Abstract：The determination of As and Se in soil by inductively coupled plasma mass spectrometry (ICP-MS) can be severely interfered by polyatomic ions such as argon compounds, chlorides, oxides and double charges, leading to high difficulty in determination of As and Se in soil. The soil samples were digested by aqua regia in the graphite digester. In the MS/MS mode, the mass charge ratio (m/z) of the first quadrupole mass filter (Q1) was set to 75 and 80, respectively. Accompanied by the introduction of oxygen into the collision/reaction cell, 75As+ and 80Se+ were converted to 75As16O+ and 80Se16O+, while the interfering ions could not react with oxygen. The m/z of the second quadrupole mass filter (Q3) was set to 91 and 96, respectively, so that 75As16O+ and 80Se16O+ could pass through and enter the detector, avoiding the mass spectrometry interferences in the sample. Accordingly, a method for the determination of As and Se in soil by graphite digestion-inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established. The oxygen flow rate was optimized and 1.0 mL/min was selected. The experimental results showed that the linear range of As and Se was 0.500-100 μg/L. The linear correlation coefficients were 0.999 93 and 0.999 98, the limits of detection were 0.008 mg/kg and 0.001 mg/kg, and the limits of quantification were 0.032 mg/kg and 0.004 mg/kg, respectively. The contents of As and Se in certified reference materials and actual samples of soil were determined according to the experimental method. The results showed that the measured values of As and Se were consistent with the certified values for the certified reference materials. The relative standard deviations (RSD, n=6) were 2.0%-4.4% and 2.6%-7.8% for As and Se, respectively. For the actual samples of soil, the measured results were basically consistent with those obtained by atomic fluorescence spectrometry. The RSDs (n=6) were 2.3%-4.5% and 3.7%-7.9%, respectively.
刘跃, 王记鲁, 李静, 王鑫, 林冬. 氧气反应模式-电感耦合等离子体串联质谱法测定土壤中砷和硒[J]. 冶金分析, 2022, 42(10): 30-37.
LIU Yue, WANG Jilu, LI Jing, WANG Xin, LIN Dong. Determination of arsenic and selenium in soil by inductively coupled plasma tandem mass spectrometry at oxygen reaction mode. , 2022, 42(10): 30-37.
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