A composite optical waveguide sensor, consisting of lithium iron phosphate (LiFePO4, LFP) as the sensing material, was constructed and utilized for the detection of volatile organic compound gases. Nano-LFP powder was prepared via the hydrothermal method and was subsequently utilized in a dip-coating procedure for the fabrication of LFP thin films. The effect of heat treating temperature on the refractive index of the thin films was studied. A glass optical waveguide gas sensor was fabricated by coating an LFP thin film on the surface of single-mode tin-diffused glass optical waveguide. The sensor was found to exhibit a linear response to xylene in the range of 50-1000 ppm, with response times of less than 5 s. (C) 2012 Elsevier B. V. All rights reserved.