The removal performance and the selectivity sequence of mixed metal ions (Co2+, Cr3+, Cu2+, Zn2+ and Ni2+) in aqueous solution were investigated by adsorption process on pure and chamfered-edge zeolite 4A prepared from coal fly ash (CFA), commercial grade zeolite 4A and the residual products recycled from CFA. The pure zeolite 4A (prepared from CFA) was synthesized under a novel temperature step-change method with reduced synthesis time. Batch method was employed to study the influential parameters such as initial metal ions concentration, adsorbent dose, contact time and initial pH of the solution on the adsorption process. The experimental data were well fitted by the pseudo-second-order kinetics model (for Co2+, Cr3+, Cu2+ and Zn2+ ions) and the pseudo-first-order kinetics model (for Ni2+ ions). The equilibrium data were well fitted by the Langmuir model and showed the affinity order: Cu2+ > Cr3+ > Zn2+ > Co2+ > Ni2+ (CFA prepared and commercial grade zeolite 4A). The adsorption process was found to be pH and concentration dependent. The sorption rate and sorption capacity of metal ions could be significantly improved by increasing pH value. The removal mechanism of metal ions was by adsorption and ion exchange processes. Compared to commercial grade zeolite 4A, the CFA prepared adsorbents could be alternative materials for the treatment of wastewater. (c) 2005 Elsevier B.V. All rights reserved.