Abstract A novel Fe–Mn–Zr was prepared by co-precipitation method and calcined at different temperature. The NO removal capacity, N2 selectivity and SO2 resistance with or without H2O over Fe–Mn–Zr were investigated in a fixed-bed microreactor. The results showed that the catalysts calcined at 400–600 °C exhibit 100% NO removal efficiency in the range of 170–360 °C. FMZ-500 shows a better tolerance to both 100 and 200 ppm SO2 than other samples and excellent resistance to H2O and can achieve over 93% NO removal efficiency in the presence of SO2 and H2O. FMZ-500 catalyst can completely recover NO removal capacity when SO2 and H2O shut off. When Fe–Mn–Zr is calcined at 700 and 800 °C, NO removal efficiency at 170 °C are 90% for FMZ-700 and 35% for FMZ-800 and their resistances to SO2 are very poor. When Fe–Mn–Zr is calcined at 400, 500 and 600 °C, MnO2, Mn2O3 and Fe2O3 are homogeneously dispersed and exist mainly in an amorphous state as well as similar reduction properties. When the calcination temperature increases to 800 °C, the crystallinity of oxides significantly increases and reduction temperatures shift from 318 and 413 °C to 420 and 478 °C. High temperature calcination causes the decrease of surface area and Lewisacid sites, corresponding to low NH3 adsorption.