Measurement of temperature in C-13 CP/MAS NMR

被引：0

作者：

Riddell, FG ^{[1
]}

Spark, RA ^{[1
]}

Gunther, GV ^{[1
]}

机构：

[1] ALBERT SZENT GYORGYI MED UNIV,INST PHARMACEUT CHEM,H-6701 SZEGED,HUNGARY

来源：

MAGNETIC RESONANCE IN CHEMISTRY | 1996年 / 34卷 / 10期

关键词：

temperature measurement; C-13 CP/MAS NMR;

D O I：

暂无

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

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 ca. 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 ca. 1 K kHz(-1)

引用

页码：824 / 828

页数：5

共 35 条

[1] TEMPERATURE-GRADIENTS AND SAMPLE HEATING IN VARIABLE TEMPERATURE HIGH-SPEED MAS NMR-SPECTROSCOPY [J].

AGUILARPARRILLA, F ;

WEHRLE, B ;

BRAUNLING, H ;

LIMBACH, HH .

JOURNAL OF MAGNETIC RESONANCE, 1990, 87 (03) :592-597

[2] SIMPLE TECHNIQUE FOR TEMPERATURE CALIBRATION OF A MAS PROBE FOR SOLID-STATE NMR-SPECTROSCOPY [J].

ALIEV, AE ;

HARRIS, KDM .

MAGNETIC RESONANCE IN CHEMISTRY, 1994, 32 (06) :366-369

[3] A SOLID-STATE N-15 NMR-STUDY OF THE PHASE-TRANSITIONS IN AMMONIUM-NITRATE [J].

ANDERSONALTMANN, KL ;

GRANT, DM .

JOURNAL OF PHYSICAL CHEMISTRY, 1993, 97 (42) :11096-11102

[4]

ANSCHUTZ R, 1925, LIEBIGS ANN CHEM, V442, P18

[5] A DYNAMIC NMR-STUDY OF STERICALLY HINDERED TRIALKYLMETHANOLS IN THE SOLID-PHASE [J].

BARRIE, PJ ;

ANDERSON, JE .

JOURNAL OF THE CHEMICAL SOCIETY-PERKIN TRANSACTIONS 2, 1992, (11) :2031-2034

[6] P-31 MAS NMR OF P4S3 - CRYSTALLINE-TO-PLASTIC PHASE-TRANSITION INDUCED BY MAS IN A DOUBLE AIR-BEARING STATOR [J].

BJORHOLM, T ;

JAKOBSEN, HJ .

JOURNAL OF MAGNETIC RESONANCE, 1989, 84 (01) :204-211

[7] C-13 CHEMICAL-SHIFTS WHICH OBEY THE CURIE LAW IN CP MAS NMR-SPECTRA - THE 1ST CP MAS NMR CHEMICAL-SHIFT THERMOMETER [J].

CAMPBELL, GC ;

CROSBY, RC ;

HAW, JF .

JOURNAL OF MAGNETIC RESONANCE, 1986, 69 (01) :191-195

[8]

CAMPBELL GC, 1986, ANAL CHEM, V58, P3127

[9] NMR-STUDY OF THE SOLID-STATE REARRANGEMENT OF 3-AMINO-1 AND 2-(CHLOROACETYL)PYRAZOLE TO 3-(CHLOROACETAMIDO)PYRAZOLE [J].

CLARKE, D ;

MARES, RW ;

MCNAB, H ;

RIDDELL, FG .

MAGNETIC RESONANCE IN CHEMISTRY, 1994, 32 (04) :255-257

[10] DESIGN OF HIGH-SPEED CYLINDRICAL NMR SAMPLE SPINNERS [J].

DOTY, FD ;

ELLIS, PD .

REVIEW OF SCIENTIFIC INSTRUMENTS, 1981, 52 (12) :1868-1875

← 1 2 3 4 →