The purpose of this study was to compare thermal oxidation of phospholipids with that of triglycerides. Two simple saturated sys‐tems were chosen: 1, 2‐dipalmitoyl‐sn‐glycerol‐3‐phosphoethanolamine and tripalmitoylglycerol. Samples were heated at 150 C for 1 hr in air and the resulting volatile compounds analyzed qualitatively and quantitatively. Alkanes, ketones and lactones were major products in both cases. However, qualitative and quantitative differences were observed. Alkanals were absent in the oxidized phospholipid. This apparently is largely due to their reaction with the amine group as evidenced by thin layer chromatography. In addition, the phospholipid produced 2‐pentanol, 2‐methyl‐l‐pro‐panol and ethyl hexadecanoate; smaller amounts of hydrocarbons and methyl ketones than with the triacylglycerol; and no 1‐alkanols. Mechanisms which could be responsible for these observations are proposed.