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Development of REE-doped CaWO4 single crystals as reference materials for in situ microanalysis of scheelite via LA-ICP-MS
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2020-03-03 , DOI: 10.1039/d0ja00015a
Yuqiu Ke 1, 2, 3, 4, 5 , Jianzong Zhou 4, 5, 6, 7, 8 , Xiaoqing Yi 3, 4, 9, 10 , Yijian Sun 1, 2, 3, 4 , Jianfeng Shao 1, 2, 3, 4 , Shiyong You 1, 2, 3, 4 , Wei Wang 1, 2, 3, 4 , Yunzhi Tang 1, 2, 3, 4 , Chaoyang Tu 1, 2, 3, 4
Affiliation  

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been widely used for in situ microanalysis of elemental concentrations in solid samples, but its application is hampered by a lack of matrix-matched and homogeneous reference materials (RMs). In this work, a new method for preparing matrix-matched and homogeneous LA-ICP-MS reference materials has been developed. A multiple rare earth element (REE) doped CaWO4 single crystal (CaW-1) was successfully prepared by the Czochralski technique. The matrix composition and crystal structure were confirmed by X-ray diffraction (XRD) and electron microprobe analysis (EMPA), which indicates that these crystals have a matrix composition of CaWO4 and are matrix-matched with natural scheelite. The homogeneity of REE distribution was systematically studied by seven methods and the results demonstrated that REEs are distributed homogeneously in the CaWO4 single crystal with slight fluctuation (RSDs: ca. 4%). It can be concluded that the synthesized CaWO4 single crystal meets both crucial requirements, matrix-matched and homogeneous distribution, for an LA-ICP-MS reference material, and therefore it was used to quantitatively calibrate REE concentrations in natural scheelite. The results showed that acceptable analytical errors (<8%) were obtained, which were more desirable than those obtained with non-matrix-matched NIST SRM 610 as the RM. It robustly validates the ability of the developed method for preparing CaWO4 single crystals as possible LA-ICP-MS reference materials to calibrate REE concentrations in natural scheelite.

中文翻译:

稀土掺杂CaWO4单晶的开发作为参考材料,用于通过LA-ICP-MS对白钨矿进行原位微分析

激光烧蚀电感耦合等离子体质谱法(LA-ICP-MS)已被广泛用于固体样品中元素浓度的原位微分析,但由于缺乏基质匹配且均一的参比物质(RMs)而受到阻碍。在这项工作中,开发了一种制备基质匹配且均质的LA-ICP-MS参考材料的新方法。通过切克劳斯基技术成功地制备了掺稀土元素(REE)的CaWO 4单晶(CaW-1)。通过X射线衍射(XRD)和电子微探针分析(EMPA)确认了基质组成和晶体结构,这表明这些晶体具有CaWO 4的基质组成。并且与天然白钨矿基质匹配。通过7种方法对REE分布的均匀性进行了系统研究,结果表明REE在CaWO 4单晶中均匀分布,且波动很小(RSD:4%)。可以得出结论,合成的CaWO 4单晶满足LA-ICP-MS参考材料的关键要求,即基质匹配和均匀分布,因此可用于定量校准天然白钨矿中的REE浓度。结果表明,获得了可接受的分析误差(<8%),比使用非基质匹配的NIST SRM 610作为RM所获得的分析误差更可取。它有力地验证了所开发的制备CaWO 4单晶作为LA-ICP-MS参考材料的方法的能力,以便校准天然白钨矿中的REE浓度。
更新日期:2020-03-03
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