Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-912 Zeitschriftenartikel Kipphardt, Heinrich; Valkiers, S.; Taylor, P.D.P.; De Bièvre, P. Calibration in isotopic measurements The meaning of calibration in general and in the field of isotopic measurements in particular is described, stressing the fundamental difference between calibration as an aim and tools to achieve calibration. The role of proper uncertainty budgeting as a prerequisite for establishing a “calibrated” measurement is explained. It leads to the recommendation that the quality of the uncertainty statement should be heavily weighed when ranking or judging “calibrated” isotopic measurement results evaluated by the Commission on Atomic Weight and Isotopic Abundances. Amsterdam Elsevier 2000 International Journal of Mass Spectrometry 198 1-2 71 76 10.1016/S1387-3806(00)00162-7 2016-02-19 OPUS4-913 Zeitschriftenartikel Kipphardt, Heinrich; Ding, T.; Valkiers, S.; Quetel, C.; De Bièvre, P.; Taylor, P.; Gonfiantini, R. Preparation of two synthetic isotope mixtures for the calibration of isotope amount ratio measurements of sulfur 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. Amsterdam Elsevier 2000 International Journal of Mass Spectrometry 197 1-3 131 137 10.1016/S1387-3806(99)00235-3 2016-02-19 OPUS4-914 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Ruße, K.; Bréas, O.; Valkiers, S.; Taylor, P. Fluorination of organic materials into CF4 for the measurements of carbon isotope ratios European Society for Isotope Research 2000 V Isotope Workshop V Isotope Workshop Krakow, Poland 2000-07-01 2000-07-06 poster P1-1 2016-02-19 OPUS4-915 Beitrag zu einem Sammelband Matschat, Ralf; Dudzus, Thomas; Meier, Klaus; Recknagel, Sebastian; Kipphardt, Heinrich; Hedrich, Martina Hirschfeld, D. Messung von Sauerstoff und Stickstoff mit klassischer Trägergasheißextraktion und Trägergasheißextraktion nach Aktivierung mit Photonen für die nationalen primären Kalibriernormale Clausthal-Zellerfeld GDMB, Ges. für Bergbau, Metallurgie, Rohstoff- und Umwelttechnik 2000 Nichtmetalle in Metallen 2000 3-9806913-1-4 8. Symposium Nichtmetalle in Metallen - NIM ; 8. Tagung des Gemeinschaftsausschusses "Nichtmetalle in Metallen" der GDMB Münster, Deutschland 2000-03-16 2000-03-17 19 27 2016-02-19 OPUS4-916 Beitrag zu einem Tagungsband Kipphardt, Heinrich; De Bièvre, P. How to establish traceability in chemical measurements and reference materials? EUROLAB 2000 Symposium "Reference Materials for Technologies in the New Millenium" Symposium "Reference Materials for Technologies in the New Millenium" Berlin, BAM, Germany 2000-05-22 2000-05-23 1(?) 7(?) 2016-02-19 OPUS4-3701 Vortrag Kipphardt, Heinrich Erfahrungen bei der Messung von Kohlenstoff in Siliciumcarbid - was geht, was geht nicht? 2003 Diskussionstreffen zu aktuellen Problemen und Entwicklungen in der Nichtmetall-/Gasanalytik Diskussionstreffen zu aktuellen Problemen und Entwicklungen in der Nichtmetall-/Gasanalytik Rathen, Germany 2003-10-01 2016-02-19 OPUS4-3702 Vortrag Kipphardt, Heinrich Verwendung und Herstellung von zertifizierten Referenzmaterialien für die anorganische Materialanalytik 2003 Universität Hamburg Universität Hamburg Hamburg, Germany 2003-12-01 2016-02-19 OPUS4-1452 Zeitschriftenartikel Kipphardt, Heinrich; Kuxenko, Sandra; Matschat, Ralf Auf dem Weg zu rückführbaren Standards für die Elementanalytik - Element-Spurenanalyse in Reinstkupfer Darmstadt GIT-Verlag 2002 GIT : Labor-Fachzeitschrift 6 718 720 2016-02-19 OPUS4-2934 Vortrag Kipphardt, Heinrich Provision of promary reference materials for calibretion ; method development for trace analysis 2002 CENAM Institutsseminar CENAM Institutsseminar Querétaro, Mexico 2002-01-30 2016-02-19 OPUS4-2935 Vortrag Kipphardt, Heinrich Measurment of oxygen and nitrogen in high purity metals by carrier gas hot extraction (HE) and HE after activation with photons 2002 CENAM Institutsseminar CENAM Institutsseminar Querétaro, Mexico 2002-02-01 2016-02-19 OPUS4-2936 Vortrag Kipphardt, Heinrich What is BAM? 2002 CENAM Institutsseminar CENAM Institutsseminar Querétaro, Mexico 2002-01-29 2016-02-19 OPUS4-989 Zeitschriftenartikel Kipphardt, Heinrich; Russe, K.; Broekaert, J.A.C. 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 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. Washington, DC American Chemical Society 2000 Analytical chemistry 72 16 3875 3880 10.1021/ac991238c 2016-02-19 OPUS4-990 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Valkiers, S.; Aregbe, Y.; Bréas, O.; Taylor, P.; Ding, T. Gills, T. Gravimetrically Prepared Isotope Mixtures to Produce Isotopic Reference Materials for Sulfur with SI Traceable Ratios Berlin Springer 2001 Biological and environmental reference materials (Fresenius' journal of analytical chemistry 370,2/3) 370 8th International Symposium on Biological and Environmental Reference Materials ; 8th BERM Bethesda, MD, USA 2000-09-17 2000-09-22 2-3 141 2016-02-19 OPUS4-1629 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Recknagel, Sebastian Measurement of Nitrogen in Steel by Carrier Gas Hot Extraction - a Challenge in Calibration 2002 6th International Workshop on progress in analytical chemistry in the steel and metals industries 6th International Workshop on progress in analytical chemistry in the steel and metals industries Luxembourg, Luxembourg 2002-05-14 2002-05-16 1(?) 2016-02-19 OPUS4-1630 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf Development of SI-traceable standards of high metrological quality for chemical analysis of the elements Berlin Springer 2002 Analytical and bioanalytical chemistry 375 12th Euroanalysis ; 12th European Conference on Analytical Chemistry Dortmund, Germany 2002-09-08 2002-09-13 8, P1-018 198 2016-02-19 OPUS4-1631 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Matschat, Ralf Development of SI-traceable standards of high metrological quality for chemical analysis of the elements 2002 Towards an integrated infrastructure for measurements Towards an integrated infrastructure for measurements Warszawa, Poland 2002-06-18 2002-06-19 66 67 2016-02-19 OPUS4-2024 Beitrag zu einem Tagungsband Merchel, Silke; Dudzus, Thomas; Ecker, Klaus; Hedrich, Martina; Kipphardt, Heinrich; Recknagel, Sebastian Viele (BAM-) Wege führen zu den leichten Elementen Interessengemeinschaft Atomspektroskopie Berlin 2002 12. Jahreskolloquium "Analyse von Feststoffen unterschiedlicher Materialien aus Industrie und Umwelt" 12. Jahrescolloquium "Analyse von Feststoffen unterschiedlicher Materialien aus Industrie und Umwelt" Berlin, Deutschland 2002-11-19 1(?) 2016-02-19 OPUS4-2028 Zeitschriftenartikel Kipphardt, Heinrich Establishing traceability to SI for elemental analysis: reporting from a difficult but worthwhile journey Weinheim Wiley-VCH Verl. 2002 Spectroscopy Europe 14 6 27 28 2016-02-19 OPUS4-2582 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Schiel, D.; Rienitz, O. Primäre Kalibriermaterialien für die Elementanalytik Weinheim Wiley-VCH Verl. Gesellschaft Deutscher Chemiker 2003 Nachrichten aus der Chemie 51 7/8 827 829 10.1002/nadc.20030510714 2016-02-19 OPUS4-3062 Zeitschriftenartikel Kipphardt, Heinrich; De Bièvre, P.; Taylor, P.D.P. New mathematical models with associated equations for isotope dilution mass spectrometry (IDMS) Vector models which progressively lead to a general model for isotope dilution mass spectrometry (IDMS) are presented for the case of two lsquomonitor isotopesrsquo and one blend involved. They enable one to find the boundary conditions for performing IDMS, and cover the cases of highly enriched isotopes, radioactive isotopes and ratios that are given with different denominator. The models identify the key measurements in their simplest form as well as the conditions which minimise the measurement effort and in some cases the propagated measurement uncertainties. The equations are discussed and compared with other published IDMS equations. Combined with discussion on fundamental aspects of IDMS, this results in an even more lsquogeneralrsquo but also more complex IDMS equation. Berlin Springer 2004 Analytical and bioanalytical chemistry 378 2 330 341 10.1007/s00216-003-2232-3 2016-02-19 OPUS4-1601 Beitrag zu einem Tagungsband Matschat, Ralf; Kipphardt, Heinrich; Czerwensky, Michael; Richter, Silke; Heinrich, Hans-Joachim Abiko, K.; Takaki, S. The System of Primary Pure Metals Established at BAM - Recent Developments Sendai Tohoku University, Japan 2002 Proceedings of the 9th international conference on ultrahigh-purity base metals 9th international conference on ultrahigh-purity base metals Sendai, Japan 2002-10-14 2002-10-16 119 2016-02-19 OPUS4-1602 Beitrag zu einem Tagungsband Matschat, Ralf; Kipphardt, Heinrich; Recknagel, Sebastian; Noack, Siegfried Abiko, K.; Takaki, S. Activities of Division "Inorganic Chemical Analysis; Reference Materials" of BAM in the Field of Analysis of Metals Sendai Tohoku University, Japan 2002 Proceedings of the 9th international conference on ultrahigh-purity base metals 9th international conference on ultrahigh-purity base metals Sendai, Japan 2002-10-14 2002-10-16 297 302 2016-02-19 OPUS4-1603 Beitrag zu einem Tagungsband Matschat, Ralf; Kipphardt, Heinrich BAM System of Primary Pure Elements - Aim and Current State 2002 CCQM Annual Meeting of Inorganic Working Group CCQM Annual Meeting of Inorganic Working Group Ottawa, Canada 2002-10-09 2002-10-11 2016-02-19 OPUS4-1606 Forschungsbericht Meier, Klaus; Wäthen, U.; Kipphardt, Heinrich; Lamberty, A.; Robouch, P. The certification of the mass fraction of Cd, Cu, Fe, Pb, Sn and TI in four grades of unalloyed zinc intended for use in emission spectrometry - BCR-322R, BCR-323R, BCR-324R, BCR-325R, Project Report EUR 20267 EN Luxembourg Office for Official Publications of the European Communities European Commission - Joint Research Centre 2002 92-894-3706-5 1 55 2016-02-19 OPUS4-1610 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Dudzus, Thomas; Meier, Klaus; Recknagel, Sebastian; Hedrich, Martina; Matschat, Ralf The measurement of O and N by classical carrier gas hot extraction (HE) - Carrier gas hot extraction after activation with photons Centro Nacional de Metrología 2002 Proceedings of CENAM CENAM Mexico City, Mexico 2002-01-28 2002-02-01 2016-02-19 OPUS4-1611 Beitrag zu einem Tagungsband Kipphardt, Heinrich; Matschat, Ralf