Nickel microparticles have been dispersed in conducting anion-exchange polymer films coated on carbon electrodes by oxidative electropolymerization of a pyrrole-alkylammonium monomer. Incorporation of nickel metal in polymeric films was effected by electroreduction of polymer coated electrodes in aqueous electrolytes containing nickel-oxalate complexes. The metal deposition process was examined by voltamperometry. Scanning electron microscopy showed a dispersion of metal particles with sizes ranging from 700 to 1200 nm. The electrocatalytic hydrogenation of a variety of cyclohexanones and cyclohexenones at these electrode materials was performed with good current and product yields.