| 碱熔融-电感耦合等离子体发射光谱法测定高硫铝土矿中的硫 |
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| 引用本文： | 胡璇,石磊,张炜华.碱熔融-电感耦合等离子体发射光谱法测定高硫铝土矿中的硫[J].岩矿测试,2017,36(2):124-129. |
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| 作者姓名： | 胡璇 石磊 张炜华 |
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| 作者单位： | 湖北省地质实验测试中心, 湖北 武汉 430034,湖北省地质实验测试中心, 湖北 武汉 430034,湖北省地质实验测试中心, 湖北 武汉 430034,湖北省地质实验测试中心, 湖北 武汉 430034,湖北省地质实验测试中心, 湖北 武汉 430034 |
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| 基金项目： | 国家重点研发计划项目“重点领域急需化学成分量标准物质研究”（2016YFF020110308） |
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| 摘 要： | 应用电感耦合等离子体发射光谱法(ICP-OES)测定高硫铝土矿(硫含量≤8%)中的硫时,由于硫存在-2、+4和+6等多种价态,常用的酸溶法和碱熔法处理高硫铝土矿时往往无法完全氧化硫而导致硫测定结果偏低。本文用过氧化钠熔融、热水浸取和盐酸酸化提取高硫铝土矿中的硫,使用基体匹配法绘制校准曲线补偿铝和钠对硫测定的光谱干扰,以S182.034 nm(184 nm)作为分析谱线,采用ICP-OES对硫进行测定。结果表明:3 g过氧化钠在700℃下熔融10 min,可以较好地氧化高硫铝土矿中的硫;校准曲线的线性相关系数为0.9999,方法检出限为0.025μg/m L,相对标准偏差(RSD,n=6)小于5%;与碳硫仪的测定结果相比较,两种方法无显著性差异。本方法溶样彻底,无样品损失,为今后实现应用ICP-OES同时测定高硫铝土矿中的硫和其他元素奠定了基础。
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| 关 键 词： | 磷矿石 磷 酸溶 内标校正 电感耦合等离子体发射光谱法 |
| 收稿时间： | 2015/7/14 0:00:00 |
| 修稿时间： | 2017/2/22 0:00:00 |
Determination of Sulfur in High-sulfur Bauxite by Alkali Fusion-Inductively Coupled Plasma-Optical Emission Spectrometry |
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| HU Xuan,SHI Lei and ZHANG Wei-hua.Determination of Sulfur in High-sulfur Bauxite by Alkali Fusion-Inductively Coupled Plasma-Optical Emission Spectrometry[J].Rock and Mineral Analysis,2017,36(2):124-129. |
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| Authors: | HU Xuan SHI Lei and ZHANG Wei-hua |
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| Institution: | Hubei Province Geological Experimental Testing Center, Wuhan 430034, China,Hubei Province Geological Experimental Testing Center, Wuhan 430034, China,Hubei Province Geological Experimental Testing Center, Wuhan 430034, China,Hubei Province Geological Experimental Testing Center, Wuhan 430034, China and Hubei Province Geological Experimental Testing Center, Wuhan 430034, China |
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| Abstract: | Inductively coupled plasma-atomic emission spectrometry has been widely used to determine major and minor components in phosphate ores, however, the analysis error caused by instruments drift and matrix effect can''t ignored during actual measured. An internal standard correction method to reduce the effects for high content of phosphorus determination utilizing tellurium as internal standard element was investigated in this study. More precise from 4.1% to 0.5% expressed as relative standard deviation (RSD, n=12)and the lower detection limit (0.0044%)were achieved by internal standard correction for phosphorus determination. Two kinds of acid digestion methods for phosphate ore were compared in this work. The results indicate that aqua regia rapid digestion method was suitable for some elements such as phosphorus, calcium, iron, magnesium, manganese analysis, but a mixture of hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid system was more effective for total dissolution of major and minor components including potassium, sodium, aluminum in phosphate ore. |
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| Keywords: | phosphate ore phosphorus acid digestion internal standard correction Inductively Coupled Plasma-Optical Emission Spectrometry |
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