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  Home > JCE Print > Journal of Chemical Education > Issues > 2006  > March  >
In the Laboratory
Advanced Chemistry Classroom and Laboratory
Microwave-Induced Chain Transfer Polymerization of a Stimuli-Responsive Polymer and Determination of Its Critical Solution Temperature
F. Fischer
Institute of Chemical and Biological Process Science, Chemistry Section, Faculty of Basic Science, Swiss Federal Institute of Technology, Lausanne, Switzerland; Hochschule Wallis, Life Technologies Institute, Biotechnology Unit, Sion 2, Switzerland

R. Freitag
Institute of Chemical and Biological Process Science, Chemistry Section, Faculty of Basic Science, Swiss Federal Institute of Technology, Lausanne, Switzerland

Cover
March 2006
Vol. 83 No. 3
p. 447

Abstract
This experiment provides an introduction for undergraduate students to the concepts of living radical polymerization (oligomerization) and to stimuli-responsive materials, namely, those showing a critical solution temperature in aqueous solution. Students learn to polymerize and examine an intelligent polymer in a 8-hour, one-day laboratory period. The poly-N-isopropylacrylamide (PNIPAM) is a thermo-responsive polymer with a critical solution temperature (CST) of approximately 32 °C in pure water. Oligomeric PNIPAM (2000 g/mol) is telomerized with AIBN as initiator and 3-mercaptopropionic acid as chain transfer agent. The reactants are heated by microwave irradiation in a solvent-free process, employing a domestic microwave oven with 2.45 GHz magnetron frequency. The isolated telomer contains a single carboxylic function at one end of the polymer chain, allowing precise determination of the average molar mass by titration with NaOH solution and phenolphthalein as indicator. The CST phenomenon is easily detected by direct observation in daylight or by a temperature-programmed UV–vis spectrometer.
Supplement
Instructions for the students and notes for the instructor are available.
*  Contents JCE2006p0447W.doc (Microsoft Word)
*  Download
JCE2006p0447W.pdf

JCE2006p0447W.zip

More Information
*  Citation
Fischer, F.; Freitag, R. J. Chem. Educ. 2006 83 447.
*  Keywords
Addition Reactions; Free Radicals; Hands-On Learning / Manipulatives; Laboratory Instruction; Mass Spectrometry; Materials Science; NMR Spectroscopy; Polymer Chemistry; Polymerization; Upper-Division Undergraduate; UV-Vis Spectroscopy
*  History
Created:
Last Updated:
1/31/2006
2/9/2006
  Home > JCE Print > Journal of Chemical Education > Issues > 2006  > March  > Page 447


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