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タイトル別名
  • 高純度金属すず中の酸化すず(IV)の定量
  • Determination of tin(IV) oxide in high purity tin metals
  • コウ ジュンド キンゾク スズチュウ ノ サンカ スズ 4 ノ テイリョウ

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抄録

A simple, fast and accurate method for the determination of tin(IV) oxide in high purity tin metals has been developed. A 50 ml of 14 % (w/v) potassium copper (II) chloride solution containing 0.4 % (w/v) of tartaric acid was put in a 100 ml separatory funnel, and nitrogen was passed through for 10 min at a rate of 700 ml min-1 to remove oxygen. In a nitrogen atmosphere a sample of tin metal, usually 200300 mg in weight, was added and the funnel was stoppered and immediately shaken vigorously for 30 min : the metal dissolved in the solution, while the oxide remained as insoluble residue. The tin(IV) oxide was collected quantitatively on a small sintered glass filter (G4) (3.6 cm × 1.4 cm o.d.) under suction and washed first with potassium copper (II) chloride solution, then with water, and finally with ethanol, and dried. The filter and tin (IV) oxide were placed in a decomposition tube (borosilicate-glass, 5 cm × 1.8 cm o.d.) ; 2 g of ammonium iodide was then added in the same tube, followed by a small piece of platinum wire as catalyst, and the tube was attached to a cold trap (borosilicate-glass, 40 cm × 1.8 cm o.d.). The decomposition tube was gently heated with a fish-tail burner for about 1 min; the sublimate, tin(IV) iodide, was quantitatively collected in the trap. After evolution of iodine had ceased, the tin(IV) iodide was dissolved with 0.5 M hydrochloric acid and the concentration of tin in the resulting solution was determined by graphite furnace atomic absorption spectrometry at the 224.6 nm. This method was applied to commercial high purity tin metal of various forms, and 0.014 to 1.01 % of tin (IV) oxide could be determined with good reproducibility.

収録刊行物

  • 分析化学

    分析化学 33 (5), 237-241, 1984

    公益社団法人 日本分析化学会

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