TY - CONF A1 - Geißler, Heinz A1 - Reinholz, Uwe A1 - Geotti-Bianchini, F. A1 - Preo, M. T1 - Water content of hydrated soda lime silica surface layers with IR spectroscopy and Nuclear Reaction Analysis (NRA) T2 - 3rd ICG TC 14 forum on "water in glass" T2 - 3rd ICG TC 14 forum on "water in glass" CY - Edinburgh, Scotland, UK DA - 2001-07-06 PY - 2001 AN - OPUS4-1065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peuker, Christel A1 - Reinholz, Uwe A1 - Jäger, Christian A1 - Pauli, Jutta A1 - Geißler, Heinz T1 - Extinction coefficients of the OH bands in the IR spectra of basic and water-enriched silicate and aluminosilicate glasses JF - Glass science and technology PY - 2003 SN - 0927-4472 VL - 76 IS - 5 SP - 227 EP - 233 PB - Elsevier CY - Amsterdam AN - OPUS4-2781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leschik, M. A1 - Heide, G. A1 - Frischat, G.H. A1 - Behrens, H. A1 - Wiedenbeck, M. A1 - Wagner, N. A1 - Heide, K. A1 - Geißler, Heinz A1 - Reinholz, Uwe T1 - Determination of H2O and D2O contents in rhyolitic glasses JF - Physics and chemistry of glasses N2 - Five distinct analytical techniques were compared for the quantification of the H2O (0·1-7·4 wt%) and D2O (up to 5·5 wt% D2O) contents in rhyolitic glasses. The hydrogen concentration in obsidians was measured using nuclear reaction analysis (NRA) and converted into H2O concentration. The bulk water content (H2O+D2O) of synthesised glasses was determined using thermal extraction in conjunction with Karl–Fischer titration (KFT). Unextracted H2O was measured by infrared (IR) spectroscopy after remelting the KFT products at high pressure. These well characterised glasses were subsequently used to calibrate secondary ion mass spectrometry (SIMS), infrared and evolved gas analysis (EGA). The calibrations of SIMS for H2O and D2O show a significant matrix effect at H2O and D2O concentrations larger than ~3 mol/l with the relative sensitivity factor (RSF) decreasing with bulk water content. Molar absorption coefficients for the OH stretching vibration band at 3570 cm-1 and the OD stretching vibration band at 2650 cm-1 in the infrared absorption spectra were reinvestigated. In the range 0·1-6 wt% the H2O content of glasses could be reproduced within analytical error using a constant linear molar absorption coefficient. However, it appears that the absorption coefficients for the 3570 cm-1 band as well as for the 2650 cm-1 band both decrease systematically with concentration of dissolved H2O and D2O (epsi3570=80 (±1) - 1·36(±0·23)CH2Ot and epsi2650=61·2(±1) - 2·52(± 0·30)CD2Ot). EGA allows quantification of the H2O content as well as the study of dehydration kinetics. It is shown that H2O is released under vacuum already at room temperature from glasses containing >7 wt% H2O. PY - 2004 UR - http://www.ingentaconnect.com/content/sgt/pcg/2004/00000045/00000004/art00003 SN - 0031-9090 VL - 45 IS - 4 SP - 238 EP - 251 PB - Thornton CY - Sheffield AN - OPUS4-6279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zier, M. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Radtke, Martin A1 - Munnik, F. T1 - Accurate stopping power determination of 15N ions for hydrogen depth profiling by a combination of ion beams and synchrotron radiation JF - Nuclear instruments and methods in physics research B N2 - Hydrogen analysis is of particular importance in thin film technology and it is often necessary to obtain a depth profile. The method with the best depth resolution is NRA using the 6385 keV resonance of the 1H(15N,αγ)12C nuclear reaction. The correct quantification of the depth and concentration scales in the measured hydrogen profiles relies on accurate stopping power values. We present a method to deduce these values from a combination of two techniques: NRA and X-ray reflectometry (XRR). This method is applied to the determination of the stopping power of ~6.4 MeV 15N ions in H-containing amorphous Si-layers (a-Si:H). Density-independent stopping powers at different H concentrations are determined by combining the results from NRA and XRR with an overall uncertainty of 3.3%, showing good agreement with SRIM values. This work shows exemplary the methodology for future evaluation of stopping powers for quality assurance in NRA. KW - Nuclear reaction analysis KW - Hydrogen depth profiling KW - Stopping cross section KW - Linear energy transfer KW - Synchrotron radiation KW - XRR PY - 2012 DO - https://doi.org/10.1016/j.nimb.2011.07.027 SN - 0168-583X SN - 1872-9584 VL - 273 SP - 18 EP - 21 PB - Elsevier CY - Amsterdam AN - OPUS4-25722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaiser, J. A1 - Szczerba, Wojciech A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Albrecht, M. A1 - Lu, Y. A1 - Ballauff, M. T1 - The structure of AuPd nanoalloys anchored on spherical polyelectrolyte brushes determined by x-ray absorption spectroscopy JF - Faraday discussions N2 - Well-defined and facetted bimetallic gold–palladium nanoalloys have been synthesized and anchored in spherical polyelectrolyte brushes (SPB) as composite particles (AuPd@SPB). These particles are better catalysts in aqueous phase than the pure metals. The atomistic arrangement of these nanoalloys has been analysed by extended X-ray absorption fine structure (EXAFS) spectroscopy at the Au–L3 and the Pd–K absorption edge. The samples with high amounts of gold appear as almost statistically mixed random alloys. Alloy compositions with less gold show slight enrichment of Pd at the surface of the particle. In addition, signals of non-metallic palladium appear at the Pd–K edge which indicate the presence of the Pd2+ species in addition to metallic palladium. The relation of these structural features to the catalytic activity is discussed. KW - EXAFS KW - Nanoalloys KW - Gold KW - Palladium KW - K-edge KW - L3-edge KW - HR-TEM KW - Synchrotron radiation KW - BAMline PY - 2013 DO - https://doi.org/10.1039/c3fd20132e SN - 1359-6640 SN - 1364-5498 VL - 162 SP - 45 EP - 55 PB - Soc. CY - Cambridge [u.a.] AN - OPUS4-28300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ordavo, I. A1 - Ihle, S. A1 - Arkadiev, V. A1 - Scharf, Oliver A1 - Soltau, H. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Holl, P. A1 - Kimmel, N. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Schaller, G. A1 - Schopper, F. A1 - Strüder, L. A1 - Thamm, C. A1 - Wedell, R. T1 - A new pnCCD-based color X-ray camera for fast spatial and energy-resolved measurements JF - Nuclear instruments and methods in physics research A N2 - We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested. KW - X-ray CCD camera KW - pnCCD KW - Fast X-ray imaging KW - XRF KW - Full-field X-ray fluorescence KW - Elemental analysis KW - High quantum efficiency KW - High energy resolution KW - Polycapillary optics PY - 2011 DO - https://doi.org/10.1016/j.nima.2011.05.080 SN - 0168-9002 SN - 0167-5087 VL - 654 SP - 250 EP - 257 PB - North-Holland CY - Amsterdam AN - OPUS4-24370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Gadebusch, R. A1 - Hahn, Oliver A1 - Reinholz, Uwe A1 - Kanngießer, B. A1 - Malzer, W. T1 - Non-destructive investigations of Mughal Miniatures by a Combined Spectroscopic approach: PIXE, 3D-muXRF and UV-VIS spectroscopy T2 - Proceedings of the 34th International Sympsoium on Archaeometry KW - PIXE KW - 3D-micro-XRF KW - UV-VIS spectroscopy KW - Archaeometry KW - Cultural heritage PY - 2004 SN - 84-7820-848-8 SP - 4 pages PB - Fernando El Católico CY - Zaragoza AN - OPUS4-7495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinholz, Uwe A1 - Bremser, Wolfram A1 - Brzezinka, Klaus-Werner A1 - Strub, Erik A1 - Weise, Hans-Peter A1 - Merchel, Silke T1 - A thin-layer reference material for hydrogen analysis JF - Nuclear instruments and methods in physics research B N2 - In many areas of material sciences, hydrogen analysis is of particular importance. For example, hydrogen is most abundant as impurity in thin film materials – depending on the deposition process – and has great influence on the chemical, physical and electrical properties of many materials. Existing bulk reference materials (RMs) are not suited for surface sensitive analytical methods like elastic recoil detection analysis (ERDA) or nuclear reaction analysis (NRA). To overcome this serious lack of (certified) thin-layer reference materials for the determination of hydrogen in the near-surface region (1–2 µm depth), we produced stable, homogeneous amorphous silicon layers on Si-wafers (aSi:H–Si) by means of chemical vapour deposition (CVD), while about 10% of hydrogen was incorporated in the Si-layer. Homogeneity and stability were proved by NRA whereas traceability of reference values has been assured by an international interlaboratory comparison. KW - Hydrogen KW - Nuclear reaction analysis KW - Depth profiling KW - Reference material KW - Ion beam analysis PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.03.015 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2418 EP - 2423 PB - Elsevier CY - Amsterdam AN - OPUS4-17553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strub, Erik A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Reznikova, E. T1 - Measurements with compound refractive lenses at the "BAMline" JF - Nuclear instruments and methods in physics research B N2 - A set of compound refractive lenses (CRLs), mounted on a silicon wafer, was obtained from the Institut für Mikrostrukturtechnik Karlsruhe. The CRLs were characterized at the BAMline at the synchrotron BESSYII in Berlin. It could be demonstrated that beam diameters below 1 µm can be obtained. The beam size accepted by the lenses is (140 × 140) µm2, thus the intensity gain in the micrometer spot, including absorption, is about 15,000. It is possible to switch between different beam energies within a few minutes. First results of scans and the application of the lenses for MicroXANES (X-ray absorption near-edge structure) measurements are presented in this paper. Also, the possibility of MicroEXAFS (extended X-ray absorption fine structure) measurements is discussed. KW - X-ray optics KW - XANES KW - EXAFS KW - XAS KW - XRF KW - Speciation PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.02.057 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2165 EP - 2168 PB - Elsevier CY - Amsterdam AN - OPUS4-17554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strub, Erik A1 - Plarre, Rüdiger A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Schoknecht, Ute A1 - Urban, Klaus A1 - Jüngel, P. T1 - Determination of Cr(VI) in wood specimen: A XANES study at the Cr K edge JF - Nuclear instruments and methods in physics research B N2 - The content of chromium in different oxidation states in chromium-treated wood was studied with XANES (X-ray absorption near-edge structure) measurements at the Cr K absorption edge. It could be shown that wood samples treated with Cr(VI) (pine and beech) did still contain a measurable content of Cr(VI) after four weeks conditioning. If such wood samples were heat exposed for 2 h with 135 °C prior conditioning, Cr(VI) was no longer detected by XANES, indicating a complete reduction to chromium (III). KW - X-ray spectroscopy KW - XANES KW - XAS KW - XRF KW - Specifikation KW - Reduction PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.03.011 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2405 EP - 2407 PB - Elsevier CY - Amsterdam AN - OPUS4-17555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Görner, Wolf A1 - Eichelbaum, Maik A1 - Matschat, Ralf A1 - Rademann, K. