Trace level tantalum and rhenium, 182Ta and 186,188Re, have been separated with liquid anion exchanger, TOA from HNO3 medium. The feasibility of the separation process has also been verified for the separation of trace level rhenium from bulk or macro quantity of tantalum. The developed radiochemical scheme will be useful for the separation of carrier-free rhenium radionuclides produced in -particle activated matrix target.