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

Research output: Contribution to journalArticle

View graph of relations Save citation

Authors

Research units

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.

Request a copy

Request a copy

Christopher Parlett

Person: Research

Documents

  • NMR cryoporometric measurements of porous silica

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

    Accepted author manuscript, 1 MB, PDF-document

    Embargo ends: 8/01/19

    License: CC BY-NC-ND Show license

Details

Original languageEnglish
JournalMicroporous and Mesoporous Materials
Early online date8 Jan 2018
DOIs
StatePublished - 8 Jan 2018

Bibliographic 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

DOI

Employable Graduates; Exploitable Research

Copy the text from this field...