In this paper, we investigate the structural and magnetic properties of Ni based alloys which are in the form of NixFeyMoz (x = 0.80; y = 0.15; z = 0.05), NixCryFez (x = 0.70; y = 0.20; z = 0.10), and NixCryAlzCut (x = 0.75; y = 0.20; z = 0.025; t = 0.025) and are prepared by heating the pellet formed samples at high temperature. For this purpose, electron paramagnetic resonance experiment is performed for analysis of paramagnetic centers of these compositions to see the behaviours of alloys in an external magnetic field. g values are calculated from electron paramagnetic resonance spectra recorded at room temperature. Structural features of NixFeyMoz, NixCryFez and NixCryAlzCut alloys are observed by x-ray diffraction technique. Line positions and line intensities are discussed by the help of x-ray diffraction spectra recorded at room temperature. In order to understand the surface morphology of samples, scanning electron microscopy; for the elemental compositions of the alloys energy dispersive spectrosopy experiments are carried out at room temperature.