Selected volatile organic species, including chloroform, 1,2‐dichloroethane, 1,1,1‐trichloroethane, benzene, carbon tetrachloride, trichloroethylene, tetrachloroethylene, p‐dichlorobenzene, o‐dichlorobenzene, and nitrobenzene, are determined in ambient air by collection and concentration on Tenax‐filled traps. The samples are recovered for analysis by a novel thermal desorption system which allows the injection of an aliquot of the sample into a 50M fused silica methyl silicone gas chromatographic column, which is programmed from ‐90 to 140° C. A standard addition process for qualitative analysis and an external standard method for quantitation are described, both using compressed gas standards. GC/MS is used for confirmation of sample identity on approximately 10% of the samples.