TY - JOUR A1 - Sittner, Jonathan A1 - Götze, Jens A1 - Müller, Axel A1 - Renno, Axel D. A1 - Ziegenrücker, René A1 - Pan, Yuanming T1 - Trace element analysis and luminescence behavior of quartz in pegmatites of the Tørdal Region, Norway N2 - This publication presents a study on the mineral chemistry and luminescence properties of quartz samples from pegmatites of the Tørdal region in Norway. A total of 12 samples were analyzed using Secondary Ion Mass Spectrometry (SIMS), Electron Paramagnetic Resonance Spectroscopy (EPR), and Cathodoluminescence (CL) to gain insights into their trace element concentration and distribution as well as their luminescence behavior. The samples are characterized by different Cl emissions at 450 nm, 500 nm 650 nm and an additional shoulder at 390 nm, which is only partially visible due to the absorption of the glass optics. Of these luminescence bands, the 500 nm band is the most dominant in most samples and it is characterized by an initial blue-green luminescence, which is not stable under electron irradiation. Moreover, it is characterized by a heterogeneous distribution within the samples. This luminescence can be mostly assigned to [AlO4/M+]0 defects, with charge compensation mostly achieved by Li+. Analyses by EPR spectroscopy prove the dominance of structurally bound Al, Li, and Ti ions in the investigated samples. Further analyses using SIMS mapping demonstrate that Na and K are mainly bound to micro fractures or inclusions, suggesting a limited role in the compensation of the luminescence centers. Additionally, the SIMS mappings show that some samples contain Al-rich clusters of 10 to 20 µm in diameter, whereas other trace elements are characterized by a homogeneous distribution. These clusters correspond to bright luminescence areas in size and shape and could potentially indicate H+ compensated [AlO4/M+]0 defects. KW - Quartz KW - Trace elements KW - SIMS KW - Cathodoluminescence KW - EPR KW - Tørdal KW - Pegmatite PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612529 DO - https://doi.org/10.1016/j.chemgeo.2024.122427 VL - 670 SP - 1 EP - 15 PB - Elsevier BV AN - OPUS4-61252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - 3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT N2 - Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network. T2 - WCNDT 2016 CY - München, Germany DA - 13.06.2016 KW - X-ray refraction KW - Computed tomography KW - Hydrogen assisted cracking KW - Duplex stainless steel PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366481 SN - 978-3-940283-78-8 VL - BB 158 SP - Tu.4.B.3, 1 EP - 9 AN - OPUS4-36648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ewers, Benjamin A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Müller, Bernd R. A1 - Hoehl, a. A1 - Müller, R. A1 - Ulm, G. T1 - Terahertz spectral computed tomography N2 - The novel technique of spectral THz computed tomography is demonstrated at an example of a small plastic figure. The data are reconstructed by conventional filtered back-projection. The reconstruction are discussed. T2 - IRMMW-THz 2009 - 34th International conference on infrared, millimeter, and terahertz waves CY - Busan, Korea DA - 2009-09-21 KW - THz KW - Computed tomography PY - 2009 SN - 978-1-4244-2120-6 SP - 1 EP - 2(?) AN - OPUS4-20546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Axel A1 - Goedecke, Caroline A1 - Eisentraut, Paul A1 - Piechotta, Christian A1 - Braun, Ulrike T1 - Microplastic analysis using chemical extraction followed by LC‑UV analysis: a straightforward approach to determine PET content in environmental samples N2 - Background: The ubiquitous occurrence of microplastic particles in marine and aquatic ecosystems was intensively investigated in the past decade. However, we know less about the presence, fate, and input paths of microplastic in terrestrial ecosystems. A possible entry path for microplastic into terrestrial ecosystems is the agricultural application of sewage sludge and solid bio-waste as fertilizers. Microplastic contained in sewage sludge also includes Polyethylene terephthalate (PET), which could originate as fiber from textile products or as a fragment from packaging products (foils, bottles, etc.). Information about microplastic content in such environmental samples is limited yet, as most of the used analytical methods are very time-consuming, regarding sample preparation and detection, require sophisticated analytical tools and eventually need high user knowledge. Results: Here, we present a simple, specific tool for the analysis of PET microplastic particles based on alkaline extraction of PET from the environmental matrix and subsequent determination of the monomers, terephthalic acid, using liquid chromatography with UV detection (LC-UV). The applicability of the method is shown for different types of PET in several soil-related, terrestrial