The synthesis of conjugated polymer materials using palladium catalysis was shown to result in a contamination of the polymer product with palladium nanoparticles that were difficult to detect and remove. The particle size was on the order of 20 nm, as evidenced by transmission electron microscopy (TEM). Further, electron spectroscopy for chemical analysis (ESCA), powder X-ray diffraction, and scanning electron microscopy (SEM) were employed to establish the chemical and physical nature of the catalyst remnants. We demonstrate the identity of many physical and chemical properties of the same polymer material prepared by two different routes: the palladium route and the condensation route. The performance in a device application of the two polymer materials was, however, very different, and the palladium route was demonstrated to give poor films with low breakdown voltages and short circuits.