NDLI: Iron Fluoroanions and Their Clusters by Electrospray Ionization of a Fluorinating Ionic Liquid

Content Provider	Springer Nature Link
Author	Zarzana, Christopher A. Groenewold, Gary S. Benson, Michael T. Delmore, James Tsuda, Tetsuya Hagiwara, Rika
Copyright Year	2015
Abstract	Metal fluoroanions are of significant interest for fundamental structure and reactivity studies and for making isotope ratio measurements that are free from isobaric overlap. Iron fluoroanions [FeF$_{4}$]$^{–}$ and [FeF$_{3}$]$^{–}$ were generated by electrospray ionization of solutions of Fe(III) and Fe(II) with the fluorinating ionic liquid 1-ethyl-3-methylimidazolium fluorohydrogenate [EMIm]$^{+}$[F(HF)$_{2.3}$]$^{-}$. Solutions containing Fe(III) salts produce predominately uncomplexed [FeF$_{4}$]$^{–}$ in the negative ion spectrum, as do solutions containing salts of Fe(II). This behavior contrasts with that of solutions of FeCl$_{3}$ and FeCl$_{2}$ (without [EMIm]$^{+}$[F(HF)$_{2.3}$]$^{–}$) that preserve the solution-phase oxidation state by producing the gas-phase halide complexes [FeCl$_{4}$]$^{–}$ and [FeCl$_{3}$]$^{–}$, respectively. Thus, the electrospray-[EMIm]$^{+}$[F(HF)$_{2.3}$]$^{–}$ process is oxidative with respect to Fe(II). The positive ion spectra of Fe with [EMIm]$^{+}$[F(HF)$_{2.3}$]$^{–}$ displays cluster ions having the general formula [EMIm]$^{+}$ $_{(n+1)}$[FeF$_{4}$]$^{–}$ $_{n}$, and DFT calculations predict stable complexes, both of which substantiate the conclusion that [FeF$_{4}$]$^{–}$ is present in solution stabilized by the imidazolium cation. The negative ion ESI mass spectrum of the Fe-ionic liquid solution has a very low background in the region of the [FeF$_{4}$]$^{–}$ complex, and isotope ratios measured for both [FeF$_{4}$]$^{–}$ and adventitious [SiF$_{5}$]$^{–}$ produced values in close agreement with theoretical values; this suggests that very wide isotope ratio measurements should be attainable with good accuracy and precision when the ion formation scheme is implemented on a dedicated isotope ratio mass spectrometer. Graphical Abstract ᅟ
Starting Page	1559
Ending Page	1569
Page Count	11
File Format	PDF
ISSN	10440305
Journal	Journal of The American Society for Mass Spectrometry
Volume Number	26
Issue Number	9
e-ISSN	18791123
Language	English
Publisher	Springer US
Publisher Date	2015-05-08
Publisher Institution	The American Society for Mass Spectrometry
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Ionic liquid Fluoroanion Electrospray Fluorohydrogenate Isotope ratio Analytical Chemistry Biotechnology Organic Chemistry Proteomics Bioinformatics
Content Type	Text
Resource Type	Article
Subject	Spectroscopy Structural Biology

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