Abstract: Preparation conditions of SbSn intermetallic compound by melting and performance of desulfurization using the new material were investigated. Gasoline and a simulated oil which consists of heptane and thiophene were used respectively in the desulfurization experiments. Before the desulfurization, both of the gasoline and the simulated oil were emulsified. The results show that the preferable preparation conditions are: m(Sb)∶m(Sn)=49∶51, melting temperature 950℃, melting time 60min, particle size of Sb less than 200mesh and using fast cooling. The positive results of desulfurization experiments for the simulated oil and gasoline were obtained by using the SbSn intermetallic compound. The sulfur removal efficiency of 15% for the simulated oil and 11.8% for the gasoline are obtained in a single pass under room temperature and ambient pressure while combined suitable emulsification. Several methods were used to clean the SbSn intermetallic compound. The results show that the clean method by using toluene is a preferable one. The removal efficiency of 32% for simulated oil and 27% for gasoline are obtained after thrice loop operations.