Zinc pyrovanadate was prepared at room temperature by using a new method, which consists of mixing zinc oxide powder, ZnO·0.3H ₂ O, with a 1.5×10 ^–3 M solution of vanadium oxide xerogel V ₂ O ₅ ·2H ₂ O. After a short time of stirring, the pH of the solution increases from 3.2 to 5.8 and a yellowish green precipitate was obtained. Although the reaction was not complete, the precipitate was composed mainly of zinc pyrovanadate. With prolonged stirring, a pure yellowish white zinc pyrovanadate was obtained while the pH of the solution, which stabilized around 5.6, was almost constant.