Least square analysis of the X-ray absorption near edge structure (XAN
ES) region of sulfur K edge X-ray absorption fine structure (XAFS) spe
ctra can provide a quantitative analysis of both the organic and inorg
anic functional forms of sulfur in coal. In the current article, this
method is applied to speciation of the sulfur forms in a number of des
ulfurized coals. The samples investigated include biologically desulfu
rized coals, samples subjected to selective chemical reactions, sample
s subjected to molten caustic leaching and specimens treated with boil
ing perchloroethylene. In all cases, analysis of XANES provides a reas
onably quantitative speciation of the changes in the sulfur forms resu
lting from the various treatments.