Abstract: The accurate determination of gold, an valuable 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.