High-yielding low-cost vanadium oxide nanotubes were prepared by the hydrothermal self-assembling process from vanadium pentoxide and organic molecules as structure-directing templates. Moreover, a new method was discovered for determining the content of V (Ⅳ) in vanadium oxide nanotubes by thermogravimetric analysis ( TGA ). This method is simple, precise and feasible and can be extended to determine the content of low oxidation state in the other transition metal oxide nanomaterials.