LaFe0.9Co0.1O3(LFCO) perovskite nanoparticles were prepared using a sol-gel method. The physical and chemical properties of the catalyst were determined using X-ray diffraction (XRD), transmission electron microscopy, scanning electron microscopy, scanning tun-neling microscopy, energy dispersive X-ray spectroscopy, thermogravimetric analysis, and Fourier transform infrared spectroscopy. The catalytic activity of the sample was evaluated using aerobic oxidation of thiols to disulfides. The XRD results indicated that the LFCO had a good crystalline phase at 750°C. The experimental data revealed that the LFCO particles were nano-sized. LFCO nanoparticles can catalyze the oxidation of various thiols, including aromatic and aliphatic thiols. The effects of reaction parameters such as temperature, solvent, and the amount of catalyst on the oxidation of 4-chlorothiophenol were investigated. In comparison with reactions using the corresponding neat complexes, i.e., Co(NO3)2·6H2O and Fe(NO3)3·9H2O, higher yields were obtained in the oxidation reaction catalyzed by LFCO nanoparti-cles.