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Simple technique for temperature calibration of a MAS probe for solid-state NMR spectroscopy

✍ Scribed by Abil E. Aliev; Kenneth D. M. Harris

Publisher
John Wiley and Sons
Year
1994
Tongue
English
Weight
373 KB
Volume
32
Category
Article
ISSN
0749-1581

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✦ Synopsis

Abstract

A simple method is reported for temperature calibration of a magic angle spinning probe for solid‐state NMR spectroscopy. The method is an extension of that developed by van Geet for temperature calibration of liquid‐state NMR probes, and consists of measuring the frequency difference (Δν) between the resonances for the methyl and hydroxyl protons of methanol in the ^1^H NMR spectrum of a sample of tetrakis(trimethylsilyl)silane soaked in liquid methanol. The successful application of this method for temperature calibration was demonstrated from an assessment, from high‐resolution solid‐state ^13^C NMR spectroscopy, of the phase transition temperatures for solid tetrakis(trimethylsilyl)silane and for solid 2,2‐dimethylpropane‐1,3‐diol.

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