Full Paper: The polymerization of methyl methacrylate (MMA) initiated by Ce-IV was conducted in DMF/Water and acetonitrile. The effect of the monomer concentration and the DMF content on the conversion were investigated. The yield of the process, which proceeds under mild conditions in the mixture of DMF and water (80/20) was high. The study was augmented by cyclic voltammetric and spectrophotometric investigation. The resulting polymer was characterized by FTIR spectroscopy, and its M-W was determined viscometrically. A possible mechanism for the polymerization is suggested.