Preparation of primary calibration substances - method development for trace analysis Centro Nacional de Metrología 2002 Proceedings of CENAM CENAM Mexico City, Mexico 2002-01-28 2002-02-01 2016-02-19 OPUS4-2627 Beitrag zu einem Tagungsband Ecker, Klaus; Dudzus, Thomas; Merchel, Silke; Kipphardt, Heinrich Vízkelethy, G. Oxygen determination in BaF2 and CaF2 by Charged Particle Activation Analysis Amsterdam Elsevier 2004 Ion beam analysis (Nuclear instruments & methods in physics research : Section B, Beam interactions with materials and atoms 219/220.2004) 219-220 16th International Conference on Ion Beam Analysis (IBA-16) Albuquerque, NM, USA 2003-06-29 2003-07-04 P2 113 2016-02-19 OPUS4-3588 Vortrag Kipphardt, Heinrich Development of SI-traceable standards of high metrological quality for chemical analysis of the elements 2002 12th EuroAnalysis 12th EuroAnalysis Dortmund, Germany 2002-09-08 2002-09-13 2016-02-19 OPUS4-1087 Zeitschriftenartikel Kipphardt, Heinrich; Aregbe, Y.; Valkiers, S.; Norgaard, J.; De Bièvre, P.; Taylor, P.D.P.; Poths, J. A primary isotopic gas standard for krypton with values for isotopic composition and molar mass traceable to the Système International d'Unités 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. Amsterdam Elsevier 2001 International Journal of Mass Spectrometry 206 129 136 10.1016/S1387-3806(00)00397-3 2016-02-19 OPUS4-1099 Zeitschriftenartikel Kipphardt, Heinrich; Taylor, P.; De Bièvre, P. The definition of primary method of measurement (PMM) of the 'highest metrological quality': a challenge in understanding and communication 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'. Berlin Springer 2001 Accreditation and quality assurance 6 103 103 106 10.1007/PL00010444 2016-02-19 OPUS4-1137 Zeitschriftenartikel Kipphardt, Heinrich; Ding, T.; Valkiers, S.; De Bièvre, P.; Taylor, P.D.P.; Gonfiantini, R.; Krouse, R. Calibrated sulfur isotope abundance ratios of three IAEA sulfur isotope reference materials and V-CDT with a reassessment of the atomic weight of sulfur 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). New York, NY Elsevier Science Geochemical Society 2001 Geochimica et cosmochimica acta 65 15 2433 2437 10.1016/S0016-7037(01)00611-1 2016-02-19 OPUS4-1408 Zeitschriftenartikel Kipphardt, Heinrich; Russe, K.; Bréas, O.; Taylor, P.D.P. Conversion of Carbon into CF4 for SI-Traceable Measurements of Absolute Carbon Isotope Amount Ratios: A Feasibility Study 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. Washington, DC American Chemical Society 2002 Analytical chemistry 74 3199 3205 10.1021/ac015700g 2016-02-19 OPUS4-1361 Zeitschriftenartikel Kipphardt, Heinrich; Dudzus, Thomas; Meier, Klaus; Recknagel, Sebastian; Hedrich, Martina; Matschat, Ralf 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 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.) Sendai Japan Institute of Metals 2002 Materials transactions 43 8th International Conference on Ultra-High Purity Base Metals (UHPM-2001) Berlin, Germany 2001-06-25 2001-06-28 2 98 100 10.2320/matertrans.43.98 2016-02-19 OPUS4-5483 Zeitschriftenartikel Kipphardt, Heinrich; Czerwensky, Michael; Matschat, Ralf ICP-MS analysis of high purity molybdenum used as SI-traceable standard of high metrological quality 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. London Royal Society of Chemistry 2005 Journal of analytical atomic spectrometry 20 1 28 34 2016-02-19 OPUS4-12443 Beitrag zu einem Sammelband Recknagel, Sebastian; Kipphardt, Heinrich; Meckelburg, Angela Angeli, J. Determination of nitrogen in ferritic electric heating steel ECRM 299-1 Essen VGE Verl. GmbH 2006 CETAS 2006 : progress in analytical chemistry in the steel industries 3-7739-6016-6 7th International Workshop "Progress in Analytical Chemistry in the Steel and Metal Industries" Luxembourg 2006-05-16 2006-05-18 409 413 2016-02-19 OPUS4-12056 Zeitschriftenartikel Rienitz, O.; Jährling, R.; Schiel, D.; Matschat, Ralf; Kipphardt, Heinrich; Gernand, W.; Oeter, D. Rückführung in der Elementanalytik Bremerhaven Wirtschaftsverl. NW Physikalisch-Technische Bundesanstalt 2005 PTB-Mitteilungen 115 4 295 299 2016-02-19 OPUS4-11253 Beitrag zu einem Sammelband Recknagel, Sebastian; Kipphardt, Heinrich; Panne, Ulrich Certified reference materials: CRM - ERM - EURONORM Medlov Cesky metrologicky institut 2005 Reference Materials and Interlaboratory Comparisons II 80-86380-30-0 Reference Materials and Interlaboratory Comparisons II Medlov, Czech Republic 2005-11-07 2005-11-09 7 12 2016-02-19 OPUS4-11907 Vortrag Kipphardt, Heinrich Certification of the first 10 National standards for element determination 2005 Abteilungsseminar: Abt. I, BAM Abteilungsseminar: Abt. I, BAM Berlin, Germany 2005-02-21 2005-02-21 2016-02-19 OPUS4-13495 Vortrag Kipphardt, Heinrich Measurement of oxygen and nitrogen in high purity iron (ONRRT 2205) 2006 13th International Conference on ultra high-purity base metals (UHPM-2006) 13th International Conference on ultra high-purity base metals (UHPM-2006) Berlin, Germany 2006-09-11 2006-09-14 2016-02-19 OPUS4-13498 Posterpräsentation Kipphardt, Heinrich Microwave induced plasma spectrometry (MIP) as detector for carrier gas hot extraction (CGHE) 2007 Winterconference on Plasmaspectrochemistry 2007 Winterconference on Plasmaspectrochemistry 2007 Taormina, Italy 2007-02-18 2007-02-23 2016-02-19 OPUS4-13773 Posterpräsentation Kipphardt, Heinrich Reinheitsbestimmung von Kupfer mit der Glimmentladungs-Massenspektrometrie (GDMS) - auf dem Weg zu rückgeführten Messwerten 2006 16. Jahrescolloquium Interessengemeinschaft Atomspektroskopie Berlin (IGAS) 16. Jahrescolloquium Interessengemeinschaft Atomspektroskopie Berlin (IGAS) Berlin, Germany 2006-11-08 2006-11-08 2016-02-19 OPUS4-5328 Vortrag Kipphardt, Heinrich Certified Reference Materials and the European Reference Material Initiative 2004 Workshop on Certified Reference Materials and ERM, Czech Metrology Institute Workshop on Certified Reference Materials and ERM, Czech Metrology Institute Prague, Czech Republic 2004-11-24 2016-02-19 OPUS4-5971 Posterpräsentation Kipphardt, Heinrich SI-traceable standards oh high metrological quality for chemical measurements 2002 EU conference "Towards an integrated infrastructure for measurements" EU conference "Towards an integrated infrastructure for measurements" Warsaw, Poland 2002-06-18 2002-06-19 2016-02-19 OPUS4-5972 Posterpräsentation Kipphardt, Heinrich Rückführungssystem für die Elementanalytik 2004 Analytica Conference 2004 Analytica Conference 2004 Munich, Germany 2004-05-11 2004-05-15 2016-02-19 OPUS4-5970 Posterpräsentation Kipphardt, Heinrich Reinststoffe für die Kalibrierung - Wie rein sind die Stoffe? 2004 Analytica Conference 2004 Analytica Conference 2004 Munich, Germany 2004-05-11 2004-05-15 2016-02-19 OPUS4-10994 Zeitschriftenartikel Lange, Britta; Kipphardt, Heinrich; Recknagel, Sebastian; Meier, Klaus Preparation and analysis of a reference material for the measurement of oxygen in copper The preparation and analysis of the oxygen mass fraction of three pure copper reference materials (BAM-379/1, BAM-379/2, BAM-379/3) intended for the calibration of spark emission spectrometry are described here. Data of homogeneity testing and round robin certification in collaboration with 12 independent laboratories from metalworking industry and research are reported. Problems with the establishment of traceability in this special case are discussed. Berlin Springer 2002 Accreditation and quality assurance 7 1 19 23 10.1007/s00769-001-0413-3 2016-02-19 OPUS4-25953 Vortrag Kipphardt, Heinrich Development of Primary standards for element determination and trace analysis 2011 Institutskolloquium (CENAM) Institutskolloquium (CENAM) Querétaro, Mexico 2011-09-08 2011-09-08 2016-02-19 OPUS4-25955 Vortrag Kipphardt, Heinrich Advance in non-metal determination 2011 Institutskolloquium (CENAM) Institutskolloquium (CENAM) Querétaro, Mexico 2011-09-09 2011-09-09 2016-02-19 OPUS4-28659 Zeitschriftenartikel Gopala, Anil; Mahn, S.; Panne, Ulrich; Kipphardt, Heinrich In situ vacuum thermal mass spectroscopy for the selection of an environmentally friendly, energy saving catalytic additive and optimization of the process by a novel ignition mechanism We report herein the utilization of vacuum thermal mass spectrometry (VTMS) for the selection of an environmentally friendly, energy saving catalytic additive and a novel ignition mechanism, which is complementary to catalysis for the reduction of zinc oxide with carbon. London RSC Publishing 2013 RSC Advances 3 25 9677 9680 10.1039/c3ra40223a 2016-02-20 OPUS4-25346 Zeitschriftenartikel Gusarova, Tamara; Methven, B.; Kipphardt, Heinrich; Sturgeon, R.; Matschat, Ralf; Panne, Ulrich Calibration of double focusing glow discharge mass spectrometry instruments with pin-shaped synthetic standards Calibration of two commercially available glow discharge double focusing mass spectrometers, the VG 9000 and Element GD, is described using synthetic pin standards pressed from solution doped copper and zinc matrices. A special pressing die was developed for this purpose and optimal results were obtained with the highest possible pressures, i.e., 95 kN·cm- 2. This calibration approach permits the determination of trace element mass fractions down to µg·kg- 1 with small uncertainties and additionally provides traceability of the GD-MS results in the most direct manner to the SI (International System of Units). Results were validated by concurrent measurements of a number of compact copper and zinc certified reference materials. The impact of the sample pin cross-section (circular or square) was investigated with the use of a new pin-sample holder system for the Element GD. The pin-sample holder was designed by the manufacturer for pin-samples having circular cross-section; however, samples with square pin cross-section were also shown to provide acceptable results. Relative Sensitivity Factors for some 50 analytes in copper (VG 9000, Element GD) and zinc matrices (VG 9000) are presented. The field of applicability of GD-MS may be considerably extended via analysis of pin geometry samples based on their ease of preparation, especially with respect to the accuracy and traceability of the results and the enhanced number of analytes which can be reliably calibrated using such