TY - JOUR A1 - Ecker, Klaus A1 - Wätjen, U. A1 - Berger, Achim A1 - Persson, L. A1 - Pritzkow, Wolfgang A1 - Radtke, Martin A1 - Riesemeier, Heinrich T1 - RBS, SY-XRF, INAA and ICP-IDMS of antimony implanted in silicon - A multi-method approach to characterize and certify a reference material JF - Nuclear instruments and methods in physics research B N2 - A layer of Sb atoms, implanted with an energy of 400 keV and a nominal dose of 5×1016 atoms/cm2 into a high purity silicon wafer, was certified for its areal density (atoms/cm2) using Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA) and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) and for its isotope ratio using INAA and ICP-IDMS. Excellent agreement between the results of the different independent methods was found. In the present work, the measurements of the homogeneity of the areal density of Sb, previously determined with RBS in spots having 1 mm diameter, are improved with synchrotron X-ray fluorescence analysis: Higher precision in even smaller sample spots allows to estimate a reduced inhomogeneity of the whole batch of samples of the order of only 0.4%. Thus the uncertainty of the certified value can further be reduced. Down to fractions of a chip with 0.3×0.4 mm2 area, the areal density is now certified as (4.81±0.06)×1016 Sb atoms/cm2, where the expanded uncertainty 0.06 (coverage factor k=2) corresponds to only 1.2%. The relative merits of the different analytical methods are discussed. KW - Certified reference material KW - RBS KW - INAA KW - ICP-IDMS KW - XRF KW - SY-XRF PY - 2002 DO - https://doi.org/10.1016/S0168-583X(01)01038-2 SN - 0168-583X SN - 1872-9584 VL - 188 IS - 1-4 SP - 120 EP - 125 PB - Elsevier CY - Amsterdam AN - OPUS4-13870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riesemeier, Heinrich A1 - Ecker, Klaus A1 - Görner, Wolf A1 - Müller, Bernd R. A1 - Radtke, Martin A1 - Krumrey, M. T1 - Layout and first XRF Applications of the BAMline at BESSY II+ JF - X-ray spectrometry N2 - The first hard x-ray beamline at BESSY II has been installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a double-multilayer monochromator and a double-crystal monochromator. Depending on the application, the two devices are used separately or in-line. The main applications of the monochromatic radiation with photon energies up to 60 keV are x-ray fluorescence analysis, micro computed tomography, x-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV is available for radiometric applications. KW - BAMline KW - XRF PY - 2005 DO - https://doi.org/10.1002/xrs.750 SN - 0049-8246 VL - 34 IS - 2 SP - 160 EP - 163 PB - Wiley CY - Chichester AN - OPUS4-11929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Radtke, Martin A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Riesemeier, Heinrich A1 - Bevers, H. T1 - Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings JF - Applied physics A N2 - New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606–1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of µg/cm². Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is – together with external micro-proton-induced X-ray emission – the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French–German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection. KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2006 DO - https://doi.org/10.1007/s00339-006-3505-4 SN - 0947-8396 VL - 83 IS - 2 SP - 169 EP - 173 PB - Springer CY - Berlin AN - OPUS4-12532 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 - 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 - 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 - 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 - JOUR A1 - Rauwolf, M. A1 - Turyanskaya, A. A1 - Roschger, A. A1 - Prost, J. A1 - Simon, R. A1 - Scharf, O. A1 - Radtke, Martin A1 - Schoonjans, Tom A1 - de Oliveira Guilherme Buzanich, Ana A1 - Klaushofer, K. A1 - Wobrauschek, P. A1 - Hofstaetter, J. G. A1 - Roschger, P. A1 - Streli, C. T1 - Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups JF - Journal of Synchrotron Radiation N2 - In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution. KW - Synchrotron KW - BAMline KW - BESSY KW - XRF KW - X-ray Color Camera PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391944 DO - https://doi.org/10.1107/S1600577516017057 SN - 1600-5775 VL - 24 SP - 307 EP - 311 PB - International Union of Crystallography AN - OPUS4-39194 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 -