Due to stringent environmental norms, a lot of research is going on to reduce exhaust emissions coming out from diesel engines. Diesel microemulsion is one of those alternate techniques. In fuel microemulsion, microexplosion triggers complete combustion of all the components and thus, high reduction in hazardous gases from diesel engines. The main focus of this research is to formulate and characterize diesel-based reverse micellar microemulsion. In a blend of two non-ionic surfactants, hydrophilic surfactant dominates the effect of lipophilic surfactant. The interfacial composition of fuel microemulsion was also investigated by Schulman’s method of co-surfactant titration. During the investigation of the effect of chain length of co-surfactants, it was found that the efficiency of microemulsion increases with increasing chain length of co-surfactants. The chain structure of surfactant and co-surfactant also plays a paramount role in microemulsion formulation. The fuel properties like viscosity, cloud and pour points also get affected by chain length and structure of co-surfactants.