Determination of niobium in pyrochlore ore by differential pulse polarography

A differential pulse polarographic method has been developed for the quantitative determination of niobium in pyrochlore ore. One-step polarographic curves were obtained in 0.01 mol L(-1) EDTA as supporting electrolyte. Analytical curves indicated that response was linearly dependent on Nb(V) concentration between 1.6 and 8.6 mg L(-1) in the pH range 2-5. The system is quasi-reversible and controlled by diffusion in 0.01 mol L(-1) EDTA as supporting electrolyte; the electrode process involves one-electron reduction of Nb(V) to Nb(IV). The results obtained so far for niobium in pyrochlore ore were comparable with those obtained by X-ray fluorescence determination. Ions such as Fe(III), Cr(III), As(III), Cu(II), Ni(II), Co(II), Mn(II), Sn(IV), Zn(II), V(V), Ta(V), W(VI), Ce(IV), and Ti(IV) did not interfere. Possible interference from Pb(II) can be avoided by complexation with the supporting electrolyte in the pH range 3.5 to 4.6; Mo(VI) ions can be tolerated when their concentration is one-tenth that of Nb(V).