Rare-earth, yttrium, and calcium doped zirconates are the materials of choice for electrolytes in solid oxide fuel cells. The dopant in these materials serves not only to stabilized the cubic phase of zirconia, but also to introduce anion defects that presumably increase the ionic conductivity. In order to understand the relationships between anion defect distribution, thermal history and ionic conductivity, the structural properties of gadolinium zirconate, Gd2Zr207, have been examined via high-temperature x-ray powder diffraction. Gadolinium zirconate is an ideal material for such a structure-property-processing study: it shows ordering of defects at low temperatures, taking on a pyrochlore structure, and disordering at elevated temperature, taking on a defect fluorite structure. Diffraction experiments, performed as functions of time and temperature, confirmed the transition temperature to lie between 1500 and 1550 °C. They also revealed that the transformation takes place most rapidly just below the transition temperature, indicating that the ordering process is kinetically constrained at low temperatures. Moreover, x-ray data collected at room temperature from quenched samples were found to be as useful, if not more so, than those collected in situ at high temperature. The latter are affected by thermal scattering, severely compromising data quality.