Phenolic compounds are common pollutants in aquatic environments. These pollutants are required to be detected at trace levels by most environment protection authorities. In present studies the GC and MS chromatograms of the solution of 4-chlorophenol, 3-bromophenol, 4-fluorophenol, 4-iodophenol and 3-chlorophenol in MeOH of 50 ppm have been taken. The peaks due to each sample in the GC chromatography is determined and corrected with MS chromatogram. The mixture of the halogenated phenols in MeOH is done and taken the GC chromatogram. As seen from this figure in these condition the halogenated phenols are determined to be well separate by suggest GC-MS method. After this determination, this condition is determined to be applying for a very kind of natural sample. The aim of this study is certain the separation of the synthetic sample with halogenated phenols found to be pollution in the nature.