TY - CONF A1 - Pauw, Brian Richard T1 - More of the same, please! Standardizing a perfectionist X-ray Scattering methodology for labs and synchrotrons N2 - After a colleague sent me a more useful measurement from a laboratory instrument than what I could get from the beamline, I knew it was time to reassess my life's choices. Over the course of several subsequent post-doc and permanent positions around lab instruments, I managed to refine a flexible, comprehensive methodology for data collection, correction and analysis which can be applied to many X-ray scattering investigations at the lab and at the synchrotron. With the help of friends at round places, this methodology was implemented and put into production, and has been delivering high-quality data since then. Now, we have almost all possible data corrections (for X-ray scattering) implemented, and are improving the hardware to deliver higher-quality metadata to enable the corrections to be performed to a higher accuracy. Simultaneously, we have set up a mini-large facility at BAM with the MAUS, the Multi-scale Analyzer for Ultrafine Structures. The MAUS combines the freedom of a laboratory instrument, with the spectrum of users of a beamline: besides measuring our own samples, and performing our own machine and methodology developments, we have opened this instrument for collaboration with fellow scientists from within BAM and from external institutes and universities. Here, we provide a comprehensive support for these collaborations, guiding the user from concept to sample selection, to interpretation and analysis. In 2019, we have supported over 30 different projects this way, leading to seven co-authored publications involving the MAUS in that year alone. As the MAUS uses the latest iteration of our comprehensive measurement methodology, the data quality is unmatched by any other lab instrument, and fully traceable to boot. The freedom of the laboratory allows for more proof-of-principle experimentation than what is possible at the synchrotron. Therefore, the MAUS provides a good first (and sometimes final) step towards many experimental materials science investigations, nicely complementing the capabilities of the synchrotron. If and when more flux is needed, the step to the synchrotron is now smaller than ever, in particular with the same method T2 - Symposium on large scale facilities CY - BAM, Berlin, Germany DA - 09.03.2020 KW - Small angle scattering KW - Methodology KW - X-ray scattering PY - 2020 AN - OPUS4-51014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Multivariate approaches in the evaluation of (hyper)spectral data for microplastics analysis - options and limitations N2 - Die zunehmende Anreicherung von Gewässern und Böden mit Plastikmüll führt zur Anhäufung von mikroskopisch kleinen Plastikpartikeln, sogenannter Mikroplastik (MP). Es werden dringend analytische Methoden benötigt, die helfen MP zu identifizieren und zu quantifizieren. Gegenwärtig kommen dafür hauptsächlich thermoanalytische und mikro¬skopische Verfahren, wie Mikro-Infrarotspektroskopie oder Mikro-Raman zum Einsatz. Letztere sind in der Regel an zeitaufwendige Probenanreicherungen und -aufbereitungen gebunden, es können nur kleine Probenmengen (Mikrogramm) untersucht werden und die Auswertung der erzielten Spektren kann anspruchsvoll sein. Im Rahmen dieser Präsentation werden zwei Ansätze vorgestellt, die über die multi-variate Analyse spektroskopischer Daten i) einen neuen methodischen Ansatz zum Screening von MP in belasteten Böden sowie ii) eine alternative Auswertung großer (Mikro)-spektroskopischer Datensätze ermöglichen. Zunächst wird ein NIR-spektroskopisches Verfahrens vorgestellt, das es gestattet MP bestehend aus Polyethylen, Polyethylenterephthalat, Polypropylen und Polystyrol im Bereich bis zu 0,5 Massenprozent zu detektieren. Aufgrund kurzer Messzeiten und robuster Technik besitzt dieser Ansatz das Potenzial, im Gegensatz zu den thermoanalytischen und mikrospektroskopischen Methoden, größere Probenmengen mit minimaler Vor¬behandlung zu untersuchen. Der zweite Ansatz befasst sich mit der Auswertung großen Datensätze, wie sie typischerweise als Resultat der Mikro-FTIR unter Nutzung moderner FPA-Detektoren erhalten werden. Die Mikro-FTIR-Technik beruht auf der spektralen Aufnahme, Abbildung und an¬schließenden Identifizierung von Schwingungsbanden, die für synthetische Polymere typisch sind. Die Bilddatensätze sind groß und enthalten Spektren von unzähligen Partikeln natürlichen und synthetischen Ursprungs. Zur Ergänzung bestehender Ansätze, die z.B. auf Recherchen von Spektren¬bibliotheken basieren, wurde die explorative multivariate Datenanalyse getestet. Als Kernkonzept wurde hierbei die Dimensionalitäts¬reduktion verwendet. Die Ergebnisse stellen nicht nur eine orthogonale Methode zur Kontrolle der Ergebnisse dar, die auf Grundlage einer automatisierten Bibliothekssuche erzielt wurden, sondern ergaben darüber hinaus eine Gruppe von Spektren, die nicht in den vorhandenen Spektrenbibliotheken erfasst wurden. N2 - The increasing enrichment of water bodies and soils with plastic waste leads to the accumulation of microscopic plastic particles, so-called microplastics (MP). There is an urgent need for analytical methods that help to identify and quantify MP. At present, mainly thermo-analytical and microscopic methods such as micro-infrared spectroscopy or micro-Raman are used for this purpose. The latter are usually tied to time-consuming sample enrichment and preparation, only small sample quantities (micrograms) can be