DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Rapid acquisition of data dense solid-state CPMG NMR spectral sets using multi-dimensional statistical analysis

Abstract

Tensor-rank decomposition methods have been applied to variable contact time29Si{1H} CP/CPMG NMR data sets to extract NMR dynamics information and dramatically decrease conventional NMR acquisition times.

Authors:
ORCiD logo [1];  [2];  [3]
  1. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
  2. Sandia National Lab. (SNL-CA), Livermore, CA (United States)
  3. Hunter College of City Univ. of New York, New York, NY (United States)
Publication Date:
Research Org.:
Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States); Sandia National Lab. (SNL-CA), Livermore, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Biological and Environmental Research (BER)
OSTI Identifier:
1463021
Alternate Identifier(s):
OSTI ID: 1456294; OSTI ID: 1464198
Report Number(s):
LLNL-JRNL-736456; SAND-2018-8223J
Journal ID: ISSN 1463-9076; PPCPFQ; 888524
Grant/Contract Number:  
AC52-07NA27344; AC04-94AL85000
Resource Type:
Accepted Manuscript
Journal Name:
Physical Chemistry Chemical Physics. PCCP (Print)
Additional Journal Information:
Journal Name: Physical Chemistry Chemical Physics. PCCP (Print); Journal Volume: 20; Journal Issue: 26; Journal ID: ISSN 1463-9076
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Mason, H. E., Uribe, E. C., and Shusterman, J. A. Rapid acquisition of data dense solid-state CPMG NMR spectral sets using multi-dimensional statistical analysis. United States: N. p., 2018. Web. doi:10.1039/C8CP02382D.
Mason, H. E., Uribe, E. C., & Shusterman, J. A. Rapid acquisition of data dense solid-state CPMG NMR spectral sets using multi-dimensional statistical analysis. United States. https://doi.org/10.1039/C8CP02382D
Mason, H. E., Uribe, E. C., and Shusterman, J. A. Wed . "Rapid acquisition of data dense solid-state CPMG NMR spectral sets using multi-dimensional statistical analysis". United States. https://doi.org/10.1039/C8CP02382D. https://www.osti.gov/servlets/purl/1463021.
@article{osti_1463021,
title = {Rapid acquisition of data dense solid-state CPMG NMR spectral sets using multi-dimensional statistical analysis},
author = {Mason, H. E. and Uribe, E. C. and Shusterman, J. A.},
abstractNote = {Tensor-rank decomposition methods have been applied to variable contact time29Si{1H} CP/CPMG NMR data sets to extract NMR dynamics information and dramatically decrease conventional NMR acquisition times.},
doi = {10.1039/C8CP02382D},
journal = {Physical Chemistry Chemical Physics. PCCP (Print)},
number = 26,
volume = 20,
place = {United States},
year = {Wed Jun 20 00:00:00 EDT 2018},
month = {Wed Jun 20 00:00:00 EDT 2018}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 3 works
Citation information provided by
Web of Science

Figures / Tables:

Figure-1 Figure-1: Data derived from the tensor-rank decomposition of variable contact time 29Si{1H} CP/MAS CPMG NMR data sets for the DPTS-SBA sample. Contributions from component 1 are given in blue and those from component 2 are given in red (a) The extracted T2 data points (solid symbols) and their corresponding least-squaremore » fits (solid lines). (b) The extracted variable contact time data points (solid symbols) and their corresponding least squares fits to standard CP kinetics equation (solid lines). (c) Extracted FID' s presented in real space as alternating real and imaginary data points. (d). Full echo Fourier transforms of the FID' s presented in (c) and corrected for difference in magnitude using the T2 fits in (a)« less

Save / Share:

Works referenced in this record:

Spatial distribution of organic functional groups supported on mesoporous silica nanoparticles: a study by conventional and DNP-enhanced 29 Si solid-state NMR
journal, January 2017

  • Kobayashi, Takeshi; Singappuli-Arachchige, Dilini; Wang, Zhuoran
  • Physical Chemistry Chemical Physics, Vol. 19, Issue 3
  • DOI: 10.1039/C6CP07642D

