A simple procedure has been developed for the isolation, concentration and gas liquid chromatographic detection of the volatile compounds in vegetable oils. The votatile compounds are isolated by bubbling purified helium through a measured quantity of vegetable oil heated in an oil bath having a temperature of 350 F. These compounds are collected on activated charcoal and then extracted from the charcoal with carbon disulfide containing an internal standard. The distribution of the volatile compounds is determined with a flame ionization detector. A 400-fold concentration of the volatile compounds is achieved with this procedure. The technique provides good reproducibility (94.3% to 105.5%) and has been successfully used for measuring the increase of volatile compounds in vegetable oils during storage and food production.