Issue 2, 2001

Abstract

The determination of S by solution nebulization quadrupole inductively coupled plasma mass spectrometry (ICP-MS) is difficult because of interferences from oxygen dimer ions. The large 16O2+ ion current from the solvent water is a serious interference at 32S, the most abundant of the four isotopes, and precludes its measurement. The isotopic composition of S varies in nature as a consequence of natural mass fractionation; therefore, high accuracy isotope dilution mass spectrometric (IDMS) determination of sulfur requires that the ratio of 32S/34S be measured, for the two isotopes represent over 99% of natural sulfur. In this work, electrothermal vaporization was used to generate a water-free aerosol of the sample. Non-solvent sources of oxygen were investigated and the spectral background minimized. Further reduction of the oxygen dimer was achieved by using nitrogen as an oxygen-scavenger in the argon plasma. The isotope ratio of 32S/34S was used for the determination of S by IDMS. The repeatability of the 32S/34S ratio in terms of the relative standard error (95% confidence level) of 6 replicate measurements of the spiked and the unspiked samples was about 0.3% and 0.7%, respectively. The detection limit of the method was 4 ng g−1. Sulfur in two fossil fuel reference materials was measured and the results were in good agreement (within 0.3%) with those obtained by the more precise thermal ionization mass spectrometry (TIMS) method.

Article information

Article type
Paper
Submitted
16 Nov 2000
Accepted
21 Dec 2000
First published
26 Jan 2001

J. Anal. At. Spectrom., 2001,16, 140-145

Determination of sulfur in fossil fuels by isotope dilution electrothermal vaporization inductively coupled plasma mass spectrometry

L. L. Yu, W. R. Kelly, J. D. Fassett and R. D. Vocke, J. Anal. At. Spectrom., 2001, 16, 140 DOI: 10.1039/B008298H

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