| 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 |
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| 引用本文： | 何海洋,董学林,于晓琪,任小荣,曾慧美.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[J].岩矿测试,2017,36(2):117-123. |
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| 作者姓名： | 何海洋 董学林 于晓琪 任小荣 曾慧美 |
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| 作者单位： | 河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省地质矿产勘查开发局第一地质勘查院, 河南 南阳 473003,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012,河南省岩石矿物测试中心, 河南 郑州 450012;国土资源部贵金属分析技术重点实验室, 河南 郑州 450012 |
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| 基金项目： | 国土资源部公益性行业科研专项（201211016-3） |
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| 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。
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| 关 键 词： | 黑色岩 铂 钯 金 相态分析 电感耦合等离子体质谱法 |
| 收稿时间： | 2016/1/27 0:00:00 |
| 修稿时间： | 2016/12/6 0:00:00 |
Determination of Phosphorus in Phosphate Ores by Inductively Coupled Plasma-Optical Emission Spectrometry Utilizing an Internal Standard Correction Method |
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| HE Hai-yang,DONG Xue-lin,YU Xiao-qi,REN Xiao-rong and ZENG Hui-mei.Determination of Phosphorus in Phosphate Ores by Inductively Coupled Plasma-Optical Emission Spectrometry Utilizing an Internal Standard Correction Method[J].Rock and Mineral Analysis,2017,36(2):117-123. |
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| Authors: | HE Hai-yang DONG Xue-lin YU Xiao-qi REN Xiao-rong and ZENG Hui-mei |
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| Institution: | Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China,Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China,Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China,Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China,Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China,The First Geo-Exploration Institute, Henan Province Bureau of Geo-Exploration and Mineral Development, Nanyang 473003, China,Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China and Henan Province Rock & Mineral Testing Centre, Zhengzhou 450012, China;Key Laboratory of Precious Metals Analysis Technology, Ministry of Land and Resources, Zhengzhou 450012, China |
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| Abstract: | Black rock as an important carrier of platinum group elements discovered in recent years, the origin and occurrence of platinum group elements in black rock are considered to be related to the geological background, sedimentary characteristics, sedimentary environment and some theories such as "collision" according to the content of iridium proposed by some scholars because of the diversity of metal sources and the complexity of mineralization. According to the mineral properties and composition of black rock, the occurrence state of Pt, Pd and Au in black rock could be divided into:exchangeable phase, organic binding phase, sulfide bound phase and residue phase. The adsorption of Pt, Pd and Au from the organic carbon in black rocks was inhibited by adding potassium thiocyanate and sodium cyanide as desorbents. The distribution of Pt, Pd and Au in each phase was identified according to the samples determined by ICP-MS after isolation and enrichment. The results showed that:(1) The ratios of the total extraction of each phase to the total amount of the element were Pt 94.4%-101%, Pd 95.8%-101% and Au 96.7%-102%. This showed that the method had good accuracy and reproducibility. (2) The enrichment of Pt, Pd and Au in black rock minerals not only had the affinity, but also had obvious correlation with the geological conditions and geological background of the formation of organic carbon. The results provide important information for studying the geochemical environment and the metallogenic regularity of the platinum group elements in black rocks. |
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| Keywords: | black rock platinum palladium gold phase analysis Inductively Coupled Plasma-Mass Spectrometry |
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