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A radiochemical separation method was developed for the separation of 109Cd from a nat.Ag target (6.6 g, pressed into a 19 mm disc). The method comprised of two stages. In the first stage, after dissolution of the target in nitric acid, silver was separated from Cd by precipitation into the metallic form using 20 g of Cu turnings for the reduction of Ag+ ions. In the second stage, 109Cd in the filtrate, that contained trace amount of silver and substantial quantity of Cu(I), was purified by use of a Bio-Rad AG1-X10 anion-exchange resin. The ion-exchange chromatography employed a column with (1.6 cm i.d. and 4 cm length) with a flow rate of 2 ml/min throughout the separation. 109Cd was quantitatively recovered from the first stage and the recovery yield from the ion-exchange chromatography was greater than 96%. 2M HCl containing H2O2 was used for the adsorption of 109Cd and elution of Cu. 109Cd was eluted by 50 ml 1M HNO3. The concentrations of stable isotopes of Ag and Cu in the final solution (5 ml 0.05M HCl) were measured by an ICP-OES method and found to be <1 ppm.