The effect of different oxidation pre-treatments on the sulphur distribution in Illinois No. 6 coal (IBC-101) was studied using Atmospheric Pressure-Temperature Programmed Reduction (AP-TPR). Oxidation pre-treatments were carried out on demineralized coal with peroxyacetic acid (PAA) as a function of reaction time. For the longest reaction time the effect of PAA on the coal was compared to the effect of several other oxidants. AP-TPR results also show a clear effect of LiAlH4 on the coal. Not only is pyrite removed, but there is also a decrease in other sulphur forms. Subsequent PAA oxidation causes an overall decrease of the AP-TPR signal, signifying the attack on organic as well as inorganic sulphur forms. With other oxidants, under the same conditions, only minor differences could be found after different treatments.