scholarly journals Preconcentration of Bismuth(III) and Copper(II) by Solid-Phase Extraction and Subsequent Determination by Differential Pulse Polarography

2001 ◽  
Vol 84 (1) ◽  
pp. 47-52 ◽  
Author(s):  
Anju Bhalotra ◽  
Bal Krishan Prui
Keyword(s):  
Solid Phase ◽  
Supporting Electrolyte ◽  
Saturated Calomel Electrode ◽  
Correlation Coefficients ◽  
Differential Pulse ◽  
Differential Pulse Polarography ◽  
Pulse Polarography ◽  
Relative Standard ◽  
Microcrystalline Naphthalene

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.

scholarly journals Differential Pulse Polarographic Determination of Lead in Complex Materials after Adsorption of Its N-Methylethylxanthocarbamate Complex on Microcrystalline Naphthalene or on NMethylethylxanthocarbamate–Benzyldimethyltetradecylammonium–Naphthalene Adsorbent

2002 ◽  
Vol 85 (3) ◽  
pp. 712-718
Author(s):  
Mohammad Farid Hussain ◽  
Anil Kumar Sangahi ◽  
Iqbal Ahmad ◽  
Bal Krishan Puri
Keyword(s):  
Flow Rate ◽  
Signal To Noise Ratio ◽  
Differential Pulse ◽  
Correlation Factor ◽  
Differential Pulse Polarography ◽  
Pulse Polarography ◽  
Relative Standard ◽  
Ph Range ◽  
Microcrystalline Naphthalene

Abstract Lead is quantitatively adsorbed as the lead N-methylethylxanthocarbamate (MEXC)–benzyldimethyltetradecylammonium (BDTA) ion pair complex on microcrystalline naphthalene in the pH range 4.0–11.0. The metal is desorbed with HCl and determined by differential pulse polarography. Alternatively lead can be quantitatively adsorbed on the adsorbent (MEXC–BDTA–naphthalene) packed in a column at a flow rate of 1–2 mL/min and determined similarly. Dissolved oxygen is removed by adding a few milliliters of 4% NaBH4 solution. The detection limit is 0.12 μg/mL at the minimum instrumental settings (signal-to-noise ratio, 2). Linearity was obtained over the concentration range 0.3–20.0 μg/mL with a correlation factor of 0.9998 and a relative standard deviation of ± 0.98%. Various parameters, such as the effect of pH, volume of aqueous phase, flow rate, and the interference of a large number of metal ions and anions, were studied in detail to optimize the conditions for the trace determination of lead in various standard alloys, standard biological materials, and environmental samples.

Polarographic and Voltammetric Determination of Trace Amounts of 3-Nitrofluoranthene

2006 ◽  
Vol 71 (11-12) ◽  
pp. 1571-1587 ◽  
Author(s):  
Karel Čížek ◽  
Jiří Barek ◽  
Jiří Zima
Keyword(s):  
River Water ◽  
Solid Phase ◽  
Mercury Electrode ◽  
Stripping Voltammetry ◽  
Differential Pulse ◽  
Differential Pulse Polarography ◽  
Pulse Polarography ◽  
Dropping Mercury Electrode ◽  
Separation And Preconcentration

The polarographic behavior of 3-nitrofluoranthene was investigated by DC tast polarography (DCTP) and differential pulse polarography (DPP), both at a dropping mercury electrode, differential pulse voltammetry (DPV) and adsorptive stripping voltammetry (AdSV), both at a hanging mercury drop electrode. Optimum conditions have been found for its determination by the given methods in the concentration ranges of 1 × 10-6-1 × 10-4 mol l-1 (DCTP), 1 × 10-7-1 × 10-4 mol l-1 (DPP), 1 × 10-8-1 × 10-6 mol l-1 (DPV) and 1 × 10-9-1 × 10-7 mol l-1 (AdSV), respectively. Practical applicability of these techniques was demonstrated on the determination of 3-nitrofluoranthene in drinking and river water after its preliminary separation and preconcentration using liquid-liquid and solid phase extraction with the limits of determination 4 × 10-10 mol l-1 (drinking water) and 2 × 10-9 mol l-1 (river water).

