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Semi-quantitative analysis of the monomer composition in co-polymer microgels using solid state Raman and NMR spectroscopy

Semi-quantitative analysis of the monomer composition in co-polymer microgels using solid state Raman and NMR spectroscopy

Nur, H., Cornelius, V.J., Benée, L.S., Mitchell, J.C. ORCID: 0000-0003-2945-3292, Day, I.J. and Snowden, M.J. (2009) Semi-quantitative analysis of the monomer composition in co-polymer microgels using solid state Raman and NMR spectroscopy. Analyst, 134 (7). pp. 1366-1372. ISSN 0003-2654 (Print), 1364-5528 (Online) (doi:https://doi.org/10.1039/B816792C)

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Abstract

A series of colloidal microgels have been prepared by surfactant-free emulsion polymerisation (SFEP) based on the N-isopropylacrylamide (NIPAM) monomer. 4-Vinylpyridine (4-VP) and butylacrylate (BuA) have been used as co-monomers. Co-polymer poly(NIPAM/4-VP) and poly(NIPAM/BuA) have been prepared with various monomer ratios, ranging from pure poly(NIPAM) to pure poly(BuA)/poly(4-VP). Freeze-dried samples of the microgels have been analysed by solid state (ss) Raman and NMR (Nuclear Magnetic Resonance) spectroscopy to investigate the monomer composition in the co-polymer microgels. Spectral data have been analysed graphically and also statistically. Spectroscopic measurements have shown that co-polymerization has occurred. The graphical and statistical analysis of the spectroscopic data for both co-polymer microgels, enables the semi-quantitative measurement of the percentage incorporation of co-monomers (4-VP/BuA) in the co-polymer microgels. A good correlation exists between the Raman and NMR results, however, Raman spectroscopy is much less time consuming (Raman spectral acquisition time is less than 10 minutes) and the measurements are easy to make and very small quantities (less than 1 mg) of the sample are required. This compares with the experimental measurements of 72 hours and 100–200 mg of sample that are required for the NMR experiments.

Item Type: Article
Additional Information: [1] First published on the web: 21 Apr 2009. [2] First published in print: July 01 2009. [3] Published as: Semi-quantitative analysis of the monomer composition in co-polymer microgels using solid state Raman and NMR spectroscopy. H. Nur, V.J. Cornelius, L.S. Benée, J.C. Mitchell, I.J. Day and M.J. Snowden. Analyst, 2009, 134, 1366-1372. DOI: 10.1039/B816792C
Uncontrolled Keywords: monomer composition, co-polymer microgels, solid state Raman, NMR spectroscopy
Subjects: Q Science > QD Chemistry
Pre-2014 Departments: School of Science
Related URLs:
Last Modified: 14 Oct 2016 09:21
Selected for GREAT 2016: None
Selected for GREAT 2017: None
Selected for GREAT 2018: None
Selected for GREAT 2019: None
URI: http://gala.gre.ac.uk/id/eprint/8591

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