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

Rottreau, Taylor J., Parlett, Christopher M.a., Lee, Adam F. and Evans, Robert D (2018). NMR cryoporometric measurements of porous silica:A method for the determination of melting point depression parameters of probe liquids. Microporous and Mesoporous Materials ,

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.

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: Engineering & Applied Sciences > Chemical engineering & applied chemistry
Engineering & Applied Sciences
Engineering & Applied Sciences > Polymer and advanced materials research group
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
Full Text Link: http://linkingh ... 387181118300040
Related URLs: https://www.sco ... 246170548c1e540 (Scopus URL)
Published Date: 2018-01-08
Authors: Rottreau, Taylor J.
Parlett, Christopher M.a. ( 0000-0002-3651-7314)
Lee, Adam F. ( 0000-0002-2153-1391)
Evans, Robert D ( 0000-0003-1471-201X)

Export / Share Citation


Statistics

Additional statistics for this record