Electron ionization mass spectrometric analysis of air- and moisture-sensitive organometallic compounds

Abstract

Electron ionization (EI) is a reliable mass spectrometric method for the analysis of the vast majority of thermally stable and volatile compounds. In direct EI-MS, the sample is placed into the probe and introduced to the source. For air-and moisture-sensitive organometallic complexes, the sample introduction step is critical. A small quantity must be briefly exposed to the atmosphere, during which time decomposition can occur. Here we present a simple tool that allows convenient analysis of air-and moisture-sensitive organometallic species by direct probe methods: a small purge-able glove chamber affixed to the front end of the mass spectrometer.Using the upgraded mass spectrometer, we successfully characterized of a series of air-and moisture-sensitive organometallic complexes, ranging from mildly to very air-sensitive.

A mechanistic investigation of the Pd-catalyzed cross-coupling betweenN-tosylhydrazones and aryl halides

“…30 In terms of air-and moisture-free sample introduction, some techniques have been described whereby a nitrogenous atmosphere is either attached to the MS source, such as a glove bag 31,32 and a small glove chamber. 33 On a larger scale, a glovebox can be modified to accommodate a feedthrough port for tubing going directly into the MS source. 34,35 The need for a simple, cheap, robust method of air-and moisturefree sample introduction was obvious, hence the development of Pressurized Sample Infusion (PSI).…”

Handling considerations for the mass spectrometry of reactive organometallic compounds

“…[10][11][12] Other modifications, such as a small purgeable glove chamber affixed to the front end of the mass spectrometer, can also be used in the analysis of reactive organometallic species by direct probe methods. 13 This modification is more robust than a glovebag and does not require a full glovebox dedicated to analysis (Figure 1). Excellent EI spectra of air-and moisture-sensitive compounds such as ZrCp 2 Cl 2 , ZrCp 2 Me 2 , TiCp 2 Cl 2 , and TiCp 2 Cl were recorded using the glove chamber (Figure 2).…”

“…Bottom: Glove chamber in place on direct probe electron ionization mass spectrum (EI-MS). Adapted with permission from Penafiel et al 13 Copyright (2016) Royal Society of Chemistry F I G U R E 2 Electron ionization mass spectrum (EI-MS) of ZrCp 2 Me 2 (m/z 250) obtained using the glove chamber. Adapted with permission from Penafiel et al 13 Copyright (2016) Royal Society of Chemistry via microsyringe into the emitter.…”

“…Adapted with permission from Penafiel et al 13 Copyright (2016) Royal Society of Chemistry F I G U R E 2 Electron ionization mass spectrum (EI-MS) of ZrCp 2 Me 2 (m/z 250) obtained using the glove chamber. Adapted with permission from Penafiel et al 13 Copyright (2016) Royal Society of Chemistry via microsyringe into the emitter. 26 These sample preparation methods make it very difficult to study air-and moisture-sensitive compounds by FD.…”

Pressurized Sample Infusion

“…In terms of air‐ and moisture‐free sample introduction, some techniques have been described whereby a nitrogenous atmosphere is either attached to the MS source, such as a glove bag [19,20] and a small glove chamber [21] . On a larger scale, a glovebox can be modified to accommodate a feedthrough port for tubing going directly into the MS source [22,23] .…”