Abstract: The silver content determination results need calibration by recovering the silver from the slag and cupel when national standard fire assay gravimetric method is used to determine the silver content in different samples.In the test,the secondary assay by slag and cupel is used to calibrate the silver content determined by fire assay gravimetric method,investigate the materials blending,sampling amount of secondary sample and cupel materials for cupels with different materials,and determine the optimal conditions.3 different samples,namely ore,silver concentrate and lead anode slime are determined.The results show that the precision and accuracy of the method,as well as the applicability,are good.