The authors create a titrimetric method of determining niobium in the presence of tantalum. The proposed method permits the determination of niobium in various objects: niobium(V) oxide, technical niobium hydroxide, and columbite concentrate, at various ratios of niobium and tantalum. The data obtained are cited in tables and it can be seen that at the selected ratios of niobium and tantalum in the sample, niobium is virtually entirely determined. Tantalum(IV), vanadium(V), molybdenum(VI), and tungsten(VI) interfere with the determination of niobium.