The iron vanadate, FeVO4, Was prepared and characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM). It was found that FeVO4 could effectively catalyze H2O2 to generate active hydroxyl radical (OH)-O-center dot, which was confirmed with electron spin resonance (ESR) spin-trapping technique. Therefore, it was employed as a heterogeneous Fenton-like catalyst in the present contribution, and its catalytic activity was mainly evaluated in terms of the degradation efficiency of Orange II. Compared with the conventional heterogeneous Fenton-like catalysts, alpha-Fe2O3, Fe3O4 and gamma-FeOOH, FeVO4 possessed a much higher catalytic activity. The high catalytic activity possibly involved in a special two-way Fenton-like mechanism. that is, the activation of H2O2 by both Fe(III) and V(V) in FeVO4. Moreover, FeVO4 possessed a wide applicable pH range and its catalytic activity was slightly affected by the solution pH values in the range of 3-8. (C) 2008 Elsevier B.V. All rights reserved.