Abstract: The aged adsorption tube （containing Tenax TA and Carbopack X fillers） was connected to the VOCs sampler, and sampling was conducted at the flow rate of 100 mL·min⁻¹ for 10 min. After sampling, the adsorption tube was placed into the thermal desorption-gas chromatography instrument. 15 acetate compounds were separated on the DB-5 capillary chromatographic column using a heating program, detected by a hydrogen flame ionization detector, and quantified by the external standard method. As shown by the results, linear relationships between values of corresponding peak area and masses of 15 acetate compounds were kept in the range of 25.0‒1 000 ng, with detection limits （3.143s） in the range of 0.003‒0.009 mg·m⁻³. Test for recovery was made by the standard addition method, giving results in the range of 93.7%‒111%, with RSDs （n=6） of the determined values in the range of 0.80%‒8.8%. This method was applied to the analysis of an actual sample, and ethyl acetate, n-propyl acetate, and n-butyl acetate were detected, with the detection amounts in the range of 1.00‒1.07 mg·m⁻³, 0.51‒0.70 mg·m⁻³, and 0.20‒0.28 mg·m⁻³, respectively, which were consistent with the components of the raw and auxiliary materials used in the emission sources.