电感耦合等离子体质谱(ICP-MS)法同时测定水系沉积物中痕量铅和砷  

Simultaneous Determination of Trace Lead and Arsenic in Sediment by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)

作　　者：吴怡 虞锐鹏[2] 陈海兰 曹玉华 李明 WU Yi;YU Ruipeng;CHEN Hailan;CAO Yuhua;LI Ming(School of Chemical and Material Engineering,Key Laboratory of Synthetic and Biological Colloids,Ministry of Education,Jiangnan University,Wuxi,Jiangsu 214122,China;State Key Laboratory of Food Science and Technology,Jiangnan University,Wuxi,Jiangsu 214122,China;Shanxi Coking Coal Yuncheng Salt Chemical Group Co.,Ltd.,Yuncheng,Shanxi 044000,China)

机构地区：[1]江南大学化学与材料工程学院,合成与生物胶体教育部重点实验室,江苏无锡214122 [2]江南大学食品科学与技术国家重点实验室,江苏无锡214122 [3]山西焦煤运城盐化集团有限责任公司,山西运城044000

出　　处：《中国无机分析化学》2024年第11期1471-1477,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：江苏省特种设备安全监督管理委员会自然科学基金资助项目(KJ(Y)2020037);国家重点研发计划项目(2018YFC1603001)。

摘　　要：为准确测定沉积物中痕量铅和砷的含量,比较不同消解方式与不同混合酸体系对沉积物中铅和砷元素的提取效果,并探讨内标法和标准加入法对质控结果的影响,采用电感耦合等离子体质谱(ICP-MS)法测定,建立了电热板消解/ICP-MS标准加入法同时测定水系沉积物中铅和砷元素含量的方法。通过分析经认证的标准参考样(GSD-9)来评价方法的准确度。结果显示:采用HCl-HNO_(3)-HF-HClO_(4)体系电热板消解,具有较高的消解回收率;标准加入法可有效清除基质干扰,提高准确度;方法线性关系良好;铅和砷元素的回收率在93.9%~104%,相对标准偏差为4.2%~5.0%(n=6),检出限分别为0.026 mg/kg和0.004 mg/kg。方法的准确度和精密度良好、灵敏度高。为环境中土壤及水系沉积物中痕量重金属元素含量的测定提供了参考分析方法。In order to accurately determine the content of trace lead(Pb) and arsenic(As) in sediment,to compare the extraction effects of different digestion methods and different mixed acid systems on Pb and As in sediment,and to discuss the influence of internal standard method and standard addition method on quality control,inductively coupled plasma mass spectrometry(ICP-MS) method was used to determine the content of lead and arsenic elements in water sediment.A method was developed for simultaneous determination 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-HNO_3-HF-HClO_(4) 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 0.004 mg/kg,respectively.The method has good accuracy,adequate precision and high sensitivity.This provides a reliable analysis method for the determination of trace heavy metal elements in soil and sediment in the environment.

关 键 词：沉积物 电热板消解 电感耦合等离子体质谱 标准加入法 铅 砷 

分 类 号：O657[理学—分析化学] TH843[理学—化学]