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 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 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-370892 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 - 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 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 U6 - 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 - 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 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 U6 - 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 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 U6 - 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 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 U6 - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Margreiter, R. A1 - Eberhardt, K. A1 - Niemeyer, B. A1 - Strub, E. T1 - Investigation on fire gilding using XRF and NAA N2 - Fire-gilding or amalgam gilding is a historical technique for the gilding of objects. The object to be gilded is coated with an amalgam (a solution of gold (Au) in mercury (Hg)). By heating, the largest part of the Hg is subsequently evaporated and there remains a gold layer, containing still detectable amounts of Hg. The information on the used gilding technique might be crucial for the conservation and preservation of archaeological objects. Therefore, the main objective of this work is the detailed understanding of the behaviour of Hg under conditions of fire gilding. I.e. the understanding of the diffusion and evaporating behaviour of Hg, depending on parameters like substrate material (silver, copper, bronze, brass...), heating temperature and duration, and the resulting Hg depth profiles under these conditions. Secondary objective is the establishment of a measurement protocol for the unambiguous identification of different types of gilding, based solely on non-destructive methods, which can be applied to historical samples. In a first step, fire-gilded samples have been prepared on Cu and Ag sheet metal, respectively. Some of the gildings were produced by a professional goldsmith; another set of samples was produced under laboratory conditions. These samples have been examined with NAA (neutron activation analysis) and SR-XRF (synchrotron radiation induced X-ray fluorescence). First results of these measurements will be presented and discussed. T2 - Synchrotron Radiation and Neutrons in Art & Archaeology (SR2A) CY - Chicago, IL, USA DA - 06.09.2016 KW - Synchrotron KW - BAMline KW - XRF KW - Archaeometry PY - 2016 AN - OPUS4-38766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Es ist nicht alles Gold was glänzt - Die Analyse von Gold mit Synchrotronstrahlung N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vortragsreihe „Naturwissenschaftliche Einsichten in Kunst- und Kulturgut" CY - Dresden, Germany DA - 13.10.2016 KW - Synchrotron KW - BAMline KW - Gold KW - XRF PY - 2016 AN - OPUS4-38809 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee – Analyse von Gold mit Synchrotronstrahlung N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 04.11.2016 KW - Synchrotron KW - BAMline KW - Gold KW - XRF PY - 2016 AN - OPUS4-38810 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. T1 - The Colour X-ray Camera – Basics and Applications of a 2D X-ray Detector N2 - The Color X-ray Camera CXC or SLcam® is an energy-resolving X-ray camera capable of energy- and space-resolved measurements. It consists of a high-speed CCD detector coupled to a polycapil-lary optic that conducts the X-ray photons from the probe to distinct pixels onto the detector. The camera is capable of fast acquisition of spatially and energy resolved fluorescence images. A dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the elements distribution in a sample. It was developed in a joint project with BAM, IFG Berlin and PN Sensors. In this contribution we will mainly discuss the use of the CXC at our beamline, the BAMline at BESSY II and imaging applications of the CXC from different areas, like biology and archaeometry. Additionally new developments for the use of the detector without optics, like wavelength dispersive detection or 1shot-XANES, will be presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - Wien, Austria DA - 20.01.2016 KW - Synchrotron KW - BAMline KW - XRF PY - 2016 AN - OPUS4-38811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kabelitz, Anke A1 - Rolf, Simone A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Emmerling, Franziska T1 - First in situ measurements with a newly developed SR-based ‘Single-shot‘ EXAFS set-up N2 - The newly developed EXAFS set-up comprises both time- and spatially-resolved EXAFS information simultaneously in a single-shot. This facile, stable and scanningless set-up was tested at the BAMline @ BESSY-II (Berlin, Germany). The primary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). 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 an area sensitive detector based on a CCD camera, in a theta - 2 theta geometry. The first in situ measurements were successfully carried out and hereby presented. The case-study involved a well known reaction, in which structural changes are induced over time, and continuously measured. We were able to track structural changes within a 1s time resolution. T2 - European Conference on X-Ray Spectrometry (EXRS) CY - Gothenburg, Sweden DA - 19.06.2016 KW - Synchrotron KW - BAMline KW - EXAFS PY - 2016 AN - OPUS4-38807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -