TY - CONF A1 - Lange, T. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Partial oxidation of o-xylene to phthalic anhydride inside of the explosion regime using a micro structured reactor N2 - The heterogeneously catalyzed gas phase oxidation of o-xylene (oX) to phthalic anhydride (PA) was investigated above the lower explosion limit of appr. 2 vol.% oxylene in air using a micro structured reactor. For these investigations a V2O5/T1O2 grafting catalyst was applied as micro fixed bed and as wall catalyst. Up to 7 voL% 0-xylene, selectivities as well as space-time-yields to PA could be increased siginificantly. At o-xylene concentrations higher than 7 vol. %, the selectivity and space-time-yield to PSA decreased, probably due to a hotspot, which was predicted at high o-xylene concentrations with an approximation and could be indirectly approved by thermal deactivation of the used catalyst. T2 - 2012 AIChE Annual meeting CY - Pittsburgh, PA, USA DA - 28.10.2012 KW - O-xylene oxidation KW - V2O5/TiO2 catalyst KW - Micro structured reactor KW - Explosion regime KW - Micro reactor KW - Explosion KW - Phthalic anhydride KW - Partial oxidation PY - 2013 SN - 9781622767380 SP - 90 EP - 93 AN - OPUS4-28706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Traulsen, C. H.-H. A1 - Kunz, V. A1 - Heinrich, Thomas A1 - Richter, S. A1 - Holzweber, Markus A1 - Schulz, A. A1 - von Krbek, L. K. S. A1 - Scheuschner, U. T. J. A1 - Poppenberg, J. A1 - Unger, Wolfgang A1 - Schalley, C. A. T1 - Synthesis and coordinative layer-by-layer deposition of pyridine-functionalized gold nanoparticles and tetralactam macrocycles on silicon substrates N2 - Coordination chemistry was applied to deposit pyridine-functionalized gold nanoparticles on silicon substrates. The particles were synthesized through the Brust/Schiffrin route with a subsequent ligand exchange reaction yielding well-defined particles of two different sizes. Multilayer deposition was carried out on a pyridine-terminated SAM, anchored on a hydroxyl-terminated silicon surface. Analogously, Hunter/Vögtle-type tetralactam macrocycle multilayers were deposited as well as mixed layers containing both either in an alternating sequence or as a macrocycle multilayer with a terminating nanoparticle layer. These composite layers were examined with respect to their ability to bind squaraine axles in the macrocycle cavities. The amount of guest bound is higher for the composite layer with alternating macrocycles and nanoparticles. KW - Layer-by-layer deposition KW - Functionalized Au nanoparticles KW - SEM KW - TEM KW - DLS KW - XPS KW - NEXAFS KW - ToF-SIMS KW - IR KW - UV-vis PY - 2013 DO - https://doi.org/10.1021/la403222x SN - 0743-7463 SN - 1520-5827 VL - 29 IS - 46 SP - 14284 EP - 14292 PB - American Chemical Society CY - Washington, DC AN - OPUS4-29699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Ding, T. A1 - Valkiers, S. A1 - De Bièvre, P. A1 - Taylor, P.D.P. A1 - Gonfiantini, R. A1 - Krouse, R. T1 - Calibrated sulfur isotope abundance ratios of three IAEA sulfur isotope reference materials and V-CDT with a reassessment of the atomic weight of sulfur N2 - Calibrated values have been obtained for sulfur isotope abundance ratios of sulfur isotope reference materials distributed by the IAEA (Vienna). For the calibration of the measurements, a set of synthetic isotope mixtures were prepared gravimetrically from high purity Ag2S materials enriched in32S, 33S, and 34S. All materials were converted into SF6 gas and subsequently, their sulfur isotope ratios were measured on the SF5+ species using a special gas source mass spectrometer equipped with a molecular flow inlet system (IRMM’s Avogadro II amount comparator). Values for the 32S/34S abundance ratios are 22.650 4(20), 22.142 4(20), and 23.393 3(17) for IAEA-S-1, IAEA-S-2, and IAEA-S-3, respectively. The calculated 32S/34S abundance ratio for V-CDT is 22.643 6(20), which is very close to the calibrated ratio obtained by Ding et al. (1999). In this way, the zero point of the VCDT scale is anchored firmly to the international system of units SI. The 32S/33S abundance ratios are 126.942(47), 125.473(55), 129.072(32), and 126.948(47) for IAEA-S-1, IAEA-S-2, IAEA-S-3, and V-CDT, respectively. In this way, the