29Si and 17O (Q)CPMG-MAS solid-state NMR experiments as an optimum approach for half-integer nuclei having long T1 relaxation times

被引:78
作者
Larsen, FH [1 ]
Farnan, I [1 ]
机构
[1] Univ Cambridge, Dept Earth Sci, Cambridge CB2 3EQ, England
关键词
D O I
10.1016/S0009-2614(02)00520-1
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
A significantly reduced experiment time for half-integer nuclei with long T-1 relaxation times has been demonstrated by Si-29 CPMG-MAS or O-17 QCPMG-MAS experiments on alpha-cristobalite, a radiation damaged Zircon and O-17 enriched alpha-quartz, respectively. For Si-29 up to 37 h were saved compared to the MAS experiment using longer recycle periods (up to 3600 s) but fewer scans. The spectrum reconstructed from the echoes provides similar spectral information as the MAS spectrum. In the O-17 spectrum increased sensitivity facilitated determination of CSA in alpha-quartz at 9.4 T and points towards a method to obtain natural abundance O-17 spectra of non-cubic oxides. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
收藏
页码:403 / 408
页数:6
相关论文
共 15 条
[1]   The degree and nature of radiation damage in zircon observed by 29Si nuclear magnetic resonance [J].
Farnan, I ;
Salje, EKH .
JOURNAL OF APPLIED PHYSICS, 2001, 89 (04) :2084-2090
[2]   Measurement of molecular motion in solids by nuclear magnetic resonance spectroscopy of half-integer quadrupole nuclei [J].
Kristensen, JH ;
Farnan, I .
JOURNAL OF CHEMICAL PHYSICS, 2001, 114 (21) :9608-9624
[3]  
KRISTENSEN JH, 2002, UNPUB J MAGN RESON
[4]   QCPMG-MAS NMR of half-integer quadrupolar nuclei [J].
Larsen, FH ;
Jakobsen, HJ ;
Ellis, PD ;
Nielsen, NC .
JOURNAL OF MAGNETIC RESONANCE, 1998, 131 (01) :144-147
[5]   Molecular dynamics from 2H quadrupolar Carr-Purcell-Meiboom-Gill solid-state NMR spectroscopy [J].
Larsen, FH ;
Jakobsen, HJ ;
Ellis, PD ;
Nielsen, NC .
CHEMICAL PHYSICS LETTERS, 1998, 292 (4-6) :467-473
[6]   Solid-state QCPMG NMR of low-γ quadrupolar metal nuclei in natural abundance [J].
Larsen, FH ;
Skibsted, J ;
Jakobsen, HJ ;
Nielsen, NC .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2000, 122 (29) :7080-7086
[7]  
Larsen FH, 1998, MOL PHYS, V95, P1185, DOI 10.1080/00268979809483250
[8]   A general strategy for the NMR observation of half-integer quadrupolar nuclei in dilute environments [J].
Lipton, AS ;
Sears, JA ;
Ellis, PD .
JOURNAL OF MAGNETIC RESONANCE, 2001, 151 (01) :48-59
[9]   67Zn solid-state NMR spectroscopy of the minimal DNA binding domain of human nucleotide excision repair protein XPA [J].
Lipton, AS ;
Buchko, GW ;
Sears, JA ;
Kennedy, MA ;
Ellis, PD .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2001, 123 (05) :992-993
[10]   MODIFIED SPIN-ECHO METHOD FOR MEASURING NUCLEAR RELAXATION TIMES [J].
MEIBOOM, S ;
GILL, D .
REVIEW OF SCIENTIFIC INSTRUMENTS, 1958, 29 (08) :688-691