Abstract
Electrodes based on amalgam materials were re-introduced in electroanalytical chemistry in the year 2000, partially as reaction to unsubstantiated public fears of liquid mercury. In this publication, the voltammetric behavior of 1-nitronaphthalene and 2-nitronaphthalene was investigated at a mercury meniscus-modified silver solid amalgam electrode. The reduction mechanism in mixed neutral buffer-methanol medium includes the four-electron reduction to hydroxylaminoderivative followed by a two-electron reduction to the amine in acidic medium, similarly to mercury electrodes. In alkaline media, both compounds show the splitting of the main four-electron reduction peak typical for mercury electrodes in two new ones, the first one corresponding to a one electron reduction of the nitroderivative to the nitro radical anion, which was confirmed by microcoulometry. Using optimized conditions (differential pulse voltammetry, Britton-Robinson buffer pH 7.0 - methanol (9:1) medium) the calibration dependences are linear in the range of 2 · 10-7 (4 · 10-7) to 1 · 10-4 mol L-1 for 1-nitronaphthalene (2-nitronaphthalene). After preconcentration of the analytes from drinking and river water samples using solid phase extraction the limit of determination was lowered to ∼3 · 10-8 mol L-1.
| Original language | English |
|---|---|
| Pages (from-to) | 2339-2363 |
| Number of pages | 25 |
| Journal | Analytical Letters |
| Volume | 42 |
| Issue number | 15 |
| DOIs | |
| Publication status | Published - 3 Nov 2009 |
| Externally published | Yes |
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Keywords
- 1-nitronaphthalene
- 2-nitronaphthalene
- Cyclic voltammetry
- Differential pulse voltammetry
- Elimination voltammetry with linear scan
- Silver solid amalgam electrode
- Solid phase extraction
ASJC Scopus subject areas
- Analytical Chemistry
- Biochemistry
- Spectroscopy
- Clinical Biochemistry
- Biochemistry, medical
- Electrochemistry
Cite this
Voltammetric determination of nitronaphthalenes at a silver solid amalgam electrode. / Pecková, Karolina; Barek, Jiří; Navrátil, Tomáš; Yosypchuk, Bogdan; Zima, Jiří.
In: Analytical Letters, Vol. 42, No. 15, 03.11.2009, p. 2339-2363.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Voltammetric determination of nitronaphthalenes at a silver solid amalgam electrode
AU - Pecková, Karolina
AU - Barek, Jiří
AU - Navrátil, Tomáš
AU - Yosypchuk, Bogdan
AU - Zima, Jiří
PY - 2009/11/3
Y1 - 2009/11/3
N2 - Electrodes based on amalgam materials were re-introduced in electroanalytical chemistry in the year 2000, partially as reaction to unsubstantiated public fears of liquid mercury. In this publication, the voltammetric behavior of 1-nitronaphthalene and 2-nitronaphthalene was investigated at a mercury meniscus-modified silver solid amalgam electrode. The reduction mechanism in mixed neutral buffer-methanol medium includes the four-electron reduction to hydroxylaminoderivative followed by a two-electron reduction to the amine in acidic medium, similarly to mercury electrodes. In alkaline media, both compounds show the splitting of the main four-electron reduction peak typical for mercury electrodes in two new ones, the first one corresponding to a one electron reduction of the nitroderivative to the nitro radical anion, which was confirmed by microcoulometry. Using optimized conditions (differential pulse voltammetry, Britton-Robinson buffer pH 7.0 - methanol (9:1) medium) the calibration dependences are linear in the range of 2 · 10-7 (4 · 10-7) to 1 · 10-4 mol L-1 for 1-nitronaphthalene (2-nitronaphthalene). After preconcentration of the analytes from drinking and river water samples using solid phase extraction the limit of determination was lowered to ∼3 · 10-8 mol L-1.
AB - Electrodes based on amalgam materials were re-introduced in electroanalytical chemistry in the year 2000, partially as reaction to unsubstantiated public fears of liquid mercury. In this publication, the voltammetric behavior of 1-nitronaphthalene and 2-nitronaphthalene was investigated at a mercury meniscus-modified silver solid amalgam electrode. The reduction mechanism in mixed neutral buffer-methanol medium includes the four-electron reduction to hydroxylaminoderivative followed by a two-electron reduction to the amine in acidic medium, similarly to mercury electrodes. In alkaline media, both compounds show the splitting of the main four-electron reduction peak typical for mercury electrodes in two new ones, the first one corresponding to a one electron reduction of the nitroderivative to the nitro radical anion, which was confirmed by microcoulometry. Using optimized conditions (differential pulse voltammetry, Britton-Robinson buffer pH 7.0 - methanol (9:1) medium) the calibration dependences are linear in the range of 2 · 10-7 (4 · 10-7) to 1 · 10-4 mol L-1 for 1-nitronaphthalene (2-nitronaphthalene). After preconcentration of the analytes from drinking and river water samples using solid phase extraction the limit of determination was lowered to ∼3 · 10-8 mol L-1.
KW - 1-nitronaphthalene
KW - 2-nitronaphthalene
KW - Cyclic voltammetry
KW - Differential pulse voltammetry
KW - Elimination voltammetry with linear scan
KW - Silver solid amalgam electrode
KW - Solid phase extraction
UR - http://www.scopus.com/inward/record.url?scp=70350495887&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=70350495887&partnerID=8YFLogxK
U2 - 10.1080/00032710903142442
DO - 10.1080/00032710903142442
M3 - Article
AN - SCOPUS:70350495887
VL - 42
SP - 2339
EP - 2363
JO - Analytical Letters
JF - Analytical Letters
SN - 0003-2719
IS - 15
ER -