environmental samples, e.g., soil, sediment, compost, fermentation residues, but also sewage sludge, suspended particles from urban water management systems, and indoor dust. Recoveries for model samples are between 94.5 and 107.1%. Limit of determination and limit of quantification are absolute masses of 0.031 and 0.121 mg PET, respectively. In order to verify the measured mass contents of the environmental samples, a method comparison with thermal extraction-desorption-gas chromatography–mass spectrometry (TED-GC/MS) was conducted. Both methods deliver similar results and corroborated each other. PET mass contents in environmental samples range from values below LOQ in agriculture soil up to 57,000 mg kg−1 in dust samples. Conclusions: We demonstrate the potential of an integral method based on chemical extraction for the Determination of PET mass contents in solid environmental samples. The method was successfully applied to various matrices and may serve as an analytical tool for further investigations of PET-based microplastic in terrestrial ecosystems. KW - Soil KW - Analysis KW - Microplastic KW - PET KW - LC-UV PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509060 DO - https://doi.org/10.1186/s12302-020-00358-x IS - 32 SP - 85 PB - Springer Open CY - Berlin AN - OPUS4-50906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Axel T1 - Analysis of tire wear particles in soil samples from roadside using TED-GC/MS N2 - Tire wear particles (TW) are generated by the abrasions of tires on the road surface through traffic. These particles can be transported by air and surface runoff and might also infiltrate the soil and consequently affect terrestrial ecosystems. The estimated tire wear (TW) emissions are immense, with 1.33 106 t a-1 in Europe. Despite this, only little is known about the environmental contents or the fate of TW. One reason for this knowledge gap is the challenging analysis of TW in environmental samples. Detection of TW with spectroscopic methods is problematic due to high fluorescence interferences caused by contained black carbon. One analytical approach is to use zinc (Zn), a typical additive in tires, as a specific marker for the quantification of tire wear. However, any Zn originating from the sample matrix must be separated beforehand and requires elaborate sample preparation. Car tires consist partly of synthetic rubbers, such as styrene-butadiene-rubber (SBR). This SBR could be identified and quantified via Thermal-Extraction-Desorption-Gas Chromatography-Mass Spectrometry (TED-GC-MS). This newly developed and fast screening method allows the simultaneous detection of microplastics and TW mass contents and requires minimal to no sample preparation. Firstly the sample is thermally extracted in a thermobalance under a nitrogen atmosphere. The resulting specific decomposition products are sorbed on a solid phase adsorber, which is then transferred to a GC-MS via an autosampler, where the products are desorbed, separated and identified. Cyclohexenylbenzene is used as a specific marker for SBR. Here we investigated top layer soil samples, collected at the roadside of highly frequented German highways. Samples were analyzed without sample preparation, and SBR was detected in all investigated samples in mass contents ranging from 67.2 to 2230 mg kg-1. A correlation between SBR and Zn content in the soil was confirmed, while the correlation between SBR and Corg was hardly pronounced. We successfully demonstrated the application of TED-GC-MS as a screening method for tire wear in soil samples. The present study will discuss these analytical results in detail as well as sampling parameters like sampling depth and distance to the roadside, and the effect of the particle size on the particle transport by water runoff and air. T2 - SETAC 2020 SciCon CY - Online meeting DA - 03.05.2020 KW - Microplastic KW - Analysis KW - Tire wear KW - Soil PY - 2020 AN - OPUS4-51086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Axel T1 - Einfluss der Alterung auf das Sorptionsverhalten von Mikroplastik, eine Laborstudie mit BTEX und Etherverbindungen N2 - Mikroplastik (MP) findet sich in aquatischen Ökosystemen weltweit und es konnte gezeigt werden, dass hydrophobe organische Schadstoffe an MP angereichert werden. Es ist bekannt, dass teilkristalline und amorphe Polymere unterschiedliche Sorptionsver-halten aufweisen. Der Einfluss des Alterungszustandes der MP-Partikel auf das Sorptionsverhalten ist nicht hinreichend geklärt. In dieser Studie wurden amorphes Polystyrol (PS) und teilkristallines Polypropylen (PP) in Form von Industriepellets gezielt gealtert und mikroskopisch sowie mittels XPS, FTIR und DSC charakterisiert. Anschließend wurde in Batchexperimenten die Sorption von potenziell wassergefährdenden Kraftstoffbestandteilen (Ether und BTEX) an den Pellets mittels Headspace-Gaschromatografie