Size- and concentration-dependent of Rayleigh scattering properties of transparent TiO2 nanohybrid polymer have been systematically investigated. By utilizing the Rayleigh scattering technique, we can obtain the Rayleigh ratio of TiO2 nanohybrid polymer prepared with different concentrations of TiO2. We observed that these Rayleigh ratios are strongly dependent on the size and concentration of the nanoparticles. The larger the size and concentration of nanoparticles is, the larger the Rayleigh scattering is. Furthermore, this technique can be used to examine the saturation effect of Rayleigh scattering observed at high input power, and evaluate the size uniformity of nanoparticles in nanohybrid polymer.