吸光光度法によるフェロモリブデン中のモリブデンの迅速定量方法

概要

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A method has been established for the rapid photometric determination of molybdenum in ferromolybdenum by the stannous chloride reduction method without thiocyanate. The best results were obtained by the following procedure : a 0.1 g sample was placed in a 300 ml beaker, and 15 ml sulfuric acid (1 : 1) and about 2 ml nitric acid (1.4) were added. The mixture was heated gently on a sand plate at 300350°C without a cover glass until white fumes were evolved. It was then cooled somewhat, diluted to about 50 ml with water, filtered into a 100 ml volumetric flask, diluted to about 80 ml, and cooled with running water. Next 0.2 ml copper sulfate solution (1 ml equivalent to 1 mg Cu) was added, and 10 ml stannous chloride solution(10 %) was added with shaking. The mixture was made up to the mark with water, and shaken thoroughly. After 2 min or so had passed, the light absorbancy of the solution was measured with an S 47 filter corresponding to 470 mμ in wave length. In the foregoing procedure it was unnecessary to add the copper sulfate solution when the sample contained more than 0.2 % of copper. The relationship between the amount of molybdenum and the light absorbancy was linear up to about 90 mg of molybdenum, and the coloration remained unchanged during the experimental period of 60 min. The time required to determine molybdenum by this method was about 20 min.
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