Abstract:In order to improve the accuracy of trace lead (Pb) and arsenic (As) in sediment, inductively coupled plasma mass spectrometry (ICP-MS) was used to compare the extraction effects of different digestion methods and different mixed acid systems on lead (Pb) and arsenic (As) in sediment, and to discuss the influence of internal standard method and standard addition method on quality control. A method was developed for the analysis of Pb and As in sediment using ICP-MS with electric heating plate digestion and standard addition method. The accuracy of the method was evaluated by analyzing the certified reference material (GSD-9). The results showed that the digestion recoveries of the samples digested by HCl-HNO3-HF-HClO4 and electric heating plate digestion were higher than other digestion methods, and the standard addition method could effectively eliminate the matrix interference with improved accuracy. The linear relationship of the method was good, and the recoveries of Pb and As were in the range of 93.9%~104% with the relative standard deviations (RSD, n=6) from 4.2% to 5.0%, and the detection limits of Pb and As were 0.026 mg/kg and 0.0036 mg/kg, respectively. It shows that the method has good accuracy, adequate precision and high sensitivity. The contents of Pb and As in sediments of three river systems were successfully determined by the proposed method, which provided a reliable analysis method for the determination of trace heavy metal elements in soil and sediment in the environment.