This paper presents the study of structural and magnetic properties in the composition Gd 0.257-x Nd x Fe 0.743 where x = 0, 0.1285, 0.257 prepared by mechanical alloying in an argon atmosphere and with a milling time of 72 hours using a high energy planetary mill. The magnetic and structural characterization was performed by Mossbauer Spectroscopy (MS) and X-Ray diffraction (XRD), respectively. The three patterns show an intense peak corresponding to the α-Fe phase. Its intensity decreases as Gd is replaced by Nd showing the minimum intensity for x =0.257, and at the same time it shows a progressive increase in the peak’s width. These effects are attributed to the rich presence of Gd and/or Nd atoms in the iron sites. Mossbauer spectra were adjusted with hyperfine field distributions, sextets and singlets using the Mosfit program. The spectra show that by substituting the Gd with Nd atoms, the magnetic order is affected in such a way that iron sites appear and show magnetic disorder.