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

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.
Authors:
 [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)
Publication Date:
OSTI Identifier:
1227210
Report Number(s):
IS--J-8827
Journal ID: ISSN 0926-2040; PII: S0926204015000053
Grant/Contract Number:
AC02-07CH11358
Type:
Accepted Manuscript
Journal Name:
Solid State Nuclear Magnetic Resonance
Additional Journal Information:
Journal Volume: 66-67; Journal Issue: C; Journal ID: ISSN 0926-2040
Publisher:
Elsevier
Research Org:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE ultrafast MAS; indirect detection; HSQC; HMQC; mesoporous silica nanoparticles