The adsorption of Pb(II) and Cd(II) ions with crosslinked carboxymethyl starch (CCS) was investigated as function of the solution pH, contact time, initial metal-ion concentration, and temperature. Isotherm studies revealed that the adsorption of metal ions onto CCS better followed the Langmuir isotherm and the DubininRadushkevich isotherm with adsorption maximum capacities of about 80.0 and 47.0 mg/g for Pb(II) and Cd(II) ions, respectively. The mean free energies of adsorption were found to be between 8 and 16 kJ/mol for Pb(II) and Cd(II) ions; this suggested that the adsorption of Pb(II) and Cd(II) ions onto CCS occurred with an ion-exchange process. For two-target heavy-metal ion adsorption, a pseudo-second-order model and intraparticle diffusion seem significant in the rate-controlling step, but the pseudo-second-order chemical reaction kinetics provide the best correlation for the experimental data. The enthalpy change for the process was found to be exothermic, and the ?S? values were calculated to be negative for the adsorption of Pb(II) and Cd(II) ions onto CCS. Negative free enthalpy change values indicated that the adsorption process was feasible. The studies of the kinetics, isotherm, and thermodynamics indicated that the adsorption of CCS was more effective for Pb(II) ions than for Cd(II) ions. (c) 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011