The composition of anode mud samples is complex,which poses challenges in accurately determining antimony.The cerium sulfate titration method was used to determine antimony in anode mud.Hydrogen peroxide was used to disrupt the complex chemical reactions between arsenic,antimony,and bismuth,ensuring complete oxidation of antimony.Nitric acid-tartaric acid mixed acid was used to suppress the hydrolysis of antimony and assist in sample dissolution.If the sample contains excessive carbon,nitric acid was added dropwise to remove carbon during the emission of white smoke from sulfuric acid,followed by nitrate removal using urea.Methyl orange-methyl blue dual indicator was used during titration for a more distinct color change at the endpoint,ensuring more accurate judgment.The relative standard deviation of the results obtained from this method ranged from 0.16 % to 0.37 %,with a recovery rate of standard substances ranging from 98.40 % to 101.20 %.The method demonstrates good accuracy and precision,meeting analytical requirements.