Colloidal Unimolecular Polymer, CUP, particles were synthesized and characterized as a potential new and useful spheroidal polymer conformation for a variety of applications. Also known as single chain nanoparticles, these nanomaterials are gaining in popularity. The route to CUP particle formation is an innovative approach utilizing a small number of hydrophilic groups along a hydrophobic polymer backbone which transitions from a random coil conformation in organic solvent to a hard sphere in water through a slow gradient with subsequent solvent removal. The CUP particles have diameters which are proportional to their molecular weights and range typically from 3 nm to over 9 nm. These CUP particles were stable in water and free of solvent or surfactants. The sodium or potassium salts of CUP particles are spheroidal and are able to be dried then re-dissolved in water with no aggregation, unlike the original polymer. The diameters of the CUP particles correlate with the absolute number average molecular weight (M-n) and distributions from the GPC. Molecular weights from 28K to 122K are reported here and are based on an acrylic copolymer having a molar ratio of 9:1 MMA:MAA. (C) 2013 Elsevier Ltd. All rights reserved.