Abstract
Abstract: This study presents a miniaturized instrumentation for the determination of a model electrochemically reducible compound, 4-nitrophenol, in micro volumes of dimethyl sulfoxide at the glassy carbon electrode. Several working configurations of a three-electrode system and different constructions of reference electrodes are described. Moreover, the problem of the removal of oxygen (which is rather difficult in micro volumes) complicating the determination by differential pulse voltammetry, especially in a cathodic potential range was successfully solved. It has been found that the interference of oxygen can be partly eliminated by square wave voltammetry which is less sensitive to the presence of oxygen in the sample. Special apparatus capable of removing dissolved oxygen from 20 mm3 of solution was also constructed and tested. It was verified that 4-nitrophenol can be determined in micro volumes of dimethyl sulfoxide by square wave voltammetry in the presence of dissolved oxygen (limit of quantification LOQ = 6.0 µmol dm−3) and by differential pulse voltammetry after the removal of dissolved oxygen (LOQ = 2.4 µmol dm−3). Both those methods are comparable with the determination in a macro volume (5.0 cm3), which has LOQ = 1.3 µmol dm−3. Graphical abstract: [Figure not available: see fulltext.].
| Original language | English |
|---|---|
| Pages (from-to) | 1639-1644 |
| Number of pages | 6 |
| Journal | Monatshefte fur Chemie |
| Volume | 148 |
| Issue number | 9 |
| DOIs | |
| Publication status | Published - 1 Sep 2017 |
| Externally published | Yes |
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Keywords
- 4-Nitrophenol
- Differential pulse voltammetry
- Dimethyl sulfoxide
- Glassy carbon electrode
- Microanalysis
- Square wave voltammetry
ASJC Scopus subject areas
- Chemistry(all)
Cite this
Micro volume voltammetric determination of 4-nitrophenol in dimethyl sulfoxide at a glassy carbon electrode. / Gajdár, Július; Barek, Jiří; Fojta, Miroslav; Fischer, Jan.
In: Monatshefte fur Chemie, Vol. 148, No. 9, 01.09.2017, p. 1639-1644.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Micro volume voltammetric determination of 4-nitrophenol in dimethyl sulfoxide at a glassy carbon electrode
AU - Gajdár, Július
AU - Barek, Jiří
AU - Fojta, Miroslav
AU - Fischer, Jan
PY - 2017/9/1
Y1 - 2017/9/1
N2 - Abstract: This study presents a miniaturized instrumentation for the determination of a model electrochemically reducible compound, 4-nitrophenol, in micro volumes of dimethyl sulfoxide at the glassy carbon electrode. Several working configurations of a three-electrode system and different constructions of reference electrodes are described. Moreover, the problem of the removal of oxygen (which is rather difficult in micro volumes) complicating the determination by differential pulse voltammetry, especially in a cathodic potential range was successfully solved. It has been found that the interference of oxygen can be partly eliminated by square wave voltammetry which is less sensitive to the presence of oxygen in the sample. Special apparatus capable of removing dissolved oxygen from 20 mm3 of solution was also constructed and tested. It was verified that 4-nitrophenol can be determined in micro volumes of dimethyl sulfoxide by square wave voltammetry in the presence of dissolved oxygen (limit of quantification LOQ = 6.0 µmol dm−3) and by differential pulse voltammetry after the removal of dissolved oxygen (LOQ = 2.4 µmol dm−3). Both those methods are comparable with the determination in a macro volume (5.0 cm3), which has LOQ = 1.3 µmol dm−3. Graphical abstract: [Figure not available: see fulltext.].
AB - Abstract: This study presents a miniaturized instrumentation for the determination of a model electrochemically reducible compound, 4-nitrophenol, in micro volumes of dimethyl sulfoxide at the glassy carbon electrode. Several working configurations of a three-electrode system and different constructions of reference electrodes are described. Moreover, the problem of the removal of oxygen (which is rather difficult in micro volumes) complicating the determination by differential pulse voltammetry, especially in a cathodic potential range was successfully solved. It has been found that the interference of oxygen can be partly eliminated by square wave voltammetry which is less sensitive to the presence of oxygen in the sample. Special apparatus capable of removing dissolved oxygen from 20 mm3 of solution was also constructed and tested. It was verified that 4-nitrophenol can be determined in micro volumes of dimethyl sulfoxide by square wave voltammetry in the presence of dissolved oxygen (limit of quantification LOQ = 6.0 µmol dm−3) and by differential pulse voltammetry after the removal of dissolved oxygen (LOQ = 2.4 µmol dm−3). Both those methods are comparable with the determination in a macro volume (5.0 cm3), which has LOQ = 1.3 µmol dm−3. Graphical abstract: [Figure not available: see fulltext.].
KW - 4-Nitrophenol
KW - Differential pulse voltammetry
KW - Dimethyl sulfoxide
KW - Glassy carbon electrode
KW - Microanalysis
KW - Square wave voltammetry
UR - http://www.scopus.com/inward/record.url?scp=85021698781&partnerID=8YFLogxK
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U2 - 10.1007/s00706-017-1954-4
DO - 10.1007/s00706-017-1954-4
M3 - Article
VL - 148
SP - 1639
EP - 1644
JO - Monatshefte fur Chemie
JF - Monatshefte fur Chemie
SN - 0026-9247
IS - 9
ER -