SEC analysis of poly(acrylic acid) and poly(methacrylic acid)

Lacik, Igor, Stach, Marek, Kasak, Peter, Semak, Vladislav, Uhelska, Lucia, Chovancova, Anna, Reinhold, Gunter, Kilz, Peter, Delaittre, Guillaume, Charleux, Bernadette, Chaduc, Isabelle, D'Agosto, Franck, Lansalot, Muriel, Gaborieau, Marianne, Castignolles, Patrice, Gilbert, Robert G., Szablan, Zachary, Barner-Kowollik, Christopher, Hesse, Pascal and Buback, Michael (2015) SEC analysis of poly(acrylic acid) and poly(methacrylic acid). Macromolecular Chemistry and Physics, 216 1: 23-37. doi:10.1002/macp.201400339

Author Lacik, Igor
Stach, Marek
Kasak, Peter
Semak, Vladislav
Uhelska, Lucia
Chovancova, Anna
Reinhold, Gunter
Kilz, Peter
Delaittre, Guillaume
Charleux, Bernadette
Chaduc, Isabelle
D'Agosto, Franck
Lansalot, Muriel
Gaborieau, Marianne
Castignolles, Patrice
Gilbert, Robert G.
Szablan, Zachary
Barner-Kowollik, Christopher
Hesse, Pascal
Buback, Michael
Title SEC analysis of poly(acrylic acid) and poly(methacrylic acid)
Journal name Macromolecular Chemistry and Physics   Check publisher's open access policy
ISSN 1521-3935
Publication date 2015-01
Year available 2014
Sub-type Article (original research)
DOI 10.1002/macp.201400339
Open Access Status
Volume 216
Issue 1
Start page 23
End page 37
Total pages 15
Place of publication Weinheim, Germany
Publisher Wiley-VCH Verlag
Collection year 2015
Language eng
Formatted abstract
The accurate characterization of molar-mass distributions of poly(acrylic acid) (PAA) and poly(methacrylic acid) (PMAA) by size-exclusion chromatography (SEC) is addressed. Two methods are employed: direct aqueous-phase SEC on P(M)AA and THF-based SEC after esterification of P(M)AA to the associated methyl esters, P(M)MA. P(M)AA calibration standards, P(M)AA samples prepared by pulsed-laser polymerization (PLP), and PAA samples prepared by reversible addition-fragmentation chain transfer (RAFT) are characterized in a joint initiative of seven laboratories, with satisfactory agreement achieved between the institutions. Both SEC methods provide reliable results for PMAA. In the case of PAA, close agreement between the two SEC methods is only observed for samples prepared by RAFT polymerization with weight-average molar mass between 80 000 and 145 000 g mol−1 and for standards with peak molar masses below 20 000 g mol−1. For standards with higher molar masses and for PLP-prepared PAA, the values from THF-based SEC are as much as 40% below the molar masses determined by aqueous-phase SEC. This discrepancy may be due to branching or degradation of branched PAA during methylation. While both SEC methods can be recommended for PMAA, aqueous-phase SEC should be used for molar-mass analysis of PAA unless the sample is not branched.
Keyword Gel-permeation chromatography (GPC)
Kinetics (polym.)
Poly(acrylic acid)
Poly(methacrylic acid)
Radical polymerization
Q-Index Code C1
Q-Index Status Confirmed Code
Institutional Status UQ
Additional Notes Published online ahead of print 27 Oct 2014

Document type: Journal Article
Sub-type: Article (original research)
Collections: Official 2015 Collection
Centre for Nutrition and Food Sciences Publications
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