The solid-state reactions of Gd 2 O 3 with NH 4 H 2 PO 4 using various molar ratios (3:6, 2:8, 1:6 and 1:8) of the reactants were investigated at different temperatures (350-1100°C) to observe the intermediate compounds.Analysis of the X-ray powder diffraction patterns of the products obtained at 350°C; for the compositions of 2:8, 1:6 and 1:8 molar ratios revealed the formation of a new compound, NH 4 GdHP 3 O 10 which was reported previously for Nd, Ho and Er. At higher temperatures, gadolinium tripolyphosphate was obtained for all of the molar ratios. On the other hand, the IR data of the products also confirmed the proposed reaction pathways.