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Distribution coefficients of Zr and Hf cations were determined in aqueous solution at different concentration of sulfuric acid and in presence of some kinds of organic solvents, by a cation exchange solfunated polystyrene resin. The effect of temperature, type and amount of solvent were studied in batch experiments. On the base of extracted results from batch experiments, separation of the mentioned cations were carried out in packed bed of the mentioned resin by a three stage chromatographic elution method. It is concluded that elution of the preloaded resin bed with Zr and Hf solution, by 0.5 N sulfuric acid solution followed by a mixture of 2 to 1 volumetric ratio of 1N sulfuric acid to methanol, can cause outlet of the major part of Zr and, at the final stage, using 2N sulfuric acid Hf cations can cause elution of remained Hf from the bed.