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
[1]   Z filtering in MQMAS NMR [J].
Amoureux, JP ;
Fernandez, C ;
Steuernagel, S .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1996, 123 (01) :116-118
[2]   Optimized multiple-quantum magic-angle spinning NMR experiments on half-integer quadrupoles [J].
Amoureux, JP ;
Fernandez, C ;
Frydman, L .
CHEMICAL PHYSICS LETTERS, 1996, 259 (3-4) :347-355
[3]   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
[4]   High-resolution NMR of quadrupolar nuclei in solids: the satellite-transition magic angle spinning (STMAS) experiment [J].
Ashbrook, SE ;
Wimperis, S .
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY, 2004, 45 (1-2) :53-108
[5]   High-resolution 17O NMR spectroscopy of wadsleyite (β-Mg2SiO4) [J].
Ashbrook, SE ;
Berry, AJ ;
Hibberson, WO ;
Steuernagel, S ;
Wimperis, S .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2003, 125 (39) :11824-11825
[6]   Satellite-transition MAS NMR of spin I=3/2, 5/2, 7/2, and 9/2 nuclei: Sensitivity, resolution, and practical implementation [J].
Ashbrook, SE ;
Wimperis, S .
JOURNAL OF MAGNETIC RESONANCE, 2002, 156 (02) :269-281
[7]   High-resolution NMR spectroscopy of quadrupolar nuclei in solids: Satellite-transition MAS with self-compensation for magic-angle misset [J].
Ashbrook, SE ;
Wimperis, S .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2002, 124 (39) :11602-11603
[8]   POWDER DETERMINATION OF K-39 NUCLEAR-QUADRUPOLE COUPLING [J].
BASTOW, TJ .
JOURNAL OF THE CHEMICAL SOCIETY-FARADAY TRANSACTIONS, 1991, 87 (15) :2453-2455
[9]   MG-25 NUCLEAR-QUADRUPOLE COUPLING IN MG(OH)2 [J].
BASTOW, TJ .
SOLID STATE COMMUNICATIONS, 1991, 77 (07) :547-548
[10]   Two-dimensional multiple-quantum MAS NMR of quadrupolar nuclei: A comparison of methods [J].
Brown, SP ;
Wimperis, S .
JOURNAL OF MAGNETIC RESONANCE, 1997, 128 (01) :42-61