In this work, polypyrrole/clinoptilolite nanocomposite was synthesized by in situ surface polymerization of pyrrole using Fe3+ as oxidant, incorporated on the inner and outer surface of clinoptilolite nanoparticles. Formation of nanocomposite and deposition of polypyrrole on the clinoptilolite surface was confirmed and characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) patterns, scanning electron microscopy (SEM), and cyclic voltammetry techniques. Elemental analysis showed the loading/incorporation of 9.18 wt% polypyrrole in the clinoptilolite structure. However the electrical conductivity of polypyrrole/clinoptilolite nanocomposite pellets was higher than that of similar pure polypyrrole pellets, synthesized through the chemical oxidation polymerization method using Fe3+ as oxidant without the presence of clinoptilolite nanoparticles. Improved structural order or crystalinity of polypyrrole chains in nanocomposite structure which was confirmed by XRD and SEM results, may be the responsible of higher electrical conductivity of nanocomposite compared to pure polypyrrole although the low content (9.18 wt%) of polypyrrole in nanocomposite. Cyclic voltammetry studies showed that polypyrrole/clinoptilolite nanocomposite is electroactive similar to pure polypyrrole. POLYM. ENG. SCI., 2013. (c) 2012 Society of Plastics Engineers