A method for sampling and analysis of airborne acetone cyanohydrin is described. The analyte is collected on Porapak QS, a silylated styrene-divinylbenzene porous polymer. Samples are desorbed with ethyl acetate and analyzed by gas chromatography using a nitrogen-specific detector and a teflon column packed with 5% OV-17 on Chromosorb T. The detection limit is estimated to be 0.1 μg/mL acetone cyanohydrin in ethyl acetate. The method was tested by evaporating from 1.0 to 50 μg of the analyte onto sorbent beds of Porapak QS and exposing the samples to a humidified airstream for 15 min. Quantitative recovery was obtained for samples stored for one day at ambient temperature or for seven days if the samples were refrigerated immediately after collection.