The synthesis of metallic nanoparticles using a reverse microemulsion medium brings controlled size and shape. In this study, reverse micelar system was employed for the synthesis of nickel hexacyanoferrate nanoparticles, NiHCF, by direct encapsulation in the water pools of reverse micelles formed in a pseudoternary system that consist of a mixture of 95 %wt. cetyltrimetyl ammonium bromide (CTAB) and 5 %wt. of a novel modified surfactant cetyltrimetyl ammonium ferrocyanate (CTA[Fe(CN6)]4-, CTAFe)/n-butanol/Hexane/Water. These NiHCF nanoparticles were produced with particle size ranging with 20 – 60 nm.