Abstract: In the fire assay test of silver in silver concentrates,the general recovery of silver is about 98.9 % due to the loss of silver in the cupellation process.In the experiment,a small amount of lead was left near the end of the cupellation process.The lead beads were extracted by water-cooling method and were dissolved by nitric acid before titrated with potassium thiocyanate.The results of conditional test show that the optimal cupellation temperature is 880 ℃,the amount of lead retained is 2.0-3.0 g and that less silver content in samples lead to higher silver loss rate.The RSD of the determination results is less than 1.50 %.The recovery rate of silver 99.83 % is higher than that of non-lead-retaining cupellation method.The method reduces silver loss in cupellation and the determination results are more accurate.