A headspace-gas chromatographic procedure, with nitrogen-phosphorous (N-P) specific detection for the determination of acrylonitrile (AN) in cold pack cheese, peanut butter, honey butter, and margarine, was collaboratively studied. Seven laboratories analyzed 7 samples of each food for AN at levels ranging from 5 to 60 ppb. For cold pack cheese, mean recoveries for AN added at about 5, 15, and 50 ppb were 65.9, 92.4, and 96.6%, respectively; for peanut butter, mean recoveries for AN added at about 10, 30, and 60 ppb were 59.6, 61.7, and 66.5%, respectively; for honey butter, mean recoveries for AN added at 5, 15, and 50 ppb were 88.6, 96.4, and 94.6%, respectively; and for margarine, mean recoveries for AN added at 5, 15, and 50 ppb were 130.6, 91.9, and 88.7%, respectively. The overall coefficients of variation for cold pack cheese, peanut butter, honey butter, and margarine spiked at the above levels were 67.7, 22.0, and 38.5%; 71.8, 23.8, and 23.8%; 45.3, 30.4, and 13.0%; and 79.7, 38.9, and 16.2%, respectively.