The cathodic reduction of NO À 3 in 1.0 M HClO 4 is investigated by voltammetry at pure Ni and Cu electrodes, and three Cu-Ni alloy electrodes of varying composition, all configured as rotated disks. Voltammetric data obtained using these hydrodynamic electrodes demonstrate significantly improved activity for NO À 3 reduction at Cu-Ni alloy electrodes as compared to the pure Ni and Cu electrodes. This observation is explained on the basis of the synergistic benefit of different surface sites for adsorption of H-atoms, generated by cathodic discharge of H at Ni-sites, and adsorption of NO À 3 at Cu-sites on these binary alloy electrodes. Koutecky-Levich plots indicate that the cathodic response for NO À 3 at a Cu 75 Ni 25 electrode corresponds to an 8-electron reduction, which is consistent with production of NH 3 . In comparison, the cathodic response at Cu 50 Ni 50 and Cu 25 Ni 75 electrodes corresponds to a 6-electron reduction, which is consistent with production of NH 2 OH. Flow injection data obtained using Cu 50 Ni 50 and Cu 25 Ni 75 electrodes with 100-mL injections exhibit detection limits for NO À 3 of ca. 0.95 mM (ca. 95 pmol) and 0.60 mM (ca. 60 pmol), respectively.