TY - JOUR A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen A1 - Berger, Achim A1 - Ecker, Klaus A1 - Grötzschel, R. A1 - Klingbeil, Patrick A1 - Persson, L. A1 - Riebe, Gundel A1 - Wätjen, U. T1 - Contribution of ICP-IDMS to the certification of antimony implanted in a silicon wafer - comparison with RBS and INAA results N2 - A thin-layer reference material for surface and near-surface analytical methods was produced and certified. The surface density of the implanted Sb layer was determined by Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA), and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) equipped with a multi-collector. The isotopic abundances of Sb (121Sb and 123Sb) were determined by multi-collector ICP-MS and INAA. ICP-IDMS measurements are discussed in detail in this paper. All methods produced values traceable to the SI and are accompanied by a complete uncertainty budget. The homogeneity of the material was measured with RBS. From these measurements the standard uncertainty due to possible inhomogeneities was estimated to be less than 0.78% for fractions of the area increments down to 0.75 mm2 in size. Excellent agreement between the results of the three different methods was found. For the surface density of implanted Sb atoms the unweighted mean value of the means of four data sets is 4.8121016 cm-2 with an expanded uncertainty (coverage factor k=2) of 0.0921016 cm-2. For the isotope amount ratio R (121Sb/123Sb) the unweighted mean value of the means of two data sets is 1.435 with an expanded uncertainty (coverage factor k=2) of 0.006. KW - ICP-MS KW - IDMS KW - Reference material KW - Surface analysis PY - 2001 U6 - https://doi.org/10.1007/s002160100987 SN - 0937-0633 VL - 371 SP - 867 EP - 873 PB - Springer CY - Berlin AN - OPUS4-7220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klingbeil, Patrick A1 - Vogl, Jochen A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Müller, J. T1 - Comparative studies on the certification of reference materials by ICPMS and TIMS using isotope dilution procedures N2 - A comparison of different isotope dilution mass spectrometric (IDMS) procedures using inductively coupled plasma mass spectrometry (ICPMS) and thermal ionization mass spectrometry (TIMS) was carried out to examine the degree of equivalence between the used procedures in terms of requirements for reference material certification. The comparison was based on the measurement results and their uncertainties. The sample used in this study is a pure zinc metal to be certified by the Bureau Communie de Référence (BCR) for amount contents of different trace elements. This study focuses on cadmium and thallium. The TIMS values contributed to the certified values. To guarantee identical conditions as far as possible for the procedures under investigation, the samples were split into subsamples after spiking and digestion took place. Thus, every IDMS procedure started with an identical set of samples. In total, four different IDMS procedures and one external calibration procedure using internal standardization as an example of routine analysis were applied. The IDMS procedures divide in a group with and a group without trace/matrix separation. Multicollector TIMS (TI-MC-MS) and multicollector ICPMS (ICP-MC-MS) were used in combination with trace/matrix separation, whereas quadrupole ICPMS (ICP-QMS) and ICP-MC-MS were also applied to nonseparated samples. All IDMS results agree well within their combined uncertainties, while some results from the external calibration procedure do not. IDMS results obtained by ICPMS without separation are comparable to those obtained by TI-MC-MS with separation regarding precision and accuracy. The smallest uncertainties were achieved using ICP-MC-MS in combination with trace/matrix separation. KW - ICP-MS KW - TIMS KW - IDMS KW - multi-collector KW - uncertainty budget KW - Certification KW - reference material PY - 2001 U6 - https://doi.org/10.1021/ac001278c SN - 0003-2700 SN - 1520-6882 VL - 73 IS - 8 SP - 1881 EP - 1888 PB - American Chemical Society CY - Washington, DC AN - OPUS4-909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Pritzkow, Wolfgang T1 - Isotope dilution mass spectrometry - a primary method of measurement and its role for RM certification KW - IDMS KW - Reference materials KW - Metrology KW - ICPMS KW - TIMS PY - 2010 SN - 0970-3950 VL - 25 IS - 3 SP - 135 EP - 164 PB - Metrology Society of India CY - New Delhi AN - OPUS4-22603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel T1 - Development of reference procedures for the quantification of toxic metals and S in plastics N2 - The quantitative analysis of toxic metals in plastics is very important for different sectors of industry and daily life. Many routine procedures have been established based on X-ray fluorescence or inductively coupled plasma atomic emission spectrometry. However, all of them require suitable reference materials to calibrate or validate. These reference materials ideally are being certified by reference procedures. The development of such reference procedures for sulfur and the four toxic elements cadmium, chromium, mercury and lead in plastics is described here. The procedures are based on double isotope dilution mass spectrometry including analyte–matrix separation. The applied