Single crystals of pure and Cu+2,Fe+2 doped potassium sulfate were grown from aqueous solutions by the slow evaporation technique at room temperature. with dimension of (11x9 x4)mm3 and ( 10x 8x 5)mm3 for crystal doping with Cu &Fe respectively. The influence of doping on crystal growth and its structure revealed a change in their lattice parameters(a=7.479 Ã… ,b=10.079 Ã… ,c=5.772 Ã…)for pure and doping (a=9.687 Ã…, b=14.926 Ã… ,c= 9.125 Ã…) & (a=9.638 Ã… , b= 8.045 Ã… ,c=3.271 Ã…) for Cu & Fe respectively. Structure analysis of the grown crystals were obtained by X-Ray powder diffraction measurements. The diffraction patterns were analyzed by the Rietveld refinement method. Rietveld refinement plots for showing the experimental (red circles)calculated (black line) and difference profiles (blue line); green tick marks indicate reflection positions XRD measurements show the crystal system of orthorhombic.