samples. Amsterdam Elsevier 2011 Spectrochimica acta B 66 11-12 847 854 10.1016/j.sab.2011.12.001 2016-02-19 OPUS4-25561 Vortrag Kipphardt, Heinrich Chemie genau genommen- Metrologie in der Chemie 2012 6. Interdisziplinäres Doktorandenseminar (GDCh&DECHEMA) 6. Interdisziplinäres Doktorandenseminar (GDCh&DECHEMA) Berlin, Germany 2012-02-26 2012-02-28 2016-02-19 OPUS4-16299 Vortrag Kipphardt, Heinrich Characterisation of high purity metals as primary standards for element determination 2007 Workshop zum EUROMET 732 Projekt (Towards more accurate temperature fixed points) Workshop zum EUROMET 732 Projekt (Towards more accurate temperature fixed points) Paris, France 2007-11-23 2007-11-24 2016-02-19 OPUS4-17455 Zeitschriftenartikel Rudtsch, S.; Fahr, M.; Fischer, J.; Gusarova, Tamara; Kipphardt, Heinrich; Matschat, Ralf High-Purity Fixed Points of the ITS-90 with Traceable Analysis of Impurity Contents 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. Dordrecht Springer 2008 International Journal of Thermophysics 29 1 139 150 10.1007/s10765-007-0358-9 2016-02-19 OPUS4-17985 Vortrag Kipphardt, Heinrich Chemical analysis 2008 Summer School of Metrology, International Graduate School of Metrology Braunschweig Summer School of Metrology, International Graduate School of Metrology Braunschweig Goslar, Germany 2008-09-03 2008-09-03 2016-02-19 OPUS4-6187 Zeitschriftenartikel Matschat, Ralf; Kipphardt, Heinrich Das Primäre Kalibriersystem der BAM für die Elementanalytik Clausthal-Zellerfeld Gesellschaft Deutscher Metallhütten- und Bergleute 2003 Erzmetall 4 179 189 2016-02-19 OPUS4-6188 Zeitschriftenartikel Matschat, Ralf; Czerwensky, Michael; Traub, Heike; Heinrich, Hans-Joachim; Kipphardt, Heinrich Special new techniques of atomic spectrometric methods for trace analysis of high purity metals Paris 2003 Matériaux et techniques 91 Décembre 37 50, N° Hors Série 2016-02-19 OPUS4-7156 Beitrag zu einem Sammelband Kipphardt, Heinrich Traceability in Isotopic Measurements Den Haag Elsevier 2004 Handbook of Stable Isotope Analytical Techniques I 044451114-8 928 943 2016-02-19 OPUS4-10889 Zeitschriftenartikel Matschat, Ralf; Heinrich, Hans-Joachim; Czerwensky, Michael; Kuxenko, Sandra; Kipphardt, Heinrich Multielement trace determination in high purity advanced ceramics and high purity metals Bangalore Indian Academy of Sciences 2005 Bulletin of materials science 28 International Symposium on Ultrapure Materials (ISUPM) Hyderabad, India 2004-11-22 2004-11-23 4 361 366 2016-02-19 OPUS4-10954 Vortrag Kipphardt, Heinrich Certification of Primary Standards for Element Determination 2005 Meeting of CCQM-Inorganic Analytical Working Group Meeting of CCQM-Inorganic Analytical Working Group Berlin, Germany 2005-10-19 2005-10-21 2016-02-19 OPUS4-10956 Vortrag Kipphardt, Heinrich CCQM-P62: purity of nickel with respect to six defined metallic analytes 2005 Meeting of CCQM-Inorganic Analytical Working Group Meeting of CCQM-Inorganic Analytical Working Group Berlin, Germany 2005-10-19 2005-10-21 2016-02-19 OPUS4-12649 Zeitschriftenartikel Matschat, Ralf; Hinrichs, J.; Kipphardt, Heinrich Application of glow discharge mass spectrometry to multielement ultra-trace determination in ultrahigh-purity copper and iron: a calibration approach achieving quantification and traceability 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. Berlin Springer 2006 Analytical and bioanalytical chemistry 386 1 125 141 10.1007/s00216-006-0645-5 2016-02-19 OPUS4-17439 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf Traceability and uncertainty of chemical measurement results exemplified in the frame of the certification and the use of the glass CRM BAM-S005 Venezia Aurora Pubbl. Stazione Sperimentale del Vetro 2007 Rivista della Stazione Sperimentale del Vetro 6 19 23 2016-02-19 OPUS4-17725 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf Purity assessment for providing primary standards for elemental determination - a snap shot of international comparability 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. Wien Springer 2008 Microchimica acta 162 1-2 269 275 10.1007/s00604-007-0937-2 2016-02-19 OPUS4-17727 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Metrology in chemistry - a rocky road The application of metrology in chemical analysis is today hampered by psychological and practical barriers. The argumentation is based on the differences in physical and chemical metrology, which arises mainly from the objects of the measurements. The term “measurement” is discussed in the realm of analytical chemistry with a special focus on the inherent relation between chemical identification and determination as well as the consequent use of the concept of traceability and uncertainty. Wien Springer 2008 Microchimica acta 162 1-2 35 41 10.1007/s00604-007-0909-6 2016-02-19 OPUS4-18397 Vortrag Kipphardt, Heinrich Production of inorganic CRMs with SI traceable values at BAM 2008 Workshop of the CCQM-IAWG on production of traceable reference materials Workshop of the CCQM-IAWG on production of traceable reference materials Vienna, Austria 2008-10-08 2008-10-09 2016-02-19 OPUS4-18398 Vortrag Kipphardt, Heinrich CCQM-P107: purity of zinc with respect to six defined metallic analytes 2008 Meeting of CCQM-Inorganic Analytical Working Group Meeting of CCQM-Inorganic Analytical Working Group Vienna, Austria 2008-10-08 2008-10-09 2016-02-19 OPUS4-14063 Zeitschriftenartikel Bremser, Wolfram; Becker, Roland; Kipphardt, Heinrich; Lehnik-Habrink, Petra; Panne, Ulrich; Töpfer, Antje Stability testing in an integrated scheme ISO Guide 35 deals with RM stability issues and scrutinizes the evaluation of stability testing results under the assumption that either there is no trend at all (a rather rare situation), or any observed deterministic change is insignificant and thus can be neglected. However, market demands for reliable reference materials are obviously not limited to stable or at least seemingly stable materials. In many analytical applications, analytes and measurands under consideration are known, or at least suspected, to be unstable on time scales that may vary widely from measurand to measurand. The Federal Institute for Materials Research and Testing (BAM) has developed (and successfully uses) an integrated approach in its certification practice. The approach is based on an initial stability study and subsequent post-certification monitoring. Data evaluation is model-based and takes advantage of all information collected in the stability testing scheme(s). It thus allows one to deal with any kind of instability observed, to assess limiting time intervals at any stress condition in the range tested, to estimate a final expiry date for materials with detected instabilities or the maximum admissible re-testing interval for seemingly stable materials, and to assess maximum admissible stress loads during delivery of the material to the customer. The article describes (and exemplifies) typical study layout, the model selection, and the integrated data assessment. Berlin Springer 2006 Accreditation and quality assurance 11 10 489 495 10.1007/s00769-006-0152-6 2016-02-19 OPUS4-14098 Vortrag Kipphardt, Heinrich Primary calibration materials and trace analysis 2006 Leibnitz-Institut für Festkörper- und Werkstoffforschung Leibnitz-Institut für Festkörper- und Werkstoffforschung Dresden, Germany 2006-12-13 2006-12-13 2016-02-19 OPUS4-14636 Posterpräsentation Kipphardt, Heinrich Mikrowelleninduzierte Plasmaspektrometrie (MIP) als Detektor für die Trägergas-Heißextraktion (CGHE) 2007 ANAKON 2007 ANAKON 2007 Jena, Germany 2007-03-27 2007-03-30 2016-02-19 OPUS4-14626 Vortrag Kipphardt, Heinrich Traceability and uncertainty of chemical measurement results exemplified by measurements in the frame of the certification of the glass CRM BAM-S005 2007 XXI International Congress on Glass - ICG 2007 XXI International Congress on Glass - ICG 2007 Strasbourg, France 2007-07-01 2007-07-06 2016-02-19 OPUS4-14801 Vortrag Kipphardt, Heinrich Measurement of oxygen, nitrogen and carbon using radiochemical photon activation analysis (RPAA) 2007 International Conference on Ultra High Purity Base Metals International Conference on Ultra High Purity Base Metals Paris, France 2007-07-02 2007-07-06 2016-02-19 OPUS4-14802 Vortrag Kipphardt, Heinrich Metrologie in der Chemie 2007 EUROLAB-D Kolloquium "Die europäische Entwicklung und ihre Auswirkungen auf Deutschland", BAM EUROLAB-D Kolloquium "Die europäische Entwicklung und ihre Auswirkungen auf Deutschland", BAM Berlin, Germany 2007-04-20 2016-02-19 OPUS4-16153 Zeitschriftenartikel Traub, Heike; Czerwensky, Michael; Matschat, Ralf; Kipphardt, Heinrich; Panne, Ulrich Homogenitätsprüfung und Analyse von reinem Kupfer mit Laserablation-ICP-Massenspektrometrie Isernhagen Giesel Verlag GmbH 2007 Metall 61 11 744 745 2016-02-19 OPUS4-16392 Zeitschriftenartikel Kipphardt, Heinrich Workshop on "Trends in Uncertainty Evaluation and Interlaboratory Comparison Analysis": a participant's view Berlin Springer 2007 Accreditation and quality assurance 12 12 659 660 10.1007/s00769-007-0331-0 2016-02-19 OPUS4-17359 Zeitschriftenartikel Kipphardt, Heinrich; Czerwensky, Michael; Matschat, Ralf Use of microwave induced plasma spectrometry as detector for the determination of O, N and H traces after carrier gas hot extraction 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. London Royal Society of Chemistry 2008 Journal of analytical atomic spectrometry 23 4 588 591 10.1039/B714734a 2016-02-19 OPUS4-12199 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Rienitz, O.; Schiel, D.; Gernand, W.; Oeter, D. Traceability system for elemental analysis 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. Berlin Springer 2006 Accreditation and quality assurance 10 11 633 639 10.1007/s00769-005-0084-6 2016-02-19 OPUS4-12147 Vortrag Kipphardt, Heinrich Reinheitsbestimmung von Kufper mit der Glimmentladungs-Massenspektrometrie (GDMS) - auf dem Weg zu rückgeführten Messwerten 2006 Analytica Cenference Analytica Cenference Munich, Germany 2006-04-25 2006-04-28 2016-02-19 OPUS4-13478 Vortrag Kipphardt, Heinrich Carrier gas hot extraction and plasma emission spectrometry for the measurement of non-metals in high purity metals 2006 13th International Conference on ultra high-purity base metals 13th International Conference