The thermal behavior of a series of poly(α-olefin-co-maleic anhydride) copolymers was studied by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Polymers with side-chain lengths of 16, 18, and 23 carbons were found to have crystallizable side chains. The melting point and heat of fusion of the side chains increased with increasing side-chain length. Glass transition temperatures were observed to be greater than the side-chain melting points. The molecular weight dependence of the Tg's obeyed the Fox-Flory relationship, with Tg∞= 129°C and k = 1.5 × 105. A spectroscopic method to monitor the extent of hydrolysis of the maleic anhydride units was developed, and the hydrodynamic volume in THF was observed to be dependent on the extent of hydrolysis.