Abstract: An accurate and simple method using gas chromatography was developed for the determination of sulfur compounds in syngas.Six-way valve with three loops for auto introduction of sample and flame photometry detector (FPD) having satisfactory selectivity for sulfur and phosphorus were used.The linear regression relationship between the logarithm of the dose versus the logarithm of the peak area were obtained giving correlation coefficients of 0.999 5,0.999 7 and 0.999 7 for H2S,COS and CS2 respectively.