The polarographic and voltammetric determination of 2-amino-5-sulphoamoylnaphthalene-azo-(2’-chloro-4’-nitrobenzene)

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.

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.


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.


1990 ◽  
Vol 55 (2) ◽  
pp. 379-390 ◽  
Author(s):  
Jiří Barek ◽  
Dagmar Civišová ◽  
Ashutosh Ghosh ◽  
Jiří Zima

The polarographic reduction of the title azo dye has been studied, a mechanism has been proposed and optimal conditions have been found for its analytical use. The detection limit using a classical dropping mercury electrode was 2 . 10-7 mol l-1 for TAST polarography and 1 . 10-8 mol l-1 for differential pulse polarography. Using a hanging mercury drop electrode, the detection limit was 9 . 10-9 mol l-1 for fast scan differential pulse voltammetry and 1 . 10-8 mol l-1 for linear scan voltammetry. Adsorption accumulation of the test substance on the surface of the hanging mercury drop electrode led to a further decrease in the detection limit to 1 . 10-9 mol l-1 for fast scan differential pulse voltammetry and 7 . 10-10 mol l-1 for linear scan voltammetry.


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.


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.


1992 ◽  
Vol 57 (11) ◽  
pp. 2263-2271
Author(s):  
Jiří Barek ◽  
Jana Kubíčková ◽  
Viktor Mejstřík ◽  
Jiří Zima

A study was made of the polarographic reduction of the title triazene, a mechanism was proposed for this process and optimal conditions were found for its analytical application using tast polarography in the range 1 . 10-4 - 2 . 10-6 mol l-1, differential pulse polarography in the range 1 . 10-4 - 2 . 10-7 mol l-1 and fast scan differential pulse voltammetry at a hanging mercury drop electrode in the range 1 . 10-4 - 2 . 10-7 mol l-1. The sensitivity of the latter technique was increased through adsorptive accumulation of the test substance on the surface of the working electrode, permitting determination in the concentration range 1 . 10-7 - 2 . 10-9 mol l-1.


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.


1988 ◽  
Vol 53 (5) ◽  
pp. 921-928
Author(s):  
Jiří Barek ◽  
Janina Balsiene ◽  
Barbara Tietzová ◽  
Jiří Zima

The reduction of mutagenic bisazodye trypane blue has been studied at a mercury electrode, a mechanism has been proposed and optimal conditions found for its analytical application. The use of a dropping mercury electrode with a renewable surface yielded a detection limit of 8 . 10-7 mol l-1 for TAST polarography, and 8 . 10-8 mol l-1 for differential pulse polarography; the use of a hanging mercury drop electrode with an unrenewed surface during the measurement yielded detection limit of 6 . 10-8 mol l-1 for fast scan differential pulse voltammetry and 4 . 10-8 mol l-1 for linear scan voltammetry. Preliminary adsorptive accumulation of the determined substance on the surface of the hanging mercury drop electrode led to a decrease in the detection limit to 5 . 10-9 mol l-1 for linear scan voltammetry.


1987 ◽  
Vol 52 (1) ◽  
pp. 81-87 ◽  
Author(s):  
Jiří Barek ◽  
Dagmar Civišová

The polarographic reduction of the title azodye has been studied, a mechanism has been proposed for this process and conditions have been found for the determination of this substance by TAST polarography, with a detection limit of 7 . 10-7 mol l-1, differential pulse polarography at a dropping mercury electrode with a detection limit of 3.5 . 10-7 mol l-1, fast scan differential pulse voltammetry at a static mercury drop electrode with a detection limit of 6.9 . 10-9 mol l-1 and voltammetry with linearly increasing voltage at a hanging mercury drop with a detection limit of 1.6 . 10-9 mol l-1.


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