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Phenol is a common pollutant found in wastewater, and its allowable discharge limit is 0.5 parts-per-million (ppm). Therefore, it is critical to monitor phenol in the sub-ppm range with high sensitivity and a low limit of detection. Herein, we report a quantitative method for detecting phenol in industrial wastewater through square wave voltammetry (SWV), in which phenol is oxidized to phenoxyl radicals and then became catechol and hydroquinone for detection. By using this method, phenol in the sub-ppm range can be detected reliably over a wide pH range. The sensitivity can be further improved by using a pre-concentration step for phenol before scanning. The method has a limit of detection of 0.1 ppb for phenol. Finally, three graphite electrodes were applied as working, counter and reference electrodes, respectively, in a millifluidic device for continuous detection of phenol in industrial wastewater flowing at 300 μL/min. Because of its simplicity, the sensor can be mass-produced and deployed on a large scale to monitor phenol in industrial wastewater.