Enhancing sensitivity of quadrupolar nuclei in solid-state NMR with multiple rotor assisted population transfers

被引:69
作者
Kwak, HT [1 ]
Prasad, S [1 ]
Clark, T [1 ]
Grandinetti, PJ [1 ]
机构
[1] Ohio State Univ, Dept Chem, Columbus, OH 43210 USA
基金
美国国家科学基金会;
关键词
D O I
10.1016/S0926-2040(03)00051-1
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
Rotor-assisted population transfer (RAPT) was developed as a method for enhancing MAS NMR sensitivity of quadrupolar nuclei by transferring polarization associated with satellite transitions to the central m = 1/2--> - 1/2 transition. After a single RAPT transfer, there still remains polarization in the satellite transitions that can be transferred to the central transition. This polarization is available without having to wait for the spill system to return to thermal equilibrium. We describe a new RAPT scheme that uses the remaining polarization of the satellites to obtain a further enhancement of the central transition by performing RAPT-enhanced experiments multiple times before waiting for re-equilibration of the spin system. For Al-27 (I = 5/2) in albite we obtain a multiple RAPT enhancement of 3.02, a 48% increase over single RAPT. For Nb-93 (I = 9/2) in NaNbO3 we obtain a multiple RAPT enhancement of 5.76, an 89% increase over single RAPT. We also describe a data processing procedure for obtaining the maximum possible signal-to-noise ratio. (C) 2003 Published by Elsevier Inc.
引用
收藏
页码:71 / 77
页数:7
相关论文
共 14 条
[1]   SINGLE-RESONANCE AND DOUBLE-RESONANCE EXPERIMENTS OF QUADRUPOLAR NUCLEI IN SOLIDS USING SENSITIVITY ENHANCEMENT OF THE CENTRAL TRANSITION [J].
HAASE, J ;
CONRADI, MS ;
OLDFIELD, E .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1994, 109 (02) :210-215
[2]   SENSITIVITY ENHANCEMENT FOR NMR OF THE CENTRAL TRANSITION OF QUADRUPOLAR NUCLEI [J].
HAASE, J ;
CONRADI, MS .
CHEMICAL PHYSICS LETTERS, 1993, 209 (03) :287-291
[3]   POPULATION TRANSFERS FOR NMR OF QUADRUPOLAR SPINS IN SOLIDS [J].
HAASE, J ;
CONRADI, MS ;
GREY, CP ;
VEGA, AJ .
JOURNAL OF MAGNETIC RESONANCE SERIES A, 1994, 109 (01) :90-97
[4]   Advantages of double frequency sweeps in static, MAS and MQMAS NMR of spin I=3/2 nuclei [J].
Kentgens, APM ;
Verhagen, R .
CHEMICAL PHYSICS LETTERS, 1999, 300 (3-4) :435-443
[5]  
KRIKPATRICK RJ, 1985, AM MINERAL, V70, P106
[6]   Enhanced sensitivity in RIACT/MQ-MAS NMR experiments using rotor assisted population transfer [J].
Kwak, HT ;
Prasad, S ;
Yao, Z ;
Grandinetti, PJ ;
Sachleben, JR ;
Emsley, L .
JOURNAL OF MAGNETIC RESONANCE, 2001, 150 (01) :71-80
[7]   PROTON-ENHANCED NUCLEAR INDUCTION SPECTROSCOPY C-13 CHEMICAL SHIELDING ANISOTROPY IN SOME ORGANIC SOLIDS [J].
PINES, A ;
WAUGH, JS ;
GIBBY, MG .
CHEMICAL PHYSICS LETTERS, 1972, 15 (03) :373-&
[8]   PROTON-ENHANCED NMR OF DILUTE SPINS IN SOLIDS [J].
PINES, A ;
GIBBY, MG ;
WAUGH, JS .
JOURNAL OF CHEMICAL PHYSICS, 1973, 59 (02) :569-590
[9]   NUCLEAR ELECTRIC QUADRUPOLE INTERACTIONS IN CRYSTALS [J].
POUND, RV .
PHYSICAL REVIEW, 1950, 79 (04) :685-702
[10]   A simple technique for determining nuclear quadrupole coupling constants with RAPT solid-state NMR spectroscopy [J].
Prasad, S ;
Kwak, HT ;
Clark, T ;
Grandinetti, PJ .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2002, 124 (18) :4964-4965