高純度トリウム化合物中の鉄の光度定量第3報(トリウム中の不純物の定量) : トリウム共存における0-フェナンスロリン発色法の研究

概要

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A method has been studied for the photometric determination of iron (>ca. 2ppm Fe/ThO_2). A sample (1∿2g as ThO_2) is dissolved in 10ml of nitric acid (1+1) and 3 drops of hydrofluoric acid (1+9) using a 50ml platinum dish and evaporated to dryness on a steam bath. The residue is dissolved in 5ml of hot water by gentle heating. Unless the solution is clear, it should be filtered through a small dry paper. After 2ml of 1% hydroquinone has been added with stirring, it is set aside for about 5 minutes. 3ml of 0.1% o-Phenanthroline is added with stirring and the solution is transfered in a 25ml volumetric flask with 10ml of 25% ammonium citrate and several ml of water. After ammonium hydroxide is added up to pH 9 against bromphenol blue paper, the solution is diluted to the mark. The solution is vigorously mixed for one minute at 20∿30℃, and the absorbancy is measured at 510mμ. A reagent blank is run through the whole procedure. The calibration curve is derived from an experimental curve plotted using the procedure and a standard series of iron solutions in which is added about the same amount of thorium compound as the sample itself, by subtracting the effect of inevitable trace of Fe in the added thorium compound with an aid of vertical translocation of the curve.
山梨大学の論文
1961-12-20