钠离子促进消解-电感耦合等离子体质谱法测定植物中的硅  

Determination of silicon in plants by sodium ion promoted digestion-inductively coupled plasma mass spectrometry

作　　者：孙文军 刘向磊 蔡焕花 张宏丽 文田耀 王腾飞 SUN Wenjun;LIU Xianglei;CAI Huanhua;ZHANG Hongli;WEN Tianyao;WANG Tengfei(No.1 Institute of Geological and Mineral Resources Survey,Henan Bureau of Geoexploration and Mineral Development,Luoyang 471023,China;Key Laboratory of Au-Ag-Polymetallic Deposit Series and Deep-seated Metallogenic Prognosis of Henan Province,Luoyang 471023,China;Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,Chinese Academy of Geological Sciences,Zhengzhou 450060,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450060,China)

机构地区：[1]河南省地质矿产勘查开发局第一地质矿产调查院,洛阳471023 [2]河南省金银多金属成矿系列与深部预测重点实验室,洛阳471023 [3]中国地质科学院郑州矿产利用研究所,郑州450006 [4]国家非金属资源综合利用工程技术中心,郑州450060

出　　处：《分析试验室》2024年第4期482-487,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金青年基金项目(21806149);中央土壤污染防治专项(2110402-农村环境保护)资助。

摘　　要：植物中的硅因具有含量低、难消解、用含氟酸处理易损失等特点,一直是湿法处理的难点。本研究选择硝酸+氢氟酸+氯化钠混合消解液和高通量微波密闭消解植物样品,通过优化消解液配比、消解温度和消解时间、碰撞气体流量,建立了钠离子促进消解-电感耦合等离子体质谱法测定植物中硅的方法。结果表明,使用硝酸+氢氟酸混合消解溶液,可有效消解植物样品基体及基体中的硅元素;向消解液中加入一定量的钠离子和使用微波密闭消解法,能够促进试样中二氧化硅消解完全,提高消解效率及避免氟硅化合物的挥发损失。使用聚四氟乙烯同心圆雾化器、聚四氟乙烯旋流雾化室和蓝宝石中心管,可有效降低由溶液中氢氟酸介质腐蚀石英进样系统引入的仪器本底值;选择氦气作为碰撞气并控制氦气流量,可以有效消除氮、碳、铝、硼、氢、氧等元素的多原子离子对28Si的质谱干扰,提高方法的灵敏度。硅的方法检出限为0.001%,相对标准偏差(RSD)和误差(RE)分别在1.8%~7.7%和-1.8%~4.5%之间。方法适合于植物样品中硅的准确、快速测定,也可为农业考古和植物碳汇潜力研究中硅的总量分析提供技术支撑。Silicon in plants has always been one of the difficulties in wet treatment because of its low content,difficult digestion,and easy loss of fluorine-containing acid treatment.In this study,HNO_(3)+HF+NaCl mixed digestion solution and high-throughput microwave closed digestion for plant samples were selected.By optimizing the ratio of digestion solution,digestion temperature and digestion time,collision gas flow,a method for the determination of silicon in plants by inductively coupled plasma mass spectrometry with sodium ion promoted digestion was established.The results showed that the use of HNO_(3)-HF mixed digestion solution could effectively digest the plant sample matrix and the silicon element in the matrix.Adding a certain amount of sodium ions to the digestion solution and using microwave closed digestion method could promote the complete digestion of silica in the sample,improve the digestion efficiency and avoid the volatilization loss of fluorosilicone compounds.The use of polytetrafluoroethylene concentric atomizer,polytetrafluoroethylene swirl atomizing chamber and sapphire central tube can effectively reduce the instrument background value introduced by the hydrofluoric acid medium corrosion quartz injection system in the solution.Choosing helium(He)as collision gas and controlling the flow rate of helium can effectively eliminate the mass spectral interference of polyatomic ions of nitrogen,carbon,aluminum,boron,hydrogen,oxygen and other elements on 28Si,and improve the sensitivity of the method.subsequently,the detection limit of silicon was 0.001%,and the relative standard deviations(RSDs)and error(RE)of the method were 1.8%-7.7%and-1.8%-4.5%,respectively.The method is suitable for the accurate and rapid determination of silicon in plant samples,and can also provide technical support for the total amount analysis of silicon in agricultural archaeology and plant carbon sink potential research.

关 键 词：硅 钠离子 植物样品 微波消解 电感耦合等离子体质谱 

分 类 号：O652.4[理学—分析化学] O657.63[理学—化学]