The kinetics of the induced codischarge of Mo with Ni in citrate-ammonia electrolytes was investigated by means of polarization and a.c. impedance measurements. Three potential ranges were considered. At low polarization, hydrogen evolution resulting from citrate reduction is the main reaction. The impedance plots exhibit a large capacitive loop with a small high frequency inflection characteristic of the development of a porous layer and a low frequency inductive feature. At intermediate polarization, the partial currents for Ni and Mo discharge increase in the same proportion; the hydrogen evolution is first constant and then rapidly decreases. Then a large low-frequency capacitive feature is observed on the impedance plots, whose size decreases with increasing polarization. At still higher polarization, the Mo discharge becomes increasingly controlled by diffusion which generates an additional capacitive loop. A reaction scheme is proposed which accounts for the polarization data and the major impedance features.