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The aqueous polymerization of pyrrole and aniline by ferricyanide and persulfate, respectively, was monitored by Raman scattering and potentiometry. Raman scattering gave well-resolved signals for monomer and oxidizer. The kinetics of polypyrrole formation could be determined by both techniques, whereas only Raman scattering was suitable for the aniline system. The stoichiometry of the pyrrole polymerization remained constant at 2.5 oxidant molecules per pyrrole consumed. The aniline reaction showed an accelerated region with aniline consumption lagging persulfate use.