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In this paper, a new method for determination of volatile phenol in water was studied with a novel solid phase extraction on a centrifugal microfluidic device and phenol-4-aminoantipyrine spectrophotometry. The detection limit was obtained with 2 mg L-1, and the linear range was from 2.00 to 80.0 mg L-1. This method is suitable for the determination of high concentration of phenol in waste water samples.