Issue 3, 1991

6Li magic angle spinning nuclear magnetic resonance spectroscopy: a powerful probe for the study of lithium-containing materials

Abstract

A narrow chemical-shift range has been established for a variety of lithium compounds via study of their 6Li magic angle spinning nuclear magnetic resonance (MAS NMR) spectra. Comparative studies of 6Li and 7Li spectra (MAS, and ‘off-angle’ spinning) establish that, for solid-state (and even solution) analytical purposes, 6Li is the preferred nucles, since the advantage of narrow absorption lines outweighs the poorer sensitivity of 6Li relative to 7Li.

6 Li MAS NMR spectra have been obtained for laponite clay, which had been thermally treated at 200, 400, 600, 800 and 1300 °C; at the lower temperatures (<800 °C) both dehydrated and rehydrated specimens were considered. The data are consistent with mobility of lithium ions from the trioctahedral clay sites at 600 °C.

Both conventional and microwave methods were used to prepare lithium-exchanged laponite. The superior resolution achievable in 6Li MAS NMR in comparison with 7Li MAS NMR is demonstrated with the microwave specimen where use of 6Li spectroscopy revealed two lithium sites. On storage of the sample for 3 months, the two sites give way to a single lithium environment. Possible causes are discussed.

Article information

Article type
Paper

J. Mater. Chem., 1991,1, 327-330

6 Li magic angle spinning nuclear magnetic resonance spectroscopy: a powerful probe for the study of lithium-containing materials

S. P. Bond, A. Gelder, J. Homer, W. R. McWhinnie and M. C. Perry, J. Mater. Chem., 1991, 1, 327 DOI: 10.1039/JM9910100327

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