Freons from an aerosol spray can were detected in the blood, liver, brain, and lung of a 14-year-old girl who died after intentional inhalation. A headspace mass spectrometric analytical technique was employed to detect the fluorocarbons. The spectra from the specimens showed the presence of m/e peaks at 101, 103, and 105 from the ion (CFCL2)+ which arises from fragmentation of trichlorofluoromethane (Freon 11) and dichlorodifluoromethane (Freon 12), and peaks at 85 and 87 from the ion (CF2Cl)+ which arises from fragmentation of dichlorodifluoromethane (Freon 12). The technique presented here provides greater specificity than previously reported analytical procedures for the identification of these volatile toxic chemical compounds in biological specimens.