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2-(5-Nitro-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)phenol (Nitro-PAPS) was used for a quantitative determination of ultratrace-level metal ions in commercially available metal salts by capillary zone electrophoresis. At pH 7, Nitro-PAPS reacts with various metal ions to form chelate compounds having large molar absorptivities. Although chelate formation is useful for the highly sensitive detection of metal ions, the resolution of the metal complexes is poor at pH 7. Cetyltrimethylammonium bromide was added to suppress any electroosmotic flow. The hydration of nitro groups of a chelating agent and chelates was controlled by the addition of urea. Sodium sulfate was also utilized to sharpen the signals of metal chelates by a field-enhanced stacking effect. As a result, the resolution was improved and the determination of 10-7 M level metal ions was possible. The proposed method was applied to the analysis of metal impurity at ultratrace levels in commercially available nickel and iron salts.市販金属塩中の極微量金属不純物の定量法として, 2-(5-ニトロ-2-ピリジルアゾ)-5-(N-プロピル-N-スルホプロピルアミノ)フェノール (Nitro-PAPS) とのキレートを分離, 検出するキャピラリー電気泳動法について検討した. 各種金属イオンと定量的に反応するpH7の条件では, 高感度検出が可能であるが, 多くの金属錯体の分離は十分でない. そこで, 電気浸透流やキレートの電気泳動移動度を変化させる効果のある第四級アンモニウム塩等の添加を検討し, 種々な相互作用試薬を用いて分離の改善を図った. その結果, 臭化セチルトリメチルアンモニウムの添加で電気浸透流が抑制され, 硫酸ナトリウムの添加によるスタッキング効果の活用によりシグナルが鋭敏化され, 尿素の添加でニトロ基周りの水和を抑制したところ, 金属キレートの分離性能が向上した. 本法により10(-7)MレベルのFe, Co, Ni, Cuの分離定量が可能になり, 市販特級金属塩中の極微量金属の分析に適用したところ, ppm (=10(-6)g/g) レベルの金属不純物を定量することができた

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Determination of trace metal impurities in nickel and iron salts using 2-(5-Nitro-2-pyridylazo)-5-(N-propyl-N-sulfopropyl-amino) phenol by capillary zone electrophoresis.