The purpose of this
work was to develop an accurate osmium (Os)
solution standard that is traceable to the International System of
Units, the SI. A gravimetric reduction (GR) method was developed to
accurately assay the Os in ammonium hexachloroosmate salt, (NH4)2OsCl6, the chosen starting material
for the Os solution standard. This GR method was also applied to −200
mesh high-purity Os metal powder, which served as an independent source
of Os for comparison. An alkali fusion method was developed to create
water-soluble salts from the Os metal GR products of both the (NH4)2OsCl6 and −200 mesh high-purity
Os metal powder. Quantitatively prepared Os solutions from each of
these water-soluble salts were compared by inductively coupled plasma
spectrometry, ICP-OES. The purities of the Os starting materials were
determined by quantitatively performed trace metallic impurities analysis,
by ICP-OES and ICP-MS; the O, N, and H impurities were determined
by inert gas fusion analysis. The percent purities of the starting
materials were applied as corrections to the Os assay results obtained
by GR. The agreement between these Os solutions, corrected for random
and systematic errors by error budget analysis, confirmed the accuracy
of the Os assay in the (NH4)2OsCl6. The SI traceability of the Os assay in the (NH4)2OsCl6 salt was established through the GR procedure
and the purity analysis of this material. An SI traceable Os solution
standard was gravimetrically prepared from this batch of (NH4)2OsCl6, based on the accurate Os assay and
the percent purity of the starting material.