An atomic absorption spectrometric method with a preconcentration and separation procedure using a DETA (diethlyenetriamine) polymer is proposed for the determination of Cd, Cu and Zn. The influence various experimental condition on retention and elution efficiencies of the analyte were investigated by applying batch and column techniques. All investigated elements were quantitatively retained at pH 3, then were completely recovered by means of nitric acid. The loading capacity of the DETA polymer is 5.2 mg Cu2+/g polymer. A contact time of one minutes is sufficient for quantitative retention and elution which is shorter than for many Other sorbents. In the presence of sodium chloride up to 0.5% the analyte elements were quantitatively Separated and recovered.