A water-in-oil (w/o) microemulsion containing high concentrations of ammonium ferric sulfate in solution was characterized by SAXS, EXAFS, electrical conductivity, and viscosity measurements and by its phase behavior. The nanometer-sized aqueous droplets are microemulsified by sodium bis(2-ethylhexyl) sulfosuccinate (AOT) in an isooctane continuous phase. Addition of small amounts of sodium dodecyl sulfate (SDS) as a cosurfactant greatly aids in the solubilization of the inorganic electrolyte-laden aqueous phase. For this five-component system there is a large region of the composition phase space that exists as a clear, stable w/o microemulsion. A portion of this w/o microemulsion phase space can be characterized as spherically shaped aqueous nanometer-sized droplets. A simple relationship between the total surfactant concentration and the amount of water on the droplet size was established. This relationship has the same form as the well-known relationship for the ternary system, AOT/water/isooctane. True thermodynamic equilibrium was not established in this microemulsion study because the reaction times for the various ferric oxyhydroxide species are prohibitively long. As a result, pseudoequilibria for this ammonium ferric sulfate microemulsion are reported. Because of the high concentration of inorganic electrolyte that can be dissolved in the microemulsion phase, these systems are useful for the synthesis of large quantities of nanophase particles.