Temperature calibration under ultrafast MAS conditions

被引:114
作者
Langer, B
Schnell, L
Spiess, HW
Grimmer, AR
机构
[1] Max Planck Inst Polymer Res, D-55021 Mainz, Germany
[2] Humboldt Univ, D-12484 Berlin, Germany
关键词
solid-state Sn-119 NMR; magic-angle spinning; temperature dependence; Joule-Thomson effect; frictional heating; temperature calibration;
D O I
10.1006/jmre.1999.1717
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
For conventional fast magic-angle spinning (MAS) frequencies (less than or equal to 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 Sn-119 NMR signal of the chemical shift thermometer Sm2Sn2O7, 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. (C) 1999 Academic Press.
引用
收藏
页码:182 / 186
页数:5
相关论文
共 15 条
[1]   The effect of RF power and spinning speed on MQMAS NMR [J].
Amoureux, JP ;
Pruski, M ;
Lang, DP ;
Fernandez, C .
JOURNAL OF MAGNETIC RESONANCE, 1998, 131 (01) :170-175
[2]  
ENGELKE F, 1998, 145 BRUK
[3]  
Friedrich U, 1998, MOL PHYS, V95, P1209, DOI 10.1080/00268979809483252
[4]   TEMPERATURE-DEPENDENT SOLID-STATE SN-119 MAS NMR OF ND2SN2O7, SM2SN2O7, AND Y1.8SM0.2SN2O7 - 3 SENSITIVE CHEMICAL-SHIFT THERMOMETERS [J].
GREY, CP ;
CHEETHAM, AK ;
DOBSON, CM .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1993, 101 (03) :299-306
[5]  
Grimmer AR, 1997, MAGN RESON CHEM, V35, P86, DOI 10.1002/(SICI)1097-458X(199702)35:2<86::AID-OMR34>3.3.CO
[6]  
2-U
[7]   High-resolution variable-temperature MAS F-19 NMR spectroscopy of fluorocarbon polymers [J].
Isbester, PK ;
Kestner, TA ;
Munson, EJ .
MACROMOLECULES, 1997, 30 (09) :2800-2801
[8]   On the origin of spinning sidebands in MQMAS NMR experiments [J].
Marinelli, L ;
Frydman, L .
CHEMICAL PHYSICS LETTERS, 1997, 275 (3-4) :188-198
[9]  
SCHELER U, 1998, P 29 AMP 13 ISMAR C, V2, P723
[10]   An investigation of hydrogen bonding in benzoxazine dimers by fast magic-angle spinning and double-quantum 1H NMR spectroscopy [J].
Schnell, I ;
Brown, SP ;
Low, HY ;
Ishida, H ;
Spiess, HW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (45) :11784-11795