A method for determination of trace silver in stream sediments, soils and rocks by graphite furnace atomic absorption spectrometry (HNO₃-H₂O₂) was developed in this study. The microwave digestion and instrument working parameters were optimized and the optimum conditions were determined. In traditional method, determination of trace silver in geochemical exploration samples is conducted by graphite furnace atomic absorption spectrometry through heating the hydrochloric acid nitric acid hydrofluoric acid and perchloric acid electric heating plate digestion, with iridium, platinum as matrix modifier; the analytical process is complex, and the cost is high. Compared with the electric heating plate digestion method, the microwave digestion technique is characterized by high-pressure closed digestion with small amounts of acid, complete digestion and less loss in the digestion process. In this paper, HNO₃ (65%) and H₂O₂ microwave digestion was used to dissolve the matrix interference by adding 12 g/L thiourea as the medium. The detection limit was 0.018 μg/g, and the analytical method was used for verification of sediment reference materials (GBW07309, GBW07311), soil standard substance (GBW07402, GBW07404) and rock reference materials (GBW07103, GBW07104). The measured results were consistent with the recommended values, the accuracy of lgC (GBW) is △lgC(GBW)≤±0.024, RE(GBW)≤±5.71%, the precision of RSD (GBW) is ≤5.97%. The method is suitable for the determination of trace silver in a large amount of geochemical samples.