3025. SANDS, A. E., GRAFINS, M. A., WAINWRIGHT, H. W., AND WILSON, M. W. Determination of Low Concentrations of Hydrogen Sulfide in Gas by the Methylene-Blue Method. Bureau of Mines Rept. of Investigations 4547, 1949, 19 pp. Colorimetric method has been developed for determining traces of H2S in synthesis gas used in the Fischer-Tropsch process. The maximum concentration of S that can be tolerated to avoid poisoning of the catalyst is 0.1 grain per 100 cu. ft. The method is applicable not only to synthetic mixtures of CO-H2 but to coke-oven gas, carburetted water gas, and blue water gas. Mercaptans, CS2, and thiophene do not interfere with H2S determination. The preferred absorbent for H2 S is 2% zinc acetate solution. H2S is determined by the photoelectric or spectrophotometric measurement of the quantity of light absorbed by solutions of methylene blue produced by the reaction of H2S with p-aminodimethylaniline sulfate. Absorption measurements are made with a Klett-Summerson photoelectric colorimeter, employing a No. 66 filter, and with a Beckman spectrophotometer at a wavelength of 745 mμ. As little as 0.001 grain of S per 100 cu. ft. can be detected by means of this test, when the volume of gas sample is 1 cu. ft. When the gas contains 0.05 grain of S as H2S, only 1 per 10 cu. ft. of gas is required, and the result is obtained in less than 30 min. |