Abstract: We use XPS technology to research Xinchen fat coal low temperature oxidation experiment. The XPS results of sulfur on the coal surface before and after oxidation show that the sulfide and pyrite content is highest for raw coal sample; thiophenic sulfur content is the highest in organic sulfur, followed by sulfoxide and sulfone; there is also some sulfate existing on the coal surface. The result of oxidized coal is different from raw sample; the relative contents of thiophenic sulfur is reduced; the sulfide oxide into sulfoxide which further oxidized to sulfone, that is the reason why sulfone relative concentration increased meanwhile sulfoxide disappeared. The nitrogen spectrogram of raw coal analysis shows that the nitrogen mainly exists on the edge of coal molecules; about 21% of nitrogen is embedded into coal molecular structure in the quaternary nitrogen form; the pyrrole nitrogen content is the highest. The XPS results of oxidation sample show that the oxygen atom linked to nitrogen removal in the process of oxidation; the oxidation nitrogen changes into other forms and most parts of it change into pyridine.