The CaFe2O4 spinel-type catalyst was synthesized by citrate gel method and well characterized by thermogravimetric analysis, atomic absorption spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction and transmission electron microscopy. The crystallization temperature of the spinel particle prepared by citrate gel method was 600 degrees C which was lower than that of ferrite prepared by other methods. CaFe2O4 catalysts prepared by citrate gel method show better activity for styrene oxidation in the presence of dilute H2O2 (30%) as an oxidizing agent. In this reaction the oxidative cleavage of carbon-carbon double bond of styrene takes place selectively with 38 +/- 2 mol% conversion. The major product of the reaction is benzaldehyde up to 91 +/- 2 mol% and minor product phenyl acetaldehyde up to 9 +/- 2 mol%, respectively. The products obtained in the styrene oxidation reaction were analyzed by gas chromatography and mass spectroscopy. The influence of the catalyst, reaction time, temperature, amount of catalyst, styrene/H2O2 molar ratio and solvents on the conversion and product distribution were studied. (C) 2010 Elsevier Ltd. All rights reserved.