linearity of the V-CDT scale is improved over this range. The values of the sulfur molar mass for IAEA-S-1 and V-CDT were calculated to be 32.063 877(56) and 32.063 911(56), respectively, the values with the smallest combined uncertainty ever reported for the sulfur molar masses (atomic weights). PY - 2001 DO - https://doi.org/10.1016/S0016-7037(01)00611-1 SN - 0016-7037 SN - 1872-9533 VL - 65 IS - 15 SP - 2433 EP - 2437 PB - Elsevier Science CY - New York, NY AN - OPUS4-1137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich A1 - Valkiers, S. A1 - Aregbe, Y. A1 - Bréas, O. A1 - Taylor, P. A1 - Ding, T. ED - Gills, T. T1 - Gravimetrically Prepared Isotope Mixtures to Produce Isotopic Reference Materials for Sulfur with SI Traceable Ratios T2 - 8th International Symposium on Biological and Environmental Reference Materials ; 8th BERM CY - Bethesda, MD, USA DA - 2000-09-17 PY - 2001 SN - 1618-2642 VL - 370 IS - 2-3 SP - 141 PB - Springer CY - Berlin AN - OPUS4-990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Ding, T. A1 - Valkiers, S. A1 - Quetel, C. A1 - De Bièvre, P. A1 - Taylor, P. A1 - Gonfiantini, R. T1 - Preparation of two synthetic isotope mixtures for the calibration of isotope amount ratio measurements of sulfur N2 - Two synthetic isotope mixtures for the calibration of sulfur isotope amount ratio measurements were gravimetrically prepared from high purity Ag2S materials enriched in 32S, 33S, and 34S. The mixtures were made so as to closely resemble the (natural) isotopic composition of the materials to be “calibrated”. This allowed a totally independent evaluation, on the same samples, of the relative combined uncertainty of: (a) the procedure to perform direct measurements of the amount of substance ratios of gas isotopes in the redetermination of the Avogadro constant and (b) the gravimetric preparation procedure. The result of both procedures, mass spectrometry and gravimetry, agree to a relative uncertainty of 3 × 10-4 for sulfur amount ratio measurements of the major abundant isotopes. Thus it seems that a direct measurement of isotopic gas mixtures (e.g. of natural isotopic composition) is now possible for sulfur—and probably also for other gaseous isotopes—without necessarily having to rely on “calibration” by means of values provided by measurements of gravimetrically prepared isotope mixtures. However, synthetic mixtures may be needed for validation and verification purposes, in particular for quality assurance. KW - Sulfur KW - Absolute isotope amount ratio KW - Synthetic isotope mixtures KW - Sulfur hexafluoride KW - Mass spectrometry PY - 2000 DO - https://doi.org/10.1016/S1387-3806(99)00235-3 SN - 0168-1176 SN - 0020-7381 SN - 1387-3806 SN - 1873-2798 VL - 197 IS - 1-3 SP - 131 EP - 137 PB - Elsevier CY - Amsterdam AN - OPUS4-913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hofmann, T. A1 - Kipphardt, Heinrich A1 - Venzago, C. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Comparison of different calibration strategies for the analysis of zinc and other pure metals by using the GD-MS instruments VG 9000 and element GD N2 - Synthetic pressed metal powder standards doped with standard solutions were used for the calibration of both commercially available high resolution GD-MS instruments Element GD and VG 9000 for zinc matrix. Different quantification procedures (IBR, Standard RSF, matrix matched RSF from the calibration with CRMs and use of doped synthetic standards) are compared using zinc matrix as an example, whereas the calibration with doped pellets turned out to be the best quantification technique for high-purity materials. The applicability of the Standard RSF concept is scrutinised. In this context, RSF values for several Matrices (Co, Cu, Fe, In and Zn) are reported additionally. PY - 2010 DO - https://doi.org/10.1039/b921649a SN - 0267-9477 SN - 1364-5544 VL - 25 SP - 314 EP - 321 PB - Royal Society of Chemistry CY - London AN - OPUS4-22376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, T. A1 - Richter, Silke A1 - Matschat, Ralf A1 - Kipphardt, Heinrich T1 - Determination of the total purity of a high-purity silver material to be used as a primary standard for element determination N2 - A candidate material for the use as primary