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液体阴极辉光放电原子发射光谱法测定盐矿中的K、Ca、Na、Mg
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作者单位
俞洁,张志超,陆泉芳,朱淑雯,张晓敏,王星,杨武 1.甘肃省生物电化学与环境分析重点实验室西北师范大学化学化工学院2.西北师范大学学报编辑部 
基金项目:国家自然科学基金资助项目(21567025,21864022,21367023);甘肃省自然科学基金资助项目(17JR5RA077,17JR5RA075)
中文摘要:以铂针尖为阳极,毛细管顶端溢出的液体为阴极,建立了一种新型的液体阴极辉光放电原子发射光谱(LCGD-AES)分析检测系统。利用该系统同时测定了格尔木化肥厂盐矿中K、Ca、Na和Mg的含量。研究了放电电压、溶液流速、电解质种类、溶液pH值、干扰物对发射强度的影响,同时与离子色谱(IC)的测量结果进行比较。结果表明,在放电电压650 V、溶液流速3 mL· min-1、pH 1.0的HNO3作为电解液时,K、Ca、Na和Mg的检出限(LOD)分别为0.100 0、0.048 0、0.002 4和0.003 9 mg·L-1,相对标准偏差(RSD)分别为0.57%、1.8%、0.94%和1.8%。LCGD-AES对盐矿中K、Ca、Na、Mg的测试结果与IC的测定结果基本一致,样品回收率为95.4%~108%。
中文关键词:液体阴极辉光放电(LCGD)  原子发射光谱(AES)  盐矿  金属元素  高灵敏检测
 
Simultaneous Determination of K,Ca,Na and Mg in Salt Mine by Liquid Cathode Glow Discharge-Atomic Emission Spectrometry
Abstract:In this study,a liquid cathode glow discharge-atomic emission spectrometry(LCGD-AES)was developed for the simultaneous determination of K,Ca,Na and Mg in salt mine of Geermu,in which needle like Pt was served as anode and overflowing electrolyte from a quartz capillary acted as the liquid cathode.The effects of discharge voltage,solution flow rate,supporting electrolyte,solution pH and interfering matrix components on the emission intensity were investigated in detail.The results were compared with those by ion chromatography(IC).The optimum conditions were as follows:discharge voltage:650 V,flow rate:3 mL·min-1 and supporting electrolyte:pH 1.0 HNO3.The detection limits(LODs)for K,Ca,Na and Mg were 0.100 0,0.048 0,0.002 4 and 0.003 9 mg·L-1,respectively.The relative standard deviations(RSDs)were 0.57%,1.8%,0.94% and 1.8%,respectively.The results obtained by LCGD-AES were consistent with those by IC,and the recoveries for the analytes were in the range of 95.4%-108%.
Key Words:liquid cathode glow discharge(LCGD)  atomic emission spectrometry(AES)  salt mine  metal elements  high sensitive detection
引用本文:俞洁,张志超,陆泉芳,朱淑雯,张晓敏,王星,杨武.液体阴极辉光放电原子发射光谱法测定盐矿中的K、Ca、Na、Mg[J].分析测试学报,2019,38(2):213-218.
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