Aromatic hydroxylation, using novel effective catalysts was developed by loading CuO and Fe2O3 nanoparticles onto Egyptian kaolin. The H2O2 was used as a green and environmentally benign oxidizing agent. The resulting catalysts were subjected to several characterization methods, including XRD, SEM, and EDX analysis. Next, the catalytic activity of these species in effecting the hydroxylation of benzene was evaluated. The compounds were loaded using two methods: impregnation and precipitation deposition. A detailed comparison between the two methods has been undertaken. EDX analysis enables us to differentiate between two types of active sites - surface and bulk active sites. (C) 2012 Elsevier B.V. All rights reserved.