TY - JOUR A1 - Ostermann, Markus A1 - Berglund, M. A1 - Taylor, P. D. P. T1 - Measurement of the content of sulfur in gas oils using a high pressure asher, isotope dilution and thermal ionization mass spectrometry JF - Journal of analytical atomic spectrometry N2 - A new method has been developed for the measurement of sulfur in gas oils using a high pressure asher (HPA) for sample digestion. This, combined with a calibrated enriched isotopic reference material, and high precision mass spectrometry, makes it a powerful tool for an accurate and precise determination of the sulfur content in fossil fuels. The method described here was one of the methods used in the certification of the candidate reference materials BCR-104R, BCR-671 and BCR-672. Approximately 0.2 g of the gas oil samples were spiked with the spike isotopic reference material IRMM-646, which is enriched in 34S, and combusted in an HPA using nitric acid. The isotopes of sulfur were measured as arsenic monosulfides (AsS+) using a thermal ionization mass spectrometer equipped with a Faraday detector. The total uncertainty of the sulfur content (k = 2) is about 1%. The certified reference materials NIST SRM-2724b and NIST SRM-1619b and BCR-105 were used as part of the method validation work. The mass content of sulfur in BCR-104R was measured to be 1014 µg g-1, BCR-671 has 450 µg g-1 sulfur and BCR-672 shows a sulfur mass content of 201 µg g-1. The sulfur content of the candidate reference materials is homogeneous for the sample size used. KW - TIMS KW - Gas-oil KW - Reference materials KW - Isotope dilution KW - Sulfur PY - 2002 DO - https://doi.org/10.1039/B111140J SN - 0267-9477 SN - 1364-5544 VL - 17 IS - 10 SP - 1368 EP - 1372 PB - Royal Society of Chemistry CY - London AN - OPUS4-1214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ostermann, Markus A1 - Kettisch, P. A1 - Becker, Dorit A1 - Vogl, Jochen T1 - Measurements of sulfur in oil using pressurised wet digestion technique in open vessels and isotope dilution mass spectrometry JF - Analytical and bioanalytical chemistry KW - Wet digestion KW - Open vessel digestion KW - Sulfur in oil KW - Reference materials KW - TIMS KW - IDMS PY - 2003 UR - http://www.springerlink.com/content/b7alk8lgly2v/?p=6237db8a9c28481d87e7b017e6474b73&pi=88 SN - 1618-2642 SN - 1618-2650 VL - 377 IS - 4 SP - 779 EP - 783 PB - Springer CY - Berlin AN - OPUS4-2738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hearn, R. A1 - Berglund, M. A1 - Ostermann, Markus A1 - Pusticek, N. A1 - Taylor, P.D.P. T1 - A comparison of high accuracy isotope dilution techniques for the measurement of low level sulfur in gas oils JF - Analytica chimica acta N2 - A comparison of high accuracy methods for the analysis of total sulfur in gas oils by three metrology institutes is described. The work contains a comparison of three different aspects of the analysis: sample digestion, instrumental measurement and isotope dilution strategies. Thermal ionisation mass spectrometry (TIMS) in combination with high pressure asher (HPA) or Carius tube digestion has traditionally been used for such high accuracy analysis. However, this paper demonstrates that the faster, less laborious technique of ICP-MS in combination with microwave digestion is equally capable. Results from the comparison experiments show excellent agreement for fuel samples containing sulfur concentrations in the range 11–200 µg g-1. This excellent agreement across the different sample preparation, measurement and isotope dilution techniques has been exploited in the certification of two new diesel fuel reference materials. KW - Sulfur KW - Gas oil KW - Isotope dilution KW - ICP-MS KW - TIMS KW - Uncertainty PY - 2005 DO - https://doi.org/10.1016/j.aca.2004.10.070 SN - 0003-2670 SN - 1873-4324 SN - 0378-4304 VL - 532 IS - 1 SP - 55 EP - 60 PB - Elsevier CY - Amsterdam AN - OPUS4-7280 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 JF - International Journal of Mass Spectrometry 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 DO - 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 -