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Trace Elemental Analysis of Bulk Thorium Using an Automated Separation–Inductively Coupled Plasma Optical Emission Spectroscopy Methodology
Applied Spectroscopy ( IF 2.2 ) Pub Date : 2020-10-08 , DOI: 10.1177/0003702820961390
Benjamin T. Manard 1 , Shalina C. Metzger 1 , Sarah K. Wysor 1 , Veronica C. Bradley 1, 2 , Benjamin D. Roach 1 , N.Alex Zirakparvar 1 , Kayron T. Rogers 1 , Debra A. Bostick 1 , Brian W. Ticknor 1 , Cole R. Hexel 1
Affiliation  

Presented here is a novel automated method for determining the trace element composition of bulk thorium by inductively coupled plasma-optical emission spectroscopy (ICP-OES). ICP-OES is a universal approach for measuring the trace elemental impurities present in actinide-rich materials; however, due to the emission rich spectrum of the actinide, a separation from the trace elements is warranted for spectrochemical analysis. Here, AG MP-1 ion exchange resin was utilized for retention of the Th matrix, while allowing the trace element impurities to be separated prior to subsequent analysis using ICP-OES. After demonstrating the separation on traditional gravity-driven columns, the methodology was transitioned to an automated platform for comparison. This automated platform utilizes syringe-driven sample and solvent flow and can collect the trace element and thorium fractions in separate locations. While reducing the sample size (500 µL, 1.5 mg of Th), maintaining the overall separation efficiency (recoveries >95%), and illustrating the sample throughput ability (n = 10+), this automated methodology could be readily adopted to nuclear facilities in which the determination of trace elemental impurities in Th samples is warranted.

中文翻译:

使用自动分离-电感耦合等离子体发射光谱方法对大块钍进行痕量元素分析

这里介绍了一种通过电感耦合等离子体光发射光谱 (ICP-OES) 测定块状钍痕量元素组成的新型自动化方法。ICP-OES 是测量富含锕系元素材料中存在的痕量元素杂质的通用方法;然而,由于锕系元素的发射光谱丰富,因此有必要将其与痕量元素分离以进行光谱化学分析。在这里,AG MP-1 离子交换树脂用于保留 Th 基质,同时允许在使用 ICP-OES 进行后续分析之前分离痕量元素杂质。在传统重力驱动柱上演示分离后,该方法被转换到自动化平台进行比较。这个自动化平台利用注射器驱动的样品和溶剂流,可以在不同的位置收集痕量元素和钍馏分。在减少样品量(500 µL,1.5 mg Th)、保持整体分离效率(回收率 > 95%)并说明样品通量能力(n = 10+)的同时,这种自动化方法可以很容易地应用于核设施其中Th样品中痕量元素杂质的测定是有保证的。
更新日期:2020-10-08
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