In the intensive cyanidation of gravity gold concentrates, sodium m-nitrobenzene sulfonate (NBS) is often used to supplement dissolved oxygen as the oxidant in the process. This paper presents the results of a largely electrochemical study of the behaviour of NBS during cyanidation. The results have confirmed that NBS acts as an oxidant in the cyanidation of gold and that the mixed potential model can be applied to describe the mechanism of its action.The mixed potential is a good initial indicator of the rate of gold dissolution and, as expected, the anodic dissolution of pure gold in cyanide solutions is characterized by passivation at potentials above about −0.35 V.The reduction of oxygen under the conditions of the present study occurs in two 2-electron steps with peroxide as an intermediate. Dissolution of gold occurs at potentials in the diffusion-controlled region for the first step. The cathodic reduction of NBS occurs in the same potential region as the reduction of oxygen. The reaction is first order in the concentration of NBS and is largely independent of the pH. The stoichiometry of the reaction involves six moles of gold per mole of NBS confirming that the amine is the final product of reduction of NBS.Rates of gold dissolution in various solutions have been measured using a calibrated linear polarisation method. The rate increases approximately linearly with increasing NBS concentration and is independent of pH. The rate in 0.5 g/L NBS is approximately the same as in oxygenated solutions.A relatively simple titration has been adapted for use in determining NBS concentrations.