The kinetic behavior of Aniline (An) emulsion polymerization using ferric chloride (FeCl3) and ammonium persulfate (APS) as the composite oxidant, dodecylbenzene sulfonic acid (DBSA) as both emulsifier and dopant was discussed by the quartz crystal microbalance (QCM) technique, and the polymerization conditions were optimized tentatively by the cyclic voltammetry (CV) testing of the polyaniline (PAn). The experimental results indicated that the reaction exhibited first order to composite oxidant, half order to An and DBSA, there were three pairs of characteristic redox peaks in the CV, the peak currents and conductivity of PAn were the largest in the conditions: FeCl3 and APS molar ratio was two, the molar ratio of composite oxidant and An was three and the concentration of DBSA was 0.05 mol/L.