 - Almeida, J A1 - Mattarozzi, M A1 - Barbaresi, M A1 - Piergiovanni, M A1 - Masino, M A1 - Bianchi, F A1 - Careri, M A1 - v Bavel, B A1 - Maltseva, A A1 - Sillanpää, M A1 - Pröfrock, D A1 - Wippermann, D A1 - Altmann, Korinna T1 - Harmonisation of sample preparation for microplastic analysis: Recovery rates of tablets containing microplastics as reference material for food and environmental matrix N2 - Microplastic are found ubiquitarians in the environment and food products. Up to now, their impact of risks on health and environment is still controversially discussed, but based on the precautionary principle alone, their presence should be monitored and emission should be reduced (see here also the status of existing EU regulations ). The crucial point is not only the reduction of microplastics pollution but also the introduction of legally binding, standardized procedures for their analysis. The limited availability of certified reference material as well as absence of standard operating procedures to identify, characterize and quantify microplastics according to number and mass have generated lack of comparability between different analytical methods and laboratories; but also, the need of time-consuming development of own protocols for each laboratory. Further on, harmonisation and standardisation of microplastics analysis requires specific reference materials that are used to validate the measurement and to ensure the comparability of results. In the first step, we developed tablets of a water-soluble matrix, containing defined numbers of microplastic particles or mass contents. These can be solved in water and can be handled as reference materials in bottled drinking water without additional sample preparation. These samples can be measured, using mass-based methods as thermo-analytical methods like thermal desorption-gas chromatography-mass spectrometry (TED-GC/MS) or pyrolysis–gas chromatography–mass spectrometry (Py-GC/MS) and using umber-based methods as vibrational spectroscopy like Infrared and Raman directly after filtration. The aim of this work was to delevop standard operating procedure to measure microplastics in more complex matrices and to harmonise and compare different detection and characterization methods. In fact, these matrices require different additional treatments to allow a reliable quantification and identification of microplastics. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics PY - 2025 AN - OPUS4-63366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -