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Surfactants consisting of hydrophilic and fluorinated blocks are promising for drug delivery as these surfactants can solubilize otherwise immiscible fluorinated drugs in aqueous environments by reducing the surface tension of water. For this study, a series of hydrophilic-fluorinated block copolymers, comprised of poly(ethylene glycol) (PEG) and a semi-fluorocarbon block, is synthesized. The one pot, UV- light-mediated polymerization required only ppm concentrations of copper, simplifying the work-up. The reaction utilized a bromine functionalized poly(ethylene glycol) (PEG) chain as a macroinitiator from which different semi-fluorinated acrylates could be polymerized with near quantitative yields. These yields combined with simple deoxygenation of the reactants and the narrow dispersities obtained (Ɖ<1.10) prove the usefulness of this facile reaction for the synthesis of well-defined block copolymers. The synthesized polymers varied in PEG-macroinitiator length (1kDa, 2kDA and 5kDa), degree of polymerization (DP) of the fluorinated block (7, 13, 26 and 52) and the degree of fluorination of the fluorinated repeat units. Pendant drop tests demonstrated that both a decrease in the hydrophilic length and fluorinated block length and higher concentrations of amphiphilic block copolymer gave a greater drop in surface tension. The lowest surface tension (35 mN/m) was observed for the block copolymer consisting of 1kDA PEG and 7 repeat units of trifluoroethyl acrylate.