Indirectly detected heteronuclear correlation solid-state NMR spectroscopy of naturally abundant 15N nuclei

被引:52
作者
Althaus, Stacey M. [1 ,2 ]
Mao, Kanmi [1 ,2 ]
Stringer, John A. [3 ]
Kobayashi, Takeshi [2 ]
Pruski, Marek [1 ,2 ]
机构
[1] US DOE, Ames Lab, Ames, IA 50011 USA
[2] Iowa State Univ, Dept Chem, Ames, IA 50011 USA
[3] Agilent Technol, Loveland, CO 80537 USA
关键词
Solid-state N-15 NMR; FastMAS; J-coupling; HETCOR; INEPT; Indirect detection; Mesoporous silica; INVERSE DETECTION; CHEMICAL-SHIFT; FAST-MAS; SENSITIVITY ENHANCEMENT; CROSS-POLARIZATION; H-1; RESOLUTION; PROTON; PEPTIDE; MAGNITUDES;
D O I
10.1016/j.ssnmr.2013.11.001
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
Two-dimensional indirectly detected through-space and through-bond H-1{N-15} solid-state NMR experiments utilizing fast magic angle spinning (MAS) and homonuclear multipulse H-1 decoupling are evaluated. Remarkable efficiency of polarization transfer can be achieve data MAS rate of 40kHz by both cross-polarization and INEPT, which makes these methods applicable for routine characterizations of natural abundance solids. The first measurement of 2D H-1{N-15} HETCOR spectrum of natural abundance surface species is also reported. (C) 2013 Elsevier Inc. All rights reserved.
引用
收藏
页码:17 / 21
页数:5
相关论文
共 54 条
[1]   Mufti-scale NMR characterisation of mesostructured materials using 1H→13C through-bond polarisation transfer, fast MAS, and 1H spin diffusion [J].
Alonso, B ;
Massiot, D .
JOURNAL OF MAGNETIC RESONANCE, 2003, 163 (02) :347-352
[2]   Solid-State NMR Studies of Fossil Fuels using One- and Two-Dimensional Methods at High Magnetic Field [J].
Althaus, Stacey M. ;
Mao, Kanmi ;
Kennedy, Gordon J. ;
Pruski, Marek .
ENERGY & FUELS, 2012, 26 (07) :4405-4412
[3]   SIMPSON: A general simulation program for solid-state NMR spectroscopy [J].
Bak, M ;
Rasmussen, JT ;
Nielsen, NC .
JOURNAL OF MAGNETIC RESONANCE, 2000, 147 (02) :296-330
[4]   CORRELATION OF PROTON AND N-15 CHEMICAL-SHIFTS BY MULTIPLE QUANTUM NMR [J].
BAX, A ;
GRIFFEY, RH ;
HAWKINS, BL .
JOURNAL OF MAGNETIC RESONANCE, 1983, 55 (02) :301-315
[5]   NATURAL ABUNDANCE N-15 NMR BY ENHANCED HETERONUCLEAR SPECTROSCOPY [J].
BODENHAUSEN, G ;
RUBEN, DJ .
CHEMICAL PHYSICS LETTERS, 1980, 69 (01) :185-189
[6]   An investigation of the hydrogen-bonding structure in bilirubin by 1H double-quantum magic-angle spinning solid-state NMR spectroscopy [J].
Brown, SP ;
Zhu, XX ;
Saalwächter, K ;
Spiess, HW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2001, 123 (18) :4275-4285
[7]   Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy [J].
Cavadini, Simone ;
Antonijevic, Sasa ;
Lupulescu, Adonis ;
Bodenhausen, Geoffrey .
JOURNAL OF MAGNETIC RESONANCE, 2006, 182 (01) :168-172
[8]   Nitrogen-14 NMR spectroscopy using residual dipolar splittings in solids [J].
Cavadini, Simone ;
Lupulescu, Adonis ;
Antonijevic, Sasa ;
Bodenhausen, Geoffrey .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2006, 128 (24) :7706-7707
[9]   Urea and Thiourea-Functionalized Mesoporous Silica Nanoparticle Catalysts with Enhanced Catalytic Activity for Diels-Alder Reaction [J].
Chen, Hung-Ting ;
Trewyn, Brian G. ;
Wiench, Jerzy W. ;
Pruski, Marek ;
Lin, Victor S. -Y. .
TOPICS IN CATALYSIS, 2010, 53 (3-4) :187-191
[10]   Ultrahigh resolution in proton solid-state NMR spectroscopy at high levels of deuteration [J].
Chevelkov, V ;
Rehbein, K ;
Diehl, A ;
Reif, B .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2006, 45 (23) :3878-3881