Satellite-transition MAS NMR of low-γ nuclei at natural abundance:: Sensitivity, practical implementation, and application to 39K (I=3/2) and 25Mg (I=5/2)

被引:25
作者
Dowell, NG
Ashbrook, SE
Wimperis, S
机构
[1] Univ Exeter, Dept Chem, Exeter EX4 4QD, Devon, England
[2] Univ Cambridge, Dept Earth Sci, Cambridge CB2 3EQ, England
关键词
D O I
10.1021/jp047868m
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
Satellite-transition magic angle spinning (STMAS) is a recently introduced technique for recording high-resolution NMR spectra of quadrupolar nuclei in solids. We present numerical calculations of STMAS signal intensity as a function of radio frequency field strength (v(1)) and spinning rate (v(R)) and show that the sensitivity advantage of STMAS over the older multiple-quantum technique (MQMAS) is greatest for low v(1) field strengths and high v(R) rates, making STMAS particularly suitable for the study of low-gamma nuclei. The practical implementation of STMAS in NMR of low-y nuclei is discussed and several experimental examples of high-resolution K-39 (I = 3/2) and Mg-25 (I = 5/2) NMR spectra are presented, including Mg-25 spectra of brucite (Mg(OH)(2)), diopside (CaMgSi2O6), and talc (Mg3Si4O10(OH)(2)) recorded at the natural Mg-25 abundance of 10%.
引用
收藏
页码:13292 / 13299
页数:8
相关论文
共 28 条
[11]   SOLID-STATE MAGNESIUM-25 NMR-SPECTROSCOPY [J].
DUPREE, R ;
SMITH, ME .
JOURNAL OF THE CHEMICAL SOCIETY-CHEMICAL COMMUNICATIONS, 1988, (22) :1483-1485
[12]  
FISKE PS, 1994, AM MINERAL, V79, P848
[13]   ISOTROPIC SPECTRA OF HALF-INTEGER QUADRUPOLAR SPINS FROM BIDIMENSIONAL MAGIC-ANGLE-SPINNING NMR [J].
FRYDMAN, L ;
HARWOOD, JS .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1995, 117 (19) :5367-5368
[14]  
GAN Z, COMMUNICATION
[15]   Isotropic NMR spectra of half-integer quadrupolar nuclei using satellite transitions and magic-angle spinning [J].
Gan, ZH .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2000, 122 (13) :3242-3243
[16]   Third-order effect in solid-state NMR of quadrupolar nuclei [J].
Gan, ZH ;
Srinivasan, P ;
Quine, JR ;
Steuernagel, S ;
Knott, B .
CHEMICAL PHYSICS LETTERS, 2003, 367 (1-2) :163-169
[18]   Solid-state 25Mg NMR of a magnesium(II) adensosine 5′-triphosphate complex [J].
Grant, CV ;
Frydman, V ;
Frydman, L .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2000, 122 (47) :11743-11744
[19]   Magnesium coordination environments in glasses and minerals: New insight from high-field magnesium-25 MAS NMR [J].
Kroeker, S ;
Stebbins, JF .
AMERICAN MINERALOGIST, 2000, 85 (10) :1459-1464
[20]   Two-dimensional magic-angle spinning isotropic reconstruction sequences for quadrupolar nuclei [J].
Massiot, D ;
Touzo, B ;
Trumeau, D ;
Coutures, JP ;
Virlet, J ;
Florian, P ;
Grandinetti, PJ .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 1996, 6 (01) :73-83