Near-infrared spectroscopy was used to quantify the cure reaction of 4,4′-methylene- bis-(2,6-diethylaniline) (MDEA)–epoxy resins (E/A = 1.4) carried out at 72 and 160 °C. The absorption bands of the functional groups of interest in MDEA–epoxy resins are assigned according to the literature. A new assignment at 6580 cm−1 is also proposed for the secondary amine: it was supported by a synthesized model compound. Two different spectrum treatments were proposed. The first one is based only on a normalization at 4610–4620 cm−1, while the second one needs the subtraction of the normalized spectrum of a post-cure sample. To follow the curing process, amines and epoxy were studied at the same time in the combination and the overtone regions. The results are compared. In the combination region, quantitative results are obtained from absorbance measurements, while in the overtone region spectrum decompositions and area measurements are necessary. Complementary and reliable information are so obtained and allow us to calculate conversions of epoxide and amine I and concentrations in amine II, amine III, hydoxyl groups, and ether links. Kinetics are also established. The curing process mechanism is at last discussed for both curing temperatures.
