Single crystals of barium oxalate have been grown by gel method using agar-agar gel as media of growth at ambient temperature. The optimum conditions were established by varying various parameters such as concentration of gel, concentration of reactant, gel setting time etc. Prismatic platy shaped transparent crystals were obtained. The grown crystals were characterized through powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR) studies, Thermogravimetric (TGA) and Differential thermal analysis (DTA). The compound crystallizes under monoclinic structure with lattice parameters a = 6.6562 Å, b = 8.0464 Å, c = 2.8090 Å, β= 96.832°, and V = 149.38 Å
3. The FT-IR spectrum indicates OH and carbonyl group along with the presence of metal-oxygen bond. The TGA indicates 17.75% weight loss at 550°C from which the decomposition pattern is formulated.