A method combining steam distillation, elevated-temperature purge-and-trap, and nitrogen-specific detection has been developed for detection of low and sub-parts-per-billion levels of acrylonitrile in aqueous systems. Steam distillation effects a sample cleanup and concentrates acrylonitrile. Combination of the elevated purge-and-trap technique with a thermal N-P detector provides selective and sensitive detection. The method has been validated for acrylonitrile In water over the range of 10 ppt to 10 ppb. Several applications of the technique are Included.Acrylonitrile (AN, 2-propenenitrile) is used in the manufacture of fibers, elastomers, resins, and latexes and in the synthesis of other chemicals, primarily adiponitrile and acrylamide. Evidence of AN toxicity can be found in the