A method for determining thiocyanate in cyanide residue has been developed.Through experiment on test conditions,it was determined that a 0.8 % sodium hydroxide solution should be used as the leaching agent,with the leaching process involving ultrasonic extraction for 5 min followed by heating on a hot plate at 180 ℃ for 1 h.Thiocyanate was then measured using the ferric salt colorimetric method.The relative standard deviation of this method ranged from 0.12 % to 0.93 %,with spiked sample recovery rates between 95.46 % and 100.50 %.This method has been widely applied for the determination of thiocyanate in cyanide residue within the gold industry.