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich T1 - Non-destructive investigation of composition, chemical properties and structure of materials by synchrotron radiation JF - Insight PY - 2006 SN - 0007-1137 VL - 48 IS - 9 SP - 540 EP - 544 PB - British Institute of Non-Destructive Testing CY - Northampton AN - OPUS4-14186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wolff, Timo A1 - Hahn, Oliver A1 - Merchel, Silke A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Denker, A. T1 - Four non-destructive X-Ray methods analyzing corroded coins: A self-critical comparison T2 - Workshop Synchrotron Radiation in Art and Archaeology 2006 T2 - Workshop Synchrotron Radiation in Art and Archaeology 2006 CY - Berlin, Germany DA - 2006-09-27 PY - 2006 AN - OPUS4-14229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Klemm, D. A1 - Reinholz, Uwe A1 - Strub, E. A1 - Röhrich, J. A1 - Bohne, W. A1 - Hoffmann, V. A1 - Wetzig, K. T1 - Potential candidates of certified reference material for determination of hydrogen concentration with glow discharge optical emission spectrometry (GD-OES) - a feasibility study JF - Journal of analytical atomic spectrometry N2 - Three different coatings/layers have been found in a feasibility study as potential candidates for certified reference materials for the determination of hydrogen concentration by GD-OES: (i) electroplated zinc, (ii) carbon-rich coatings and (iii) amorphous silicon layers. KW - CRM KW - Hydrogen KW - GDS PY - 2008 DO - https://doi.org/10.1039/b717924c SN - 0267-9477 SN - 1364-5544 VL - 23 SP - 460 EP - 462 PB - Royal Society of Chemistry CY - London AN - OPUS4-17335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Britzke, Ralf A1 - Bukalis, Gregor A1 - Reinholz, Uwe A1 - Weise, Hans-Peter A1 - Gadebusch, R.D. T1 - An external PIXE study: Mughal painting pigments JF - X-ray spectrometry KW - PIXE KW - Mughal painting KW - Pigments KW - Archaeometry PY - 2005 SN - 0049-8246 VL - 34 SP - 42 EP - 45 PB - Wiley CY - Chichester AN - OPUS4-6846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Castaing, J. A1 - Calligaro, T. A1 - Salomon, J. A1 - Aucouturier, M. A1 - Reinholz, Uwe A1 - Weise, Hans-Peter T1 - Analyses of hydrogen in quartz and in sapphire using depth profiling by ERDA at atmospheric pressure: Comparison with resonant NRA and SIMS JF - Nuclear instruments and methods in physics research B N2 - Hydrogen is present in anhydrous materials as a result of their synthesis and of their environment during conservation. IBA provides techniques to measure H concentration depth profiles allowing to identify various aspects of the materials including the history of objects such as gemstones used in cultural heritage. A newly established ERDA set-up, using an external microbeam of alpha particles, has been developed to study hydrated near-surface layers in quartz and sapphire by non-destructive H depth profiling in different atmospheres. The samples were also analysed using resonant NRA and SIMS. KW - Hydrogen KW - Gemstones KW - ERDA KW - External beam KW - Depth profiling PY - 2006 DO - https://doi.org/10.1016/j.nimb.2006.03.066 SN - 0168-583X SN - 1872-9584 VL - 249 IS - 1-2 SP - 608 EP - 611 PB - Elsevier CY - Amsterdam AN - OPUS4-12844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Gadebusch, R.D. A1 - Hahn, Oliver A1 - Reinholz, Uwe A1 - Kanngießer, B. A1 - Malzer, W. T1 - Non-destructive investigations of indian miniatures by a combined spectroscopic approach: Pixe, 3D-muXRF and UV-vis spectroscopy T2 - Proceedings of the 34th International Sympsoium on Archaeometry T2 - 34th International Sympsoium on Archaeometry CY - Zaragoza, Spain DA - 2004-05-03 PY - 2004 SN - 84-7820-848-8 SP - 333 EP - 339 PB - Fernando El Católico CY - Zaragoza AN - OPUS4-12362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simons, C. A1 - Mans, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Ostermann, Markus A1 - Michaelis, Matthias A1 - Wienold, Julia A1 - Alber, D. A1 - Kreyenschmidt, M. T1 - Study on microscopic homogeneity of polymeric candidate reference materials BAM H001-BAM H010 by means of synchrotron µ-XRF and LA-ICP-MS JF - Journal of analytical atomic spectrometry N2 - In this study the microscopic homogeneity of the newly developed plastic reference materials BAM H001-BAM H010 was investigated. The materials consist of an acrylonitryle-butadien-styrene terpolymer, doped with different amounts of the elements Br, Cd, Cr, Hg and Pb. For the quantitative determination of the degree of homogeneity, a procedure proposed by Kempenaers et al. (Fresenius J. Anal. Chem., 2001, 369, 733-737) was used. On every sample an extensive number of different points were analyzed and standard deviation for every element mentioned above was used to calculate a minimal sampling mass that is necessary to reach a certain level of uncertainty caused by inhomogeneity (mmin,5%). The experiments were taken out with synchrotron µ-XRF (SR µ-XRF) at BESSYII in Berlin and by laser ablation inductively coupled plasma mass spectroscopy (LA-ICP-MS). The calculated values for mmin,5% of both techniques showed comparable results for all elements. It could be shown that the materials are suitable for calibration of micro analytic techniques if at least 64 µg are used. KW - XRF KW - LA-ICP-MS KW - RoHS KW - CRM PY - 2010 DO - https://doi.org/10.1039/b917008a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 40 EP - 43 PB - Royal Society of Chemistry CY - London AN - OPUS4-20938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vasilescu, A. A1 - Constantinescu, B. A1 - Bugoi, R. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Simon, R. ED - Denecke, M. ED - Walker, C. T1 - Gold provenance studies for Romanian archaeological objects using micro-SR-XRF T2 - 20th International congress on X-ray optics and microanalysis (Proceedings) N2 - Studies by Synchrotron Radiation-X-Ray Fluorescence (SR-XRF) for the search of the presence of trace elements like Sb, Sn, Te and Pb in archaeological metallic objects found on the territory of Romania-old coins and Bronze Age jewelry, aimed to determine the provenance of the gold used in their manufacture. The results are compared with the detailed elemental composition of alluvial or primary gold samples, obtained by the same technique. This work attempted to establish the origin of the gold used for the mint of two different types of koson coins. We found that the kosons with monogram are made of refined gold, while the one used for the kosons without monogram is mainly alluvial. The gold used in the manufacture of the Calarasi Vulchitrun-type disk and the Tauteu hair ring is also of alluvial origin. T2 - 20th International congress on X-ray optics and microanalysis CY - Karlsruhe, Germany DA - 2009-09-14 KW - Provenance KW - Gold KW - SR-XRF KW - Trace elements PY - 2010 UR - http://link.aip.org/link/?APCPCS/1221/139/1 SN - 978-0-7354-0764-0 DO - https://doi.org/10.1063/1.3399240 SN - 0094-243X SP - 139 EP - 143 PB - American Institute of Physics AN - OPUS4-21182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brücher, M. A1 - von Bohlen, A. A1 - Jacob, P. A1 - Franzke, J. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Müller, Bernd R. A1 - Scharf, Oliver A1 - Hergenröder, R. T1 - The charge of solid-liquid interfaces measured by X-ray standing waves and streaming current JF - ChemPhysChem : a European journal of chemical physics and physical chemistry N2 - Measurements of ion distributions at a charged solid–liquid interface using X-ray standing waves (XSW) are presented. High energy synchrotron radiation (17.48 keV) is used to produce an XSW pattern inside a thin water film on a silicon wafer. The liquid phase is an aqueous solution containing Br and Rb ions. The surface charge is adjusted by titration. Measurements are performed over a pH range from 2.2–9, using the native Si oxide layer and functional (amine) groups as surface charge. The Debye length, indicating the extension of the diffuse layer, could be measured with values varying between 1–4 nm. For functionalized wafers, the pH dependent change from attraction to repulsion of an ion species could be detected, indicating the isoelectric point. In combination with the measurement of the streaming current, the surface charge of the sample could be quantified. KW - Interfacial charge KW - Solid/liquid interfaces KW - Surface analysis KW - Surface functionalization KW - X-ray spectrometry KW - X-ray KW - Standing waves KW - XSW KW - Streaming current KW - Synchrotron radiation PY - 2010 DO - https://doi.org/10.1002/cphc.201000166 SN - 1439-4235 SN - 1439-7641 VL - 11 IS - 10 SP - 2118 EP - 2123 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-22057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich T1 - Synchrotron radiation induced X-ray fluorescence for the characterization of ancient gold objects JF - ArcheoSciences KW - Gold KW - Hiddensee treasure KW - Nebra sky disc KW - Non-destructive testing KW - Silver point drawings KW - Synchrotron KW - X-ray fluorescence KW - Or KW - Trésor d´Hiddensee KW - Disque déleste de Nebra KW - Analyse non-destructive KW - Dessins à pointe d´argent KW - Synchrotron KW - Fluorescence à rayons X PY - 2009 SN - 0399-1237 VL - 33 SP - 39 EP - 44 PB - Groupe CY - Rennes AN - OPUS4-23219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Vasilescu, A. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - A study on gold and copper provenance for Romanian prehistoric objects using micro-SR XRF JF - Journal of analytical atomic spectrometry N2 - This study intends to clarify the metal provenance of gold archaeological items using the variation of the Au–Ag ratio and the presence of trace elements as Sn, Sb, Te, and Pb, concentrating on gold Dacian Koson coins, recovered recently. It also extends the area of our investigations to the copper provenance of Bronze Age artifacts—axes, sickles, and celts—found on Romanian territory. The experiments were performed by micro-SR XRF at BESSY Berlin, at the BAM-line facility. Two types of coins (Koson, with and without monogram) were analysed. The conclusions we reached were that most of the monogram coins are made from refined gold (3–5% Ag, less than 0.5% Cu), while the without monogram coins are made from native Transylvanian gold (9–20% Ag, 0.5–2% Cu), of alluvial origin, proved by the presence of Sn, Sb and Te embedded in the gold. The problem of provenance for prehistoric Romanian copper and bronze objects consists in linking their elemental compositional patterns to the ones of the Bronze Age regional mines from Bulgaria, Serbia or Transylvania, most likely used as ore sources for their manufacture. The studied samples present relevant traces of As, Ag, Sb, and Co, suggesting the most probable use of copper from Serbia or northern Bulgaria for their manufacture. KW - X-ray fluorescence KW - Synchrotron radiation KW - Proton induced X-ray emission KW - Archaeometry KW - Gold PY - 2011 DO - https://doi.org/10.1039/c0ja00215a SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 5 SP - 917 EP - 921 PB - Royal Society of Chemistry CY - London AN - OPUS4-23191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grunewald, Christian A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Riesemeier, Heinrich T1 - SRXRF-measurements at non-planar objects: automatic determination of the angle of incidence of the exciting X-ray JF - Journal of analytical atomic spectrometry N2 - For quantitative SRXRF measurements the angle of incidence of the incoming X-ray beam is an important factor. When the sample is focused by a long-range-microscope, the determination of the angle can be automatized using a simple algorithm. This was developed to improve the orientation of especially round or ornate samples. As a side effect the three dimensional surface can be reconstructed, too. KW - X-ray fluorescence KW - Synchrotron radiation KW - Long-range microscope PY - 2011 DO - https://doi.org/10.1039/c0ja00237b SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 5 SP - 1088 EP - 1089 PB - Royal Society of Chemistry CY - London AN - OPUS4-23193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabral, A.R. A1 - Radtke, Martin A1 - Munnik, F. A1 - Lehmann, B. