中国地质学会岩矿测试技术专业委员会、国家地质实验测试中心主办

树脂柱串联法分离地质样品中Sr-Nd-U

骆正骅, 李超, 赖正, 王晨羽, 郭玉龙, 段知非, 徐娟, 杨守业. 树脂柱串联法分离地质样品中Sr-Nd-U[J]. 岩矿测试, 2023, 42(1): 102-113. doi: 10.15898/j.cnki.11-2131/td.202204060072
引用本文: 骆正骅, 李超, 赖正, 王晨羽, 郭玉龙, 段知非, 徐娟, 杨守业. 树脂柱串联法分离地质样品中Sr-Nd-U[J]. 岩矿测试, 2023, 42(1): 102-113. doi: 10.15898/j.cnki.11-2131/td.202204060072
LUO Zhenghua, LI Chao, LAI Zheng, WANG Chenyu, GUO Yulong, DUAN Zhifei, XU Juan, YANG Shouye. Separation of Sr, Nd, and U from Geological Samples Using Tandem Resin Column[J]. Rock and Mineral Analysis, 2023, 42(1): 102-113. doi: 10.15898/j.cnki.11-2131/td.202204060072
Citation: LUO Zhenghua, LI Chao, LAI Zheng, WANG Chenyu, GUO Yulong, DUAN Zhifei, XU Juan, YANG Shouye. Separation of Sr, Nd, and U from Geological Samples Using Tandem Resin Column[J]. Rock and Mineral Analysis, 2023, 42(1): 102-113. doi: 10.15898/j.cnki.11-2131/td.202204060072

树脂柱串联法分离地质样品中Sr-Nd-U

  • 基金项目:
    国家自然科学基金项目(42076063, 41991324);上海市自然科学基金项目(20ZR1460400, 21590712700)
详细信息
    作者简介: 骆正骅,硕士研究生,海洋地球化学专业。E-mail:luozh@tongji.edu.cn
    通讯作者: 李超,博士,副教授,从事边缘海沉积地球化学研究。E-mail:cli@tongji.edu.cn
  • 中图分类号: O657.63

Separation of Sr, Nd, and U from Geological Samples Using Tandem Resin Column

More Information
  • Sr、Nd、U等同位素体系被广泛应用于地球表生过程中年代测定及物源示踪等研究, 高效地分离这些同位素体系,对于推广这些同位素方法的应用具有重要现实意义。若要同时分析地质样品中Sr、Nd、U三种元素的同位素,现有方法往往需要消解两份样品,一份用于Sr-Nd而另一份用于U的分离提纯。这种方法不但增加了样品用量,而且需要多次蒸干溶液转换介质,既延长了分离流程也增加了样品被污染的风险。为了提高样品利用率和分析效率,本文通过将树脂柱串联改进了分离流程,提出一种仅需消解一份样品,便可同时提取Sr、Nd、U三种元素的新方法。本方法中Sr的分离采用Sr特效树脂,包含Nd在内的稀土元素(REE)的分离采用AG50W-X8树脂,U的分离采用UTEVA特效树脂。实验中将三种树脂柱串联,采用3mol/L硝酸淋洗液淋洗,同步进行平衡树脂、上样、洗杂志,避免了蒸干操作。分离后的淋出液使用电感耦合等离子体质谱仪(ICP-MS)测试元素含量。结果表明:U的回收率接近99.9%,Sr的回收率超过90%,Nd的回收率超过80%;同时三种树脂柱串联的分离流程,主要基体元素(K、Ca、Na、Ba、Fe、Rb等)的去除率均超过99%,降低了对Sr、Nd、U高精度同位素分析的干扰;REE中的Sm则可以通过后续使用Ln树脂等进一步去除。此外,本文还交换了Sr特效树脂和UTEVA树脂的位置,比对两种不同串联顺序对分离结果的影响,结果表明两种树脂柱串联顺序对目标元素的分离并无显著影响。使用该方法可以有效地实现Sr、Nd、U的分离,在减少操作步骤的同时节省约一半的样品用量,提高了同位素分析效率。

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  • 图 1  Sr、Nd、U同位素联合分离流程示意图

    Figure 1. 

    图 2  方案一中Sr-Nd-U在不同馏分中的回收率

    Figure 2. 

    图 3  方案二中Sr-Nd-U在不同馏分中的回收率

    Figure 3. 

    图 4  更新AG50W-X8树脂后Nd的回收率

    Figure 4. 

    表 1  Sr、Nd、U同位素联合过柱分离流程

    Table 1.  Procedure of combined Sr, Nd, U isotopes separation

    流程 分离步骤 树脂柱 淋洗试剂 试剂总体积
    (mL)
    馏分
    编号

    预清洗
    本底清洗 Sr特效树脂 3mol/L硝酸 6 -
    超纯水 6 -
    3mol/L硝酸 5 -
    超纯水 5 -
    3mol/L硝酸 5 -
    超纯水 5 -
    AG50W-X8
    树脂
    6mol/L盐酸 15 -
    超纯水 5 -
    UTEVA特效
    树脂
    3mol/L硝酸 4 -
    3mol/L盐酸 4 -
    3mol/L盐酸 4 -
    超纯水 4 -

    三柱串联
    平衡树脂 - 3mol/L硝酸 3 -
    上样 3mol/L硝酸 2 1
    洗杂质 3mol/L硝酸 6

    三柱分离
    洗杂质 Sr特效
    树脂
    3mol/L硝酸 9 2
    收集Sr 超纯水 4 3
    回收树脂 6mol/L盐酸+超纯水 11 4
    洗杂质 AG50W-X8
    树脂
    2.5mol/L盐酸 4 5
    收集REE 6mol/L盐酸 10 6
    回收树脂 6mol/L盐酸 5 7
    洗杂质 UTEVA特效
    树脂
    3mol/L盐酸 6 8
    收集U 1mol/L盐酸 4 9
    回收树脂 超纯水+3mol/L硝酸 +3mol/L盐酸 +1mol/L盐酸 20 10
    下载: 导出CSV
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出版历程
收稿日期:  2022-04-06
修回日期:  2022-05-17
录用日期:  2022-05-23
刊出日期:  2023-01-28

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