on ultra high-purity base metals Berlin, Germany 2006-09-11 2006-09-14 2016-02-19 OPUS4-28971 Zeitschriftenartikel Zhou, T.; Richter, Silke; Matschat, Ralf; Kipphardt, Heinrich Determination of the total purity of a high-purity silver material to be used as a primary standard for element determination 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. Berlin Springer 2013 Accreditation and quality assurance 18 4 341 349 10.1007/s00769-013-0988-5 2016-02-20 OPUS4-21291 Zeitschriftenartikel Gopala, Anil; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Use of mass spectrometric detection as a versatile process monitoring tool: reduction patterns in a milled ZnO/Al mixture Mass spectrometric detection can play a prominent role in the assessment of different reactions occurring at varied temperatures in a milled ZnO/Al mixture. This is the first time that online mass spectrometric information was used as a tool for monitoring and understanding the chemical reduction process mechanism. We have observed four different types of reaction taking place: (1) distillation of Zn metal, (2) reduction of ZnO by activated Al, (3) melting of Al and finally (4) reduction of ZnO by inactivated Al. The experimental conditions and results observed by QMS were supported with literature data and physical measurement data from X-Ray Diffraction (XRD) which gave us an idea about the complex reaction cascade which occurred during the formation of the zinc metal. Cambridge RSC Publ. Royal Society of Chemistry 2010 Analytical methods 2 451 454 10.1039/c0ay00057d 2016-02-19 OPUS4-21628 Zeitschriftenartikel Recknagel, Sebastian; Noack, Siegfried; Steiger, Thomas; Kipphardt, Heinrich; Matschat, Ralf International comparability of determination of mass fractions of chromium, copper, iron, manganese and zinc in aluminium alloy: Comité consultatif pour la quantité de matière key comparison K42 The degree of equivalence within the participating national metrology institutes for the measurement results of the mass fractions of the analytes Cr, Cu, Fe, Mn and Zn in an aluminium alloy was assessed. This interlaboratory comité consultatif pour la quantité de matière key comparison (CCQM-K42) was organised as an activity of the Inorganic Analytical Working Group of CCQM. In total seven laboratories participated, six of them for all analytes. Measurands were the mass fractions of the analytes in a range of 0.05 and 0.2%. As an outcome the consistency of the results for all elements investigated was acceptable, hence satisfactory comparability was established. An aluminium based certified reference material—undisclosed to the analysts which one it was—was used as test sample. For the purpose of this study homogeneity was tested at BAM. Each laboratory was free to choose any analytical method they wanted to use for the analysis. Consequently various methods of measurement were employed: instrumental neutron activation analysis, X-ray fluorescence spectrometry (XRF) using fused cast-bead method combined with reconstitution technique, inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry. Metrological traceability of the measurement results to the SI unit had to be demonstrated. Therefore, methods such as spark OES or XRF (without fused cast-bead technique)—both of them being most important methods for the analysis of metals and alloys in industrial laboratories—could not be used in the frame of the key comparison. Berlin Springer 2010 Accreditation and quality assurance 15 7 401 407 10.1007/s00769-010-0641-5 2016-02-19 OPUS4-22376 Zeitschriftenartikel Gusarova, Tamara; Hofmann, T.; Kipphardt, Heinrich; Venzago, C.; Matschat, Ralf; Panne, Ulrich 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 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. London Royal Society of Chemistry 2010 Journal of analytical atomic spectrometry 25 314 321 10.1039/b921649a 2016-02-19 OPUS4-20662 Vortrag Kipphardt, Heinrich The Importance of UHPM conferences and of ultrahigh metals in view of analytical challenges 2009 UHPM 2009 UHPM 2009 Sendai, Japan 2009-12-15 2009-12-15 2016-02-19 OPUS4-20628 Vortrag Kipphardt, Heinrich Advances in purification and trace analysis of Zinc 2009 UHPM 2009 UHPM 2009 Sendai, Japan 2009-12-15 2009-12-15 2016-02-19 OPUS4-20767 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Vogl, Jochen; Gusarova, Tamara; Czerwensky, Michael; Heinrich, Hans-Joachim; Hioki, A.; Konopelko, L.A.; Methven, B.; Miura, T.; Petersen, O.; Riebe, Gundel; Sturgeon, R.; Turk, G.C.; Yu, L. L. Purity determination as needed for the realisation of primary standards for elemental determination: status of international comparability 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. Berlin Springer 2010 Accreditation and quality assurance 15 1 29 37 10.1007/s00769-009-0557-0 2016-02-19 OPUS4-20727 Zeitschriftenartikel Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Development of SI traceable standards for element determination In Germany a system of primary amount of substance standards for elemental analysis is being developed, which forms the material´s basis for the National Standards for element determination. The metrological concept and technical approach is briefly described. The objective of traceability in chemistry, in this case for elemental determination, is illustrated on the example of copper. Basel Schweizerische Chemische Gesellschaft European Peptide Symposium 2009 Chimia 63 10 637 639 10.2533/chimia.2009.637 2016-02-19 OPUS4-20837 Vortrag Kipphardt, Heinrich Material Technology and Corrosion Science at BAM 2009 UHPM Symposium 2009 UHPM Symposium 2009 Kawasaki, Japan 2009-12-18 2009-12-18 2016-02-19 OPUS4-21195 Zeitschriftenartikel Traub, Heike; Czerwensky, Michael; Matschat, Ralf; Kipphardt, Heinrich; Panne, Ulrich Different calibration strategies for the analysis of pure copper metal by nanosecond laser ablation inductively coupled plasma mass spectrometry In this work, different calibration strategies for the determination of trace elements in pure copper metal by nanosecond laser ablation ICP-MS were investigated. In addition to certified reference materials (CRMs), pellets of doped copper powder were used for calibration. The micro homogeneity of the CRMs as well as the solution-doped pellets was sufficient to use them as calibration samples in combination with a laser spot size of 200 µm. In contrast, pellets doped with analytes in solid form showed a significant heterogeneity. For most of the investigated analytes and copper CRMs the measured mass fractions were within ± 20% of their certified values when other copper CRMs were used as calibration samples. When solution-doped powder pellets were used as calibration samples a systematic trend towards mass fractions below the certified values was observed for nearly all elements determined in the analysed CRMs. Thermal fractionation effects during the ablation of the solution-doped pellets were suspected as the extent of the fractionation depends on the irradiance, whereas fractionation is reduced at higher irradiance. London Royal Society of Chemistry 2010 Journal of analytical atomic spectrometry 25 5 690 696 10.1039/b915564c 2016-02-19 OPUS4-23202 Zeitschriftenartikel Ried, Peter; Gaber, Martin; Beyer, Katrin; Müller, Ralf; Kipphardt, Heinrich; Kannengießer, Thomas Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS. Düsseldorf Verl. Stahleisen 2011 Steel research international 82 1 14 19 10.1002/srin.201000237 2016-02-19 OPUS4-23812 Vortrag Kipphardt, Heinrich Non-metal determination - a chalenge in elemental analysis 2011 CCQM IAWG workshop CCQM IAWG workshop Paris, France 2011-04-13 2011-04-13 2016-02-19 OPUS4-23813 Vortrag Kipphardt, Heinrich Special ways to achieve metrological traceability of results in GD-MS and in some other direct solid sampling methods 2011 CCQM IAWG workshop CCQM IAWG workshop Paris, France 2011-04-13 2011-04-13 2016-02-19 OPUS4-26702 Vortrag Kipphardt, Heinrich Messtechnische Rückführung in der Elementanalytik 2012 18.Kolloquium von EUROLAB-D, BAM 18.Kolloquium von EUROLAB-D, BAM Berlin, Germany 2012-05-04 2016-02-19 OPUS4-26050 Zeitschriftenartikel Heinrich, Hans-Joachim; Kipphardt, Heinrich Application of methane as a gaseous modifier for the determination of silicon using electrothermal atomic absorption spectrometry For determination of silicon in aqueous solutions by electrothermal atomic absorption spectrometry methane/argon mixtures as a gaseous modifier were applied during the pyrolysis step to improve the analytical performance. The beneficial effects observed on thermal stabilization, signal enhancement and shape of absorbance signals were attributed to the thermal decomposition products of methane, which were hydrogen and carbon black (soot). Using a 5% CH4 mixture with argon, the optimized pyrolysis and atomization temperatures were 1350 °C and 2450 °C, respectively. A flushing step following the pyrolysis was mandatory to avoid background absorption and accelerated deposition of pyrolytic graphite. Characteristic masses of 50 and 30 pg were obtained for standard transversely heated graphite atomizer (THGA) tubes and end-capped THGA tubes, respectively, which were lower than with other previously applied modifiers. A limit of detection of 0.2 µg L- 1 (3 s, n = 10) has been obtained. In addition, this gaseous modifier did not contribute to contamination which often was significant when a liquid modifier solution was co-injected. The proposed method has been applied to the determination of silicon in ultrapure water, nitric and hydrochloric acids. Amsterdam Elsevier 2012 Spectrochimica acta B 70 68 73 10.1016/j.sab.2012.04.001 2016-02-19 OPUS4-29893 Zeitschriftenartikel Balski, Matthias; Kipphardt, Heinrich; Berger, Achim; Meyer, S.; Panne, Ulrich Determination of impurities in solar grade silicon by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) subsequent to matrix evaporation A method for the determination of 22 trace impurities in solar grade silicon after dissolution in a mixture of HF and HNO3 and subsequent matrix evaporation is reported. The presented method involves a simple, inexpensive, one-vessel sample preparation apparatus design. The recoveries of B, Na, Mg, Al, P, K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Mo, Sb, W, and Tl at 250 µg kg-1 level are in the range