In this work, the pyromellitic dianhydride (PMDA)-grafted b-cyclodextrin (b-CD) microspheres have been prepared for the removal of lead and cadmium metal ions in aqueous solution by a batch-equilibration technique. The effects of the pH of the solution, contact time, and initial metal concentration were studied. The adsorption capacities for the two metal ions increase significantly as a large number of carboxyl groups are present on the microspheres surface. The equilibrium process is better described by the Langmuir isotherm than the Freundlich isotherm. The maximum adsorption capacities are 135.69 and 92.85 mg g À1 for Pb(II) and Cd(II), respectively. Kinetic studies show good correlation coefficients for a pseudosecond-order kinetic model, confirming that the sorption rate is controlled by chemical adsorption. The regeneration of the adsorbent can be carried out by treating the loaded microspheres with 0.2 (mol L À1) HCl obtaining high desorption rate for the two metal ions.