Abstract: GC was applied to the determination of methyl tertiary butyl ether in industrial waste gases. The sample was absorbed by charcoal tube and desorbed by CS2. The analyte was separated on FFAP quartz capillary column (50 m×0.32 mm, 0.5 μm), and detected by FID. Linear relationship between values of peak area and mass concentration of methyl tertiary butyl ether was kept in the range of 1.48-185 mg·L-1, with detection limit (4S/N) of 0.3 mg·L-1. Precision of the method was tested at 3 concentration levels for 6 determination, values of RSD′s found were in the range of 2.6%-5.7%. The sample can be kept stable for 8 d, at 6 ℃.