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The composition of matte is relatively complex, if the content of noble metals is directly determined by inductively coupled plasma atomic emission spectrometry after acid dissolution, the content of impurity elements is too high, the interference is serious, leading to the large deviation of results. In this experiment, the lead assay method was first used to remove most of the impurity elements in the matte sample in a high-temperature molten state to enrich the precious metal into the lead buckle, and then the lead was removed from the lead buckle to obtain the precious metal particles after ash blowing. The results were corrected using second assay, the combined particles were dissolved in nitric acid to separate gold from other elements, and the mass of the gold particles was weighed, added an appropriate amount of hydrochloric acid solution to the gold separation solution and continued heating treatment, and then the concentrations of gold, lead, bismuth, copper, and palladium in the gold separation solution were measured by inductively coupled plasma atomic emission spectrometer under selected optimal instrument operating conditions. The contents of gold, silver, and palladium in the matte sample were calculated using the given formula. The effects of lead oxide dosage, ash blowing temperature and matrix interference on the determination results were discussed. When the amount of lead oxide added was 200 g and the ash blowing temperature was 890 °C, the test results were the best. The interference test showed that the high or low content of silver in the sample would not affect the determination of Au, Pb, Bi, Cu, and Pd. The test results showed that the recovery of silver was 97. 7%--100%, the recovery of gold was 98. 6%--102%, and the recovery of palladium was 98.0%--102%. this method was easy to operate, and had good accuracy and precision the RSD values were between 1. 1% and 3. 3%, and could meet the needs of actual detection. [ABSTRACT FROM AUTHOR]