氟化氢铵消解-甲烷增敏-电感耦合等离子体质谱法测定土壤中的碘  

Determination of Iodine in Soil Samples by Signal Enhanced Inductively Coupled Plasma-Mass Spectrometry using Methane Gas Addition after Ammonium Hydrogen Fluoride Digestion

作　　者：黄锐敏 吴智威 郑云云 黄崇耀 HUANG Ruimin;WU Zhiwei;ZHENG Yunyun;HUANG Chongyao(Ministry of Agriculture and Rural Affairs,Institute of Agricultural Quality Standards and Testing Technology Research,Fujian Academy of Agricultural Sciences,Fujian Key Laboratory of Quality and Safety of Agri-Products,Fuzhou 350003;Hangzhou Puyu Technology Co.,Ltd.,Hangzhou 311305;College of Control Science and Engineering,Zhejiang University,Hangzhou 310014)

机构地区：[1]福建省农产品质量安全重点实验室,福建省农业科学院农业质量标准与检测技术研究所,福建福州350003 [2]杭州谱育科技发展有限公司,浙江杭州311305 [3]浙江大学控制工程与科学学院,浙江杭州310014

出　　处：《分析科学学报》2024年第1期105-110,共6页Journal of Analytical Science

基　　金：福建省“5511”协同创新工程项目(XTCXGC2021020);福建省农业科学院科技创新团队建设项目(CXTD2021011);福建省自然科学基金(2022J01448);福建省属公益类科研院所科研专项(2020R1022003)。

摘　　要：本文基于氟化氢铵(NH_(4)HF_(2))半敞开式消解与甲烷基体改进气增敏-电感耦合等离子体质谱(ICP-MS)技术,建立了一种简单有效、高灵敏的土壤碘含量分析方法。在220℃的温度下,耗时3 h的半敞开式消解过程下,使用250 mg的NH_(4)HF_(2)即可获得50 mg土壤样品的彻底消解效果,且未观察到碘的挥发损失。使用甲烷作为基体改进气,将其与样品气溶胶在线混合后引入ICP,获得2.4倍的ICP-MS碘信号增敏效果。在最佳化的运行条件下,本方法碘的检出限为0.012μg/g,19种国家土壤一级标准物质的测定值与标准值具有良好的一致性,结果表明,本方法能充分应用于批量土壤样品中的碘含量分析。A rapid and high sensitive method has been developed to quantify iodine concentrations in soil samples by inductively coupled plasma-mass spectrometry(ICP-MS).The method is based on an ammonium hydrogen fluoride(NH_(4)HF_(2))semi-open digestion and signal enhancement by adding methane gas during analysis.Fifty mg sample of soils can be completely digested by using 250 mg of NH_(4)HF_(2)at 220℃for 3h and no volatilization loss of iodine was observed.Methane gas,used as a matrix modifier,is online mixed with the sample aerosols before introducing to the ICP plasma.Through careful optimization of the methane gas and carrier gas flow rates,2.4 times increasement in the iodine sensitivity was obtained.Under the optimized operational conditions,the limit of detection(LOD,3σ)of iodine is 0.012μg/g.The measured iodine results for nineteen national soil standard reference materials are in good agreement with the certified values,further highlihgting the reliability and analytical capabilities of our new approach.

关 键 词：土壤 碘 氟化氢铵 甲烷增敏 电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学]