The direct titration of alkaline ferricyanide in presence of zinc sulfate with hydroxylamine sulfate has been studied. A clear white precipitate of zinc potassium ferrocyanide indicates the end-point. Hydroxylamine is oxidized to nitric acid and water, and millingram-quaantities of hydroxylamine; can be determinred. In the absence of zinc sulfate and in weakly alkaline medium, hydrazine and hydroxylamine are converted to nitrogen, while in presence of zine sulfate hydrazine is oxidized to nitrogen By ferricyanide oxidation of a mixed sample uinler different conditions, hydrarine and hydroxylamine when present together can be determined rapidly.