TY - JOUR A1 - Kipphardt, Heinrich A1 - Russe, K. A1 - Broekaert, J.A.C. T1 - Determination of main and minor components of silicon based materials by a combustion with elemental fluorine. Separation of gaseous fluorination products by carrier gas distillation and gas mass spectrometry N2 - For the determination of main and minor components in silicon-based ceramic powders, a decomposition by a combustion with elemental fluorine and separation of the volatile fluorination products by a carrier-gas distillation with a subsequent detection by quadrupole mass spectrometry is described. The necessity and success of the separation step is demonstrated for the determination of boron as a minor constituent in SiC, where the spectral interferences of silicon on the boron signals are decreased considerably. The method developed is shown to be directly applicable to determination of silicon in Si3N4, SiC, and SiO2. The determination of nitrogen in Si3N4 requires additional effort, to separate nitrogen from the excess of fluorine. For the determination of boron, a complete mobilization of BF3 is assured by the presence of an adequate amount of GeF4. Analysis results obtained with different types of calibration show a precision of 30 g for boron at the milligram-per-gram level and a precision between 0.5 and 2% (m/m) for the main components, silicon and nitrogen. Within these standard deviations, the results agree well with the values expected from the stoichiometry, with the results for silicon and boron obtained by wet chemical decomposition and slurry techniques in combination with ICP-OES and with the results for nitrogen obtained by carrier gas heat extraction. PY - 2000 DO - https://doi.org/10.1021/ac991238c SN - 0003-2700 SN - 1520-6882 VL - 72 IS - 16 SP - 3875 EP - 3880 PB - American Chemical Society CY - Washington, DC AN - OPUS4-989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Aregbe, Y. A1 - Valkiers, S. A1 - Norgaard, J. A1 - De Bièvre, P. A1 - Taylor, P.D.P. A1 - Poths, J. T1 - A primary isotopic gas standard for krypton with values for isotopic composition and molar mass traceable to the Système International d'Unités N2 - Isotope amount ratios of krypton were measured on subsamples from one large batch of high purity krypton separated from the atmosphere. Synthetic mixtures of enriched krypton isotopes were used to “calibrate” the measurements with small uncertainties. The result is a primary isotopic gas standard (PIGS) IRMM-2030 with certified values for isotope ratios, isotopic composition, and molar mass of krypton with small combined uncertainties uc, evaluated according to the ISO/BIPM Guide (GUM). It is commercially available from IRMM-Geel or from MESSER (Duisburg, D). The certified krypton isotope amount ratios in the PIGS IRMM-2030 are as follows: n(78Kr)/n(84Kr)=0.006 232 5(55), n(80Kr)/n(84Kr)=0.040 107(17), n(82Kr)/n(84Kr)=0.203 43(12), n(83Kr)/n(84Kr)=0.201 79(11), and n(86Kr)/n(84Kr)=0.303 205(59) with expanded uncertainty U=kuc and coverage factor k=2. The molar mass of Kr in this sample is M(Kr)=83.798 02(16) g/mol. These values are in good agreement with published measurements of atmospheric krypton but have smaller combined uncertainties and are “calibrated” by means of synthetic isotope mixtures. The values of the PIGS are traceable to the SI. Measurements of isotope amount ratios of krypton in other samples can be linked to SI using this PIGS. KW - Molar mass KW - Isotopic composition KW - Primary isotopic gas standard KW - Gas isotope mass spectrometry KW - Isotope amount ratio KW - Traceability KW - SI KW - Krypton PY - 2001 DO - https://doi.org/10.1016/S1387-3806(00)00397-3 SN - 0168-1176 SN - 0020-7381 SN - 1387-3806 SN - 1873-2798 VL - 206 SP - 129 EP - 136 PB - Elsevier CY - Amsterdam AN - OPUS4-1087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Merchel, Silke A1 - Berger, Achim A1 - Görner, Wolf A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reiche, I. A1 - Riederer, J. A1 - Duval, A. A1 - Guicharnaud, H. T1 - Non-Destructive Investigations of Dürer's Silver Point Drawings by Pixe and SY-XRF T2 - 7th International Conference on Non-destructive testing and Microanalysis for the Diagnostics and Conservation of the Cultural and Environmental Heritage ; art 2002 CY - Antwerp, Belgium DA - 2002-06-02 PY - 2002 UR - http://srs.dl.ac.uk/arch/publications/reiche/reiche_fullcorr.pdf SP - 82 AN - OPUS4-1400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reiche, I. A1 - Riederer, J. T1 - Non-destructive investigations of Dürer's silver point drawings by Sy-XRF PY - 2002 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2001.pdf#page=292 SN - 0179-4159 SP - 292 EP - 293 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-1324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reiche, I. A1 - Riederer, J. T1 - A closer look at Albrecht Dürer's drawings (1471-1528) PY - 2002 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/infos/bessy/highlights2001.pdf#page=32 SN - 0179-4159 SP - 32 EP - 33 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-1323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Berger, Achim A1 - Buck, St. A1 - Görner, Wolf A1 - Ketelsen, Th. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich T1 - BAMline meets Dürer and van Eyck - Multi-disciplinary investigation of Renaissance silver point drawings by µ-SR-XRF N2 - - http://www.bessy.de/publications/05.annual_reports/files/AnnualReport2002.pdf - PY - 2003 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2002.pdf#page=416 SN - 0179-4159 SP - 416 EP - 418 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-2496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Reiche, I. A1 - Berger, Achim A1 - Merchel, Silke A1 - Riesemeier, Heinrich A1 - Görner, Wolf A1 - Riederer, J. A1 - Roth, M. ED - Simionovici, A. T1 - BAMline meets Dürer and Van Eyck - Spatially resolved SR-XRF analyses of silver point drawings and their mysterious inscriptions T2 - 17th International Conference on X-Ray Optics and Microanalysis ; 17th ICXOM CY - Chamonix, France DA - 2003-09-22 PY - 2003 N1 - Serientitel: Spectrochimica acta : Part B, Atomic spectroscopy – Series title: Spectrochimica acta : Part B, Atomic spectroscopy IS - 59.2004,10/11 SP - 48 PB - Elsevier CY - Amsterdam AN - OPUS4-2690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Haibel, A. A1 - Rack, A. A1 - Weidemann, Gerd A1 - Riesemeier, Heinrich A1 - Goebbels, Jürgen A1 - Banhart, J. T1 - Investigation of pore formation in metallic foams by synchrotron computed tomography PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=324 SN - 0179-4159 SP - 324 EP - 325 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Haibel, A. A1 - Rack, A. A1 - Bütow, A. A1 - Kropf, H. A1 - Helwig, H.-M. A1 - Banhart, J. A1 - Weidemann, Gerd A1 - Riesemeier, Heinrich A1 - Goebbels, Jürgen T1 - Synchrotron-µ-tomography on complex materials PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=326 SN - 0179-4159 SP - 326 EP - 328 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3511 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 -