Abstract: In this paper a method for separation and preconcentration of trace gold and silver in geological samples with tributyl phosphate （TBP） triphenyl phosphine (TPP) acetic cellulose is developed. The sample was digested with aqua regia and Au and Ag in the sample solution were preconcentrated with tributyl phosphate triphenyl phosphine acetic cellulose in medium of aqua regiaHCl. After eluting with thiourea solution (20 g/L), Au and Ag were determined by inductively coupled plamasatomic emission spectrometry(ICP-AES). Detection limits of the method are 0.001 μg/gwith recovery of 98%~101% for both Au and Ag.