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焦距, 杨啸涛, 袁继海, 樊兴涛, 刘晓, 詹秀春. 便携式Li-K分析仪的研制及其在锂辉石中锂的分析应用[J]. 岩矿测试, 2016, 35(4): 366-372. DOI: 10.15898/j.cnki.11-2131/td.2016.04.005
引用本文: 焦距, 杨啸涛, 袁继海, 樊兴涛, 刘晓, 詹秀春. 便携式Li-K分析仪的研制及其在锂辉石中锂的分析应用[J]. 岩矿测试, 2016, 35(4): 366-372. DOI: 10.15898/j.cnki.11-2131/td.2016.04.005
Ju JIAO, Xiao-tao YANG, Ji-hai YUAN, Xing-tao FAN, Xiao LIU, Xiu-chun ZHAN. Development of a Portable Li-K Analyzer and Its Application in the Determination of Lithium in Spodumene[J]. Rock and Mineral Analysis, 2016, 35(4): 366-372. DOI: 10.15898/j.cnki.11-2131/td.2016.04.005
Citation: Ju JIAO, Xiao-tao YANG, Ji-hai YUAN, Xing-tao FAN, Xiao LIU, Xiu-chun ZHAN. Development of a Portable Li-K Analyzer and Its Application in the Determination of Lithium in Spodumene[J]. Rock and Mineral Analysis, 2016, 35(4): 366-372. DOI: 10.15898/j.cnki.11-2131/td.2016.04.005

便携式Li-K分析仪的研制及其在锂辉石中锂的分析应用

Development of a Portable Li-K Analyzer and Its Application in the Determination of Lithium in Spodumene

  • 摘要: 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0.03 μg/mL,检测范围0.1~10 μg/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: 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 0.03 μg/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.

     

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