In the process of gold determination in high antimony and bismuth content materials by conventional lead fire assay,the determination accuracy is poor when the antimony and bismuth mass fraction is over 15 % because antimony and bismuth go into lead button and influence cupellation.The experiment uses stannous chloride for gold reduction and hydrochloric acid for antimony and bismuth separation,and establishes the method of gold determination in high antimony and bismuth content materials by lead fire assay.The experiment investigates the dosage of stannous chloride,hydrochloric acid and auxiliaries.The RSD of the determination results is below 1.95 % and the recovery rate of reference material is 97.4 %-103.0 %.The precision and accuracy are good,meeting the requirement of gold determination in complex high antimony and bismuth content material.