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 - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification report for the reference materials ERM-AE140 and ERM-AE141 - Pd and Pt single spikes certified for their Pd and Pt mass fraction and isotopic composition N2 - Isotope dilution mass spectrometry often is applied for the quantification of platinum group elements in environmental and geological samples. In most cases, however, certified spike solutions offering complete uncertainty statements and SI-traceability are missing. This report describes the production and certification of two isotope reference materials, ERM-AE140 and ERM-AE141, serving as calibrated spike solutions for IDMS based quantification of Pd and Pt, respectively. Both materials were produced by dissolving highly enriched isotopes 106Pd and 194Pt and determining the mass fraction of 106Pd and 194Pt in the final solution by reverse IDMS. Two independent back-spikes were produced for each material from high purity Pd and Pt. Characterization measurements were carried out by MC-ICPMS. For ERM-AE140 the certified mass fractions are w(106Pd) = 20.24(5) mg/kg and w(Pd) = 20.54(5) mg/kg. For ERM-AE141 the certified mass fractions are w(194Pt) = 18.18(11) mg/kg and w(Pt) = 19.90(12) mg/kg. These values are traceable to the International System of Units (SI) in the shortest possible way. KW - Palladium KW - Enriched isotope KW - Platinum KW - Spike KW - IDMS PY - 2015 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-355833 SP - 1 EP - 25 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -