Versatility of the dipolar filter selection: From 1H nuclear spin diffusion experiment to the measurement of nuclear Overhauser effect in homopolymer melts

Gaborieau, Marianne, Graf, Robert and Spiess, Hans Wolfgang (2004) Versatility of the dipolar filter selection: From 1H nuclear spin diffusion experiment to the measurement of nuclear Overhauser effect in homopolymer melts. Solid state nuclear magnetic resonance, 28 2-4: 160-172. doi:10.1016/j.ssnmr.2005.07.006


Author Gaborieau, Marianne
Graf, Robert
Spiess, Hans Wolfgang
Title Versatility of the dipolar filter selection: From 1H nuclear spin diffusion experiment to the measurement of nuclear Overhauser effect in homopolymer melts
Journal name Solid state nuclear magnetic resonance   Check publisher's open access policy
ISSN 0926-2040
Publication date 2004-09-01
Sub-type Article (original research)
DOI 10.1016/j.ssnmr.2005.07.006
Open Access Status
Volume 28
Issue 2-4
Start page 160
End page 172
Total pages 13
Place of publication Amsterdam
Publisher Academic Press
Language eng
Subject 0303 Macromolecular and Materials Chemistry
Abstract Dipolar filters select 1H magnetization according to local dipolar dephasing, which corresponds to site mobility in systems with heterogeneous molecular mobility. Combined with a conventional exchange experiment, it is usually applied to polymeric samples exhibiting structures on the nanometer length scale associated with a strong dynamic contrast. There, the resulting 1H nuclear spin diffusion experiment yields the size of the structure. When the same experiment is applied to homopolymer melts exhibiting a weak dynamic contrast and dynamic heterogeneities on significant shorter length scales, the recorded magnetization decay is in agreement with decays expected from a heterogeneous nanostructure. However, dipolar filters actually can also select mobile parts of the repeat unit, e.g. the end of the alkyl side chains and the subsequent magnetization transfer then can occur via cross relaxation due to non coherent zero-quantum transitions (nuclear Overhauser effect, NOE). The difficulties of distinguishing these two cases are examined and it is demonstrated that NOE experiments exploiting magnetization selection via the dipolar filter allow quantifying the local dynamics of the side chains. This opens new possibilities for measurements of local dynamics in non isotopically labeled homopolymer melts.
Keyword Solid state NMR
Dipolar filter
Spin diffusion
Nuclear Overhauser effect
NOE
Local dynamics
Homopolymer melt
Poly(ethyl methacrylate)
Polymethacrylate
Q-Index Code C1
Q-Index Status Provisional Code
Institutional Status Unknown

Document type: Journal Article
Sub-type: Article (original research)
Collections: Excellence in Research Australia (ERA) - Collection
Centre for Nutrition and Food Sciences Publications
 
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Created: Thu, 02 Apr 2009, 19:44:09 EST by Ms Lynette Adams on behalf of Centre for Nutrition and Food Sciences