Abstract: Samples were digested with HNO₃-HF-H₂O₂ in a microwave oven and the contents of rare and rare earth elements in sample solution were determined by ICP-MS. The method has been applied to the determination of rare and rare earth elements in standard reference shale sample (GBW 07107)and standard reference stream sediments(GBW 07305 and GBW 07310). The results were in good agreement with certified values, especially for the standard reference shale sample. The recovery of the method is 97.9％~100.1％ with precision of less than 4％RSD(n=6) for each element. The method provides the advantages of high accuracy, high efficiency, and capability of simultaneous multi-element determination.