Zirconium and hafnium compounds are widely used in today's technology. Zirconium or hafnium carbides and borides are high temperature ceramics.The present study concerns primarily with optimizing the extraction of zirconium and hafnium from their naturally occurring mineral, zircon, via a wet chemical process. First , zircon heated with molten sodium hydroxide to form zironate and silicate frit. Simple separation technique of sodium silicate from the zirconate and hafnate sodium was then applied to obtain a silicate-free frit, then the extraction of the zirconium ( IV ) and hafnium ( IV ) basic sulfates from their oxychloride solution leaving almost all other ions soluble in the mother liquor was achieved by adjusting the pH value. The precipitate of zirconium ( IV ) and hafnium ( IV ) basic sulfates was dried, weighed, analyzed and percent of the zirconium and hafnium extracted were found to be 97 % of their original concentration.