Determination of cyanide ion and cyanogen chloride by using photometric detection with 4-pyridinecarboxylic acid-pyrazolone in ion-exclusion chromatography.

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  • INOUE Yoshinori
    Department of Chemistry and Biotechnology, Faculty of Engineering, Yamanashi University
  • SUZUKI Yoshihito
    Department of Chemistry and Biotechnology, Faculty of Engineering, Yamanashi University
  • ANDO Masanori
    National Institute of Hygienic Science

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Other Title
  • 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
  • 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

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Description

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.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 42 (10), 617-623, 1993

    The Japan Society for Analytical Chemistry

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