Uranium as a nuclear element with strategic importance and gold as one of the important economic precious metals made their selective leaching from the sedimentary lower carbonaceous sandstone rocks, Southwestern Sinai, Egypt with economic concentrations (5ppm gold and 160 ppm uranium), an important issue for facilitating either their accurate determination or highest percentage recovery. A sequential leaching of uranium followed by gold was proposed in this work after studying individually their optimized leaching conditions. From the latter; a lixiviant mixture of sample to sodium carbonate ratio 1:1, sample to sodium bicarbonate ratio 1:1 together with sodium thiosulphate, as oxidant, 0.5g was used for the selective leaching of uranium. On the other hand, a leaching reagent mixture of 5% (w/v) from each of potassium cyanide, sodium thiosulphate and 10 ml from 30% hydrogen peroxide was used for the selective leaching of gold where several factors were optimized; concentration of individual component in each lixiviant, agitation time, solid to liquid ratio, temperature and pH. A percentage leaching of 97% and 96% for uranium and gold respectively were reached. Uranium was selectively separated using Amberlite IRA 402 Cl resin ion exchange resin with 99.5 % percentage recovery. The recovery of gold needs a large bulk weight from the sample due to its relatively low concentration.