Abstract: To determine the Pb, Sn, Mo and V contents in the regional geochemical samples by emission spectrometry, select a mixture of potassium pyrophosphate, sodium fluoride, aluminum oxide and carbon powder as solid buffer, Ge as the internal standard element, and also appropriate analysis line pairs and national first-level geochemical standard materials (GBW stream sediments and soil) for parallel determination(n=12). The test results show that the accuracy meets the specification and test requirements of regional geochemical samples.