standard for silver determination was characterized with respect to total purity. Except the radioactive elements and He, all possible impurities were considered. Based on glow discharge mass spectrometry, inductively coupled plasma-mass spectrometry and carrier gas hot extraction measurements, the demonstrated total purity and its standard uncertainty is w(Ag) = (99.999 52 ± 0.000 11) %. The purity value and its uncertainty is dominated by the contributions from the measurements of the nonmetallic impurities, namely S, N, C and O. KW - Silver KW - Purity KW - Total purity KW - Primary standard KW - Element determination PY - 2013 DO - https://doi.org/10.1007/s00769-013-0988-5 SN - 0949-1775 SN - 1432-0517 VL - 18 IS - 4 SP - 341 EP - 349 PB - Springer CY - Berlin AN - OPUS4-28971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mühler, T. A1 - Wirth, Cynthia A1 - Ascheri, Mary A1 - Nicolaides, Dagmar A1 - Heinrich, J. A1 - Günster, Jens T1 - Slurry-based powder beds for the selective laser sintering of silicate ceramics N2 - Selective laser sintering of ceramic powders is a promising technique for the additive manufacturing of complex- and delicate-shaped ceramic parts. Most techniques have in common that the powder to be sintered is spread to a thin layer as a dry powder by means of a roller or shaker system. These layers have a relatively low density. On the other hand, appreciable densities can be reached with the use of ceramic slurries as the starting material. Therefore, the layer-wise slurry deposition (LSD) process has been developed. Layer stacks, i.e. powder beds, built up by employing the LSD technology exhibit a density comparable to ceramic powder compacts processed by means of conventional forming technologies. Writing the layer information with a focused laser beam in these dense ceramic powder compacts enables the manufacture of ceramic bodies with a high density and precision in contour. KW - Additive Fertigung KW - Keramik PY - 2015 DO - https://doi.org/10.4416/JCST2015-0007 SN - 2190-9385 VL - 6 IS - 2 SP - 113 EP - 118 PB - Göller CY - Baden-Baden AN - OPUS4-34962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mühler, T. A1 - Helsch, G. A1 - Heinrich, J.G. A1 - Yao, Dongxu A1 - Gräf, S. A1 - Müller, F.A. A1 - Günster, Jens T1 - Strategies for the selective volume sintering of ceramics N2 - The present study is dealing with the basic physics for a novel way to generate a free-formed ceramic body, not like common layer by layer, but directly by Selective Volume Sintering (SVS) in a compact block of ceramic powder. To penetrate with laser light into the volume of a ceramic powder compact it is necessary to investigate the light scattering properties of ceramic powders. Compared with polymers and metals, ceramic materials are unique as they offer a wide optical window of transparency. The optical window typically ranges from below 0.3 up to 5 µm wave length. In the present study thin layers of quartz glass (SiO2) particles have been prepared. As a function of layer thickness and the particle size, transmission and reflection spectra in a wave length range between 0.5 and 2.5 µm have been recorded. Depending on the respective particle size and by choosing a proper relation between particle size and wave length of the incident laser radiation, it is found that light can penetrate a powder compact up to a depth of a few millimeters. With an adjustment of the light absorption properties of the compact the initiation of sintering in the volume of the compact is possible. KW - Additive Manufacturing PY - 2014 DO - https://doi.org/10.1557/jmr.2014.174 SN - 0884-2914 VL - 29 IS - 17 SP - 2095 EP - 2099 PB - Materials Research Society CY - Warrendale, Pa. AN - OPUS4-32544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Williams, S. H. A1 - Hilger, A. A1 - Kardjilov, N. A1 - Manke, I. A1 - Strobl, M. A1 - Douissard, P.A. A1 - Martin, T. A1 - Riesemeier, Heinrich A1 - Banhart, J. T1 - Detection system for microimaging with neutrons N2 - A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hardware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 µm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution measurements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 