AbstractA rapid and convenient volumetric method is reported for the estimation of chromium (VI) and vanadium (V) in mixtures. The procedure consists in the estimation of (1) chromiumplusvanadium in the mixture by titration of the mixture in about 0.25Nsulfuric acid containing 5 ml of phosphoric acid and 1 ml of 0.1% barium diphenylamine sulfonate with ferrous ammonium sulfate to the exact end‐point; (2) vanadium in the mixture by titration of the solution, left after the first titration, with permanganate, using ferroin as indicator, and (3) chromium in the mixture by calculation from the difference of the two value