Abstract: An analytical method was established for the determination of trace sulfides in sulfur recovery hydrogenation process using a two-dimensional gas chromatographic center-cutting technique in combination with a dual detector. The target compound was separated into TCD through a precolumn and the target compound was cut into the PFPD for detection by setting a valve switching time which is controlled by an assisting electronic circuit through the system pressure change. The retention time of hydrogen sulfide, sulfur dioxide, carbonyl sulfide, methanethiol, ethanethiol and disulfide in the process of hydrogenation and reduction was determined. The double column and dual detector were established for qualitative and quantitative analysis method. The method was applied to the analysis of gas during hydrogenation and reduction. The relative standard deviation (RSD)of the target compound was below 1.0%, the lowest detection limit was less than 1×10^-6 and the linear correlation coefficient R was greater than or equal to 0.9999. The method completely separates the hydrogen sulfide from the trace sulfide, saves the pretreatment step of the hydrogen sulfide, and solves the accurate and quantitative analysis of the sulfur form under the coexistence of hydrogen sulfide, trace sulfur dioxide and trace organic sulfur compound.