Manard Benjamin T, Metzger Shalina C, Wysor Sarah K, Bradley Veronica C, Roach Benjamin D, Zirakparvar N Alex, Rogers Kayron T, Bostick Debra A, Ticknor Brian W, Hexel Cole R
Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA.
Department of Chemistry, University of Missouri, Columbia, MO, USA.
Appl Spectrosc. 2021 May;75(5):556-564. doi: 10.1177/0003702820961390. Epub 2020 Oct 8.
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.
本文介绍了一种通过电感耦合等离子体发射光谱法（ICP-OES）测定大量钍中微量元素组成的新型自动化方法。ICP-OES是一种用于测量富含锕系元素材料中痕量元素杂质的通用方法；然而，由于锕系元素发射光谱丰富，在进行光谱化学分析时，需要将其与微量元素分离。在此，使用AG MP-1离子交换树脂保留钍基体，同时在后续使用ICP-OES分析之前，使微量元素杂质得以分离。在传统重力驱动柱上演示了分离过程后，该方法被转移到自动化平台进行比较。这个自动化平台利用注射器驱动样品和溶剂流动，并能在不同位置收集微量元素和钍馏分。在减少样品量（500 μL，1.5 mg钍）、保持整体分离效率（回收率>95%）并展示样品通量能力（n = 10+）的同时，这种自动化方法可以很容易地应用于需要测定钍样品中微量元素杂质的核设施。