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Tupinambá, M. A1 - Kwitko-Ribeiro, R. T1 - Iodine in alluvial platinum-palladium nuggets: evidence for biogenic precious-metal fixation JF - Chemical geology N2 - Synchrotron radiation-induced X-ray fluorescence (SR-XRF) spectrometry was applied to determine iodine concentrations in alluvial Pt–Pd aggregates with delicate morphological features from Córrego Bom Sucesso, Minas Gerais, Brazil. The millimetre-sized botryoidal and rod-shaped grains of alluvial Pt–Pd–Hg intermetallic compounds have surprisingly high concentrations of iodine, in the range from 10 to ~ 120 μg/g. Because iodine is a strongly biophile element, known to be enriched in peatlands and plant remains in soils by microbial activity, its concentration in the Pt–Pd nuggets suggests biogenic precious-metal fixation in the aqueous alluvial milieu. Biogenic and inorganic processes, such as bioreduction and electrochemical metal accretion, could mutually have contributed to the growth of nanoparticles, formed on organic templates, to millimetric Pt–Pd nuggets. KW - Lodine KW - Pt-Pd nuggets KW - Córrego Bom Sucesso KW - Minas Gerais KW - Brazil PY - 2011 DO - https://doi.org/10.1016/j.chemgeo.2010.12.003 SN - 0009-2541 SN - 1872-6836 VL - 281 IS - 1-2 SP - 125 EP - 132 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-23174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guilherme, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Coroado, J. A1 - Dos Santos, J.M.F. A1 - Carvalho, M.L. T1 - Synchrotron micro-XRF with compound refractive lenses (CRLs) for tracing key elements on Portuguese glazed ceramics JF - Journal of analytical atomic spectrometry N2 - Several glazed ceramic fragments (XVIth to XVIIIth centuries) from two production centers in Portugal (Coimbra and Lisbon) were the object of this study. The ones from Coimbra comprise two sets of samples: faiences and tiles. The ones from Lisbon are only tiles (azulejos, in Portuguese). The three main divisions of such pieces are the ceramic support (body), glaze and surface decoration. The system decoration/glaze is not easy to investigate, due to the high heterogeneity resulting from the mixing procedures and firing temperatures used. Moreover, the ability of the pigment to diffuse into the base glaze varies depending on the composition of both the pigment and the glaze in terms of fusibility. In order to raster these effects, high resolution techniques are required. In this work, synchrotron micro-X-ray fluorescence (µ-XRF) analysis was performed to monitor the profiles of the characteristic elements from the colors used and the glaze in well prepared cross-sections of the samples. Key elements are: Co for blue, Mn for purple, Cu for green, Sb for yellow, Pb for the glaze and Fe for the body. The major difference observed is that faiences have glaze thicknesses between 150 and 200 µm and tiles have glaze thicknesses between 350 and 400 µm. Furthermore, in faiences all the pigments except the yellow ones are well dispersed into the glassy matrix, while in tiles, all of them are just partially diffused throughout the glaze. However, differences between the tiles from Coimbra and Lisbon were observed. In the samples from Lisbon, a higher intake from the pigment throughout the glaze is observed. KW - Synchrotron micro-XRF KW - Compound refractive lenses (CRLs) KW - Portuguese glazed ceramics PY - 2012 DO - https://doi.org/10.1039/c2ja30030c SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 6 SP - 966 EP - 974 PB - Royal Society of Chemistry CY - London AN - OPUS4-26789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Streli, C. T1 - Micro-X-ray absorption spectroscopy with compound refractive lenses JF - Journal of analytical atomic spectrometry N2 - A study regarding the possibility to use compound refractive lenses (CRLs) for X-ray absorption spectroscopy (XAS) was conducted. For XAS measurements the energy of the monochromatic incident beam has to be tuned over an energy range which is broader than the energy bandwidth of a CRL. To prove that µ-XAS with compound refractive lenses is possible, it had to be investigated how changes in the energy influence the beam parameters. This was done by tuning the energy around the nominal energy of the lens and recording images with a high resolution X-ray imaging setup. To investigate the changes in the spot size the scintillator was placed at the nominal focal distance and scans along the beam axis were performed. The effect on the photon flux of the incident beam due to absorption in the lens was investigated by performing XANES measurement on different reference materials with and without CRL. The results of these measurements using a CRL designed for 9 keV are shown and discussed. KW - Micro-XAS KW - Compound refractive lens PY - 2012 DO - https://doi.org/10.1039/c2ja30130j SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 10 SP - 1803 EP - 1808 PB - Royal Society of Chemistry CY - London AN - OPUS4-26790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Vasilescu, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Pacheco, C. A1 - Pichon, L. A1 - Oberländer-Târnoveanu, E. T1 - SR XRF and micro-PIXE studies on ancient metallurgy of thirteen Dacian gold bracelets JF - Applied physics A N2 - A thorough microscopic investigation by SR XRF and micro-PIXE brings insight into the probable techniques used in the manufacture of thirteen Dacian gold bracelets, one of the most spectacular archaeological finds ever on the territory of Romania. KW - Micro-SR-XRF KW - Micro-PIXE KW - Archaeometry KW - Gold KW - Romania PY - 2012 DO - https://doi.org/10.1007/s00339-012-7306-7 SN - 0947-8396 VL - 109 IS - 2 SP - 395 EP - 402 PB - Springer CY - Berlin AN - OPUS4-26902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Vasilescu, A. A1 - Stan, D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Ceccato, D. A1 - Oberländer-Târnoveanu, E. T1 - Studies on archaeological gold items found in Romanian territory using X-ray-based analytical spectrometry JF - Journal of analytical atomic spectrometry N2 - This paper is an overview of the work developed by our group in the investigations of museum objects and alluvial gold, reflected in a series of studies published between 2000–2011, supplemented with new results, unpublished up-to-date. The X-ray based spectrometric techniques employed range from various X-Ray Fluorescence (XRF) investigations to ion beam analysis, including synchrotron radiation XRF and micro-Particle Induced X-ray Emission. The gold objects discussed are mainly part of the Sarmizegetusa Dacian hoards—spiraled bracelets (armbands) and coins. After obtaining in 2011 the permission of the Romanian authorities to take very small (1–2 mg) samples from the most 'unimportant' areas of the Dacian bracelets and several Koson staters, to analyze them by micro-SR-XRF at BESSY, in February 2012, the investigation of several micro-areas of 17 stater and 28 bracelet samples revealed important micro-structural inhomogeneity, especially in Sn and Cu. The same inhomogeneous micro-structure has been seen in Transylvanian alluvial gold. The analyses revealed details on the fingerprint of geological gold deposits and also the main characteristics of ancient gold metallurgy procedures used by the Dacians: a relatively low temperature (lower than Au melting point) and hammering during heating to obtain an ingot through sintering. The use of the sintering procedure was proved for the spiraled bracelets and the Koson without monogram coins, a tradition starting in the Bronze Age in Transylvanian gold processing. The existence of micro-inclusions of Ta-minerals in alluvial gold was also detected, explaining Ta trace presence in the artifacts from the Pietroasa hoard. KW - Micro-SR-XRF KW - Micro-PIXE KW - Archaeometry KW - Gold KW - Romania PY - 2012 DO - https://doi.org/10.1039/c2ja30158j SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 12 SP - 2076 EP - 2081 PB - Royal Society of Chemistry CY - London AN - OPUS4-26991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Margreiter, R. A1 - Baumann, J. A1 - Mantouvalou, I. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Strub, E. T1 - Investigations on fire-gilding JF - Archaeometry N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings. Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered. KW - BAMline KW - X-Ray Fluorescence KW - Gilding KW - Depth profile KW - Archaeometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885 DO - https://doi.org/10.1111/arcm.12797 SN - 0003-813X SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-55288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging JF - Advances in x-ray analysis N2 - X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Katsikini, M. A1 - Filintoglou, K. A1 - Pinakidou, F. A1 - Pilatsikas, N. A1 - Arvanitidis, J. A1 - Christofilos, D. A1 - Paloura, E.C. A1 - Ves, S. A1 - Reinholz, Uwe A1 - Papadomanolaki, E. A1 - Lliopoulos, E. T1 - Scaling of phonon frequencies and electron binding energies with interatomic distances in InxGa1−xN JF - Journal of Applied Physics N2 - In-K-edge x-ray absorption fine structure (EXAFS), x-ray photoelectron, and Raman spectroscopy results are combined for a comprehensive study of InxGa1−xN layers with energy gaps extending over nearly the whole visible spectrum. The In–N and In–(In,Ga) distances determind by EXAFS are used for the derivation of the In–N bond ionicity as well as for the phonon frequency dependence of the LO and B21 modes, assessed by Raman, and the N 1s, In 3d5/2, Ga 3s, and Ga 2p1/2 electron binding energies on those distances. Phonon confinement due to perturbation of the periodic potential caused by the alloying is also quantified. KW - Band gap KW - Phonons KW - Epitaxy KW - Electronic structure KW - X-ray photoelectron KW - Nitrides PY - 2021 DO - https://doi.org/10.1063/5.0069359 VL - 130 IS - 20 SP - 205706 - 1 EP - 205706 - 9 PB - AIP Publishing AN - OPUS4-53956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smekhova, A. A1 - Kuzmin, A. A1 - Siemensmeyer, K. A1 - Luo, C. A1 - Chen, K. A1 - Radu, F. A1 - Weschke, E. A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Yusenko, Kirill T1 - Al-driven peculiarities of local coordination and magnetic properties in single-phase Alx-CrFeCoNi high-entropy alloys JF - Nano Research N2 - Modern design of superior multi-functional alloys composed of several principal components requires in-depth studies of their local structure for developing desired macroscopic properties. Herein, peculiarities of atomic arrangements on the local scale and electronic states of constituent elements in the single-phase face-centered cubic (fcc)- and body-centered cubic (bcc)-structured high-entropy Alx-CrFeCoNi alloys (x = 0.3 and 3, respectively) are explored by element-specific X-ray absorption spectroscopy in hard and soft X-ray energy ranges. Simulations based on the reverse Monte Carlo approach allow to perform a simultaneous fit of extended X-ray absorption fine structure spectra recorded at K absorption edges of each 3d constituent and to reconstruct the local environment within the first coordination shells of absorbers with high precision. The revealed unimodal and bimodal distributions of all five elements are in agreement with structure-dependent magnetic properties of studied alloys probed by magnetometry. A degree of surface atoms oxidation uncovered by soft X-rays suggests different kinetics of oxide formation for each type of constituents and has to be taken into account. X-ray magnetic circular dichroism technique employed at L2,3 absorption edges of transition metals demonstrates reduced magnetic moments of 3d metal constituents in the sub-Surface region of in situ cleaned fcc-structured Al0.3-CrFeCoNi compared to their bulk values. Extended to nanostructured versions of multicomponent alloys, such studies would bring new insights related to effects of high entropy mixing on low dimensions. KW - X-ray magnetic circular dichroism (XMCD) KW - High-entropy alloys KW - Reverse Monte Carlo KW - Magnetism KW - Element-specific spectroscopy KW - Extended X-ray absorption fine structure (EXAFS) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530668 DO - https://doi.org/10.1007/s12274-021-3704-5 SN - 1998-0124 VL - 15 IS - 6 SP - 4845 EP - 4858 PB - Springer AN - OPUS4-53066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smekhova, A. A1 - Kuzmin, A. A1 - Siemensmeyer, K. A1 - Abrudan, R. A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Schneider, M. A1 - Laplanche, G. A1 - Yusenko, Kirill T1 - Inner relaxations in equiatomic single-phase high-entropy Cantoralloy JF - Journal of Alloys and Compounds N2 - The superior properties of high-entropy multi-functional materials are strongly connected with their atomic heterogeneity through many different local atomic interactions. The detailed element-specific studies on a local scale can provide insight into the primary arrangements of atoms in multicomponent systems and benefit to unravel the role of individual components in certain macroscopic properties of complex compounds. Herein, multi-edge X-ray absorption spectroscopy combined with reverse Monte Carlo simulations was used to explore a homogeneity of the local crystallographic ordering and specific structure relaxations of each constituent in the equiatomic single-phase facecentered cubic CrMnFeCoNi high-entropy alloy at room temperature. Within the considered fitting approach, all five elements of the alloy were found to be distributed at the nodes of the fcc lattice without any signatures of the additional phases at the atomic scale and exhibit very close statistically averaged interatomic distances (2.54 – 2.55 Å) with their nearest-neighbors. Enlarged structural displacements were found solely for Cr atoms. The macroscopic magnetic properties probed by conventional magnetometry demonstrate no opening of the hysteresis loops at 5 K and illustrate a complex character of the long-range magnetic order after field-assisted cooling in ± 5 T. The observed magnetic behavior is assigned to effects related to structural relaxations of Cr. Besides, the advantages and limitations of the reverse Monte Carlo approach to studies of multicomponent systems like high-entropy alloys are highlighted. KW - Magnetism KW - High-entropy alloys KW - Reverse Monte Carlo (RMC) KW - Element-specific spectroscopy KW - Extended X-ray absorption fine structure (EXAFS) KW - X-ray absorption near edge structure (XANES) PY - 2022 DO - https://doi.org/10.1016/j.jallcom.2022.165999 SN - 0925-8388 VL - 920 SP - 1 EP - 31 PB - Elsevier AN - OPUS4-55457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska T1 - Time- & spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot – new analytical possibilities for in situ material characterization JF - Journal of Synchrotron Radiation N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Time resolution KW - Single-shot XAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370892 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 IS - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Chester, UK AN - OPUS4-37089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menzel, M. A1 - Scharf, O. A1 - Novak, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Hischenhuber, P. A1 - Buzanich, Günter A1 - Meyer, A. A1 - Lopez, V. