高 S 含有鋼の真空溶融法による酸素分析

概要

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When high sulfur steels were analysed by the constant volume pressure measuring type vacuun fusion method, the sulfur gave positive errors on the determination of oxygen. The CS and CS_2 gases were generated by the reaction of sulfur and graphite crucible and then extracted together with CO from the crucible. These CS and CS_2 were oxidized by the oxidizing reagent in the system and CO_2 and SO_2 were generated, the volume becoming two or three times. Of the sulfide generation the lower limit of sulfur content was about 0.1% in ordinary samples. To prevent these errors, a circulating system containing a Liq. O_2 trap was newly set in the apparatus and with it the sulfides in extracted gases were separated. Thereby a good analytical precision (standard deviations were 3.7 ppm and 14 ppm for samples of 34 ppm and 135.5 ppm respectively.) was obtained on the determination of oxygen. The components of the evaporated-condensed film on the inner wall of reaction tube and the residual metals in the crucible were analysed and the reaction mechanisms of evaporation, deposition, adsorption, and reduction of extracted gases and metals were discussed.
社団法人日本鉄鋼協会の論文
1971-08-01