Polymer Molecular Weight Analysis by 1H NMR Spectroscopy
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Date
2011
Authors
Izunobi, J. U.
Higginbotham, C. L.
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Abstract
The measurement and analysis of molecular weight and molecular weight distribution remain matters of fundamental importance for the characterization and physical properties of polymers. Gel permeation chromatography (GPC) is the most routinely used method for the molecular weight determination of polymers whereas matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a fast-emerging absolute, and therefore accurate, technique. Although NMR spectroscopy is one of the most powerful tools available for polymer microstructure characterization, among others, its utility in the molecular weight analysis of polymers is somewhat under appreciated. It is a reliable and more readily available teaching tool in comparison to other known techniques, such as GPC and MALDI-TOF MS, for the molecular weight determination of polymers. Demonstrated herein are the simplicity, reproducibility, and
convenience of 1H NMR spectroscopy in the analysis of polymer number-average molecular weight (Mn), using alpha-methoxy-ω-aminopolyethylene glycol (MPEG-NH2) and alpha-methoxy-polyethylene glycol-block-poly-ε-(benzyloxycarbonyl)-L-lysine (MPEG-b-PLL(Z)) as model homopolymer and block copolymer, respectively. The molecular weight data from 1H NMR analysis are compared to those from GPC and MALDI-TOFMS.
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Keywords
Graduate Education/Research, Upper-Division Undergraduate, Polymer Chemistry, Inquiry-Based/Discovery Learning, Problem Solving/Decision Making, Chromatography, Mass Spectrometry, NMR Spectroscopy
Citation
J. Chem. Educ. 2011, 88, 1098–1104