Surface analysis is one area stressed in the Pimentel Report Opportunities in Chemistry (1). The ultra-high vacuum surface sensitive technique that is generally considered to provide the most chemical information is X-ray photoelectron spectroscopy (XPS). XPS is routinely finding application in such diverse areas as heterogeneous catalysis (2, 3), semiconductor materials (4,5), polymers (6-8), thin films (5,9), chemisorption (70, 11), etc. The diverse areas of application ensure that the professional chemist will have occasion to employ surface analysis techniques such as XPS or need to know their basic principles in their specific areas of interest. In an attempt to provide an opportunity for the undergraduate student to apply XPS to a typical analytical problem, we developed a simple variable-angle XPS experiment designed to measure the thickness of the oxide layer on aluminum metal for use in the Methods of Chemical Investigation course. Methods is an integrated, two-semester, lecture/laboratory sequence generally taken by seniors in the ACS-certified BS curriculum at the University of South Florida. Background X-ray photoelectron spectroscopy is concerned with the measurement of core-electron binding energies (12). A molecule or atom is bombarded with an X-ray of sufficient energy to eject an electron. The kinetic energies of the photoelectrons are then measured by an electron analyzer. The coreelectron binding energies (E\,) relative to the Fermi level can then be compared via the simple relationship E^E'-Ey-W, (1) where Fx is the energy of the exciting X-ray, is the electron kinetic energy, and IT'] is the spectrometer work function, a constant for a given analyzer.The utility of XPS for the chemist is the result of "chemical shifts" that are observed in Ey,. The binding energy of a core electron is affected by the atom's electron density and, thereby, by the oxidation state and/or the chemical environment of the atom. As the oxidation state becomes more