Starch/poly(N,N-Diethylaminoethyl methacrylate) graft copolymer was synthesized by graft polymerizing N,N-Diethylaminoethyl methacrylate monomers onto cooked starch using ceric ammonium nitrate/nitric acid mixture as an initiator. After extracting the graft copolymer from the homopolymer and evaluating the graft yield, the graft copolymer was subjected to crosslinking treatment using epichlorohydrin in alkaline medium to convert it to hydrogel. The so prepared hydrogel was evaluated for its swelling ratio which was found to be 100. The hydrogel with its cationic functionality was tried for removing the anionic dye Direct Red 81 from its aqueous solution and all factors affecting the hydrogel adsorption capacity towards the anionic dye, like the hydrogel graft yield, the adsorbate pH, the immersion time and the hydrogel dose were studied. The data obtained from the adsorption results were found to fit well to the Langmuir adsorption model. (C) 2013 Elsevier Ltd. All rights reserved.