Abstract: Through solidstate ionic exchange technique, a series of Cu(I), Ag(I) cation modified zeolite β sorbents were prepared on the base of preparation of Na β zeolite with different Si/Al ratio. The samples were characterized by XRD, FTIR and N2 adsorptiondesorption technique. Although the crystallicity and BET surface area of the sorbents are affected by exchanged metal cation in the framework, the XRD results show that asmade samples were kept framework structure integrity. The BET surface areas of asmade Na β samples decrease as the Si/Al ratio increase, and BET surface areas of Cu(I β , Ag(I)β sorbents decrease comparing with the same Si/Al ratio Na βzeolite. FTIR spectra of the samples show that the peak of framework vibration moves to low wave number as Cu(I), Ag(I) were inserted. Then the thiophene adsorption properties of Cu(I) β , Ag(I) β , Na β were evaluated at ambient conditions. Static state experimental results show that Cu(I)β exhibits stronger adsorption for thiophene. As the Si/Al mol ratio of zeolite β is 25 about 95% thiophene was adsorbed by Cu(I) β and 87% by Ag(I) β . Through dynamic adsorption experiments, the breakthrough capacities of the Cu(I)β and Ag(I) β sorbents are 0.144mmol/g and 0.132mmol/g, respectively.