Catalytic reduction of NO by CO was studied over perovskite-like La2-xSrxCuO4 (x = 0.0, 0.5, 1.0) catalysts prepared by citrate method and calcined at 900 degrees C. The catalysts were characterized by O-2-TPD, H-2-TPR and cyclic voltammetry (CV) measurements. Results obtained from CV were in well agreement with those obtained from O-2-TPD and H2-TPR, suggesting that CV is also a powerful means in the study of heterogeneous catalytic reaction carried out at high temperatures. In O-2-TPD experiment, the desorption area of P oxygen, which was contributed by the oxygen adsorbed on the oxygen vacancy, increased with the increase of Sr content and was in the same order as the activity, indicating that the activity depended largely on the oxygen vacancy resulted by Sr addition. In H2-TPR measurements, the increasing area of the first reduction peak indicating that the oxygen vacancy resulted by Sr addition plays important role in this peak, since the Cu3+ content in La1.5Sr0.5CuO4 and LaSrCuO4 is the same. And in the CV curves, the area of redox peak, which represents the amount of oxygen vacancy participating in the reaction, has close correlations with the activity of NO + CO reaction, while the symmetry of redox potentials does not contribute much to the activity. Overall, with the link of oxygen vacancy, CV was introduced and has obtained great success in explaining reaction in heterogeneous catalysis. Besides, from the result that none reductive peak was observed in the first CV curves of LaSrCuO4, it suggested that the first step of a catalytic reaction is reduction, corresponding to the oxidation of catalyst i.e., Mn+(Cu2+)-> M(n+1)+(Cu3+). (c) 2005 Elsevier B.V. All rights reserved.