XRF和LA-ICPMS测定硫化物熔片中的主次量元素

徐娟; 杨守业; 胡兆初; 罗涛; 黄湘通

doi:doi:10.3964/j.issn.1000-0593(2016)11-3683-06

光谱学与光谱分析, 2016, 36 (11): 3683, 网络出版: 2016-12-30

XRF和LA-ICPMS测定硫化物熔片中的主次量元素

A New Sample Fusion Technique for Quantitative Analysis of Major and Minor Elements in Sulfides with X-Ray Fluorescence Spectrometry and Laser Ablation Inductively Coupled Plasma Mass Spectrometry

论文大纲

徐娟 ¹杨守业 ¹胡兆初 ²罗涛 ²黄湘通 ¹

作者单位

¹ 同济大学海洋地质国家重点实验室, 上海 200092

² 中国地质大学地质过程与矿产资源国家重点实验室, 湖北武汉 430074

硫化物 X射线荧光光谱仪激光剥蚀电感耦合等离子体质谱仪氧化剂二氧化锗 X-ray fluorescence spectrometry Laser ablation inductivelycoupled plasma mass spec Oxidant Germanium dioxide

摘要

采用高纯HNO3为氧化剂代替传统的氧化剂, 以GeO2为玻璃化试剂, 建立了一种简单、高效的硫化物熔融玻璃片的前处理方法。 XRF和LA-ICPMS分析结果表明, 相对于粉末压片法, 熔片法制备的样品具有更好的均一性和可靠性。 3种硫化物国家一级标准物质的XRF和LA-ICPMS主次量元素（Si, Al, Fe, Mg, K, Ca, Na, Mn, Cu, Zn）分析测试结果均与推荐值相吻合(Ti缺少推荐值), 测定误差都在允许范围内, XRF三次熔片测试结果的精密度RSD<5.6%; LA-ICPMS 15次测试结果精密度RSD<3%。表明建立的硫化物熔融玻璃片的前处理方法可较好的应用于XRF和LA-ICPMS分析硫化物中的主次量元素。

Abstract

A new sample fusion method for sulfides has been developed in this study. HNO3 was used as a short pre-oxidation reagent instead of the traditional solid oxidant (e.g., NaNO3, KNO3), which avoid the erosion of the platinum crucible. GeO2 was also added in samples to avoid the break of glass beads. The good analytical precisions of X-ray fluorescence spectrometry (RSD<5.6%, 1σ) and laser ablation inductivity coupled plasma mass spectrometry (RSD<3%, 1σ) demonstrated that the major elements were homogeneously distributed in the fused beads of sulfides. The determined major and minor elements (Si, Al, Fe, Mg, K, Ca, Na, Mn, Cu and Zn) values by using XRF and LA-ICP-MS are in excellent agreement with published values in three reference sulfide standards(reference values for Ti were absent). These results clearly demonstrate that the present fusion technique is well suitable for routine sulfide sample preparation for both XRF and LA-ICP-MS analysis.

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徐娟, 杨守业, 胡兆初, 罗涛, 黄湘通. XRF和LA-ICPMS测定硫化物熔片中的主次量元素[J]. 光谱学与光谱分析, 2016, 36(11): 3683. XU Juan, YANG Shou-ye, HU Zhao-chu, LUO Tao, HUANG Xiang-tong. A New Sample Fusion Technique for Quantitative Analysis of Major and Minor Elements in Sulfides with X-Ray Fluorescence Spectrometry and Laser Ablation Inductively Coupled Plasma Mass Spectrometry[J]. Spectroscopy and Spectral Analysis, 2016, 36(11): 3683.

XRF和LA-ICPMS测定硫化物熔片中的主次量元素

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