Abstract: Primary beneficiation was successfully performed prior to dissolution of manganotantalite (sample A) and ferrotantalite (sample C) samples obtained from two different mines in the Naquissupa area, Mozambique. Magnetic separation removed the majority of iron and titanium, whereas H₂SO₄ leaching removed a large portion of thorium and uranium in these samples. Analytical results indicated that 64.14wt% and 72.04wt% of the total Fe and Ti, respectively, and ~2wt% each of Nb₂O₅ and Ta₂O₅ were removed from sample C (ferrotantalite) using the magnetic separation method, whereas only 9.64wt% and 8.66wt% of total Fe₂O₃ and TiO₂, respectively, and ~2wt% each of Nb₂O₅ and Ta₂O₅ were removed from sample A (manganotantalite). A temperature of 50°C and a leaching time of 3 h in the presence of concentrated H₂SO₄ were observed to be the most appropriate leaching conditions for removal of radioactive elements from the tantalite ores. The results obtained for sample A under these conditions indicated that 64.14wt% U₃O₈ and 60.77wt% ThO₂ were leached into the acidic solution, along with 4.45wt% and 0.99wt% of Nb₂O₅ and Ta₂O₅, respectively.