Abstract:A gravimetric method for the determination of gold and silver in crude bismuth by bismuth - fire assay was established. The crude bismuth roasting oxidation first, and then dissolved in acetic acid crude bismuth oxide, filter to remove bismuth, to eliminate the influence of bismuth against fire assay method, after sediment ashing, ingredients, high temperature melting, molten metal lead capture precious metals in a sample form clasp, button will lead ash blowing, get the gold and silver grain, nitric acid dissolved in separating gold, gold content was determined by gravimetric method. The method has high accuracy and precision, and the recovery of gold is 99.21-100.50% and silver 98.18-99.72%. It can satisfy the determination of gold and silver in coarse bismuth well.