NMR cryoporometric measurements of porous silica: A method for the determination of melting point depression parameters of probe liquids

Taylor J. Rottreau, Christopher M.a. Parlett, Adam F. Lee, Robert D Evans

Research output: Contribution to journalArticle

Abstract

Nuclear magnetic resonance (NMR) cryoporometry is a non-invasive method for determining the pore size distributions of materials such as porous silica. Cryoporometry has several advantages over other porometric techniques. It is able to measure the melting process in a series of discrete steps, whereas transient heat flow techniques, such as differential scanning calorimetry (DSC), have a minimum rate of measurement, and, secondly, NMR cryoporometry can analyze pore shapes with any geometry, where nitrogen porosimetry is complicated for samples with spherical pores with narrow necks. However, one key drawback of the method is that, for any one liquid observed in any one material, there is a lack of consensus in the two parameters, kckc andView the MathML source2sl , used to convert experimental NMR melting point depression data into a pore size distribution. By considering two decades worth of literature data, values for both were obtained for water in porous silica supports, in particular an estimate of a non-freezing layer between the solid ice and the inner surface of the pore. These values were used to produce pore size distributions for three silica materials, SBA-15 and KIT-6, both with cylindrical pores but possessing different structures, and SBA-16, which has spherical pores. This represents the first time KIT-6 has been characterized by the NMR method. Furthermore, this work demonstrates a general method for obtaining values for kckc and View the MathML source2sl which can be applied to any liquid for which suitable literature data is available.
LanguageEnglish
JournalMicroporous and Mesoporous Materials
Early online date8 Jan 2018
DOIs
Publication statusPublished - 8 Jan 2018

Fingerprint

Magnetic resonance measurement
Silicon Dioxide
melting points
Melting point
Silica
Nuclear magnetic resonance
silicon dioxide
Pore size
porosity
nuclear magnetic resonance
probes
Liquids
liquids
Ice
Differential scanning calorimetry
Melting
Nitrogen
Heat transfer
Geometry
Water

Bibliographical note

© 2018, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/

Funding: Ph.D. studentship from the School of Engineering and Applied Science, Aston University, Engineering and Physical Sciences Research Council (Grant Number EP/N009924/1).

Keywords

  • NMR cryoporometry
  • Mesoporous silica
  • NMR characterization

Cite this

@article{84f864ec988b45d38b172bdcf5ce4323,
title = "NMR cryoporometric measurements of porous silica: A method for the determination of melting point depression parameters of probe liquids",
abstract = "Nuclear magnetic resonance (NMR) cryoporometry is a non-invasive method for determining the pore size distributions of materials such as porous silica. Cryoporometry has several advantages over other porometric techniques. It is able to measure the melting process in a series of discrete steps, whereas transient heat flow techniques, such as differential scanning calorimetry (DSC), have a minimum rate of measurement, and, secondly, NMR cryoporometry can analyze pore shapes with any geometry, where nitrogen porosimetry is complicated for samples with spherical pores with narrow necks. However, one key drawback of the method is that, for any one liquid observed in any one material, there is a lack of consensus in the two parameters, kckc andView the MathML source2sl , used to convert experimental NMR melting point depression data into a pore size distribution. By considering two decades worth of literature data, values for both were obtained for water in porous silica supports, in particular an estimate of a non-freezing layer between the solid ice and the inner surface of the pore. These values were used to produce pore size distributions for three silica materials, SBA-15 and KIT-6, both with cylindrical pores but possessing different structures, and SBA-16, which has spherical pores. This represents the first time KIT-6 has been characterized by the NMR method. Furthermore, this work demonstrates a general method for obtaining values for kckc and View the MathML source2sl which can be applied to any liquid for which suitable literature data is available.",
keywords = "NMR cryoporometry, Mesoporous silica, NMR characterization",
author = "Rottreau, {Taylor J.} and Parlett, {Christopher M.a.} and Lee, {Adam F.} and Evans, {Robert D}",
note = "{\circledC} 2018, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ Funding: Ph.D. studentship from the School of Engineering and Applied Science, Aston University, Engineering and Physical Sciences Research Council (Grant Number EP/N009924/1).",
year = "2018",
month = "1",
day = "8",
doi = "10.1016/j.micromeso.2018.01.004",
language = "English",
journal = "Microporous and Mesoporous Materials",
issn = "1387-1811",
publisher = "Elsevier",

}

TY - JOUR

T1 - NMR cryoporometric measurements of porous silica

T2 - Microporous and Mesoporous Materials

AU - Rottreau, Taylor J.

