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In the present paper, we present an electron magnetic resonance (EMR) study of <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><msub><mi>Ni</mi><mrow><mn>50.2</mn></mrow></msub><msub><mi>Mn</mi><mrow><mn>28.3</mn></mrow></msub><msub><mi>Ga</mi><mrow><mn>21.5</mn></mrow></msub></mrow></semantics></math></inline-formula> powders obtained from melt-spun ribbons in the milling process. We registered EMR spectra in various temperatures at the X-band. In the EMR spectra recorded for the samples taken at the beginning of the milling process, the “training effect” was observed. After 2 h of milling, this phenomenon was no longer observed. To determine the basic EMR parameters, such as linewidth, resonance field, and asymmetry parameters, the experimental data were fitted using a single metallic Lorentz line. In high-temperature regions, we observed the influence of dispersion on the shape of the spectra, but as the temperature decreased, the asymmetry of line was reduced. The shift in the resonance field value at high temperatures and the temperature dependence of the linewidth below Curie temperature indicate that the investigated samples exhibited a characteristics of a spin-glass alloy.