Abstract: Water sample (200 mL) was extracted with toluene (10.0 mL), and after dehydration with anhydrous Na2SO4, the extract was used for GC analysis, using HP-1 chromatographic column for separation in the temperature range from 60 ℃ to 200 ℃ with programmed temperature elevation. ECD was used in the determination. Qualitative analysis was performed according to the retention times, and quantification was attained by external standard curves. Linear relationships between values of peak area and mass concentration of the 15 nitrobenzene homologues were found in definite ranges, with detection limits in the range of 0.072-0.96 μg·L-1. Tests for recovery and precision were made, giving values of recovery in the range of 92.6%-99.2% and of RSD′s (n=6) ranged from 1.7% to 4.2%.