A method of controlling the size and morphology of polypyrrole nanoparticles (PPy-NPs) is successfully developed by using the combination of various non-ionic and anionic surfactants and polymerization temperatures during the synthesis. Uniform PPy-NPs are prepared via water-based redox heterogeneous polymerization of pyrrole in the presence of ammonium persulphate as an oxidant. The properties of the prepared materials are evaluated by a transmission electron microscopy and dynamic light scattering in terms of particles morphology, colloidal stability, zeta potential and hydrodynamic size and distribution. Raman, infrared and UV–Vis spectral characteristics of the particles are used to elucidate structural and optical properties of PPy-NPs. The size and morphology of polypyrrole nanoparticles prepared by a polymerization of pyrrole with ammonium persulphate can be controlled by various types and concentrations of surfactants with the hydrophilic-lipophilic balance values between 10‒16 and also by the polymerization temperature. Spectroscopic studies confirm that the surfactants can be washed out from the surface, although some residues remain enclosed inside particles matrix.