Abstract: Five acrylates, including methyl acrylate, ethyl acrylate, methyl methacrylate, propyl acrylate and butyl acrylate in soil and sediments were determined by head-space GC. The temperature and time chosen for equilibration of the sample in the head-space vessel were 70 ℃ and 20 min respectively. HP-INNOWAX capillary chromatographic column (30 m×0.32 mm, 0.32 μm) was used for separation, and hydrogen FID was adopted in the determination. Under the optimum conditions, the 5 compounds were separated within 9 min. Linear relationships between values of peak area and mass concentration of 5 acrylates were obtained in the same range of 20.0-2 000 μg·kg-1, with detection limit (3S/N) in the range of 2.0-10.0 μg·kg-1. The proposed method was applied to the analysis of samples of soil and sediment, giving values of recovery found by standard addition method in the range of 86.8%-104%. Values of RSD′s (n=6) were found in the range of 3.5%-5.4%.