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Macerals of NW coal were separated by isopycnic density gradient centrifugation (IDGC) (ZnCl2 was used as density fluid) and each macerals were undertaken forms of sulfur. Sulfur was removed by peroxyacetic acid-oxidation under ultrasonic and microwave radiation. Transformations of organic sulfur forms were expressed by XPS spectra. The results showed that forms of organic sulfur were enriched in different macerals, thiophenes in vitrinite and thioethers, thiols in exinite. Desulfurization rate of NW raw coal was up to 38.1% with peroxyacetic acid under ultrasonic and microwave radiation. From easy to difficult, the order of desulfurization of each macerals was the same as mineral and inertinite > inertinite > exinite > vitrinite, the most high desulfurization rate of macerals was 53.1%.