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采用光化学蒸气发生-电感耦合等离子体质谱法同时检测钌和锇。

Simultaneous Detection of Ruthenium and Osmium by Photochemical Vapor Generation-Inductively Coupled Plasma-Mass Spectrometry.

机构信息

Key Laboratory of Green Chemistry & Technology of MOE, College of Chemistry, Sichuan University, Chengdu, Sichuan 610064, China.

College of Chemistry and Material Science, Sichuan Normal University, Chengdu, Sichuan 610068, China.

出版信息

Anal Chem. 2022 Jan 18;94(2):593-599. doi: 10.1021/acs.analchem.1c03357. Epub 2021 Dec 21.

Abstract

Efficient simultaneous photochemical vapor generation (PVG) of ruthenium (Ru) and osmium (Os) in the medium of formic acid was demonstrated. A flow-through photoreactor hyphenated to an inductively coupled plasma-mass spectrometer (ICP-MS) was used for the PVG and subsequent detection of the two elements. A similar synergistic enhancement from cobalt and cadmium ions on the PVG efficiency of both Ru and Os was discovered. Following the critical evaluation of the impacts of various transition metal ions, the concentrations of formic acid, cobalt, and cadmium ions, the flow rate of carrier gas, and the UV irradiation time, impressive limits of detection (LODs) of 5 and 0.5 ng L were achieved for Ru and Os, respectively. The accuracy of the proposed PVG-ICP-MS method was validated by the analysis of several water samples with desirable spike recoveries obtained. Furthermore, the volatile compounds of Ru were directed and cryogenically trapped in acetonitrile and generation of carbonyls of Ru was verified by high-resolution electrospray ionization-mass spectra (ESI-MS).

摘要

本文展示了在甲酸介质中高效同时光化学汽相发生(PVG)钌(Ru)和锇(Os)的方法。采用流通式光反应器与电感耦合等离子体质谱仪(ICP-MS)联用,用于 PVG 以及随后对这两种元素的检测。发现钴和镉离子对 Ru 和 Os 的 PVG 效率具有类似的协同增强作用。在对各种过渡金属离子的影响进行了关键性评估后,确定了甲酸、钴和镉离子的浓度、载气流速和 UV 照射时间,从而实现了对 Ru 和 Os 的检测限(LOD)分别达到 5 和 0.5 ng L 的优异水平。通过对几个水样的分析,验证了所提出的 PVG-ICP-MS 方法的准确性,得到了令人满意的加标回收率。此外,通过高分辨率电喷雾电离质谱(ESI-MS)证实了 Ru 的挥发性化合物被引导并在乙腈中低温捕获,生成了 Ru 的羰基化合物。

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