Oxide-based ceramic matrix composites (CMCs) are prime candidates for high temperature turbine applications. Increasing demand of CMCs necessitates the development of quality monitoring procedures. Sol-gel derived Nextel-720 fiber/alumina matrix CMC is one of the potential candidate material for land-based gas turbine applications. X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) were utilized to investigate any surface/interface chemical alteration of the Nextel-720 fiber reinforcement and the alumina matrix during fabrication. The calculated XPS spectra of the composite were obtained by simply adding the spectra of the as-received Nextel-720 fiber and the alumina matrix. The calculated XPS spectra and the acquired XPS Al(2p), Si(2p(3)), and O(1s) spectra from the as-received materials were compared using a superimposition method to investigate any chemical alteration during composite fabrication for quality control measures. This paper is aimed to serve as a reference for future XPS studies of CMCs exposed to aggressive turbine environments. (C) 2002 Elsevier Science B.V. All rights reserved.