Abstract The influence of the chemical composition and structure of nickel base alloys on their catalytic activity was examined using the electrochemical reduction of 1-nitropropane as a test reaction. The electrocatalytic activity of cathodes consisting of crystalline and amorphous Ni-alloys, respectively, with systematically varying composition was analyzed. Aluminum, iron, and palladium were added as alloying elements. The effects of the nonmetallic components of the amorphous alloys, i.e., boron and silicon, which are required as glass formers, were also assessed. The results are discussed in terms of the effects of alloy composition and structure of the cathode materials on electrocatalytic hydrogenation and the electron transfer/protonation process at the cathode as a test reaction.