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Title: 1 H- 19 F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers

Solid state NMR spectroscopy is inherently sensitive to chemical structure and composition, and thus makes an ideal method to probe the heterogeneity of multicomponent polymers. Specifically, NMR spin diffusion experiments can be used to extract reliable information about spatial domain sizes on multiple length scales, provided that magnetization selection of one domain can be achieved. In this paper, we demonstrate the preferential filtering of protons in fluorinated domains during NMR spin diffusion exper-iments using 1H- 19F heteronuclear dipolar dephasing based on rotational echo double resonance (REDOR) MAS NMR techniques. Three pulse sequence variations are demonstrated based on the different nuclei detected: direct 1H detection, plus both 1H→ 13C cross polarization (CP) and 1H→ 19F CP detection schemes. This 1H- 19F REDOR-filtered spin diffusion method was used to measure fluorinated domain sizes for a complex polymer blend. The efficacy of the REDOR-based spin filter does not rely on spin relaxation behavior or chemical shift differences, and thus is applicable for performing NMR spin diffu-sion experiments in samples where traditional magnetization filters may prove unsuccessful. This REDOR-filtered NMR spin diffusion method can also be extended to other samples where a heteronuclear spin pair exists that is unique to the domain of interest.
Authors:
 [1] ; ORCiD logo [1]
  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Publication Date:
Report Number(s):
SAND2016-8394J
Journal ID: ISSN 0749-1581; 646944
Grant/Contract Number:
AC04-94AL85000
Type:
Accepted Manuscript
Journal Name:
Magnetic Resonance in Chemistry
Additional Journal Information:
Journal Volume: 55; Journal Issue: 11; Journal ID: ISSN 0749-1581
Research Org:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org:
USDOE National Nuclear Security Administration (NNSA)
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE
OSTI Identifier:
1469656

Sorte, Eric G., and Alam, Todd M.. 1 H- 19 F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers. United States: N. p., Web. doi:10.1002/mrc.4623.
Sorte, Eric G., & Alam, Todd M.. 1 H- 19 F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers. United States. doi:10.1002/mrc.4623.
Sorte, Eric G., and Alam, Todd M.. 2017. "1 H- 19 F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers". United States. doi:10.1002/mrc.4623. https://www.osti.gov/servlets/purl/1469656.
@article{osti_1469656,
title = {1 H- 19 F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers},
author = {Sorte, Eric G. and Alam, Todd M.},
abstractNote = {Solid state NMR spectroscopy is inherently sensitive to chemical structure and composition, and thus makes an ideal method to probe the heterogeneity of multicomponent polymers. Specifically, NMR spin diffusion experiments can be used to extract reliable information about spatial domain sizes on multiple length scales, provided that magnetization selection of one domain can be achieved. In this paper, we demonstrate the preferential filtering of protons in fluorinated domains during NMR spin diffusion exper-iments using 1H-19F heteronuclear dipolar dephasing based on rotational echo double resonance (REDOR) MAS NMR techniques. Three pulse sequence variations are demonstrated based on the different nuclei detected: direct 1H detection, plus both 1H→13C cross polarization (CP) and 1H→19F CP detection schemes. This 1H-19F REDOR-filtered spin diffusion method was used to measure fluorinated domain sizes for a complex polymer blend. The efficacy of the REDOR-based spin filter does not rely on spin relaxation behavior or chemical shift differences, and thus is applicable for performing NMR spin diffu-sion experiments in samples where traditional magnetization filters may prove unsuccessful. This REDOR-filtered NMR spin diffusion method can also be extended to other samples where a heteronuclear spin pair exists that is unique to the domain of interest.},
doi = {10.1002/mrc.4623},
journal = {Magnetic Resonance in Chemistry},
number = 11,
volume = 55,
place = {United States},
year = {2017},
month = {6}
}