untersucht. T2 - Wasser 2017 - Jahrestagung der Wasserchemischen Gesellschaft CY - Donaueschingen, Germany DA - 22.05.2017 KW - Mikroplastik KW - Alterung KW - Sorption KW - BTEX PY - 2017 AN - OPUS4-40445 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Axel A1 - Becker, Roland A1 - Braun, Ulrike A1 - Dorgerloh, Ute T1 - Einfluss der Alterung auf das Sorptionsverhalten von Mikroplastik, eine Laborstudie mit BTEX und Etherverbindungen N2 - Die Präsenz von Mikroplastik in aquatischen Ökosystemen ist ein globales Problem und steht zunehmend im Fokus der Öffentlichkeit. In mehreren Studien konnten Anreicherungen hydrophober, organischer Schadstoffe an MP nachgewiesen werden. Der Einfluss des Alterungszustandes der MP-Partikel auf das Sorptionsverhalten von hydrophoben organischen Substanzen ist nicht hinreichend geklärt. Ziel der vorliegenden Arbeit war die Untersuchung des Sorptionsverhaltens von Schadstoffen mit Bedeutung für limnische Gewässer an künstlich gealterten Partikeln relevanter Polymere. Das Modell verwendete die Aromaten Benzol, Toluol, Ethylbenzol und Xylol (BTEX) sowie Etherverbindungen. Diese Substanzen sind oder waren Bestandteile in unterschiedlichen Kraftstoffen und finden sich daher in vielen aquatischen Ökosystemen weltweit. Als Sorbentien kamen teilkristallines Polypropylen (PP) und amorphes Polystyrol (PS) in Form von Industriepellets zum Einsatz. Die Pellets wurden jeweils sowohl unbehandelt als auch mittels UV-Bestrahlung künstlich gealtert verwendet und mikroskopisch sowie mittels XPS, FTIR und DSC charakterisiert. Die Alterung führte bei PS zu einer verringerten Sorptionskapazität, während bei PP keine Veränderung im Sorptionsverhalten beobachtet wurde. T2 - Wasser 2017 - Jahrestagung der Wasserchemischen Gesellschaft CY - Donaueschingen, Germany DA - 22.05.2017 KW - Mikroplastik KW - Organische Schadstoffe KW - Sorption KW - Polypropylen Polystyrol PY - 2017 SN - 978-3-947197-01-9 SP - 1 EP - 606 PB - Gesellschaft Dt. Chemiker AN - OPUS4-40447 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hentschel, Manfred P. A1 - Harbich, Karl-Wolfram A1 - Lange, Axel A1 - Schors, Jörg A1 - Müller, Bernd R. T1 - Röntgen-Topographie mit Klein- und Weitwinkel-Streuung N2 - Röntgen-Topographische Verfahren sind dadurch gekennzeichnet, daß die Streueigenschaften eines Probekörpers ortskorreliert erfaßt werden. Somit vereinigen sie die Vorzüge der bildgebenden Eigenschaft der Radiographie mit der Strukturselektivität der Röntgenanalyse. Sowohl die Röntgen-Weitwinkel-Streuung als auch die Röntgen-Kleinwinkel-Streuung (-Beugung und -Refraktion) werden topographisch für die Materialcharakterisierung eingesetzt. Die Topographie-Verfahren und Untersuchungsbeispiele an nichtmetallischen Werkstoffen werden dargestellt. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2002 CY - Weimar, Deutschland DA - 2002-05-06 KW - Röntgen-Streuung KW - Materialcharakterisierung KW - Komposite KW - Keramik PY - 2002 UR - http://www.ndt.net/article/dgzfp02/papers/v15/v15.htm SN - 3-931381-39-0 N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 80-CD PB - DGZfP CY - Berlin AN - OPUS4-2027 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hentschel, Manfred P. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Müller, Bernd R. A1 - Schors, Jörg T1 - Das Anwendungspotential der Röntgen-Topographie vom Mikroriss bis zur Gepäckprüfung T2 - DGZfP-Jahrestagung 2007 CY - Fürth, Deutschland DA - 2007-05-14 KW - CFK KW - Bildgebende Röntgenverfahren KW - Röntgen-Topographie und -Streuung KW - Keramik KW - Explosivstoffe KW - Ermüdungsrisse PY - 2007 SN - 978-3-931381-98-1 SP - 1 EP - 9 PB - DGZfP CY - Berlin AN - OPUS4-15799 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Marco A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Goebbels, Jürgen A1 - Bamberg, J. A1 - Heutling, F. ED - Danny Van Hemelrijck, ED - Igor Solodov, ED - Anastasopoulos, Athanasios ED - Gerhard Busse, T1 - Synchrotron-Refraction-Computed-Tomography for NDT and characterisation of lightweight composite materials T2 - 4th International Conference of Emerging Technologies in Non-Destructive Testing (ETNDT 4) CY - Stuttgart, Germany DA - 2007-04-02 KW - Refraction KW - Computed Tomography KW - NDE KW - Ti-MMC PY - 2008 SN - 978-0-415-46476-5 SP - 217 EP - 221 PB - Taylor & Francis CY - London, UK AN - OPUS4-18680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Goebbels, Jürgen A1 - Bamberg, J. A1 - Heutling, F. T1 - Micro Crack Characterization of Metal Matrix Composites by 3D-Refraction-Computed-Tomography T2 - 16th World Conference on Nondestructive Testing CY - Montreal, Canada DA - 2004-08-30 KW - NDE KW - X-ray refraction KW - Composites KW - MMC PY - 2004 SP - 9 pages PB - International Committee for Non-Destructive Testing CY - Montreal AN - OPUS4-5486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -