Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy

被引:126
作者
Blanc, Frederic [1 ,2 ]
Sperrin, Luke [1 ]
Jefferson, David A. [1 ]
Pawsey, Shane [3 ]
Rosay, Melanie [3 ]
Grey, Clare P. [1 ,4 ]
机构
[1] Univ Cambridge, Dept Chem, Cambridge CB2 1EW, England
[2] Univ Liverpool, Stephenson Inst Renewable Energy, Dept Chem, Liverpool L69 7ZD, Merseyside, England
[3] Bruker BioSpin Corp, Billerica, MA 01821 USA
[4] SUNY Stony Brook, Dept Chem, Stony Brook, NY 11794 USA
基金
英国工程与自然科学研究理事会;
关键词
SOLID-STATE NMR; INTEGER QUADRUPOLAR NUCLEI; MAS-NMR; CROSS-POLARIZATION; POPULATION; CHEMISTRY; OXYGEN;
D O I
10.1021/ja4004377
中图分类号
O6 [化学];
学科分类号
070301 [无机化学];
摘要
We show that natural abundance oxygen-17 NMR of solids could be obtained in minutes at a moderate magnetic field strength by using dynamic nuclear polarization (DNP). Electron spin polarization could be transferred either directly to O-17 spins or indirectly via H-1 spins in inorganic oxides and hydroxides using an oxygen-free solution containing a biradical polarization agent (bTbK). The results open up a powerful method for rapidly acquiring high signal-to-noise ratio solid-state NMR spectra of O-17 nuclear spins and to probe sites on or near the surface, without the need for isotope labeling.
引用
收藏
页码:2975 / 2978
页数:4
相关论文
共 53 条
[1]
Dynamic Nuclear Polarization of Deuterated Proteins [J].
Akbey, Uemit ;
Franks, W. Trent ;
Linden, Arne ;
Lange, Sascha ;
Griffin, Robert G. ;
van Rossum, Barth-Jan ;
Oschkinat, Hartmut .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2010, 49 (42) :7803-7806
[2]
Solid-state 17O nuclear magnetic resonance spectroscopy without isotopic enrichment:: direct detection of bridging oxygen in radiation damaged zircon [J].
Ashbrook, SE ;
Farnan, I .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2004, 26 (02) :105-112
[3]
Multiple-quantum cross-polarization in MAS NMR of quadrupolar nuclei [J].
Ashbrook, SE ;
Brown, SP ;
Wimperis, S .
CHEMICAL PHYSICS LETTERS, 1998, 288 (2-4) :509-517
[4]
Solid state 17O NMR -: an introduction to the background principles and applications to inorganic materials [J].
Ashbrook, Sharon E. ;
Smith, Mark E. .
CHEMICAL SOCIETY REVIEWS, 2006, 35 (08) :718-735
[5]
Functional and shunt states of bacteriorhodopsin resolved by 250 GHz dynamic nuclear polarization-enhanced solid-state NMR [J].
Bajaj, Vikram S. ;
Mak-Jurkauskas, Melody L. ;
Belenky, Marina ;
Herzfeld, Judith ;
Griffin, Robert G. .
PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA, 2009, 106 (23) :9244-9249
[6]
High-field dynamic nuclear polarization for solid and solution biological NMR [J].
Barnes, A. B. ;
De Paepe, G. ;
van der Wel, P. C. A. ;
Hu, K. -N. ;
Joo, C. -G. ;
Bajaj, V. S. ;
Mak-Jurkauskas, M. L. ;
Sirigiri, J. R. ;
Herzfeld, J. ;
Temkin, R. J. ;
Griffin, R. G. .
APPLIED MAGNETIC RESONANCE, 2008, 34 (3-4) :237-263
[7]
O-17 NMR IN SIMPLE OXIDES [J].
BASTOW, TJ ;
STUART, SN .
CHEMICAL PHYSICS, 1990, 143 (03) :459-467
[8]
High resolution solid state NMR spectroscopy in surface organometallic chemistry:: access to molecular understanding of active sites of well-defined heterogeneous catalysts [J].
Blanc, Frederic ;
Coperet, Christophe ;
Lesage, Anne ;
Emsley, Lyndon .
CHEMICAL SOCIETY REVIEWS, 2008, 37 (03) :518-526
[9]
POLARIZATION OF NUCLEAR SPINS IN METALS [J].
CARVER, TR ;
SLICHTER, CP .
PHYSICAL REVIEW, 1953, 92 (01) :212-213
[10]
EXPERIMENTAL VERIFICATION OF THE OVERHAUSER NUCLEAR POLARIZATION EFFECT [J].
CARVER, TR ;
SLICHTER, CP .
PHYSICAL REVIEW, 1956, 102 (04) :975-980