Abstract
The precise estimation of the degree of derivatization of functional groups in polymers is important for determining their macroscopic properties. In this work, the quantitative estimation of the extent of esterification of novolac copolymers with di‐tert‐butyl dicarbonate was studied. Although the extent of esterification has been calculated previously by quantifying the signals from FT‐IR and UV–Vis spectroscopy, these were restricted to monitoring the progress of the derivatization process. The ^13^C NMR signal intensities from the inverse‐gated ^1^H‐decoupled NMR spectrum have been used recently for the quantitative estimation of the degree of esterification of polymers. An alternative methodology has been suggested by us based on the fully relaxed ^1^H chemical shift intensities. However, since the proton signals of novolac resins are generally broad and overlapping, the proton decoupled ^13^C NMR spectrum was used to identify the ^1^H NMR signals using the 2‐D HSQC technique. A TOCSY experiment was also performed to confirm further the ^1^H NMR sigal assignments and, finally, the deconvoluted ^1^H NMR spectrum was used for the calculation of the extent of derivatization. Copyright © 2003 John Wiley & Sons, Ltd.