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

Abstract

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:
Research Org.:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1227210
Alternate Identifier(s):
OSTI ID: 1360657
Report Number(s):
IS-J-8827
Journal ID: ISSN 0926-2040; PII: S0926204015000053
Grant/Contract Number:  
AC02-07CH11358
Resource 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
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ultrafast MAS; indirect detection; HSQC; HMQC; mesoporous silica nanoparticles

Citation Formats

Nishiyama, Y., Kobayashi, T., Malon, M., Singappuli-Arachchige, D., Slowing, I. I., and Pruski, M. Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS. United States: N. p., 2015. Web. doi:10.1016/j.ssnmr.2015.02.001.
Nishiyama, Y., Kobayashi, T., Malon, M., Singappuli-Arachchige, D., Slowing, I. I., & Pruski, M. Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS. United States. doi:10.1016/j.ssnmr.2015.02.001.
Nishiyama, Y., Kobayashi, T., Malon, M., Singappuli-Arachchige, D., Slowing, I. I., and Pruski, M. Mon . "Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS". United States. doi:10.1016/j.ssnmr.2015.02.001. https://www.osti.gov/servlets/purl/1227210.
@article{osti_1227210,
title = {Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS},
author = {Nishiyama, Y. and Kobayashi, T. and Malon, M. and Singappuli-Arachchige, D. and Slowing, I. I. and Pruski, M.},
abstractNote = {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.},
doi = {10.1016/j.ssnmr.2015.02.001},
journal = {Solid State Nuclear Magnetic Resonance},
number = C,
volume = 66-67,
place = {United States},
year = {2015},
month = {2}
}

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