Transmission electron microscope (TEM), ultraviolet-visible (UV/vis), electrospray mass spectrometric (ESMS), and X-ray photoelectron spectroscopic (XPS) studies are presented on a little studied rhenium hydrosol system produced by reduction of aqueous K2ReCl6 with hydrazine in the presence or absence of a gum arabic protecting agent. The studies indicate that hydrazine-generated "rhenium hydrosols" are unstable in water and slowly dissolve over time in aqueous media to form the highly stable perrhenate ion.