The objective of the research is to obtain a more complete understanding of how aging affects the viscoelastic properties of polymer solutions to be used as starting materials for gel spinning of polymer fibers. Specifically, poly(acrylonitrile-co-methacrylic acid) solutions were prepared and characterized using rheological measurements and nuclear magnetic resonance spectroscopy. The results indicate that elastic character increased with increasing polymer concentration and that gelation of these solutions continued up to aging times of several weeks. Additionally, comparing the results from the two characterization methods show that while gelation continues to occur, the viscoelastic properties decrease after a critical time point suggesting that a chemical change occurs in the solutions at long times. However, these changes impact the solution dynamics minimally as the effective network properties were similar at the aging times studied here, but considerations for long-term storage of polymer solutions for gel spinning are warranted. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014, 131, 39821.