The determination of 4-substituted derivatives of N-nitroso-N-methyl aniline by fast scan differential pulse voltammetry at a hanging mercury drop electrode

1991 ◽  
Vol 56 (12) ◽  
pp. 2815-2826 ◽  
Author(s):  
Jiří Barek ◽  
Viktor Mejstřík ◽  
Ivana Švagrová ◽  
Jiří Zima

Optimum conditions were found for the determination of N-nitroso-N-methyl aniline and its derivatives substituted in the 4 position by -CH3, -OCH3, -Cl, -CN, -OH or -NO2 groups by fast scan differential pulse voltammetry at a hanging mercury drop electrode in the concentration range 1 10-5-2 10-7 mol l-1. It was demonstrated that these techniques are useful for the analysis of a mixture of the test substances either directly or after separation by thin-layer chromatography and that false positive results can be eliminated by UV irradiation of the test sample. An attempt to further increase the sensitivity by adsorptive accumulation of the test substances on the surface of the hanging mercury drop electrode was not successful as the test N-nitroso compounds are practically not adsorbed on this electrode.

1988 ◽  
Vol 53 (1) ◽  
pp. 19-33 ◽  
Author(s):  
Jiří Barek ◽  
Jana Balsiene ◽  
Antonín Berka ◽  
Ivana Hauserová ◽  
Jiří Zima

The polarographic reduction of the title azo dye was studied, a mechanism was suggested and optimal conditions were determined for analytical utilization of this process. A detection limit of 3 . 10-7 mol 1-1 was obtained using fast scan differential pulse voltammetry and 0.7 . 10-7 mol 1-1 using linear potential scan voltammetry at a hanging mercury drop electrode. The detection limit can be decreased by adsorptive accumulation of the determined substance on the surface of the hanging mercury drop electrode, to 1 . 10-8 mol 1-1 for fast scan differential pulse voltammetry and 0.6 . 10-8 mol 1-1 for linear scan voltammetry. The selectivity of the determination can be improved by preliminary separation by extraction or thin-layer chromatography.


1991 ◽  
Vol 56 (3) ◽  
pp. 595-601 ◽  
Author(s):  
Jiří Barek ◽  
Gulamustafa Malik ◽  
Jiří Zima

Optimum conditions were found for the determination of 4-nitrobiphenyl by fast scan differential pulse voltammetry at a hanging mercury drop electrode in the concentration range 1 . 10-5 to 2 . 10-7 mol l-1. A further increase in sensitivity was attained by adsorptive accumulation of this substance on the surface of the working electrode, permitting determination in the concentration range (2 – 10) . 10-8 mol l-1 with one minute accumulation of the substance in unstirred solution or (2 – 10) . 10-9 mol l-1 with three-minute accumulation in stirred solution. Linear scan voltammetry can be used to determine 4-nitrobiphenyl in the concentration range (2 – 10) . 10-9 mol l-1 with five-minute accumulation in stirred solution, with the advantage of a smoother baseline and smaller interference from substances that yield only tensametric peaks.


1989 ◽  
Vol 54 (6) ◽  
pp. 1538-1548
Author(s):  
Jiří Barek ◽  
Ashutosh Ghosh ◽  
Jiří Zima

The polarographic reduction of the azodye semitrypane blue has been studied, a mechanism has been proposed and optimal conditions have been found for the determination of this substance by TAST polarography (to 2.10-6 mol l-1) and differential pulse polarography (to 1.10-7 mol l-1) at a classical dropping mercury electrode and by fast scan differential pulse voltammetry (to 1.10-8 mol l-1) and linear scan voltammetry (to 1.10-8 mol l-1) at a hanging mercury drop electrode. The detection limit was decreased to 1.10-9 mol l-1 for fast scan differential pulse voltammetry and 1.10-10 mol l-1 for linear scan voltammetry by using adsorptive accumulation of the determined substance at the hanging mercury drop electrode.


1993 ◽  
Vol 58 (9) ◽  
pp. 2021-2038 ◽  
Author(s):  
Jiří Barek ◽  
Dana Dřevínková ◽  
Jiří Zima

The polarographic behaviour of 1-(2'-nitrophenyl)-3,3-dimethyltriazene in mixed aqueous-methanolic solvent was investigated by tast polarography, differential pulse polarography, and fast scan differential pulse voltammetry at a hanging mercury drop electrode. A mechanism is suggested for the reduction of the compound investigated. The optimum conditions were found for the determination of this analyte by tast polarography over the concentration region of 100 to 2 μmol l-1 and by differential pulse polarography or fast scan differential pulse voltammetry at a hanging mercury drop electrode over the region of 100 to 0.2 μmol l-1. Additional sensitivity increase in the last-mentioned technique was achieved by adsorptive accumulation of analyte on the hanging mercury drop surface, owing to which the concentration region was depressed to 0.1 - 0.02 μmol l-1.