of 93 to 108%. After careful selection of monitored isotopes and their respective resolutions, a sector field mass spectrometer has been used to carry out the measurements. Limits of determination down to 120 ng kg-1 have been obtained using a calibration by three-point standard addition. The method was tested on diluted NIST SRM 57b silicon powder as well as on synthetic test samples and also applied successfully on raw solar grade silicon samples in an interlaboratory comparison including NAA. Cambridge RSC Publ. Royal Society of Chemistry 2014 Analytical methods 6 1 77 85 10.1039/C3AY41213J 2016-02-20 OPUS4-54840 Zeitschriftenartikel Recknagel, Sebastian; Bresch, Harald; Kipphardt, Heinrich; Resch-Genger, Ute; Koch, Matthias; Rosner, M. Trends in selected fields of reference material production For more than 110 years, BAM has been producing reference materials for a wide range of application fields. With the development of new analytical methods and new applications as well as continuously emerging more stringent requirements of laboratory accreditation with regard to quality control and metrological traceability, the demand and requirements for reference materials are increasing. This trend article gives an overview of general developments in the field of reference materials as well as developments in selected fields of application in which BAM is active. This includes inorganic and metal analysis, gas analysis, food and consumer products, and geological samples. In addition to these more traditional fields of application, developments in the areas of optical spectroscopy, particulary fluorescence methods, and nanomaterials are considered. Berlin Springer 2022 Analytical and bioanalytical chemistry 414 150 years BAM: Science with impact Berlin, Germany 01.01.2021 31.12.2021 Topical collection: Analytical methods and applications in the materials and life sciences 4281 4289 urn:nbn:de:kobv:b43-548407 10.1007/s00216-022-03996-7 https://creativecommons.org/licenses/by/4.0/deed.de 2022-05-16 OPUS4-56083 Zeitschriftenartikel Kipphardt, Heinrich; Tuma, Dirk; Khanipour, Peyman; Maiwald, Michael Voll normal - Normen in der Gasanalytik In dieser Arbeit werden die Grundlagen der Normung, die Entstehung einer Norm und die für die Gasanalytik relevanten Normungsgremien kurz dargestellt. Dazu werden die wichtigsten Normen zur Gasanalytik entlang des analytischen Prozesses gruppiert und aufgeführt. Schließlich wird als Anwendungsbeispiel aus der eigenen Praxis der Prozess von der Herstellung bis zur Zertifizierung eines Kalibriergases beschrieben. Essen Vulkan Verlag 2022 gwf Gas + Energie 10 73 80 2022-10-24 OPUS4-56308 Zeitschriftenartikel van der Veen, A. M H; Zalewska, E. T.; Kipphardt, Heinrich; Beelen, R. R.; Tuma, Dirk; Maiwald, Michael; Fükő, J.; Büki, T.; Szilágyi, Z. N.; Beránek, J.; Cieciora, D.; Ochman, G.; e.t al., Metrologia International Bureau of Weights and Measures (BIPM), find out more - KEY COMPARISON International comparison CCQM-K118 natural gas CCQM-K118 was an international key comparison on natural gas composition with two types of gases, i.e., a low calorific hydrogen-enriched natural gas and a high calorific LNG type of gas. There were 14 participating laboratories. The traveling standards (i.e., 14 mixtures each) were obtained from an external source and checked for homogeneity and stability before and after the participants' measurements at the two coordinating laboratories. The data evaluation was performed using a consensus value and a laboratory effect model. The results of the participants were benchmarked against a key comparison reference value computed from the largest consistent subset (LCS) of the submitted results, adjusted for the differences between the travelling standards. For the first time in a key comparison in gas analysis, the model included a term to account for excess variability in the LCS. Most of the participants reported one or a few (slightly) discrepant results. Partly this is due to the heterogeneity and heteroscedasticity of the datasets. In all, the results in this key comparison demonstrate the good comparability of the national measurement standards for natural gas composition maintained by the participating NMIs. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA). To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). IOP Publishing LTD 2022 Metrologia 59 1A 10.1088/0026-1394/59/1A/08017 2022-11-21 OPUS4-30772 Zeitschriftenartikel Vogl, Jochen; Kipphardt, Heinrich; del Rocío Arvizu Torres, M.; Manzano, J.V.L.; Rodrigues, J.M.; de Sena, R.C.; Yim, Y.-H.; Heo, S.W.; Zhou, T.; Turk, G.C.; Winchester, M.; Yu, L. L.; Miura, T.; Methven, B.; Sturgeon, R.; Jährling, R.; Rienitz, O.; Tunc, M.; Can, S.Z. Final report of the key comparison CCQM-K72: Purity of zinc with respect to six defined metallic analytes KEY COMPARISON High purity elements can serve as a realization of the SI unit amount of substance for the specific element. Solutions prepared from high purity metals by applying gravimetric preparation and the concept of molar mass are used as 'calibration' solutions in many fields of analytical chemistry and provide the metrological basis in elemental analysis. Since ideal purity does not exist for real materials, the actual purity of the high purity material must be known with a specified uncertainty. As required uncertainties around 10-4 relative on the purity statement are not accessible in almost all cases by a direct measurement of the element in itself, the indirect approach is followed, where all elements excepting the matrix element itself are measured and their sum is subtracted from the value for ideal purity, which is 1 kg/kg. It was the aim of this comparison to demonstrate the capability of national metrology institutes and designated institutes to determine the purity of pure elements. In order to limit the effort within this comparison, only six metallic impurities (Ag, Al, Cd, Cr, Ni, Tl) in the low mg/kg range are considered in a zinc matrix. It has to be underlined here that the task was to measure the purity of zinc based on the determination of six analytes. The task is not trace analysis of specific analytes in zinc. This subtle distinction defines different measurands. The sample, pure Zn, was cut in pieces of cubic geometry for wet chemical analysis or of pin geometry for GDMS analysis and was sent to the participants. The comparison was run under the auspices of the Inorganic analysis Working Group (IAWG) of the CCQM and was piloted by the BAM Federal Institute for Materials Research and Testing, Berlin, Germany. The majority of the participants applied ICP-MS techniques and only two participants used additionally atomic absorption spectrometry. GDMS was used only by one participant. The observed spreads for the measurement results reported by the participants were significantly lower than those of the preceding study CCQM-P107 and were well below the target uncertainty of 30% relative. As a consequence, comparability within the participating laboratories is demonstrated to be established. The individual measurement results, mean values and medians derived were in all cases very consistent with the reference values obtained by IDMS and so the accuracy of the measurement results for the participating laboratories is as well demonstrated to be established. Especially with the results of CCQM-P62 and CCQM-P107 in mind, the outcome of CCQM-K72 can be considered as a big step forward in the community. CCQM is aware of the difference between a characterization based on only six analytes and a complete characterization. Therefore, the pilot study CCQM-P149 has been initiated and already started, which focuses on the fit-for-purpose approaches for the purity determination of metals (here: zinc) to be used as primary standards in elemental analysis. Another follow-up in the form of a pilot study on non-metal impurities is mandatory, because non-metal impurities such as oxygen, nitrogen and sulfur often make up the largest contributions. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). Bristol Inst. of Physics Publ. 2014 Metrologia 51 1A (Tech.Suppl. 2014) 08008, 1 40 10.1088/0026-1394/51/1A/08008 2016-02-20 OPUS4-30301 Zeitschriftenartikel Richter, Silke; Sargent, M.; Schiel, D.; Kipphardt, Heinrich Known purity - the fundament of element determination by atomic spectrometry Millions of measurements are performed each year by liquid based analytical atomic spectrometry to support healthcare, diagnostic tests, environmental monitoring, material assay, product development and safety. Despite the effort to develop absolute methods, most methods still depend on calibration solutions, which are gravimetric mixtures of high purity solvents and high purity (source material) metals or compounds. As in the real world ideal purity does not exist, the impurity of the solvent and the purity of the source material needs to be known. The impurity of a solvent with respect to one analyte can be measured rather easily and with low limits of determination. In contrast the measurement of the purity of the source material, i.e., the mass fraction of the main constituent in a high purity metal, is more difficult to determine. It becomes even more difficult when the source material is not a pure metal but a compound since problems regarding stoichiometry arise additionally. Although the major producers of calibration solutions make a special effort to determine the purity of the source material, the actual purity statement is often incomplete or not demonstrated. The main reason for this situation is the complexity and high effort necessary to fully characterize such a material. This problem holds to a very wide extent also for the primary standards for element determination at the National Metrology Institutes and Designated Institutes (NMIs and DIs). It is the task of the NMIs and DIs to realise and disseminate primary standards for providing traceability to the International System of Units (SI). The primary elemental standards at the NMIs should provide the link to secondary standards produced by commercial producers and other independently prepared standards for element determination. Without such primary standards, elemental calibration solutions may vary and, depending on the uncertainty required, comparability