A nickel-sodium triphosphate NiNa 3 P 3 O 10 ·12H 2 O already known has been prepared by the method of ion exchange resin of aqueous chemistry and studied by X-Ray diffraction, thermal analyses (TGA-DTA) and infrared spectrometry which show the characteristic bands of a triphosphate P 3 O 10 5-. The results of the compound heated at different temperatures showed that, after dehydration, NiNa 3 P 3 O 10 ·12H 2 O decomposes into an amorphous compound, then it crystallizes at 700 °C in order to give the new triphosphate NiNa 3 P 3 O 10 . NiNa 3 P 3 O 10 crystallizes in the hexagonal system, space group P -3 1 c, Z = 2 with the following unit-cell dimensions: a = b = 13.310 (5)