Porous acrylonitrile (AN)/methyl acrylate (MA) copolymer beads were prepared by suspended emulsion polymerization. The cyano groups in AN/MA copolymer beads were converted to amidoxime (AO) groups by reaction with hydroxylamine hydrochloride (NH2OH center dot HCl) to remove metal ions in aqueous solution. The untreated AN/MA and amidoximated AN/MA (AO AN/MA) copolymer beads were characterized by FTIR spectroscopy, SEM, and porous structural analysis. Both mesopores and macropores were presented in AN/MA and AO AN/MA copolymer beads. Qualitative experiments of adsorption were conducted to evaluate modified and unmodified resins on fixing Hg2+, Ag+, Cu2+, Fe3+ and Pb2+ from aqueous solution using batch extractions. It was found that AO AN/MA copolymer beads have excellent adsorption capacities for Hg2+, Ag+ and Cu2+ especially for Hg2+, and it have good selectivity for Hg2+. The equilibrium was established in 10 h through adsorption kinetics study. The Langmuir model was much better than the Freundlich model to describe the isothermal process. (C) 2009 Elsevier B.V. All rights reserved.