A process for recovering tantalum and/or niobium metal compounds substantially free of radioactive contamination from an ore containing one or more compounds of said metal or metals and further containing at least one complex of a member selected from the group consisting of uranium, thorium, radium, titanium, and rare earth metals, wherein the crushed ore is first decomposed with hydrofluoric acid at an elevated temperature for more than three hours with substantially all the uranium, thorium, and radium compounds remaining in the residue, and substantially all the tantalum and/or niobium being dissolved as complexes with fluoride, and subsequently said hydrofluoric solution is further treated in an appropriate manner to recover niobium and/or tantalum compounds in said ore.