内标法在电解液阴极大气压辉光放电原子发射光谱检测水体金属元素含量中的应用  

Determination of metal elements in aqueous solution with electrolyte cathode atmospheric glow discharge atomic emission spectroscopy by the internal standard method

作　　者：郑培超[1] 杨蕊[1] 王金梅[1] 王晓蒙[1] 刘红弟[1] 张斌[1] 于斌[1] 

机构地区：[1]重庆邮电大学光电工程学院,重庆400065

出　　处：《分析试验室》2015年第1期18-21,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(61205149);重庆市自然科学基金(CSTC2012JJA50033)资助

摘　　要：电解液阴极大气压辉光放电-原子发射光谱ELCAD-AES是一种新兴的快速、高效、实时、在线的元素分析方法。将ELCAD-AES技术应用于水体中金属元素检测,选取K I 766.5 nm,Ca I 422.7 nm,Zn I 213.8 nm和Pb I 405.78nm为分析谱线,Hβ为内标谱线,分别建立基本定标法和内标法的光谱分析定标曲线,对4种元素的检验样品进行测定。实验结果表明,K,Ca,Zn和Pb基本定标曲线拟合度R2分别为0.9951,0.9985,0.9917和0.9934,相对误差为1.1%和2.4%,1.2%和0.94%,8.3%和0.83%,4.0%和1.9%;采用内标法,4种元素定标曲线的拟合度分别达到0.996,0.9996,0.9994和0.9996,相对误差可达到0.25%和1.8%,0.44%和0.34%,2.6%和0.19%,2.4%和0.94%。说明内标法可提高定标曲线的拟合度,减少定量分析误差,提高测量精度。Electrolyte cathode atmospheric glow discharge atomic emission spectroscopy （ELCAD-AES） is a promising technique for element analysis with many advantages including rapidness, efficiency, real time and on- line detection. ELCAD-AES was applied to measurement of metal elements in aqueous solution, and the lines of K （K I 766.5 nm）, Ca （Ca I 422.7 nm）, Zn （Zn I 213.8 nm） and Pb （Pb I 405.78 nm） were selected as the analysis spectral lines, and the spectral line of H_β was selected as the internal standard line. The calibration curves were drawn with basic calibration method and internal calibration method respectively to quantitatively analyze the concentrations of the four elements. The experimental results show that the correlation coefficients （R^2） of K, Ca, Zn, Pb are 0. 9951, 0. 9985, 0. 9917 and 0. 9934 when using basic calibration method, and the relative errors of measurement are 1.1% and 2.4% , 1.2% and 0. 94% , 8.3% and 0. 83% , 4. 0% and 1. 9% respectively; When using internal calibration method, the correlation coefficients （R2） of four different elements are 0. 996, 0. 9996, 0. 9994 and 0. 9996, the relative errors are 0. 25% and 1.8%, 0. 44% and 0. 34%, 2.6% and 0. 19%, 2.4% and 0. 94%. The results show that the internal standard method can improve the correlation coefficients of the calibration curve, reduce the errors in quantitative analysis and improve the accuracy of measurement.

关 键 词：电解液阴极大气压辉光放电-原子发射光谱 定量分析 内标法 

分 类 号：O657.3[理学—分析化学]