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Title: Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS

Journal Article · · Solid State Nuclear Magnetic Resonance
 [1];  [2];  [1];  [3];  [3];  [3]
  1. JEOL Resonance Inc., Tokyo (Japan); RIKEN CLST-JEOL Collaboration Center, Kanagawa (Japan)
  2. Ames Lab., Ames, IA (United States)
  3. Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)
+ Show Author Affiliations

Two-dimensional 1H{13C} heteronuclear correlation solid-state NMR spectra of naturally abundant solid materials are presented, acquired using the 0.75-mm magic angle spinning (MAS) probe at spinning rates up to 100 kHz. In spite of the miniscule sample volume (290 nL), high-quality HSQC-type spectra of bulk samples as well as surface-bound molecules can be obtained within hours of experimental time. The experiments are compared with those carried out at 40 kHz MAS using a 1.6-mm probe, which offered higher overall sensitivity due to a larger rotor volume. The benefits of ultrafast MAS in such experiments include superior resolution in 1H dimension without resorting to 1H–1H homonuclear RF decoupling, easy optimization, and applicability to mass-limited samples. As a result, the HMQC spectra of surface-bound species can be also acquired under 100 kHz MAS, although the dephasing of transverse magnetization has significant effect on the efficiency transfer under MAS alone.

Research Organization:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC02-07CH11358
OSTI ID:
1227210
Report Number(s):
IS--J-8827; PII: S0926204015000053
Journal Information:
Solid State Nuclear Magnetic Resonance, Journal Name: Solid State Nuclear Magnetic Resonance Journal Issue: C Vol. 66-67; ISSN 0926-2040
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English

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  • Wiench, Jerzy W.; Bronnimann, Charles E.; Lin, Victor S. -Y
  • Journal of the American Chemical Society, Vol. 129, Issue 40, p. 12076-12077 https://doi.org/10.1021/ja074746+
journal September 2007
Observation of a Low-Temperature, Dynamically Driven Structural Transition in a Polypeptide by Solid-State NMR Spectroscopy journal January 2009
Band-Selective 1 H− 13 C Cross-Polarization in Fast Magic Angle Spinning Solid-State NMR Spectroscopy journal December 2008
Nanomole-scale protein solid-state NMR by breaking intrinsic 1H T1 boundaries journal February 2009
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Cited By (4)

Understanding hydrogen-bonding structures of molecular crystals via electron and NMR nanocrystallography journal August 2019
Understanding hydrogen-bonding structures of molecular crystals via electron and NMR nanocrystallography journal August 2019
Natural abundance 14 N and 15 N solid-state NMR of pharmaceuticals and their polymorphs journal January 2016
Forcing the ‘lazy’ protons to work journal January 2018

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Related Subjects

36 MATERIALS SCIENCE
HMQC
HSQC
indirect detection
mesoporous silica nanoparticles
ultrafast MAS