This is an integrated polarographic and potentiostatic study on the mechanism of the cathodic reduction of m‐dinitrobenzene for various pH values of aqueous electrolytes. The polarographic results confirmed previous results of a two‐stage reduction involving four electrons in each step. The supporting coulometric work was performed potentiostatically at a graphite cathode under a nitrogen atmosphere at a controlled potential of −0.48v on a solution of pH 6.00. The product of the first step, 3‐nitrophenylhydroxylamine, was quantitatively isolated and identified for coulometric equivalencies of 25, 50, 75, and 90% reduction.