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- 2015 (19) (entfernen)
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- Vortrag (10)
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- IDMS (3)
- Palladium (3)
- Platinum (3)
- Automotive exhaust emissions (2)
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- Boron isotopes (1)
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- Cationic exchange (1)
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Eingeladener Vortrag
- nein (10)
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.
Measurement strategies
(2015)
Designing an appropriate measurement strategy for a particular analytical question is not always obvious, since a number of factors have to be considered, whereby some of them might be difficult to define. A set of key questions generally precede the experimental design in analytical measurements and help to choose the measurement strategy, which is fit for the intended use – in the particular case of the content of this book – either for quantification, elemental ratio or isotope ratio analyses, accordingly.
Thermal ionisation, also known as surface ionisation, was one of the first ionisation techniques developed for mass spectrometry, having been invented as early as 1918. The ionization process, described by the empirically derived “fractionation laws”, is widely understood. Isotope ratio measurements can be achieved with high precision and accuracy. Due to this, thermal ionisation has paved the way for great scientific achievements including: the discovery of new isotopes, the determination of radioactive half-lives and atomic weights of the elements, the accurate determination of the age of the earth and investigations on human society in the past such as mobility and trade. TIMS is still regarded as ‘golden standard’ in isotope ratio measurements. Thus the method is a reference technique that remains at the forefront of isotopic analysis particularly in the fields of metrology. A concise overview is given here of the technical background of thermal ionisation as well as the numerous applications of this technique in earth sciences, industry, metrology, and nuclear forensics.
CCQM-P149 - Purity determination of zinc to be used as primary standard for zinc determination
(2015)
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 dessais, 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.