Nagai Yuichiro, Yokoyama Tetsuya
Department of Earth and Planetary Sciences, Tokyo Institute of Technology , Ookayama, Tokyo 152-8551, Japan.
Anal Chem. 2014 May 20;86(10):4856-63. doi: 10.1021/ac404223t. Epub 2014 May 6.
A new two-stage chemical separation method was established using an anion exchange resin, Eichrom 1 × 8, to separate Mo and W from four natural rock samples. First, the distribution coefficients of nine elements (Ti, Fe, Zn, Zr, Nb, Mo, Hf, Ta, and W) under various chemical conditions were determined using HCl, HNO3, and HF. On the basis of the obtained distribution coefficients, a new technique for the two-stage chemical separation of Mo and W, along with the group separation of Ti-Zr-Hf, was developed as follows: 0.4 M HCl-0.5 M HF (major elements), 9 M HCl-0.05 M HF (Ti-Zr-Hf), 9 M HCl-1 M HF (W), and 6 M HNO3-3 M HF (Mo). After the chemical procedure, Nb remaining in the W fraction was separated using 9 M HCl-3 M HF. On the other hand, Nb and Zn remaining in the Mo fraction were removed using 2 M HF and 6 M HCl-0.1 M HF. The performance of this technique was evaluated by separating these elements from two terrestrial and two extraterrestrial samples. The recovery yields for Mo, W, Zr, and Hf were nearly 100% for all of the examined samples. The total contents of the Zr, Hf, W, and Mo in the blanks used for the chemical separation procedure were 582, 9, 29, and 396 pg, respectively. Therefore, our new separation technique can be widely used in various fields of geochemistry, cosmochemistry, and environmental sciences and particularly for multi-isotope analysis of these elements from a single sample with significant internal isotope heterogeneities.
建立了一种新的两步化学分离方法,使用阴离子交换树脂Eichrom 1×8从四个天然岩石样品中分离钼和钨。首先,使用HCl、HNO₃和HF测定了九种元素(Ti、Fe、Zn、Zr、Nb、Mo、Hf、Ta和W)在各种化学条件下的分配系数。基于获得的分配系数,开发了一种新的钼和钨两步化学分离技术以及Ti-Zr-Hf的分组分离技术,具体如下:0.4 M HCl-0.5 M HF(主要元素)、9 M HCl-0.05 M HF(Ti-Zr-Hf)、9 M HCl-1 M HF(W)和6 M HNO₃-3 M HF(Mo)。化学分离步骤完成后,使用9 M HCl-3 M HF分离钨组分中残留的Nb。另一方面,使用2 M HF和6 M HCl-0.1 M HF去除钼组分中残留的Nb和Zn。通过从两个地球样品和两个外星样品中分离这些元素来评估该技术的性能。对于所有检测样品,Mo、W、Zr和Hf的回收率接近100%。化学分离步骤所用空白样品中Zr、Hf、W和Mo的总含量分别为582、9、29和396 pg。因此,我们的新分离技术可广泛应用于地球化学、宇宙化学和环境科学的各个领域,尤其适用于对具有显著内部同位素非均一性的单个样品中的这些元素进行多同位素分析。