X-Ray diffraction analysis (XRD) is a non-destructive technique that provides detailed information about the crystallographic structure, chemical composition, and physical properties of a material. It is based on the constructive interference of monochromatic X-rays and a crystalline sample. X-rays are shorter wavelength electromagnetic radiation that is generated when electrically charged particles with sufficient energy are deceleratedMgSO4.7H2O and ZnSO4.7H2O are considered as metal sulphate single crystals. It was grown by slow evaporation method of pure and mixed Mgϰ Zn(1-x) SO4 .7H2Owith aqueous solution. The grown crystals werecharacterized structurally by using XRD and confirm that the crystals belong to orthorhombic system with space group p2, p2, p21. The variation in lattice volume of the mixed crystals confirms the formation of binary system.FTIR spectral investigations the strong absorption band visible in below 1067cm-1range was attributed to the ν3SO4symmetric stretch. The bond peak observed 3120 to 3458 cm-1confirmed the presence of H2O molecules.