Technical Abstract: Waxy maize starch was treated by a variety of gentle and severe methods: direct dispersion/solubilization into 90% DMSO-H2O solvent, extrusion followed by dispersion/solubilization of the ground exudate into solvent, or jet-cooking or stirred autoclaving of an aqueous starch slurry followed by transfer into solvent. Intrinsic viscosities and multi-angle light scattering measurements were made in 90% DMSO-H2O. A Mark-Houwink relation, [eta] = (0.28 to 1.2) Mw**0.29+/0.04, was obtained over a molecular weight range of about 30 to 700 million Daltons. However, there was a large amount of scatter in the data when intrinsic viscosities were greater than 140 mL/g. The following power law relationship: Rg alpha Mw**0.41+/0.04, was noted between radii of gyration and molecular weights. We infer from our data that over the entire range of molecular weight distributions the amylopectin existed in solution as relatively compact molecules/aggregates and that in the higher molecular weight region the size and possibly the shape of the "dissolved" amylopectin was highly sensitive to the method of dispersal and treatment.