TY - JOUR A1 - Knobbe, N. A1 - Vogl, Jochen A1 - Pritzkow, Wolfgang A1 - Panne, Ulrich A1 - Fry, H. A1 - Lochotzke, H.M. A1 - Preiss-Weigert, A. T1 - C and N stable isotope variation in urine and milk of cattle depending on the diet N2 - The stable carbon and nitrogen isotopic composition of urine and milk samples from cattle under different feeding regimes were analysed over a period of six months. The isotope ratios were measured with isotope ratio mass spectrometry (IRMS). The δ13C values of milk and urine were dependent on different feeding regimes based on C3 or C4 plants. The δ13C values are more negative under grass feeding than under maize feeding. The δ13C values of milk are more negative compared to urine and independent of the feeding regime. Under grass feeding the analysed milk and urine samples are enriched in 13C relative to the feed, whereas under maize feeding the 13C/12C ratio of urine is in the same range and milk is depleted in 13C relative to the diet. The difference between the 15N/14N ratios for the two feeding regimes is less pronounced than the 13C/12C ratios. The δ15N values in urine require more time to reach the new equilibrium, whereas the milk samples show no significant differences between the two feeding regimes. KW - Cattle KW - Urine KW - Milk KW - Feeding regime KW - Stable isotope PY - 2006 U6 - https://doi.org/10.1007/s00216-006-0644-6 SN - 1618-2642 SN - 1618-2650 VL - 386 IS - 1 SP - 104 EP - 108 PB - Springer CY - Berlin AN - OPUS4-12746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Rosner, Martin A1 - Pritzkow, Wolfgang T1 - Development and validation of a single collector SF-ICPMS procedure for the determination of boron isotope ratios in water and food samples N2 - Boron isotope studies on technical materials and geological and environmental samples are one hot topic in nowadays isotope research. Provenance studies of artefacts, food and other products might become another one, as several recent studies demonstrate. Typically boron isotope determinations have been carried out by TIMS. To open up this research field to a broader scientific community we developed two analytical procedures for boron isotope determinations based on single collector SF-ICPMS combined with a sample preparation procedure consisting of dry-ashing and a three step ion chromatographic boron-matrix separation. The developed procedures consist of one low resolution (LR) and one medium resolution (MR) procedure. The repeatability for the δ11B determination in three independently measured aliquots lies between 0.2 and 0.8‰ for the LR procedure and between 0.3 and 1.5‰ for the MR procedure. The expanded uncertainties with a coverage factor of k=2 range between 1.4 and 1.6‰ for the LR procedure and between 2.9 and 3.2‰ for the MR procedure. The accuracy, expressed as average deviation from the reference values, is 0.43‰ for the LR procedure and 0.33‰ for the MR procedure. To test the practicability of the procedures the matrix tolerance has been investigated as well and was found to be up to 2 mg kg-1 of alkaline and alkaline earth elements in the final measurement solution containing 100 µg kg-1 boron. Thus a highly efficient matrix separation for SF-ICPMS boron isotope determinations is required, similar to TIMS. PY - 2011 U6 - https://doi.org/10.1039/c0ja00220h SN - 0267-9477 SN - 1364-5544 VL - 26 IS - 4 SP - 861 EP - 869 PB - Royal Society of Chemistry CY - London AN - OPUS4-23419 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 - 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 - 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 - Bohn, T. A1 - Walczyk, Th. A1 - Davidsson, L. A1 - Pritzkow, Wolfgang A1 - Klingbeil, Patrick A1 - Vogl, Jochen A1 - Hurrell, R.F. T1 - Comparison of urinary monitoring, faecal monitoring and erythrocyte analysis of stable isotope labels to determine magnesium absorption in human subjects KW - Magnesium absorption KW - Stable isotopes KW - Faecal monitoring KW - Urinary monitoring KW - Erythrocytes PY - 2004 SN - 0007-1145 SN - 1475-2662 VL - 58 SP - 113 EP - 120 PB - CABI Publ. CY - Wallingford AN - OPUS4-3362 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 - Vogl, Jochen A1 - Pritzkow, Wolfgang A1 - Klingbeil, Patrick T1 - The need for new SI-traceable magnesium isotopic reference materials KW - Isotopic Reference Material KW - Multi-collector ICP-MS KW - Isotopic abundance variations KW - Primary Isotopic Reference Material KW - Magnesium PY - 2004 U6 - https://doi.org/10.1007/s00216-004-2859-8 SN - 1618-2642 SN - 1618-2650 VL - 380 SP - 876 EP - 879 PB - Springer CY - Berlin AN - OPUS4-6904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Paz, B. A1 - Koenig, Maren A1 - Pritzkow, Wolfgang T1 - A modified lead-matrix separation procedure shown for lead isotope analysis in Trojan silver artefacts as an example N2 - A modified Pb–matrix separation procedure using NH4HCO3 solution as eluent has been developed and validated for determination of Pb isotope amount ratios by thermal ionization mass spectrometry. The procedure is based on chromatographic separation using the Pb·Spec resin and an in-house-prepared NH4HCO3 solution serving as eluent. The advantages of this eluent are low Pb blanks (<40 pgmL-1) and the property that NH4HCO3 can be easily removed by use of a heating step (>60 °C). Pb recovery is >95 % for water samples. For archaeological silver samples, however, the Pb recovery is reduced to approximately 50 %, but causes no bias in the determination of Pb isotope amount ratios. The validated procedure was used to determine lead isotope amount ratios in Trojan silver artefacts with expanded uncertainties (k=2) <0.09 %. KW - Analyte-matrix separation KW - Mass spectrometry KW - Pb isotope ratio thermal ionization mass spectrometry KW - Archaeometry PY - 2013 U6 - https://doi.org/10.1007/s00216-012-6323-x SN - 1618-2642 SN - 1618-2650 VL - 405 IS - 9 SP - 2995 EP - 3000 PB - Springer CY - Berlin AN - OPUS4-28170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -