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

Mason, H. E.; Uribe, E. C.; Shusterman, J. A.

doi:10.1039/C8CP02382D

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

Journal Article · Wed Jun 20 00:00:00 EDT 2018 · Physical Chemistry Chemical Physics. PCCP (Print)

DOI:https://doi.org/10.1039/C8CP02382D· OSTI ID:1463021

^[1]; Uribe, E. C. ^[2]; Shusterman, J. A. ^[3]

Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sandia National Lab. (SNL-CA), Livermore, CA (United States)
Hunter College of City Univ. of New York, New York, NY (United States)

The development of multi-dimensional statistical methods has been demonstrated on variable contact time (VCT) ²⁹Si{¹H} cross-polarization magic angle spinning (CP/MAS) data sets collected using Carr–Purcell–Meiboom–Gill (CPMG) type acquisition. These methods utilize the transformation of the collected 2D VCT data set into a 3D data set and use tensor-rank decomposition to extract the spectral components that vary as a function of transverse relaxation time (T₂) and CP contact time. The result is a data dense spectral set that can be used to reconstruct CP/MAS spectra at any contact time with a high signal to noise ratio and with an excellent agreement to ²⁹Si{¹H} CP/MAS spectra collected using conventional acquisition. These CPMG data can be collected in a fraction of time that would be required to collect a conventional VCT data set. Here, we demonstrate the method on samples of functionalized mesoporous silica materials and show that the method can provide valuable surface specific information about their functional chemistry.

View Accepted Manuscript (DOE)

Research Organization:: Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States); Sandia National Laboratories (SNL-CA), Livermore, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Biological and Environmental Research (BER); USDOE Office of Science (SC), Biological and Environmental Research (BER) (SC-23)

Grant/Contract Number:: AC04-94AL85000; AC52-07NA27344

OSTI ID:: 1463021

Alternate ID(s):: OSTI ID: 1456294
OSTI ID: 1464198

Report Number(s):: LLNL-JRNL--736456; SAND--2018-8223J; 888524

Journal Information:: Physical Chemistry Chemical Physics. PCCP (Print), Journal Name: Physical Chemistry Chemical Physics. PCCP (Print) Journal Issue: 26 Vol. 20; ISSN 1463-9076; ISSN PPCPFQ

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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