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G. A1 - Fittschen, U. T1 - Shading in TXRF: calculations and experimental validation using a color X-ray camera JF - Journal of Analytical Atomic Spectrometry N2 - Absorption effects in total reflection X-ray fluorescence (TXRF) analysis are important to consider, especially if external calibration is to be applied. With a color X-ray camera (CXC), that enables spatially and energy resolved XRF analysis, the absorption of the primary beam was directly visualized for mL-droplets and an array of pL-droplets printed on a Si-wafer with drop-on-demand technology. As expected, deposits that are hit by the primary beam first shade subsequent droplets, leading to a diminished XRF signal. This shading effect was quantified with enhanced precision making use of sub-pixel analysis that improves the spatial resolution of the camera. The measured absorption was compared to simulated results using three different model calculations. It was found they match very well (average deviation < 10%). Thus errors in quantification due to absorption effects can be accounted for in a more accurate manner. KW - absorption KW - X-ray Fluorescence analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-359000 DO - https://doi.org/10.1039/C5JA00127G IS - 10 SP - 2184 EP - 2193 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana ED - Strange, R. W. T1 - Time- and spatial-resolved XAFS spectroscopy in a single shot: new analytical possibilities for in situ material characterization JF - Journal of Synchrotron Radiation N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ–2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 mm is achieved. KW - Single-shot XAFS KW - Time resolution PY - 2016 UR - http://scripts.iucr.org/cgi-bin/paper?S1600577516003969 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Liverpool, UK AN - OPUS4-35903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Katsikini, M. A1 - Pinakidou, F. A1 - Paloura, E.C. A1 - Arvanitidis, J. A1 - Ves, S. A1 - Reinholz, Uwe A1 - Ppadomanolaki, E. A1 - Iliopoulos, E. T1 - Simulation of the EXAFS and Raman spectra of InxGa1-xN utilizing the equation of motion routine of FEFF8 JF - Journal of Physics: Conference Series N2 - A combined analysis of EXAFS and Raman spectra is applied for the study of InxGa1-xN alloys with 0.3 Zr69.5Cu12Ni11Al7.5). This difference is explained by inciting the relative importance of strong chemical order, icosahedral content, cluster symmetry and configuration diversity. KW - Multi-component alloy KW - Glass-forming ability KW - XAFS KW - Local structure KW - AIMD simulation PY - 2014 DO - https://doi.org/10.1107/S1600577514017792 SN - 0909-0495 SN - 1600-5775 VL - 21 IS - 6 SP - 1296 EP - 1304 PB - Blackwell Publishing CY - Oxford AN - OPUS4-31837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mans, C. A1 - Simons, C. A1 - Hanning, S. A1 - Janßen, A. A1 - Alber, D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Bühler, A. A1 - Kreyenschmidt, M. T1 - New polymeric candidate reference materials for XRF and LA-ICP-MS - development and preliminary characterization JF - X-ray spectrometry N2 - A set of ten calibration materials based on acrylonitrile-butadiene-styrene terpolymer (ABS) containing the elements Br, Pb, Cd, Cr, and Hg was produced in order to control polymer samples in regard to the restriction on the use of certain hazardous substances (RoHS) directive. The materials were produced with respect to the special demands of X-ray fluorescence analysis (XRF) and inductively coupled plasma mass spectrometry in combination with laser ablation (LA-ICP-MS). The mass fractions of all elements were 0-1500 mg/kg and the materials were produced as granulates and solid discs with a diameter of 40 mm and thicknesses of 1, 2, and 6 mm. It could be shown that the signals measured by XRF strongly depend on the thickness of polymeric samples. Macroscopic homogeneity was assessed with XRF measuring a total of 180 samples. The microscopic homogeneities were determined for a material with average elemental mass fractions with the aid of synchrotron radiation (SR) µ-XRF and LA-ICP-MS. Sufficient macroscopic and microscopic homogeneities for all elements could be achieved. It was observed that organic additives show a better homogeneity than oxides. XRF and LA-ICP-MS were successfully calibrated with the new materials. Limits of detection were in the range of 0.4-22 mg/kg for XRF and 2.3-26.8 mg/kg for LA-ICP-MS. The materials are considered as candidate reference materials (RM) by the Federal Institute of Materials Research and Testing (BAM, Germany). KW - XRF KW - LA.ICP-MS Plastics KW - RoHS KW - CRM PY - 2009 DO - https://doi.org/10.1002/xrs.1120 SN - 0049-8246 VL - 38 IS - 1 SP - 52 EP - 57 PB - Wiley CY - Chichester AN - OPUS4-18681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, M. A1 - Cappa, F. A1 - Schreiner, M. A1 - Ferloni, P. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Woytek, B. A1 - Alram, M. T1 - Further metallurgical analyses on silver coins of Trajan (AD 98-117) JF - Journal of analytical atomic spectrometry N2 - Within an interdisciplinary project, preliminary results of which were published in 2007, a group of 65 silver coins (denarii) of Trajan, evenly distributed over the entire span of his reign (2nd to 6th consulate), as well as 3 coins from the reign of his predecessor, the emperor Nerva (AD 96–98), had been acquired on the coin market. These pieces could be cross-sectioned in order to carry out analyses. Measurements were performed with µ-XRF and µ-SRXRF to check the fineness of the denarius alloy as well as to investigate if the coins of the different consulates showed distinct traits concerning the main impurities which could suggest a change of ore sources. Furthermore, it was examined whether the influx of precious metals into the Roman treasury after Trajan's Dacian campaigns (AD 101/102 and 105/106) could have had any repercussions on the composition of the denarius alloy; comparative data was provided by the analysis of nine imitations of Roman Republican denarii presumably struck in Dacia. Documentation of the cross-sections was performed with SEM/EDX in order to clarify details concerning the specific microstructure of the coins. An enrichment of Ag of approx. 100 to 200 µm in the near surface regions of most of the coins could be observed, which is due to corrosion effects. Previous metallographic analyses done by several scholars had been inadequate to clarify the central numismatic and economic questions. With the presented analyses, it was possible to correct the results of the earlier research and to provide, for the first time, a secure basis of data for the investigation of the development of the silver alloy used for denarii in Trajan's reign. PY - 2011 DO - https://doi.org/10.1039/c0ja00252f SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 5 SP - 873 EP - 1100 PB - Royal Society of Chemistry CY - London AN - OPUS4-23623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Vasilescu, A. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - Micro-SR-XRF studies for archaeological gold identification - the case of carpathian gold and romanian museal objects JF - Applied physics A N2 - In the determination of the provenance of gold in archaeological artifacts, trace elements are more significant than the main components. Several minute fragments of natural Carpathian gold-placer and primary-and some very small (a few milligrams) fragments of archaeological items were studied using micro Synchrotron Radiation X-Ray Fluorescence (micro SR-XRF) at the BESSY Synchrotron Facility in Berlin, Germany. The goal of the study was to identify the trace elements characterizing Carpathian gold, looking especially at Sn, Sb, Pb and Te, and to determine if the gold in the archaeological items is native or refined. Applications to the authentication and provenance of nine Dacian gold bracelets, koson coins and two Bronze Age items are presented. KW - Gold KW - Provenance KW - Archeometry KW - Sy-XRF PY - 2010 DO - https://doi.org/10.1007/s00339-010-5624-1 SN - 0947-8396 VL - 99 IS - 2 SP - 383 EP - 389 PB - Springer CY - Berlin AN - OPUS4-21395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Vincze, L. A1 - Reuter, Dirk T1 - X-ray scattering in X-ray fluorescence spectra with X-ray monochromatic, polarised excitation - modelling, experiment, and Monte-Carlo simulation JF - Nuclear instruments and methods in physics research B N2 - A systematic series of measurements has been carried out with monochromatic X-ray excitation with synchrotron radiation in order to check a physical model on X-ray scattering. The model has recently been successfully tested for the case of polychromatic, unpolarised excitation emitted by an X-ray tube. Our main purpose is the modelling of a physical background in X-ray fluorescence spectra, so that improved quantitative results can be achieved especially for strongly scattering specimens. The model includes single Rayleigh and Compton scattering in the specimen, the effect of bound electrons, the challenging Compton broadening and the polarisation degree. Representative specimens, measurement geometries and excitation energies have been selected with synchrotron monochromatic light at BAMline/BESSY II. Monte-Carlo simulations have been also carried out in order to evaluate the quality of the results achieved with the model. KW - X-ray scattering KW - Monochromatic excitation KW - Polarisation KW - Modelling KW - Monte-Carlo simulation PY - 2011 DO - https://doi.org/10.1016/j.nimb.2011.04.009 SN - 0168-583X SN - 1872-9584 VL - 269 IS - 13 SP - 1493 EP - 1498 PB - Elsevier CY - Amsterdam AN - OPUS4-23765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Gorelik, T. E. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Kolb, U. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The crystallisation of copper(II) phenylphosphonates JF - Dalton Transactions N2 - The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384217 DO - https://doi.org/10.1039/C6DT02904C SN - 1477-9226 SN - 1477-9234 VL - 45 IS - 43 SP - 17453 EP - 17463 PB - The Royal Society of Chemistry AN - OPUS4-38421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Derr, I. A1 - Schökel, A. A1 - Roth, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A combined in-situ XAS–DRIFTS study unraveling adsorbate induced changes on Pt nanoparticle structure JF - Journal od Catalysis N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Δμ X-ray Absorption Near Edge Structure analysis (Δμ XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the Pt-Pt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from Pt-CO to Pt-O. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsoprtion KW - Platinum KW - String metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 SN - 0021-9517 VL - 339 SP - 57 EP - 67 PB - Elsevier AN - OPUS4-38367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana T1 - Time- and spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot: new analytical possibilities for in situ material characterization JF - Journal of Synchrotron Radiation N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Single-shot XAFS KW - Time resolution KW - Spatial resolution KW - Divergent XAFS PY - 2016 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography AN - OPUS4-38370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gauert, C. A1 - Schannor, M. A1 - Hecht, L. