Cited by 201Advanced NMR Techniques and ApplicationsMineralogy and Gemology StudiesNMR spectroscopy and applications

Characterization of hydrous species in minerals by high-speed proton MAS-NMR

Yesinowski, James P., Eckert, Hellmut., Rossman, George R.·1988·Journal of the American Chemical Society

Abstract

Proton magic-angle spinning (MAS) NMR at 200 and 500 MHz and at high spinning speeds (ca. 8 kHz) has been used to characterize hydrous species, both stoichiometric and nonstoichiometric, in a variety of minerals. High-resolution \n^1H MAS-NMR spectra of minerals containing stoichiometric hydroxyl groups as the only hydrous species are obtainable provided that the hydrogen density in the sample is less than about 15 atoms/nm^3. Structurally isolated water molecules in analcite, NaAlSi_2O_6•H_2O, and gypsum, CaSO_4•2H_2O, yield characteristic ^1H MAS-NMR spectra with numerous spinning sidebands extending over a range of about 100 kHz, reflecting the strong, largely inhomogeneous character of the homonuclear dipolar coupling. The field dependence of both line widths and spinning sideband patterns provides evidence about the nature of the \nbroadening interactions. Lawsonite and hemimorphite, minerals containing stoichiometric amounts of both OH and H_2O groups, yield spectra with numerous intense spinning sidebands; strong dipolar interactions preclude discrimination of OH and H_2O. \nNonstoichiometric hydrogen in nominally anhydrous minerals (feldspars, nepheline, quartz, and grossular garnet) is found to occur in a variety of forms: mobile H_2O in fluid inclusions, anisotropically constrained, isolated H_2O molecules, and clustered species consistent with H_4O_4^(4-) groups in a hydrogarnet substitution.

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Crossref · 10.1021/ja00213a007

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Authors
Yesinowski, J. P., Eckert, H., & Rossman, G. R.
Venue
Journal of the American Chemical Society
Published
1988-03
Volume
110
Issue
5
Pages
1367-1375
ISSN
  • 0002-7863 (ISSN-L)
  • 1520-5126
OpenAlex
W2026899018
Cited by
200
References
0
Citations by year
2025: 2 · 2024: 3 · 2023: 5 · 2022: 5 · 2021: 5 · 2020: 6 · 2019: 7 · 2018: 4 · 2017: 7 · 2016: 2 · 2015: 12 · 2014: 8 · 2013: 7 · 2012: 5
FWCI
4.09
Type
journal article
Language
en
Open access
closed
Locations
  • Journal of the American Chemical Society (publishedVersion)
  • CaltechAUTHORS (California Institute of Technology) (submittedVersion)
Topics
  • Physical Sciences › Chemistry › Spectroscopy › Advanced NMR Techniques and Applications
  • Physical Sciences › Earth and Planetary Sciences › Geochemistry and Petrology › Mineralogy and Gemology Studies
  • Physical Sciences › Physics and Astronomy › Nuclear and High Energy Physics › NMR spectroscopy and applications
Keywords
hydrous minerals, hydroxyl groups, water molecules, analcime, gypsum, lawsonite, hemimorphite, fluid inclusions, hydrogarnet, feldspar, nepheline, grossular garnet, spinning sidebands, dipolar coupling, hydrogen density

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