An experimental study of the separation of 1,2,4- and 1,3,5-trimethylbenzenes from a mixture containing the weight composition 56% 1,2,4-trimethylbenzene and 44% 1,3,5-trimethylbenzene on molecular sieves 13X in high pressure carbon dioxide was performed. For a pulse of 1.18 cm(3) of trimethylbenzene isomers and 40 g of molecular sieves 13X, the effects of pressure, temperature, and flow rate on separation effectiveness were examined. The results indicated that the most appropriate operating conditions for obtaining a higher recovery of each isomer with a purity of at least 98% and a shorter mean retention time for 1,3,5-trimethylbenzene were a temperature of around 363 K, a pressure of 74.8 atm, and a flow rate of 15.0 cm(3)/min.