内标校正-电感耦合等离子体发射光谱法测定磷矿石中的磷

发布时间：2018-04-24 21:43

本文选题：磷矿石 + 磷　；参考：《岩矿测试》2017年02期

【摘要】：采用电感耦合等离子体发射光谱法(ICP-OES)可以同时测定磷矿石中的主、次量元素,但在实际测量过程中,仪器的漂移以及基体效应引起的分析误差不容忽视。本文以碲为内标,对高含量磷的测定进行校正,可以有效降低由仪器漂移以及基体效应引起的分析误差,12次平行测定磷的相对标准偏差(RSD)为0.5%,与未经校正的RSD值(4.1%)相比,显著提高了分析精度,极大地降低了仪器波动对测定结果的影响,因此获得了更低的方法检出限(0.0044%)。实验还对比了王水溶样与盐酸-硝酸-氢氟酸-高氯酸(四酸)溶样两种样品前处理方法对磷矿石分析的影响,结果表明:以王水对磷矿石标准物质进行快速溶解,磷、钙、铁、镁、锰等元素的测定结果与标准值间的相对误差范围为-6.7%~1.6%,满足日常测定要求;而钾、钠、铝是否能够完全溶出与样品的矿物组成及氟含量存在联系,若需要分析钾、钠、铝等元素,如果样品中的硅酸盐矿物组成不多,氟含量较高时可以考虑采用王水溶解;四酸可以完全溶解样品,适合于磷、钙、铁、镁、铝、钾、钠、锰、锶等元素的同时测定。
[Abstract]:The inductively coupled plasma emission spectrometry (ICP-OES) can be used to determine the principal and secondary elements in phosphate rock simultaneously, but in the actual measurement process, the drift of the instrument and the analysis error caused by the matrix effect can not be ignored. In this paper, using tellurium as internal standard, the determination of high content phosphorus can be corrected. The relative standard deviation (RSD) of 12 times parallel determination of phosphorus caused by instrument drift and matrix effect can be reduced to 0.5, compared with the uncorrected RSD value of 4.1). The accuracy of analysis is improved significantly and the influence of instrument fluctuation on the determination results is greatly reduced. Therefore, a lower detection limit of 0.0044 is obtained. The effects of two pretreatment methods on the analysis of phosphate rock were compared between hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid (tetracarboxylic acid). The results showed that Wang Shui was used for rapid dissolution, phosphorus and calcium of phosphate rock. The relative error between the results of determination of iron, magnesium and manganese and the standard value is -6.7 and 1.6 to meet the requirements of daily determination. However, whether potassium, sodium and aluminum can be completely dissolved is related to the mineral composition and fluorine content of the sample, if potassium, sodium, and aluminum need to be analyzed, Aluminum and other elements, if the composition of silicate minerals in the sample is not large, high fluorine content can be considered to be dissolved by Wang Shui, tetracarboxylic acid can completely dissolve the sample, suitable for phosphorus, calcium, iron, magnesium, aluminum, potassium, sodium, manganese, phosphorus, calcium, iron, magnesium, aluminum, potassium, sodium, manganese, Simultaneous determination of strontium and other elements.
【作者单位】：湖北省地质实验测试中心;
【基金】：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)
【分类号】：P575;P619.213

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