TY - CONF A1 - Kipphardt, Heinrich T1 - Non-metal determination - a chalenge in elemental analysis T2 - CCQM IAWG workshop CY - Paris, France DA - 2011-04-13 PY - 2011 AN - OPUS4-23812 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich T1 - Special ways to achieve metrological traceability of results in GD-MS and in some other direct solid sampling methods T2 - CCQM IAWG workshop CY - Paris, France DA - 2011-04-13 PY - 2011 AN - OPUS4-23813 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich T1 - Advance in non-metal determination T2 - Institutskolloquium (CENAM) CY - Querétaro, Mexico DA - 2011-09-09 PY - 2011 AN - OPUS4-25955 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich T1 - Messtechnische Rückführung in der Elementanalytik T2 - 18.Kolloquium von EUROLAB-D, BAM CY - Berlin, Germany DA - 2012-05-04 PY - 2012 AN - OPUS4-26702 LA - deu 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 - JOUR A1 - Kipphardt, Heinrich A1 - Taylor, P. A1 - De Bièvre, P. T1 - The definition of primary method of measurement (PMM) of the 'highest metrological quality': a challenge in understanding and communication N2 - Problems with understanding, explaining and communication of the present definition of primary method of measurement are described and amendments put forward for discussion. The conclusion is drawn that in many cases more attention should be given to the measurement result and its uncertainty statement, rather than to a method. Some cases are discussed where methods might have a fundamental characteristic that other methods do not have, a condition for the epitheton ’primary'. KW - Primary method of measurement KW - PMM KW - Metrology KW - Uncertainty KW - Chemistry PY - 2001 DO - https://doi.org/10.1007/PL00010444 SN - 0949-1775 SN - 1432-0517 VL - 6 IS - 103 SP - 103 EP - 106 PB - Springer CY - Berlin AN - OPUS4-1099 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 - JOUR A1 - Kipphardt, Heinrich A1 - Dudzus, Thomas A1 - Meier, Klaus A1 - Recknagel, Sebastian A1 - Hedrich, Martina A1 - Matschat, Ralf T1 - Measurement of oxygen and nitrogen in high purity metals used as national standards for elemental analysis in Germany by classical carrier gas hot extraction (HE) and HE after activation with photons N2 - The special importance of the analysis of non-metals in high purity metals, which will serve as national standards for elemental analysis in Germany, is illustrated for oxygen and nitrogen. The typical range of the mass fraction of oxygen and nitrogen in these materials is below 10.MU.g/g, often close to 1.MU.g/g. The two methods applied at BAM for these measurements are classical carrier gas hot extraction (HE) and carrier gas hot extraction after activation with photons (PAA-HE). The approach, the methods and their advantages and limitations are discussed. Comparative results from the measurement of oxygen and nitrogen in Cu, Fe, Ga, Pb, Sn and W are presented. (author abst.) T2 - 8th International Conference on Ultra-High Purity Base Metals (UHPM-2001) CY - Berlin, Germany DA - 2001-06-25 KW - Oxygen determination KW - Nitrogen determination KW - High purity metals KW - Carrier gas hot extraction KW - Photon activation analysis PY - 2002 DO - https://doi.org/10.2320/matertrans.43.98 SN - 1345-9678 SN - 1347-5320 VL - 43 IS - 2 SP - 98 EP - 100 PB - Japan Institute of Metals CY - Sendai AN - OPUS4-1361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Russe, K. A1 - Bréas, O. A1 - Taylor, P.D.P. T1 - Conversion of Carbon into CF4 for SI-Traceable Measurements of Absolute Carbon Isotope Amount Ratios: A Feasibility Study N2 - The feasibility of performing SI-traceable carbon isotope amount ratio measurements following conversion of carbon into CF4 was studied. A procedure for the direct fluorination of carbon with elemental fluorine was developed, and the conversion step was checked for losses, blank contributions, and the absence of systematic isotope effects. Gas chromatography was used to identify and quantify the gaseous fluorination products and to isolate CF4 from byproducts. After fluorination of graphite carbon, CF4 and perfluoroalkanes with up to six carbon atoms were observed as reaction products. Within an uncertainty of 10%, the graphite carbon was fully recovered in the gaseous carbon fluorides, with the main product being CF4 (80-90%) and C2F6 as the major byproduct. The fluorination and GC procedures were found to introduce an alteration not bigger than 0.03 ± 0.04” on the isotopic composition of CF4. Carbon blank contributions introduced during the fluorination procedure were below 0.5% relative to a typical sample of 4 mg of carbon. For two of the materials investigated, the carbon isotope ratios measured on a differential mass spectrometer were reproducible within a standard deviation of ~0.1” for several individual fluorinations. For these materials, the developed fluorination procedure is a straightforward process, which can be used as a foundation to establish SI-traceable measurements of carbon isotope amount ratios. However, for the third graphite material the formation of byproducts (C2F6-C6F14) was found to induce significant isotopic fractionation. PY - 2002 DO - https://doi.org/10.1021/ac015700g SN - 0003-2700 SN - 1520-6882 VL - 74 SP - 3199 EP - 3205 PB - American Chemical Society CY - Washington, DC AN - OPUS4-1408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Kuxenko, Sandra A1 - Matschat, Ralf T1 - Auf dem Weg zu rückführbaren Standards für die Elementanalytik - Element-Spurenanalyse in Reinstkupfer KW - Reinstkupfer KW - Elementspurenanalytik KW - Standards KW - Rückführbarkeit PY - 2002 SN - 0016-3538 IS - 6 SP - 718 EP - 720 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-1452 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -