Nanocrystalline NdFeO3 perovskite oxide was prepared by the combustion method using polyvinyl alcohol (PVA) and corresponding metal nitrate precursors under optimum process conditions, using a solution with a pH of 2, a metal/PVA molar ratio of 1:3, and a calcination temperature of 600 degrees C, and was characterized by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, Brunauer-Emmett-Teller nitrogen adsorption and desorption, energy dispersive x-ray spectroscopy, Fourier transform infrared spectroscopy, laser Raman spectroscopy, and thermogravimetric and differential thermal analysis. The synthesized perovskite NdFeO3, which had an average size of 20 nm and a relatively high surface area of 20 m(2) g(-1), was investigated for adsorbing hazardous arsenate from aqueous solution. Arsenate adsorption by perovskite NdFeO3 is a pH-dependent process with a high adsorption capacity at pH levels between 4 and 7 and a maximum As(V) adsorption capacity of 126.58 mg g(-1), higher than most arsenate adsorbents reported in the literature. Kinetic and equilibrium data of reaction under the experimental conditions are best described by a pseudo-second-order and the Langmuir isotherm equation. The values of enthalpy, Gibbs free energy and entropy changes (Delta H-0 = + 63.916 kJ mol(-1), Delta G(0) = -6.551 kJ mol(-1) to -14.021 kJ mol(-1) at T = 283-313 K, Delta S-0 = + 0.249 kJ mol(-1) K-1) suggested that the reaction was endothermic, spontaneous, and took place with increasing entropy.