Quantitation of functionality of poly(methyl methacrylate) by liquid chromatography under critical conditions followed by evaporative light-scattering detection. Comparison with NMR and titration.
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.
Peters
R
R
DSM Research, Competence Center Molecular Identification & Quantification, Geleen, The Netherlands. RonPeters@dsm.com
Mengerink
Y
Y
Langereis
S
S
Frederix
M
M
Linssen
H
H
van Hest
J
J
van der Wal
Sj
S
D001274:Atmospheric Pressure; D002853:Chromatography, Liquid / Q000379:methods*; D008027:Light; D009682:Magnetic Resonance Spectroscopy; D019904:Polymethyl Methacrylate / Q000737:chemistry*; D012542:Scattering, Radiation; D021241:Spectrometry, Mass, Electrospray Ionization
D019904:Polymethyl Methacrylate