Different inorganic sulfur species distributed in overlying water, pore water and sediment in a heavily polluted river were determined. The concentrations of S(2-) and SO(4)(2-) in the overlying water were much more than those in the pore water. This result perhaps indicates the S(2-) was mainly from discharged wastewater, not from sediment resuspension. In the sediments, acid-volatile sulfide, chromium(ii)-reducible sulfide, and elemental sulfur were determined by a modified diffusion method. The results indicate that acid-volatile sulfide was the dominant component of the reduced inorganic sulfur, making up about 62% of the total reduced inorganic sulfur.