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SI-traceable certification of Cu, Cr, Cd and Pb in sediment and fly ash candidate reference materials

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Journal of Environmental Monitoring Vol - 2 Issue - 5

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SI-traceable certification of Cu, Cr, Cd and Pb in sediment and fly ash candidate reference materials

Content Provider	Royal Society of Chemistry (RSC)
Author	Prohaska, T. Latkoczy, C. Hann, S. Stingeder, G. Quétel, C. R. Hennessy, C. Taylor, P. D. P. Liesegang, D. Papadakis, I.
Copyright Year	2000
Abstract	Many fields in environmental analytical chemistry deal with very low limits and thresholds as set by governmental legislations or transnational regulations. The need for the accuracy, comparability and traceability of analytical measurements in environmental analytical chemistry has significantly increased and total uncertainties are even asked for by accreditation bodies of environmental laboratories. This paper addresses achieving these goals to guarantee accuracy, quality control, quality assurance or validation of a method by means of certified reference materials. The assessment of analytical results in certified reference materials must be as accurate as possible and every single step has to be fully evaluated. This paper presents the SI-traceable certification of Cu, Cr, Cd and Pb contents in geological and environmentally relevant matrices (three sediments and one fly ash sample). Certification was achieved using isotope dilution (ID) ICPMS as a primary method of measurement. In order to reduce significantly the number of analytical steps and intermediate samples a multiple spiking approach was developed. The full methodology is documented and total uncertainty budgets are calculated for all certified values. A non-element specific sample digestion process was optimised. All wet chemical digestion methods examined resulted in a more or less pronounced amount of precipitate. It is demonstrated that these precipitates originate mainly from secondary formation of fluorides (essentially CaF2) and that their formation takes place after isotopic equilibration. The contribution to the total uncertainty of the final values resulting from the formation of such precipitates was in general <0.1% for all investigated elements. Other sources of uncertainty scrutinised included the moisture content determination, procedural blank determination, cross-contamination from the different spike materials, correction for spectral interferences, instrumental background and deadtime effects, as well as the use of either certified values or IUPAC data in the IDMS equation. The average elemental content in the sediment samples was 30–130 µg g−1 for Pb, 0.5–3 µg g−1 for Cd and 50–70 µg g−1 for Cu. Cr was measured in one sample and was about 60 µg g−1. The concentrations in the fly ash sample were up to 2 orders of magnitude higher. Expanded uncertainty for the investigated elements was about 3% (coverage factor k = 2) except for Cr, (measured by high resolution ICPMS), for which the expanded uncertainty was about 7% (k = 2).
Starting Page	613
Ending Page	620
Page Count	8
File Format	HTM / HTML PDF
ISSN	14640325
Volume Number	2
Issue Number	6
Journal	Journal of Environmental Monitoring
DOI	10.1039/b005017m
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	IUPAC Analytical chemistry Lead Fly ash Isotope Content determination International Union of Pure and Applied Chemistry IDMS Sediment
Content Type	Text
Resource Type	Article
Subject	Public Health, Environmental and Occupational Health Management, Monitoring, Policy and Law

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SI-traceable certification of Cu, Cr, Cd and Pb in sediment and fly ash candidate reference materials

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SI-traceable certification of Cu, Cr, Cd and Pb in sediment and fly ash candidate reference materials