定電位クーロメトリーの自動記録液体クロマトグラフィーへの応用　ＶＩ　　Ｈ型陽イオン交換樹脂によるカルボン酸の分離

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書誌事項

タイトル別名
  • Liquid chromatographic separation of carboxylic acids with the H-form cation-exchange resin
  • Hケイ ヨウイオン コウカン ジュシ ニ ヨル カルボンサン ノ ブンリ
  • 定電位クーロメトリーの自動記録液体クロマトグラフィーへの応用(第6報)

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A flow coulometric detector for liquid chromatography was applied to the study of ion-exchange chromatographic separation of carboxylic acids. The detection was based on the electrochemical reaction of a p-benzoquinone and two protons dissociated from acids producing hydroquinone on the working electrode. The detection limit was about 10-9 mole.<BR>The chromatographic behavior of lower fatty acids ranging C1 to C6 and maleic, fumaric, oxalic, citric, tartaric, phthalic, succinic, lactic and salicylic acids on a H-form strong cation-exchange resin was studied. Zero to 50% methyl cellosolve was used as an eluent. The particle size and distribution of resin was important to obtain a high resolution. For example, the height equivalent of a theoretical plate (HETP) on n-butyric acid measured with 200400 mesh resin was 0.58 mm, while with 18μ±2μ diameter resin composed of finner and evener particles it was 0.056 mm.<BR>The effect of the concentration of eluent on the retention time and the resolution was also studied. The greater the carbon number is, the more the elution of fatty acid except formic acid is accelerated by raising the concentration of methyl cellosolve. On the other hand, the retention time of the most of polybasic acids and hydroxy acids is not very affected by the concentration of the eluent. For the separation, 1015% and 20% methyl cellosolves were thought to be suitable in the fatty acids and the others, respectively.<BR>Water as a solvent of the sample solution eluates just before formic acid. Therefore, when the eluent contains free acid or salt as an impurity, a negative peak of water appears on the chromatogram. In regard to column efficiency, the resin of 18μ±2μ diameter was sufficient to separate these acids since the HETP of the most of fatty acids was less than 0.1 mm. Consequently, a mixture of ten components containing lower fatty acids, fumaric acid and maleic acid were completely separated each other with 10% methyl cellosolve as an eluent within 60 minutes.<BR>This method was applied to the analysis of various brands of sake, and vinegar. In the case of sake, it has become apparent that amounts and/or ratios of succinic acid and lactic acid are different among brands or grades. On the other side, in addition to acetic acid the principal ingredient, several acids were detected in vinegar. This work suggests that the chromatographic pattern will be effective for the control of brewing.

収録刊行物

  • 分析化学

    分析化学 23 (12), 1522-1527, 1974

    公益社団法人 日本分析化学会

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