A new voltammetric method for the determination of nitrate Ion at a pyrolytic graphite electrode has been developed. It is based on the electrocatalytic reduction of nitrate Ion which occurs at -1.0 V vs. SCE when copper metal and cadmium metal have been electrochemically deposited onto the surface of the working electrode. The presence of iron, chloride, and sulfate Ions, and of organic matter, does not interfere with the analysis, but nitrite ion is reduced at the same conditions. With the sample solution adjusted to contain 0.1 M NaH2P04, 10 µ CdCI2, and 50 µ CuCI2, linear calibration curves are obtained for the concentration range from 1 µ (62 ppb) to 1 mM (62