examined and the evaluation of the obtained spectra can be demanding. In the context of this presentation, two approaches are presented which, via the multi-variate analysis of spectroscopic data, allow i) a new methodological approach to screening MP in contaminated soils and ii) an alternative evaluation of large (micro)-spectroscopic data sets. First, a NIR spectroscopic method is presented which allows MP consisting of polyethylene, polyethylene terephthalate, polypropylene and polystyrene to be detected in the range of up to 0.5 mass percent. Due to short measurement times and robust technology, this approach has the potential, in contrast to thermo-analytical and micro-spectroscopic methods, to examine larger sample quantities with minimal pre-treatment. The second approach deals with the evaluation of large data sets, as typically obtained as a result of micro-FTIR using modern FPA detectors. The micro-FTIR technique is based on the spectral recording, imaging and subsequent identification of vibration bands typical of synthetic polymers. The image data sets are large and contain spectra of numerous particles of natural and synthetic origin. Exploratory multivariate data analysis has been tested to complement existing approaches based on e.g. spectrum library searches. The core concept used was dimensionality reduction. The results not only represent an orthogonal method for checking the results obtained by an automated library search, but also revealed a group of spectra that were not recorded in the existing spectrum libraries. T2 - analytica conference 2020 CY - Online meeting DA - 19.10.2020 KW - Microplastics KW - Multivariate Datenanalyse KW - NIR KW - Hyperspectral data PY - 2020 AN - OPUS4-51516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise T1 - Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements N2 - In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles. The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum. 1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties. 2. Iron oxide nanoparticles are under development as new candidate reference material at BAM. 3. Narrow particle size distribution confirmed by light scattering and electron microscopy. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Electron microscopy KW - Nanoplattform PY - 2020 AN - OPUS4-52774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Microstructure characterization of oligomers by analysis of UPLC / ESI-TOF-MS reconstructed ion chromatograms N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available. The challenge consists in a clever combination of these techniques with a specific approach of data analysis. In this presentation different liquid chromatographic separation modes were combined with Electrospray Time-of-Flight mass spectrometry. The online coupling allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples e.g. the topology elucidation of branched EO-PO copolymers, the possibilities and limitations of this approach were demonstrated. T2 - Analyticon 2020 CY - Online meeting DA - 05.11.2020 KW - Microstructure KW - Copolymer KW - LC-MS PY - 2020 AN - OPUS4-51540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; nPSize offer after 2 Ys N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Size KW - Shape KW - Traceability KW - EMPIR KW - Reference materials KW - VAMAS PY - 2020 AN - OPUS4-51477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Marcoulaki, E. A1 - van Duuren, B T1 - Testing and benchmarking nanosafety services N2 - One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network. T2 - Review Meeting EC4SafeNano CY - Brussels, Belgium DA - 16.01.2020 KW - Nanosafety KW - EC4SafeNano KW - Nanosafety services KW - EU KW - Case studies PY - 2020 AN - OPUS4-50273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Preparation of Nanoparticulate Samples for Electron Microscopy N2 - This presentation addresses the importance of proper sample preparation to obtain suitable samples for electron microscopic measurements. The objective as well as the requirements are discussed. Further, different sample deposition methods for various types of nanoparticulate samples are shown. T2 - nPSize Web Conference CY - Online meeting DA - 23.07.2020 KW - Nanoparticles KW - Electron microscopy KW - Sample preparation KW - Particle size distribution KW - Particle number concentration PY - 2020 AN - OPUS4-51047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Feltin, N. T1 - Hybrid metrology for microscopy of nanoparticles N2 - This presentation is structured in two parts: i) Hybrid metrology by combining SEM with AFM (N. Feltin) and ii) hybridization and corelative microscopy by SEM, STEM-in-SEM, TEM, EDS, Auger Electron Microscopy, TKD and more (D. Hodoroaba). The first part is focused on the metrological part of the hybrid measurement SEM-AFM, the second part offers some further possibilities of correlative microscopy of nanoparticles based on practical examples. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - SEM KW - AFM KW - Metrology KW - Particle size distribution KW - Correlative imaging KW - STEM-in-SEM (TSEM) PY - 2020 AN - OPUS4-51476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative Microstructural Analaysis under VAMAS/TWA 37 N2 - The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 45th Steering Committee Meeting CY - Online meeting DA - 30.09.2020 KW - VAMAS KW - Microbeam analysis KW - Inter-laboratory comparison KW - EBSD KW - FIB PY - 2020 UR - http://www.vamas.org/ AN - OPUS4-51360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer after 2Ys? