TY - JOUR A1 - Dudek, Gabriele A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel A1 - Görner, Wolf A1 - Alber, D. T1 - Characterization of neutron transmuted zinc traces in pure copper materials by isotope dilution mass spectrometry N2 - The neutron transmutation doping (NTD) of highly pure copper with zinc was investigated as a promising means of achieving controlled gradation of the zinc content in the range 1-20 wg g-1. The doping process leads to the enrichment of two stable isotopes 64Zn and 66Zn in a ratio which differs from that of natural isotopic distribution. Mass spectrometric investigations by thermal ionization mass spectrometry (TIMS) were performed to validate the results obtained by gamma spectrometry. The investigations included both determination of the isotopic ratios of the doped zinc isotopes and the analysis of the accumulated zinc contents by isotope dilution (ID) analysis. Thereby a sample-specific correction of the blank could be performed because the isotope 68Zn was not influenced, because of the transmutation process. The results obtained by TIMS prove the strict proportionality of the doped zinc content, in the range 5 to 20 wg g-1, to the neutron fluence. Comparison with gamma spectrometric results showed a very good agreement within the uncertainties. PY - 2001 U6 - https://doi.org/10.1007/s002160100784 SN - 0937-0633 N1 - Geburtsname von Dudek, Gabriele: Wermann, G. - Birth name of Dudek, Gabriele: Wermann, G. VL - 370 IS - 5 SP - 606 EP - 611 PB - Springer CY - Berlin AN - OPUS4-1145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riebe, Gundel A1 - Ostermann, Markus A1 - Pritzkow, Wolfgang A1 - Vogl, Jochen T1 - Combination of sophisticated sample digestion methods and highly accurate determination procedures shown for Sulphur in oil and Cadmium and Lead in sediment T2 - Internationale Konferenz "Trends in Sample Preparation 2002" CY - Seggau, Austria DA - 2002-06-30 PY - 2002 AN - OPUS4-1398 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 - 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 - 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 - 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 - Vogl, Jochen A1 - Klingbeil, Patrick A1 - Pritzkow, Wolfgang A1 - Riebe, Gundel T1 - High accuracy measurements of Fe isotopes using hexapole collision cell MC-ICP-MS and isotope dilution for certification of reference materials N2 - An ICP-MS equipped with collision cell, sector field and multi-collector technology has been applied to developing analytical procedures for Fe in terms of isotope ratio measurements and isotope dilution analysis. Therefore a detailed study on the reduction of molecular interferences by a variety of collision gases (He, Ar, Kr, H2, D2 and N2) was performed. The efficiency of the reduction has been checked by high resolution mass scans. The argon based interferences disturbing the determination of 54Fe and 56Fe could be completely removed when using Faraday detectors. The interferences on mass 57 could be reduced to a level which enables accurate measurements. Also, the 40Ar12C interference, which disturbs the chromium correction, could be completely removed. Reproducibilities of 0.01% could be reached for 54Fe/56Fe isotope ratios and 0.02% for 57Fe/56Fe isotope ratios. Under these measurement conditions a sensitivity of 1.2 V per 50 µg kg–1 Fe is available. This corresponds to 1.5 × 109 cps per mg kg–1. Based on these results highly accurate procedures for Fe isotope ratio determinations were set up, reaching a performance level superior to that of other ICP-MS instruments. Consequently, IDMS procedures were developed on this basis in order to perform certification measurements at the highest metrological level. The first application was the contribution to the Fe reference value by IMEP-12, an interlaboratory comparison with approximately 350 participants worldwide. The analysed Fe mass content is 0.2150 mg kg–1 with its expanded uncertainty (k= 2) of 0.0012 mg kg–1(0.56%), which is ten times less than the uncertainty of the second certification laboratory. Another application was the certification campaign of the two reference materials Tea Leaves and Polish Herbs. The results obtained with the ICP-MS procedure, 542 ± 11 mg kg–1 and 543 ± 12 mg kg–1, were compared with the results analysed by TIMS, 541 ± 12 mg kg–1 and 541 ± 13 mg kg–1, and agree very well within the stated uncertainties (k= 2). The results presented demonstrate quite well the suitability of the developed IDMS procedures for certification or reference measurements. PY - 2003 U6 - https://doi.org/10.1039/b301812a SN - 0267-9477 SN - 1364-5544 VL - 18 SP - 1125 EP - 1132 PB - Royal Society of Chemistry CY - London AN - OPUS4-2739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -