A new styryl-type monomer, 2-(4-vinylbenzyloxy)-1naphthaldehyde thiosemicarbazone (VNT), was synthesized and then copolymerized with methyl methacrylate (MMA) by reversible addition fragmentation chain transfer polymerization affording a series of poly(MMA-co-VNT)s with different functional unit content, predetermined molecular weight, and narrow molecular-weight distribution. The desired copolymers were structurally confirmed by various spectroscopic characterizations. Colorimetric and fluorescent titration spectra revealed that the copolymers are highly selective toward fluoride anions over other competitive species including Cl À , Br À , I À , H 2 PO 4 À , AcO À , and HSO 4 À