Measuring the pore size and pore-size distributions and exploring the fluid-exchange dynamics between different types of pores in porous materials remains a significant experimental challenge but is critical to understanding catalysis, chromatography, nutrient cycling, and a whole range of geochemical phenomena, including shale gas and tight gas extraction. Here, we present the results of 1D 13C NMR and 2D exchange spectroscopy (EXSY) NMR investigations of a porous silica using supercritical methane (scCH4) as a direct probe of pore size and fluid exchange between pore types. The results show that the 13C chemical shift of scCH4 adsorbed in nanometer-scale silica pores becomes more negative with increasing pore diameter, in agreement with trends reported for gas hydrates, zeolites, MOFs, and clays and other microporous (
Revised: August 26, 2020 |
Published: May 28, 2020
Citation
Bowers G.M., E.D. Walter, S.D. Burton, K.C. Schwarz, D.W. Hoyt, and R.J. Kirkpatrick. 2020.Probing Pore Size and Connectivity in Porous Silicas Using 13C MAS NMR Spectroscopy of Supercritical Methane.Journal of Physical Chemistry C 124, no. 21:11536–11543.PNNL-SA-153506.doi:10.1021/acs.jpcc.0c02718