Structural and elemental investigations of isolated aquatic humic substances using X-ray photoelectron spectroscopy

Structural and elemental investigations of aquatic humic substances (HS) by means of X-ray photoelectron spectroscopy (XPS) are described. For that purpose small amounts (10-50 mu g) of dissolved reference HS, which were characterized within the German research program DFG-ROSIG, were dried as thin films on small pieces of a high-purity silicon wafer. The photoelectrons from such HS layers exhibited characteristic signals of carbon Cls, nitrogen N1s, oxygen O1s and sulfur S2s, which could be fitted by Gaussian curves and used for the quantification of various moieties of HS: carbon (C-C, C-O, C=O, O=C-O), oxygen (C-O, C=O), nitrogen (C-N, C-N+) and sulfur. Moreover, by adding up the element signals of the HS samples their elemental composition of C, O. N and S was assessed. A comparison of the data based on solution state NMR and conventional elementary analysis revealed a satisfactory accuracy with those obtained by XPS.