Separation of ytrrium and dysprosium from the prepared chloride liquor of REEs concentrate (44.1% Y, 9.04% Dy, 5.15% Er, 4.56% Gd, 2.31% Yb, 1.33%Ho and 1.23% Sm) has been studied. The concentrate was obtained by the sulfatizing roasting of the xenotime bearing ferruginous sandstone (from southwestern Sinai) followed by precipitation as oxalates and dissolution in HCl. Treatment of the prepared REEs chloride with Na2CO3 was achieved under optimum conditions. By addition of H2O2 to carbonate solution, Dy, Gd, Sm and Yb are precipitated while Y and Er left behind in the filtrate. Extraction of 87.3% Dy from the produced precipitate was studied using Cyanex 272. The relevant conditions for the extraction and stripping processes have been optimized. After acidified, Y in the filtrate and Dy in the stripping solution are precipitated as oxalates. Pure products of Y2O3 and Dy2O3 have been prepared and subjected to different analyses.