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Temperature calibration of a high‐resolution magic‐angle spinning NMR probe for analysis of tissue samples
Author(s) -
Nicholls Andrew W.,
MortishireSmith Russell J.
Publication year - 2001
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.924
Subject(s) - chemistry , magic angle spinning , thermometer , analytical chemistry (journal) , spinning , calibration , magic angle , nuclear magnetic resonance spectroscopy , high resolution , chromatography , thermodynamics , stereochemistry , physics , remote sensing , polymer chemistry , geology , statistics , mathematics
The increase in tissue sample temperature caused by the spinning of a rotor in high‐resolution magic‐angle spinning (HRMAS) NMR spectroscopy was investigated using two literature NMR thermometers. The classical methanol thermometer was used to calibrate the temperature difference between the set temperature and the actual sample temperature. At spin speeds of 2, 4, 6 and 8 kHz, a mean increase in sample temperature over the set temperature of 0.8 ± 0.1, 2.2 ± 0.1, 5.0 ± 0.1 and 7.9 ± 0.2 K, respectively, was noted. This calibration was used to gauge the accuracy of the literature glucose thermometer, which was shown to have a mean increase over the set temperature of −0.3 ± 0.1, 1.2 ± 0.2, 3.0 ± 0.2 and 6.1 ±0.1 K at 2, 4, 6 and 8 kHz, respectively. By correcting for the errors measured in this study, a more accurate determination and adjustment of sample temperature in HRMAS NMR spectroscopic analyses of intact tissues is now possible. Copyright © 2001 John Wiley & Sons, Ltd.