Abstract: Nontronite and biotite were analyzed by Electron Spectroscopy for Chemical Analysis (ESCA). Both minerals yielded ESCA spectra with well-defined peaks and the elements identified by the ESCA spectra were in good agreement with the molecular formulas. High resolution scans were made of the iron (2p3/2) and oxygen (1s) electron binding energies for oxidized and reduced forms of nontronite and biotite. Binding energies for Fe3+ were observed at 711.8 eV in dithionite-reduced nontronite and in oxidized biotite. Peaks for Fe2+ occurred at 710.0 eV for unaltered biotite, at 709 eV for oxidized biotite and at 708.6 eV for hydrazine-reduced and dithionite-reduced nontronite. The oxygen (1s) peak for unaltered nontronite was skewed to the high energy side of the 530.6 eV maximum, but became more symmetrical as the Fe2+ content increased.