Abstract: The method was established for determination of sulfur compounds in high sour natural gas by gas chromatography with sulfur chemiluminescent detector. The pollution to detector and interference from high concentration H₂S has been solved by using micro flow controller. A fast and economical method has been established to detect several sulfides in sulfur-bearing natural gas with only one standard material. The qualitative analysis of sulfides was performed according to retention time of standard material and the quantitative analysis was performed on the basis of External Standard Method. The linear relationship between sulfur content and chromatographic peak area is obvious with this method for testing high sulfur natural gas sample and the correlation coefficient r was 0.999 7. The relative standard deviation for sulfides under the concentration of 2 mg/m³ was less than 6.1%, and that of the sample with the concentration above 2 mg/m³ was less than 2.2%. The methods can completely meet the needs to analyze the high sulfur natural gas.