Abstract A novel method for the study of non-oxidative methane conversion process into higher value hydrocarbon and hydrogen has been invented. The method involves the multiphoton dissociation of methane under the influence of the high power pulsed ultraviolet laser radiation at 355 nm wavelength at room temperature (293 K) and standard pressure (1 atm). The products generated as a result of methane conversion like ethane, ethylene, propane, propylene and isobutane are analyzed using an online gas chromatograph while the other species such as CH, CH 2 and C 2H 2, atomic and molecular hydrogen are characterized by real-time laser-induced fluorescence technique for the first time. A typical 7% conversion of methane into ethane has been achieved using 80 mJ of laser irradiation at 355 nm. The important features of this method are that it is non-oxidative, does not require any catalyst, high temperatures or pressures, which is normally the case in conventional techniques for methane conversion.