Modular Ion Mobility Calibrants for Organometallic Anions Based on Tetraorganylborate Salts
| Autor: | Konrad Koszinowski, Thomas Auth, Márkó Grabarics, Maria Schlangen, Kevin Pagel |
|---|---|
| Rok vydání: | 2021 |
| Předmět: |
010405 organic chemistry
Ion-mobility spectrometry Aryl Electrospray ionization Analytical chemistry 010402 general chemistry 01 natural sciences Mass spectrometric 0104 chemical sciences Analytical Chemistry Catalysis Characterization (materials science) Ion chemistry.chemical_compound chemistry Cuprate |
| Zdroj: | Analytical Chemistry |
| ISSN: | 1520-6882 |
| Popis: | Organometallics are widely used in catalysis and synthesis. Their analysis relies heavily on mass spectrometric methods, among which traveling-wave ion mobility spectrometry (TWIMS) has gained increasing importance. Collision cross sections (CCS) obtainable by TWIMS significantly aid the structural characterization of ions in the gas phase, but for organometallics, their accuracy has been limited by the lack of appropriate calibrants. Here, we propose tetraorganylborates and their alkali-metal bound oligomers [Mn–1(BR4)n]− (M = Li, Na, K, Rb, Cs; R = aryl, Et; n = 1–6) as calibrants for electrospray ionization (ESI) TWIMS. These species chemically resemble typical organometallics and readily form upon negative-ion mode ESI of solutions of alkali-metal tetraorganylborates. By combining different tetraorganylborate salts, we have generated a large number of anions in a modular manner and determined their CCS values by drift-tube ion mobility spectrometry (DTIMS) (DTCCSHe = 81–585, DTCCSN2 = 130–704 Å2). In proof-of-concept experiments, we then applied these DTCCS values to the calibration of a TWIMS instrument and analyzed phenylcuprate and argentate anions, [Lin–1MnPh2n]− and [MnPhn+1]− (M = Cu, Ag), as prototypical reactive organometallics. The TWCCSN2 values derived from TWIMS measurements are in excellent agreement with those determined by DTIMS ( |
| Databáze: | OpenAIRE |
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