Examples of Hartmann-Hahn match conditions for CP MAS between two half-integer quadrupolar nuclei

被引:19
作者
Eastman, MA [1 ]
机构
[1] Oklahoma State Univ, Dept Chem, Stillwater, OK 74078 USA
基金
美国国家科学基金会;
关键词
quadrupole; CP MAS; spin lock; Hartmann-Hahn; double quantum;
D O I
10.1006/jmre.1999.1773
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Hartmann-Hahn match conditions for n/2 --> m/2 CP/MAS between two quadrupolar nuclei, spin-lock signal as a function of effective nutation frequency, and the correlation of effective nutation frequency and radio frequency field strength are reported for three samples: sodium diborate (Na2B4O7), aluminum boride (AlB2), and lithium aluminate (LiAlO2), Radiofrequency field strengths used for CP/MAS are both greater and less than the sample spinning speed of 10 kHz, resulting in the observation of both zero-quantum and double-quantum matches, which have signals of opposite sign. The match conditions for Na2B4O7 are as expected from published theory and CP/MAS experiments on spins 1/2 and n/2 (n = 3 or 5) with quadrupole frequencies (omega(Q)) large compared to the radiofrequency field strength of the CP contact pulse, consisting mainly of sideband matches at one and two times the sample spinning frequency, and the correlation of effective nutation frequency and radiofrequency field strength supports the conclusion that wp is large for both B-11 and Na-23 Aluminum-27 in AlB2 may have either small or intermediate omega(Q), and Li-7 in LiAlO2 is proposed to have intermediate omega(Q) in relation to the radiofrequency field strength, and both have curves of the spin-lock signal as a function of effective nutation frequency nith central minima, differing from those of the nuclei nith large omega(Q). The sign of the CP/MAS signal for AlB2 and LiAlO2 appears to vary with the CP field strengths for the two nuclei so that positive or negative signals cannot be consistently correlated with zero- or double-quantum matches. However, it is possible to assign at least some of the matches as close to integral multiples of the sample spinning frequency, and some of these are matches at greater than two times the sample spinning frequency. (C) 1999 Academic Press.
引用
收藏
页码:98 / 108
页数:11
相关论文
共 29 条
[1]   Double-quantum cross-polarization between half-integer quadrupolar spin systems:: 11B⇆23Na and 11B ⇆ 27Al [J].
Chan, JCC ;
Bertmer, M ;
Eckert, H .
CHEMICAL PHYSICS LETTERS, 1998, 292 (1-2) :154-160
[2]   Cross-polarization from quadrupolar nuclei to silicon using low-radio-frequency amplitudes during magic-angle spinning [J].
DePaul, SM ;
ERnst, M ;
Shore, JS ;
Stebbins, JF ;
Pines, A .
JOURNAL OF PHYSICAL CHEMISTRY B, 1997, 101 (16) :3240-3249
[3]   SPIN-LOCKING SPECTRAL LINESHAPES OF THE CENTRAL TRANSITION OF HALF-INTEGER QUADRUPOLE SYSTEMS UNDER MAGIC-ANGLE-SPINNING [J].
DING, SW ;
MCDOWELL, CA .
JOURNAL OF MOLECULAR STRUCTURE, 1995, 355 (01) :135-142
[4]   THEORETICAL CALCULATIONS OF THE CPMAS SPECTRAL LINESHAPES OF HALF-INTEGER QUADRUPOLE SYSTEMS [J].
DING, SW ;
MCDOWELL, CA .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1995, 114 (01) :80-87
[5]   CROSS-POLARIZATION FOR QUADRUPOLAR NUCLEI PROTON TO MO-95 [J].
EDWARDS, JC ;
ELLIS, PD .
MAGNETIC RESONANCE IN CHEMISTRY, 1990, 28 :S59-S67
[6]   SOLID-STATE DOUBLE-RESONANCE NMR EXPERIMENTS INVOLVING QUADRUPOLAR AND SPIN 1/2 NUCLEI [J].
FYFE, CA ;
MUELLER, KT ;
GRONDEY, H ;
WONGMOON, KC .
JOURNAL OF PHYSICAL CHEMISTRY, 1993, 97 (51) :13484-13495
[7]   NUCLEAR DOUBLE RESONANCE IN ROTATING FRAME [J].
HARTMANN, SR ;
HAHN, EL .
PHYSICAL REVIEW, 1962, 128 (05) :2042-&
[8]   MAGIC-ANGLE-SPINNING NUCLEAR-MAGNETIC-RESONANCE OF HALF-INTEGER QUADRUPOLE NUCLEI - EFFECT OF SPIN-LOCKING EFFICIENCY ON POWDER LINESHAPES [J].
HAYASHI, S .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 1994, 3 (02) :93-101
[9]   Spin locking of I=3/2 nuclei in static and spinning samples: A description by abstract spins and Floquet formalism [J].
Jeschke, G .
JOURNAL OF CHEMICAL PHYSICS, 1998, 108 (03) :907-917
[10]   TWO-DIMENSIONAL SOLID-STATE NUTATION NMR OF HALF-INTEGER QUADRUPOLAR NUCLEI [J].
KENTGENS, APM ;
LEMMENS, JJM ;
GEURTS, FMM ;
VEEMAN, WS .
JOURNAL OF MAGNETIC RESONANCE, 1987, 71 (01) :62-74