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NaO 烧结和 ICP-MS 分析测定富硅酸盐样品中稀土元素的分析方法的开发与应用。

Development and application of an analysis method for the determination of rare earth elements in silicate-rich samples by NaO sintering and ICP-MS analysis.

机构信息

Faculty of Chemistry, "Alexandru Ioan Cuza" University of Iasi, 11 Carol I, 700506, Iasi, Romania.

Department of Exact and Natural Sciences, Integrated Center of Environmental Science Studies in the North Eastern Region (CERNESIM), The Institute of Interdisciplinary Research, "Alexandru Ioan Cuza" University of Iasi, 11 Carol I, 700506, Iasi, Romania.

出版信息

Anal Sci. 2022 Nov;38(11):1395-1406. doi: 10.1007/s44211-022-00172-w. Epub 2022 Aug 8.

Abstract

The performance of a fast and simple analytical procedure for rare earth elements (REEs) quantification from secondary sources was investigated in the present work. Seven silicate-rich certified reference materials (CRMs) in the form of Andesite (JA-1), Basalt (JB-3), Rhyolite (JR-1, JR-2), Granite (JG-2), Granodiorite (JG-3), and Till (TILL-1), were used for the optimization and characterization of the analysis method. The optimized method was used in the analysis of nine mining wastes selected within the ENVIREE project, under the ERA-MIN Program of the 7th Framework, having as the main aim to ensure a policy securing long-term access of REEs secondary sources at reasonable costs. For silicate-rich samples efficient solid dissolution involves sintering with NaO at 460 °C and a sample to oxidizing reagent ratio of 1:6.5. Inductively coupled plasma-mass spectrometry (ICP-MS) was used in the quantification of the REEs with aerosol dilution of samples applied to minimize the salt effect on the plasma and interface regions. The work performed in the present study clearly shows that accurate reports on the REE concentrations from geological matrices also involves as mandatory the estimation of the overall uncertainty from various sources (sample preparation or analyte measurements). In the analysis of geological samples, the proposed analysis method has on average 23% of the overall uncertainty explained by the sample preparation and 77% accounted by the analysis steps. Moreover, the method described by effective, cheap, robust and safe attributes, can be recommended as an accessible alternative to the HF wet digestion method. Although from all the investigated tailings samples, only those from Sweden and Czech Republic can be regarded as potential secondary sources for REEs, investigation of other resources with interest at European level might bring a great benefit in the general attempt to develop an economically viable method for the production of rare earth elements.

摘要

本工作研究了一种快速、简单的分析程序,用于从二次资源中定量测定稀土元素(REEs)。使用 7 种富含硅酸盐的认证参考物质(CRMs),形式为安山岩(JA-1)、玄武岩(JB-3)、流纹岩(JR-1、JR-2)、花岗岩(JG-2)、花岗闪长岩(JG-3)和底土(TILL-1),优化和表征分析方法。在 ERA-MIN 计划的 7 框架下的 ENVIREE 项目中,选择了 9 种矿业废料进行分析,优化后的方法用于分析,主要目的是确保以合理的成本长期获得稀土元素二次资源的政策安全。对于富含硅酸盐的样品,有效的固相溶解需要在 460°C 下与 NaO 烧结,并将样品与氧化试剂的比例控制在 1:6.5。电感耦合等离子体质谱法(ICP-MS)用于定量测定 REEs,通过气溶胶稀释样品,以最大程度地减少盐对等离子体和界面区域的影响。本研究表明,准确报告地质基质中的 REE 浓度还需要估算来自各种来源的总不确定性(样品制备或分析物测量)。在分析地质样品时,所提出的分析方法中,有 23%的总不确定性是由样品制备引起的,77%是由分析步骤引起的。此外,该方法具有有效、廉价、稳健和安全的特点,可作为 HF 湿法消解方法的替代方法。虽然从所有调查的尾矿样品中,只有瑞典和捷克共和国的尾矿样品可以被视为 REEs 的潜在二次资源,但对欧洲感兴趣的其他资源进行调查可能会在开发经济可行的稀土元素生产方法方面带来巨大益处。

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