SYNOPSISPoly (glycidyl methacrylate) -starch graft copolymer was prepared using hydrogen peroxide/ ferrous sulphate/thiourea dioxide redox system as initiator. The copolymer was treated with orthophosphoric acid ( H3P04) under a variety of conditions to discover appropriate conditions for synthesizing the copolymer that can serve as cation exchanger. Results obtained indicated that the cation-exchange capacity is enhanced by: ( a ) increasing the H3P04/epoxy molar ratio up to 4; ( b ) using material-to-liquor ratio 1 : 2; ( c ) increasing duration (15-300 min) and temperature (60-90°C); ( d ) increasing the amount of epoxy groups of the copolymer; and ( e ) increasing the percent neutralization of H3P04 up to 33.3%. Based upon the results obtained with these parameters, it was postulated that three reactions are involved during treatment of the copolymer with &PO,. These reactions are phosphorylation, crosslinking, and hydrolysis. Conditions were established under which the phosphorylation reaction occurs exclusively. Studied also were the ion-exchange properties of the phosphorylated copolymer, namely, p K , values, capacity for heavy metal ions removal, moisture content, durability, swellability, and solubility.