Magnetic nanoscaled Fe(3)O(4)/CeO(2) composite was prepared by the impregnation method and characterized as a heterogeneous Fenton-like catalyst for 4-chlorophenol (4-CP) degradation. The catalytic activity was evaluated in view of the effects of various processes, pH value, catalyst addition, hydrogen peroxide (H(2)O(2)) concentration, and temperature, and the pseudo-first-order kinetic constant of 0.11 min(-1) was obtained for 4-CP degradation at 30 °C and pH 3.0 with 30 mM H(2)O(2), 2.0 g L(-1) Fe(3)O(4)/CeO(2), and 0.78 mM 4-CP. The high utilization efficiency of H(2)O(2), calculated as 79.2%, showed a promising application of the catalyst in the oxidative degradation of organic pollutants. The reusability of Fe(3)O(4)/CeO(2) composite was also investigated after six successive runs. On the basis of the results of metal leaching, the effects of radical scavengers, intermediates determination, and X-ray photoelectron spectroscopic (XPS) analysis, the dissolution of Fe(3)O(4) facilitated by CeO(2) played a significant role, and 4-CP was decomposed mainly by the attack of hydroxyl radicals (•OH), including surface-bound •OH(ads) generated by the reaction of Fe(2+) and Ce(3+) species with H(2)O(2) on the catalyst surface, and •OH(free) in the bulk solution mainly attributed to the leaching of Fe.