鋼中マンガン自動吸光光度分析法

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As a series of studies on automatic chemical analysis of steel, an automatic spectrophotometric method for determination of manganese has been developed using the automatic analyzer that the present authors have previously reported for determination of acid-soluble aluminum in steel. The analyzer (Fig..1) was automated and mainly composed of a sample changer, solution adding devices, a coloring reaction vessel, a spectrophotometer, a controller and a recorder. The spectrophotometric method based on the principle of oxidizing manganese by sodium periodate under the co-existance of silver nitrate, was found to be suitable for automatic determination of manganese in steel by the analyzer. The optimum conditions obtained from the fundamental studies (Fig. 28) were as follows. The concentration of sulphuric acid was 2.3 N. The amount of urea (5%)-silver nitrate (2%) solution was 5.9 ml, sodium periodate solution (10%) was 25.5 ml. The coloring reaction time was 30 seconds. Effects of less than 100 mg of Cr(III) and less than 1 g of Fe were negligible in the present automatic analytical procedure in which the absorbancy of permanganate ion was always corrected by the blank absorbancy. The automatic analysis of manganese is performed according to the predetermined program (Fig. 9). The sample solution with beaker washings (28 ml) are transferred quantitatively to the reaction vessel from the automatic sample changer. The sample solution is preliminarily prepared manually by dissolving 0.100 g of steel sample by heating with 50 ml of mixed acid (H2SO4: 7 ml, H3PO4: 7 ml, HNO3: 6 ml, H2O: 30 ml). The solutions in the reaction vessel are heated and circulated through the circulating pipe which is composed of a bubble remover, an absorbancy measuring flow-cell, a gas blowing tube and a magnetic drain cock. After measuring of the blank absorbancy, 25.5 ml of sodium periodate solution and 5.9 ml of urea-silver nitrate solution are added at the same period by opening a magnetic cock of the reagent solution adding devices. The absorbancy of colored solution was measured by the spectrophotometer. The solution in the reaction vessel is drained off and the vessel is washed by water. This automatic analysis had a merit of simplicity and rapidity. The time required for analysis of one sample was only 5 minutes as compared with the manual analysis which occupies about 25 minutes. The analytical results of carbon steel, low alloy steel, chromium steel and stainless steel were well agreed with the standard values.
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鋼中マンガン自動吸光光度分析法

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