Chlorofluorocarbons (CFCs) and hydrochlorofluorocarbons (HCFCs) are fully or partially halogenated paraffin hydrocarbons. CFCs, in the form of polyether polyol mixtures, have been widely used as blowing agents in the manufacture of rigid polyurethane foams (PU) used as insulation products. Owing to the contribution to ozone depletion, the manufacturing and use of CFCs and HCFCs have been phased out under the Montreal Protocol (1987), however, recent studies have found that atmospheric levels of CFCs are significantly higher than expected, suggesting that production and use of CFCs are still on-going. In this study, trichlorofluoromethane (CFC-11), chlorodifuoromethane (HCFC-22) and dichlorofluoroethane (HCFC-141b) in a polyether polyol matrix are investigated using a PerkinElmer Clarus® GC/MS with a TurboMatrix™ HS-40. Instrument method parameters utilized in the study are presented herein, with detailed results demonstrating superior precision, linearity, sensitivity and recovery.