Abstract
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 language | English |
|---|---|
| Pages (from-to) | 469-478 |
| Number of pages | 10 |
| Journal | bunseki kagaku |
| Volume | 67 |
| Issue number | 8 |
| DOIs | |
| Publication status | Published - Jan 1 2018 |
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All Science Journal Classification (ASJC) codes
- Analytical Chemistry
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On-line redox derivatization liquid chromatography using a carbon monolithic column. / Miyashita, Ken; Tanaka, Ryo; Hasegawa, George; Nakanishi, Kazuki; Morioka, Kazuhiro; Zeng, Hulie; Kato, Shungo; Uchiyama, Katsumi; Saitoh, Kazunori; Shibukawa, Masami; Nakajima, Hizuru.
In: bunseki kagaku, Vol. 67, No. 8, 01.01.2018, p. 469-478.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - On-line redox derivatization liquid chromatography using a carbon monolithic column
AU - Miyashita, Ken
AU - Tanaka, Ryo
AU - Hasegawa, George
AU - Nakanishi, Kazuki
AU - Morioka, Kazuhiro
AU - Zeng, Hulie
AU - Kato, Shungo
AU - Uchiyama, Katsumi
AU - Saitoh, Kazunori
AU - Shibukawa, Masami
AU - Nakajima, Hizuru
PY - 2018/1/1
Y1 - 2018/1/1
N2 - 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.
AB - 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.
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U2 - 10.2116/bunsekikagaku.67.469
DO - 10.2116/bunsekikagaku.67.469
M3 - Article
AN - SCOPUS:85053424956
VL - 67
SP - 469
EP - 478
JO - Bunseki Kagaku
JF - Bunseki Kagaku
SN - 0525-1931
IS - 8
ER -