Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy

Longo Jr, Luiz S. and Smith, Emily F. and Licence, Peter (2016) Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy. ACS Sustainable Chemistry and Engineering . ISSN 2168-0485

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Abstract

A series of highly pure 1-alkyl-3-methylimidazolium hexafluoroantimonate (V) ionic liquids was firstly investigated by XPS. Reliable binding energy values for all elements within the samples were obtained by applying a C 1s fitting model previously employed for other imidazolium ionic liquids, based on setting the C 1s aliphatic component to 285.0 eV when alkyl chains are longer than 8 carbons. We also observed a straightforward X-ray-mediated photoreduction of Sb (V) to Sb (III) species, i.e. reduction of [SbF6]- anion to volatile SbF3. Thus, binding energies values observed at 542.5 eV and 533.1 eV were attributed to Sb 3d3/2 (V) and Sb 3d5/2 (V), respectively, whereas values at 541.0 eV and 531.7 eV were found for Sb 3d3/2 (III) and Sb 3d5/2 (III), respectively. The SbF3 being formed can be lost either by evaporation and/or redistribution to the bulk. Providing the sample is cooled to freezing temperatures, the SbF3 is prevented from escaping the ionic liquid and it accumulated on the surface of cooled [C4C1Im][SbF6] and [C8C1Im][SbF6]. Particularly in the case of prolonged X-ray exposure of a cooled [C4C1Im][SbF6], an unprecedented further reduction of Sb (III) to Sb (0) was noticed. This study provides fundamental knowledge on the XPS data for antimony compounds as well as providing a step towards the surface analysis of materials composed by antimony species, notably the hexafluoroantimonate (V) anion.

Item Type: Article
Additional Information: This document is the Accepted Manuscript version of a Published Work that appeared in final form in ACS Sustainable Chemistry and Engineering, copyright © American Chemical Society after peer review and technical editing by the publisher.
Schools/Departments: University of Nottingham UK Campus > Faculty of Science > School of Chemistry
Identification Number: https://doi.org/10.1021/acssuschemeng.6b00919
Depositing User: Bramwell, Roseanna
Date Deposited: 22 Aug 2016 15:41
Last Modified: 22 Aug 2016 15:41
URI: http://eprints.nottingham.ac.uk/id/eprint/35933

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