In marine phosphate of şafağa, Egypt, tetravalent Uranium, U(IV) is found to be between 70 to 80 % of the total uranium. However, the phosphatic sandstone of Qatrani, Egy¬pt, is nearly devoıd of U(IV). As shown by autoradiographs, uranium is mainly concentrated in the carbonate Fluorapatite, Francolite or Collophane minerals. The U(IV) and U(VI) content of process solution samples during phosphoric acid produc- tion are obtained. Firstly by dissolving the samples by hydrochloric acid under normal conditi- ons. Secondary by dissolving the samples in an oxidizing atmosphere. The uranium concentra- tion is determined by fluorimetry. The achieved results are presented and found to be in good agreement with that obtained by tri-n-octylamine extraction and polar-ography