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Ta2O5 nanoparticles have been synthesized from alkoxy carboxylates of tantalum via the sol–gel route. Tantalum alkoxides were reacted with chlorocarboxylic acids in order to lower the susceptibility hydrolysis. When these modified alkoxy carboxylates were used in the sol–gel synthesis, they yielded Ta2O5 nanoparticles of better properties than those of the alkoxide-derived Ta2O5 nanoparticles. These nanoparticles efficiently removed rhodamine B under UV light irradiation.