非色散原子荧光光谱法同时检测硒和铅的光源干扰校正方法研究  

Correction Method of Light Source Interference for Simultaneous Determination of Selenium and Lead by Non-dispersive Hydride Generation-Atomic Fluorescence Spectrometry

作　　者：陶琛 李春生[1] 初威澄 高冉冉 周志恒 李云梦 马振予 田地[1] TAO Chen;LI Chun-Sheng;CHU Wei-Cheng;GAO Ran-Ran;ZHOU Zhi-Heng;LI Yun-Meng;MA Zhen-Yu;TIAN DI(College of Instrumentation&Electrical Engineering,JiLin University,Changchun 130023,China;Beijing Bohui Innovation Optoelectronic Technology Co.,Ltd,Beijing 102206,China;Changchun Institute of Optics,Fine Mechanics and Physics,Chinese Academy of Sciences,Changchun 130033,China)

机构地区：[1]吉林大学仪器科学与电气工程学院,长春130026 [2]北京博晖创新光电技术股份有限公司,北京102206 [3]中国科学院长春光学精密机械与物理研究所,长春130033

出　　处：《分析化学》2019年第1期163-168,共6页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划重大科学仪器设备开发专项基金项目(No.2016YFF0103303)资助~~

摘　　要：空心阴极灯(HCL)是氢化物发生-原子荧光光谱仪(HG-AFS)最为常用的激发光源,实验发现硒(Se)元素HCL的发射谱中存在铅(Pb)元素干扰,在Se、Pb同时测定时,会造成Se结果产生失真。本研究详细地讨论了Se元素HCL的光谱干扰,并提出一种光源干扰因子法,可对检测结果进行有效校正。此方法具有操作简单、可靠性高等优点,能够有效降低激发光源阴极的纯度要求。对Se、Pb同时测定的K3[Fe(CN)6]-HCl-KBH4化学发生体系进行了校正和优化,在2～50μg/L范围内获得Se标准曲线r=0.9995,Pb标准曲线的r=0.9997,检出限分别为0.034μg/L(Se)和0.019μg/L(Pb),方法精密度为0.85%(10μg/L,Se,n=9)和0.47%(10μg/L,Pb,n=9)。对国家标准样品大米GBW10010(GSB-1)、小麦GBW10011(GSB-2)和豆粉进行了测定,校正后的Se检测结果与标准值相符。Hollow cathode lamps(HCL)are the most commonly used excitation sources for hydride generation-atomic fluorescence spectrometry(HG-AFS).In general,there was lead(Pb)interference in selenium(Se)HCL.This kind of light source interference affected the accuracy of the detection results when Se and Pb simultaneously were determined by HG-AFS.In this work,the effects of light source interference were discussed and analyzed,and a light source interference factor method was proposed to correct the spectral interference.This method had many advantages including simple operation and high reliability,and appropriately reduced the purity of the cathode of the light source.The spectral interference of Se HCL was discussed.The conditions of simultaneous determination of Se and Pb in K 3[Fe(CN)6]-KBH 4-HCl chemical generation system were optimized,and the influence of Pb interference in HCL of Se was discussed.In the concentration range of 2-50μg/L,the detection limit of Se was 0.034μg/L(r=0.9995),and the detection limit of Pb was 0.019μg/L(r=0.9997).The method precisions were 0.85%(10μg/L,Se,n=9)and 0.47%(10μg/L,Pb,n=9),respectively.The feasibility of the method was confirmed by the simultaneous detection of national standard sample rice GBW10010(GSB-1),wheat GBW10011(GSB-2)and soy flour.The results of the light source calibration were consistent with the standard values.

关 键 词：原子荧光光谱 硒 铅 干扰校正 

分 类 号：O657.31[理学—分析化学]