Heat-treatment is one of the ancient technologies used for the enhancement of the color in gem stone. Several reports are there by Achiwawanich et al. [9–11] in exploring the heat treatment of the ruby and sapphire stones under different atmosphere. This group also reported the removal of yellow patches and change in color of the ruby and sapphire using heat treatment. Also, some reports are there in the enhancement of the color, clarity and crack healing of the ruby stone through lead glass filling [12,13]. Jitwatcharakomolet al. [14] reported the sticking kinetics of the lead glass inside the ruby based on the optical characteristics.The density of ruby stones after the high temperature heat treatment with PbO remains unaltered. Thus, PbO is basically used for the pore filling and crack healing of the ruby stones [12]. Moreover,the ZnO and lead dioxide both are used as the glazing material [15]to improve the glaringness of the ceramic materials surface. Hence,a simple attempt is carried out to study the change in surface color and lustre of the natural ruby by heat treatment using both these oxides.Several researchers have been trying to improve the quality of gem ruby for its value addition. Although some investigations have been carried out to study optical properties of ruby, there are limited reports on a comparative study on the effect of two metal oxide treatments (PbO and ZnO) on the surface of the ruby. In this investigation an attempt has been made to improve the aesthetic value of ruby available in Nuapada district of Odisha through heat treatment with metal oxide additives. The treated samples are characterize dusing X-ray photo electron spectroscopy (XPS) for compositional analysis, X-ray diffraction (XRD) for structural analysis, photoluminescent (PL) for optical analysis and Raman spectroscopy for vibrational analysis, to study the typical surface behavior of the ruby stones before and after heat treatment. Based on the above observations, the surface behavior of ruby stones before and after the heat treatment have been compared and reported.