Quantitation of functionality of poly(methyl methacrylate) by liquid chromatography under critical conditions followed by evaporative light-scattering detection. Comparison with NMR and titration |
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Authors: | Peters R Mengerink Y Langereis S Frederix M Linssen H van Hest J van der Wal Sj |
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Institution: | DSM Research, Competence Center Molecular Identification & Quantification, Geleen, The Netherlands. RonPeters@dsm.com |
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Abstract: | Atom transfer radical polymerisation (ATRP) is a versatile 'living' controlled polymerisation technique for the synthesis of well-defined architectures such as block copolymers, gradient copolymers, hyperbranched polymers and telechelic polymers. ATRP provides control over molecular mass and molecular mass distribution and is suitable for the polymerisation of a wide variety of monomers, including methyl methacrylate. A chromatographic method was developed for an endgroup-based separation of low-molecular-mass poly(methyl methacrylate) (PMMA), based on liquid chromatography under critical conditions. With this method the PMMA, irrespective of its low-molecular-mass, is separated according to endgroups (functionality) due to interactions of the polar endgroups with the non-modified silica based stationary phase. The different series were identified using on-line atmospheric pressure ionisation electrospray mass spectrometry and quantified by evaporative light scattering detection. These results were compared with those obtained by NMR and titration. |
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