The synthesis of intermetallic Ni-Al nanoparticles by co-reduction approach of several organometallic precursors with sodium naphthelide in non-aqueous solution was studied. The state of the art in nanoparticles synthesisation is the selection of suitable precursors and the adaption of colloid chemistry to non-aqueous media at the room temperature under inert atmosphere. The reduction of an organometallic precursor, nickel (II) acetylacetonate, Ni(Acac) 2 as a source of Ni element of the intermetallic, and aluminum trichloride, AlCl 3 in tetrahydrofuran (THF) solution gave a black particles. The powder X-ray diffraction spectroscopy (pXRD) result shows an expansion of lattice parameter for FCC-Ni indicating the cooperation of Al atoms in Ni structures. The estimation value of Al concentration using Scherrer's equation is 10 at%. The particles were investigated in more detail by hard X-ray photoemission spectroscopy (HX-PES). The HX-PES spectrums confirmed that the black particles has binding energy consistent to standard materials of Ni 3Al. The absence of organic residues shown by the Fourier-transform infrared, FTIR spectrometer indicates that the as prepared Ni-Al nanoparticles are free from by-products.