A reduced graphene oxide layer was decorated with polypyrrole nanoparticles (PPy-NPs), and nanocomposite layers were deposited using the electro-chemical technique. The nanocomposite layer was used to detect pyrene using the surface plasmon resonance technique and the results were compared with the polypyrrole layer. The layers were characterized using a field emission scanning electron microscope (FE-SEM), Fourier transfer infrared spectroscopy (FT-IR) and X-Ray diffraction (XRD). Variations in shift of the resonance angle with time were registered to evaluate the sensing layers. It was found that the sensitivity of polypyrrole nanoparticles and reduced graphene oxide nanocomposite layer was higher than that of the polypyrrole layer. The limitation of the nanocomposite sensing layer was about 0.01 ppm which was larger than that of the polypyrrole sensing layer. Polycyclic aromatic hydrocarbons (PAHs) contains carbon and hydrogen and have several aromatic rings. 1 Pyrene (C 16 H 10 ), one of the best-known PAHs, contains four benzene rings. Pyrene can be found in the environment and in water, food and milk.2 Pyrene is used in producing dyes, and it has a high quantum yield, along lifetime, 3 and fluorescence emission in the range of 375-405 nm; 4,5 hence, pyrene also is used as a probe to recognize some biomolecules in the environment. The disadvantages of these methods are that they require special chemical knowledge and the equipment required is expensive. The surface plasmon resonance (SPR) sensor is a versatile instrument that is used for the detection of heavy metals, 17 biomolecules and toxic materials. 18 In order to enhance the sensitivity, selectivity, and accuracy of the SPR sensor, carefully chosen polymers films are used to modify the gold or silver layer. Hence, polypyrrole, 19 polypyrrolechitosan, 20 and polypyrrole/multi-walled carbon nanotubes 17 are used to improve the pertinent parameters of the SPR sensor.Conducting polymers such as polypyrrole, polypyrrole-chitosan, polyanilin, and polythiophene 21 have particularly optical and magnetic properties, thermal stability, high conductivity. 22 They have π-electron conjugation 23,24 which is responsible for electronic properties, low energy optical transition and high electron affinity. 25 Generally, the sensing mechanism of polypyrrole can involve the oxidation-reduction, chain conformational changes and ion or molecule adsorption and desorption which are considerable in surface plasmon sensor.26 Thus, they are useful as sensor and biosensors. Recently, polypyrrole nanoparticles have been fabricated to improve the chemical and physical properties of this polymer.27 z E-mail: suraya_ar@upm.edu.my Graphene oxide (GO) is derived from graphite by depicting covalent C-O bonds. GO is a two-dimensional material that has a single atomic layer. 28 It is soluble in organic and inorganic solutions such as alcohol and water. The hydroxyl (OH − ) and epoxy (-COO-) groups are the main functional groups in GO molecules at the basal plane and carboxyl groups (-CO...