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Issue 1, 2018
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SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS

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Abstract

Previously applied methods for the quantification of sulphur in copper and other pure metals revealed a lack of SI-traceability and additionally showed inconsistent results, when different methods were compared. Therefore, a reference procedure is required which allows SI-traceable values accompanied by a sound uncertainty budget. In this study a procedure was developed for the quantification of total sulphur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The major part of the copper matrix was separated by adding ammonia which forms a complex with the copper while releasing the sulphur followed by chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion exchange method and second a chelating resin. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (>99.999%) while keeping the recovery of sulphur above 80%. Procedure blanks are in the order of 3–53 ng resulting in LOD and LOQ values of 0.2 μg g−1 and 0.54 μg g−1, respectively. The procedure is sufficient to facilitate value assignment of the total sulphur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated to be below 1% and the measurement results were traceable to the SI. The procedure reported in this study is a new reference procedure for sulphur measurement in copper, being fit for two major purposes, certification of reference materials and assignment of reference values for inter-laboratory comparison.

Graphical abstract: SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS

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Article information


Submitted
10 Oct 2017
Accepted
15 Nov 2017
First published
15 Nov 2017

J. Anal. At. Spectrom., 2018,33, 90-101
Article type
Paper

SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS

P. Phukphatthanachai, U. Panne, N. Jakubowski and J. Vogl, J. Anal. At. Spectrom., 2018, 33, 90
DOI: 10.1039/C7JA00338B

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