Studies of surface tension, adsorption parameters, and dynamic surface tension were performed on a series of bolaamphiphilic α,ω-(diammonium disulfato)poly(fluorooxetane)s of several perfluoroalkyl chain lengths. Similar measurements were performed on a small-molecule, anionic fluorosurfactant with a −C8F17 perfluoroalkyl group that is known to be an effective flow and leveling aid in aqueous coatings. Molecular area demands for the poly(fluorooxetane)s were found to be relatively small for a polymeric species and may indicate a change in conformation between bulk solution and interface. Other adsorption parameters were found to be similar to those of the small-molecule fluorosurfactant. Diffusion coefficients were found to be slightly smaller for the poly(fluorooxetane)s compared to the small-molecule fluorosurfactant.