The electrocatalytic activity of several materials for the nitrate reduction reaction was studied by cyclic voltammetry on a rotating ring disc electrode in solutions with different concentrations of sodium bicarbonate. Copper exhibited highest catalytic activity among the materials studied. Nitrate reduction on copper was characterized by two cathodic shoulders on the polarization curve in the potential region of the commencement of hydrogen evolution. In this potential range an anodic current response was observed on the Pt ring electrode identified as nitrite to nitrate oxidation. This indicates that nitrite is an intermediate product during nitrate reduction. These conclusions were verified by batch electrolysis using a plate electrode electrochemical cell. Copper and nickel, materials representing the opposite ends of the electrocatalytic activity spectra, were used in batch electrolysis testing.