Probing the interaction of U( vi ) with phosphonate-functionalized mesoporous silica using solid-state NMR spectroscopy
journal, January 2016

  • Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.
  • Dalton Transactions, Vol. 45, Issue 25
  • DOI: 10.1039/C6DT01200K

Solid-state NMR spectroscopy of Pb-rich apatite
journal, December 2009

  • Mason, Harris E.; Hirner, Joshua J.; Xu, Wenqian
  • Magnetic Resonance in Chemistry, Vol. 47, Issue 12
  • DOI: 10.1002/mrc.2514

Development and Testing of Diglycolamide Functionalized Mesoporous Silica for Sorption of Trivalent Actinides and Lanthanides
journal, September 2015

  • Shusterman, Jennifer A.; Mason, Harris E.; Bowers, Jon
  • ACS Applied Materials & Interfaces, Vol. 7, Issue 37
  • DOI: 10.1021/acsami.5b04481

119 Sn MAS NMR Study of the Interaction of Probe Molecules with Sn-BEA: The Origin of Penta- and Hexacoordinated Tin Formation
journal, December 2016

  • Yakimov, Alexander V.; Kolyagin, Yury G.; Tolborg, Søren
  • The Journal of Physical Chemistry C, Vol. 120, Issue 49
  • DOI: 10.1021/acs.jpcc.6b09999

Unmixing the NMR spectra of similar species – vive la différence
journal, January 2013

  • Colbourne, Adam A.; Meier, Sebastian; Morris, Gareth A.
  • Chemical Communications, Vol. 49, Issue 89
  • DOI: 10.1039/c3cc46228e

Synthesis and characterization of polymeric C18 stationary phases for liquid chromatography
journal, March 1984

  • Sander, Lane C.; Wise, Stephen A.
  • Analytical Chemistry, Vol. 56, Issue 3
  • DOI: 10.1021/ac00267a047

Site-resolved 2H relaxation experiments in solid materials by global line-shape analysis of MAS NMR spectra
journal, July 2016


Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy
journal, March 2013

  • Rossini, Aaron J.; Zagdoun, Alexandre; Lelli, Moreno
  • Accounts of Chemical Research, Vol. 46, Issue 9
  • DOI: 10.1021/ar300322x

Global least‐squares analysis of large, correlated spectral data sets and application to chemical kinetics and time‐resolved fluorescence
journal, December 1996

  • Stilbs, Peter; Paulsen, Kim
  • Review of Scientific Instruments, Vol. 67, Issue 12
  • DOI: 10.1063/1.1147539

One hundred fold overall sensitivity enhancements for Silicon-29 NMR spectroscopy of surfaces by dynamic nuclear polarization with CPMG acquisition
journal, January 2012

  • Rossini, Aaron J.; Zagdoun, Alexandre; Lelli, Moreno
  • Chem. Sci., Vol. 3, Issue 1
  • DOI: 10.1039/C1SC00550B

Natural Abundance 17 O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy
journal, June 2015

  • Perras, Frédéric A.; Kobayashi, Takeshi; Pruski, Marek
  • Journal of the American Chemical Society, Vol. 137, Issue 26
  • DOI: 10.1021/jacs.5b03905

Probing the Surface Structure of Divalent Transition Metals Using Surface Specific Solid-State NMR Spectroscopy
journal, February 2012

  • Mason, Harris E.; Harley, Stephen J.; Maxwell, Robert S.
  • Environmental Science & Technology, Vol. 46, Issue 5
  • DOI: 10.1021/es203733c

Kinetics of Cross-Polarization in Solid-State NMR:  A Guide for Chemists
journal, March 2002

  • Kolodziejski, Waclaw; Klinowski, Jacek
  • Chemical Reviews, Vol. 102, Issue 3
  • DOI: 10.1021/cr000060n

Synthesis of ordered large pore SBA-15 spherical particles for adsorption of biomolecules
journal, July 2006

  • Katiyar, Amit; Yadav, Santosh; Smirniotis, Panagiotis G.
  • Journal of Chromatography A, Vol. 1122, Issue 1-2
  • DOI: 10.1016/j.chroma.2006.04.055

