Polyaniline was synthesized by the chemical oxidative polymerization procedure at room temperature employing hydrogen peroxide (H 2 O 2 ) as oxidant and ferrous chloride (FeCl 2 Á2H 2 O) and vanadyl sulphate (VOSO 4 ÁH 2 O) as co-catalysts, respectively. The obtained polymers were characterized by high resolution powder X-ray diffraction, Fourier transform infrared spectroscopy, Raman, UV-Visible, photoluminescence spectroscopy, thermogravimetric Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM) techniques. Ordered arrangement indicative of semi-crystalline nature of polyaniline was evidenced from the presence of intense reflection at d ¼ 13.72 Å in the powder X-ray diffraction pattern followed by two lesser intense peaks at 4.61 and 3.47 Å . Fourier transform infrared spectroscopy and Raman spectroscopic results indicated the polyaniline to be emeraldine salt form. Fibrous morphology was observed in scanning electron microscope images. Nearly 93% of Methyl Orange dye was adsorbed in 30 min by the ordered polyaniline at room temperature. No significant difference in the crystallinity and/or ordering was noticed in the powder X-ray diffraction pattern after dye adsorption. The correlation between the ordered structure of polyaniline and its higher adsorption property derived in the current study has the potential to fabricate devices consisting polyaniline to detect dye molecules.