THE 2D QUADSHIFT EXPERIMENT - SEPARATION OF DEUTERIUM CHEMICAL-SHIFTS AND QUADRUPOLAR COUPLINGS BY 2-DIMENSIONAL SOLID-STATE MAS NMR-SPECTROSCOPY

被引：12

作者：

CHANDRAKUMAR, N ^{[1
]}

VONFIRCKS, G ^{[1
]}

GUNTHER, H ^{[1
]}

机构：

[1] CSIR,CENT LEATHER RES INST,CHEM PHYS LAB,MADRAS 600020,TAMIL NADU,INDIA

来源：

MAGNETIC RESONANCE IN CHEMISTRY | 1994年 / 32卷 / 07期

关键词：

NMR; H-2; SOLID-STATE MAS H-2 NMR; 2D MAS H-2 NMR; DEUTERIUM CHEMICAL SHIFT; QUADRUPOLAR COUPLING;

D O I：

10.1002/mrc.1260320710

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

The two-dimensional QUADSHIFT experiment is introduced, which permits the separation of chemical shifts and quadrupolar couplings in solid-state magic angle spinning MMR spectra of powder samples. The technique was applied to partially deuteriated norcamphor and camphor under slow magic angle spinning. Double quantum chemical shift resolutions down to 0.2 ppm were achieved, with double quantum linewidths in the range 6-12 Hz. Separation and correlation of deuterium chemical shifts and quadrupolar couplings is demonstrated for individual sites.

引用

页码：433 / 435

页数：3

共 21 条

[1] EXPERIMENTAL RESULTS ON DEUTERIUM NMR IN THE SOLID-STATE BY MAGIC ANGLE SAMPLE SPINNING [J].

ACKERMAN, JL ;

ECKMAN, R ;

PINES, A .

CHEMICAL PHYSICS, 1979, 42 (03) :423-428

[2] TWO-DIMENSIONAL ROTATIONAL SPIN-ECHO NMR IN SOLIDS - RESOLUTION OF ISOTROPIC AND ANISOTROPIC CHEMICAL-SHIFTS [J].

AUE, WP ;

RUBEN, DJ ;

GRIFFIN, RG .

JOURNAL OF MAGNETIC RESONANCE, 1981, 43 (03) :472-477

[3] COMPOSITE SEQUENCES FOR EFFICIENT DOUBLE-QUANTUM EXCITATION OVER A RANGE OF SPIN COUPLING STRENGTHS [J].

BARBARA, TM ;

TYCKO, R ;

WEITEKAMP, DP .

JOURNAL OF MAGNETIC RESONANCE, 1985, 62 (01) :54-64

[4] TWO-DIMENSIONAL SOLID-STATE NMR-SPECTROSCOPY - NEW POSSIBILITIES FOR THE INVESTIGATION OF THE STRUCTURE AND DYNAMICS OF SOLID POLYMERS [J].

BLUMICH, B ;

SPIESS, HW .

ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1988, 27 (12) :1655-1672

[5]

BRUNNER P, 1980, J CHEM PHYS, V73, P1086, DOI 10.1063/1.440258

[6] 13C AND 220 MHZ ANALYSIS OF CAMPHOR AND THIOCAMPHOR . ANISOTROPY AND SOLVENT EFFECTS OF C=S BOND [J].

DEMARCO, PV ;

DODDRELL, D ;

WENKERT, E .

JOURNAL OF THE CHEMICAL SOCIETY D-CHEMICAL COMMUNICATIONS, 1969, (23) :1418-&

[7] DEUTERIUM DOUBLE-QUANTUM NMR WITH MAGIC ANGLE SPINNING [J].

ECKMAN, R ;

MULLER, L ;

PINES, A .

CHEMICAL PHYSICS LETTERS, 1980, 74 (02) :376-378

[8] SEPARATED LOCAL FIELD SPECTRA IN NMR - DETERMINATION OF STRUCTURE OF SOLIDS [J].

HESTER, RK ;

ACKERMAN, JL ;

NEFF, BL ;

WAUGH, JS .

PHYSICAL REVIEW LETTERS, 1976, 36 (18) :1081-1083

[9] ROTATIONAL SPIN ECHOES AND HIGH-RESOLUTION NMR IN POWDERS [J].

MARICQ, M ;

WAUGH, JS .

CHEMICAL PHYSICS LETTERS, 1977, 47 (02) :327-329

[10] NMR IN ROTATING SOLIDS [J].

MARICQ, MM ;

WAUGH, JS .

JOURNAL OF CHEMICAL PHYSICS, 1979, 70 (07) :3300-3316

← 1 2 3 →