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - A comparison of in situ analytical methods for trace element measurement in gold samples from various South African gold deposits JF - Geostandards and geoanalytical research N2 - Trace element concentrations in gold grains from various geological units in South Africa were measured in situ by field emission-electron probe microanalysis (FE-EPMA), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and synchrotron micro X-ray fluorescence spectroscopy (SR-µ-XRF). This study assesses the accuracy, precision and detection limits of these mostly non-destructive analytical methods using certified reference materials and discusses their application in natural sample measurement. FE-EPMA point analyses yielded reproducible and discernible concentrations for Au and trace concentrations of S, Cu, Ti, Hg, Fe and Ni, with detection limits well below the actual concentrations in the gold. LA-ICP-MS analyses required larger gold particles (> 60 µm) to avoid contamination during measurement. Elements that measured above detection limits included Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, As and Te, which can be used for geochemical characterisation and gold fingerprinting. Although LA-ICP-MS measurements had lower detection limits, precision was lower than FE-EPMA and SR-µ-XRF. The higher variability in absolute values measured by LA-ICP-MS, possibly due to micro-inclusions, had to be critically assessed. Non-destructive point analyses of gold alloys by SR-µ-XRF revealed Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y and Zr in the various gold samples. Detection limits were mostly lower than those for elements measured by FE-EPMA, but higher than those for elements measured by LA-ICP-MS. N2 - Les concentrations en éléments traces de grains d'or provenant de différentes unités géologiques d'Afrique du Sud ont été mesurées in situ par microsonde électronique à émission de champ (FE-EPMA), spectrométrie de masse couplée à une source plasma et un système d'ablation laser (LA-ICP-MS) et micro spectroscopie de fluorescence des rayons X au Synchrotron (SR-µ-XRF). Cette étude évalue l'exactitude, la précision et les limites de détection de ces méthodes d'analyse pour la plupart non-destructives en utilisant des matériaux de référence certifiés, et discute de leur application dans les mesures sur échantillon naturel. Les points d'analyses FE-EPMA ont fournis des concentrations reproductibles et discernables pour l'Au et des concentrations en traces de S, Cu, Ti, Hg, Fe et Ni, avec des limites de détection bien inférieures aux concentrations réelles dans l'or. Les analyses LA-ICP-MS ont nécessitées des particules d'or de plus grande taille (> 60 µm) pour éviter toute contamination pendant la mesure. Les éléments mesurés au-dessus des limites de détection inclus Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, A et Te, qui peuvent être utilisés pour les caractérisations géochimique et le «fingerprinting» de l'or. Bien que les mesures LA-ICP-MS aient des limites de détection plus basses, la précision est inférieure par rapport à celles de la microsonde FE et de la SR-µ-XRF. La plus grande variabilité des valeurs absolues mesurées par LA-ICP-MS, probablement reliée à la présence de micro-inclusions, a du être évaluée de manière critique. Les points d'analyse non-destructifs des alliages d'or par SR-µ-XRF ont révélés la présence de Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y et Zr dans les différents échantillons. Les limites de détection ont été pour la plupart inférieures à celles des éléments mesurés par FE-EPMA, mais supérieures à celles des éléments mesurés par LA-ICP-MS. KW - Trace elements KW - Gold KW - FE-EPMA KW - LA-ICP-MS KW - SR-µ-XRF KW - Precision KW - Précision KW - Comparison of techniques KW - Éléments traces PY - 2016 DO - https://doi.org/10.1111/j.1751-908X.2015.00362.x SN - 1639-4488 SN - 1751-908X VL - 40 IS - 2 SP - 267 EP - 289 PB - Blackwell CY - Oxford AN - OPUS4-34882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Buzanich, Günter A1 - Curado, Jessica A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. T1 - Slicing - a new method for non destructive 3D elemental sensitive characterization of materials JF - Journal of analytical atomic spectrometry N2 - Recent advances in synchrotron sources and detector technology have led to substantial improvements in spatial resolution and detection limits for X-ray fluorescence analysis (XRF). However, the non-destructive three-dimensional elemental sensitive characterization of samples remains a challenge. We demonstrate the use of the so-called 'Color X-ray Camera' (CXC) for 3D measurements for the first time. The excitation of the sample is realized with a thin sheet-beam. The stepwise movement of the sample allows getting the elemental distribution for each layer with one measurement. These layers can be combined to a full 3D dataset for each element afterwards. Since the information is collected layer by layer, there is no need to apply reconstruction techniques, which quite often are the reason for artifacts in the results achieved by computed tomography (CT). The field of applications is wide, as the 3D elemental distribution of a material contains clues to processes inside the samples from a variety of origins. The technique is of special interest and well suited for biological specimens, because their light matrix minimizes restricting absorption effects. Measurement examples of a hornet and the teeth of a Sorex araneus are shown. KW - SR-microXRF KW - 3D KW - CXC PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324330 DO - https://doi.org/10.1039/c4ja00085d SN - 0267-9477 SN - 1364-5544 VL - 29 IS - 8 SP - 1339 EP - 1344 PB - Royal Society of Chemistry CY - London AN - OPUS4-32433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Schäfers, F. A1 - Adam, Christian T1 - Chemical state of chromium, sulfur, and iron in sewage sludge ash based phosphorus fertilizers JF - ACS sustainable chemistry & engineering N2 - As an essential element of all life forms, phosphorus (P) is vital to the fertilizer industry. With decreasing quantity and quality of phosphate rock resources, recycling P-fertilizers from wastewater is of increasing interest. The P-fertilizer products of a recently developed thermochemical process for P recovery from sewage sludge ash (SSA) were investigated by chromium, sulfur, and iron K-edge X-ray near-edge structure (XANES) spectroscopy. This paper focuses the formation and prevention of toxic chromium(VI) and toxic sulfides during the thermochemical processes. Reducing conditions prevent the oxidation of chromium(III) in the SSA to toxic chromium(VI). Sulfides formed under the reducing conditions are nontoxic iron sulfides. Hematite (Fe2O3) present in the SSA is reduced to magnetite (Fe3O4). A gentle post-treatment at 400 °C under oxidizing conditions converts the iron sulfides into plant-available iron sulfates. This oxidative post-treatment does not form undesired chromium(VI) compounds. KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Phosphorus recovery KW - Sewage sludge ash KW - Chromium KW - Sulfur KW - Iron PY - 2015 DO - https://doi.org/10.1021/acssuschemeng.5b00678 SN - 2168-0485 VL - 3 IS - 10 SP - 2376 EP - 2380 PB - ACS Publ. CY - Washington, DC AN - OPUS4-34166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, S.H. A1 - Bjeoumikhov, A. A1 - Von Borany, J. A1 - Buchriegler, J. A1 - Munnik, F. A1 - Petric, M. A1 - Renno, A.D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Strüder, L. A1 - Wedell, R. A1 - Ziegenrücker, R. T1 - Examples of XRF and PIXE imaging with few microns resolution using SLcam® a color X-ray camera JF - X-ray spectrometry N2 - We present results of recent development of the color X-ray camera, type SLcam®, allowing detection of X-ray images with few microns resolution. Such spectral resolution is achieved with the use of high-quality polycapillary optics combined with sub-pixel resolution. Imaging of Siemens star resolution test chart reveals that the resolution limit of SLcam® can go down to nearly 5µm. Several real sample examples of measurements carried out at the laboratory, synchrotron, and particle-induced X-ray emission beamlines are shown. This is the first time SLcam® is used as particle-induced X-ray emission detector. KW - X-ray KW - Color X-ray camera KW - CXC KW - Synchrotron radiation KW - BESSY KW - BAMline PY - 2015 DO - https://doi.org/10.1002/xrs.2590 SN - 0049-8246 VL - 44 IS - 3 SP - 135 EP - 140 PB - Wiley & Sons, Ltd. CY - Chichester AN - OPUS4-33170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tissot, I. A1 - Troalen, L.G. A1 - Manso, M. A1 - Ponting, M. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Barreiros, M. A. A1 - Shaw, I. A1 - Carvalho, M.L. A1 - Guerra, M.F. T1 - A multi-analytical approach to gold in Ancient Egypt: Studies on provenance and corrosion JF - Spectrochimica acta B N2 - Recent results from a three-year multi-disciplinary project on Ancient Egyptian gold jewellery revealed that items of jewellery from the Middle Kingdom to the New Kingdom were manufactured using a variety of alluvial gold alloys. These alloys cover a wide range of colours and the majority contain Platinum Group Elements inclusions. However, in all the gold foils analysed, these inclusions were found to be absent. In this work a selection of gilded wood and leather items and gold foil fragments, all from the excavations by John Garstang at Abydos (primarily from Middle Kingdom graves), were examined using Scanning Electron Microscopy-Energy Disperse Spectroscopy (SEM-EDS), X-Ray Fluorescence (µXRF), Particle Induced X-Ray Emission (µPIXE) and Double Dispersive X-Ray Fluorescence (D²XRF). The work allowed us to characterise the composition of the base-alloys and also to reveal the presence of Pt at trace levels, confirming the use of alluvial gold deposits. Corrosion products were also investigated in the foils where surface tarnish was visually observed. Results showed that the differences in the colour of corrosion observed for the foils are related not only to the thickness of the corrosion layer but also to a multi-layer structure containing the various corrosion products. KW - Gold KW - Egypt KW - PGE KW - Provenance KW - Corrosion KW - muXRF KW - muPIXE KW - D2XRF KW - SEM-EDS PY - 2015 DO - https://doi.org/10.1016/j.sab.2015.03.012 SN - 0584-8547 SN - 0038-6987 VL - 108 SP - 75 EP - 82 PB - Elsevier CY - Amsterdam AN - OPUS4-33155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vasilescu, A. A1 - Constantinescu, B. A1 - Stan, D. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Ceccato, D. T1 - Studies on ancient silver metallurgy using SR XRF and micro-PIXE JF - Radiation physics and chemistry N2 - This work presents a complex evaluation of a series of Geto-Thracian silver adornments found on Romanian territory, part of the 4th century BC Agighiol (Northern Dobruja) hoard and of an ingot from the 1st century BC Geto-Dacian Surcea (Transylvania) hoard, using Synchrotron Radiation X-Ray Fluorescence and micro- Proton Induced X-ray Emission analysis and mapping in order to investigate aspects related to the elemental composition of the metal and the metallurgy implied in their manufacture. One of the samples can be linked to Laurion as the source of metal, and several items contain silver probably originated in Macedonia. The set of silver items was found to be heteregenous as composition and microstructure, and corrosion-related elements could be also identified in the X-Ray maps. KW - Synchrotron radiation XRF KW - Micro-PIXE KW - Archaeological silver PY - 2015 DO - https://doi.org/10.1016/j.radphyschem.2015.07.008 SN - 0969-806X SN - 0020-7055 SN - 0146-5724 VL - 117 SP - 26 EP - 34 PB - Pergamon Press CY - Oxford [u.a.] ; Frankfurt, M. AN - OPUS4-33809 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reifschneider, O. A1 - Vennemann, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Hogeback, J A1 - Köppen, C. A1 - Großgarten, M. A1 - Sperling, M. A1 - Wiemann, M. A1 - Karst, U. T1 - Revealing Silver Nanoparticle Uptake by Macrophages Using SR-μXRF and LA-ICP-MS JF - Chemical Research in Toxicology N2 - To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed. KW - Synchrotron KW - BAMline KW - XRF KW - Nanoparticle KW - Macrophagen PY - 2020 DO - https://doi.org/10.1021/acs.chemrestox.9b00507 VL - 33 IS - 5 SP - 1250 EP - 1255 PB - American Chemical Society AN - OPUS4-50855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Buzanich, Günter A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. A1 - Scholz, Philipp A1 - Guerra, M.F. T1 - Double Dispersive X-Ray Fluorescence (D2XRF) based on an Energy Dispersive pnCCD detector for the detection of platinum in gold JF - Microchemical Journal N2 - With the aim of improving limits of detection (LOD) of trace elements in a matrix with adjacent fluorescence energies, a simple double dispersive X-ray fluorescence detection system (D2XRF) was constructed to operate at the beamlines BAMline and the mySpot @ BESSY II. This system is based on the combination of a crystal analyzer with an energy resolving single photon counting pnCCD. Without further collimators, the efficient suppression of the background by the pnCCD and the good energy resolution of the crystal results in improved LOD. In first order reflections, an energy resolution of 13 eV for Cu Kα was reached, and an energy range of 1 keV was covered in one shot. This new system was applied to the detection of platinum (Pt) in gold leaves with a LOD of 0.9 mg/kg, which is the lowest attained by totally non-destructive methods nowadays. The presence of Pt in gilded objects from Abydos and Byzantine mosaics provides vital information, as it indicates the alluvial origin of the gold for these examples. KW - Platinum Wavelength dispersive D2XRF KW - Gold Synchrotron XRF PY - 2016 DO - https://doi.org/10.1016/j.microc.2015.10.039 VL - 125 SP - 56 EP - 61 PB - Elsevier Science CY - Amsterdam AN - OPUS4-35777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Schoeckel, A. A1 - Roth, C. T1 - A combined in-situ XAS-DRIFTS study unraveling adsorbate induced changes on the Pt nanoparticle structure JF - Journal of Catalysis N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Dl X-ray Absorption Near Edge Structure analysis (Dl XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the PtAPt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from PtACO to PtAO. