A rapid, accurate method for detecting and measuring hydrogen sulfide production during processing of milk products was developed. A gas-liquid chromatograph equipped with a flame photometric detector and a Teflon column containing 40/60 mesh Haloport-F treated with 12% polyphenyl ether and .5% orthophos-phoric acid was used for hydrogen sulfide analysis. Headspace sampling was accomplished by adding 10 ml of water to the milk sample, forcing headspace vapors into a 6-port sampling valve attached to the chromatograph. A 1-ml vapor sample was flushed into the column for analysis. As little as 10 μg of hydrogen sulfide/ml of milk were detected. Instrumental responses were compared to sensory evaluation of several heated milk samples. A correlation was established between hydrogen sulfide in milk headspace and the degree of cooked flavor determined organoleptically.