mass spectrometric techniques are thermal ionization mass spectrometry as well as inductively coupled plasma mass spectrometry. Memory effects of mercury and dissolution of chromium(III) oxide have been considered especially. The expanded uncertainties have been improved from the percent range down to the per mill range during the development of the procedure from the early analysis of BCR-680/681 to the recent analysis of CCQM-P106. With the fully developed procedures expanded uncertainties (k = 2) between 0.1 and 0.4% for cadmium, chromium, lead and sulfur and around 1% for mercury can be achieved. The so developed procedures have been successfully applied to the certification of reference materials as well as to intercomparisons organized by CCQM. KW - ICPMS KW - TIMS KW - Reference materials KW - IDMS PY - 2010 U6 - https://doi.org/10.1039/c0ja00034e SN - 0267-9477 SN - 1364-5544 VL - 25 IS - 10 SP - 1633 EP - 1642 PB - Royal Society of Chemistry CY - London AN - OPUS4-22044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudek, Gabriele A1 - Alber, D. A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Vogl, Jochen A1 - Görner, Wolf T1 - Determination of the beta- branching ratio of 64Cu by mass spectrometric investigations of the decay products in neutron transmuted copper N2 - The ?- branching ratio of 64Cu was determined by investigating the resulting decay products in copper doped by neutron transmutation. The numbers of 64Zn and 64Ni atoms were analyzed using isotope dilution analysis combined with thermal ionization mass spectrometry. A ?- branching ratio of (38.06±0.30)% was obtained, which agrees with the study of Kawada (Appl. Radiat. Isot. 37 (1) (1986) 7) to a higher accuracy. However, our result differs from the value cited in the NUDAT database of (39.0±0.3)%. KW - NTD KW - Copper KW - Zinc KW - Nickel KW - Branching ratio KW - Cu-64 KW - TIMS KW - IDMS KW - Isotope dilution KW - Thermal ionization mass spectrometry KW - Neutron transmutation doping PY - 2002 U6 - https://doi.org/10.1016/S0969-8043(01)00180-4 SN - 0883-2889 SN - 0969-8043 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. VL - 56 SP - 145 EP - 151 PB - Elsevier CY - Amsterdam AN - OPUS4-7221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen A1 - Köppen, Robert A1 - Ostermann, Markus T1 - Determination of sulfur isotope abundance ratios for SI-traceable low sulfur concentration measurements in fossil fuels by ID-TIMS N2 - The present work describes the development of an existing TIMS procedure to a reference procedure for low sulfur concentration measurements in fossil fuels. With this enhanced procedure SI-traceable sulfur mass fractions below 10 mg kg-1 can be obtained. The achieved detection limit is approximately 0.2 mg kg-1. The procedure was validated by certified reference materials. The procedure was already applied to candidate reference materials and to samples analysed within projects of the “Comité Consultatif pour la Quantité de Matière – CCQM”. Additionally the influence of the isotopic composition on the results and its corresponding uncertainty was studied. Reference data published in the literature on the isotopic composition of sulfur were assessed. KW - TIMS KW - IDMS KW - Low sulfur KW - Fossil fuel KW - Reference procedure PY - 2005 U6 - https://doi.org/10.1016/j.ijms.2004.10.024 SN - 0168-1176 SN - 0020-7381 SN - 1387-3806 SN - 1873-2798 VL - 242 SP - 309 EP - 318 PB - Elsevier CY - Amsterdam AN - OPUS4-7222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linsinger, T. A1 - Andrzejuk, W. A1 - Bau, A. A1 - Charoud-Got, J. A1 - De VOs, P. A1 - Emteborg, H. A1 - Hearn, R. A1 - Lamberty, A. A1 - Oostra, A. A1 - Pritzkow, Wolfgang A1 - Quétel, C. A1 - Roebben, G. A1 - Tresl, I. A1 - Vogl, Jochen A1 - Wood, S. T1 - Production of three certified reference materials for the sulfur content in gasoline (petrol) N2 - Directive 2003/17/EC of the European Parliament and the European Council stipulates that petrol (gasoline) with a total sulfur content below 10 mg kg-1 must be available in all European Union member states by 2009. Three certified reference materials were produced in support of this directive in a joint effort of the members of the European Reference Materials Initiative (ERM). Two of the materials were made from commercial petrol, while the third one was prepared from a blend of commercial petrols. Relative between-ampule heterogeneity of the materials was quantified and found to be below 2.5%. Potential degradation during storage and dispatch was quantified, and shelf lives based on these values were set. The three materials were characterized by three institutes using different variants of isotope-dilution mass spectrometry. The results from the three institutes were combined, and the final uncertainties of the respective sulfur mass fractions were estimated including contributions from heterogeneity, stability, and characterization. The following mass fractions were derived: ERM-EF211, 48.8 ± 1.7 mg kg-1; ERM-EF212, 20.2 ± 1.1 mg kg-1; and ERM-EF213, 9.1 ± 0.8 mg kg-1. KW - CRM KW - IDMS KW - ERM PY - 2007 U6 - https://doi.org/10.1021/ef070155t SN - 0887-0624 SN - 1520-5029 VL - 21 IS - 4 SP - 2240 EP - 2244 PB - ACS Publ. CY - Washington, DC AN - OPUS4-16371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -