A new method for preconcentration of ultratrace amounts of Co (II), Ni(II) and Cu(II) ions in various matrices has been proposed. The method is based on the adsorption and chelation of the metal ions on Amberlite XAD-4 resin modified with Quinol via azotisation prior to their determination by standard spectrophotometric method. The effect of pH, type, concentration and volume of eluent, sample volume,flow rates of sample and elution solutions, and interfering ions have been investigated. The optimum pH for retention of the metal ion were10.0, 7.0 and 7.0 respectively. Eluent for quantitative elution was 5 ml of 2 mol l−1 HCl. The optimum sample and eluent flow rates were found to be 2.5 ml min−1. The sorption capacity of the resin was found to be 0.60, 0.45 and 0.52mmolg-1 for Co (II), Ni (II) and Cu (II) respectively. The preconcentration factor of the method was 250 for all the metals. The detection limit values were in the range of 3.0- 5.0 µgl-1. The accuracy of the method was confirmed by analyzing standard synthetic mixtures and standard addition methods. This procedure was applied to the determination of Cobalt, Nickel and Copper from various water samples and SRM’s.