Dokument-ID Dokumenttyp Autoren/innen Persönliche Herausgeber/innen Haupttitel Abstract Auflage Verlagsort Verlag Herausgeber (Institution) Erscheinungsjahr Titel des übergeordneten Werkes Jahrgang/Band ISBN Veranstaltung Veranstaltungsort Beginndatum der Veranstaltung Enddatum der Veranstaltung Ausgabe/Heft Erste Seite Letzte Seite URN DOI Lizenz Datum der Freischaltung OPUS4-7280 Zeitschriftenartikel Hearn, R.; Berglund, M.; Ostermann, Markus; Pusticek, N.; Taylor, P.D.P. A comparison of high accuracy isotope dilution techniques for the measurement of low level sulfur in gas oils 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. Amsterdam Elsevier 2005 Analytica chimica acta 532 1 55 60 10.1016/j.aca.2004.10.070 2016-02-19 OPUS4-16371 Zeitschriftenartikel Linsinger, T.; Andrzejuk, W.; Bau, A.; Charoud-Got, J.; De VOs, P.; Emteborg, H.; Hearn, R.; Lamberty, A.; Oostra, A.; Pritzkow, Wolfgang; Quétel, C.; Roebben, G.; Tresl, I.; Vogl, Jochen; Wood, S. Production of three certified reference materials for the sulfur content in gasoline (petrol) 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. Washington, DC ACS Publ. American Chemical Society (ACS) 2007 Energy and Fuels 21 4 2240 2244 10.1021/ef070155t 2016-02-19 OPUS4-10905 Zeitschriftenartikel Sturgeon, R. E.; Wahlen, R.; Brandsch, T.; Fairman, B.; Wolf-Briche, C.; Alonso, J. I. G.; González, P. R.; Encinar, J. R.; Sanz-Medel, A.; Inagaki, K.; Takatsu, A.; Lalere, B.; Monperrus, M.; Zuloaga, O.; Krupp, E.; Amouroux, D.; Donard, O. F. X.; Schimmel, H.; Sejeroe-Olsen, B.; Konieczka, P.; Schultze, P.; Taylor, P.; Hearn, R.; Mackay, L.; Myors, R.; Win, Tin; Liebich, Almuth; Philipp, Rosemarie; Yang, L.; Willie, S. Determination of tributyltin in marine sediment: Comité Consultatif pour la Quantité de Matière (CCQM) pilot study P-18 international intercomparison The capabilities of National Metrology Institutes (NMIs—those which are members of the Comité Consultatif pour la Quantité de Matière (CCQM)of the CIPM) and selected outside "expert" laboratories to quantitate (C4H9)3Sn+ (TBT) in a prepared marine sediment were assessed. This exercise was sanctioned by the 7th CCQM meeting, April 4–6, 2001, as an activity of the Inorganic Analysis Working Group and was jointly piloted by the Institute for National Measurement Standards of the National Research Council of Canada (NRC) and the Laboratory of the Government Chemist (LGC), UK. A total of 11 laboratories submitted results (7 NMIs, and 4 external labs). Two external laboratories utilized a standard calibration approach based on a natural abundance TBT standard, whereas all NMIs relied upon isotope dilution mass spectrometry for quantitation. For this purpose, a species specific 117Sn-enriched TBT standard was supplied by the LGC. No sample preparation methodology was prescribed by the piloting laboratories and, by consequence, a variety of approaches was adopted by the participants, including mechanical shaking, sonication, accelerated solvent extraction, microwave assisted extraction and heating in combination with Grignard derivatization, ethylation and direct sampling. Detection techniques included ICP–MS (with GC and HPLC sample introduction), GC–MS, GC–AED and GC–FPD. Recovery of TBT from a control standard (NRCC CRM PACS-2 marine sediment) averaged 93.5±2.4% (n=14). Results for the pilot material averaged 0.680±0.015 µmol kg–1 (n=14; 80.7±1.8 µg kg–1) with a median value of 0.676 µmol kg–1. Overall, performance was substantially better than state-of-the-art expectations and the satisfactory agreement amongst participants permitted scheduling of a follow-up Key comparison for TBT (K-28), a Pilot intercomparison for DBT (P-43), and certification of the test sediment for TBT content and its release as a new Certified Reference Material (HIPA-1) with a TBT content of 0.679±0.089 µmol kg–1 (expanded uncertainty, k=2, as Sn) (80.5±10.6 µg kg–1). Electronic Supplementary Material Supplementary material is available in the online version of this article at http://dx.doi.org/10.1007/s00216-003-2016-9. Berlin Springer 2003 Analytical and bioanalytical chemistry 376 6 780 787 10.1007/s00216-003-2016-9 2016-02-19 OPUS4-20787 Zeitschriftenartikel Ma, L.; Feng, L.; Hioki, A.; Cho, K.H.; Vogl, Jochen; Berger, Achim; Turk, G.; Macleod, S.; Labarraque, G.; Tong, W.F.; Schiel, D.; Yafa, C.; Valiente, L.; Konopelko, L.A.; Quetel, C.; Vermaercke, P.; Manzano, J.V.L.; Linsky, M.; Cortés, E.; Tangpitayakul, S.; Plangsangmas, L.; Bergamaschi, L.; Hearn, R. International comparison of the determination of the mass fraction of cadmium, chromium, mercury and lead in polypropylene: the Comité Consultatif pour la quantité de matière pilot study CCQM-P106 Berlin Springer 2010 Accreditation and quality assurance 15 1 39 44 10.1007/s00769-009-0574-z 2016-02-19 OPUS4-35580 Forschungsbericht Andrzejuk, W.; Bau, A.; Charoud-Got, J.; de Vos, P.; Emteborg, H.; Lamberty, A.; Linsinger, T.; Oostra, A.; Quetel, C.; Roebben, G.; Tresl, I.; Hearn, R.; Wood, S.; Pritzkow, W.; Vogl, Jochen Certification of the sulfur mass fraction in three commercial petrol materials - Certified reference materials ERM-EF211, ERM-EF212 and ERM-EF213 Three petrol reference materials were certified for their total sulfur content in support of Directive 2003/17/EC of the European Parliament and of the European Council, which stipulates that petrol with a maximum S content of 10 mg/kg must be available in all member states by 2009. Commercially available petrol was obtained and filled into borosilicate ampoules without further treatment. Homogeneity of the materials was tested and no heterogeneity was detected for two of the materials, whereas minor heterogeneity was observed for the third material. Stability of the materials was tested for 8-12 months at 60 °C and no degradation was observed. Characterisation was based on isotope-dilution mass spectrometry (IDMS) applied as primary method of measurement by three European metrology institutes and certified values were assigned using all results. The certified uncertainties include contributions of (potential) heterogeneity, potential degradation as well as characterisation. The final assigned values are: ERM-EF211: 48.8 ± 1.7 mg/kg ERM-EF212: 20.2 ± 1.1 mg/kg ERM-EF213: 9.1 ± 0.8 mg/kg The materials are available from IRMM (ERM-EF211), LGC (ERM-EF212) and BAM (ERMEF213) Luxembourg European Communities 2007 978-92-79-05370-2 1 37 urn:nbn:de:kobv:b43-355804 http://www.gesetze-im-internet.de/urhg/index.html 2016-03-29