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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]
+ Show Author Affiliations
  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.
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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. https://doi.org/10.1016/j.ssnmr.2015.02.001
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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. https://doi.org/10.1016/j.ssnmr.2015.02.001. https://www.osti.gov/servlets/purl/1227210.
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@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 = {Mon Feb 16 00:00:00 EST 2015},
month = {Mon Feb 16 00:00:00 EST 2015}
}
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https://doi.org/10.1016/j.ssnmr.2015.02.001
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    Works referencing / citing this record:

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