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タイトル: 高純度金属スズ中の酸化スズ(IV)の定量
その他のタイトル: Determination of tin(IV) oxide in high purity tin metals
著者: 松本, 健 link image
輿石, 秀美
寺田, 喜久雄
Matsumoto, Ken
Koshiishi, Hidemi
Terada, Kikuo
発行日: 1984年 5月 5日
出版社(者): The Japan Society for Analytical Chemistry = 日本分析化学会
雑誌名: 分析化学 = Japan analyst
ISSN: 0525-1931
巻: 33
号: 5
開始ページ: 237
終了ページ: 241
キーワード: determination of tin (IV) oxide in tin metal
selective dissolution of tin metal by potassium copper(II) chloride solution
decomposition of tin(IV) oxide by fusion with ammonium iodide
graphite furnace atomic absorption spectrometry for tin (IV)
抄録: 100ml分液漏斗に14%塩化銅(II)カリウム溶液50mlを入れ,窒素を通じ脱酸素してから,試料の高純度金属スズ片を加えて振り混ぜると,金属スズは溶解し,酸化スズ(IV)は不溶残留物となる.酸化スズ(IV)を〓別した後,ヨウ化アンモニウム融解法によって迅速,簡便に分解する.昇華分離したヨウ化スズ(IV)を捕集し,0.5M塩酸で溶解した溶液中のスズ量を黒鉛炉原子吸光法で定量して酸化スズ(IV)量を求める.本法はイオン化傾向の差を利用した置換溶解法であり,選択溶解性は良好であった.数百mgの試料を用い,微量の酸化スズ(IV)を短時間に高い精度で正確に定量できる. 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 200〜300 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 (borosilicateglass, 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.
URI: http://hdl.handle.net/2297/24934
関連URI: http://www.jsac.or.jp/index.html
http://ci.nii.ac.jp/naid/110002908925/en/
資料種別: Journal Article
権利関係: Copyright (c) 1984 日本分析化学会
版表示: publisher
出現コレクション:1. 査読済論文

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