The polymerization of acrylamide, initiated by a cerium (IV) [Ce(IV)] ammonium nitrate-methionine redox initiator system, was carried out in an aqueous solution at different reaction conditions. The dependence of molecular weight and polymerization yield on the concentration of Ce(IV), polymerization time, and temperature was determined. The molecular weight distributions (MWD) of the resulting polymers were examined using the HPLC method. Based on the HPLC results, optimum reaction conditions were determined that provided an opportunity to obtain a polymer that had a narrow MWD.