In this work, the immobilization of 4-aminoantipyrine onto bentonite was carried out and it was then used to investigate the adsorption behavior of Cr(III). Hg(II) and Pb(II) ions from aqueous solutions. The separation and preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. Under optimum pH value (pH 4.0), the maximum static adsorption capacity of the sorbent was found to be 38.8, 52.9 and 55.5 mg g(-1) for Cr(III). Hg(II) and Pb(II), respectively. 2.0 mL of 2% thiourea in 1.0 M HCl solution effectively eluted the adsorbed metal ions. The detection limit (3 sigma) of this method defined by IUPAC was found to be 0.12, 0.09 and 0.23 ng mL(-1) for Cr(III), Hg(II) and Pb(II), respectively. The relative standard deviation (RSD) was lower 3.0% (n = 8). The developed method has been validated by analyzing certified reference materials and successfully applied to the determination of trace Cr(III), Hg(II) and Pb(II) in water samples with satisfactory results. (C) 2010 Elsevier B.V. All rights reserved.