Optimizing the conditions of quantitative 13C-NMR spectroscopy analysis for phenol-formaldehyde resol resins

Abstract

The experimental time of 13C-NMR quantitative analysis of phenol-formaldehyde resins was reduced so that quantitativeness was maintained. The quantitative spectra of 14 model resins were obtained using a gated decoupling technique suppressing the NOE. The paramagnetic additive, Cr(acac)3, was used to shorten relaxation times of carbon atoms. The use of Cr(acac)3 was optimized in two deuterated solvents, DMSO and acetone. To reach short relaxation times and further the measurement times, the concentration of relaxation reagent, the delay time, and the number of NMR scans were optimized. Quantitativeness was proved by analyzing the spectra of accurate mixture of model compounds, and the spectra of the condensed model resins. © 1998 John Wiley & Sons, Inc.