Organophosphorous compounds can be reduced by zinc metal in acidic solution after alkaline hydrolysis. Although phosphates and phosphonates did not evolve any gas, dithioates did evolve hydrogen sulfide and phosphine, thionates and thiolates did evolve only hydrogen sulfide. The evolved gases were qualitatively detected by means of lead acetate and silver nitrate or mercuric bromide papers and determined by spectrophotometrically. The reduction mechanism and analytical method of dithioates were proposed.