Samples of YBa2Cu3O7−x were prepared by solid state reaction of Y2O3, BaO2, and CuO powders mixed in stoichiometric proportions. Powders reacted at 900°C-925°C in air were pressed at 35 MPa into rectangular bars and sintered at 950°C in air for six hours. Slow cooling at 50°C/hour promoted complete transformation to the orthorhombic structure. The effects of subsequent oxidation processing on superconducting properties were also investigated. Oxidation anneals at one atmosphere pressure in flowing O2over the temperature range from 300 to 550°C were performed. Results indicate that oxidation at 450°C optimized the superconducting transition temperature at 91K with a 2-degree transition width. Subsequent high-pressure oxidation (2000 psi O2) at 200°C for one week significantly degraded the superconducting characteristics. Results based on i udometric titration, thermogravimetric analysis, and x-ray photoelectron spectroscopy suggest that the copper valency is about 2.3 and oxygen stoi chiometry is 6.94 (x = 0.06) in samples processed to optimize superconducting properties.