Iproniazid was found to be irreversibly reduced in two steps, involving the exchange of two electrons and two protons each, by using tast polarography, normal pulse polarography (NPP), and cyclic voltammetry (a7). The rate constants of these two steps were found to be 5.8 x and 4.2 X and 4.2 X cm s -I , respectively, and their corresponding diffusion coefficients 4.5 X lo-' and 8.3 X lo-' cm' s-I. Also, a, the coefficient of cathodic transfer, m7as found to be 0.20 to 0.25 for the first peak and 0.17 to 0.15 for the second. On the basis of the electrochemical study performed, a differential pulse polarographic method for the determination of iproniazid over the concentration range of j X 10-M to 1 X lo-' M was developed.