Coal liquefaction process streams characterization and evaluation: Investigation of the forms of sulfur in five Wilsonville resid samples by XAFS and moessbauer spectroscopy

摘要

This study demonstrated the feasibility of using XAFS and Moessbauer spectroscopy for the examination of distillation resid materials derived from direct coal liquefaction. The least-squares analysis of the XANES region of the K-shell XAFS spectra was shown to be technique which can be used to determine the sulfur forms in coal liquefaction-derived resid samples. The large amount of pyrrhotite in the resid samples (71 to 99% (plus minus)10% of the total sulfur) interfered with the precise quantitative analysis of the organic sulfur. However, a spectral subtraction routine was successfully used to provide semi-quantitative results for sulfur species other than the pyrrhotite. Moessbauer spectroscopy, considered a more accurate method than XAFS for the quantitative analysis of inorganic iron-sulfur species (pyrite, pyrrhotite, iron sulfates), was successfully used to speciate these materials in the coal liquefaction resids. Further application of XAFS and Moessbauer spectroscopy as process development tools appears justified by these results.