A simple chromatographic procedure for clean separation of the important radionuclide, 99mTc, in the equilibrium mixture, 99Mo--99mWc, has been demonstrated. Separation of pure 99mTc has been achieved by preferential extraction of the radioisotope through an anion exchange resin column of Amberlite IRA-410 using Na-ascorbate solution at pH 7 as an el uent. The radiochemical purity of the separated radiotracer has been verified by taking recourse to T-ray spectrometry. The potentiality of the developed procedure lies in the facts that the eluting agent, ascorbic acid, itself has got its own biomedical importance as Vitamin C and the concerned radioisotope can be obtained in both Tc(IV) and Tc(VII) states as per requirement for diagnostic purposes.