Abstract: The sample of surface coating exhaust gas was concentrated with sorbent adsorption. After thermal desorption, GC-MS was applied to the determination of 36 volatile organic compounds in surface coating exhaust gas. The SH-Rtx-624 chromatographic column was used for GC separation and the full scanning mode was adopted in MS determination. Internal standard method was used for quantitative. Detection limits (3S/N) of the 36 volatile organic compounds were in the range of 0.018-2.96 ng. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 84.5%-111%, with RSDs (n=6) of determined values in the range of 1.7%-14%.