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


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.

Publication DOI: https://doi.org/10.1016/j.micromeso.2018.01.004
Dataset DOI: https://doi.org/10.17036/researchdata.aston.ac.uk.00000326
Divisions: College of Engineering & Physical Sciences > School of Infrastructure and Sustainable Engineering > Chemical Engineering & Applied Chemistry
College of Engineering & Physical Sciences
College of Engineering & Physical Sciences > Aston Institute of Materials Research (AIMR)
Additional Information: © 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).
Uncontrolled Keywords: NMR cryoporometry,Mesoporous silica,NMR characterization
Publication ISSN: 1387-1811
Last Modified: 17 Jun 2024 07:29
Date Deposited: 09 Jan 2018 12:00
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Related URLs: https://www.sco ... 246170548c1e540 (Scopus URL)
http://linkingh ... 387181118300040 (Publisher URL)
PURE Output Type: Article
Published Date: 2018-01-08
Published Online Date: 2018-01-08
Accepted Date: 2018-01-03
Authors: Rottreau, Taylor J.
Parlett, Christopher M.a. (ORCID Profile 0000-0002-3651-7314)
Lee, Adam F.
Evans, Robert D (ORCID Profile 0000-0003-1471-201X)

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