A simple titrimetric method has been developed for the determination of aldehydes and keto- nes. The method is based on the reaction of hydroxylamine hydrochloride in alkaline medium with carbonyl group to form the corresponding oxime. Excess hydroxylamine was determined by titration with ferricyanide solution with or without phenolphthalin as indicator. Acetaldehy- de, p-nitrobenzaldehyde, salicylaldehyde, benzaldehyde, Anizaldehyde, cyclohexanone, methyl ethyl ketone, ethyl-acetoacetate, acetylacetone and acetophenone give satisfactory results with maximum error 2.67 % and an average recovery of 101.45 %.