Effect of the synthesis conditions of Pechini technique on crystallinity and purity of Na3Ce(PO4)2 compound was investigated. Nano-sized cerium-sodium phosphate obtained when EDTA was used as an additional chelating agent
for Ln3+. The total enthalpy change of Na3Ce(PO4)2 phase transition was determined as 14.2±0.7 kJ mol−1 for sample synthesized by conventional solid-solid reaction. The phase transition process was confirmed to occur at 1060°C
or in temperature range 920–1060°C depending on thermal treatment of powders.