scholarly journals DIFFERENTIAL PULSE POLAROGRAPHIC DETERMINATION OF ARSENIC IN BITUMINOUS COAL

1998 ◽  
Vol 6 (7) ◽  
pp. 27-32
Author(s):  
M. Nogami Eurica ◽  
M. Dalmeida Gracinda ◽  
Jorge Nozaki
Keyword(s):  
Coal Sample ◽  
Bituminous Coal ◽  
Supporting Electrolyte ◽  
Arsenic Concentration ◽  
Differential Pulse ◽  
Polarographic Determination ◽  
Differential Pulse Polarography ◽  
Acidic Media ◽  
Pulse Polarography

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.

scholarly journals Electrochemical Analysis of Antichemotherapeutic Drug Zanosar in Pharmaceutical and Biological Samples by Differential Pulse Polarography

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Chennupalle Nageswara Reddy ◽  
Puthalapattu ReddyPrasad ◽  
NeelamYughandhar Sreedhar
Keyword(s):  
Human Urine ◽  
Supporting Electrolyte ◽  
Differential Pulse ◽  
Pharmaceutical Formulation ◽  
Urine Samples ◽  
Differential Pulse Polarography ◽  
Human Urine Samples ◽  
Pulse Polarography ◽  
Spiked Human Urine

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.

Rapid Differential Pulse Polarographic Determination of Tiaprofenic Acid

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
Keyword(s):  
Supporting Electrolyte ◽  
Tiaprofenic Acid ◽  
Reference Electrode ◽  
Differential Pulse ◽  
Differential Pulse Polarography ◽  
Experimental Conditions ◽  
Tablet Form ◽  
Peak Current ◽  
Pulse Polarography

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.

Collaborative Study of the Differential Pulse Polarographic Analysis of Cacodylate Injections

1977 ◽  
Vol 60 (5) ◽  
pp. 1015-1017
Author(s):  
Walter Holak
Keyword(s):  
Supporting Electrolyte ◽  
Collaborative Study ◽  
Standard Addition ◽  
Differential Pulse ◽  
Magnesium Nitrate ◽  
Differential Pulse Polarography ◽  
Pulse Polarography ◽  
Trivalent State ◽  
Cacodylic Acid ◽  
Relative Standard

Abstract Samples containing cacodylate are heated with magnesium nitrate to decompose the cacodylate moiety, releasing pentavalent arsenic. The arsenic is reduced to the polarographically active trivalent state by heating with hydrobromic acid and hydrazine sulfate. Differential pulse polarography is performed in a 1M HQ supporting electrolyte, using a standard addition method for quantitation. The results from 6 collaborators showed an average of 97.00% of declared potency for commercial ampoules, with a relative standard deviation of 2.99%. Two synthetic cacodylic acid solutions prepared to contain 9.01 and 30.02 mg/ml gave averages of 100.03 and 99.38% of amount added, with relative standard deviations of 1.56 and 1.42%, respectively. The method has been adopted as official first action.

Determination of Arsenic and Selenium in Foods By Electroanalytical Techniques

1976 ◽  
Vol 59 (3) ◽  
pp. 650-654 ◽  
Author(s):  
Walter Holak
Keyword(s):  
Stripping Voltammetry ◽  
Differential Pulse ◽  
Magnesium Nitrate ◽  
Differential Pulse Polarography ◽  
Cathodic Stripping Voltammetry ◽  
Pulse Polarography ◽  
Trivalent State ◽  
Relative Standard ◽  
Cathodic Stripping

Abstract Arsenic and selenium are determined in foods by differential pulse polarography and cathodic stripping voltammetry. The sample is digested with nitric acid and magnesium nitrate and then dissolved in dilute hydrochloric acid. An aliquot is removed, the arsenic is chemically reduced to the trivalent state, and interferences are removed by ion exchange before polarography. Selenium is determined in a second aliquot by cathodic stripping voltammetry. Recoveries for both elements in several foods were from 90 to 110%. The relative standard deviations for arsenic at 5 ppm and selenium at 0.48 ppm were 5.8 and 7.3%, respectively.

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