Morphology, spectroscopic properties and molecular structure defects are characterized and compared for two types of poly{[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylene]vinylene} (MEH-PPV) - Au nanoparticles (NPs) nanocomposites prepared by different procedures known for nanocomposites with other polymers: (a) nanocomposites M,prepared by mixing a dichloromethane (DCM) solution of MEH-PPV with Au nanoparticle organosol in DCM, and (b) nanocomposites R, prepared by the in situ reduction of Au3 salt with NaBH4 in the presence of polymer.