Sulfur chemiluminescence detector-vast capillary gas chromatography has been conducted on the analysis of volatile sulfur compounds in waste gases.The recoveries of hydrogen sulfide,carbon disulfide,methyl mercaptan,ethyl mercaptan,carbon disulfide,dimethyl sulphide,diethyl sulphide,n-propyl merrcaptan,i-propyl merrcaptan,thiophene and dimethyl disulfide were from 83.7% to 108.8%,the relative standard deviations were less than 5.1%.When inject volumn was 0.2 ml,the minimum detection levels of the above-mentioned volatile sulfur compounds varied between 0.03 mg/m3 and 0.1 mg/m3.Volatile sulfur compounds in waste gases from sour water tanks and oil tanks in an refinery and Gas were analyzed.