A process for the separation of 99mTc from molybdenum targets is described. The method for separation of 99mTc isotope from molybdenum targets includes: i) providing an initial multicomponent mixture of elements, the mixture containing 99mTc; ii) dissolving the multicomponent mixture of elements with an oxidizing agent to oxidize the mixture of elements; iii) heating the mixture of elements at a temperature sufficiently high enough to sublimate a vaporized compound containing 99mTc; iv) condensing the vaporized compound containing 99mTc to form a reaction product; v) adding a base to the condensed reaction product to dissolve the 99mTc containing reaction product to form sodium pertechnetate (Na99mTcO4); and vii) purifying the crude solution of sodium pertechnetate Na99mTc04 using column chromatography to provide the 99mTc isotope as a radiochemical compound.