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

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...

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Main Authors: Longo Jr, Luiz S., Smith, Emily F., Licence, Peter
Format: Article
Published: American Chemical Society 2016
Online Access:https://eprints.nottingham.ac.uk/35933/
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author Longo Jr, Luiz S.
Smith, Emily F.
Licence, Peter
author_facet Longo Jr, Luiz S.
Smith, Emily F.
Licence, Peter
author_sort Longo Jr, Luiz S.
building Nottingham Research Data Repository
collection Online Access
description 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.
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spelling nottingham-359332020-05-04T18:07:27Z https://eprints.nottingham.ac.uk/35933/ Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy Longo Jr, Luiz S. Smith, Emily F. Licence, Peter 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. American Chemical Society 2016-08-09 Article PeerReviewed Longo Jr, Luiz S., 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 http://pubs.acs.org/doi/abs/10.1021/acssuschemeng.6b00919 doi:10.1021/acssuschemeng.6b00919 doi:10.1021/acssuschemeng.6b00919
spellingShingle Longo Jr, Luiz S.
Smith, Emily F.
Licence, Peter
Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title_full Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title_fullStr Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title_full_unstemmed Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title_short Study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(V) based ionic liquids using xray photoelectron spectroscopy
title_sort study of the stability of 1alkyl-3-methylimidazolium hexafluoroantimonate(v) based ionic liquids using xray photoelectron spectroscopy
url https://eprints.nottingham.ac.uk/35933/
https://eprints.nottingham.ac.uk/35933/
https://eprints.nottingham.ac.uk/35933/