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 - Vogl, Jochen A1 - Ostermann, Markus T1 - On the measurement of the moisture content in different matrix materials JF - Accreditation and quality assurance N2 - Twelve different samples were analyzed for their water content by the classical oven-drying method and a commercial moisture analyzer. Nominal values have been set by Karl Fischer titration and gravimetry. The decomposition during the drying process of samples containing organic compounds was checked by thermogravimetry coupled with Fourier transform infrared spectrometric and mass spectrometric detection. Summarizing all measurement results, the commercial moisture analyzer demonstrated an average bias for the determination of water contents, which is much smaller than the stated uncertainty and thus is negligible. Compared to the classical oven-drying method, the commercial moisture analyzer shows a smaller bias, more ease in handling and less time consumption per analysis. When validated by a reference procedure like Karl Fischer titration the commercial moisture analyzer is the method of choice for routine analysis. KW - Classical oven-drying KW - Commercial moisture analyzer KW - Karl Fischer titration KW - Moisture KW - Reference materials KW - Thermogravimetry KW - Matrix samples PY - 2006 DO - https://doi.org/10.1007/s00769-006-0159-z SN - 0949-1775 SN - 1432-0517 VL - 11 IS - 7 SP - 356 EP - 362 PB - Springer CY - Berlin AN - OPUS4-12638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -