Tracing an Osmium Solution Standard to the International System of Units (SI)

Gozzi, Madeline; Gaines, Paul; Kozikowski, Thomas; Alexander, Brian W.

doi:10.1021/acs.analchem.1c03033

Cited by 1 publication

(1 citation statement)

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“…For each sample weight recorded, the glovebox temperature, % humidity, % O 2 , and glovebox barometric pressure were documented at the time of the weighing, as well as the room temperature and % humidity. Modifications to the oxygen/moisture/hydrocarbon scrubbers were made since the earlier work on developing the SI traceable Os solution standard was completed …”

Section: Methodsmentioning

confidence: 99%

Development of a Primary Iridium Solution Standard Traceable to the International System of Units

Gozzi¹,

Gaines²,

Kozikowski³

et al. 2023

Anal. Chem.

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The purpose of this work was to develop a primary solution standard for iridium (Ir) that is directly traceable to the International System of Units (SI). The candidate starting material was ammonium hexachloroiridate hydrate, ((NH 4 ) 3 IrCl 6 •3H 2 O), the Ir salt. The SI traceability of the Ir salt was established by the gravimetric reduction (GR) of the salt to the metal under H 2 . GR traces the results of the analysis directly to the SI base unit of mass, the kg. The GR was also performed on high-purity Ir metal powder, an independent source of Ir, used as a comparison material for the salt. A method for dissolving the Ir metal was developed by modifying information found in the literature. Trace metallic impurities (TMI) analysis was performed on the Ir salt using ICP-OES and ICP-MS. Inert gas fusion (IGF) analysis provided data for the O, N, and H content of the gravimetrically reduced and unreduced Ir metals. The combined results of the TMI and IGF analyses provided the purity data, a required component for the claim to SI traceability. Solution standards were gravimetrically prepared from the candidate SI traceable Ir salt. Solution standards for comparison were prepared from the dissolved, unreduced high-purity Ir metal powder. These solutions were compared by a high-precision ICP-OES method. Agreement in the results between these Ir solutions, with uncertainty estimates calculated by error budget analysis, confirmed the accuracy of the Ir assay in the candidate SI traceable Ir salt, (NH 4 ) 3 IrCl 6 •3H 2 O, thus confirming the concentrations and uncertainties for the primary SI traceable Ir solution standards made from the (NH 4 ) 3 IrCl 6 •3H 2 O.

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Section: Methodsmentioning

confidence: 99%