Emissions of five volatile organic sulfur compounds (VOSCs), including methanethiol, carbonyl sulfide, dimethyl sulfide, carbon disulfide, and dimethyl disulfide, from a heavily polluted river, Shijing River in Guangzhou of South China, was studied. The results showed that the amounts of all VOSCs emitted from the river increased from downstream to upstream along the river with increasing magnitude of water pollution. The emission of carbonyl sulfide was the highest among the target analytes, ranging from 23.8 microg m(-2) h(-1) to 42.6 microg m(-2) h(-1) at the water surface of Shijin River. The concentration levels of VOSCs on the riverbank were lower than those at the water surface either in Shijing River or in Liuxi River. However, the contribution of dimethyl disulfide to the total VOSCs on the riverbank was higher than that at the water surface in most sampling sites, indicating that there might be a point source of dimethyl disulfide on the riverbank besides diffusion from water surface. The 24-h semi-continuous monitoring data revealed that the emissions of VOSCs at the water surface peaked at 9:00 and 21:00, which was consistent with the water quality variability in Shijin River caused by daily tidal variation.