A simple solid phase extraction procedure on cation exchange resin Purolite C100 is presented. The procedure based on a column technique for separation and recovery of lead ions from synthetic binary mixtures. Equilibrium distribution coefficient, k(d) for the different metal ions such as Al(III), Fe(III), Ba(II) and Pb(II) in the presence of nitric acid and ammonium acetate solutions of variable concentrations was determined at 25 degrees C. The values of separation factor, alpha were evaluated. Quantitative separation of lead ions from a synthetic binary mixtures are based on the fact that ammonium acetate is a good elute for lead ions but fails to elute the other cations. (C) 2008 Elsevier B.V. All rights reserved.