Instrumental Methods of Analysis of Sulfur Compounds in Synfuel Process Streams. Quarterly Technical Progress Report, October-December 1983

摘要

Task 1. Methods development for the speciation of the polysulfides. The contributions of this project to the electrochemical analysis of sulfides and polysulfides are reviewed and summarized. Electrochemical reduction at the dropping mercury electrode (DME) is the method of choice for the determination of polysulfidic sulfur. Total sulfidic sulfur can conveniently be quantitated in mixtures of sulfides and polysulfides, by measuring diffusion currents engendered by the anodic depolarization of the DME in the presence of the moieties HS exp - and S/sub x/ exp 2- . Task 2. Methods development for the speciation of dithionite and polythionates. In a solvent consisting of 40% ethanol-60% water, electrocapillary curves substantiated the adsorption of ethanol at the dropping mercury electrode. The potentials where adsorption occurred paralleled a shift of 1 volt in the polarographic half potential of the reaction: S sub 4 O sub 62- + 2e = 2S sub 2 O sub 32- . Task 3. Total accounting of the sulfur balance in representative samples of synfuel process streams. Two H-Coal liquefaction sour water samples were analyzed representing different stages in the PETC clean-up procedures. One specimen was a sample stripped of H sub 2 S and ammonia; the other, resulting from a different batch, was stripped and subsequently extracted with methyl isobutyl ketone. The stripped effluent contained less than 0.001 M concentrations of sulfide, polysulfide, thiosulfate, and sulfate. On the other hand, sulfate accounted for 90% of the total sulfur present in the stripped and extracted sample; the remainder consisted of sulfidic and polysulfidic sulfur as well as thiosulfate. 13 references, 2 figures, 3 tables. (ERA citation 09:015823)