The adsorption behaviour of La/Ce system on Dowex 50W-X8 in different media, namely, nitric acid, acetate buffer and citrate buffer was studied as a function of the concentration of nitric acid and buffer pH. In addition, in cation-exchange column chromatography experiments, three different eluants, namely, citrate buffer of pH 5.5, 0.1 M EDTA and 0.2 M α-HIBA, were employed for separation of Ce(III) from La(III). The optimum conditions for improvement of radiochemical separation of no-carrier-added 139Ce from proton irradiated lanthanum were applied using the most suitable chelating agent 0.2 M α-HIBA. The purification of 139Ce from macro amount of La(III) was done using two columns in a sequence. The target was prepared by pressing. The production of high radionuclidic and chemical purity 139Ce via irradiation of lanthanum oxide target at MGC-20 cyclotron of proton energy 14.5 MeV was described. The experimental yield was found to be 200 kBq/μA h.