33S solid state NMR of sulphur speciation in silicate glasses

Solid State Nuclear Magnetic Resonance
S CouchM E Smith

Abstract

33S solid-state NMR is reported from some model crystalline sulphides, sulphates, sulphites and thiosulphates. This is the first report of (33)S NMR signals of the latter two species from a solid. Good quality spectra, which have distinct, well separated shift ranges can be identified for all these groupings, except for sulphites and hydrogen sulphites whose resonances are very broad. Nonetheless the presence of sulphites and hydrogen sulphites can be confirmed from their characteristic sharp, intense time domain echoes. (33)S MAS NMR is also applied to a range of dry and hydrous silicate glasses with approximately 1wt% 99at% (33)S-enriched sulphur. It is clear that in all these glasses sulphate is present, and in mixed cation systems there is some evidence of preferential association of sulphate with a specific cation. In a dry potassium silicate glass sample two resolved (33)S resonances are observed, a sulphate, and the second from thiosulphate. Hence solid state (33)S NMR is shown to be a feasible probe that can be applied to this problem that can readily distinguish different sulphur species.

Citations

Sep 25, 2010·Journal of Magnetic Resonance·Luke A O'Dell, Igor L Moudrakovski
Jul 8, 2010·Solid State Nuclear Magnetic Resonance·J V Hanna, M E Smith
Dec 23, 2008·Chemical Communications : Chem Comm·Andre SutrisnoYining Huang
Mar 23, 2018·Materials·Randall Youngman
Aug 25, 2017·Physical Chemistry Chemical Physics : PCCP·Akiko SasakiStephen Wimperis
Aug 5, 2009·Physical Chemistry Chemical Physics : PCCP·Sharon E Ashbrook
Jun 14, 2017·Philosophical Transactions. Series A, Mathematical, Physical, and Engineering Sciences·Reiner Kirchheim
Aug 5, 2009·Physical Chemistry Chemical Physics : PCCP·Hans J JakobsenWolfgang Bensch
Jan 9, 2010·The Journal of Physical Chemistry. a·Igor MoudrakovskiJohn Ripmeester
Dec 23, 2010·The Journal of Physical Chemistry. a·Luke A O'Dell, Christopher I Ratcliffe
Jun 15, 2006·Analytical Chemistry·Cecil Dybowski, Shi Bai

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