Abstract: Six sulfur compounds in high sour petroleum and natural gas were determined qualitatively and quantitatively using gas chromatography equipped with capillary column and FPD (Flame Photometric Detector). The relationship between concentrations of sulfur compounds and response peak heights was obtained, and the effect of sample collection bag made of different materials on analytical results was investigated. The sulfur compounds mentioned above can be separated effectively with the capillary column. The natural logarithm of concentrations and response peak heights show good linear correlation with a correlation coefficient above 0.980. The sample collection bag made of common rubber material is not suitable for the quantitative analysis because of its evident adsorption of organic sulfur compounds. petroleum and natural gas; sulfur compounds; gas chromatography; FPD detector