Samples of Nylon-6,6 were analyzed by 1-D and 2-D NMR techniques to determine the degradation structures resulting from UV exposure of Nylon films and heat aging of Nylon pellets. The dominant degradation structure in all cases was the terminal methyl group which was attributed to chain scission reactions. Further evidence for chain scission was found through the presence of aldehyde and formamide structures upon UV exposure and heat aging (in the presence of air) and terminal vinyl structures upon UV exposure. The presence of oxygen during UV exposure resulted in OH substitution adjacent to the amide group and at the end of a cleaved alkyl chain. Terminal amide groups were observed in the starting material and did not increase in concentration upon heat aging or UV exposure. In heat-aged samples, no evidence was found for olefinic or hydroxyl-containing structures in nitrogen, but hydroxyl structures were observed. A degradation mechanism was proposed to account for the structures observed in our work.