Abstract: Yima and American Pocahontas No. 3 coal samples were exhaustively extracted with carbon disulfide (CS2)/tetrahydrofuran mixed solvent and cyclohexanone, respectively. The residues after extraction were oxidized in 30% hydrogen peroxide aqueous solution at 40 ℃. Water-soluble and insoluble fractions were separated in the reaction mixture by filtration, and then extracted with benzene and CS2, respectively. The extraction solutions were analyzed with GC/MS. The results show that both water-soluble fractions from the two oxidized coal residues contain small amount of phenol. Oxygen-containing compounds and long-chain alkanes are detected in the extraction solution with CS2 from the water-insoluble fraction.