This article carries the objectives of our current acrylamide copolymer project further by examining the synthesis, characterization, and testing of a series of poly(methacrylamide-co-acrylamide)s and some homopolymer control products. These are characterized by traditional Fourier transform photoacoustic infrared, C-13 NMR, and elemental analysis. A composite picture of the hydrodynamic volumes of the high molecular weight products was then obtained by a series of viscometric, gel permeation chromatographic, and multiangle laser light scattering methods. These give a good quantitative picture of the effect of the introduction of the backbone methyl group on the hydrodynamic volumes of the copolymer products. Yields were generally greater than 60%. The copolymer products generally had lower molecular weights than those obtained from the control polyacrylamide preparations. Copolymer samples with comparable molecular weights did have larger radii of gyration and intrinsic viscosities than samples of control polyacrylamides.