A simple ion exchange procedure for clean separation of the biomedically important radionuclide,90Y, in the equilibrium mixture,90Sr−90Y, has been demonstrated. Separation of90Y in the carrier-free state has been achieved by preferential elution of the radiotracer through a cation exchange resin column of Dowex-50W-X8 with freshly prepared Na-ascorbate solution of <1% concentration at pH7. The radionuclidic purity of the separated90Y has been verified by taking recourse to the studies of beta decay curves. The procedure developed has the added advantage that the complexing reagent, ascorbic acid, itself has got its own biomedical importance as vitamin C and the technique can also conveniently be used as a generator for the isotope90Y.