A practical process has been developed for the preparation of high-purity, ductile columbium metal. The process consists of reducing Cb2O5 with aluminum powder in a “bomb”-type reduction. The massive columbium contains approximately 2 wt % Al and 0.8 wt % O2. These impurities, along with nitrogen and iron, can be satisfactorily removed in subsequent treatments by volatilization. Much of the impurities in the as-reduced columbium can be removed by heating in vacuum to 2000°C for 8 hr, leaving a sponge. These impurities may also be largely removed by heating for a shorter time at 2200°C; however, some loss of the columbium is encountered. Heating to 1800°C for 8 hr was found to be less efficient for impurity removal.