便携式Li-K分析仪的研制及其在锂辉石中锂的分析应用

我国锂钾主要矿产资源大多分布在西部偏远地区,其勘查找矿或综合利用迫切需要现场快速分析技术的支持。本文介绍了自行开发的便携式Li-K分析仪的主要性能及其在锂辉石中锂的分析应用。Li-K分析仪是一种基于大气压的液体阴极辉光放电光谱仪,以待测液体为放电阴极,实现了样品中Li、K等元素的原子化和激发。该仪器以光纤传导CCD光谱仪作为检测器,其波长范围为345-1015 nm,分辨率3 nm;以Li 670.78 nm和K 769.90 nm分析谱线,在仪器最佳工作条件下测定Li、K的精密度(RSD,n=14)均低于2%,检出限为0.03μg/m L,检测范围0.1-10μg/m L。研究表明,不同酸度...

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Published in岩矿测试 Vol. 35; no. 4; pp. 366 - 372
Main Author 焦距 杨啸涛 袁继海 樊兴涛 刘晓 詹秀春
Format Journal Article
LanguageChinese
Published 国家地质实验测试中心,北京,100037 2016
Subjects
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ISSN0254-5357
DOI10.15898/j.cnki.11-2131/td.2016.04.005

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Abstract 我国锂钾主要矿产资源大多分布在西部偏远地区,其勘查找矿或综合利用迫切需要现场快速分析技术的支持。本文介绍了自行开发的便携式Li-K分析仪的主要性能及其在锂辉石中锂的分析应用。Li-K分析仪是一种基于大气压的液体阴极辉光放电光谱仪,以待测液体为放电阴极,实现了样品中Li、K等元素的原子化和激发。该仪器以光纤传导CCD光谱仪作为检测器,其波长范围为345-1015 nm,分辨率3 nm;以Li 670.78 nm和K 769.90 nm分析谱线,在仪器最佳工作条件下测定Li、K的精密度(RSD,n=14)均低于2%,检出限为0.03μg/m L,检测范围0.1-10μg/m L。研究表明,不同酸度和酸的类型对谱线强度影响较大,且存在显著的样品基体效应,标准曲线法分析锂辉石中Li的结果偏差高达267%;而标准加入法可克服基体效应的影响,获得与ICP-OES一致性较好的分析结果,为现场开展固体样品中Li的测定奠定了基础。
AbstractList 我国锂钾主要矿产资源大多分布在西部偏远地区,其勘查找矿或综合利用迫切需要现场快速分析技术的支持。本文介绍了自行开发的便携式Li-K分析仪的主要性能及其在锂辉石中锂的分析应用。Li-K分析仪是一种基于大气压的液体阴极辉光放电光谱仪,以待测液体为放电阴极,实现了样品中Li、K等元素的原子化和激发。该仪器以光纤传导CCD光谱仪作为检测器,其波长范围为345-1015 nm,分辨率3 nm;以Li 670.78 nm和K 769.90 nm分析谱线,在仪器最佳工作条件下测定Li、K的精密度(RSD,n=14)均低于2%,检出限为0.03μg/m L,检测范围0.1-10μg/m L。研究表明,不同酸度和酸的类型对谱线强度影响较大,且存在显著的样品基体效应,标准曲线法分析锂辉石中Li的结果偏差高达267%;而标准加入法可克服基体效应的影响,获得与ICP-OES一致性较好的分析结果,为现场开展固体样品中Li的测定奠定了基础。
TH744.1%P578.954; 我国锂钾主要矿产资源大多分布在西部偏远地区,其勘查找矿或综合利用迫切需要现场快速分析技术的支持。本文介绍了自行开发的便携式Li-K分析仪的主要性能及其在锂辉石中锂的分析应用。Li-K分析仪是一种基于大气压的液体阴极辉光放电光谱仪,以待测液体为放电阴极,实现了样品中Li、K等元素的原子化和激发。该仪器以光纤传导CCD光谱仪作为检测器,其波长范围为345~1015 nm,分辨率3 nm;以Li 670.78 nm和K 769.90 nm分析谱线,在仪器最佳工作条件下测定Li、K的精密度(RSD,n=14)均低于2%,检出限为0.03μg/mL,检测范围0.1~10μg/mL。研究表明,不同酸度和酸的类型对谱线强度影响较大,且存在显著的样品基体效应,标准曲线法分析锂辉石中Li的结果偏差高达267%;而标准加入法可克服基体效应的影响,获得与ICP-OES一致性较好的分析结果,为现场开展固体样品中Li的测定奠定了基础。
Abstract_FL Most of the mineral resources of lithium and potassium are distributed in remote western China.Fast, on-site analytical techniques are urgently needed for their exploration and comprehensive utilization.In this work,a newly developed portable Li-K analyzer was introduced for its analytical performance and the application of this equipment in determining lithium in spodumene is also discussed.The analyser is a type of atomic emission spectrometer based on solution cathode atmospheric glow discharge. Sample solution was used as a graphite cathode,which atomized and excited the elements Li and K.A charge coupled device (CCD)was used to detect the characteristic lines of Li and K,which had wavelengths ranging from 345 to 1015 nm with a 3 nm resolution. Using a Li analytical line of 670.78 nm and a K analytical line of 769.90 nm under the optimized working conditions,the measurement precisions for Li and K were greater than 2%RSD with the limit of detection of 0.03μg/mL.Results show that different types and concentrations of acids strongly affect the intensities of Li and K,and co-existent elements produce serious matrix effect.Quantification of Li in spodumene ores by use of a calibration curve without matched matrix could not produce accurate results with relative standard deviation up to 267%. Standard addition methods can eliminate the influence of the matrix effect and obtain analytical results consistent with those by Inductively Coupled Plasma-Optical Emission Spectrometry,which thus provides a basis for on-site determination of Li in solid samples.
Author 焦距 杨啸涛 袁继海 樊兴涛 刘晓 詹秀春
AuthorAffiliation 国家地质实验测试中心,北京100037
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YANG Xiao-tao
FAN Xing-tao
YUAN Ji-hai
ZHAN Xiu-chun
LIU Xiao
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DocumentTitleAlternate Development of a Portable Li-K Analyzer and Its Application in the Determination of Lithium in Spodumene
DocumentTitle_FL Development of a Portable Li-K Analyzer and Its Application in the Determination of Lithium in Spodumene
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Keywords standard addition method
solution cathode atmospheric glow discharge
portable Li-K analyzer
charge coupled device (CCD)
CCD光谱仪
液体阴极辉光放电
标准加入法
便携式Li-K分析仪
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Notes Most of the mineral resources of lithium and potassium are distributed in remote western China. Fast,on-site analytical techniques are urgently needed for their exploration and comprehensive utilization. In this work,a newly developed portable Li-K analyzer was introduced for its analytical performance and the application of this equipment in determining lithium in spodumene is also discussed. The analyser is a type of atomic emission spectrometer based on solution cathode atmospheric glow discharge. Sample solution was used as a graphite cathode,which atomized and excited the elements Li and K. A charge coupled device( CCD) was used to detect the characteristic lines of Li and K,which had wavelengths ranging from 345 to 1015 nm with a 3 nm resolution.Using a Li analytical line of 670. 78 nm and a K analytical line of 769. 90 nm under the optimized working conditions,the measurement precisions for Li and K were greater than 2% RSD with the limit of detection of 0. 03μg / m L. Results show that different types
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SubjectTerms CCD光谱仪
便携式Li-K分析仪
标准加入法
液体阴极辉光放电
锂辉石
Title 便携式Li-K分析仪的研制及其在锂辉石中锂的分析应用
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