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Instrumental methods of analysis of sulfur compounds in synfuel process streams. Quarterly technical progress report, April-June 1983. [Thermometric titration of polysulfides with Lewis acid p-hydroxymercuribenzoate; polarography of trithionate, tetrathionate and pentathionate]

Technical Report ·
OSTI ID:5826570

Task 1: Methods Development for the Speciation of Polysulfides. The contributions of this project in fundamental thermochemistry and thermodynamics of Lewis acid-base reactions are reviewed and summarized. The use of the reagent p-hydroxymercuribenzoate, p-HMB (/sup -/OOC phi Hg-OH), as a preferred analytical reagent for polysulfides is warranted on considerations of specificity, selectivity, and its monovalent coordination number. p-HMB is a Lewis acid-base adduct. The Lewis acidity of /sup -/OOC phi Hg/sup +/ measured as log K of a reaction with a given Lewis base was found to be 15% greater than that of the classical Lewis acid H/sub 3/CHg/sup +/. Task 2: Methods Development for the Speciation of Dithionite and Polythionates. A new electroanalytical method has been developed for the speciation of trithionate, tetrathionate, and pentathionate. Five well-resolved differential pulse polarographic peaks were obtained at the dropping mercury electrode in a mixed solvent (60% water, 40% ethanol) containing trithionate, tetrathionate, and pentathionate at comparable concentration levels. Two peaks were accounted for by the electroreduction of trithionate and tetrathionate, respectively. Pentathionate yielded three peaks. Trithionate, tetrathionate and pentathionate concentrations were linearly correlated to selected differential peak currents. Task 3: Total Accounting of the Sulfur Balance in Representative Samples of Synfuel Process Streams. Analyses of two aqueous specimens, a gasification effluent from Grand Forks, ND, and an H-Coal liquefaction process effluent were carried out. The liquefaction effluent contained predominantly hydrogen sulfide and no thiosulfate. A variety of sulfur species were observed in the gasification effluent, including thiocyanate. 9 references, 11 figures, 5 tables.

Research Organization:
Pennsylvania State Univ., University Park (USA). Dept. of Chemistry
DOE Contract Number:
FG22-81PC40783
OSTI ID:
5826570
Report Number(s):
DOE/PC/40783-T11; ON: DE83016803
Country of Publication:
United States
Language:
English