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A composite film of Nafion and MCFCNT whiskers was applied to a gold electrode surface to form a mechanically stable sensor. The sensor was then used for zinc detection in both acetate buffer solution and extracted bovine serum solution. A limit of detection of 53\u2005nM was achieved for a 120\u2005s deposition time. The zinc in bovine serum was extracted via a double extraction procedure using dithizone in chloroform as a zinc chelating ligand. 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