Simplex optimization was used to optimize the temperature programmed gas chromatographic separation of octane, 2-methyltetrahydrofuran, butylcyclohexane, and ethylbenzene. The initial temperature and the programming rate were the factors studied and a 5 minute time constraint was placed on the system. The Chromatographic Response Function (CRF) used by Deming and Morgan1was used as an operational measure of performance. Further experiments in the region of the optimum and regression analysis of the data obtained were carried out to further understand the factor effects.