Quantitation of Carbon in Oil Shale Process Wastewaters: Coulometry Coupled with Ultraviolet-Peroxydisulfate and High-Temperature Oxidation

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Abstract
Wastewaters from the production of synfuels, in particular oil shale retort waters, present several major problems to various instrument configurations designed for carbon analysis. A carbon analyzer was fabricated from commercially available oxidation and detection units. Carbon oxidation occurred in an ultraviolet (UV) photochemical reactor using acid peroxydisulfate; quantitation of the evolved carbon dioxide was accomplished with an automatic coulometric titrator. This new design eliminated the problems of (1) instrument downtime caused by fouling of high-temperature combustion catalysts and corrosion of furnace combustion tubes, (2) limited linear dynamic range and upper detection limit (namely, infrared detection), and (3) frequent detector calibration (namely, infrared and flame ionization detection). The UV-persulfate/coulometric titration carbon analyzer was compared statistically with a high-temperature combustion system that is suitable for use with an ASTM method on the basis of (1) the accuracy and precision of recovery of total dissolved carbon (TDC) and dissolved organic carbon (DOC) for nitrogen heterocycles, which were of primary interest because of their preponderance in oil shale process waters and their reported resistance to certain oxidation methods, and (2) the precision of TDC and DOC determinations for nine oil shale process wastewaters. Several qualitative considerations are discussed for both analyzers, including ease of operation, instrument downtime, and maintenance costs.