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsorption KW - Platinum KW - Strong metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 IS - 339 SP - 57 EP - 67 PB - Elsevier Inc. CY - Philadelphia, Pennsylvania, USA AN - OPUS4-35815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, S.H. A1 - Bjeoumikhov, A. A1 - Von Borany, J. A1 - Buchriegler, J. A1 - Munnik, F. A1 - Petric, M. A1 - Radtke, Martin A1 - Renno, A.D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Wedell, R. T1 - Sub-pixel resolution with a color X-ray camera JF - Journal of analytical atomic spectrometry N2 - The color X-ray camera SLcam® is a full-field, single photon detector providing scanning-free, energy and spatially resolved X-ray imaging. Spatial resolution is achieved with the use of polycapillary optics guiding X-ray photons from small regions on a sample to distinct energy dispersive pixels on a charged-coupled device detector. Applying sub-pixel resolution, signals from individual capillary channels can be distinguished. Therefore, the SLcam® spatial resolution, which is normally limited to the pixel size of the charge-coupled device, can be improved to the size of individual polycapillary channels. In this work a new approach to a sub-pixel resolution algorithm comprising photon events also from the pixel centers is proposed. The details of the employed numerical method and several sub-pixel resolution examples are presented and discussed. KW - Color X-ray camera KW - Sub pixel analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-334948 DO - https://doi.org/10.1039/c5ja00028a SN - 0267-9477 SN - 1364-5544 SP - 1890 EP - 1897 PB - Royal Society of Chemistry CY - London AN - OPUS4-33494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kabelitz, Anke A1 - de Oliveira Guilherme Buzanich, Ana A1 - Joester, Maike A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Bienert, Ralf A1 - Schulz, K. A1 - Schmack, R. A1 - Kraehnert, R. A1 - Emmerling, Franziska T1 - Time-resolved in situ studies on the formation mechanism of iron oxide nanoparticles using combined fast-XANES and SAXS JF - CrystEngComm N2 - The reaction of iron chlorides with an alkaline reagent is one of the most prominent methods for the synthesis of iron oxide nanoparticles. We studied the particle formation mechanism using triethanolamine as reactant and stabilizing agent. In situ fast-X-ray absorption near edge spectroscopy and small-angle X-ray scattering provide information on the oxidation state and the structural information at the same time. In situ data were complemented by ex situ transmission electron microscopy, wide-angle X-ray scattering and Raman analysis of the formed nanoparticles. The formation of maghemite nanoparticles (γ-Fe2O3) from ferric and ferrous chloride was investigated. Prior to the formation of these nanoparticles, the formation and conversion of intermediate phases (akaganeite, iron(II, III) hydroxides) was observed which undergoes a morphological and structural collapse. The thus formed small magnetite nanoparticles (Fe3O4) grow further and convert to maghemite with increasing reaction time. KW - oxidation state KW - structural information KW - maghemite PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351376 DO - https://doi.org/10.1039/C5CE01585E SN - 1466-8033 VL - 17 IS - 44 SP - 8463 EP - 8470 CY - London, UK AN - OPUS4-35137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U.E.A. A1 - Menzel, M. A1 - Scharf, O. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Lopez, V.M. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G.J. T1 - Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera JF - Spectrochimica acta B N2 - Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by 'drop on demand' technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. KW - TXRF KW - Full field micro-XRF KW - Color X-ray camera PY - 2014 DO - https://doi.org/10.1016/j.sab.2014.06.025 SN - 0584-8547 SN - 0038-6987 VL - 99 SP - 179 EP - 184 PB - Elsevier CY - Amsterdam AN - OPUS4-31180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De Samber, B. A1 - Scharf, Oliver A1 - Buzanich, Günter A1 - Garrevoet, J. A1 - Tack, P. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Evens, R. A1 - De Schamphelaere, K. A1 - Falkenberg, G. A1 - Janssen, C. A1 - Vincze, L. T1 - Three-dimensional X-ray fluorescence imaging modes for biological specimens using a full-field energy dispersive CCD camera JF - Journal of analytical atomic spectrometry N2 - Besides conventional scanning X-ray fluorescence imaging at synchrotron sources, full-field X-ray fluorescence (FF-XRF) imaging techniques that do not implicitly require spatial scanning of the sample have become available. FF-XRF has become achievable thanks to the development of a new type of energy dispersive CCD-based 2D detector, also referred to as a 'color X-ray camera (CXC)' or 'SLcam'. We report on different imaging schemes for biological samples using FF-XRF imaging: (a) 2D 'zoom' imaging with pinhole optics using the 'camera obscura' principle; (b) 2D 'fixed magnification' imaging using magnifying polycapillary optics; and (c) 3D-FF-XRF imaging using an X-ray sheet beam or computed tomography (CT). The different FF-XRF imaging modes are illustrated using the crustacean Daphnia magna, a model organism for investigating the effects of metals on organism/ecosystem health, and foraminifera, a class of amoeboid protist. Detailed analytical characterization of the set-up is performed through analyzing various reference materials in order to determine limits of detection (LODs) and sensitivities. Experiments were performed using the BAMline at the BESSY synchrotron (Berlin, Germany) and using the P06 Hard X-ray Microprobe at the PETRAIII synchrotron (Hamburg, Germany). KW - CXC KW - BAMline KW - Maia detector KW - Synchrotron PY - 2019 DO - https://doi.org/10.1039/c9ja00198k VL - 34 IS - 10 SP - 2083 EP - 2093 PB - Royal Society of Chemistry CY - Cambridge, United Kingdom AN - OPUS4-49359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Streli, C. A1 - Radtke, Martin T1 - On the way to full-field X-ray fluorescence spectroscopy imaging with coded apertures JF - Journal of Analytical Atomic Spectrometry N2 - Imaging with X-rays is a challenging field, due to the optical properties of X-rays. The fabrication of appropriate optics is usually expensive and requires an elaborate manufacturing process. One simpler and less expensive possibility of imaging high energy radiation is coded aperture imaging, a technique well established in astrophysics and also used in nuclear medicine or radiation detection, e.g., for nuclear decommissioning. Our aim is to adapt coded aperture imaging for X-ray fluorescence spectroscopy in the nearfield. In this work we show theoretical considerations and preliminary simulations of Image formation through a coded aperture and three different reconstruction methods to prepare the experiments. We used a new mask based on an inverted modified uniformly redundant array (MURA) that could be used for the construction of a decoding mask for all investigated geometrical arrangements. The most commonly used reconstruction method, convoluting the detected image with a Decoding mask, does not always deliver satisfactory results. This is more noticeable for small distances between the object, mask and detector. Hence, we developed two new reconstruction methods, one based on iterative algebraic optimization and another one based on a genetic algorithm. Both show good performance even in those cases where the convolution method fails. This provides a basis for further investigations of the ideal parameters for near field coded aperture imaging and refinements of the algorithms. We performed first measurements with a coded aperture at the BAMline at BESSY II and could successfully reconstruct a test object from the obtained recorded images. KW - X-ray fluorescence spectroscopy KW - Coded aperture KW - Imaging KW - Iterative reconstruction PY - 2020 DO - https://doi.org/10.1039/c9ja00232d VL - 35 IS - 2 SP - 347 EP - 356 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Kulla, Hannes A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Advances in Nickel Nanoparticle Synthesis via Oleylamine Route JF - nanomaterials N2 - Nickel nanoparticles are an active research area due to their multiple applications as catalysts in different processes. A variety of preparation techniques have been reported for the synthesis of these nanoparticles, including solvothermal, microwave-assisted, and emulsion techniques. The well-studied solvothermal oleylamine synthesis route comes with the drawback of needing standard air-free techniques and often space-consuming glassware. Here, we present a facile and straightforward synthesis method for size-controlled highly monodisperse nickel nanoparticles avoiding the use of, e.g., Schlenk techniques and space-consuming labware. The nanoparticles produced by this novel synthetic route were investigated using small-angle X-ray scattering, transmission electron microscopy, X-ray diffraction, and X-ray spectroscopy. The nanoparticles were in a size range of 4–16 nm, show high sphericity, no oxidation, and no agglomeration after synthesis. KW - Nanoparticle synthesis KW - Nickel nanoparticles KW - SAXS KW - TEM KW - XAS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507531 DO - https://doi.org/10.3390/nano10040713 VL - 10 IS - 4 SP - 713 PB - MDPI AN - OPUS4-50753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kulow, Anicó A1 - Kabelitz, Anke A1 - Grunewald, C. A1 - Seidel, R. A1 - Chapartegui-Arias, Ander A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Beyer, S. T1 - Observation of early ZIF-8 crystallization stages with X-ray absorption spectroscopy JF - Soft Matter N2 - The present study investigates early stages of ZIF-8 crystallization up to 5 minutes post mixing of precursor solutions. Dispersive X-ray Absorption Spectroscopy (DXAS) provides a refined understanding of the evolution of the coordination environment during ZIF-8 crystallization. Linear Combination Fiting (LCF) suggests tetrakis(1-methylimidazole)zinc2+ to be a suitable and stable mononuclear structure analogue for some early stage ZIF-8 intermediates. Our results pave the way for more detailed studies on physico-chemical aspects of ZIF-8 crystallization to better control tailoring ZIF-8 materials for specific applications. KW - In-situ KW - XANES KW - ZIF-8 KW - Crystallization PY - 2020 DO - https://doi.org/10.1039/D0SM01356K SN - 1744-6848 VL - 17 IS - 2 SP - 331 EP - 334 PB - Royal Scociety of Chemistry AN - OPUS4-51723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, U.E.A. A1 - Streli, C. A1 - Radtke, Martin T1 - Comparison of three reconstruction methods based on deconvolution, iterative algorithm and neural network for X-ray fluorescence imaging with coded apertures JF - Journal of Analytical Atomic Spectrometry N2 - X-ray imaging methods are used in many fields of research, as they allow a non-destructive Investigation of the elemental content of various samples. As for every imaging method, for X-ray imaging the optics are of crucial importance. However, these optics can be very expensive and laborious to build, as the requirements on surface roughness and precision are extremely high. Angles of reflection and refraction are often in the range of a few mrad, making a compact design hard to achieve. In this work we present a possibility to simplify X-ray imaging. We have adapted the coded aperture method, a high energy radiation imaging method that has its origins in astrophysics, to full field X-ray fluorescence imaging. In coded aperture imaging, an object is projected through a known mask, the coded aperture, onto an area sensitive detector. The resulting image consists of overlapping projections of the object and a reconstruction step is necessary to obtain the information from the recorded image. We recorded fluorescence images of different samples with an energy-dispersive 2D detector (pnCCD) and investigated different reconstruction methods. With a small coded aperture with 12 holes we could significantly increase the count rate compared to measurements with a straight polycapillary optic. We show that the reconstruction of two different samples is possible with a deconvolution approach, an iterative algorithm and a neural network. These results demonstrate that X-ray fluorescence imaging with coded apertures has the potential to deliver good results without scanning and with an improved count rate, so that measurement times can be shortened compared to established methods. KW - X-ray fluorescence imaging KW - Coded apertures KW - Imaging KW - Elemental mapping KW - Image reconstruction PY - 2020 DO - https://doi.org/10.1039/d0ja00146e VL - 35 IS - 7 SP - 1423 EP - 1434 PB - Royal Society of Chemistry CY - United Kingdom AN - OPUS4-51518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Fischer, M. