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阳国运, 唐裴颖, 张洁, 战大川, 覃盛, 何雨珊. 电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗[J]. 岩矿测试, 2019, 38(2): 154-159. DOI: 10.15898/j.cnki.11-2131/td.201805070055
引用本文: 阳国运, 唐裴颖, 张洁, 战大川, 覃盛, 何雨珊. 电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗[J]. 岩矿测试, 2019, 38(2): 154-159. DOI: 10.15898/j.cnki.11-2131/td.201805070055
Guo-yun YANG, Pei-ying TANG, Jie ZHANG, Da-chuan ZHAN, Sheng QIN, Yu-shan HE. Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(2): 154-159. DOI: 10.15898/j.cnki.11-2131/td.201805070055
Citation: Guo-yun YANG, Pei-ying TANG, Jie ZHANG, Da-chuan ZHAN, Sheng QIN, Yu-shan HE. Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(2): 154-159. DOI: 10.15898/j.cnki.11-2131/td.201805070055

电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗

Determination of Boron, Iodine, Tin and Germanium in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry

  • 摘要: 在多目标的配套方法中,硼、碘、锡、锗四个元素的分析涉及三个配套方法,发射光谱法测定硼、锡,原子荧光光谱法测定锗,分光光度法或电感耦合等离子体质谱法(ICP-MS)测定碘,分析成本高、检测效率低。本文建立了一种ICP-MS同时测定地球化学样品中硼、碘、锡、锗的方法。样品用过氧化钠熔矿,使难熔元素锡分解完全,熔盐经水提取后加入铼内标,再用阳离子交换树脂分离大量钠盐及大部分阳离子,保证了盐分满足质谱测定的要求。方法检出限分别为硼0.92μg/g、碘0.10μg/g、锡0.29μg/g、锗0.09μg/g,满足多目标测试要求。用国家一级标准物质验证,测定值与认定值一致,相对标准偏差(RSD,n=12)≤ 5%,适用于批量地球化学样品中硼、碘、锡、锗的测定,样品处理过程简便,检测效率高。

     

    Abstract:
    BACKGROUNDIn the multi-objective method, the analysis of four elements of boron, iodine, tin and germanium involves three supporting methods. Boron and tin were determined by Emission Spectrometry, germanium was determined by Atomic Fluorescence Spectrometry, and iodine was determined by Spectrophotometry or Inductively Coupled Plasma-Mass Spectrometry. The analysis cost is high and the detection efficiency is low.
    OBJECTIVESTo establish an easy, highly efficient and precise, low-cost method for determination of boron, iodine, tin and germanium in geochemical samples by Inductively Coupled Plasma-Mass Spectrometry.
    METHODSThe sample is fused with sodium peroxide to completely decompose the refractory element tin. The molten salt is extracted by water and the internal standard is added, and then the cation exchange resin is used to separate a large amount of sodium salt and most of the cations, ensuring that the salt meets the requirements of mass spectrometry analysis.
    RESULTSThe element detection limits were 0.92μg/g, 0.10μg/g, 0.29μg/g, 0.09μg/g for boron, iodine, tin and germanium, respectively. The relative standard deviation (RSD, n=12) was smaller than 5%. The method was verified by certified reference materials, and the measured values were consistent with the certified values.
    CONCLUSIONSThe method is suitable for the determination of boron, iodine, tin and germanium in batch geochemical samples.

     

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