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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.


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