Temperature Calibration under Ultrafast MAS Conditions
✍ Scribed by Benedikt Langer; Ingo Schnell; Hans Wolfgang Spiess; Arnd-Rüdiger Grimmer
- Publisher
- Elsevier Science
- Year
- 1999
- Tongue
- English
- Weight
- 71 KB
- Volume
- 138
- Category
- Article
- ISSN
- 1090-7807
No coin nor oath required. For personal study only.
✦ Synopsis
For conventional fast magic-angle spinning (MAS) frequencies (<15 kHz), there is a known heating of the sample due to the friction between the rotor and the bearing gas. At the recently achievable ultrafast MAS frequencies of up to 35 kHz, a more dramatic heating effect is expected. Using the 119 Sn NMR signal of the chemical shift thermometer Sm 2 Sn 2 O 7 , this frictional heating effect is quantified, and a calibration of the sample temperature under ultrafast MAS conditions is described. An empirical expression is given which allows the determination of the sample temperature as a function of the bearing gas temperature and the spinning frequency.
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## 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 (
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Novel procedures for the spectral assignment of peaks in highresolution solid-state 13 C NMR are discussed and demonstrated. These methods are based on the observation that at moderate and already widely available rates of magic-angle spinning (10 -14 kHz MAS), CH and CH 2 moieties behave to a large