of measurement in time and space results cannot be achieved. London Royal Society of Chemistry 2013 Journal of analytical atomic spectrometry 28 10 1540 1543 10.1039/c3ja90045b 2016-02-20 OPUS4-30302 Zeitschriftenartikel D'Agostino, G.; Bergamaschi, L.; Giordani, L.; Oddone, M.; Kipphardt, Heinrich; Richter, Silke Use of instrumental neutron activation analysis to investigate the distribution of trace elements among subsamples of solid materials The results of analytical measurements performed with solid-sampling techniques are affected by the distribution of the analytes within the matrix. The effect becomes significant in case of determination of trace elements in small subsamples. In this framework we propose a measurement model based on Instrumental Neutron Activation Analysis to determine the relative variability of the amount of an analyte among subsamples of a material. The measurement uncertainty is evaluated and includes the counting statistics, the full-energy gamma peak efficiency and the spatial gradient of the neutron flux at the irradiation position. The data we obtained in a neutron activation experiment and showing the relative variability of As, Au, Ir, Sb and W among subsamples of a highly pure Rh foil are also presented. Bristol Inst. of Physics Publ. 2014 Metrologia 51 1 6 2016-02-20 OPUS4-30375 Vortrag Kipphardt, Heinrich Primary Standards for Challenging Elements - WP 1.3 "Non-metallic impurities" 2014 EMRP stakeholder meeting EMRP stakeholder meeting Teddington, England 2014-02-03 2014-02-04 2016-02-20 OPUS4-30956 Zeitschriftenartikel Balski, Matthias; Emmerling, Franziska; Kipphardt, Heinrich; Panne, Ulrich Determination of boron in silicon without use of additional complexing agents Methods for the determination of boron in various matrices described in the literature usually employ complexing agents like mannitol to retain the volatile boron species during matrix evaporation steps. However, also relatively high boron recoveries from silicon containing samples have been reported when no complexing agents were added to the digestion acids. The mechanism behind this matrix-dependant recovery has been investigated by studying the boron recovery in the analysis of solar grade silicon. It was found that the NH4+ ion formed by the reduction of nitric acid during sample digestion is responsible for the higher recovery of boron, which leads to a possible analysis method without the use of complexing agents if the sample preparation procedure is carefully optimized. Cambridge RSC Publ. Royal Society of Chemistry 2014 Analytical methods 6 12 4003 4008 10.1039/c4ay00410h 2016-02-20 OPUS4-31975 Zeitschriftenartikel Plotnikov, Alexei; Pfeifer, Jens; Richter, Silke; Kipphardt, Heinrich; Hoffmann, V. Determination of major nonmetallic impurities in magnesium by glow discharge mass spectrometry with a fast flow source using sintered and pressed powder samples Fast flow glow discharge mass spectrometry with a Grimm-type ion source providing a high sputter rate was used for the determination of major nonmetallic impurities in magnesium. The analytical signal was found to be strongly influenced by the electrical discharge parameters. For calibration by standard addition, synthetic standard samples were produced in two different ways—namely, by pressing and by sintering doped metal powders. The observed sensitivity of the calibration curves was shown to depend on the particle size of the powder. For the magnesium powders, the mass fractions of oxygen, nitrogen, boron, and silicon were determined to be about 0.01 kg·kg-1 (relative standard deviation approximately 10-20 %), 2,700 mg·kg-1, 150 mg·kg-1, and 300 mg·kg-1, respectively. Berlin Springer 2014 Analytical and bioanalytical chemistry 406 29 7463 7471 10.1007/s00216-014-8185-x 2016-02-20 OPUS4-19600 Zeitschriftenartikel Gusarova, Tamara; Hodoroaba, Vasile-Dan; Matschat, Ralf; Kipphardt, Heinrich; Panne, Ulrich Exploitation of the hollow cathode effect for sensitivity enhancement of Grimm-type DC glow discharge optical emission spectroscopy 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. London Royal Society of Chemistry 2009 Journal of analytical atomic spectrometry 24 680 684 10.1039/b814977a 2016-02-19 OPUS4-19595 Zeitschriftenartikel Gopala, Anil; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Mass spectrometry insight of the process mechanism during the vacuum distillation of zinc Detection and monitoring of volatile elements released during the preparation of ultra high purity zinc by vacuum distillation (VD) is reported using online quadrupole gas source mass spectrometry (QMS). The theoretically calculated vapour pressures (pv) for the volatile impurity elements using Dushman constants and the practically observed mass spectra were found to be consistent (S. Dushman and J. M. Lafferty, Scienific Foundations of Vacuum Technique, 2nd ed., Wiley, New York, 1962). This is the first time that the potential ability of an online mass spectrometer was used for monitoring and understanding the process mechanism during the purification of metals (Zn) using VD. We here also illustrate our findings with the results from high resolution glow discharge mass spectrometer (HR-GDMS) analysis before and after the purification of Zn. London Royal Society of Chemistry 2009 Journal of analytical atomic spectrometry 24 887 890 10.1039/b904133h 2016-02-19 OPUS4-21991 Vortrag Kipphardt, Heinrich Primary standards for element determination & trace analysis 2010 RM 2010-Beijing International Symposium on Reference Materials RM 2010-Beijing International Symposium on Reference Materials Beijing, China 2010-10-26 2010-10-29 2016-02-19 OPUS4-19320 Vortrag Kipphardt, Heinrich CCQM-P107 - purity of zinc with respect to six metallic analytes 2009 CCQM-IAWG-Meeting CCQM-IAWG-Meeting Paris, France 2009-04-20 2009-04-20 2016-02-19 OPUS4-20402 Zeitschriftenartikel Traub, Heike; Wälle, M.; Koch, J.; Panne, Ulrich; Matschat, Ralf; Kipphardt, Heinrich; Günther, D. Evaluation of different calibration strategies for the analysis of pure copper and zinc samples using femtosecond laser ablation ICP-MS Solution-doped metal powder pellets as well as aspirated liquids were used as calibration samples to analyze pure copper and zinc certified reference materials (CRMs) by femtosecond laser ablation ICP-MS. It was demonstrated that calibration by copper pellets resulted in relative deviations up to 20%, whereas fs-LA-ICP-MS among copper-based CRMs led to inaccuracies in the same range unless nominal mass fractions were chosen to be <3 mg/kg. Calibration by zinc pellets generally provided better accuracy. Depending on the analyte considered, deviations below 10% were obtained even for mass fractions close to the limit of quantification. Our data, therefore, indicate solution-doped metal powder pellets to be suitable as calibration samples for fs-LA-ICP-MS of metals. Furthermore, the utilization of liquid standards for calibration was found to result in stronger deviations of up to 50% for both copper and zinc samples which, in addition, turned out to be dependent on the plasma conditions. Berlin Springer 2009 Analytical and bioanalytical chemistry 395 5 1471 1480 10.1007/s00216-009-3061-9 2016-02-19 OPUS4-21127 Zeitschriftenartikel Gopala, Anil; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Process methodology for the small scale production of m6N5 purity zinc using a resistance heated vacuum distillation system Ultra high purity Zn (m6N5) was obtained through triple vacuum distillation using an m4N5 Zn as input material. High-volatile impurities were removed from the zinc matrix by vacuum evaporation, while traces having lower volatility than the matrix remained in the residual material after finishing of the entire purification process. The time required for the removal of the main high-volatile impurity (Cd) was monitored using a connected gas source mass spectrometer. During distillation the Zn vapor of the distillate was condensed on the cap of a glassy carbon crucible which was water cooled by a movable copper block. The temperatures were optimized for the removal of the volatiles and for the distillation process using vapor pressure data. High resolution glow discharge mass spectrometry was applied for the analysis and purity evaluation of the distilled and input zinc. The analysis confirmed the reduction of the metallic impurities from 43 mg kg-1 to 0.5 mg kg-1 (m6N5) after three consecutive vacuum distillations. An increase in the grain size and a decrease in the micro-hardness were observed for the purified Zn material. Amsterdam Elsevier 2010 Materials chemistry and physics 122 1 151 155 10.1016/j.matchemphys.2010.02.080 2016-02-19 OPUS4-21910 Zeitschriftenartikel Gopala, Anil; Zellmann, M.; Kipphardt, Heinrich; Jakubowski, Norbert; Panne, Ulrich Mass spectrometric study of the impurity profile in Zn during reduction-distillation of ZnO with activated and inactivated Al In this work, we report on the application of hyphenated gas source mass spectrometry to study and understand the mechanism of the reduction-distillation of ZnO using Al powder as reductant in its activated and inactivated form. The experiments revealed that the purity of the Zn metal produced were superior using activated Al with respect to inactivated Al, i.e., m5N8 (99.9998% metallic based) versus m5N3. The achieved purity levels of Zn and the absence of high volatile Cd, Mg, and Sb impurities in the gas phase and the material collected were explained with respect to the impurity elements free-energy values, vapor pressure data, and an observed scavenging effect of the Ta crucible, which was supported by the on-line observed mass spectrometric profiles of the residual gas. New York, NY Elsevier American Society for Mass Spectrometry 2010 Journal of the American society for mass spectrometry 21 9 1620 1623 10.1016/j.jasms.2010.04.009 2016-02-19 OPUS4-21911 Zeitschriftenartikel Gopala, Anil; Jakubowski, Norbert; Panne, Ulrich; Kipphardt, Heinrich Real time monitoring of chemical transformations during catalytic reduction using gas source mass spectrometry: carbon/zinc carbonate hydroxide We report herein the utilization of a vacuum reduction distillation system (VRDS) coupled with mass spectrometry (MS) to characterize chemical transformations in thermal