Part-per-billion levels of cyanide react rapidly and quantitatively with excess Iodine at pH ~6.0 to form Iodine cyanide. The excess Iodine Is selectively removed from solution by nitrogen purging. Acidification of the resultant iodine cyanide solution with perchloric acid In the presence of iodide to a final concentration of 3.0 M HCI04 and 1.0 X 10~4 rapidly and quantitatively regenerates Iodine in an amount equivalent to the original cyanide. This iodine is transferred to the gas phase by purging with nitrogen, where It Is determined at a gold gas porous electrode by electro-oxidation to lodate. The detection limit for cyanide is estimated to be 5 ng In a 4-mL sample.