Nanomaterials found to be potent catalyst for various applications in today’s era. The subtle Nanomaterials are the promising material in the field of catalysis. The nanomaterials are premordeal but their existence came into light with astonishing catalytical properties. The present research explains the synthesis of LaFeO3 doped by transition metals such Cr3+ and Co2+. These Nanomaterials are prepared by Sol-gel method followed by preparation of thick films and subsequent gas sensing by methanol. The nanoparticles were characterized by XRD, SEM, EDS and IR. XRD study reveals that the average particle size calculate by Scherer formula is 15.35 nm. The morphological properties and surface of nanomaterials can be imaged by SEM. The SEM investigation shows surface texture, colour and porosity of LaFeO3.It has homogeneous surface, microspores and mesopores as seen from its surface micrographs. EDS shows the elemental composition of every element in doped Pervoskite LaFeO3.The IR characterization shows the typical metal oxygen linkages for prepared nanomaterial. The characterized nanomaterials were subjected for investigation of methanol gas sensing properties by preparing thick films of doped LaFeO3.