Application of 119 Sn CPMG MAS NMR for Fast Characterization of Sn Sites in Zeolites with Natural 119 Sn Isotope Abundance
journal, March 2016

  • Kolyagin, Yury G.; Yakimov, Alexander V.; Tolborg, Søren
  • The Journal of Physical Chemistry Letters, Vol. 7, Issue 7
  • DOI: 10.1021/acs.jpclett.6b00249

Direct dynamic nuclear polarization targeting catalytically active 27 Al sites
journal, January 2015

  • Lund, Alicia; Hsieh, Ming-Feng; Siaw, Ting-Ann
  • Physical Chemistry Chemical Physics, Vol. 17, Issue 38
  • DOI: 10.1039/C5CP03396A

Analysis of trivalent cation complexation to functionalized mesoporous silica using solid-state NMR spectroscopy
journal, January 2014

  • Shusterman, Jennifer; Mason, Harris; Bruchet, Anthony
  • Dalton Trans., Vol. 43, Issue 44
  • DOI: 10.1039/C4DT02380C

Communication: Phase incremented echo train acquisition in NMR spectroscopy
journal, June 2012

  • Baltisberger, Jay H.; Walder, Brennan J.; Keeler, Eric G.
  • The Journal of Chemical Physics, Vol. 136, Issue 21
  • DOI: 10.1063/1.4728105

Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13 C and 29 Si NMR Enhanced by Dynamic Nuclear Polarization
journal, January 2013

  • Lafon, Olivier; Thankamony, Aany S. Lilly; Kobayashi, Takeshi
  • The Journal of Physical Chemistry C, Vol. 117, Issue 3
  • DOI: 10.1021/jp310109s

Organic layer formation and sorption of U( vi ) on acetamide diethylphosphonate-functionalized mesoporous silica
journal, January 2017

  • Uribe, Eva C.; Mason, Harris E.; Shusterman, Jennifer A.
  • Dalton Transactions, Vol. 46, Issue 16
  • DOI: 10.1039/C7DT00362E

Sensitivity-Enhanced Quadrupolar-Echo NMR of Half-Integer Quadrupolar Nuclei. Magnitudes and Relative Orientation of Chemical Shielding and Quadrupolar Coupling Tensors
journal, November 1997

  • Larsen, Flemming H.; Jakobsen, Hans J.; Ellis, Paul D.
  • The Journal of Physical Chemistry A, Vol. 101, Issue 46
  • DOI: 10.1021/jp971547b

Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials
journal, January 2013

  • Kobayashi, Takeshi; Lafon, Olivier; Lilly Thankamony, Aany S.
  • Physical Chemistry Chemical Physics, Vol. 15, Issue 15
  • DOI: 10.1039/c3cp00039g

Surface-selective direct 17 O DNP NMR of CeO 2 nanoparticles
journal, January 2017

  • Hope, Michael A.; Halat, David M.; Magusin, Pieter C. M. M.
  • Chemical Communications, Vol. 53, Issue 13
  • DOI: 10.1039/C6CC10145C

Constraints on aluminum and scandium substitution mechanisms in forsterite, periclase, and larnite: High-resolution NMR
journal, June 2017

  • McCarty, Ryan J.; Stebbins, Jonathan F.
  • American Mineralogist, Vol. 102, Issue 6
  • DOI: 10.2138/am-2017-5976

Spectral deconvolution of NMR cross polarization data sets
journal, July 2009

  • Hedin, Niklas; Ng, Jovice B. S.; Stilbs, Peter
  • Solid State Nuclear Magnetic Resonance, Vol. 35, Issue 4
  • DOI: 10.1016/j.ssnmr.2009.04.001

Speedy Component Resolution: An Improved Tool for Processing Diffusion-Ordered Spectroscopy Data
journal, May 2008

  • Nilsson, Mathias; Morris, Gareth A.
  • Analytical Chemistry, Vol. 80, Issue 10
  • DOI: 10.1021/ac7025833

29Si NMR in solid state with CPMG acquisition under MAS
journal, August 2008


Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.