A method is described for the determination of cyclopropenoid fatty acids in small samples of refined and crude glyceride oils and methyl esters. Approximately 0.5 g of cottonseed oil is titrated with HBr-HOAc by a stepwise procedure at 3 C and 55 C after removal of interfering substances by adsorption on activated alumina. Side reactions occurring to the extent of 15% during the titration were uniform and highly reproducible, permitting application of a correction factor. A procedure is given for preparing methyl esters on a small scale to determine the cyclopropenoid content of highly oxidized oils. © 1970 AOCS Press.