Abstract: GC-MS was applied to the determination of 7 benzene homologues in automobile materials. HP-5MS chromatographic column was used for GC separation and modes of full-scanning and selected ion monitoring were adopted in MS determination. Deuterated benzene-D6 was used as internal standard. Linearity ranges of the 7 benzene homologues found were in the same range of 10-1 000 ng with detection limits (3s) in the range of 9-18 ng. RSD′s (n=6) of analytical results for the benzene homologues found were in the range of 0.81%-2.4%, and values of recovery found by standard addition method were in the range of 99.0%-102%.