Determination of Sulfide and Total Sulfur in Ore by Wavelength-Dispersive X-ray Fluorescence

This paper describes the determination of total sulfur and sulfide in ore by X-ray fluorescence. The X-ray emission spectra of sulfur were measured by a wavelength-dispersive spectrometer. The samples were prepared as pressed powder pellets on boric acid substrates. The SK alpha(1,2) line was used to determine total sulfur. The ratio between sulfide and total sulfur was measured by the ratio of satellite SK beta' and SK beta(1,3) line intensities. The total relative standard deviation (SD) of the measurements and preparation repeatability was less than 2%. Sample preparation was contributed to the error of the analysis. To determine total sulfur, the calibration curve was obtained from the samples of certified reference materials of gold-bearing sulfide-containing ore. The accuracy was verified by comparison with a gravimetric method. The relative SD was 6% for sulfur concentrations from 1 to 8 wt%. The calibration curve was defined using pure reagents to determine sulfide. The ore was analyzed by a gravimetric procedure with a relative SD of 6.5% for the sulfide concentration from 1 to 6 wt%.