Abstract: Head-space GC was applied to the determination of methanol in air. The equilibrium temperature and time of head space were set at 75 ℃ and 60 min respectively, with 2 mL of the sample in head-space bottle. The analyte were separated on DB-WAX column and detected by FID. Linear relationship between values of peak area and mass concentration of methanol was kept in the range within 91.20 mg·L-1 with detection limit (3s) of 1.8 mg·L-1. Tests for recovery were made at the concentration levels of 11.40,22.80 and 45.60 mg·L-1 of methanol standard, giving values of RSD′s (n=6) in the ranges of 2.6%-3.4%. The rate of desorption found was in the range of 96.5%-98.2%.