This work describes two methods of preparation of hydrous tantalum phosphates and their characterization as ion exchangers. The hydrous metallic phosphate compounds were chemically and physically characterized by thermal gravimetric analysis, X-ray diffractometry and surface area measurements. By the first method, tantalum phosphate was prepared by alkaline fusion of Ta2O5 with an excess of K2CO3, followed by lixiviation of the tantalate fusion product with hot water, and precipitation with diluted H3PO4. Preparation II was performed using metallic Ta dissolved in concentrated HF/HNO3 acidic mixture followed by hydrolysis of fluortantalic acid intermediary and precipitation with diluted H3PO4. Both freshly prepared materials (I and II) were exaustively refluxed with concentrated H3PO4, in its boiling point temperature, resulting respectively in Ta2O5. 2.1 H2O, (IR) and Ta2O5. 1.3 H2O, (IIR). Characterization of the prepared products have presented the following values: surface area of 108.27 ± 2.80; 220.14 ± 2.67; 117.07 ± 5.25 and 141.61 ± 0.27 m².g-1 respectively for I, IR, II and IIR. All these materials were amorphous. The ion exchange behavior for all four hydrous tantalum phosphates was studied using Na+, K+ and Ba+2 as the exchanged species. The values for typical ion exchange capacity were 1.64; 1.23; 1.47 and 1.01 miliequivalent.g-1, respectively for I, IR, II and IIR products.