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The synthesis and characterization of anhydorus Mg3(PO4)2 was investigated. Mg3(PO4)2 is reported to have similar structural arrangements with Co3(PO4)2 and g-Zn3(PO4)2 compounds. The sample was prepared by a new technique which is the reaction of MgCl2.6H2O and Na3PO4.12H2O solutions at pH=5.1, which was adjusted by adding concentrated H3PO4 to the reaction mixture and heating the precipitated product at 600\circC untill constant weight. The purity of the product was checked by X-ray powder diffraction, IR, density measurement, SEM and DTA analysis. The monoclinic unit cell dimensions of product are a=7.605 (2), b=8.233 (3), c=5.080 (1)A\circ and b= 94.19\circ (3), which was in good agreement with the reported data for Mg3(PO4)2. In the IR spectra, peaks due to PO4 anion of Td symmetry split because of the monoclinic crystal structure with the space group of P21/m. The SEM micrographs showed a spongy appearance with cavities. DTA analysis proved that anhydrous Mg3(PO4)2 is stable up to melting point which is 1184\circC.
