电感耦合等离子体发射光谱法测定磷矿石中常量元素硅磷硫钙镁铝铁钛锰
Determination of Major Components in Phosphate Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 以粒状氢氧化钠作熔剂,样品在银坩锅中700℃熔融,热水浸取后用盐酸酸化,溶液冷却定容后直接用电感耦合等离子体发射法测定磷矿石中硅、磷、硫、钙、镁、铝、铁、钛、锰9种常量元素,采用基体匹配和离峰扣背景等方式有效消除了测定的干扰。对样品分解条件、试剂用量、元素分析谱线的选择、干扰的影响及消除等进行了优化处理和讨论。方法精密度(RSD)为0.28%~1.85%(n=12),回收率为97.92%~107.1%,具有快捷、成本低等特点。经国家一级标准物质分析验证,结果满意,适用于磷矿石中常量元素的快速分析。
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关键词:
- 磷矿石 /
- 常量元素 /
- 氢氧化钠熔融 /
- 电感耦合等离子体发射光谱法
Abstract: The phosphate ore samples were fused by grainy NaOH in a silver crucible at 700℃, and then dissolved with HCl acid solution. A method for the determination of Si, P, S, Ca, Mg, Al, Fe, Ti and Mn in phosphate ores by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) was then established. The interferences were eliminated by using matched matrix and off peak background correction. The sample digestion conditions and reagent usage were optimized. The selection of analysis spectral lines, the effects and elimination of interferences and instrument parameters are presented in this paper. This method provides the advantages of high recoveries of 97.92%-107.1% with relative standard deviations (RSD, n=12) of 0.28%-1.85% and is rapid and inexpensive. The presented method has been applied to the analysis of major elements in national standard reference of phosphate ores and the results are in agreement with certified values. -
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