We demonstrate here a novel oxidative process to control the metallic bismuth (Bi degrees) nanoparticles (NPs) formation in bismuth glass nanocomposites by using KClO4 and KNO3 as oxidant instead of usual reducing technique. The formation of Bi degrees NPs has been monitored by its distinctive surface plasmon resonance (SPR) band at 460 nm in the UV-vis absorption spectra. It is further confirmed by the TEM images of Bi degrees NPs using KNO3 and KClO4 which show the formation of spherical Bi degrees NPs of 2-15 nm sizes and the SAED pattern reveals their crystalline rhombohedral phase. Using this technique it is possible to control the SPR band of nanobismuth (Bi degrees) in bismuth glasses. (C) 2009 Elsevier B.V. All rights reserved.