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - Inca figurines from the Ethnologisches Museum in Berlin: an analytical study of some typical and atypical productions JF - Bulletin de l’Institut Français d’Études Andines N2 - Fourteen hollow and one cast anthropomorphic and zoomorphic figurines produced in Incan times for ritual offerings from the Ethnologisches Museum in Berlin were selected to investigate the technologies and alloys used for their fabrication with portable optical microscopy and non-destructive XRF elemental analysis. This group of gold and silver figurines includes typical specimens of the Inca production, such as the four silver figurines from the Island Coati in Lake Titicaca and the two gold figurines from Pachacamac, as well as specimens that are seldom present in collections, which makes them atypical. In addition to the tall figurines with atypical hair or standing pose, one bicolour figurine half silver, half gold) and another with coloured inlays were included in this study for comparison. The large majority of the silver specimens are made from very high quality alloys and the gold figurines are made from alloys containing low copper contents and silver ranging from 30wt% to 52wt%. KW - Gold KW - pXRF KW - Inca PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-436015 DO - https://doi.org/10.4000/bifea.8232 SN - 0303-7495 VL - 46 IS - 1 SP - 221 EP - 251 PB - Institut Français d'Études Andines AN - OPUS4-43601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nowak, S. H. A1 - Petric, M. A1 - Buchriegler, J. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, Z. A1 - von Borany, J. A1 - Munnik, F. A1 - Radtke, Martin A1 - Renno, A. D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Tilgner, J. A1 - Wedell, R. T1 - Road to micron resolution with a color X-ray camera – polycapillary optics characterization T2 - arXiv.org N2 - In a color X-ray camera spatial resolution is achieved by means of a polycapillary optic conducting X-ray photons from small regions on a sample to distinct energy dispersive pixels on a CCD matrix. At present, the resolution limit of color X-ray camera systems can go down to several microns and is mainly restricted by Pixel dimensions. The recent development of an efficient subpixel resolution algorithm allows a release from pixel size, limiting the resolution only to the quality of theoptics. In this work polycapillary properties that influence the spatial resolution are systematized and assessed both theoretically and experimentally. It is demonstrated that with the current technological Level reaching one micron resolution is challenging, but possible. KW - Color X-ray camera KW - Polycapillary optics PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404404 UR - https://arxiv.org/abs/1705.08939 SN - 2331-8422 SP - 1 EP - 11 PB - Cornell University CY - Ithaca, NY AN - OPUS4-40440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manso, M. A1 - Pessanha, S. A1 - Guerra, M. A1 - Reinholz, Uwe A1 - Afonso, C. A1 - Radtke, Martin A1 - Lourenco, H. A1 - Carvalho, M. L. A1 - de Oliveira Guilherme Buzanich, Ana T1 - Assessment of Toxic Metals and Hazardous Substances in Tattoo Inks Using Sy-XRF, AAS, and Raman Spectroscopy JF - Biological Trace Element Research N2 - Synchrotron radiation X-ray fluorescence spectroscopy, in conjunction with atomic absorption and Raman spectroscopy, was used to analyze a set of top brand tattoo inks to investigate the presence of toxic elements and hazardous substances. The Cr, Cu, and Pb contents were found to be above the maximum allowed levels established by the Council of Europe through the resolution ResAP(2008)1 on requirements and criteria for the safety of tattoos and permanent makeup. Raman analysis has revealed the presence of a set of prohibited substances mentioned in ResAP(2008)1, among which are the pigments Blue 15, Green 7, and Violet 23. Other pigments that were identified in white, black, red, and yellow inks are the Pigment White 6, Carbon Black, Pigment Red 8, and a diazo yellow, respectively. The present results show the importance of regulating tattoo ink composition. KW - Synchrotron KW - Tattoo inks KW - XRF KW - Toxic metals KW - Hazardous substances PY - 2019 DO - https://doi.org/10.1007/s12011-018-1406-y VL - 187 IS - 2 SP - 596 EP - 601 PB - Springer AN - OPUS4-47369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - Witte, S. A1 - Beyer, S. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, H. A1 - Streli, C. T1 - A new experimental setup for time- and laterally-resolved X-ray absorption fine structure spectroscopy in a 'single shot' JF - Journal of Analytical Atomic Spectrometry N2 - In this work, a new setup for dispersive XAFS measurements is presented. This reproducible and scanningfree setup yields both time- and laterally-resolved XAFS experiments in a ‘single-shot’. It allows a straightforward adjustment for probing different elements covering many relevant applications in materials science. An incoming energetic broadband beam is diffracted by a Si (111) crystal after passing through the sample and collected by an area sensitive detector. Depending on the energy range of the incoming beam, XANES and/or EXAFS spectra can be recorded with a time resolution down to 1 s. The feasibility of this setup was demonstrated at the BAMline at BESSY II (Berlin, Germany) with reference Fe and Cu foils and the results are hereby presented and discussed. Additionally, an application where time resolution on the second scale is required is briefly evaluated. The presented example concerns studying early stages of zinc(II)2-methylimidazolate (ZIF-8) crystallization. This is particularly important for biomedical applications. KW - X-ray spectroscopy KW - X-ray absorption fine structure KW - Time-resolved KW - Laterally-resolved KW - Experimental setup PY - 2019 DO - https://doi.org/10.1039/c8ja00313k SN - 0267-9477 SN - 1364-5544 VL - 34 IS - 1 SP - 239 EP - 246 PB - Royal Society of Chemistry CY - London AN - OPUS4-47207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Gebhard, R. T1 - Synchrotron radiation–induced X-ray fluorescence (SRXRF) analyses of the Bernstorf Gold JF - Archeometry N2 - The gold finds from Bernstorf, in the Freising district of Bavaria, were discovered in 1998, in the area of a Bronze Age settlement. First analyses with X-ray fluorescence (XRF) revealed gold of an unusually high purity grade, which was explained by the use of cementation techniques. A newer analysis with laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) indicated an even higher purity. The analytical results were the starting point of an ongoing discussion. In this study, we re-analysed 11 gold samples with Synchrotron radiation–induced X-ray fluorescence at the BAMline at BESSY. In a thorough analysis, different excitation and detection conditions were applied to confirm or disprove the previous results. It was shown that the purity of the gold from the specimen is higher than 99.9%. The main impurities are silver in a range between 20 and 200 μg/g and copper between 1 and 10 μg/g. The results are in very good agreement with the LA–ICP–MS measurements and provide basic information for discussions about provenance, processing techniques or considerations of authenticity. KW - Gold KW - Synchrotron KW - XRF KW - BESSY KW - Archeometry PY - 2017 DO - https://doi.org/10.1111/arcm.12294 SN - 0003-813X SN - 1475-4754 VL - 59 IS - 5 SP - 891 EP - 899 PB - Wiley AN - OPUS4-42540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Michael A1 - Buzanich, Günter A1 - Jähn, Katharina A1 - Reinholz, Uwe A1 - Radtke, Martin T1 - Analysis of cobalt deposition in periprosthetic bone specimens by high-resolution synchroton XRF in undecalcified histological thin sections JF - Materialia N2 - Increasing numbers of implant revisions are a current clinical issue. Interactions of the endoprosthesis biomaterial with the body affect implantation time by wear processes, i.e. corrosion and abrasion. Previously, cobalt-chrome implants were shown to cause high levels of cobalt ions being deposited in the bone matrix. To determine a poten- tial functional role of these ions on bone homeostasis, we have developed a non-destructive dual analysis of highly sensitive elemental analysis by synchrotron XRF directly in undecalcified histological bone thin sections (4 μm). In this study, samples from 28 bone samples from hip endoprosthesis carriers (Surface Replacement Arthroplasty, metal-on-metal bearing) with an implant lifetime of 17–1750 days were used. Results were compared to age- matched control specimens. The histological analysis identified areas of bone cell activity and assigned them for XRF measurements. Co-Cr wear particles were identified in the bone marrow. In addition, Co ions were highly enriched in the mineralized bone matrix. The cobalt deposits were not homogeneously distributed, and areas of high signal intensity were identified. Co was distinctly deposited in the newly formed osteoid layer, but also within deeper layers of the bone matrix, whereby the Co concentration increased with higher degrees of bone matrix mineralization. In the current study, we determined cobalt accumulations in the bone matrix and showed for the first time via synchrotron XRF with a high spatial resolution direct on histological slides, that cobalt deposits in the mineralized bone matrix in a mineral-specific way that is dependent upon the implant lifetime. KW - Implant material KW - Cobalt deposition KW - Bone matrix KW - High-resolution synchrotron XRF KW - Histology PY - 2019 DO - https://doi.org/10.1016/j.mtla.2019.100290 SN - 2589-1529 VL - 6 SP - 100290, 1 EP - 8 PB - Elsevier Inc. CY - Amsterdam, Niederlande AN - OPUS4-47620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharf, Oliver A1 - Ihle, S. A1 - Ordavo, I. A1 - Arkadiev, V. