SEPARATION of ytrrium and dysprosium from the prepared chloride liquor of HREEs 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 xenotime bearing ferruginous sandstone (from southwestern Sinai) followed by precipitation as oxalates then dissolution in HCl. Treatment of the prepared REEs chloride with Na2CO3 was achieved under suitable conditions by the addition of H2O2 to the carbonate solution where Dy, Gd, Sm, and Yb are precipitated while Y & Er left behind in the filtrate. Extraction of 87.3% Dy from the produced precipitate was studied using Cyanex 272. The relevant conditions for extraction and stripping processes have been optimized. After acidification, 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.