A qualitative and semi-quantitative method was established for the investigation of low-molecular-weight volatile carbonyl compounds in cigarette whole smoke. The carbonyls were trapped on a silica gel "column" and eluted with water. The aqueous solution was then treated with benzyloxyamine to form the corresponding oximes, which were then separated on a short (12 m) FFAP glass-capillary gas chromatographic column with temperature programming, and detected by a nitrogen selective detector. An internal standard was added both as a reference for retention time determinations, and as an aid in estimating the amounts of the individual carbonyls in the smoke samples.