Journal
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
Volume 35, Issue 4, Pages 397-429Publisher
WILEY-BLACKWELL
DOI: 10.1111/j.1751-908X.2011.00120.x
Keywords
microanalysis; glass reference materials; NIST; characterisation; sample inhomogeneity; microanalyse; verre de reference; NIST; caracterisation; inhomogeneite de l'echantillon
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We present new reference values for the NIST SRM 610617 glasses following ISO guidelines and the International Association of Geoanalysts protocol. Uncertainties at the 95% confidence level (CL) have been determined for bulk- and micro-analytical purposes. In contrast to former compilation procedures, this approach delivers data that consider present-day requirements of data quality. New analytical data and the nearly complete data set of the GeoReM database were used for this study. Data quality was checked by the application of the Horwitz function and by a careful investigation of analytical procedures. We have determined quantitatively possible element inhomogeneities using different test portion masses of 1, 0.1 and 0.02 mu g. Although avoiding the rim region of the glass wafers, we found moderate inhomogeneities of several chalcophile/siderophile elements and gross inhomogeneities of Ni, Se, Pd and Pt at small test portion masses. The extent of inhomogeneity was included in the determination of uncertainties. While the new reference values agree with the NIST certified values with the one exception of Mn in SRM 610, they typically differ by as much as 10% from the Pearce (1997) values in current use. In a few cases (P, S, Cl, Ta, Re) the discrepancies are even higher.
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