A purification process was developed for the first time for boron nitride (BN) nanotubes. BN nanotubes, prepared using a ball milling and annealing method, contain a high yield of nanotubes and a small amount of BN and metal catalyst particles. The metal particles can be dissolved in an HCl solution. Fine BN nanoparticles and thin layers were first converted to water soluble B2O3 via a partial oxidation treatment at 800 °C. The oxide particles and layers can then be dissolved in hot water. Thermogravimetric analysis has been used to determine an adequate oxidation temperature at which fine BN particles were oxidized.