The present study involves the development of solid-phase extraction (SPE) procedure for the preconcentration of trace amounts of copper (Cu2+), iron (Fe3+) and zinc (Zn2+) ions on duolite XAD 761 modified by bis(2-hydroxyacetophenone)-2,2-dimethyl-1,3-propanediimine(BHAPDMPDI). The complexation between the metal ions and the proposed ligand was investigated potentiometrically. The metal ions retained on the sorbent were quantitatively determined via complexation with BHAPDMPDI. The complexed metal ions were efficiently eluted using 6 mL of 4 mol L-1 nitric acid in acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ions were optimized. Using the optimized parameters, the linear response of the SPE method for Cu2+, Zn2+ and Fe3+ ions were in the ranges of 0.01-034, 0.01-0.28 and 0.02-0.31 mu g mL(-1), respectively, and the detection limits for Cu2+, Zn2+ and Fe3+ ions were 1.8, 1.6 and 2.4 mu g mL(-1), respectively. The proposed method exhibits a preconcentration factor of 208 for all of the ions studied and an enhancement factor for Cu2+, Fe3+ and Zn2+ ions of 34, 28 and 38, respectively. The presented results demonstrate the successful application of the proposed method for the determination of these metal ions in some real samples with high recoveries (>95%) and reasonable relative standard deviation (RDS<5%). (C) 2013 Elsevier B.V. All rights reserved.