BACKGROUND: PLATINUM IS CONSIDERED AS THE BEST CATALYST FOR ethanol ELECTROOXIDATION IN DIRECT ethanol FUEL CELLS (DEFC) BUT ITS SURFACE IS RAPIDLY POISONED BY THE SPECIES FORMED DURING THE ethanol OXIDATION. THUS ADDITIONAL METAL SHOULD BE INVESTIGATED AS THE ANODIC CATALYST FOR DEFC. THEORETICAL INVESTIGATIONS HAVE INDICATED THAT THE SEGREGATION PROCESSES THAT LEAD TO PT SURFACE ENRICHMENT OCCUR IMPROBABLY IN THE PT–NI SYSTEM [1]. FURTHERMORE, NI FROM THE PT–NI ALLOY WOULD NOT DISSOLVE IN THE ELECTROLYTE IN THE POTENTIAL RANGE OF THE ALCOHOL ELECTROOXIDATION []. CHITOSAN HAS GREAT APPLICATIONS AS A SUPPORT FOR CATALYSTS. HERE, TO IMPROVE THE ELECTROCATALYTIC ACTIVITY OF PLATINUM, BOTH THE ADDITION OF ELEMENTS TO PLATINUM AND INCORPORATION OF METAL PARTICLES INTO POLYMER WERE STUDIED. PT-NI BI NANOCATALYSTS DISPERSED IN CHITOSAN WERE PREPARED FOR ELECTROOXIDATION OF ethanol AND THEIR ELECTROCHEMICAL ACTIVITY FOR ethanol OXIDATION WAS MEASURED BY CYCLIC VOLTAMMETRY AND CHRONOAMPEROMETRY.METHODS: TO PREPARE PT-NI-CHITOSAN NANOCOMPOSITES, A 25 ML METAL SALT AQUEOUS SOLUTION (1 M H2PTCL6 AND 0.04 M NICL2 OR A MIXTURE OF METAL SALTS AQUEOUS SOLUTION) WAS MIXED WITH 3 ML 1% (W/V) CHITOSAN, THE MIXTURE WAS STIRRED BY A ROTARY FOR 30 MIN, THEN AQUEOUS SOLUTION OF NABH4 WAS ADDED QUICKLY TO THE MIXTURE, AND STIRRED FOR 90 MIN. GC-PTNPS-CHITOSAN AND GC-PT-NINPS-CHITOSAN ELECTRODES WERE PREPARED AND ELECTROCHEMICAL INVESTIGATIONS WERE DONE WITH SAMA500 ELECTROANALYSER IN 1.07 M C2H5OH AND 0.125 M H2SO4 AQUEOUS SOLUTION.RESULTS: PT-NI-CHITOSAN NANOCOMPOSITES WERE CHARACTERIZED BY UV-VIS SPECTRA AND TEM IMAGES. FROM TEM IMAGES, THE PARTICLE SIZE OF THE PLATINUM RANGES FROM 2 TO 7 NM. THE ELECTROCHEMICAL ACTIVE SURFACE AREA OF GC-PT-NINPS-CHITOSAN ELECTRODE ESTIMATED BY CYCLIC VOLTAMMETRY WAS 219.98 M2G-1 PT. ELECTROCHEMICAL PROPERTIES OF THE ELECTRODES WERE INVESTIGATED BY CYCLIC VOLTAMMETRY. IT IS SHOWN THAT INVOLVEMENT OF NI SIGNIFICANTLY INCREASES THE ELECTRODE ACTIVITY. THE BEST RESULTS WERE OBTAINED WITH 1.07 M ethanol, 8 MM PT AND 0.33 MM NINPS.CONCLUSION: IN THIS PAPER, BI NANOCOMPOSITES OF PT-NI-CHITOSAN WERE SUCCESSFULLY SYNTHESIZED. THE CATALYTIC ACTIVITY OF GC/PT-NINPS-CHITOSAN ELECTRODES TOWARD ethanol OXIDATION WAS INVESTIGATED THROUGH CYCLIC VOLTAMMETRY AND CHRONOAMPEROMETRY. OUR RESULTS REVEALED THAT THE ELECTRODE PERFORMANCE FOR ethanol ELECTROOXIDATION CAN BE SIGNIFICANTLY IMPROVED BY ADDITION OF NI NANOPARTICLES INTO PT CATALYST AND USE OF A MORE POROUS MATRIX OF CHITOSAN. THIS IMPROVEMENT IS ASCRIBED TO THE OXYGENATED SPECIES IN THE VICINITY OF PT SITES PROVIDED BY NI NANOPARTICLES.