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实现对高空气敏感有机金属化合物的 LIFDI-MS 测量:一种 MS/手套箱联用技术。

Enabling LIFDI-MS measurements of highly air sensitive organometallic compounds: a combined MS/glovebox technique.

机构信息

Department of Chemistry, Technical University of Munich, Lichtenbergstraße 4, D-85748 Garching, Germany.

LINDEN CMS GmbH, Auf dem Berge 25, D-28844 Weyhe, Germany.

出版信息

Dalton Trans. 2021 Jul 6;50(26):9031-9036. doi: 10.1039/d1dt00978h.

DOI:10.1039/d1dt00978h
PMID:33970171
Abstract

A new setup combining a ThermoFisher Exactive Plus Orbitrap Mass Spectrometer with a liquid injection field desorption ionization (LIFDI) source directly connected to an inert atmosphere glovebox is presented. The described setup allows for the analysis of very air- and moisture sensitive samples. Furthermore, the soft nature of LIFDI ionization gives access to the molecular ions of fragile molecules. This new setup is therefore especially useful for sensitive organometallic complexes. The functionality of the new setup is tested against [(Cp)2TiCl]˙, which is known for its notorious sensitivity to air and moisture. Its drastic colour change from green to orange upon exposure to air further supports the easy detection of traces of oxygen during the experiment. In addition, we applied this setup to the mass spectrometric analysis of the qualitative composition of a Cu/Al cluster mixture, which is not accessible by other analytical methods.

摘要

一种新的组合,将 ThermoFisher Exactive Plus Orbitrap 质谱仪与直接连接到惰性气氛手套箱的液体注射场解吸电离(LIFDI)源相结合,被呈现出来。该描述的组合允许对非常空气和水分敏感的样品进行分析。此外,LIFDI 电离的软性质使得可以获得脆弱分子的分子离子。因此,这种新的组合对于敏感的有机金属配合物特别有用。该新组合的功能通过 [(Cp)2TiCl]˙进行了测试,该物质因其对空气和水分的敏感性而闻名。它在暴露于空气中时从绿色变为橙色的剧烈颜色变化进一步支持了在实验过程中容易检测到氧气痕迹。此外,我们将该组合应用于 Cu/Al 团簇混合物的质谱分析,这是其他分析方法无法获得的。

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