µm with a field of view of 6 mm × 6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments. KW - Instrumentation for neutron sources KW - Neutron radiography KW - Neutron detectors (cold, thermal, fast neutrons) PY - 2012 DO - https://doi.org/10.1088/1748-0221/7/02/P02014 SN - 1748-0221 VL - 7 IS - P02014 SP - 1 EP - 26 PB - Inst. of Physics Publ. CY - London AN - OPUS4-26433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wirth, Cynthia A1 - Müller, Ralf A1 - Günster, Jens A1 - Mühler, T. A1 - Görke, R. A1 - Heinrich, J.G. T1 - Submicrometer silica spheres generated by laser fuming N2 - The production of agglomerate-free SiO2 particles exhibiting a monomodal distribution of particle sizes of around 300 nm by means of direct laser fuming of micrometric SiO2 powders has been successfully demonstrated. With a 12 kW cw CO2 laser system, a production rate of up to 1 kilogram powder per hour was achieved. Almost ideal spherical amorphous SiO2 particles in a broad particle size distribution between 10 nm and several 100 nm (d50 ≈ 300 nm) were synthesized. Several observations suggest weak agglomeration forces between the particles. A temperature reduction of 200 °C for sintering powder compacts was observed. KW - Laser KW - SiO2 KW - Nanopowder PY - 2013 DO - https://doi.org/10.4416/JCST2012-00033 SN - 2190-9385 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 4 IS - 1 SP - 11 EP - 18 PB - Göller CY - Baden-Baden AN - OPUS4-31423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mühler, T. A1 - Heinrich, J. A1 - Wirth, Cynthia A1 - Günster, Jens T1 - Slurry-based additive manufacturing of ceramics N2 - Most additive manufacturing (AM) techniques have in common that material is spread out as thin layers of a dried powder/granulate by a roller or a shaker system. These layers are mostly characterized by a low packing rate. On the other hand, appreciable densities can be reached by the use of ceramic slurries. In this context, the layer-wise slurry deposition (LSD) has been developed. Specific features of the LSD process are reflected on the basis of already existing additive manufacturing technologies. The microstructure of laser-sintered bodies will be discussed, and strategies for an improved microstructure during sintering will be introduced. KW - Additive manufacturing KW - Ceramic KW - Selective laser sintering PY - 2015 DO - https://doi.org/10.1111/ijac.12113 SN - 1546-542X SN - 1744-7402 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. VL - 12 IS - 1 SP - 18 EP - 25 PB - American Ceramic Soc. CY - Westerville, Ohio AN - OPUS4-29937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Colombo, P. A1 - Günster, Jens A1 - Mühler, T. A1 - Heinrich, J.G. T1 - Selective laser densification of lithium aluminosilicate glass ceramic tapes N2 - Tapes, cast by blade deposition of a lithium aluminosilicate glass slurry, were sintered using a YAG-fiber laser, with the aim of finding suitable parameters for an additive manufacturing process based on layer-wise slurry deposition and selective laser densification. The influence of the laser parameters (output power and scan velocity) on the sintering was evaluated, by scanning electron microscopy and by X-ray diffraction, on the basis of the quality of the processed layer. Well densified samples could be obtained only in a small window of values for the output power and the scan velocity. The measurement of the width of a set of single scanned lines allowed also to estimate the minimum resolution of the system along the layer plane. KW - Selective laser sintering (SLS) KW - Laserwise-slurry-deposition (LSD) KW - Glass-ceramic KW - LAS PY - 2013 UR - http://ac.els-cdn.com/S0169433212020168/1-s2.0-S0169433212020168-main.pdf?