Determination of Ge, As, Se and Te in Silicate Samples Using Isotope Dilution‐Internal Standardisation Octopole Reaction Cell ICP‐QMS by Normal Sample Nebulisation

Abstract

A method for the determination of Ge, As, Se and Te in silicate samples using isotope dilution‐internal standardisation (ID‐IS) octopole reaction cell (ORC) ICP‐QMS by normal sample nebulisation was developed. The method does not involve either hydride generation or ion exchange. Germanium, Se and Te were determined by isotope dilution (ID), and As was determined by ID‐IS. A silicate sample with an added Ge‐Se‐Te spike was digested with an HF‐HNO3‐HBr mixture, dried, re‐dissolved with HF and the supernatant liquid was directly aspirated into an ORC‐ICP‐QMS instrument with He or H2 gas. No matrix effects were observed down to a dilution factor (DF) of ∼ 70 for Ge, Se and Te and DF of ∼ 1000 for As, which resulted in 3s detection limits in silicates of 2, 1, 0.1 and 4 ng g−1, respectively. Advantages of the method are the simple sample introduction as well as a capability of determining S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by ID‐IS‐ICP‐QMS/SFMS from the same solution. Furthermore, the total sample solution consumption was only 0.253 ml with DF = 2000. Therefore, only a 0.13 mg test portion was required. To demonstrate the applicability of this technique, Ge, As, Se and Te in eight silicate reference materials were determined, as well as S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta in four carbonaceous chondrites.