This work describes a procedure for the separation-preconcentration of Fe(III), Pb(II) and Cr(III) from some water samples using a column-filled Amberlite XAD-2000 resin. The analyte ions retained on the column were eluted with 0.5 mol L-1 HNO3. The analytes in the effluent were determined by atomic absorption spectrometry. Several parameters governing the efficiency of the method were evaluated including pH, resin amount, sample volume, flow rates, eluent type and divers ion effects. The recoveries under the optimum working conditions were found to be as 100 +/- 1% Fe, 96 +/- 1% Pb and 93 +/- 2% Cr. The relative standard deviations and errors were less than 2% and 5%, respectively. The detection limit based on three standard deviations of the blank was found to be 0.32, 0.51 and 0.81 mu g L-1, for Fe, Pb and Cr, respectively. The procedure was applied to the determination of Fe, Cr and Pb in hot spring water and drinking water samples. (c) 2007 Elsevier B.V. All rights reserved.