Abstract: This paper discusses some main points in atomic absorption spectrometry measurement of gold and silver in rock, mineral and chemistrys exploration of mineral sample. Experiment results and practice experience demonstrate that the need to notice the treating of sample and the existence appearance of the gold and silver, to guarantee the enough representatives with the sample. According to different kinds of mineral, choose proper sample processing method, so as to avoid the occurrence of lose of evaporation, wrapping up, precipitating to adsorb etc. in sample handle processing. It was suggested that measurement of gold and silver of the single mineral should be done continuously, and the adoption of many processing with sour wet method to guarantee the decomposition of the sample, and carry on separation enrich to gather or dilution according to the content, thus satisfy the requirement.