書誌事項
- タイトル別名
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- Spectrophotometric analysis of average valence of bismuth and copper in superconductor by use of small amounts of sample.
- キュウコウ コウドホウ ニ ヨル ビ ショウリョウ チョウデンドウタイ シリョ
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抄録
The analysis of the average valence of Bi and Cu in superconductor Bi-Sr-Ca-Cu-O by use of small amounts of sample was investigated by the spectrophotometry. Bi(V) reacts with Mn(II) ion to form permanganate ion in nitric acid solution. Therefore, Bi(V) could be determined in the presence of large amount of Mn(II) ion. The apprropriate procedure for the determination of Mn(II) ion was as follows: The sample (ca. 1 mg) was dissolved into 3 ml of a 3M HNO3 containing 1.0×10-3 M Mn(II) ion, and stood for 15 min. The absorbance of the sample solution was measured at 525 nm in order to calculate the amount of Bi(V). Then, the total amount of Bi was determined to obtain the average valence of Bi by the extraction/spectrophotometry with KI. The procedure was as follows: All the sample solution used for the determination of the Bi(V) were transported into a beaker. Then, 10 ml of a 0.1 % ascorbic acid was added into the sample solution to reduce the Mn(VII) and Cu(II). One gram of KI and 15 ml of a 0.1 % Zephiramine (Zeph+Cl-) were added into the sample solution. The solution was shaken for 2 min with 20 ml of chloroform in order to extract the total Bi as Zeph+BiI4-, which was measured at 492 nm. On the other hand, by using another sample (ca. 0.3 mg), the mixture of Cu(II) and Cu(III) was determined by iodometry. The liberated I2 corresponding to the sum of the valence change of copper was extracted with chloroform as Zeph+I3-. One part of sample solution prepared was used for the extraction of the I2. The absorbances due to both Bi(V) and Bi(III) were corrected from the calibration curves constructed previously. The total amount of copper in the sample was determined with bathocuproine by using the other parts of the sample remained as a solution. One of the analysis results was 3.16±0.03 for Bi and 2.03±0.05 for Cu.
収録刊行物
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- 分析化学
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分析化学 42 (1), 33-38, 1993
公益社団法人 日本分析化学会
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詳細情報 詳細情報について
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- CRID
- 1390282679030532736
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- NII論文ID
- 110002906454
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- NII書誌ID
- AN00222633
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- COI
- 1:CAS:528:DyaK3sXhtlyrt7Y%3D
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- NDL書誌ID
- 3810403
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- ISSN
- 05251931
- http://id.crossref.org/issn/05251931
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- 本文言語コード
- ja
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- データソース種別
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- JaLC
- NDL
- Crossref
- NDL-Digital
- CiNii Articles
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- 抄録ライセンスフラグ
- 使用不可