On-line redox derivatization liquid chromatography using a carbon monolithic column

Ken Miyashita, Ryo Tanaka, George Hasegawa, Kazuki Nakanishi, Kazuhiro Morioka, Hulie Zeng, Shungo Kato, Katsumi Uchiyama, Kazunori Saitoh, Masami Shibukawa, Hizuru Nakajima

    Research output: Contribution to journalArticlepeer-review


    A macroporous resorcinol-formaldehyde (RF) xerogel was synthesized via sol–gel reaction, accompanied by phase separation; a graphitized carbon monolith was then prepared by calcining the RF xerogel at a relatively low temperature (1200 °C) utilizing catalytic graphitization. The retention behaviors of metal-EDTA complexes on the carbon monolithic column were investigated. The carbon monolith exhibited catalytic activity for redox reactions, like porous graphitic carbon packing materials do; they oxidized Co(II)-EDTA to Co(III)-EDTA during elution. Their redox activity could be modified by treating with an eluent containing an oxidizing or reducing agent. A novel on-line redox derivatization HPLC system using a carbon monolithic column was developed for enhancing the separation selectivity. This on-line redox derivatization HPLC system consisted of two ODS columns as a separation column and one carbon monolithic column as redox derivatization unit placed between them. The Co(II)-EDTA migrated as its original oxidation state in the first ODS column, while it migrated as Co(III)-EDTA in the second ODS column, since Co(II)-EDTA was rapidly oxidized to Co(III)-EDTA in the carbon monolithic column. On the other hand, other metal-EDTA complexes migrated as their original oxidation states in these columns. Therefore, the Co-EDTA could be separated from the other metal-EDTA complexes. This on-line redox derivatization HPLC system was successfully used for determining the trace amount of cobalt in a reference copper alloy.

    Original languageEnglish
    Pages (from-to)469-478
    Number of pages10
    Journalbunseki kagaku
    Issue number8
    Publication statusPublished - 2018

    All Science Journal Classification (ASJC) codes

    • Analytical Chemistry


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