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. T2 - 28th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 16.10.2020 KW - Nanoparticles KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Traceability PY - 2020 AN - OPUS4-51437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Minimale Anforderungen an Referenzdaten anhand von Beispielen aus der Elektronenmikroskopie und Oberflächenanalytik N2 - In dem Vortrag werden, anhand ausgewählten Beispielen aus der Elektronenmikroskopie und Oberflächenanalytik (EDX und XPS), die minimalen Anforderungen an Referenzdaten für zuverlässige und reproduzierbare Ergebnisse (z.B. Partikelgrößenverteilung, Elementzusammensetzung) vorgestellt und diskutiert. T2 - Workshop "Referenzdaten" CY - Berlin, Germany DA - 13.03.2020 KW - Referenzdaten KW - Nanopartikel KW - Elektronenmikroskopie KW - Oberflächenanalytik KW - Standardarbeitsanweisung KW - SOP KW - Standardisierung PY - 2020 AN - OPUS4-50571 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - In this work, we present various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - NANOSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Bimodal KW - SiO2 KW - Gold PY - 2020 AN - OPUS4-51714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennet, Francesca T1 - Microprinting and SEM analysis for quantitative evaluation of nanoparticles in solution N2 - Nanoparticle suspensions were microprinted onto TEM grids for subsequent analysis by SEM/TSEM and evaluation of particle numbers using Image J software. Various nanoparticle types, concentrations and printing conditions (temperature, rel. humidity) were evaluated in order to determine the optimal conditions for producing a uniform distribution of particles on the substrate and eliminating the coffee ring effect. T2 - H2020 ACEnano Project Meeting CY - Amsterdam, Netherlands DA - 04.03.2020 KW - Nanoparticle KW - Imaging KW - Microprinting KW - Homogeneous deposition PY - 2020 AN - OPUS4-50584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marcoulaki, E. T1 - Blueprint for a sustainable new European Centre to support safe innovation for nanotechnology N2 - This paper presents the blueprint for the operation of a sustainable and permanent European Centre of collaborating reference laboratories and research centres, to establish a one-stop shop for a wide variety of nanosafety related services, and to provide a central contact point for questions about nanosafety in Europe. The Centre aims to harmonise service provision, and bring novel risk assessment and management approaches closer to practice. T2 - NANOSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - EC4SafeNano KW - European Centre KW - Nanomaterials KW - Nanosafety KW - Catalogue of Services (CoS) PY - 2020 UR - https://www.nanosafe.org/cea-tech/pns/nanosafe/en AN - OPUS4-51694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - MinimUm Information Requirements for Electron Microscopy and Surface analysis Data For Risk Assessment of Nanoforms N2 - The European legislation has responded to the wide use of nanomaterials in our daily life and defined the term “nanoform” in the Annexes to the REACH (Registration, Evaluation, Authorization of Chemicals) Regulation. Now specific information of the nanomaterials is required from the companies when registering the appropriate materials in a dossier. In the context of REACH eleven physicochemical properties were considered as relevant, of which the following six are essential for registration of nanoforms (priority properties): chemical composition, crystallinity, particle size, particle shape, chemical nature of the surface (“surface chemistry”), and specific surface area (SSA). A key role is the reliable, reproduceable and traceable character of the data of these priority properties. In this context, we want to discuss which ‘analytical’ information is exactly required to fulfill these conditions. Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) were chosen as the most popular surface analytical methods. Both methods allow a detailed understanding of the surface chemistry with an information depth below ten nanometers. As a rather bulk method for the analysis of nanoforms, Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS) is considered for the quick identification of the main chemical elements present in the sample. Furthermore, Scanning Electron Microscopy (SEM) results are discussed which provide results on particle size and shape. Thus, four of the six priority properties can be obtained with these methods. T2 - Nanosafe 2020 CY - Online meeting DA - 17.11.2020 KW - Risk assessment KW - Nanomaterials KW - Standardization KW - Regulation PY - 2020 AN - OPUS4-51612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize Improved Traceability Chain of Nanoparticle Size Measurement - Outcomes for the Strategy/Metrology Groups of ISO/TC 229 Nanotechnologies N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. T2 - Annual Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Groups CY - Online meeting DA - 06.11.2020 KW - Nanoparticles KW - Size KW - nPSize KW - Inter-laboratory comparison KW - ISO/TC 229 KW - VAMAS PY - 2020 AN - OPUS4-51544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - Various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Particle size distribution KW - Sample peparation KW - Electron microscopy PY - 2020 AN - OPUS4-51716 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 - 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 -