Chemical polymerization of acrylamide at room temperature was examined by using thioglycolic acid-cerium (IV) sulfate and thioglycolic acid-KMnO 4 redox systems in acid aqueous medium. Water soluble polyacrylamides containing thioglycolic acid end groups were synthesized. The effects of the molar ratio of acrylamide to Ce(IV) n AAm /n Ce(IV ) , the polymerization time, the temperature, the monomer concentration, the molar ratio of cerium (IV) sulfate to thioglycolic acid and the concentration of sulfuric acid on the yield and molecular weight of polymer were investigated. Lower molar ratios of acrylamide/Ce(IV) at constant monomer concentration resulted in an increase in the yield but a decrease in molecular weight of polymer. The increase of reaction temperature from 20 to 70 • C resulted in a decrease in the yield but generally resulted in a constant value for the molecular weight of polymer. With increasing polymerization time, the yield and molecular weight of polymer did not change substantially. Ce(IV) and Mn(VII) ions are reduced to Ce(III) and Mn(II) ions respectively in the polymerization reaction. The existence of Ce(III) ion bound to polymer was investigated by UV-visible spectrophotometry and fluorescence measurements. The amount of Mn(II) incorporated into the polymer was determined using graphite furnace atomic absorption spectrometry. The mechanism of this phenomenon is discussed.