We have synthesized a poly(p-phenylene vinylene) (PPV) derivative bearing nonyloxy side groups via two different precursor routes: "the sulphinyl precursor route" and "the dithiocarbamate route", both developed within our research group. The conversion process, in which the soluble precursor is transformed into the insoluble conjugated polymer, is examined by means of several spectroscopic techniques like in situ UV-VIS, in situ FTIR, TGA and DIP-MS. By post-heat treatment, the conjugated polymer shows additional structural ordering. This specificity was studied by X-ray Diffraction Spectroscopy (XRD). (c) 2005 Elsevier B.V. All rights reserved.