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ÎÒµÄÂÛÎÄÉó¸åÒâ¼ûÖÐÓÐÕâôһÌõIn the Experimental Section, procedure for preparation of samples for XPS studies is to be described in more details. It seems that authors supported powders on double -sided scotch, which precludes any pretreatment of samples before spectra recording. In this case, the surface of samples is known to be hydroxylated, covered by carbonates and adsorbed CHx species trapped from air. Carbonates are also well known to be trapped in the bulk of high-surface-area ceria samples. Organic species trapped from air could reduce the surface even at room temperature especially during sample evacuation before measurements or under effect of the electron flood gun. All this makes difficult (if possible at all) reliable interpretation of XPS spectra in both O1s and Ce 3d ranges. Moreover, for sample studied after redox cycles, its inevitable transfer from reactor into the spectrometer through the air also affects its surface state even if it was reoxidized in the reactor before discharging (not mentioned, by the way). Hence, XPS data interpretation is certainly to be supported by experiments with sample supported on a metal holder which allows pretreatment in controlled conditions providing reproducible state of the surface.  If it is not possible for authors, I would advise just to remove this part of research from the article.
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Henderson reported a high-resolution electron energy loss spectroscopy (HREELS)-temperature-programmed desorption (TPD) study that oncluded that the adsorption of water on rutile (110) is molecular on the stoichiometric surface and dissociative on the reduced surface, which is conventionally produced by heat treatment, presumably forming oxygen defects.

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1Â¥: Originally posted by lkzmaster at 2010-10-15 10:21:14:
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