The solubility of the (NH 4 ) 2 C 2 O 4 −NH 4 VO 3 −H 2 O system has been measured over a temperature range from 313.15 to 363.15 K. On the basis of the results, a solubility diagram has been drawn. Additionally, the densities of the solutions have been measured. From analysis of the solubility data, a separation method for NH 4 VO 3 from the (NH 4 ) 2 C 2 O 4 −NH 4 VO 3 −H 2 O system was proposed, involving cooling and salting-out crystallization from (NH 4 ) 2 C 2 O 4 solution.