Objective: To establish a method for the determination of acetylacetone in the air of workplace by gas chromatography. Methods: In August 2020, acetylacetone in the air of workplace was collected by silica gel tube, eluted with methanol, separated and detected by gas chromatography with flame ionization detector. The detection limit and precision of the method were also analyzed. Results: The linear range of acetylacetone was 1.95-1950.60 μg/ml with the regression equation of y=0.815x-3.667, and the correlation coefficient was 0.99993. The limit of detection of the method was 0.18 μg/ml and the minimum detection concentration was 0.12 mg/m(3) (collected sample volume was 1.50 L). The within-run precisions were 1.08%-4.11% and the between-run precisions were 1.98%-2.80%. The desorption rates were 99.68%-100.45%. The sealed samples could be kept at least 15 days at room temperature without significant loss. Conclusion: The solvent desorption-gas chromatography method for the determination of acetylacetone has good precision, high sensitivity and simple operation, and is suitable for the determination of acetylacetone in the air of the workplace.