Abstract: The accurate determination of gold,an valuation element,in crude silver is significant.A new method for the determination of gold in crude silver by wet separation and enrichment-flame atomic absorption spectrometry was established.The sample was decomposed by nitric acid,substrate silver and other metals were separated by filtration,filter residue was dissolved by aqua regia.In 5 % hydrochloric acid medium,the determination of gold was conducted by flame atomic absorption spectrometry.The mass concentration of gold in 0-8.0 μg/mL has a good linear relationship with the absorbance.The recovery rate of reference material was greater than 98 %,the relative standard deviation was less than 3 % (n=7)and the determination results are consistent with that of lead assay.The method is simple,fast,accurate and reliable,suitable for the determination of gold in crude silver.