ポーラログラフによる鉄鉱石,鉄鋼中のヒ素の定量
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After being separated from iron by the manganese coprecipitate method, arsenic was distilled by adding carbon dioxide to it; and then the arsenic was determined by the polarographic method using a solution composed of 1<I>M</I> tartaric acid, about 1.7<I>N</I> hydrochloric acid, and 0.004% gelatin, which had been made by adding to the distillate, tartaric acid and gelatin solution and diluting it with water. If arsenic is distilled by adding carbon dioxide to it after being separated from a large quantity of iron beforehand, the distillation is completed easily and rapidly with a small volume of the distillate. In order to coprecipitate arsenic with manganese dioxide in iron solution, about 0.5<I>N</I> is the most suitable for nitric acid concentration. With more than 0.7<I>N</I> arsenic does not coprecipitate quantitatively. This method can not be adapted to samples which contain much chromium.<BR>1g sample is dissolved in 16m<I>l</I> of (1 + 1) nitric acid with the aid of heat, and diluted up to 100m<I>l</I> with water. After addition of 5m<I>l</I> of 5% manganese nitrate solution, the solution is heated until it comes to a boil and 3m<I>l</I> of 2% potassium permanganate solution is added; and then the solution is continuously boiled for 2 to 3 minutes. Filtered and washed, the precipitate is dissolved with 30m<I>l</I> of (1 +29) sulfuric acid and a few drops of 30% hydrogen peroxide solution in a distilling flask, and then the solution is evaporated to sulfur trioxide fumes. After cooling it, 20m<I>l</I> of concentrated hydrochloric acid, 0.5g of hydrazine sulfate and 2 m<I>l</I> of hypophosphorous acid are added into the flask, and the distillation is performed with the help of carbon dioxide. The distillate is got dipping the end of the condenser into 50m<I>l</I> of cold water in a small beaker, and about 10m<I>l</I> of distillate is caught.<BR>The solution, transferred to a 100m<I>l</I> volumetric flask in which 15g of tartaric acid has been put beforehand, is diluted to the mark with water after the solid is dissolved, and then 2m<I>l</I> of 0.2% gelatin solution is added. The polarogram of the solution is recorded in the usual manner, and the first wave of arsenic occurs at -0.33 V <I>vs</I>. the S. C. E...
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