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Soltau, H. A1 - Strüder, L. A1 - Thünemann, Andreas A1 - Wedell, R. T1 - Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera JF - Analytical chemistry N2 - For many applications there is a requirement for nondestructive analytical investigation of the elemental distribution in a sample. With the improvement of X-ray optics and spectroscopic X-ray imagers, full field X-ray fluorescence (FF-XRF) methods are feasible. A new device for high-resolution X-ray imaging, an energy and spatial resolving X-ray camera, is presented. The basic idea behind this so-called 'color X-ray camera' (CXC) is to combine an energy dispersive array detector for X-rays, in this case a pnCCD, with polycapillary optics. Imaging is achieved using multiframe recording of the energy and the point of impact of single photons. The camera was tested using a laboratory 30 µm microfocus X-ray tube and synchrotron radiation from BESSY II at the BAMline facility. These experiments demonstrate the suitability of the camera for X-ray fluorescence analytics. The camera simultaneously records 69696 spectra with an energy resolution of 152 eV for manganese Kα with a spatial resolution of 50 µm over an imaging area of 12.7 × 12.7 mm². It is sensitive to photons in the energy region between 3 and 40 keV, limited by a 50 µm beryllium window, and the sensitive thickness of 450 µm of the chip. Online preview of the sample is possible as the software updates the sums of the counts for certain energy channel ranges during the measurement and displays 2-D false-color maps as well as spectra of selected regions. The complete data cube of 264 × 264 spectra is saved for further qualitative and quantitative processing. KW - Color X-ray camera KW - X-ray fluorescence KW - pnCCD KW - Polycapillary optic KW - Synchrotron radiation PY - 2011 DO - https://doi.org/10.1021/ac102811p SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 7 SP - 2532 EP - 2538 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Emmerling, Franziska A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas T1 - Real-time monitoring of copolymer stabilized growing gold nanoparticles JF - Langmuir N2 - A great challenge in the production of nanoparticles with defined sizes and properties is to control their growth in situ. We developed a dedicated combined small-angle X-ray scattering (SAXS) and X-ray absorption spectroscopy (XAS) setup to monitor nanoparticle formation in solution. The capabilities of simultaneously deriving particle sizes and oxidation states of atoms/ions are illustrated for the formation of spherical gold nanoparticles by the reduction of hydrogen tetrachloroaureate (HAuCl4). Particles with initial radii of 4.60 ± 0.10 nm and final radii of 5.67 ± 0.10 nm were produced in a levitated droplet with a volume of 4 µL. An ethylene oxide/propylene oxide triblock copolymer PEO-PPO-PEO (Pluronic F-127) functions as reducing agent and colloidal stabilizer. XANES shows in situ how the gold was reduced in the droplet from Au(III) to Au(0), and simultaneously SAXS recorded the size distribution of the formed nanoparticles. It is shown that the final particle number is reached quickly. Thereafter, only the particles’ sizes increase. Comparison of XANES and SAXS shows that the quantity of Au(0) is higher than the quantity of gold located in the nanoparticles while the particles are growing. Finally, all the Au(0) is found in the nanoparticles. We tentatively attribute this finding to the pseudo crown ether effect of the polymer surfactant that kinetically stabilizes gold atoms when formed from gold ions within their protecting cavity. A simple “burst” mechanism for the gold nanoparticle formation is the consequence. The possibility of an inhomogeneous particles structure with an enhanced density near the particle surface is discussed. PY - 2010 DO - https://doi.org/10.1021/la903829q SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 8 SP - 5889 EP - 5894 PB - American Chemical Society CY - Washington, DC AN - OPUS4-21223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Kraehnert, R. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Emmerling, Franziska T1 - New insights of the nucleation and growth process of gold nanoparticles via in situ coupling of SAXS and XANES JF - Journal of physics / Conference series N2 - Although metallic nanoparticles play an important role in the area of nanotechnology, a coherent mechanistic explanation for the evolution of the particles during their chemical synthesis has not yet been provided in many cases. To gain a profound understanding of the growth mechanism of colloidal nanoparticles, new approaches using Small Angle X-Ray Scattering (SAXS) combined with X-ray absorption near-edge structure (XANES) are presented. This combination allows for insights into two prominent syntheses routes of gold nanoparticles (GNP): The 'slow' reaction using sodium citrate (30-90 min) as a reducing agent and the 'fast' reaction employing NaBH4 (within few seconds). In the first case data derived with the coupled XANES and SAXS suggests a four-step particle formation mechanism. For the second system a time resolution in the order of 100-200 ms was achieved by coupling a common laboratory SAXS instrument with a microstructured mixer, which allows data acquisition in a continuous-flow mode. The results indicate a coalescence driven growth process. Based on the capabilities to deduce the size, number and polydispersity of the particles, the results of both methods enable the development of mechanistic schemes explaining the different phases of particle formation and growth, thus providing a basis for improved control over the synthesis processes. KW - SAXS KW - XANES KW - Nanoparticle formation PY - 2010 DO - https://doi.org/10.1088/1742-6596/247/1/012051 SN - 1742-6588 SN - 1742-6596 VL - 247 IS - 1 SP - 012051-1 - 012051-10 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-22684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Streli, C. T1 - Impurities in multicrystalline silicon wafers for solar cells detected by synchrotron micro-beam X-ray fluorescence analysis JF - Journal of analytical atomic spectrometry N2 - We report on the trace analysis of copper and iron impurities in multicrystalline silicon wafers with the microbeam X-ray fluorescence (µ-XRF) technique. The efficiency of solar cells, which are based on multicrystalline silicon wafers, is strongly influenced by minor contamination with metals such as copper and iron. Application of compound refractive lenses (CRLs) in µ-XRF allows versatile two-dimensional mapping of relevant contaminations and localization of their sites of deposition. In this context, the measured bulk average limit of detection (LOD) was one picogram of iron and copper per gram of silicon. We suggest that µ-XRF is a valuable tool for non-destructive spatial (3D) quantification of metal impurities in a wide range of materials and devices whose functioning could be critically affected by impurities. KW - X-ray micro beam KW - Compound refractive lens KW - Solar cell KW - Silicon impurities PY - 2012 DO - https://doi.org/10.1039/c2ja30188a SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 11 SP - 1875 EP - 1881 PB - Royal Society of Chemistry CY - London AN - OPUS4-26791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Piotrowiak, T. A1 - Reinholz, Uwe A1 - Ludwig, A. A1 - Emmerling, Franziska A1 - Streli, C. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Exploring the Depths of Corrosion: A Novel GE-XANES Technique for Investigating Compositionally Complex Alloys JF - Analytical Chemistry N2 - In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD detector, we provide a scanning-free, nondestructive, depth-resolved analysis in a sub-micrometer depth range, which is especially relevant for layered materials, such as corroded CCAs. Our setup allows for spatial and energy-resolved measurements and directly extracts the desired fluorescence line, free from scattering events and other overlapping lines. We demonstrate the potential of our approach on a compositionally complex CrCoNi alloy and a layered reference sample with known composition and specific layer thickness. Our findings indicate that this new GE-XANES approach has exciting opportunities for studying surface catalysis and corrosion processes in real-world materials. KW - Degradation mechanisms KW - Grazin exit XANES KW - Depth resolved XANES KW - Compositional complex alloys KW - Corrosion PY - 2023 DO - https://doi.org/10.1021/acs.analchem.3c00404 VL - 95 SP - 4810 EP - 4818 PB - ACS Publications AN - OPUS4-57823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Förste, F. A1 - Bauer, L. A1 - Streeck, C. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Kadow, D. A1 - Keil, C. A1 - Mantouvalou, I. T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques JF - Analytical Chemistry N2 - As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time. KW - BAMline KW - Synchrotron KW - XRF KW - CXC KW - Cocoa PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05370 VL - 95 SP - 5627 EP - 5635 PB - ACS Publications AN - OPUS4-57832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Guerra, M.F. A1 - Martinón-Torres, M. A1 - Lemasson, Q. A1 - Moignard, B. A1 - Pacheco, C. A1 - Pichon, L. A1 - Macdonald, L. A1 - Hess, M. A1 - Tissot, I. ED - Guerra, M. F. ED - Martinón-Torres, M. ED - Quirke, S. T1 - Analytical approaches to Egyptian goldwork T2 - Ancient Egyptian gold: Archaeology and science in jewellery (3500–1000 bc) N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail. KW - Gold KW - Synchrotron KW - D2XRF KW - Egypt PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039 DO - https://doi.org/10.17863/CAM.99681 SP - 131 EP - 191 AN - OPUS4-58603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Stephan-Scherb, Christiane T1 - A µ‐XANES study of the combined oxidation/sulfidation of Fe–Cr model alloys JF - Materials and Corrosion N2 - The precise analysis of cation diffusion profiles through corrosion scales is an important aspect to evaluate corrosion phenomena under multicomponent chemical load, as during high‐temperature corrosion under deposits and salts. The present study shows a comprehensive analysis of cation diffusion profiles by electron microprobe analysis and microbeam X‐ray absorption near edge structure (µ‐XANES) spectroscopy in mixed oxide/sulfide scales grown on Fe–Cr model alloys after exposing them to 0.5% SO2. The results presented here correspond to depth‐dependent phase identification of oxides and sulfides in the corrosion scales by µ‐XANES and the description of oxidation‐state‐dependent diffusion profiles. Scales grown on low‐ and high‐alloyed materials show both a well‐pronounced diffusion profile with a high concentration of Fe3+ at the gas and a high concentration of Fe2+ at the alloy interface. The distribution of the cations within a close‐packed oxide lattice is strongly influencing the lattice diffusion phenomena due to their different oxidation states and therefore different crystal‐field preference energies. This issue is discussed based on the results obtained by µ‐XANES analysis. KW - X-ray absorption spectroscopy KW - Oxidation KW - Sulfidation PY - 2019 DO - https://doi.org/10.1002/maco.201810644 VL - 70 IS - 8 SP - 1360 EP - 1370 PB - Wiley VCH-Verlag AN - OPUS4-47934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kühn, Andreas A1 - Scharf, Oliver A1 - Ordavo, I. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Berger, Achim A1 - Ostermann, Markus A1 - Panne, Ulrich T1 - Pushing the limits for fast spatially resolved elemental distribution patterns JF - Journal of analytical atomic spectrometry N2 - A new setup for fast spatially resolved measurements of elemental trace amounts under total reflection conditions using a new colour X-ray camera is described. Samples prepared on conventional total reflection X-ray fluorescence (TXRF) reflectors were measured at BESSY II synchrotron. A spatial resolution of 50 × 50 µm² was obtained, while the required time for the investigation of a 10 × 10 mm² sample is 30 seconds. The set-up is up to 350 times faster than conventional X-ray fluorescence systems for elemental traces. The major components of the X-ray camera are polycapillary optics and a pn-CCD chip with an active area of 13 × 13 mm². This area is divided into 264 × 264 pixels of 48 × 48 µm². A full X-ray spectrum with a resolution of 152 eV @ 5.9 keV and a chip temperature of 246 K is recorded for each pixel. The chip has a read-out rate of 400 Hz. PY - 2011 DO - https://doi.org/10.1039/c1ja10069f SN - 0267-9477 SN - 1364-5544 VL - 26 SP - 1986 EP - 1989 PB - Royal Society of Chemistry CY - London AN - OPUS4-24386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Wilke, Manuel A1 - Szczerba, Wojciech A1 - Reinholz, Uwe A1 - Emmerling, Franziska T1 - Mechanochemical synthesis and characterisation of two new bismuth metal organic frameworks JF - CrystEngComm N2 - Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine-2,5-dicarboxylate and bismuth cations are presented: (H2Im)[Bi(1,4-bdc)2] (1) and [Bi(pydc)(NO3)2(H2O)2]*H2O (2) (bdc = benzenedicarboxylate, H2Im = imidazole cation, pydc = pyridinedicarboxylate). Both compounds were synthesised via grinding and the crystal structure of compound (2) was solved based on its powder diffraction pattern. Compound 1 crystallises isostructurally to the dimethyl ammonium containing compound (dma)[(Bi(1,4-bdc)2]. Raman spectroscopy and Extended X-ray absorption fine structure (EXAFS) measurements provided additional information about the two mechanochemically synthesised metal organic compounds. KW - Crystal structure KW - Mechanochemically synthesis KW - Powder diffraction measurements PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306296 DO - https://doi.org/10.1039/C3CE42633E SN - 1466-8033 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. VL - 16 IS - 25 SP - 5560 EP - 5565 CY - London, UK AN - OPUS4-30629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -