The present invention provides a method enabling the high purification of a niobium compound and/or tantalum compound in a simplified manner at a low cost. This is accomplished by providing a method enabling the high purification of a niobium compound and/or tantalum compound comprising the steps of preparing a solution containing niobium and/or tantalum, allowing a precipitate comprising niobium and/or tantalum to develop, separating the precipitate by filtration from the filtrate, converting the precipitate to a liquid melt or taking the filtrate, and separating a niobium compound from a tantalum compound or vice versa by utilizing the difference in solubility to the solvent between the niobium compound and the tantalum compound.