The chiroptical properties of electrochemically deposited emeraldine salt PAn(.)(+)-HCSA (HCSA) 10-camphorsulfonic acid) films have been found to vary markedly with the temperature employed during polymerization. The circular dichroism spectra of such films grown at > 40 degrees C are inverted compared to the spectra of analogous films deposited at temperatures <= 25 degrees C, indicating an inversion of conformation for the polyaniline chains. These observations are rationalized in terms of a temperature-induced interconversion between the two diastereomeric emeraldine salt products from the doping of the growing polyaniline chains by the chiral (+)-CSA-anion. The marked temperature dependence of the diastereoselectivity highlights the importance of employing a fixed temperature during the electrosynthesis of optically active polyanilines.