TY - JOUR A1 - Matschat, Ralf A1 - Heinrich, Hans-Joachim A1 - Czerwensky, Michael A1 - Kuxenko, Sandra A1 - Kipphardt, Heinrich T1 - Multielement trace determination in high purity advanced ceramics and high purity metals JF - Bulletin of materials science T2 - International Symposium on Ultrapure Materials (ISUPM) CY - Hyderabad, India DA - 2004-11-22 KW - Advanced ceramics KW - Pure metals KW - SS ET AAS KW - HR ICP-MS PY - 2005 SN - 0250-4707 SN - 0973-7669 VL - 28 IS - 4 SP - 361 EP - 366 PB - Indian Academy of Sciences CY - Bangalore AN - OPUS4-10889 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 JF - Accreditation and quality assurance 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 - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - Development of SI-traceable standards of high metrological quality for chemical analysis of the elements JF - Analytical and bioanalytical chemistry T2 - 12th Euroanalysis ; 12th European Conference on Analytical Chemistry CY - Dortmund, Germany DA - 2002-09-08 PY - 2002 SN - 1618-2642 SN - 1618-2650 VL - 375 IS - 8, P1-018 SP - 198 PB - Springer CY - Berlin AN - OPUS4-1630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Schiel, D. A1 - Rienitz, O. T1 - Primäre Kalibriermaterialien für die Elementanalytik JF - Nachrichten aus der Chemie PY - 2003 DO - https://doi.org/10.1002/nadc.20030510714 SN - 1439-9598 SN - 1521-3854 VL - 51 IS - 7/8 SP - 827 EP - 829 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-2582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Czerwensky, Michael A1 - Matschat, Ralf T1 - ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality JF - Journal of analytical atomic spectrometry N2 - The need, concept and technical approach for the certification of SI-traceable standards of high metrological quality for chemical analysis of the elements is briefly explained. As an example of problems occurring in the certification of these standards, special technical aspects related to the analysis of high purity Mo by ICP-MS, namely blank reduction for Na, Li and Ni by protective coating of the cones with silicon, as well as dealing with the interferences from the Mo matrix, are discussed. PY - 2005 UR - http://cat.inist.fr/?aModele=afficheN&cpsidt=16469686 SN - 0267-9477 SN - 1364-5544 VL - 20 IS - 1 SP - 28 EP - 34 PB - Royal Society of Chemistry CY - London AN - OPUS4-5483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 JF - International Journal of Thermophysics 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 - Matschat, Ralf A1 - Hinrichs, J. A1 - Kipphardt, Heinrich T1 - Application of glow discharge mass spectrometry to multielement ultra-trace determination in ultrahigh-purity copper and iron: a calibration approach achieving quantification and traceability JF - Analytical and bioanalytical chemistry N2 - A new approach was developed for quantitative calibration in GD-MS which can afford reliable and metrologically traceable results for many trace elements and was exemplified for pure copper and pure iron. It can be assumed that the technique can be further improved and applied to the analysis of other pure metals. Pressed copper and iron powder samples were used to calibrate the glow discharge mass spectrometry applied to the analysis of pure copper and iron. The new type of glow discharge mass spectrometer—the Element GD (Thermo Electron Corporation)—was used with a Grimm-type discharge cell for flat samples. Two series of powder samples were prepared for each of the copper and iron matrixes. The powders were quantitatively doped with solutions of graduated and defined concentrations of 40 or 20 analytes, respectively. The mass fractions of the analytes in the dried and homogenized metal powder samples ranged from µg/kg levels up to 10 mg/kg levels. A special technique was developed to press the samples and to form mechanically stable pellets with low risk of contamination. Ion beam ratios of analyte ions to matrix ions were used as measurands. The calibration curves were determined and the linear correlation coefficients were calculated for different intervals of the curves. The linear correlation coefficients are very satisfactory for most of the calibration curves, which include the higher segments of mass fractions; however, they are less satisfactory for the lower segments of the calibration curves. Nevertheless, in many cases rather acceptable and rather promising values were achieved even for these lower segments, representing mass fractions of analytes at ultra-trace level. The comparison of the certified values of different reference materials with the measured values based on calibrations with the pressed powder samples led to deviations less than 30% for most of the considered examples. KW - Glow discharge mass spectrometry (GD-MS) KW - High-purity copper KW - High-purity iron KW - Doped and pressed metal powder samples KW - Grimm-type cell KW - Metrological traceability PY - 2006 DO - https://doi.org/10.1007/s00216-006-0645-5 