Instrumental Methods of Analysis of Sulfur Compounds in Synfuel Process Streams. Quarterly Technical Progress Report for April-June 1984

摘要

Task 1: methods development for the speciation of the polysulfides. Work on this task has been completed in December 1983 and reported accordingly in DOE/PC/40783-T13. Task 2: methods development for the speciation of dithionite and polythionates. Electrochemical reduction of tetrathionate and pentathionate at the dropping mercury electrode (DME) proceeds through a mechanism involving specific adsorption of the reactant at the DME surface and yielding polarographic waves at -0.2 volt (versus the saturated calomel electrode) in aqueous solution. Ethanol interferes with the specific adsorption of tetrathionate and pentathionate in a range of potentials between 0.0 and -1.1 volt, because EtOH is preferentially adsorbed. This results in a shift of the polarographic half-wave potentials of tetrathionate and pentathionate, which facilitates their determination in polythionate mixtures. On the other hand, the polarographic reduction of trithionate is unaffected by ethanol, because it occurs at -1.5 volt where ethanol is not adsorbed at the surface of the DME. Task 3: total accounting of the sulfur balance in representative samples of synfuel process streams. Analyses of two aqueous gasifier effluents from Grand Forks, ND, were performed. An untreated specimen contained sulfidic and polysulfidic sulfur, thiosulfate and thiocyanate. On the other hand, sulfite, sulfate, and thiocyanate were the only sulfur moieties observed in the Grand Forks sample which had been stripped at PETC. 7 references, 1 figure, 3 tables. (ERA citation 09:039367)