Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry

Thermal decomposition (TD) products of the ionic liquids (ILs) [CnC1Im][BF4] and [CnC1Im][PF6] ([CnC1Im]+ = 1-alkyl-3-methylimidazolium, [BF4]- = tetrafluoroborate, and [PF6]- = hexafluorophosphate) were prepared, ex situ, by bulk heating experiments in a bespoke setup. The respective products, CnC...

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Main Authors: Clarke, Coby James, Puttick, Simon, Sanderson, Thomas J., Taylor, Alasdair, Bourne, Richard A., Lovelock, Kevin R.J., Licence, Peter
Format: Article
Published: Royal Society of Chemistry 2018
Online Access:https://eprints.nottingham.ac.uk/52225/
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author Clarke, Coby James
Puttick, Simon
Sanderson, Thomas J.
Taylor, Alasdair
Bourne, Richard A.
Lovelock, Kevin R.J.
Licence, Peter
author_facet Clarke, Coby James
Puttick, Simon
Sanderson, Thomas J.
Taylor, Alasdair
Bourne, Richard A.
Lovelock, Kevin R.J.
Licence, Peter
author_sort Clarke, Coby James
building Nottingham Research Data Repository
collection Online Access
description Thermal decomposition (TD) products of the ionic liquids (ILs) [CnC1Im][BF4] and [CnC1Im][PF6] ([CnC1Im]+ = 1-alkyl-3-methylimidazolium, [BF4]- = tetrafluoroborate, and [PF6]- = hexafluorophosphate) were prepared, ex situ, by bulk heating experiments in a bespoke setup. The respective products, CnC1(C3N2H2)BF3 and CnC1(C3N2H2)PF5 (1-alkyl-3-methylimidazolium-2trifluoroborate and 1-alkyl-3-methylimidazolium-2-pentafluorophosphate), were then vaporized and analyzed by direct insertion mass spectrometry (DIMS) in order to identify their characteristic MS signals. During IL DIMS experiments we were subsequently able, in situ, to identify and monitor signals due to both IL vaporization and IL thermal decomposition. These decomposition products have not been observed in situ during previous analytical vaporization studies of similar ILs. The ex situ preparation of TD products is therefore perfectly complimentary to in situ thermal stability measurements. Experimental parameters such as sample surface area to volume ratios and heating rates are consequently very important for ILs that show competitive vaporization and thermal decomposition. We have explained these experimental factors in terms of Langmuir evaporation and Knudsen effusion-like conditions, allowing us to draw together observations from previous studies to make sense of the literature on IL thermal stability. Hence, the design of experimental setups are crucial and previously overlooked experimental factors.
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spelling nottingham-522252020-05-04T19:38:35Z https://eprints.nottingham.ac.uk/52225/ Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry Clarke, Coby James Puttick, Simon Sanderson, Thomas J. Taylor, Alasdair Bourne, Richard A. Lovelock, Kevin R.J. Licence, Peter Thermal decomposition (TD) products of the ionic liquids (ILs) [CnC1Im][BF4] and [CnC1Im][PF6] ([CnC1Im]+ = 1-alkyl-3-methylimidazolium, [BF4]- = tetrafluoroborate, and [PF6]- = hexafluorophosphate) were prepared, ex situ, by bulk heating experiments in a bespoke setup. The respective products, CnC1(C3N2H2)BF3 and CnC1(C3N2H2)PF5 (1-alkyl-3-methylimidazolium-2trifluoroborate and 1-alkyl-3-methylimidazolium-2-pentafluorophosphate), were then vaporized and analyzed by direct insertion mass spectrometry (DIMS) in order to identify their characteristic MS signals. During IL DIMS experiments we were subsequently able, in situ, to identify and monitor signals due to both IL vaporization and IL thermal decomposition. These decomposition products have not been observed in situ during previous analytical vaporization studies of similar ILs. The ex situ preparation of TD products is therefore perfectly complimentary to in situ thermal stability measurements. Experimental parameters such as sample surface area to volume ratios and heating rates are consequently very important for ILs that show competitive vaporization and thermal decomposition. We have explained these experimental factors in terms of Langmuir evaporation and Knudsen effusion-like conditions, allowing us to draw together observations from previous studies to make sense of the literature on IL thermal stability. Hence, the design of experimental setups are crucial and previously overlooked experimental factors. Royal Society of Chemistry 2018-06-01 Article PeerReviewed Clarke, Coby James, Puttick, Simon, Sanderson, Thomas J., Taylor, Alasdair, Bourne, Richard A., Lovelock, Kevin R.J. and Licence, Peter (2018) Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry. Physical Chemistry Chemical Physics, 20 (24). pp. 16786-16800. ISSN 1463-9084 http://pubs.rsc.org/en/content/articlelanding/2018/cp/c8cp01090k#!divAbstract doi:10.1039/C8CP01090K doi:10.1039/C8CP01090K
spellingShingle Clarke, Coby James
Puttick, Simon
Sanderson, Thomas J.
Taylor, Alasdair
Bourne, Richard A.
Lovelock, Kevin R.J.
Licence, Peter
Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title_full Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title_fullStr Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title_full_unstemmed Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title_short Thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
title_sort thermal stability of dialkylimidazolium tetrafluoroborate and hexafluorophosphate ionic liquids: ex situ bulk heating to complement in situ mass spectrometry
url https://eprints.nottingham.ac.uk/52225/
https://eprints.nottingham.ac.uk/52225/
https://eprints.nottingham.ac.uk/52225/