AU - Parlett, Christopher M.a.

AU - Lee, Adam F.

AU - Evans, Robert D

N1 - © 2018, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ Funding: Ph.D. studentship from the School of Engineering and Applied Science, Aston University, Engineering and Physical Sciences Research Council (Grant Number EP/N009924/1).

PY - 2018/1/8

Y1 - 2018/1/8

N2 - Nuclear magnetic resonance (NMR) cryoporometry is a non-invasive method for determining the pore size distributions of materials such as porous silica. Cryoporometry has several advantages over other porometric techniques. It is able to measure the melting process in a series of discrete steps, whereas transient heat flow techniques, such as differential scanning calorimetry (DSC), have a minimum rate of measurement, and, secondly, NMR cryoporometry can analyze pore shapes with any geometry, where nitrogen porosimetry is complicated for samples with spherical pores with narrow necks. However, one key drawback of the method is that, for any one liquid observed in any one material, there is a lack of consensus in the two parameters, kckc andView the MathML source2sl , used to convert experimental NMR melting point depression data into a pore size distribution. By considering two decades worth of literature data, values for both were obtained for water in porous silica supports, in particular an estimate of a non-freezing layer between the solid ice and the inner surface of the pore. These values were used to produce pore size distributions for three silica materials, SBA-15 and KIT-6, both with cylindrical pores but possessing different structures, and SBA-16, which has spherical pores. This represents the first time KIT-6 has been characterized by the NMR method. Furthermore, this work demonstrates a general method for obtaining values for kckc and View the MathML source2sl which can be applied to any liquid for which suitable literature data is available.

AB - Nuclear magnetic resonance (NMR) cryoporometry is a non-invasive method for determining the pore size distributions of materials such as porous silica. Cryoporometry has several advantages over other porometric techniques. It is able to measure the melting process in a series of discrete steps, whereas transient heat flow techniques, such as differential scanning calorimetry (DSC), have a minimum rate of measurement, and, secondly, NMR cryoporometry can analyze pore shapes with any geometry, where nitrogen porosimetry is complicated for samples with spherical pores with narrow necks. However, one key drawback of the method is that, for any one liquid observed in any one material, there is a lack of consensus in the two parameters, kckc andView the MathML source2sl , used to convert experimental NMR melting point depression data into a pore size distribution. By considering two decades worth of literature data, values for both were obtained for water in porous silica supports, in particular an estimate of a non-freezing layer between the solid ice and the inner surface of the pore. These values were used to produce pore size distributions for three silica materials, SBA-15 and KIT-6, both with cylindrical pores but possessing different structures, and SBA-16, which has spherical pores. This represents the first time KIT-6 has been characterized by the NMR method. Furthermore, this work demonstrates a general method for obtaining values for kckc and View the MathML source2sl which can be applied to any liquid for which suitable literature data is available.

KW - NMR cryoporometry

KW - Mesoporous silica

KW - NMR characterization

UR - http://doi.org/10.17036/researchdata.aston.ac.uk.00000326

UR - https://www.scopus.com/record/display.uri?eid=2-s2.0-85041383966&origin=SingleRecordEmailAlert&dgcid=raven_sc_search_en_us_email&txGid=4f200267f8466a025246170548c1e540

U2 - 10.1016/j.micromeso.2018.01.004

DO - 10.1016/j.micromeso.2018.01.004

M3 - Article

JO - Microporous and Mesoporous Materials

JF - Microporous and Mesoporous Materials

SN - 1387-1811

ER -