Abstract: Amounts of nitrobenzenes in water sample were determined by GC with microelectron capture detector. Nitrobenzene compounds in water sample were extracted with a mixture of ethylacetate, benzene and diethyl ether (2+1+0.02), and separated on HP-1701 capillary column (30 m×0.25 mm, 0.25 μm). The 9 nitrobenzenes were separated within 11.5 min. Linear relationships between values of peak area and mass concentration of the 9 nitrobenzenes were obtained in the same range of 0.001-5.0 mg·L-1. Test for recovery was made by standard addition method, giving recovery in the range of 92.0%-108% with RSD′s (n=5) less than 5.0%.