The performance of chitosan/hydroxyapatite (Cs/HAp) composite nanofiber membrane prepared by electrospinning process for the removal of lead, cobalt and nickel ions from aqueous solution was investigated. The prepared nanofiber membranes were characterized by FTIR, SEM and BET analysis. A response surface methodology based on Box-Behnken Design (BBD) was used to predict the average diameter of electrospun nanofibers. In optimum conditions (voltage of 18.90 kV, tip-collector distance of 15.60 cm and flow rate of 0.43 ml/h), the minimum experimental fiber diameter was obtained 198 nm which was in good agreement with the predicted value by the BBD analysis (200.6 nm). Then, the adsorption experiments were carried out to investigate the effect of different adsorption parameters, such as contact time, initial concentration and temperature in a batch system. The kinetic and equilibrium data were well described by pseudo-second-order and Langmuir models, respectively. Thermodynamic parameters were evaluated to obtain the nature of adsorption process onto the Cs/HAp composite nanofibers. The obtained results of reusability of nanofiber membrane after five sorption-desorption cycles offer promising potential in industrial activities. (C) 2013 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.