The kinetics of aqueous polymerization of Acrylonitrile initiated by the Cerium (IV)-Oxalic acid redox system in Sulfuric acid medium has studied under nitrogen atmosphere in the temperature range of 25-50 degrees C. The rate of polymerization (R-p) and the disappearance of Cerium (IV) have been measured. The water-miscible organic solvents and inorganic salts were depressed both the rate and the conversion. The effects of ionic strength, effects of surfactant have been investigated. The temperature dependence of the rate was studied and the activation parameters were computed using Arrhenius and Eyring plots. A mechanism consistent with the experimental data, involving Ce(IV)-Oxalic acid complexation that generates free radical was suggested. The chain termination step of the polymerization reaction was determined. (c) 2008 Wiley Periodicals, Inc.