Abstract: Residual amounts of 7 volatile organic compounds, i.e., toluene, ethylbenzene, xylene, hexamethylacetone, 3-ethoxypropionate, 6-methyl-2-heptanone and benzylalcohol in solidified paint were determined by GC-MS. The sample was crushed and extracted (by ASE) thrice with acetone consecutively, at 50 ℃ for 3 min in each extraction. HP-5MS column was used for separation. Linear relationships between values of peak area and mass concentration of the 7 volatile organic compounds were kept in definite ranges, with detection limits (3S/N) in the range of 0.01-1.35 μg. Using blank sample as matrix, test for recovery was made by standard addition method, and values of recovery obtained were in the range of 84.4%-104%, with values of RSD′s (n=6) in the range of 0.80%-13%.