_tid=4ba0c92c-31d4-11e4-84f1-00000aab0f02&acdnat=1409575040_15d5256291262aca99cc5321374ab879 DO - https://doi.org/10.1016/j.apsusc.2012.11.058 SN - 0169-4332 SN - 1873-5584 VL - 265 SP - 610 EP - 614 PB - North-Holland CY - Amsterdam AN - OPUS4-31283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gonzales-Gago, C. A1 - Smid, P. A1 - Hofmann, T. A1 - Venzago, C. A1 - Hoffmann, V. A1 - Gruner, W. A1 - Pfeifer, Jens A1 - Richter, Silke A1 - Kipphardt, Heinrich T1 - Investigations of matrix independent calibration approaches in fast flow glow discharge mass spectrometry N2 - The performance of glow discharge mass spectrometry (GD-MS) is investigated for the accurate quantification of metallic impurities and oxygen in solid samples using the fast flow source GD-MS instrument ELEMENT GD. Different quantification approaches based on relative and absolute sensitivity factors are evaluated for the determination of metallic impurities using three sample matrixes (Al, Cu and Zn). The effect of the discharge conditions (voltage, current, discharge gas pressure/flow) on the sensitivity is investigated and the parameters are optimized to favour matrix independent calibrations. Improved standard relative sensitivity factors (StdRSFs) are calculated under optimal conditions based on multi-matrix calibrations. The sputtering rate corrected calibration is also presented as a multi-matrix calibration approach. The capabilities of GD-MS for oxygen determination are also investigated using a set of new conductive samples containing oxygen with mass fractions in the percent range in three different matrices (Al, Mg and Cu) produced by a sintering process. Poor limits of detection (in the order of g/kg) were obtained as consequence of the reduced sensitivity of oxygen in GD-MS and high oxygen background signal intensity as well as its variations. The absolute sensitivity procedure is shown as a matrix-independent approach, which provides quantitative values consistent with those obtained by carrier gas hot extraction (CGHE). KW - Fast flow GD KW - GDMS KW - Calibration KW - Matrix independent calibration PY - 2019 DO - https://doi.org/10.1039/c9ja00023b SN - 1364-5544 SN - 0267-9477 VL - 34 IS - 6 SP - 1109 EP - 1125 PB - Royal Society of Chemistry CY - London AN - OPUS4-47842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Hasan, T. A1 - Szczerba, Wojciech A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Kersten, M. T1 - Cr(VI)/Cr(III) and As(V)/As(III) ratio assessments in Jordanian spent oil shale produced by aerobic combustion and anaerobic pyrolysis N2 - With the increase in the awareness of the public in the environmental impact of oil shale utilization, it is of interest to reveal the mobility of potentially toxic trace elements in spent oil shale. Therefore, the Cr and As oxidation state in a representative Jordanian oil shale sample from the El-Lajjoun area were investigated upon different lab-scale furnace treatments. The anaerobic pyrolysis was performed in a retort flushed by nitrogen gas at temperatures in between 600 and 800 °C (pyrolytic oil shale, POS). The aerobic combustion was simply performed in porcelain cups heated in a muffle furnace for 4 h at temperatures in between 700 and 1000 °C (burned oil shale, BOS). The high loss-on-ignition in the BOS samples of up to 370 g kg–1 results from both calcium carbonate and organic carbon degradation. The LOI leads to enrichment in the Cr concentrations from 480 mg kg–1 in the original oil shale up to 675 mg kg–1 in the ≥850 °C BOS samples. Arsenic concentrations were not much elevated beyond that in the average shale standard (13 mg kg–1). Synchrotron-based X-ray absorption near-edge structure (XANES) analysis revealed that within the original oil shale the oxidation states of Cr and As were lower than after its aerobic combustion. Cr(VI) increased from 0% in the untreated or pyrolyzed oil shale up to 60% in the BOS ash combusted at 850 °C, while As(V) increased from 64% in the original oil shale up to 100% in the BOS ash at 700 °C. No Cr was released from original oil shale and POS products by the European compliance leaching test CEN/TC 292 EN 12457-1 (1:2 solid/water ratio, 24 h shaking), whereas leachates from BOS samples showed Cr release in the order of one mmol L–1. The leachable Cr content is dominated by chromate as revealed by catalytic adsorptive stripping voltammetry (CAdSV) which could cause harmful contamination of surface and groundwater in the semiarid environment of Jordan. KW - Trace-elements KW - Fly-ash KW - Speciation KW - Chromium KW - Sediments KW - Behavior KW - Metals KW - Xanes KW - Cr KW - Transformation PY - 2011 DO - https://doi.org/10.1021/es200695e SN - 0013-936X SN - 1520-5851 VL - 45 IS - 22 SP - 9799 EP - 9805 PB - ACS