Intercalation compounds of pyrene and 8-anilino-1-naphthalenesulfonic acid into MoS2 have been synthesized and characterized. This was achieved by using the exfoliation/re-stacking properties of LiMoS2. The degree of intercalation was found to be dependent on the amount of guest species used, the reaction time employed and the method of flocculation. The materials were also characterized by thermogravimetric analysis, four probe electrical conductivity measurements and fluorescence spectroscopy. (C) 2004 Kluwer Academic Publishers.