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A very careful X-ray diffraction (XRD) data collection and analysis is inherently important prior to further materials characterizations. More importantly when we deal with structural analysis, XRD is the best choice in terms of a simpler and easier approach as against other sophisticated instruments, like high-resolution transmission electron microscopy (HR-TEM) or small angle neutron scattering (SANS). Furthermore, the Scherrer equation provides an excellent feature to calculate the size of sub-micrometer crystallites or particles through the XRD pattern-s broadening peak. This present paper explores some analytical approaches to accurately extract the crystallografic structure and estimated particle size of magnetite (Fe3O4) and zincite (ZnO) nanoparticles which were prepared by simple coprecipitation approach. Single line analysis on the broadening XRD peak was computed with Lorentzian fitting to calculate the full width at half maximum (FWHM) for particle size calculation using Scherrer equation. Further full pattern XRD data analysis was executed by means of Rietveld method using Rietica and MAUD open-source softwares. From the refinement results, our analysis confirmed both softwares are powerful in determining the lattice parameters and particle size, even MAUD can plot the size distribution, and the results are in line with the HR-TEM and SANS data.