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In the present work the catalytic effect of copper (II) on the hydrogen peroxide-thiosulfate reaction was evaluated with capillary electrophoresis by in-capillary reaction methodology and kinetics of the initial stage was also investigated by changing reactants concentration,length of injection and voltage applied in separation.In the process,a mixture of hydrogen peroxide and copper ion,and thiosulfate were injected sequentially,reaction started upon the application of electric field.The optimized background electrolytes composed of 5 mM KH2PO4 and 5 mM (NH4)2SO4 adjusted with sulfuric acid to pH 5.0.Under the separation conditions applied,thiosulfate(S2O32-),dithionate(S2O62-),trithionate(S3O62-),tetrathionate(S4O62-),pentathionate(S5O62-) and hexathionate(S6O62-) were determined simultaneously after the in-capillary reaction with zone-passing technique of reactants.Kinetics of the reaction was first order with respect to concentration of every reactant,hydrogen peroxide,thiosulfate and copper (Ⅱ),with the rate constant k =3×108 M-3s-1,which was agree well with literatures that obtained from simulation works.Reactions occurred in the capillary and the performances of zone-passing technique were also discussed.