4-ピリジンカルボン酸-ピラゾロン吸光検出イオン排除クロマトグラフィーによるシアン化物及び塩化シアンの定量

• 井上 嘉則

  山梨大学工学部生物工学科

• 鈴木 義仁

  山梨大学工学部生物工学科

• 安藤 正典

  厚生省国立衛生試験所

書誌事項

タイトル別名

• Determination of cyanide ion and cyanogen chloride by using photometric detection with 4-pyridinecarboxylic acid-pyrazolone in ion-exclusion chromatography.
• ４‐ピリジンカルボン酸‐ピラゾロン吸光検出イオン排除クロマトグラフィーによるシアン化物及び塩化シアンの定量
• 4 ピリジンカルボンサン ピラゾロン キュウコウ ケンシュツ イオン ハイジョ

抄録

4-Pyridinecarboxylic acid(PCA)-pyrazolone was used for the determination of cyanide ion and cyanogen chloride as a reagent in the postcolumn derivatization method. The cyanide ion and cyanogen chloride were separated by ion-exclusion chromatography (IEC). The cyanide ion was then converted into cyanogen chloride by a reaction with Chloramine T. The cyanogen chloride derived from the cyanide ion, as well as that present in the sample solution, were treated with a PCA-pyrazolone solution and detected at 638 nm. The reaction parameters were optimized for cyanide ion and cyanogen chloride as follows : reaction coil for the conversion of cyanide ion into cyanogen chloride, 2 m × 0.5 mm i.d. ; reaction coil for reaction with PCA-pyrazolone reagent, 10 m × 0.5 mm i.d.; concentration of Chloramine T, 0.1 % in 0.02 mol dm ^-3 phosphate buffer (pH 7.4) ; concentration of PCA-pyrazolone reagent, 0.2 mol dm ^-3 PCA and 0.03 mol dm ^-3 pyrazolone; flow rate of the reagent, 0.5 cm³ min^-1 each; reaction temperature, 100°C. The chromatographic conditions were as follows : column, IEC column (300 mm × 8 mm i.d.) packed with hydrogen form sulfonated polystyrene gel (ion exchange capacity : 3.5 meq/g · dry) ; mobile phase, 1 × 10^-3 mol dm ^-3 sulfuric acid ; flow rate, 1.5 cm³ min ^-1 ; detection wavelength, 638 nm. The detection limits (S/N =3) for the cyanide ion and cyanogen chloride were 2.5× 10 ^-4 and 2.9× 10 ^-4 mg dm ^-3 as cyanide ion. The linear range was over 3 orders of magnitude, from 0.001 to 1 mg dm ^-3. The relative standard deviation was 3.8% (n=10) for 0.001 mg dm ^-3 cyanide ion solution.

収録刊行物

• 分析化学

  分析化学 42 (10), 617-623, 1993

  公益社団法人 日本分析化学会

キーワード

• determination of cyanide ion and cyanogen chloride
• ion exclusion chromatography
• postcolumn derivatization : photometric detection
• 4-pyridinecarboxylic acid-pyrazolone method.

詳細情報

• CRID: 1390001204051944576
• NII論文ID: 110002906469
• NII書誌ID: AN00222633
• DOI: 10.2116/bunsekikagaku.42.10_617
• COI: 1:CAS:528:DyaK2cXit1KntQ%3D%3D
• NDL書誌ID: 3846888
• ISSN: 05251931
• ISSN: http://id.crossref.org/issn/05251931
• Web Site: https://ndlsearch.ndl.go.jp/books/R000000004-I3846888
• Web Site: http://www.jstage.jst.go.jp/article/bunsekikagaku1952/42/10/42_10_617/_pdf
• Web Site: http://dl.ndl.go.jp/info:ndljp/pid/10893170
• 本文言語コード: ja
• データソース種別:
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  • CiNii Articles
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