Publ. CY - Washington, DC AN - OPUS4-25290 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 - Ketelsen, T. A1 - Merchel, Silke A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Spatially resolved synchrotron-induced X-ray fluorescence analyses of metal point drawings and their mysterious inscriptions N2 - Synchrotron-induced X-ray fluorescence (Sy-XRF) analysis was used to study the chemical composition of precious Renaissance silverpoint drawings. Drawings by famous artists such as Albrecht Dürer (1471–1528) and Jan van Eyck (approximately 1395–1441) must be investigated non-destructively. Moreover, extremely sensitive synchrotron- or accelerator-based techniques are needed since only small quantities of silver are deposited on the paper. New criteria for attributing these works to a particular artist could be established based on the analysis of the chemical composition of the metal points used. We illustrate how analysis can give new art historical information by means of two case studies. Two particular drawings, one of Albrecht Dürer, showing a profile portrait of his closest friend, “Willibald Pirckheimer” (1503), and a second one attributed to Jan van Eyck, showing a “Portrait of an elderly man”, often named “Niccolò Albergati”, are the object of intense art historical controversy. Both drawings show inscriptions next to the figures. Analyses by Sy-XRF could reveal the same kind of silverpoint for the Pirckheimer portrait and its mysterious Greek inscription, contrary to the drawing by Van Eyck where at least three different metal points were applied. Two different types of silver marks were found in this portrait. Silver containing gold marks were detected in the inscriptions and over-subscriptions. This is the first evidence of the use of gold points for metal point drawings in the Middle Ages. KW - Sy-XRF analysis KW - Drawing KW - Metal point KW - Albrecht Dürer KW - Jan van Eyck KW - Renaissance PY - 2004 DO - https://doi.org/10.1016/j.sab.2004.07.023 SN - 0584-8547 SN - 0038-6987 VL - 59 IS - 10-11 SP - 1657 EP - 1662 PB - Elsevier CY - Amsterdam AN - OPUS4-4575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lahiri, D. A1 - Sharma, S.M. A1 - Verma, A.K. A1 - Vishwanadh, B. A1 - Dey, G.K. A1 - Schumacher, G. A1 - Scherb, T. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Banerjee, S. T1 - Investigation of short-range structural order in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 glasses, using X-ray absorption spectroscopy and ab initio molecular dynamics simulations N2 - Short-range order has been investigated in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 metallic glasses using X-ray absorption spectroscopy and ab initio molecular dynamics simulations. While both of these alloys are good glass formers, there is a difference in their glass-forming abilities (Zr41.5Ti41.5Ni17 > 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 - GEN A1 - Berger, Achim A1 - Calligaro, T. A1 - Duval, A. A1 - Görner, Wolf A1 - Guerra, M.-F. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Study of Ag and Au based historical and archaeological objects by high energy Sy-XRF KW - Synchrotron KW - XRF analysis KW - Drawings KW - Archaeometry KW - Gold KW - Röntgenfluoreszenzanalyse KW - RFA KW - Zeichnungen KW - Archäometrie KW - Albrecht Dürer KW - gold PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=544 SN - 0179-4159 SP - 544 EP - 546 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Calligaro, T. A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich T1 - Fingerprinting ancient gold by measuring Pt with spatially resolved high energy Sy-XRF N2 - Trace elements of ancient gold such as Pt, give fundamental information on the circulation of the metal in the past. In the case of objects from the cultural heritage, the determination of trace elements requires non-destructive point analysis in general. These conditions and the need of good detection limits restrain the number of applicable analytical techniques. After the development of a PIXE set-up with a selective Cu or Zn filter of 75 µm and of a PIXE-XRF set-up using a primary target of As, we tested the possibilities of spatially resolved Sy-XRF to determine Pt in gold alloys. With a Zn filter, PIXE