Polycarbonate (PC) membrane and PC based hydrogen active intermetallic compound Fe0.5Ti0.5 particles doped composite membrane have been prepared by solution cast method. The membranes have been characterized by H2 and CO2 permeability and selectivity measurements with increasing temperature. Higher gas permeation has been observed with increasing temperature. In case of doped composite membrane H2/CO2 gas pair selectivity first increases then decreases with temperature whereas in case of pure PC it decreases with temperature. The effect of doping increases the activation energies for permeation of H2 and CO2 in the doped membrane in comparison to pure PC. Doping was found to suppress plasticization effect in polycarbonate. The doped membrane was analyzed by optical micrograph and XRF study.