電子管用ニッケル材料中のマグネシウムの定量

概要

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A spectrophotometric method with magnesium-Xylidyl Blue complex was applied to the determination magnesium in nickel used for electron tubes. The method is characterized by the elimination of interfering elements, such as nickel and trace of manganese, with mercury cathode electrolysis and subsequent solvent extraction. The established procedure is as follows : - In 20ml of nitric acid (1+1) and 4ml of perchloric acid is dissolved 0.10.2g of the sample, of which the amount depends on the magnesium content, and after heating the mixture on a sand bath to dense white fumes, nickel and other interfering elements are removed by mercury cathode electrolysis and subsequent solvent extraction. The aqueous solution is then evaporated to dryness on a heater in order to expel ammonium chloride and to decompose diethyldithiocarbamate. The residues are dissolved in hot water, and the solution is diluted to 100ml with water. To a 10ml portion of the solution is added 5ml of 0.03% Xylidyl Blue alcohol solution, and then 2ml of 0.08M sodium borate buffer solution. The final mixture is diluted with water to 50ml. After allowing the solution to stand for 20 minutes, photometric measurement at 520mμ is carried out against a reagent blank. The method is suitable for the determination of magnesium less than 0.1% of in nickel metal.
社団法人日本分析化学会の論文