showed a detection limit of 1000 ppm in gold while PIXE-XRF lowers this detection limit down to 80 ppm. This last value being constrained by the resonant Raman effect produced on gold. In order to improve the detection limit of Pt keeping the non-destructiveness and access to point analysis, we developed an analytical protocol for XRF with synchrotron radiation at BESSY II, using the BAMline set-up. The L-lines of Pt were excited by a beam of energy above and below 11.564 keV and measured using a Si(Li) detector with a 50 µm Cu filter. A µ-beam of 100–250 µm2 was used according to the size of the sample. The determination of the Pt content in the samples was carried out by Monte-Carlo simulation and subtraction of Au and Pt spectra obtained on pure standards. The limit of detection for Pt of 20 ppm was determined by using certified standards. The detection limits of a small set of other characteristic elements of gold were also measured using an incident energy of 33 keV. KW - PIXE-XRF KW - Sy-XRF KW - Pt KW - Ancient gold KW - Fingerprinting PY - 2005 DO - https://doi.org/10.1016/j.nimb.2005.06.150 SN - 0168-583X SN - 1872-9584 VL - 240 IS - 1-2 SP - 505 EP - 511 PB - Elsevier CY - Amsterdam AN - OPUS4-14236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nusser, K. A1 - Mosbauer, T. A1 - Schneider, G. J. A1 - Brandt, K. A1 - Weidemann, Gerd A1 - Goebbels, Jürgen A1 - Riesemeier, Heinrich A1 - Göritz, D. T1 - Silica dispersion in styrene butadiene rubber composites studied by synchrotron tomography N2 - By means of synchrotron X-ray computed tomography, model composites consisting of silica and styrene–butadiene rubber were studied with a very high spatial resolution. By our analysis technique we were able to determine the nano- and micro dispersion from the experimental results by our numerical analysis. These results are discussed with respect to crucial advantages of the generically 3-dimensional tomography technique as compared to 2-dimensional methods. Our quantitative analysis of the 3d images demonstrates that in the case of our model composites the filler dispersion is good, independent on the filler concentration. Our new 3-dimensional results evidence that considering only 2-d pictures may lead to ambiguities that can lead to wrong conclusions. KW - X-ray tomography KW - Silica KW - Styrene butadiene rubber KW - Dispersion PY - 2012 DO - https://doi.org/10.1016/j.jnoncrysol.2011.10.009 SN - 0022-3093 VL - 358 IS - 3 SP - 557 EP - 563 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-26105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, T. A1 - Heinrich, Sebastian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Reaction engineering investigations of the heterogeneously catalyzed partial oxidation of o-xylene in the explosion regime using a microfixed bed reactor N2 - The heterogeneously catalyzed selective gas phase oxidation of o-xylene was investigated, using a microstructured fixed bed reactor, inside of the explosion regime. The reaction was carried out with high amounts of o-xylene in air and stoichiometric with oxygen using a V2O5/TiO2-catalyst prepared through grafting. There were no significant losses in the selectivity to phthalic anhydride observable, during the measurements in the explosion regime, with feed compositions of up to 7 vol% o-xylene. Also the space-time yield was up to 2.3 times higher in comparison to conventional reaction conditions. An increase of the selectivity to total oxidation products was observed at higher o-xylene concentrations between 10 and 25 vol% o-xylene, which possibly was caused by the formation of a hotspot. The investigation of the used catalyst revealed a thermally induced deactivation due to phase transition of anatase into rutil and formation of crystalline vanadium oxide. Despite that expected hotspot at high oxylene concentrations, there was no ignition or explosion of the gas mixture observable. KW - O-xylene oxidation KW - Phthalic anhydride KW - V2O5/TiO2-catalyst KW - Microfixed bed reactor KW - Explosion regime KW - Hotspot PY - 2012 DO - https://doi.org/10.1016/j.ces.2011.10.072 SN - 0009-2509 VL - 69 IS - 1 SP - 440 EP - 448 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-25463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Sebastian