X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素

张莉娟; 徐铁民; 李小莉; 安树清; 韩伟; 张楠; 刘义博

X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素

1.
中国地质调查局天津地质调查中心, 天津 300170
2.
中国地质调查局天津地质调查中心, 天津 300170
3.
中国地质调查局天津地质调查中心, 天津 300170
4.
中国地质调查局天津地质调查中心, 天津 300170
5.
中国地质调查局天津地质调查中心, 天津 300170
6.
中国地质调查局天津地质调查中心, 天津 300170
7.
中国地质调查局天津地质调查中心, 天津 300170

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- 收稿日期: 2010-12-20

Quantification of Major and Minor Components in Iron Ores with Sulfur, Arsenic and Vanadium by X-ray Fluorescence Spectrometry

1.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
2.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
3.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
4.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
5.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
6.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China
7.
Tianjin Institute of Geology and Mineral Resources, China Geological Survey, Tianjin 300170, China

摘要

摘要: 以钴(钴玻璃粉形式)作内标元素,准确测定全铁含量;加入保护剂硝酸铵和稳定剂碳酸锂,使硫转化为硫酸盐,有效地防止硫的挥发损失。通过条件实验,确立了样品熔融温度和钴玻璃粉的用量。选择经筛选的仪器测定条件,用X射线荧光光谱法同时测定铁矿石中TFe、SiO₂、CaO、MgO、Al₂O₃、TiO₂、P、S、Mn、V₂O₅、As、K₂O、Na₂O、Cu、Ni 等15种主次量元素。采用干扰曲线法对几乎完全重叠的Ti Κβ谱线与V Κα谱线进行谱线重叠校正,用理论α系数法校正基体效应。建立的方法可以准确测定全铁和质量分数高达5.29%的S。采用多种标准物质和人工配制标准物质制作工作曲线,可以测定质量分数为5.00%的V₂O₅及0.1%的As,测定值与标准值符合较好,除低含量钠外方法精密度(RSD)<3.5%,分析误差符合实验质量要求。本法可以快速、准确地测定含砷的钒钛铁矿及含硫高的铁矿石中的主次量元素,满足了日常生产对铁矿石中硫和钒的测定要求。
- X射线荧光光谱法 /
- 铁矿石 /
- 钴玻璃粉 /
- 硫 /
- 砷 /
- 五氧化二钒
Abstract: A method for the determination of 15 elements of TFe, SiO₂, CaO, MgO, Al₂O₃, TiO₂, P, S, Mn, V₂O₅, As, K₂O, Na₂O, Cu and Ni in high sulfur, arsenic iron ore by X-ray Fluorescence Spectrometry (XRF) was developed. Co in the form of cobalt glass powder was selected as the internal standard element for Fe determination. NH₄NO₃ served as the oxidant and Li₂CO₃ as the protective agent and were used for preventing the sulfur from volatilizing. Multi-kinds of standard references and artificial preparation iron ores were used for calibration. The almost overlapping spectral lines of Ti Κβ and V Κα were corrected by using the interfering curve method and the matrix effects were corrected by the theoretical alpha coefficient. The established method was possible to determine the TFe, the mass fraction of 5.29% S, 5.00% of V₂O₅ and 0.1% of As. The results were in accordance with certified values of standard reference materials. The RSDs met the requirements of lab qualify control, except the low content Na with RSD of <3.5%. The established method is a fast way to accurately obtain major and minor components in high S, As and V contents iron ores which is satisfied by the requirements of routine analysis.
- X-ray /
- fluorescence /
- spectrometry /
- iron /
- ores /
- cobalt

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X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素

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Quantification of Major and Minor Components in Iron Ores with Sulfur, Arsenic and Vanadium by X-ray Fluorescence Spectrometry

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