1986 ◽  
Vol 51 (11) ◽  
pp. 2466-2472 ◽  
Author(s):  
Jiří Barek ◽  
Antonín Berka ◽  
Ludmila Dempírová ◽  
Jiří Zima

Conditions were found for the determination of 6-mercaptopurine (I) and 6-thioguanine (II) by TAST polarography, differential pulse polarography and fast-scan differential pulse voltammetry at a hanging mercury drop electrode. The detection limits were 10-6, 8 . 10-8, and 6 . 10-8 mol l-1, respectively. A further lowering of the detection limit to 2 . 10-8 mol l-1 was attained by preliminary accumulation of the determined substances at the surface of a hanging mercury drop.


2011 ◽  
Vol 76 (12) ◽  
pp. 1991-2004 ◽  
Author(s):  
Vlastimil Vyskočil ◽  
Ivan Jiránek ◽  
Aleš Daňhel ◽  
Jiří Zima ◽  
Jiří Barek ◽  
...  

Electrochemical behavior of genotoxic nitro derivatives of quinoline, namely 5-nitroquinoline (5-NQ), 6-nitroquinoline (6-NQ) and 8-nitroquinoline (8-NQ), was investigated by DC tast polarography (DCTP) and differential pulse polarography (DPP), both at a classical dropping mercury electrode (DME), and by differential pulse voltammetry (DPV) and adsorptive stripping differential pulse voltammetry (AdSDPV), both at a miniaturized hanging mercury drop minielectrode (HMDmE), in buffered aqueous (for 5-NQ) or aqueous-methanolic (for 6-NQ and 8-NQ) solutions. Optimum conditions were found for the determination of 5-NQ, 6-NQ and 8-NQ by DCTP at DME (with limits of quantification, LQ ≈ 9 × 10–7, 3 × 10–7 and 2 × 10–6 mol l–1, respectively), by DPP at DME (LQ ≈ 1 × 10–8, 9 × 10–8 and 1 × 10–7 mol l–1, respectively), by DPV at HMDmE (LQ ≈ 2 × 10–8, 1 × 10–7 and 1 × 10–7 mol l–1, respectively), and by AdSDPV at HMDmE (LQ ≈ 1 × 10–8 mol l–1 for 8-NQ; an attempt at increasing the sensitivity using AdSDPV at HMDmE was not successful for 5-NQ and 6-NQ). Practical applicability of the developed methods was verified on the direct determination of the studied compounds in model samples of drinking and river water in submicromolar concentrations and on the determination in model samples of drinking and river water using preliminary separation and preconcentration by solid phase extraction (SPE) in nanomolar concentrations.


1992 ◽  
Vol 57 (6) ◽  
pp. 1230-1236
Author(s):  
Jiří Barek ◽  
Viktor Mejstřík ◽  
Saafa Toubar ◽  
Jiří Zima

A study was made of the polarographic behaviour of 1-(4'-carbamoylphenyl)-3,3-dimethyltriazene and optimum conditions were found for its determination by tast polarography and differential pulse polarography at a static mercury drop electrode and by fast scan differential pulse voltammetry at a hanging mercury drop electrode in the concentration range 1 . 10-4 to 2 . 10-7 mol l-1. A further increase in the sensitivity can be achieved through adsorptive accumulation of the test substance on the surface of a hanging mercury drop, permitting the determination to be extended to the concentration range 1 . 10-7 - 2 . 10-9 mol l-1.


1995 ◽  
Vol 60 (8) ◽  
pp. 1247-1260
Author(s):  
Jiří Barek ◽  
Roman Hrnčíř ◽  
Josino C. Moreira ◽  
Jiří Zima

The polarographic and voltammetric behaviour of the title compound, which is the basic component in many commercial optical whitening agents, was investigated. The optimum conditions were found for the determination of the substance in dimethylformamide solutions containing 5% (v/v) water by tast polarography, differential pulse polarography, linear sweep voltammetry using a hanging mercury drop electrode, and differential pulse polarography using a hanging mercury drop electrode over the concentration regions of 100-500, 10-500, 10-500, and 1-100 mmol l-1, respectively. Practical applicability of the newly developed methods to the determination of the analyte in technical products, either direct or following separation by thin layer chromatography, was verified.


1984 ◽  
Vol 49 (5) ◽  
pp. 1282-1288 ◽  
Author(s):  
Věra Stará ◽  
Miloslav Kopanica

The herbicide methomyl (2-methylthio-propionaldehyde-o-methylcarbamoyloxime) can be determined using fast scan differential pulse voltammetry with hanging mercury drop electrode by the measurement of the peak at -1.30 V (S.C.E.) which caused by the presence of methomyl in the ammoniacal buffer solution containing cobalt(II) salt. The peak current vs methomyl concentration dependence is linear over the concentration range 0.5 to 20.0 μg . l-1. The herbicide aldicarb (2-methyl-2(methylthio)propionaldehyde-o-methylcarbamoyloxime) is determined by its influence on the differential pulse voltammetric curve of copper(II) recorded in electrochemically enriched solution in acidic medium. The corresponding peak current at the potential + 0.08 V (S.C.E.) depends linearly on the aldicarb concentration in the range 0.07 to 5.00 μg ml-1.


Sign in / Sign up

Export Citation Format

Share Document