高純度金属銅表面の酸化銅(I)と酸化銅(II)の分別定量

フォーマット:

論文

責任表示:

松本, 健 ; 木羽, 敏泰

言語:

日本語

出版情報:

The Japan Society for Analytical Chemistry = 日本分析化学会, 1981-01-05

著者名:

• 松本, 健
• 木羽, 敏泰

掲載情報:

分析化学 = Japan analyst

ISSN:

0525-1931      

巻:

30

通号:

1

開始ページ:

12

終了ページ:

16

バージョン:

publisher

概要:

金沢大学イノベーション創成センター<br />100 ml 分液漏斗に1M塩化アンモニウム-炭酸アンモニウム-アンモニア水溶液(pH10) 50 ml を入れ,窒素を通じ脱酸素してから,金属銅試料を加え振り混ぜると,酸化銅(I)と酸化銅(II)はアンミン錯イオンとなって溶解し,金属は溶けないで残る.水溶液について銅の量を原子吸光法で定量すれば,酸化銅(I)と酸化銅(II)の合量が求められる.一方,水溶液について窒素ふん囲気の下でバクソプロイン-クロロホルム抽出した … 後,銅を比色定量して酸化銅(I)の量を求める.酸化銅(II)は酸化銅(I)と酸化銅(II)の合量から酸化銅(I)を差し引いて算出した.本法は精度が高く,金属銅表面の酸化銅(I)と酸化銅(II)とを簡単迅速に分別定量できる. Fractional determination of cuprous oxide and cupric oxide attaching on the surface of high purity copper metal. Ken MATSUMOTO and Toshiyasu KIBA (Department of Chemistry, Faculty of Science, Kanazawa University, 1-1, Marunouchi, Kanazawa-shi, Ishikawa) A 50 ml portion of 1 M ammonium chloride-ammonium carbonate buffer solution at pH 10 was placed in a 100 ml separatory funnel and several pieces of high purity copper metal sample were put into the solution. Then a sufficient amount of nitrogen gas to remove oxygen from the solution as well as the vessel was passed through and the whole was agitated vigorously for 5 min. It was found that the cuprous and cupric oxide on the surface of the sample were dissolved as tetraammine copper complex cations and their oxidation states were retained while the metallic copper remained undissolved. The copper content in the resulting solution which should give the sum of the cuprous and cupric oxide was determined by atomic absorption spectrometry. The determination of cuprous oxide was carried out as follows. A 5 ml portion of the sample solution containing both of copper (I) and (II) was placed in a 50 ml separatory funnel which contained a 20 ml portion of 1 M ammonium chloride-hydrochloric acid at pH 1 and a 5ml portion of 0.1 % Bathocuproine-ethanol solution under nitrogen atmosphere. The pH of the solution was about 8. After standing for 5 min, the solution was agitated with 5.00 ml of chloroform for 2 min and the absorbance of the chloroform phase at 477 nm was measured against chloroform. This gave the cuprous oxide content. At the same time, a 5 ml portion of the sample solution was pipetted into a 50 ml separatory funnel and about 20 ml of 1 M ammonium chloride solution adjusted at pH 1, a 5 ml portion of 0.1 % Bathocuproin solution and a 2 ml portion of 10 % hydroxyl amine were added. The copper(I) in the solution was extracted by the same procedures as above and the total copper content was also determined from the absorption of this chloroform phase at 477 nm. The cupric oxide content was calculated from the total copper determined by either the atomic absorption spectrometry or the colorimetry and the copper (I) content obtained by the colorimetry. These procedures enabled the analysis of small amounts of cuprous and cupric oxide on the surface of commercial copper metal samples in various forms and the selectivity and the reproducibility were concluded to be excellent. (Received June 5, 1980) 続きを見る

URL:

http://hdl.handle.net/2297/24883