Synthesis of GeS2 via a sol-gel process using germanium ethoxide and hydrogen sulfide in toluene resulted in a gel aggregate with an apparent Ge/S ratio 1:1.8. Special precautions were necessary to protect the reaction mixture from water contamination which produced GeO2. Results indicated that the main source of water was the hydrogen sulfide gas. Heat treatment of the produced GeSx gel yielded a product with Ge/S ratio 1:2.3. The sol-gel prepared materials and their heat-treated products were characterized by various methods.