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X-Ray Photoemission Spectroscopy Analysis. X-ray photoemission spectroscopy (XPS or ESCA) is a surface analytical technique whereby electrons photoemitted from atomic core levels are detected as a function of energy. The shifts of core-level energies give information on the chemical environment of the atoms (oxidation state) and the surface (composition). Since this technique has been used to describe the electronic environment in a large number of transition metal complexes, an investigation using XPS seems appropriate for the study of charge distribution in oxygen-binding cobalt complexes and those same complexes immobilized on or in meso- and microporous solids. The reaction whereby these materials are formed is generally believed to be an oxidative addition wherein the cobalt ion is oxidized to a certain extent that is dependent on the electronic nature of a given cobalt(II) precursor. Burness et al. studied several O2- binding cobalt complexes in an effort to make correlations between cobalt core-electron binding energies and parameters such as reversible vs. irreversible behavior, and the differences, if any, between μ-peroxo and superoxo complexes.30 The authors presented unambiguous evidence that the cobalt(II) ion is oxidized during the oxygenation process, though the electron transfer from cobalt to dioxygen is likely not 100%. We have measured XPS spectra for CoCl2, Co2+ ion-exchanged X zeolite, free Co(fluomine), and Co(fluomine)-LSX. The Co(fluomine) sample was in an oxygenated state since heat is required in order to deoxygenate and the samples were not heated in the staging cell. The Co-LSX sample did not contain adsorbed oxygen since it is easily desorbed in high vacuum; and the Co(fluomine)-LSX sample, based on the adsorption and desorption isotherms (in Figure 5), should be partially oxygenated since it is not fully 169PDF Image | PSA USING SUPERIOR ADSORBENTS
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