A method for solid phase extraction of Fe(II), Cu(II), and Cd(II) metal ions using Amberlite XAD-2 immobilized with 2-mercaptobezimidazole has been developed. The optimal experimental conditions for quantitative sorption of three metals, pH, and effect of amount of ligand, effect of sample volume, effect of flow rate, concentration of eluent and effect of diverse ions were investigated. The adsorbed metal ions on the adsorbent were quantitatively eluted by 5ml of 3N HCl. The detection limits were 0.42, 0.61 and 0.95μg. L–1 for Fe(II), Cu(II) and Cd(II) respectively. The method was successfully applied for the determination of Fe(II), Cu(II), and Cd(II) metal ions in sewage water and industrial waste waters samples.