The aqueous polymerization of pyrrole with varying FeCl3/Py mol ratio produces black insoluble powders. IR characterization reveals the shifting of the N-H stretching band to higher frequency with increasing FeCl3 amount in the feed composition due to lowering of intermolecular H-bonding. SEM shows a spongy texture of the polymer. TGA indicates the initial decomposition temperatures (180 degrees-237 degrees C) to be somewhat dependent on the FeCl3/Py feed ratio. DSC suggests the glass-transition temperature to be in the range 160-170 degrees C for the polymers prepared with various feed compositions. The conductivity is also dependent on the FeCl3/Py feed composition and levels off at a value of similar to 3 ohm(-1) cm(-1).