a b s t r a c tUniformly sized poly(N-isopropylacrylamide-co-acrylic acid) (NIPA/AA) hydrogel particles were synthesized in order to modify an electrode with a carboxyl group-immobilized one-particle layer. They were spheres with a common diameter under given conditions, which ranged from 0.5 lm to 1.0 lm depending on the pH, ionic concentration and temperature. They were swollen at low salt concentrations, low temperatures and high pH of aqueous suspensions. One particle contained 6.0 Â 10 8 carboxyl groups, the concentration of which was ca. 1 M, exhibiting pK a = 5.2. The particles were adsorbed spontaneously on the platinum surface in a one-particle layer with regular arrangement. The particle-adsorbed electrode showed the voltammetric peak for the reduction of hydrogen ions which were dissociated from the carboxylic groups of the adsorbed layer. The amount of the dissociated hydrogen ions per particle was 19% of the loaded amount of carboxyl groups, whereas the non-gelized particles had 3% of the loaded amount. The film worked as a source of supply of hydrogen ions for the electrochemical reduction of 1,4-naphthoquinone. It provided acidic environment of pH 4.5 for the reduction in the neutral solution.