Abstract-A new analysis method of gold in sulfate leaching solution is introduced in this paper. Hydrochloric acid is added into solution to decompose thiosulfate for quickly and effectively undermining the gold thiosulfate complex. In the medium of aqua fortis, gold is adsorbed and separated by mercapto group resin. After elution, isoamyl alcohol is used as extractant to enrich and separate Au3+ from solution. In HAc-NaAc buffer solution, CTMAB and TMK are used to determine the gold concentration in solution. In this method, mercapto group resin adsorption technology and isoamyl alcohol organic extraction technology are used together. The minimum determination concentration of Au is 0.2mg / L. The precision is better than ±± 2.5%. The recovery rate is 94% -100%. Because of rapid analysis process and high sensitivity, this new method has been used to test control analysis with fine results.