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Probing hysteresis during sorption of cyclohexane within mesoporous silica using NMR cryoporometry and relaxometry

Shiko, Elenica ; Edler, Karen J. LU orcid ; Lowe, John P. and Rigby, Sean P. (2013) In Journal of Colloid and Interface Science 398. p.168-175
Abstract

The conventional data analysis methods for obtaining a pore size distribution (PSD) from gas sorption data make several critical assumptions that impact significantly on the accuracy of the PSD thereby obtained. In particular, assumptions must be made concerning the nature of the pore-filling or emptying process in adsorption, or desorption, respectively. The possibility of pore-pore interactions is also generally neglected. In this work, NMR cryoporometry and relaxometry have been used to study the adsorption and desorption of cyclohexane within a mesoporous, sol-gel silica catalyst support pellet with the aim of assessing the impact of the aforementioned problems for gas sorption PSDs and developing solutions. The advanced melting... (More)

The conventional data analysis methods for obtaining a pore size distribution (PSD) from gas sorption data make several critical assumptions that impact significantly on the accuracy of the PSD thereby obtained. In particular, assumptions must be made concerning the nature of the pore-filling or emptying process in adsorption, or desorption, respectively. The possibility of pore-pore interactions is also generally neglected. In this work, NMR cryoporometry and relaxometry have been used to study the adsorption and desorption of cyclohexane within a mesoporous, sol-gel silica catalyst support pellet with the aim of assessing the impact of the aforementioned problems for gas sorption PSDs and developing solutions. The advanced melting effect makes cryoporometry a particularly sensitive probe of adsorbate ganglia spatial distribution. It has been demonstrated that utilising gas sorption scanning curves provided insufficient additional information to alleviate the aforementioned problems with interpreting gas sorption data. The NMR data has shown how the nature of the sorption hysteresis changed with amount adsorbed, due to detectable variations in the mechanisms of pore-filling and emptying along the isotherm. Hence, relating a particular condensation or evaporation pressure to a specific characteristic pore size is not as straightforward as assumed in typical pore size analysis software. However, the NMR techniques reveal the additional information required to improve pore size estimates from gas sorption for disordered solids.

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author
; ; and
publishing date
type
Contribution to journal
publication status
published
keywords
Adsorption, Catalyst support, NMR cryoporometry, Phase change, Porous media
in
Journal of Colloid and Interface Science
volume
398
pages
8 pages
publisher
Elsevier
external identifiers
  • scopus:84876479167
  • pmid:23489607
ISSN
0021-9797
DOI
10.1016/j.jcis.2013.02.002
language
English
LU publication?
no
id
ccbb7393-4bc6-401e-96f5-7c0c3cff5cbf
date added to LUP
2023-05-04 18:04:34
date last changed
2024-01-05 01:07:11
@article{ccbb7393-4bc6-401e-96f5-7c0c3cff5cbf,
  abstract     = {{<p>The conventional data analysis methods for obtaining a pore size distribution (PSD) from gas sorption data make several critical assumptions that impact significantly on the accuracy of the PSD thereby obtained. In particular, assumptions must be made concerning the nature of the pore-filling or emptying process in adsorption, or desorption, respectively. The possibility of pore-pore interactions is also generally neglected. In this work, NMR cryoporometry and relaxometry have been used to study the adsorption and desorption of cyclohexane within a mesoporous, sol-gel silica catalyst support pellet with the aim of assessing the impact of the aforementioned problems for gas sorption PSDs and developing solutions. The advanced melting effect makes cryoporometry a particularly sensitive probe of adsorbate ganglia spatial distribution. It has been demonstrated that utilising gas sorption scanning curves provided insufficient additional information to alleviate the aforementioned problems with interpreting gas sorption data. The NMR data has shown how the nature of the sorption hysteresis changed with amount adsorbed, due to detectable variations in the mechanisms of pore-filling and emptying along the isotherm. Hence, relating a particular condensation or evaporation pressure to a specific characteristic pore size is not as straightforward as assumed in typical pore size analysis software. However, the NMR techniques reveal the additional information required to improve pore size estimates from gas sorption for disordered solids.</p>}},
  author       = {{Shiko, Elenica and Edler, Karen J. and Lowe, John P. and Rigby, Sean P.}},
  issn         = {{0021-9797}},
  keywords     = {{Adsorption; Catalyst support; NMR cryoporometry; Phase change; Porous media}},
  language     = {{eng}},
  month        = {{05}},
  pages        = {{168--175}},
  publisher    = {{Elsevier}},
  series       = {{Journal of Colloid and Interface Science}},
  title        = {{Probing hysteresis during sorption of cyclohexane within mesoporous silica using NMR cryoporometry and relaxometry}},
  url          = {{http://dx.doi.org/10.1016/j.jcis.2013.02.002}},
  doi          = {{10.1016/j.jcis.2013.02.002}},
  volume       = {{398}},
  year         = {{2013}},
}