吸脱着還元を利用した金属中のイオウの吸光光度定量(ノート)

概要

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An adsorption-desorption-reduction spectrophotometric method for the determination of sulfur in metals has been developed. Sulfur dioxide formed after combustion of the sample in oxygen atmosphere is adsorbed on silica gel under the room temperature and desorbed to free by heating, and hydrogenated over a quartz catalyst to hydrogen sulfide, which is determined by methylene blue method. The combustion furnace was adjusted to 12001450°C (1200°C for copper base alloy, 1450°C for iron and nickel base alloys), the desorption furnace was adjusted to about 300°C and the hydrogenation furnace was adjusted to 800°C. The sample was burned in the combustion tube with a stream of 200 ml/min O2 gas for 8 minutes, and the sulfur dioxide produced was passed through a stainless tube filled with silica gel. After the oxygen in the apparatus was purged with N2 gas, the vessel containing 20 ml of the alkaline solution of zinc acetate as the hydrogen sulfide absorber was connected with the edge of the apparatus. The stainless tube was inserted into the desorption furnace and immediately passed with a stream of 200 ml/min H2 gas for 3 minutes. When the hydrogenation was complete, 3 ml of p-amino-dimethylaniline sulfate solution (0.1%) and 2 ml of ferric chloride solution(0.4%) were added to the vessel, and the sulfur was determined by the absorbance of 665 nm.
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