In the manufacturing method of hexafluorophosphate (MPF6: M=Li, Na, K, Rb, Cs, NH4, and Ag) of the present invention, at least a HxPOyFz aqueous solution, a hydrofluoric acid aqueous solution, and MF.r (HF) are used as raw materials (wherein, r≧0, 0≦x≦3, 0≦y≦4, and 0≦z≦6). According to the above description, a manufacturing method of hexafluorophosphate can be provided which is capable of manufacturing hexafluorophosphate (GPF6: G=Li, Na, K, Rb, Cs, NH4, and Ag) at a low cost in which the raw materials can be easily obtained, the control of the reaction is possible, and the workability is excellent.