Detection and quantification of branching in polyacrylates by size-exclusion chromatography (SEC) and melt-state 13C NMR spectroscopy

Castignolles, Patrice, Graf, Robert, Parkinson, Matthew, Wilhelm, Manfred and Gaborieau, Marianne (2009) Detection and quantification of branching in polyacrylates by size-exclusion chromatography (SEC) and melt-state 13C NMR spectroscopy. Polymer, 50 11: 2373-2383. doi:10.1016/j.polymer.2009.03.021


Author Castignolles, Patrice
Graf, Robert
Parkinson, Matthew
Wilhelm, Manfred
Gaborieau, Marianne
Title Detection and quantification of branching in polyacrylates by size-exclusion chromatography (SEC) and melt-state 13C NMR spectroscopy
Formatted title
Detection and quantification of branching in polyacrylates by size-exclusion chromatography (SEC) and melt-state 13C NMR spectroscopy
Journal name Polymer   Check publisher's open access policy
ISSN 0032-3861
1873-2291
Publication date 2009-05
Sub-type Article (original research)
DOI 10.1016/j.polymer.2009.03.021
Volume 50
Issue 11
Start page 2373
End page 2383
Total pages 11
Place of publication Oxford, United Kingdom
Publisher Elsevier
Language eng
Formatted abstract
Chain branching has been investigated in a homologous series of poly(n-alkyl acrylates) (methyl, ethyl, n-butyl, n-hexyl) obtained by radical polymerization. The total amount of chain branching was quantified using melt-state 13C nuclear magnetic resonance (NMR) spectroscopy. It gave access to low degrees of branching in both soluble and insoluble polyacrylates, homopolymers and copolymers. The lowest degree of branching was found for the ethyl member of the series with quantification by conventional solution-state NMR found to take a prohibitively long time. The method proposed here is compared to the ones published previously, and previous literature results are critically reviewed.

The presence of long-chain branching (LCB) was selectively detected using multiple-detection size-exclusion chromatography (SEC), with LCB being found for all soluble homopolymers but the poly(n-butyl acrylate). This finding was confirmed by close examination of the Mark–Houwink parameters for the various polyacrylates studied in this work or those previously published.
Keyword Branching
NMR
Size-exclusion chromatography
Q-Index Code C1
Q-Index Status Provisional Code
Institutional Status UQ

Document type: Journal Article
Sub-type: Article (original research)
Collection: Centre for Nutrition and Food Sciences Publications
 
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Created: Thu, 03 Sep 2009, 08:04:02 EST by Mr Andrew Martlew on behalf of Centre for Nutrition and Food Sciences