Abstract: By optimizing the column temperature, carrier gas flow rate, photomultiplier polarization voltage, flow ratio of hydrogen to air (hydrogen-air ratio), and detector temperature, a method of gas chromatography with flame photometric detector (FPD) was proposed for the determination of hydrogen sulfide, carbonyl sulfur in blast furnace gas, and hydrogen sulfide, carbonyl sulfur, carbon disulfide, methyl mercaptan, methyl sulfide, ethyl mercaptan, thiophene, dimethyl disulfide in coke oven gas. The samples were diluted by different procedures and analyzed by gas chromatograph. In the analysis of blast furnace gas, the GDX-502 column was used as the stationary phase. The column temperature was 60 ℃, the carrier gas flow rate was 30 mL·min^-1, the photomultiplier polarization voltage was 900 V, the hydrogen flow rate was 80 mL·min^-1, the hydrogen-air ratio was 1∶0.67, and the detector temperature was 160 ℃. In the analysis of coke oven gas, HF-Sulfur column was used as the stationary phase, and detection was made under the condition of column temperature program (except for sampling volume, other conditions were consistent with those of blast furnace gas). It was shown that linear relationships between the natural logarithmic value of the mass concentration of each component in blast furnace gas and coke oven gas and the response value were kept in defite ranges. The detection limits of the two components in blast furnace gas ranged from 0.56 mg·m^-3 to 0.87 mg·m^-3, the relative errors (standard gas) ranged from -4.6% to 0.88%, and the RSDs (n=5) of the determined values ranged from 0.22% to 2.4%. The detection limits of 8 components in coke oven gas ranged from 0.711 mg·m^-3 to 1.145 mg·m^-3, the recoveries obtained by standard addition method were found in the range of 94.4%-105%, and the RSD (n=6) of the determined values ranged from 1.4% to 8.8%.