analysis. The system initially designed to monitor metal purification by distillation is applied for the first time to the catalytic reaction of in situ formed nickel oxide during the carbothermic reduction of zinc oxide. London Royal Society of Chemistry 2010 Journal of analytical atomic spectrometry 25 1378 1380 10.1039/c004179c 2016-02-19 OPUS4-24065 Zeitschriftenartikel Wienold, Julia; Traub, Heike; Bresch, Harald; Seeger, Stefan; Recknagel, Sebastian; Kipphardt, Heinrich Effort on calibration of infrared spark ablation of copper with synthetic copper standards Two types of copper samples, compact certified copper reference materials and calibration samples prepared from liquid doped, pressed copper powders, were studied in terms of accuracy of obtained calibration functions originating from infrared spark ablation. Additionally, corresponding particle size distributions of the aerosols from infrared spark ablation were recorded. It is shown that the differences in quantification results, originating from the two sets of calibration functions, could not mainly be ascribed to different particle size distributions of the two copper sample types. Possible other causes, as different ablation rates, parts of melting and differences of the chemical constitutions of the two sample types were explored. Amsterdam Elsevier B.V. 2011 Spectrochimica acta B 66 6 432 438 10.1016/j.sab.2011.04.005 2016-02-19 OPUS4-23373 Zeitschriftenartikel Rudtsch, S.; Gusarova, Tamara; Aulich, A.; Fahr, M.; Fischer, J.; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Procedure for the impurity-related correction at the indium fixed-point Determining the influence of impurities on the fixed-point emperatures of the ITS-90 requires the completion of several tasks. In this paper, the Progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAMFederal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical Analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell’s freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. Dordrecht Springer 2011 International Journal of Thermophysics 32 1-2 293 302 10.1007/s10765-011-0915-0 2016-02-19 OPUS4-20257 Zeitschriftenartikel Wienold, Julia; Traub, Heike; Lange, Britta; Giray, Thorsten; Recknagel, Sebastian; Kipphardt, Heinrich; Matschat, Ralf; Panne, Ulrich Elemental analysis of copper and magnesium alloy samples using IR-laser ablation in comparison with spark and glow discharge methods Three methods for direct solid sampling of bulk material namely IR laser ablation, glow discharge and spark OES, were compared with respect to analytical figures of merit obtained for elemental analysis with atomic spectrometry. Matrices investigated were copper, pressed doped copper powder, and magnesium alloys. For the vast majority of analytes, statistical equivalence regarding precision (usually ≤ 5%) and the performance of the calibrations between the compared methods was demonstrated. London Royal Society of Chemistry 2009 Journal of analytical atomic spectrometry 24 1570 1574 10.1039/b903251g 2016-02-19 OPUS4-23762 Beitrag zu einem Tagungsband Recknagel, Sebastian; Kipphardt, Heinrich; Lange, Britta; Hoppe, Marion Traceable analysis of impurities in metallic reference materials using GD-MS The traceabiiity requirements for certification analyses of reference materials are much more stringent than for routine analysis, where certified matrix reference materials (CRM) can be used for calibration and to establish traceabiiity. Although the ISO-Guides related to CRM production and certification are not fully clear concerning calibration, many established CRM-producers do not accept matrix-CRMs for calibration in case of certification analyses, e.g. to avoid circular reasoning. These requirements limit the methods used for certification to those that can be calibrated using Standards of known high purity and stoichiometry or mixtures of such Standards. Powerful solid sampling techniques such as glow discharge mass spectrometry (GD-MS) or spark-optical emission spectrometry (SOES), where usually compact CRMs are used for calibration, seem not be applicable for certification analyses. Especially GD-MS is a powerful tool for trace element determination of solid samples. Beside metallic impurities the use of specific gas mixtures enables also the determination of interesting nonmetallic impurities such as sulfur and phosphorus. Within BAM a calibration approach, was developed which enables to use mixtures of Standards of known high purity and stoichiometry also for GD-MS. Analogue to matrix adaption in solution based techniques, the calibration approach is based on doped pressed powder pellets. Approach and application on the certification analyses of copper and Steel CRMs are presented. Centre for research in metallurgy (CRM) 2011 CETAS 2011 - 8th International workshop on progress in analytical chemistry & materials characterisation in the steel and metal industries CETAS 2011 - 8th International workshop on progress in analytical chemistry & materials characterisation in the steel and metal industries Luxembourg, Luxembourg 17.05.2011 19.05.2011 OC53 361 365 2016-02-19 OPUS4-33065 Zeitschriftenartikel Kaltenbach, A.; Nordmann, J.; Görlitz, V.; Pape, C.; Richter, Silke; Kipphardt, Heinrich; Kopp, G.; Jährling, R.; Rienitz, O.; Güttler, B. Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of Urel(w)<0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools. Berlin Springer 2015 Analytical and bioanalytical chemistry 407 11 3093 3102 10.1007/s00216-014-8395-2 2016-02-20 OPUS4-33137 Vortrag Kipphardt, Heinrich Quantification in GD-MS 2015 CCQM IAWG Workshop: Approach to purity assessment of metal standards CCQM IAWG Workshop: Approach to purity assessment of metal standards Paris, Frankreich 2015-04-17 2015-04-17 2016-02-20 OPUS4-33613 Zeitschriftenartikel Kramer, Claus; Ried, Peter; Mahn, Stefan; Richter, Silke; Langhammer, Nicole; Kipphardt, Heinrich Design and application of a versatile gas calibration for non-metal determination by carrier gas hot extraction In carrier gas hot extraction the calibration of low amounts of non-metals with masses of a few micrograms with small uncertainty remains a challenge. To achieve high flexibility a high precision gas mixture pump was combined with an automated syringe drive. The gas mixing pump allows filling the syringe with different gas compositions; the automated syringe drive allows matching to modulate the signal profiles to those of real samples. The system was designed and its experimental potential explored. The resulting calibration curves were comparable to those obtained by calibration using solid materials of sufficient purity and stoichiometry. However smaller uncertainties and lower limits of quantification (i.e. 0.5 µg and 0.6 µg for O and N, respectively) were found using the gas calibration device. Cambridge RSC Publ. Royal Society of Chemistry 2015 Analytical methods 7 13 5468 5475 urn:nbn:de:kobv:b43-336130 10.1039/c5ay00845j http://creativecommons.org/licenses/by/3.0/de/deed.de 2016-02-20 OPUS4-44257 Zeitschriftenartikel Vogl, Jochen; Kipphardt, Heinrich; Richter, Silke; Bremser, Wolfram; Arvizu Torres, M.; Lara Manzano, J.; Buzoianu, M.; Hill, S.; Petrov, P.; Goenaga-Infante, H.; Sargent, M.; Fisicaro, P.; Labarraque, G.; Zhou, T.; Turk, G. C.; Winchester, M.; Miura, T.; Methven, B.; Sturgeon, R.; Jährling, R.; Rienitz, O.; Mariassy, M.; Hankova, Z.; Sobina, E.; Krylov, A. I.; Kustikov, Y. A.; Smirnov, V. V. Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute's applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and - 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process. Bristol Institute of Physics Publishing Bureau International des Poids et Mesures (BIPM) 2018 Metrologia : international journal of pure and applied metrology 55 2 211 221 10.1088/1681-7575/aaa677 2018-02-21 OPUS4-44471 Zeitschriftenartikel van der Hout, J. W.; van der Veen, A. M. H.; Ziel, P. R.; Kipphardt, Heinrich; Tuma, Dirk; Maiwald, Michael; Fernández, T. E.; Gómez, C.; Cieciora, D.; Ochman, G.; Dias, F.; Silvino, V.; Macé, T.; Sutour, C.; Marioni, F.; Ackermann, A.; Niederhauser, B.; Fükő, J.; Büki, T.; Szilágyi, Z. N.; Tarhan, T.; Engin, E. International Comparison Euramet.QM-K111 - Propane in Nitrogen This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison. The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within ± 1 % of the KCRV. IOP Science BIPM 2017 Metrologia 54 Technical Supplement 08020, 1 34 10.1088/0026-1394/54/1A/08020 2018-03-15 OPUS4-35258 Zeitschriftenartikel Bremser, Wolfram; Maiwald, Michael; Kipphardt, Heinrich Anwendung von Normen in der Gasanalytik - Teil 4 - Messunsicherheit und Rückführbarkeit von Messergebnissen Zusammen mit der Genauigkeit von Messungen ist die ihnen zugeordnete Messunsicherheit Ausdruck und Maß von Vergleichbarkeit und Richtigkeit. Die Messunsicherheit spielt ebenso die Schlüsselrolle im Aufbau einer Rückführbarkeitskette, wie in diesem Beitrag beschrieben. Es ist der vierte und letzte Teil einer Artikelserie (siehe Infokasten), die Einblicke gibt in die Arbeit des DIN-Normenausschusses „Gasanalyse und Gasbeschaffenheit" (DIN NA 062-05-73 AA) sowie der international tätigen Technical Committees 158 und 193 der ISO. Weinheim GIT-Verl., Wiley-VCH DECHEMA, GDCh, GVC-VDI 2015 CITplus 12 29 31 2016-02-20 OPUS4-35055 Posterpräsentation Kipphardt, Heinrich Experimental determination of (p, p, T) data for binary mixures of methane and helium 2015 19 th Symposium on Thermophysical Properties 19 th Symposium on Thermophysical Properties Boulder; CO, USA 2015-06-21 2015-06-26 2016-02-20 OPUS4-34945 Zeitschriftenartikel Maiwald, Michael; Kipphardt, Heinrich; Bremser, Wolfram Vom Abgas zum Erdgas - Wie genau sind Sondergase? - Normungsarbeit rund um aktuelle High-Tech Verfahren und Prozesse - Teil 1 In vielen industriellen High-Tech Verfahren und Prozessen, Forschung und Wissenschaft, Medizin und Umwelttechnik werden Sondergase eingesetzt. Als Gattungsbegriff umfasst diese Bezeichnung ein ansehnliches Spektrum höchster Qualitäten an Gasen. Dazu gehören u. a. Reinstgase mit besonders hohen Anforderungen an ihre Reinheit, Gasgemische genau definierter Zusammensetzung und Isotopengemische. Wie genau kann man Gaszusammensetzungen heute messen? Wie schafft man es, dass alle dasselbe messen? Welche Techniken kommen dabei zum Einsatz? Weinheim GIT-Verl., Wiley-VCH DECHEMA, GDCh, GVC-VDI 2015 CITplus 5 6 8 2016-02-20 OPUS4-49608 Zeitschriftenartikel Richter, Silke; Roethke, A.; Rienitz, O.; Matschat, Ralf; Schiel, D.; Jaehrling, R.; Goerlitz, V.; Kipphardt, Heinrich SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM - 25 years ago - up to latest achievements in the field of inorganic analysis. Bristol IOP BIPM - Bureau International des Poids et Mesures 2019 Metrologia 1 23 urn:nbn:de:kobv:b43-496080 10.1088/1681-7575/ab5636 http://creativecommons.org/licenses/by/3.0/de/deed.de 2019-11-20 OPUS4-40013 Zeitschriftenartikel Zhou, Z.; Han, Q.; Wang, D.; Macé, T.; Kipphardt, Heinrich; Maiwald, Michael; Tuma, Dirk; Uehara, S.; Akima, D.; Shimosaka, T.; Jung, J.; Oh, S.