Recently, the air pollution in A and B industrial area has become one of the most important issues, then 60 VOCs in the area were measured using a highly sensitive method. The VOCs were adsorbed onto Carbotrap using air sampler and subsequently desorbed by a thermal desorber system into gas chromatograph-mass spectrometry (TDS-GC-MS). The peaks of all compounds had good chromatographic properties and offered very sensitive response for the EI-MS (SIM). Method detection limits (MDL) ranged from 0.01 to 0.1 ppt(v/v), and linearities of calibration curves were over 0.995. We analyzed total 90 atmosphere air samples of A and B industrial complex using the method. Benzene, toluene, ethylbenzene, xylene, n-hexane, fluorotrichloromethane, carbon tetrachloride, 1,2-dichloroethane, 1,1,1-trichloroethane, trichloroethylene, tetrachloroethylene, styrene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene, sec-butylbenzene and naphthalen were identified as the major compounds in the air, and their average concentrations were 0.81, 5.02 1.30, 3.0, 0.81, 37.9, 0.07, 0.15, 0.15, 0.79, 0.06, 0.33, 0.03, 0.12, 0.23, and 0.35 ppb(v/v), respectively. The concentrations of VOCs were low in summer and high in fall or winter. When the concentrations detected in air compare with WHO's norm, no case exceed it.