We successfully prepared the biodegradable cellulose/chitin beads by coagulating a blend of cellulose and chitin in 6 wt% NaOH/5 wt% thiourea aqueous solution with 5 % H2SO4 as coagulant, and investigated the adsorption of heavy metals (Pb2+, Cd2+, Cu2+) from an aqueous solution on the beads by atomic absorption spectrophotometer. Batch adsorption experiments were carried out as a function of ion concentrations, initial pH, ionic strength, temperature, 21 adsorption time and desorption time. The results revealed that the cellulose/chitin beads could adsorb effectively Pb Cd2+ and Cu2+ ions, and the uptakes of Pb2+ Cd2+ and ions on cellulose/chitin beads were 0.33 mmol/g at pH(0) 4 0.32 mmol/g at pH(0) 5 and 0.30 mmol/g at pH(0) 4, respectively. Experimental results also showed that the adsorption of these heavy metals was selective to be in the order of Pb2+ > Cd2+ > Cu2+ in a low ion concentration solution. The adsorption equilibrium time of these heavy metals on beads was 4-5 h, but the desorption time was 5-15 min. Moreover, these beads could be regenerated up to about 98% by treating with 1 mol/L HCl aqueous solution. The mechanisms for the removal of free heavy metal ions by cellulose/chitin beads was based on mainly complexation adsorption model, as well as a affinity of hydroxyl groups of the materials on metals. Therefore, we developed new environment-friendly beads prepared by a simple produce process for removal and recovery of heavy metals. (C) 2004 Elsevier Ltd. All rights reserved.