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UBC Theses and Dissertations

Analytical applications of X-Ray photoelectron spectroscopy Chan, Paul Ka-Hang


The surface-specific analytical technique of X-ray photoelectron spectroscopy (XPS) is described, and was used to study various geochemical materials and organic compounds. Variation of surface pyrite density with coal particle size (53-250/µm) in a typical Canadian coal (Minto) provided some interesting data- it is very likely that as coal is crushed, one eventually reaches a particle size where the surface pyrite/carbon ratio maximizes. It is this parameter that is examined here, and correlations were found between (i) surface pyrite concentration,(ii) surface pyrite/sulfate ratio, and (iii) oxidized and non-oxidized sulfur with particle size. This is information which should find useful application in coal cleaning technology. For non-oxidized coal, we find the area of exposed pyrite on the coal surface is approximately inversely proportional to coal particle radius. However, for oxidized coal the appearance of curves depends on the oxidation times, but there is a particle size which exhibits maximum surface pyrite relative to 1/radius, corresponding to the intercept point of the two linear segments (low and higher values of 1/R) for the non-oxidized coal (fig. 3.9), and which is evidently that we will call the "characteristic" size of constituent pyrite. XPS 2p₃/₂ sulfur peaks from major sulfur constituents other than sulfate in sediment recovered from Mahoney Lake (south-central British Columbia, Canada) show a surprisingly periodic variation in sulfur 2p₃/₂ binding energy (BE), and hence molecular structure, with sediment age. The pattern ceases at a core depth of about 3.2 meters, where a major deposit of fine sandy sediment occurs just below ash deposition (2.6m) from a major eruption of Mount Mazama, Oregon, approximately 6500 year ago, which led to the formation of Crater Lake. Sedimental sulfur exists mainly as sulfate; however, there is a pronounced increase in amount of the lower BE sulfur species relative to sulfate toward lower depths. The "reduced" species also shows a trend towards slightly higher oxidation level at lower depths. We are able to suggest the probable chemical forms in which the sulfur species exist, which is of interest to biologists working on sulfur transformation studies in lakes. BE' s for nitrogen Is and sulfur 2p₃/₂ in the metal chelates of dibenzyldithiocarbamic acid M(DBDTC)n for n=2, M=Cu(II) and Zn(II), and for n=3, M=Bi(III), have been measured. The nature of the spectral peaks and core BE's indicates that the nitrogen atom in the DBDTC is not intramolecularly bound with the metal as had been previously suggested. The relatively high BE's for the nitrogen Is orbitals indicate planar geometry for the coordinated ligands, and the form [formula omitted] to reasonably represent their structure, which agrees with previous infrared studies.

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