SN - 1618-2642 SN - 1618-2650 VL - 386 IS - 1 SP - 125 EP - 141 PB - Springer CY - Berlin AN - OPUS4-12649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf T1 - Purity assessment for providing primary standards for elemental determination - a snap shot of international comparability JF - Microchimica acta N2 - An inter-laboratory study was performed by some National Metrology Institutes in order to take a snap shot of the comparability and the capability of performing purity assessments of high purity materials as needed for providing national standards for elemental determination. The measurand was defined as the value of the sum of the mass fractions of Ag, Al, Cu, Fe, Pb and Zn in the bulk of a high purity nickel material and the interim results for the six individual impurities. Whereas for the analytes Ag, Al, Cu and Fe there was no agreement within the target uncertainty of 30%, agreement could be achieved for Pb and Zn. The discrepancies observed for the individual analytes resulted in a variation of a factor of 8 of the reported values for the impurity of nickel with respect to the six defined metallic analytes. The reference measurements using IDMS and for Al using GD-MS confirmed the lower reported values. KW - Primary standards KW - Elemental determination KW - Inter laboratory comparison KW - Metrology KW - Purity assessment KW - Comparability PY - 2008 DO - https://doi.org/10.1007/s00604-007-0937-2 SN - 0026-3672 SN - 1436-5073 VL - 162 IS - 1-2 SP - 269 EP - 275 PB - Springer CY - Wien AN - OPUS4-17725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Czerwensky, Michael A1 - Matschat, Ralf T1 - Use of microwave induced plasma spectrometry as detector for the determination of O, N and H traces after carrier gas hot extraction JF - Journal of analytical atomic spectrometry N2 - The determination of O, N and H using a microwave induced plasma coupled to carrier gas hot extraction was exploratory investigated. The signal intensities versus time of blanks and calibration materials were recorded. To check for interferences the signal intensities versus wavelength were recorded at the times just before increase and at the maximum of the time dependent analytical signal. O, N and H were investigated at their prominent wavelengths of 777 nm, 174 nm and 486 nm, respectively. Calibration was performed for O, N and H in the ranges of 0–27 µg, 35–1000 µg and 3–43 µg respectively. For concentration values in the middle of the linear part of the investigated calibration interval, a relative precision of 5% at 13 µg, 2% at 74 µg and 0.6% at 23 µg for O, N and H respectively was found. The maximum matrix load to the plasma used was found to be 150 µg min-1. From the signal to noise ratio and the sensitivity obtained, instrumental limits of detection (3s) of 0.01 µg for O, 1 µg for N and 0.1 µg for H were found. Assuming a typical sample mass of 1 g this corresponds to relative LODs of 0.01 µg g-1, 1 µg g-1 and 0.1 µg g-1 for O, N and H respectively. KW - Non-metal determination KW - Microwave induced plasma spectrometry KW - Carrier gas hot extraction PY - 2008 DO - https://doi.org/10.1039/B714734a SN - 0267-9477 SN - 1364-5544 VL - 23 IS - 4 SP - 588 EP - 591 PB - Royal Society of Chemistry CY - London AN - OPUS4-17359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Rienitz, O. A1 - Schiel, D. A1 - Gernand, W. A1 - Oeter, D. T1 - Traceability system for elemental analysis JF - Accreditation and quality assurance N2 - A complete metrological traceability system for measurement results of chemical analysis was set up. Core components are pure substances (national standards) characterised at the highest metrological level, primary solutions prepared from these pure substances and secondary solutions deduced from the primary solutions and intended for sale. The relative uncertainty of the element mass fraction of the primary substances and solutions is < 0.01 and < 0.05%, respectively. For the certification of transfer solutions and for stability testing, a precision measurement method for element contents has been developed by means of optical emission spectrometry (ICP OES) by which uncertainties between 0.1 and 0.05% can be achieved. The dissemination to field laboratories is effected with the aid of a calibration laboratory of the German Calibration Service (DKD) which certifies the element content of the secondary solutions with an uncertainty <= 0.3%. Calibration with these solutions enables the user to establish traceability of his measurement results to the International System of Units (SI). Currently, the system comprises Cu, Fe, Bi, Ga, Si, Na, K, Sn, W, and Pb. KW - Elemental analysis KW - Traceability KW - Elemental calibration solutions KW - Pure substances KW - Precision measurement of elements PY - 2006 DO - https://doi.org/10.1007/s00769-005-0084-6 SN - 0949-1775 SN - 1432-0517 VL - 10 IS - 11 SP - 633 EP - 639 PB - Springer CY - Berlin AN - OPUS4-12199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -