合金鉄中の微量硫黄の光度定量

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  • Spectrophotometric Determination of Micro-Amount of Sulfur in Ferro-Alloys
  • ゴウキンテツ チュウ ノ ビリョウ イオウ ノ コウド テイリョウ

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Previously, the authors have conducted a fundamental investigation on the reduction distillation spectrophotometric method (methylene blue method) for the exact determination of micro-amounts of sulfur in iron and steel. In this work, the authors applied the method for the exact determination of micro-amounts of sulfur in various ferro-alloys-ferro-molybdenum, ferro-tungsten, ferro-chromium, ferro-titanium, ferro-manganese and ferro-vanadium. In the determination of a micro-amounts of sulfur in ferro-alloys by means of the combustion method, some difficulties such as incomplete combustion of samples or contamination of metallic oxides in the titration solution may take place, causing titration error and lack of reproducibility of the resulting value. In the reduction distillation spectrophotometric method presented in this reports, ferro-tungsten and ferro-titanium were dissolved in hydrofluoric acid and nitric acid using Platinum dish, while other ferro-alloys were dissolved in hydrochloric acid and nitric acid in the presence of potassium chlorate. Then the mixture of hydrogen iodide, hypophosphorous acid and hydrochloric acid was added to it to reduce the sulfuric acid to hydrogen sulfide. The hydrogen sulfide then was distilled and absorbed in alkaline cadmium chloride and precipitated as cadmium sulfide. Then methylene blue was formed by the reaction of sulfide ion, p-amino-dimethyl-aniline and ferric chloride and the sulfur content was determined by measuring the absorbance of methylene blue at 670 mμ. By this method Japan Iron and steel standard samples and actual samples were analysed. Standard deviation of the each value for the 0.005% sulfur content was less than 5%. This procedure does not require any special expensive apparatus and moreover it is not necessary to eliminate the main alloying elements. This process may be said therefore a simple and convenient one.

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