TY - JOUR A1 - Vogl, Jochen A1 - Meyer, Christian A1 - Koenig, Maren A1 - Becker, Dorit A1 - Noordmann, J. A1 - Rienitz, O. A1 - Mamakos, A. A1 - Riccobono, F. T1 - A new two-stage separation procedure for the IDMS based quantification of low Pd and Pt amounts in automotive exhaust emissions N2 - A two-step separation procedure for the quantification of Pd and Pt in automotive exhaust emissions using isotope dilution mass spectrometry was established using a combination of cation and anion exchange chemistry. AG 50W-X12 was used as cation exchange resin and DGA as weakly basic anion exchange resin. This procedure enabled the effective separation of Pd and Pt from the matrix and from interfering elements. Additionally Pd and Pt were collected in separate chromatographic fractions, which increased the precision of the isotope ratio determination by separate measurements using single collector sector field ICPMS. The analytical procedure was validated by analysing the synthetically prepared samples and the certified reference materials BCR-723 (road dust) and IAEA-450 (algae). For the SI-traceable results complete uncertainty budgets were calculated yielding relatively expanded uncertainties (k = 2) of ≈1% for analyte masses in the ng range. Procedure blanks of 55 pg Pd and 3 pg Pt were obtained. The detection limits were calculated as 12 pg for Pd and 7 pg for Pt. Additionally, Pd and Pt blank levels of different filter materials are presented as well as the first results for automotive exhaust particles collected on cellulose filters. KW - Palladium KW - Platinum KW - Automotive exhaust emissions KW - IDMS PY - 2015 U6 - https://doi.org/10.1039/c4ja00251b SN - 0267-9477 SN - 1364-5544 VL - 30 IS - 2 SP - 479 EP - 486 PB - Royal Society of Chemistry CY - London AN - OPUS4-32539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Labarraque, G. A1 - Oster, C. A1 - Fisicaro, P. A1 - Meyer, Christian A1 - Vogl, Jochen A1 - Noordmann, J. A1 - Rienitz, O. A1 - Riccobono, F. A1 - Donet, S. T1 - Reference measurement procedures for the quatification of platinum-group elements (PGEs) from automotive exhaust emissions N2 - The major source of the anthropogenic platinum group element (PGE) emission is attributed to the use of catalytic converters in automobiles. This paper describes the work performed by three National Metrology Institutes (Laboratoire national de métrologie et d’essais, by the Physikalisch-technische bundesanstalt, Bundesanatalt für materialforschung und prûfung), in the framework of the Joint Research Project 'PartEmission' under the European Metrology Research Program. An analytical procedure based on a cationic exchange protocol and the isotope dilution or standard addition using an Inductived Coupled Plasma Mass Spectrometer, ICP-MS, for the quantification of the elements Pt, Pd and Rh from automotive exhaust emissions is described. Results obtained on a road dust certified reference (BCR 723) material showed a good agreement with the certified values, at ng/g levels, and relative expanded uncertainties within the range of 7–10%. Analysis of filters impacted with automotive exhaust particle emissions (from a diesel engine) showed the amount of collected PGE at levels of 10–1000 pg/filter. Their quantifications followed the developed analytical protocol that had been carried out with relative expanded uncertainties in the range of a few per cent up to 20% per filter. Nevertheless, a lack of homogeneity between the filters was observed, making the comparison between the project partners difficult in the sake of the validation of their analytical procedures on real samples. KW - Automotive pollution KW - Catalytic converters KW - Platinum group elements (PGE) KW - ICP-MS KW - Isobaric interferences KW - Cationic exchange KW - Reference measurement procedures KW - Double isotope dilution KW - Palladium KW - Platinum KW - Automotive exhaust emissions KW - IDMS PY - 2015 U6 - https://doi.org/10.1080/03067319.2015.1058931 SN - 0306-7319 SN - 1029-0397 SN - 0092-9085 VL - 95 IS - 9 SP - 777 EP - 789 PB - Gordon and Breach CY - New York, NY AN - OPUS4-34015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -