Abstract: The investigation of a reversible reaction at disk microelectrode by deeonvolution voltammetry including semi-(e),1.5th(e′)and 2.5th(e″)differential voltammetry is presented. The peak shape of e-E curve is similar to the voltammgram obtained at conventional electrode.The relationship between the peak height of e,e′or e″and scan rate shows 0,5,1.5 and 2.5 order at disk microelectrode respectively,0.5 order lower than that at HMDE,The advantage of using microelectrode in deconvolution voltammetry is high sensitivity and selectivity,The behavior of a redox reaction at disk microelectrode by phase-selective AC voltammetry for the first and second harmonics is also described.

Key words: Microelectrode, Deconvolution, AC voltammetry