The paper presents the results of studying tantalum and niobium separation from fluoride solutions after decomposition of tantalite-columbite concentrates. The most efficient separation was found to occur from solutions with a minimal concentration of HF and the H_2SO_4 content of about 200 g/l. The washing of tantalum and niobium solutions by water, HF and H_2SO_4 solutions and niobium and tantalum solutions is discussed in detail. A flowsheet is suggested whereby samples of tantalum and niobium pentoxides with the contents of 22 controlled impurities <0.0001-0.001 w/o each (Nb in Ta_2O_5<0.002w/o, Ta in Nb_2O_5<0.005 w/o) were obtained.
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