Journal
JOURNAL OF MAGNETIC RESONANCE
Volume 167, Issue 2, Pages 328-333Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2004.01.006
Keywords
convection; diffusion; ion-ion and ion-solvent interactions; low viscosity liquid; NMR tube; PGSE-NMR
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Pulsed gradient spin-echo (PGSE) NMR measurements of the self-diffusion coefficients of low viscosity liquids are greatly hampered by the effects of convection especially away from ambient temperature. Here we report on a new NMR tube designed to minimize the deleterious effects of convection. In this tube, which derives from a Shigemi symmetrical NMR tube, the sample is contained in an annulus formed from a concentric cylinder of susceptibility matched glass. The performance of this tube was demonstrated by conducting measurements on the electrochemically important LiN(So(3)CF(3))(2) (LiTFSI)-diglyme (DG) system. Calibrations were first made using DG at column heights of 2, 3, and 4-mm in the temperature range between -40 and 100degreesC. Measurements of the diffusion coefficients of the lithium, anion, and DG were then performed to probe the solvent-ion and ion-ion interactions in the DG doped with LiTFSI. Changes in the H-1, Li-7, and F-19 PGSE-NMR attenuation curves at -40degreesC provided clear evidence of interactions between the DG and lithium ion. (C) 2004 Elsevier Inc. All rights reserved.
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