Abstract: Gold industrial wastewater often contains thiocyanate,and there are problems such as higher measurement results and poor repeatability when measuring low concentrations of cyanide.A method for determining low concentrations of cyanide in water containing thiocyanate was developed,using isonicotinic acid-pyrazolone spectrophotometry to measure the cyanide the calibrates cntribution value in thiocyanate in the distillate.The precision of this method is less than 4 %,with spike recoveries ranging from 94 % to 102 %,indicating good accuracy and precision.