| 陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196 |
| CHEN Bo,LIU Hong-qing,XING Ying-xiang.Simultaneous Determination of Ge, Se and Te in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196.DOI: |
| 电感耦合等离子体质谱法同时测定地质样品中锗硒碲 |
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| Simultaneous Determination of Ge, Se and Te in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry |
| 投稿时间：2013-07-05 修订日期：2014-01-23 |
| DOI： |
| 中文关键词: 地质样品 锗 硒 碲 电感耦合等离子体质谱法 乙醇 |
| 英文关键词: geological samples Ge Se Te Inductively Coupled Plasma-Mass Spectrometry ethanol |
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| 摘要点击次数: 1431 |
| 全文下载次数: 1639 |
| 中文摘要: |
| 锗、硒、碲三个元素的分析需要分别采用硝酸-氢氟酸-高氯酸-磷酸、硝酸-氢氟酸-高氯酸两种溶样体系，原子荧光光谱（AFS）、电感耦合等离子体质谱（ICP-MS）两种仪器进行测定，对于大批量地质样品的分析成本高、测试效率低。本文建立了在同一份溶液中用ICP-MS同一种仪器测定锗、硒、碲三元素的方法。样品用硝酸-氢氟酸-硫酸一种体系分解，试液以50%硝酸提取，3%乙醇定容，避免乙醇在复溶时的挥发损失，保证了试样溶液中的乙醇浓度均为最佳增敏作用所需值。试样分解过程中没有使用盐酸，避免了氯离子存在给锗、碲造成的损失。在3%硝酸-3%乙醇介质中硒、碲的灵敏度提高了2.2倍、3.7倍。同时克服了ICP-MS测定硒、碲难电离、灵敏度低的问题，保证了方法稳定性；CCT碰撞池技术消除了氩的多原子离子对硒测定干扰，提高了方法准确度。本方法通过分析国家一级标准物质进行验证，测定值与标准值基本一致，相对标准偏差（RSD，n=4）小于5%，样品前处理过程简单，分析效率高。 |
| 英文摘要: |
| The analysis of Ge, Se and Te requires that samples be dissolved by two different acid systems of HNO3-HF-HClO4-H3PO4 and HNO3-HF-HClO4, and determined by Atomic Fluorescence Spectrometry (AFS) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This method is expensive and has a low efficiency for large quantities of geological samples. A method for determination of Ge, Se and Te in the same solution by using HNO3-HF-HClO4 acid system with ICP-MS has been developed. By this method, the sample solutions are extracted with 50% nitric acid, and 3% ethanol added. In order to avoid alcohol volatilization in the secondary dissolved solution, the concentration of ethanol is the optimal value for the best sensitization. No HCl was used for sample decomposition, avoiding the loss of Ge and Te by chloride ion. The sensitivities of Se and Te in 3% Nitrate-3% ethanol medium were increased by 2.2 and 3.7 times, respectively. The difficult ionization and low sensitivity for Se and Te by ICP-MS was also overcome by using this method, which improved the method's stability. CCT eliminated the interferences of polyatomic ions of argon on Se, and improved the accuracy of the method. This method was verified by determine Standard Reference materials, and the results are in agreement with the certified values with precision of less than 10% RSD (n=4). This method can be used for the rapid determination of Ge, Se and Te in geological samples and has the advantages of simple preparation and high analysis efficiency. |
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