Polyaniline (PANI) and polypyrrole (PPy) doping with hydrochloric acid (HCl), p-toluenesulfonate (pTSA) were successfully synthesized by chemical oxidation polymerization. Ammonium peroxydisulfate was used as an oxidizing agent at room temperature. Microstructure of PPy and PANI was studied by scanning electron microscopy (SEM). Discussed the acid concentration how influenced on the electrical conductivity properties of PANI and PPy, and also compared their resistivity and thermal stability. The results showed that HCl effectively improved conductive properties of PANI in a wide range concentrations, and pTSA in narrow range concentrations. When doping with HCl, the minimum volume resistivity of PANI was 0.24 Ω • cm, and PPy was about 10.5 Ω • cm. When doping with pTSA, the volume resistivity minimum of PANI was 1.3 Ω • cm, and PPy was 15.8 Ω • cm. The conductivity of PPy was weaker than PANI. The thermal stability of conducting polymers which doping with pTSA was better than which doping with HCl.