【引用本文】 周学忠, 谢华林, . 微波等离子体原子发射光谱法测定偏远矿区海泡石中的主微量元素[J]. 岩矿测试, 2021, 40(5): 680-687. doi: 10.15898/j.cnki.11-2131/td.202011160144
ZHOU Xue-zhong, XIE Hua-lin. Determination of Major and Trace Elements in Sepiolite of Remote Mining Area by Microwave Plasma-Atomic Emission Spectroscopy[J]. Rock and Mineral Analysis, 2021, 40(5): 680-687. doi: 10.15898/j.cnki.11-2131/td.202011160144

微波等离子体原子发射光谱法测定偏远矿区海泡石中的主微量元素

1. 

湖南工学院材料科学与工程学院, 湖南 衡阳 421002

2. 

长江师范学院材料科学与工程学院, 重庆 涪陵 408100

收稿日期: 2020-11-16  修回日期: 2021-01-31  接受日期: 2021-07-02

基金项目: 国家自然科学基金项目(81603400);湖南省自然科学基金项目(2019JJ60026);湖南省教育厅重点项目(18A428);湖南省应用特色学科材料科学与工程学科资助基金(湘教通[2018]469号);湖南省工程研究中心资助基金(湘发改委高技[2019]853号)

作者简介: 周学忠, 高级实验师, 主要从事分析化学的理论与应用研究。E-mail: zxz108909@163.com

通信作者: 谢华林, 博士, 教授, 主要从事材料化学的理论与应用研究。E-mail: hualinxie@vip.163.com

Determination of Major and Trace Elements in Sepiolite of Remote Mining Area by Microwave Plasma-Atomic Emission Spectroscopy

1. 

College of Materials Science and Engineering, Hunan Institute of Technology, Hengyang 421002, China

2. 

College of Materials Science and Engineering, Yangtze Normal University, Fuling 408100, China

Corresponding author: XIE Hua-lin, hualinxie@vip.163.com

Received Date: 2020-11-16
Revised Date: 2021-01-31
Accepted Date: 2021-07-02

摘要:海泡石是具有层状结构的含水富镁硅酸盐黏土矿物,其中无机元素含量是揭示其成矿物质来源、成矿流体性质和矿床成因的重要依据,通常采用电感耦合等离子体发射光谱/质谱法(ICP-OES/MS)进行测定,等离子体(ICP)的高温激发会产生成大量谱线干扰,维持ICP稳定工作需使用高纯氩气,持续供气对于偏远矿区海泡石的检测还将面对气体采购和运输不便的问题。本文基于微波等离子体原子发射光谱(MP-AES)的低温激发技术减少光谱干扰,建立了准确测定偏远矿区海泡石中主量元素Mg、Al、Ca、Fe、K、Na和微量元素Cu、Zn、Mn、Pb含量的分析方法。利用硝酸-盐酸-氢氟酸混合酸对海泡石进行微波消解,避免了样品处理过程中分析元素的损失,加快了样品处理速度,同时提高了样品溶液的稳定性。通过选择各元素光谱线的分析波长,并利用快速线性干扰校正(FLIC)技术校正光谱干扰,以Lu为内标元素校正基体效应,提高了灵敏度和准确度。各元素的检出限为0.19~14.6μg/L。海泡石国家标准物质(GBW07138)各元素测定值与认定值的相对误差在-5.0%~6.7%之间。本方法具有检出限低、线性范围宽、结果准确等优点;MP-AES采用自带的氮气发生器为等离子体提供氮气作为工作气,无需引入复杂气体,提高了分析效率,尤其适用于气体采购和运输不便的偏远矿区。

关键词: 偏远矿区, 海泡石, 主微量元素, 微波等离子体原子发射光谱法, 光谱干扰, 基体效应

要点

(1) MP-AES以氮气作为工作气,无需引入复杂气体,提高了分析效率。

(2) 利用快速线性干扰校正(FLIC)技术校正光谱干扰。

(3) 利用Lu作为内标元素补偿由基体效应引起的谱线强度变化。

Determination of Major and Trace Elements in Sepiolite of Remote Mining Area by Microwave Plasma-Atomic Emission Spectroscopy

ABSTRACT

BACKGROUND:

Sepiolite is a layered hydrous magnesium-rich silicate clay mineral. The content of inorganic elements in sepiolite is an important basis for revealing the source of ore-forming materials, the nature of ore-forming fluids and the genesis of the deposit. It is usually determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS), high temperature excitation of inductively coupled plasma (ICP) will produce a large number of spectral interferences. High purity argon is needed to maintain the stability of ICP. Continuous gas supply for sepiolite detection in remote mining areas will also cause the problem of inconvenient gas procurement and transportation.

OBJECTIVES:

In order to reduce the spectral interference and realize the accurate analysis of major and trace elements in sepiolite samples from remote mining areas.

METHODS:

An analytical method was developed for accurate determination of major elements Mg, Al, Ca, Fe, K, Na and trace elements Cu, Zn, Mn and Pb in sepiolite by microwave plasma-atomic emission spectroscopy (MP-AES). Microwave digestion of sepiolite by using HNO3-HCl-HF as a mixed acid not only avoids the loss of analytes during sample processing, but also speeds up the sample processing and improves the stability of the sample solution. By selecting the analysis wavelength of the spectral line for analyte, using the fast linear interference correction (FLIC) technology to correct the spectral interference, and selecting Lu as the internal standard element corrected the matrix effect, which improved sensitivity and accuracy.

RESULTS:

The limit of detection (LOD) was 0.19-14.6μg/L. The accuracy of the method was verified by the national standard reference material sepiolite (GBW07138). The relative error between the measured value and the certified value of analytes was between -5.0% and 6.7%, which verified the accuracy and reliability of the method.

CONCLUSIONS:

The method has the advantages of low LOD, wide linear range, and accurate results. MP-AES uses its own nitrogen generator to provide nitrogen as the working gas for plasma, without introducing a complex gas, which improves the analysis efficiency, and is especially suitable for remote mining areas where gas procurement and transportation are inconvenient.

KEY WORDS: remote mining area, sepiolite, major and trace elements, microwave plasma-atomic emission spectroscopy, spectral interference, matrix effect

HIGHLIGHTS

(1) The MP-AES uses nitrogen as the working gas, which is not necessary to introduce complex gases and thus improves the analysis efficiency.

(2) Rapid linear interference correction (FLIC) technique was used to correct spectral interference.

(3) Lu was used as the internal standard element to compensate for the change of spectral intensity caused by the matrix effect.

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微波等离子体原子发射光谱法测定偏远矿区海泡石中的主微量元素

周学忠, 谢华林