Objective To establish a flow injection analysis method for simultaneous determination of volatile phenol and cyanide in tap water. Methods The tap water was pretreated by a mixed solution of EDTA and ascorbic acid (20.0 g/L), and the flow injection analyzer was used for simultaneous determination of volatile phenol and cyanide. Results The result show that the mixed solution of EDTA and ascorbic acid (20.0 g/L) of 0.5 ml in 50 ml tap water was the best pretreatment. The recovery rate of the tap water was 90.0%-105.0%, and the relative standard deviation was 0.39%-5.85%. The detection limits of volatile phenol and cyanide were 0.000 2 and 0.000 4 mg/L. Conclusion This method showed good precision, high accuracy, and met the requirements of quality control.