Sulfur Determination in Geological Samples Based on Coupled Analytical Techniques: Electric Furnace‐IC and TGA‐EGA

Abstract

A study has been undertaken to determine sulfur in geological samples by coupled analytical techniques. Two measurement methods have been developed: one using an electric furnace coupled to an ion chromatograph (electric furnace‐IC) and another using infrared (IR) and quadrupole mass spectrometry (QMS) for evolved gas analysis (EGA) coupled with a thermogravimetric analyser (TGA). In the electric furnace‐IC method, measurement was performed without any sample pre‐treatment. The measurement conditions were optimised by varying sample quantity, type of catalyst (WO3, Cu, W and V2O5) and sample/catalyst ratio, and the detection limit was 10 μg g−1. Sulfur ores decompose at different temperatures. However, TGA‐EGA allowed identification of the different forms of sulfur in the sample, even when they were found in very low concentrations, because the sulfur was continuously analysed. The developed chromatographic method allowed simultaneous analysis of several sample components, such as S, Cl and F, with a low detection limit. The method was much faster and more specific than the methods described in the literature. The results of the sulfur determination had low scatter, possibly because the samples underwent little handling during analysis: the operator only weighed and placed the sample in the furnace, the rest of the measurement process was fully automated. The results obtained by both the developed methods have been validated by using reference materials and comparison with combustion‐IR spectroscopy, a standard method for determining total sulfur in a sample.