A process for separating perfluoro compound gas or vapor from another gas, typically nitrogen, in a gas mixture. The process involves a combination of membrane separation and condensation, and is particularly useful in the semiconductor industry, for treating exhaust gases from cleaning of chemical vapor deposition chambers. Operation of the condensation step at temperatures no lower than about -30.degree. C. reduces the need for refrigeration equipment and controls the amount of gas dissolved in the recovered perfluoro compound.