Nitroxide-Mediated Polymerization of N-Isopropylacrylamide: Electrospray Ionization Mass Spectrometry, Matrix-Assisted Laser Desorption Ionization Mass Spectrometry, and Multiple-Angle Laser Light Scattering Studies on Nitroxide-Terminated Poly-N-isopropylacrylamides

Nitroxide-mediated controlled living free radical polymerization of N-isopropylacrylamide using highly sterically hindered 2,2,6,6-tetraethylpiperidin-4-on-N-oxyl 1 is described. In addition, an improved synthesis for nitroxide 1 is presented. Poly-N-isopropylacrylamides (PNIPAMs) prepared are analy...

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Bibliographic Details
Published in:Macromolecules 2005-08, Vol.38 (16), p.6833-6840
Main Authors: Schulte, Tobias, Siegenthaler, Kai Oliver, Luftmann, Heinrich, Letzel, Matthias, Studer, Armido
Format: Article
Language:English
Subjects:
Applied sciences
Exact sciences and technology
Organic polymers
Physicochemistry of polymers
Polymerization
Preparation, kinetics, thermodynamics, mechanism and catalysts
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Summary:Nitroxide-mediated controlled living free radical polymerization of N-isopropylacrylamide using highly sterically hindered 2,2,6,6-tetraethylpiperidin-4-on-N-oxyl 1 is described. In addition, an improved synthesis for nitroxide 1 is presented. Poly-N-isopropylacrylamides (PNIPAMs) prepared are analyzed by multiple-angle laser light scattering. Moreover, the nitroxide-terminated PNIPAMs are characterized using electrospray ionization mass spectrometry, matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS), and Fourier transform ion cyclotron MALDI-MS. Careful MS analysis reveals that chain-end degradation of nitroxide-terminated PNIPAMs occurs during MALDI analysis. A mechanism for chain end degradation is presented.
ISSN:0024-9297
1520-5835
DOI:10.1021/ma050343n