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使用电感耦合等离子体发射光谱法(ICP-OES)检测进行痕量元素分析的在线铀分离评估与规范

Evaluation and Specifications for In-Line Uranium Separations Using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) Detection for Trace Elemental Analysis.

作者信息

Manard Benjamin T, Metzger Shalina C, Quarles C Derrick, Rogers Kayron T, Ticknor Brian W, Bostick Debra A, McBay Eddy H, Hexel Cole R

机构信息

1 Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN, USA.

2 Elemental Scientific, Inc., Omaha, NE, USA.

出版信息

Appl Spectrosc. 2019 Aug;73(8):927-935. doi: 10.1177/0003702819837650. Epub 2019 Mar 27.

DOI:10.1177/0003702819837650
PMID:30803262
Abstract

Automated introduction platforms integrated with inductively coupled plasma optical emission spectroscopy (ICP-OES) systems are continuously being improved. Expanding on the introduction systems, a newly developed automated ion chromatography system was explored for performing rapid in-line separations coupled to ICP-OES for the detection of trace elements in uranium. Trace elements are separated from a uranium material and the analytes are directed into the ICP-OES for subsequent detection. Detection parameters such as exposure time frequency, wavelength selection, and settling times were explored to gain insight on optimal detection schemes for in-line trace elemental analysis. The methodology was applied in the analysis of a uranium oxide (UO) certified reference material, CRM-124. It was found here that the sensitivity and uncertainty of the technique are greatly affected by how the ICP-OES is employed to collect data. Overall it was determined that faster exposure replicates can provide greater peak resolution with higher fidelity measurements but are limited with respect to the total analysis time (i.e., limited in detection timely separations). Zeta scores, which combine accuracy and uncertainty of certified values and experimental values, were used to validate the ICP-OES modes of operation.

摘要

与电感耦合等离子体发射光谱仪(ICP - OES)系统集成的自动化进样平台在不断改进。在进样系统方面进行拓展,研究了一种新开发的自动化离子色谱系统,用于与ICP - OES联用进行快速在线分离,以检测铀中的微量元素。从铀材料中分离出微量元素,并将分析物导入ICP - OES进行后续检测。研究了诸如曝光时间频率、波长选择和稳定时间等检测参数,以深入了解在线痕量元素分析的最佳检测方案。该方法应用于氧化铀(UO)标准参考物质CRM - 124的分析。在此发现,该技术的灵敏度和不确定度受ICP - OES用于收集数据的方式影响很大。总体而言,确定更快的曝光重复次数可以提供更高的峰分辨率和更高保真度的测量,但在总分析时间方面受到限制(即,在检测及时分离方面受到限制)。结合认证值和实验值的准确性和不确定度的Zeta分数用于验证ICP - OES的操作模式。

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