-H.; van der Veen, A.; van Wijk, J.I.T.; Ziel, P. R.; Konopelko, L.; Valkova, M.; Mogale, D.M.; Botha, A.; Brewer, P.; Murugan, A.; Minnaro, M.D.; Miller, M.; Guenther, F.; Kelly, M.E. CCQM K101 Final report international comparison CCQM-K101:Oxygen in nitrogen-a track B comparison and that the matrix contains argon This key comparison aims to assess the capabilities of the participants to determine the amount-of-substance fraction oxygen in nitrogen. The GAWG has classified this as a track B comparison, due to the unexpected 50 μmol/mol argon mole fraction content of the transfer standards, which effects the achievable performance of some measurement techniques such a GC-TCD. The separation of oxygen and argon is challenging, and not all systems in use are equally well designed for it. As this analytical challenge due to a substantial fraction of argon in the transfer standards became a reality, the Gas Analysis Working Group (GAWG) decided to qualify this key comparison as a regular key comparison and not as a core comparison, which may be used to support calibration and measurement capabilities (CMCs) for oxygen in nitrogen, or for oxygen in nitrogen mixtures containing argon only (see also the section on support to CMCs). IOP publishing BIPM 2016 Metrologia 53 Techn Suppl 08013, 1 71 2017-04-28 OPUS4-40015 Zeitschriftenartikel Konopelko, L.A.; Kolobova, A.V.; Rozhnov, M.S.; Melnyk, D.M.; Petryshyn, P.V.; Shpilnyi, S.A.; Iakubov, S.E.; Bakovec, N. V.; Kluchits, A.S.; Kipphardt, Heinrich; Aleksandrov, V. V. COOMET.QM-S5 (COOMET project № 576/RU/12) : "Supplementary comparison of national standards in the field of analysis of gas mixtures containing СО2, СО, С3Н8 in nitrogen ("automotive" gas mixtures)" The relevance of the COOMET.QM-S5 comparison is founded on tightening of requirements to a control of automobile emissions (realization of environmental standards of EURO 4, EURO-5). Participating laboratories: VNIIM, BAM, BelGIM, Ukrmetrteststandart, KazInMetr. This comparison was carried out in 2013-2014. This supplementary comparison supports CMC claims for: CO2 in the range (4-16) 10⁻² mol/mol; CO in the range (0.5-5) 10⁻² mol/mol; C3H8 in the range (0.01-0.3) 10⁻² mol/mol. Results: Component CO: All laboratories identified the values of carbon monoxide mole fraction in the gas mixture within ±0.9134%. Component CO2: All laboratories identified the values of carbon dioxide mole fraction in the gas mixture within ±0.3042%. Component C3H8: All laboratories identified the values of propane mole fraction in the gas mixture within ±0.443%. IOP publishing BIPM 2016 Metrologia 53 Technical Supplement Article 08004, 1 33 2017-04-28 OPUS4-47842 Zeitschriftenartikel Gonzales-Gago, C.; Smid, P.; Hofmann, T.; Venzago, C.; Hoffmann, V.; Gruner, W.; Pfeifer, Jens; Richter, Silke; Kipphardt, Heinrich Investigations of matrix independent calibration approaches in fast flow glow discharge mass spectrometry 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). London Royal Society of Chemistry 2019 JAAS 34 6 1109 1125 10.1039/c9ja00023b 2019-04-18 OPUS4-58868 Vortrag Kipphardt, Heinrich Introduction to Metrology in Chemistry Measurements are an important fundament of natural science in general and of chemical analysis in particular. Metrology is the science (and art) of performing measurements. The basic concepts and terms of metrology and their practical implementation are introduced. The very special peculiarities of chemical measurements that are absent in physical measurements are discussed. 2023 7th PhD Seminar of the German Working Group for Analytical Spectroscopy (DAAS) in the GDCh Division of Analytical Chemistry Berlin, Germany 15.11.2023 17.11.2023 2023-11-22 OPUS4-57005 Zeitschriftenartikel Lozano-Martín, D.; Tuma, Dirk; Kipphardt, Heinrich; Khanipour, Peyman; Chamorro, C. R. Thermodynamic characterization of the (H2 + C3H8) system significant for the hydrogen economy: Experimental (p, rho, T) determination and equation-of-state modelling For the gradual introduction of hydrogen in the energy market, the study of the properties of mixtures of hydrogen with typical components of natural gas (NG) and liquefied petroleum gas (LPG) is of great importance. This work aims to provide accurate experimental (p, rho, T) data for three hydrogen-propane mixtures with nominal compositions (amount of substance, mol/mol) of (0.95 H2 + 0.05 C3H8), (0.90 H2 + 0.10 C3H8), and (0.83 H2 + 0.17 C3H8), at temperatures of 250, 275, 300, 325, 350, and 375 K, and pressures up to 20 MPa. A single-sinker densimeter was used to determine the density of the mixtures. Experimental density data were compared to the densities calculated from two reference equations of state: the GERG-2008 and the AGA8-DC92. Relative deviations from the GERG-2008 EoS are systematically larger than those from the AGA8-DC92. They are within the ±0.5% band for the mixture with 5% of propane, but deviations are higher than 0.5% for the mixtures with 10% and 17% of propane, especially at low temperatures and high pressures. Finally, the sets of new experimental data have been processed by the application of two different statistical equations of state: the virial equation of state, through the second and third virial coefficients, B(T, x) and C(T, x), and the PC-SAFT equation of state. Amsterdam Elsevier B. V. 2023 International Journal of Hydrogen Energy 48 23 8645 8667 urn:nbn:de:kobv:b43-570056 10.1016/j.ijhydene.2022.11.170 https://creativecommons.org/licenses/by-nc-nd/4.0/deed.de 2023-02-20 OPUS4-58650 Vortrag Kipphardt, Heinrich MefHySto - Metrology for Advanced Hydrogen Storage Solutions An overview on the almost completed EMPIR-MefHySto-Project is given. 2023 Workshop on Green Hydrogen Montevideo, Uruguay 12.10.2023 12.10.2023 2023-10-26 OPUS4-57274 Zeitschriftenartikel Matschat, Ralf; Richter, Silke; Vogl, Jochen; Kipphardt, Heinrich On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10−4). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. Berlin Springer 2023 Analytical and bioanalytical chemistry 415 3057 3071 urn:nbn:de:kobv:b43-572743 10.1007/s00216-023-04660-4 https://creativecommons.org/licenses/by/4.0/deed.de 2023-04-05 OPUS4-59230 Vortrag Tiebe, Carlo; Mieller, Björn; Maiwald, Michael; Kipphardt, Heinrich; Tuma, Dirk; Prager, Jens; Schukar, Marcus; Strohhäcker, J. Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien Die Nutzung von Sensortechnologien, insbesondere im Bereich der Gasdetektion mit einem Schwerpunkt auf Wasserstoff, spielt eine entscheidende Rolle in verschiedenen Anwendungsbereichen der Wasserstofftechnologie. Sicherheitsüberwachung, Leckdetektion und Prozesskontrolle gehören zu den prominenten Anwendungsgebieten dieser Sensortechnologien. Ein zentrales Ziel ist die Erkennung von freigesetztem Wasserstoff sowie die genaue Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren. Dies ist von entscheidender Bedeutung, um potenzielle Gefahren frühzeitig zu erkennen und angemessene Maßnahmen zu ergreifen. Ein weiterer Schwerpunkt dieses Beitrags liegt auf der Analytik und der Verwendung zertifizierter Referenzmaterialien in Verbindung mit Metrologie für die Wasserstoffspeicherung. Dies gewährleistet eine präzise und zuverlässige Charakterisierung von Wasserstoff und unterstützt die Entwicklung sicherer Speichertechnologien. Im Rahmen des Euramet-Vorhabens Metrology for Advanced Hydrogen Storage Solutions (MefHySto) wird eine Kurzvorstellung präsentiert. Der Vortrag stellt zwei zerstörungsfreie Prüfverfahren zum strukturellen Zustandsüberwachung (Structural Health Monitoring, SHM) für Wasserstofftechnologien vor. Insbesondere die Fehlstellenerkennung mittels geführter Ultraschallwellen spielt eine bedeutende Rolle bei der Lebensdauerüberwachung von Wasserstoffspeichern. Ein weiterer Aspekt ist die Anwendung faseroptischer Sensorik zur Schadensfrüherkennung von Wasserstoffspeichern. Diese zerstörungsfreien Prüfverfahren ermöglichen eine präzise und frühzeitige Identifizierung von Schäden, was die Sicherheit und Effizienz von Wasserstoffspeichersystemen entscheidend verbessert. 2023 DVGW Kongress H2 Sicherheit Online meeting 15.11.2023 2023-12-28 OPUS4-58904 Zeitschriftenartikel Ziel, Ruben P.; Zalewska, Ewelina; van der Veen, Adriaan M. H.; Kipphardt, Heinrich; Tuma, Dirk; Esteban, Andres Rojo; Fernandez Vicente, Teresa Esperanza; Mace, Tatiana; Sutour, Christophe; Marioni, Fabrice; Fükö, Judit; Szücs, László; Büki, Tamás; Szilágyi Nagyné, Zsófia; Cieciora, Dariusz; Ochman, Grzegorz; Romanowski, Przemysław; Lis, Anna; Garnuszek, Magdalena; Valkova, Miroslava; Ackermann, Andreas; Pascale, Celine; Niederhauser, Bernhard; Tarhan, Tanil; Boztepe, Aylin; Beránek, Jan; Bárta, Miroslav International comparison EURAMET.QM-K3.2019 - Automotive exhaust gases EURAMET.QM-K3.2019 was a repeat of the key comparison EURAMET.QM-K3 on the composition of automotive exhaust gases. New in EURAMET.QM-K3.2019 was the addition of the amount fraction oxygen to the programme. The key comparison reference values were obtained independently, using static gravimetry and appropriate corrections from purity analysis and are linked to those of CCQM-K3.2019. The key comparison results show equivalence between the measurement standards maintained by the participating national metrology institutes. The demonstrated equivalence can be used to underpin services related to automotive exhaust gases as well as generically through the flexible scheme ("track A"). Bristol IOP Publishing 2023 Metrologia 60 1A 1 63 10.1088/0026-1394/60/1A/08030 2023-11-27