Solutions of poly(p‐phenylene terephthalamide) in fuming sulfuric acid were characterized by 13C NMR spectroscopy and solution viscosity measurements over the 2–28% w/w concentration range. The spectra showed the presence of two distinct amide carbonyl resonances at low concentration, tentatively assigned to cis and trans conformations. As the concentration increased, additional carbonyl lines were observed along with significant broadening. Peak area measurements showed that only the polymer molecules in the isotropic environments contributed to the 13C NMR spectra and a considerable amount of the polymer remained in the isotropic phase at concentrations previously considered to consist of polymer in highly anisotropic regions. Spin‐lattice relaxation times were measured at six concentrations using the inversion recovery method. The aromatic carbons relaxed at a much faster rate (ca. 0.10 s) than the carbonyls (ca. 0.45 s), but the relaxation rates for both carbons were essentially constant over the concentration range, indicating that the observed isotropic phase is not affected by changes in the macroscopic solution behavior so as to alter spin‐lattice relaxation mechanisms.
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