The test of volatile phenol in water often uses traditional manual methods for pretreatment, distillation and liquid-liquid extraction, but the operation is cumbersome and inefficient. This report is based on the national standard method and uses the new STEHDB-106-3RW intelligent integrated distiller and STC-302B automatic liquid-liquid extractor for operation, which is simple, convenient and fast, and the experimental results have proved to be reliable.