A method of removing niobium from a uranium-niobium alloy includes dissolving the uranium-niobium alloy metal pieces in a first aqueous solution containing an acid selected from a group consisting of HCl and H.sub.2 SO.sub.4 and a fluoboric acid as a catalyst to provide a second aqueous solution which includes uranium (U.sup.+4), acid radical ions, the acids and insolubles including uranium oxides and niobium oxides; adding nitric acid to the insolubles to complete the oxidation of the niobium oxides to yield niobic acid and further solubilizing thr uranium oxide; and separating the niobic acid, nitric acid and solubilized uranium oxides.