Fe2O3/Al2O3 catalyst was prepared and the catalytic oxidation of toluene over the catalyst was investigated. The catalyst was prepared by wet impregnation of commercial alumina support. The support was impregnated with an aqueous solution of iron nitrate. The wet support was dried and calcined at 600-800 °C. The catalytic property of the catalyst was measured by the light-off curve of CO2 yield. All these catalysts were active for total oxidation of toluene above 250 °C. The catalytic activity of catalyst calcined at 600 °C was better than those of catalysts calcined at 700 and 800 °C.