Abstract: As described in the paper,volatile phenols in waste water sample were prederivatized with bromine and separated by extraction with cyclohexane.An aliquot of the extract was taken for GC analysis and 4 compounds,namely ① phenol and 3 derivatives of methyl phenol (i.e.② ortho,③ meta and ④ para methyl phenol) were determined.Relationships between peak area and concentration of the 4 compounds mentioned above were obtained in the following ranges with their detection limits (S/N=3) in the parenthesis: ① 0.008~80 μg·L-1 (8.4 ng·L-1),② 0.010~100 μg·L-1 (10.6 ng·L-1),③ 0.018~100 μg·L-1 (19 ng·L-1) and ④ 0.012~100 μg·L-1 (12.8 ng·L-1).Results of recovery and precision tests obtained were as follows: values of recovery were in the range of 87%-98%,and values of RSD′s (n=6) were in the range of 4.0%-7.0%.