A1 - Edeling, Florian A1 - Liebner, Christian A1 - Hieronymus, Hartmut A1 - Lange, T. A1 - Klemm, E. T1 - Catalyst as ignition source of an explosion inside a microreactor N2 - The present issue reports on a specific aspect of safety engineering of the heterogeneously catalysed oxidation of ethene in a continuous-flow microreactor. Conversion of ethene and the corresponding surface temperature of the catalyst were monitored for different reactor temperatures and total flow rates with a stoichiometric ethene/oxygen mixture for total oxidation. Safe operation of the highly exothermic oxidation was possible, but not in the whole parameter range. At high reactor temperatures and flow rates, ignition of an explosion inside the microreactor caused by a hot spot on the surface of the catalyst was observed for the first time. KW - Catalyst KW - Ethene KW - Explosions KW - Hot spot KW - Microstructure KW - Safety PY - 2012 DO - https://doi.org/10.1016/j.ces.2012.08.049 SN - 0009-2509 VL - 84 SP - 540 EP - 543 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-26782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liebner, Christian A1 - Fischer, J. A1 - Heinrich, Sebastian A1 - Lange, T. A1 - Hieronymus, Hartmut A1 - Klemm, E. T1 - Are micro reactors inherently safe? An investigation of gas phase explosion propagation limits on ethene mixtures N2 - A method for the determination of safety properties for micro reactors and micro structured components is presented. Micro structured reactors are not inherently safe but the range of safe operating conditions of micro reactors are extended since the explosion region is reduced. The λ/3 rule was demonstrated to be applicable to micro scale tubes for stoichiometric mixtures of ethane–oxygen and ethane–nitrous oxide. Furthermore first results from an investigation concerning detonation propagation through a micro reactor of non-ideal geometry are shown. Initial pressure investigated is ranging from low pressure up to 100 kPa. KW - Micro reactor KW - Explosion propagation limits KW - Chemical safety KW - Investigation method PY - 2012 DO - https://doi.org/10.1016/j.psep.2011.08.006 SN - 0957-5820 SN - 1744-3598 VL - 90 IS - 2 SP - 77 EP - 82 PB - Elsevier CY - Amsterdam AN - OPUS4-25594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, T.K. A1 - Kraus, Werner A1 - Pietzsch, H.-J. A1 - Smuda, C. A1 - Spies, H. T1 - Novel Rhenium Chelate System Derived from Dimercaptosuccinic Acid for the Selective Labeling of Biomolecules N2 - This work is part of an effort to develop chelating agents for stable binding and easy conjugation of Re-188 to biologically interesting structures. Starting from the well-known in vivo stability of [188ReO(DMSA)2]-, we want to exploit this coordination system for the design of 188ReO(V) chelates, which are stable toward reoxidation to perrhenate and toward ligand exchange under all conditions of radiopharmaceutical development. Therefore, a new type of tetradentate ligand has been synthesized by bridging two molecules of N,N'-diisobutyl-2,3-dimercaptosuccinamide with N-(3-aminopropyl)propane-1,3-diamine. The resulting stereoisomeric tetrathiolato S4 ligand of composition (iBu)2N(O)C-C(SH)-C(SH)-C(O)NH-(CH2)3-NH-(CH2)3-NHC(O)-C(SH)-C(SH)-C(O)N(iBu)2 forms anionic five-coordinate oxorhenium(V) complexes by a ligand-exchange reaction of NBu4[ReOCl4] in methanol. In the absence of a base, the compounds were isolated as "betaine", [ReO(S4)], with the protonated nitrogen of the bridge serving as an internal "counterion". Two representatives have been fully characterized in both the solid and solution states and found to adopt the expected square-pyramidal coordination geometry. The equatorial plane is formed by four thiolate sulfur atoms, whereas the oxygen occupies the apical position. The orientation of the metal oxo group is exo in relation to the carbamido groups in both isomers. Both complexes are stereoisomeric regarding the junction of the triamine chain. PY - 2005 DO - https://doi.org/10.1021/ic051148s SN - 0020-1669 SN - 1520-510X VL - 44 IS - 26 SP - 9930 EP - 9937 PB - American Chemical Society CY - Washington, DC AN - OPUS4-12507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -