TY - JOUR A1 - Rudtsch, S. A1 - Fahr, M. A1 - Fischer, J. A1 - Gusarova, Tamara A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - High-Purity Fixed Points of the ITS-90 with Traceable Analysis of Impurity Contents N2 - The International Temperature Scale of 1990 (ITS-90) is based on thermodynamic equilibrium states of ideally pure substances. The largest contribution to the uncertainty budgets of most metallic fixed points is the influence of impurities on the fixed-point temperature. Therefore, a traceable chemical analysis of the remaining impurities with small uncertainty is the basis of further progress. Further requirements are better knowledge of the phase diagrams at very low impurity contents, impurity segregation, and the quantification and correction of thermal effects during a fixed-point realization. In this article, current and future activities at PTB and BAM in order to develop improved metallic fixed-point cells of the ITS-90 are reviewed. KW - Chemical analysis KW - Fixed points KW - Impurities KW - ITS-90 KW - Phase diagrams KW - Thermal effects PY - 2008 DO - https://doi.org/10.1007/s10765-007-0358-9 SN - 0195-928X SN - 1572-9567 VL - 29 IS - 1 SP - 139 EP - 150 PB - Springer CY - Dordrecht AN - OPUS4-17455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Vogl, Jochen A1 - Gusarova, Tamara A1 - Czerwensky, Michael A1 - Heinrich, Hans-Joachim A1 - Hioki, A. A1 - Konopelko, L.A. A1 - Methven, B. A1 - Miura, T. A1 - Petersen, O. A1 - Riebe, Gundel A1 - Sturgeon, R. A1 - Turk, G.C. A1 - Yu, L. L. T1 - Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability N2 - Within the National Metrology Institutes (NMIs) and designated laboratories, an interlaboratory comparison, CCQM-P107, was conducted to verify the degree of international comparability concerning the results of purity analysis. The mass fractions of Ag, Bi, Cd, Cr, Ni, Tl at the lower mg/kg-level in a high purity zinc material were determined, but the real measurand in metrological sense was the sum of the six mass fractions. Homogeneity was investigated by glow discharge mass spectrometry, reference values were obtained using isotope dilution mass spectrometry. Six NMIs participated, contributing eight independent data sets. The agreement amongst the results of the participants, their median and the agreement with the reference values were usually excellent and in almost all cases below the target uncertainty of 30% relative. In this manner, the accuracy of results and the comparability between the participants was demonstrated to be established. KW - Interlaboratory comparison KW - Purity analysis KW - High purity metals KW - CCQM-P107 KW - Zinc PY - 2010 DO - https://doi.org/10.1007/s00769-009-0557-0 SN - 0949-1775 SN - 1432-0517 VL - 15 IS - 1 SP - 29 EP - 37 PB - Springer CY - Berlin AN - OPUS4-20767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gusarova, Tamara A1 - Lange, Britta A1 - Kipphardt, Heinrich A1 - Venzago, C. A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - GD-MS: calibration for VG9000 and Element GD - Do RSF- and StRSF-concepts always work? T2 - EuroAnalysis XIV CY - Antwerp, Belgium DA - 2007-09-09 PY - 2007 AN - OPUS4-14800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gusarova, Tamara A1 - Hodoroaba, Vasile-Dan A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Panne, Ulrich T1 - Exploitation of the hollow cathode effect for sensitivity enhancement of Grimm-type DC glow discharge optical emission spectroscopy N2 - The hollow cathode (HC) effect was investigated in non-cooled 15 mm deep drilled flat metallic analytical samples that were easy to prepare. The deep cavity used ("complete HC" in contrast to "recessed HC" with 2-3 mm deep cavity) intensified the HC effect notably and therefore distinctly improved the detection power of the common GD-OES with planar cathodes. A signal enhancement of up to a factor of 150, not reported earlier, in comparison with flat conventional samples was achieved. A better separation of the analytical lines from spectral interferences was observed when the HC assembly was applied. Additionally, an effect of strongly enhanced intensities of atomic lines and somewhat decreased intensities of ionic lines was detected in the case of HC in comparison to usual planar cathodes. The investigations were carried out with samples of copper, steel and zinc matrices using both the same and individually optimised glow discharge (GD) electrical parameters. KW - Hollow cathode KW - Grimm type glow discharge KW - Emission spectroscopy KW - GD-OES KW - Sensitivity PY - 2009 DO - https://doi.org/10.1039/b814977a SN - 0267-9477 SN - 1364-5544 VL - 24 SP - 680 EP - 684 PB - Royal Society of Chemistry CY - London AN - OPUS4-19600 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 - CONF A1 - Gusarova, Tamara A1 - Lange, Britta A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Comparison of different quantification procedures in glow discharge mass spectrometry applied to high-purity metals T2 - 2007 European Winter Conference on Plasma Spectrochemistry CY - Taormina, Italy DA - 2007-02-18 PY - 2007 AN - OPUS4-13680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gusarova, Tamara A1 - Lange, Britta A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Analysis of high purity zinc by glow discharge mass spectrometry for use in thermometry T2 - 13th International Conference on ultra high-purity base metals CY - Berlin, Germany DA - 2006-09-11 PY - 2006 AN - OPUS4-13485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gusarova, Tamara A1 - Zayed, Mahamed Mokhtar A1 - Hodoroaba, Vasile-Dan A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Improvement of signal sensitivity using hollow cathode effect in glow discharge optical emission spectroscopy T2 - 13. GDS-Anwendertreffen CY - Hanau, Germany DA - 2006-09-04 PY - 2006 AN - OPUS4-13483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gusarova, Tamara A1 - Lange, Britta A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Analysis of high purity zinc by glow discharge mass spectrometry for use in thermometry T2 - Euromet Workshop -732 / LNE - INM CY - Paris, France DA - 2006-11-23 PY - 2006 AN - OPUS4-13497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gusarova, Tamara A1 - Hodoroaba, Vasile-Dan A1 - Matschat, Ralf A1 - Panne, Ulrich T1 - Enhancement of signal sensitivity in glow discharge optical emission spectroscopy by use of the hollow cathode effect for the analysis of pure metals T2 - 2007 European Winter Conference on Plasma Spectrochemistry CY - Taormina, Italy DA - 2007-02-18 PY - 2007 AN - OPUS4-14639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -