Measurement of Temperature in 13C CP/MAS NMR
✍ Scribed by Frank G. Riddell; Roger A. Spark; Gabor V. Günther
- Publisher
- John Wiley and Sons
- Year
- 1996
- Tongue
- English
- Weight
- 410 KB
- Volume
- 34
- Category
- Article
- ISSN
- 0749-1581
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✦ Synopsis
A method for temperature calibration of CP/MAS NMR probes and their temperature controllers is described that relies upon known phase changes in the compounds adamantane, d-camphor, pivalic acid and DABCO. The method appears to give a convenient and reliable calibration over the temperature range cu. 173-373 K. In a separate experiment, making use of a well defined lineshape coalescence, it was shown that the temperature effect of spinning in a 4 mm Bruker MAS probe with zirconia rotors could be fitted by a squared relationship but that if treated as approximately linear the variation was cu.
📜 SIMILAR VOLUMES
Solid-state 13C CP/MAS NMR spectra are reported for di †erent EDTA-metal complexes. The e †ect of metal binding on the isotropic 13C chemical shift and principal elements of the carboxyl 13C chemical shift anisotropy (CSA) tensor are discussed.