The elucidation of the exact microstructure of polymers is always a challenging task. The range of molecular weights and uncontrolled polymerization leading to branching necessitates the development of better analytical methodologies. An improved methodology is presented for quantitatively estimating the microstructure of novolac resins and the percent incorporation of different monomers therein. An analysis is used that is based on the fully relaxed H-1-NMR spectrum in combination with the results of two-dimensional heteronuclear single quantum correlation, double quantum filtered correlation spectroscopy, and total correlation spectroscopy. (C) 2003 Wiley Periodicals, Inc.