A complex Sol-Gel process has been used for synthesis of silica glasses designed to contain high-level nuclear wastes. Cs, Sr, Co, and Nd (generically denoted Me) were used, the last as surrogate for actinides. Gels in the form of powders and sintered compacts were prepared by hydrolysis and polycondensation of tetraethoxide/Me nitrate solutions, which contained ascorbic acid as a catalyst. Thermal treatment studies were conducted on the resulting gels. Transformation to final products was studied by thermogravimetric analysis, infrared spectroscopy, and X-ray diffraction. Preliminary testing of Me leaching was also completed in quiescent water. Only a single dense form was resistant to leaching