Determination of Rhenium in Geological Samples by Isotope Dilution–Multicollector–Inductively Coupled Plasma-Mass Spectrometry with Novel Chromatographic Separation
Determination of Rhenium in Geological Samples by Isotope Dilution–Multicollector–Inductively Coupled Plasma-Mass Spectrometry with Novel Chromatographic Separation
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DOI：
10.1080/00032719.2017.1371727
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发表时间：
2018-02
影响因子：
2
通讯作者：
Xiaoxiao Huang;Yali Sun;Yahui Yue;Shouqian Zhao;X. Long
中科院分区：
文献类型：
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作者：
Xiaoxiao Huang;Yali Sun;Yahui Yue;Shouqian Zhao;X. Long
摘要建立了离子交换树脂萃取-多接收电感耦合等离子体质谱法（MC-ICP-MS）测定地质样品中痕量稀土元素的方法。样品在Carius管中消化，锇转化为挥发性OsO 4，通过蒸馏和微蒸馏纯化。用负热电离质谱法测定了纯化的锇含量和同位素比值。Os蒸馏后，样品用HF处理，然后用1.2 M HCl处理，并加载到离子交换树脂柱上。Re用0.75 M HNO 3洗脱并直接用MC-ICP-MS测定。该方法使用一系列参比物质进行了验证，分析Re数据与文献值一致。该方法的精密度（相对标准偏差）范围为0.8%至6%。Re的程序空白和检测限（3σ）分别为1.1 pg和0.5 pg/g（样品量为2g）。结果表明，该方法可用于地质样品中痕量铼的测定。采用Carius管消解结合HF脱硅和复溶的方法，测定了几种标准物质可溶相和不溶相中的Re和Os含量，结果表明Re和Os的分布分别为均匀和不均匀分布。
ABSTRACT A method was developed to determine rhenium contents in geological samples using multicollector–inductively coupled plasma-mass spectrometry (MC–ICP-MS) and extraction with an ion-exchange resin. Samples were digested in Carius tubes and osmium was converted into volatile OsO4, which was purified by distillation and microdistillation. The purified Os contents and isotopic ratios were determined using negative thermal ionization mass spectrometry. After the distillation of Os, the samples were treated with HF, then 1.2 M HCl, and loaded on ion-exchange resin columns. Re was eluted using 0.75 M HNO3 and directly determined by MC–ICP-MS. This method was validated using a series of reference materials and the analytical Re data are consistent with the literature values. This method precision (relative standard deviation) ranged from 0.8 to 6%. The procedural blank and detection limit (3σ) of Re were 1.1 pg and 0.5 pg/g (for a sample size of 2g), respectively. These results indicate that the proposed method can be applied to determine trace Re in geological samples. Using Carius tube digestion combined with HF desilicification and redissolution, the Re and Os contents found in the soluble and insoluble phases of several reference materials indicated that the distributions of Re and Os were homogeneous and heterogeneous, respectively.