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Title: Variable-temperature magic-angle-spinning technique for studies of mobile species in solid state NMR

Abstract

We demonstrate the utility of variable-temperature (VT) magic-angle-spinning (MAS) Fourier transform nuclear magnetic resonance (FT-NMR) spectroscopy for the study of mobile species in solids, especially when quadrupolar nuclei are being observed. A new VT-MAS probe is described for use in the temperature range 150 - 400 K, using spectrometers with high-field superconducting magnets. It has been utilized in studies of the bonding and dynamics of alkali cations in hydrated zeolites at an applied field of 7.05 T. Results are presented for the cases of Cs/Na-A and Cs/Li-A zeolites, in which the Cs/sup +/ ions exchange rapidly, at 293 K, between six-ring and eight-ring sites in the large cage, so that on the time scale of the NMR measurements the ions are indistinguishable and a single /sup 133/Cs resonance is observed. Below 250 K, two well-resolved signals are observed in the Cs/Na-zeolite, 107 ppM apart. These are easily assigned to the Cs/sup +/ ions in the two sites, the large difference in chemical shifts being attributed to the stronger bonding of Cs/sup +/ ions at the six-ring sites. Three sites are distinguished in the Cs/Li-A zeolite, the third site being assigned to a position near to a four-ring in the largemore » cage. 26 refs., 3 figs., 1 tab.« less

Authors:
; ; ;
Publication Date:
Research Org.:
Argonne National Lab., IL (USA)
OSTI Identifier:
6417413
Report Number(s):
ANL/PPRNT-89-161
ON: DE89008346
DOE Contract Number:  
W-31109-ENG-38
Resource Type:
Technical Report
Resource Relation:
Other Information: Portions of this document are illegible in microfiche products
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CESIUM IONS; MOBILITY; LITHIUM IONS; NMR SPECTROMETERS; SODIUM IONS; BONDING; CATIONS; CHEMICAL SHIFT; ION EXCHANGE; MEDIUM TEMPERATURE; PROBES; ZEOLITES; CHARGED PARTICLES; FABRICATION; INORGANIC ION EXCHANGERS; ION EXCHANGE MATERIALS; IONS; JOINING; MATERIALS; MEASURING INSTRUMENTS; MINERALS; SPECTROMETERS; 400102* - Chemical & Spectral Procedures

Citation Formats

Tokuhiro, Tadashi, Mattingly, M, Iton, L E, and Ahn, M K. Variable-temperature magic-angle-spinning technique for studies of mobile species in solid state NMR. United States: N. p., 1987. Web.
Tokuhiro, Tadashi, Mattingly, M, Iton, L E, & Ahn, M K. Variable-temperature magic-angle-spinning technique for studies of mobile species in solid state NMR. United States.
Tokuhiro, Tadashi, Mattingly, M, Iton, L E, and Ahn, M K. 1987. "Variable-temperature magic-angle-spinning technique for studies of mobile species in solid state NMR". United States.
@article{osti_6417413,
title = {Variable-temperature magic-angle-spinning technique for studies of mobile species in solid state NMR},
author = {Tokuhiro, Tadashi and Mattingly, M and Iton, L E and Ahn, M K},
abstractNote = {We demonstrate the utility of variable-temperature (VT) magic-angle-spinning (MAS) Fourier transform nuclear magnetic resonance (FT-NMR) spectroscopy for the study of mobile species in solids, especially when quadrupolar nuclei are being observed. A new VT-MAS probe is described for use in the temperature range 150 - 400 K, using spectrometers with high-field superconducting magnets. It has been utilized in studies of the bonding and dynamics of alkali cations in hydrated zeolites at an applied field of 7.05 T. Results are presented for the cases of Cs/Na-A and Cs/Li-A zeolites, in which the Cs/sup +/ ions exchange rapidly, at 293 K, between six-ring and eight-ring sites in the large cage, so that on the time scale of the NMR measurements the ions are indistinguishable and a single /sup 133/Cs resonance is observed. Below 250 K, two well-resolved signals are observed in the Cs/Na-zeolite, 107 ppM apart. These are easily assigned to the Cs/sup +/ ions in the two sites, the large difference in chemical shifts being attributed to the stronger bonding of Cs/sup +/ ions at the six-ring sites. Three sites are distinguished in the Cs/Li-A zeolite, the third site being assigned to a position near to a four-ring in the large cage. 26 refs., 3 figs., 1 tab.},
doi = {},
url = {https://www.osti.gov/biblio/6417413}, journal = {},
number = ,
volume = ,
place = {United States},
year = {Fri May 01 00:00:00 EDT 1987},
month = {Fri May 01 00:00:00 EDT 1987}
}

Technical Report:
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