These would be used to verify the results obtained by sequential chemical extraction and SEM-EDS for the substrate withdrawn from anaerobic constructed wetlands treating metal-laden wastewater. The main removal process would be precipitation of metal sulphides and their retention in the system.
I have no experience with XPS Spectroscopy, but I successfully used Raman microspectroscopy to verify results of sequential extraction. Using the Raman mirospectroscopy I was able to identify some newly formed (during sequential extraction procedure) phases. I think therefore that it should work also with your sulfides.
Best regards.
XPS might be useful for speciation of sulfur (see e.g. http://srdata.nist.gov/xps/EngElmSrchQuery.aspx?EType=PE&CSOpt=Retri_ex_dat&Elm=S), and also of metals, but it's absolutely surface technique (for Angstrom-sized surface layers); thus you don't get bulk information. Laser Raman is also applicable for micro-sized areas, unless you use an old Raman spectromete. However, in that case the spectral resolution is low. I think that the best way for solid-state speciation (bulk and micro-) is to contact a group in any of the European synchrotrons, through CALIPSO (http://www.calipso.wayforlight.eu/Sections.aspx?section=382.621) and try XANES/EXAFS. For metals would be easy to check oxidation states and spciation (using various references) but for sulfur could be more difficult. My colleague Dr. Goettlicher is experienced in sulfur, you could ask him about a potential collaborative project (http://www.anka.kit.edu/english/1352_1422.php).
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