Determination of tungsten with iron(III) after reduction with mercury in thiocyanate medium

Tungsten(V) is formed by shaking for 2 min sodium tungstate solution in 0.4 M potassium thiocyanate-4M hydrochloric acid medium, with mercury. It is titrated with standard iron(III) solution. The thiocyanate present stabilizes W(V) to aerial oxidation and also acts as indicator. The W(V) can also be titrated potentiometrically in 7M hydrochloric acid, a tungsten wire electrode being used. Fe, Ni, Cr, Zr, Bi, Sb, Ce, Al, Pb, Ca and U do not interfere. Cu, V and As can be tolerated up to 5 mg. Co, Mo, Re, Nb and Mn interfere, but not in the potentiometric determination. The method is direct, simple, rapid, accurate and reproducible.