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Structure Determination of Cellulose Esters via Subsequent Functionalization and NMR Spectroscopy
Author(s) -
Liebert Tim,
Hussain Muhammad A.,
Heinze Thomas
Publication year - 2005
Publication title -
macromolecular symposia
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.257
H-Index - 76
eISSN - 1521-3900
pISSN - 1022-1360
DOI - 10.1002/masy.200550506
Subject(s) - cellulose , acylation , surface modification , nuclear magnetic resonance spectroscopy , transesterification , chemistry , spectroscopy , nmr spectra database , proton nmr , two dimensional nuclear magnetic resonance spectroscopy , polymer chemistry , organic chemistry , spectral line , stereochemistry , catalysis , physics , quantum mechanics , astronomy
New paths for the fast and reliable analysis of cellulose esters (CE) via subsequent functionalization and 1 H NMR spectroscopy were studied. Perpropionylation of the CE is an inexpensive and efficient method. For cellulose diacetates used as representative ester well resolved 1 H NMR spectra were obtained, which can be used for the calculation of the over all degree of substitution (DS) and the partial DS values at position 2, 3, and 6. No transesterification occurs during the subsequent acylation and a standard deviation of S 2 = 1.32 x 10 −4 was found for a series of experiments. In case of more complex ester structures especially with extended aliphatic moieties per‐4‐nitrobenzoylation need to be applied prior to NMR measurements. The spectra obtained can be completely assigned and applied for the calculation of DS values.