Removal of lead from aqueous solution with chitosan/PVA (poly(vinyl alcohol)) hydrogel beads was studied in batch adsorption experiments at various solution pH values (2-7.6). Lead adsorption on chitosan/PVA beads was found to be strongly pH-dependent and displayed a maximum uptake capacity at pH around 4 and a minimum at pH about 6.4. zeta-Potential study indicated that chitosan/PVA beads possessed positive zeta-potentials at pH < 6.3 and negative zeta-potentials at pH > 6.3. Hence, adsorption occurred even though the interaction between lead and chitosan/PVA beads was electrostatically repulsive at pH < 6.3. Complexation, ion exchange, and electrostatic interaction are all believed to play a role in lead adsorption on chitosan/PVA beads, but the relative importance of each of these mechanisms varies with solution pH values. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy spectra suggested that lead adsorption was mainly through interactions with the N atoms in chitosan in the pH range studied.