The objective of this research is to use semi-cokes as raw material to prepare sorbents for sulfur removal from gasoline, to find the optimal preparation methods and determine the operating conditions. The result shows that the granular semi-cokes, pre-activated with 30%-45% HNO3, calcined at 700A degrees C at N-2 atmosphere mixed with vapor for l h, then impregnated with 3%CuO, give the best performance for sulfur removal. With this desulfurizer, the adsorption capacity observed was 0.933 mg/g at breakthrough level for a high-sulfur FCC gasoline (650 ng/mu l), 1.155 mg/g for a low-sulfur gasoline (400 ng/mu l), and 3.528 mg/g for thiophene-cyclohexane solution (300 ng/mu l). Compared with the GC-FPD chromatograms of FCC gasoline and desulfurized gasoline, it showed that all of the benzothiophenes (BT) and their derivatives and most other sulfides in FCC gasoline were removed by this desulfurizer. In this study, the optimal operating conditions were 160A degrees C and a space velocity of 4 h (-aEuro parts per thousand 1).