Issue 10, 2021

High-efficiency photoreductive vapor generation of osmium

Abstract

A novel, high yield (91 ± 5%) photochemical vapor generation (PVG) method is reported for Os, achieved via photo-reduction reactions in a 1% CH3COOH medium containing 50 mg L−1 Fe3/2+. A sample flow rate of 2 mL min−1 delivered to a flow-through photoreactor provided a 21 s irradiation time prior to passage of the volatile product to an inductively coupled plasma mass spectrometer for detection at m/z 192. A method detection limit of 0.16 pg mL−1 was achieved, a 10-fold enhancement over that obtained using parallel photo-oxidation synthesis of OsO4 from a 5% HNO3 medium. Precision of replicate measurement was 4% (RSD) at 10 ng mL−1. Although the identity of the product has not yet been ascertained by GC-MS, based on the chemistry of Os and the reaction conditions, as well as its difference in volatility from OsO4, a carbonyl or alkyl-substituted carbonyl is suspected e.g., Osw(CO)x(CH3)yHz.

Graphical abstract: High-efficiency photoreductive vapor generation of osmium

Article information

Article type
Paper
Submitted
03 Jun 2021
Accepted
27 Jul 2021
First published
19 Aug 2021

J. Anal. At. Spectrom., 2021,36, 2097-2106

High-efficiency photoreductive vapor generation of osmium

R. M. de Oliveira, D. L. G. Borges, P. Grinberg and R. E. Sturgeon, J. Anal. At. Spectrom., 2021, 36, 2097 DOI: 10.1039/D1JA00192B

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