Polarographic determination of some nitro group-containing pesticides

1983 ◽  
Vol 48 (9) ◽  
pp. 2636-2643 ◽  
Author(s):  
Hana Beňadiková ◽  
Milan Popl ◽  
Věra Jakubíčková

The differential pulse polarography technique was applied to the determination of some pesticides containing nitro groups in their molecules. The nitro groups were found to be reduced to hydroxylamines or to the corresponding amines. The effect of medium, particularly of pH of the supporting electrolyte, was examined. The pesticides were determined in concentrations less than 10 μg l-1, which shows primose for the application of the technique to environmental water purity monitoring.

Author(s):  
M. Nogami Eurica ◽  
M. Dalmeida Gracinda ◽  
Jorge Nozaki

Differential pulse polarography was employed for the determination of arsenic in bituminous coal from Figueiras, Parana, Brazil. The dried coal sample was crushed to -100 mesh, ashed, and treated with reducing reagents in acidic media. The arsine generated was collected and selectively oxidized to Al +3 using an absorbing solution of 0.1 mol.L -1 [tris(hydroxymethyl) aminomethane] ( TRIS) and 0. 002 mol.L -1 silver nitrate. A solution of TRIS and hydrochloric acid, pH -1, was used as supporting electrolyte for differential pulse polarographic determination of Al+3 in the concentration range 0.05 -0.60 μglmL. The average arsenic concentration found was 69.0 ± 2.6 mg.kg -1 and was in agreement with the spectrophotometric method using silver-diethyldithiocarbamate-pyridine.


2001 ◽  
Vol 84 (1) ◽  
pp. 47-52 ◽  
Author(s):  
Anju Bhalotra ◽  
Bal Krishan Prui

Abstract A differential pulse polarographic method is proposed for the trace determination of bismuth and copper from large volumes of aqueous samples after adsorption of their 1-(2-thiazolylazo)-2-naphthol complexes onto microcrystalline naphthalene in the pH ranges of 7.2–9.0 and 4.0–7.8, respectively. Bismuth and copper are desorbed from microcrystalline naphthalene with 9 mL 1M HCl. Well-defined peaks are obtained at Ep = −0.09 and −0.20 V versus a saturated calomel electrode, in an HCl–isoquinoline medium as the supporting electrolyte, for bismuth and copper, respectively. Bismuth is reduced reversibly with a 3-electron change, whereas copper is reduced irreversibly under these conditions. The detection limits are 55 ng/mL for bismuth and 91 ng/mL for copper. Linearity is maintained in the concentration ranges of 0.18–13.5 and 0.30-17.3 μg/mL for bismuth and copper, respectively, with corresponding correlation coefficients of 0.9996 and 0.9885. The relative standard deviations are 1.0% for bismuth at 2.0 μg/mL and 1.4% for copper at 5.0 μg/mL. Various parameters were optimized to develop conditions for the determination of these metal ions in various samples.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Chennupalle Nageswara Reddy ◽  
Puthalapattu ReddyPrasad ◽  
NeelamYughandhar Sreedhar

The electrochemical reduction of zanosar was investigated systematically by direct current polarography, cyclic voltammetry, and differential pulse polarography (DPP). A simple DPP technique was proposed for the direct quantitative determination of anticancer drug zanosar in pharmaceutical formulation and spiked human urine samples for the first time. The reduction potential was −0.28 V versus Ag/AgCl with a hanging mercury drop electrode in Britton-Robinson buffer as supporting electrolyte. The dependence of the intensities of currents and potentials on pH, concentration, scan rate, deposition time, and nature of the supporting electrolyte was investigated. The calibration curve was found to be linear with the following equation:y=0.4041x+0.012, with a correlation coefficient of 0.992 (R2) over a concentration range from1.0×10-7 M to1.0×10-3 M. In the present investigation, the achieved limit of detection (LOD) and limit of quantization (LQD) were7.42×10-8 M and2.47×10-8 M; respectively. Excipients did not interfere with the determination of zanosar in pharmaceutical formulation and spiked urine samples. Precision and accuracy of the developed method were checked by recovery studies in pharmaceutical formulation and spiked human urine samples.


1985 ◽  
Vol 50 (8) ◽  
pp. 1673-1684
Author(s):  
Jiří Barek ◽  
Ivo Daňhel

Conditions are sought for the determination of 4-nitrotoluene-2-sulphonic acid (I) and 4,4'-dinitrostilbene-2,2'-disulphonic acid (II) by TAST polarography within the concentration range of 10-2 - 10-6 mol l-1 and by differential pulse polarography (DPP) within the concentration range of 10-3 - 10-8 mol l-1. DPP is applied to the determination of these substances after the thin layer chromatographic separation of their mixtures. Methods are also worked out for their analysis without prior separation, based either on the combined DPP determination of I and the TAST polarographic determination of the sum of I and II in sulphuric acid solutions, or on the DPP determination of the C=C bond in II and the TAST polarographic determination of the sum of the two substances in tetramethylammonium bromide solutions.


1984 ◽  
Vol 67 (4) ◽  
pp. 684-687
Author(s):  
Mohamed E Mohamed ◽  
Abdel-Aziz M Wahbi ◽  
EL Rasheed A Gad-Kariem ◽  
Mahmoud M A Hassan

Abstract Tiaprofenic acid (Surgam®) has been determined directly by using differential pulse polarography (DPP) and pH 5.5 acetate buffer as a supporting electrolyte. The differential pulse polarogram was obtained under constant amplitude pulses of 50 mV superimposed on a linearly increasing dc ramp. Peak current was measured at the peak potential of — 0.990 V vs Ag/AgCl reference electrode. Under the experimental conditions used, a linear relationship between peak current and concentration was established over the range 0.5-5.0 ng/mL. Mean percentage recoveries for tiaprofenic acid in authentic and tablet forms were 100.27 ± 2.25 and 99.45 ± 1.44, respectively. The results obtained by the DPP method were compared with those of the spectrophotometric method used by the manufacturer for the analysis of tiaprofenic acid and its tablet form.


1995 ◽  
Vol 60 (5) ◽  
pp. 802-812
Author(s):  
Jiří Barek ◽  
Roman Hrnčíř ◽  
Josino C. Moreira

The polarographic behaviour of the title optical whitening agent was studied in aqueous-methanolic solutions. Conditions for its quantitation were found within the concentration regions of 10 to 100 μmol l-1 by tast polarography, 1 to 100 μmol l-1 by differential pulse polarography on the conventional dropping mercury electrode, and 0.1 to 10 μmol l-1 by differential pulse polarography on a static mercury drop electrode. The analytical procedures developed were applied to the determination of the compound in technical products.


1992 ◽  
Vol 57 (11) ◽  
pp. 2248-2262 ◽  
Author(s):  
Jiří Barek ◽  
Dana Dřevínková ◽  
Jiří Zima ◽  
Arnold Fogg

A study has been made of the polarographic behaviour of genotoxic 1-[4'-(phenylazo)phenyl]-3,3-dimethyltriazene in mixed water-methanol medium. A mechanism has been proposed for its polarographic reduction and optimal conditions have been found for its determination by tast polarography in the concentration range 1 . 10-4 - 2 . 10-6 mol l-1 and using differential pulse polarography in the concentration range 1 . 10-4 - 2 . 10-7 mol l-1.


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