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industrial waste-water and analyzed by GC/MS. To establish the optimal conditions, species of extraction solvent,sample amount, pH of sample, salting out effect, a number of sampling and plunger movement speed wereinvestigated. As a result, the linearities of calibaration curves ranged from 0.9913 to 0.9999, while LODs andLOQs were from 0.05 to 10.0 ng/mL except 2,3,4,5-tetrachlorophenol and pentachlorophenol. Using this method,4-chloro-3-methylphenol confirmed from waste.applicable to detect chlorophenols from industrial waste-water.