scholarly journals DEVELOPMENT AND VALIDATION OF DIFFERENTIAL PULSE ANODIC STRIPPING VOLTAMMETRIC ANALYSIS OF SELENIUM (IV) IN BULK AND IN DOSAGE FORMULATIONS AT A GOLD ELECTRODE MULTI-MODIFIED WITH A MIXTURE OF 3, 3′-DIAMINOBENZIDINE.4HCL AND VITAMIN E

Author(s):  
Abdul Azizs Ramadan ◽  
Hasna Mandil ◽  
Abdulrahman Shikh-debes

Objective: A simple, direct and very sensitive differential pulse anodic stripping voltammetric analysis (DPASVA) of selenium (IV) in bulk and in dosage formulations using a gold electrode multi-modified with a mixture of 3,3′-diaminobenzidine.4HCl (Dab) and vitamin E (VE)-Nafion (AuEMDabVEN) has been studied.Methods: The method involves the study of various parameters (electrolyte, deposition time, pulse duration, pulse amplitude, etc.) affecting the Se(IV) determination. The proposed method was validated for specificity, linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ), robustness and solution stability with an average recovery of 98.1-100.32%.Results: Se(IV)was determined in an aqueous HClO4 (0.2M) medium of pH 0.22 at an accumulation potential of-250 mV and an accumulation time of 200 s for CSe(IV) at 1x10-8 to 1x10-6 mol/l (0.7896-78.96 ng/ml) and 350 s for CSe(IV) at 1x10-9 to 1x10-8 mol/l (0.07896-0.7896 ng/ml) with relative standard deviations (RSD)2.4% and 4.8%, respectively.Conclusion: This method showed very sensitive results for the determination of Se(IV) using an AuEMDabVEN than that obtained using the individual Dab or VE. This method could be applicable for the quantitative determination of the bulk Se(IV) as well as dosage formulations.

2018 ◽  
Vol 15 (2) ◽  
pp. 6248-6261 ◽  
Author(s):  
Abdul Aziz Ramadan ◽  
Hasna Mandil ◽  
Abdulrahman Shikh-Debes

The effect of gold electrode modified with 2,3-Diaminonaphthalene (GEMDANN) or multi-modified or a mixture 2,3-diaminonaphthalene and o-phenylenediamine -nafion (GEMDAN-OPDAN) on determination of selenium (IV) using differential pulse anodic stripping voltammetric analysis (DPASVA) has been studied. Various parameters (electrolyte, deposition time, pulse duration, pulse amplitude, etc.) are affecting determination of the Se(IV) in HClO4 (0.2 M) at pH 0.22 were examined. Under the optimum conditions, liner calibration graph, Ip=f(CSe4+), were obtained in the concentration ranges of 5x10-8 - 1x10-6 M (3.948 -78.96 ng.mL-1 ) with relative standard deviations (RSD) 4.2% and detection limit 0.056 ng.mL-1, and 1x10-9 -1x10-6 M (0.07896 -78.96 ng.mL-1 ) with relative standard deviations (RSD) 4.9% and detection limit was 0.014 ng.mL-1 on GEMDANN and GEMDAN-OPDAN, respectively. This method showed a good accumulation efficiency for selenium and good resistance to interferences from metal ions as well as those associated with selenium in pharmaceuticals. The results for the determination of Se4+ using GEMDAN-OPDAN (multi-modified) were more sensitive (about 50 times) than that obtained using GEMDANN.


1982 ◽  
Vol 65 (4) ◽  
pp. 987-991 ◽  
Author(s):  
R Duane Satzger ◽  
Charles S Clow ◽  
Evelyn Bonnin ◽  
Fred L Fricke

Abstract A method is described for the simultaneous determination of ultratrace levels of lead and cadmium in selected agricultural crop samples by differential pulse anodic stripping voltammetry. Samples are dry ashed at high temperature with H2SO4 as an ashing aid. Techniques are described to control the lead and cadmium blank levels of 2 ng and 0.4 ng, respectively. Typical relative standard deviations for the crop analyses are 13% at 100 ng/g and 25% at 10 ng/g for lead, and 5% at 100 ng/g and 10% at 10 ng/g for cadmium. The lowest quantifiable level, based on 3 g dry sample, is 2 ng/g for lead and 1 ng/g for cadmium. Recovery studies, precision studies, and analyses of NBS Standard Reference Materials demonstrate the accuracy and reproducibility of this technique. A summary of results for over 1700 crop samples is reported.


2014 ◽  
Vol 15 (1&2) ◽  
pp. 195-199
Author(s):  
Udit Mohan ◽  
Randhir Singh ◽  
Prem Singh ◽  
Suhas N. ◽  
Poonam Kashyap Prusty ◽  
...  

In the present communication determination of Zn, Cd, Pb and Cu metals has been carried out from ground water of Hapur District, Uttar Pradesh (India) using differential pulse anodic stripping voltammetry (DPASV) at Hanging Mercury Dropping Electrode (HMDE). Determination of Zn, Cd, Pb and Cu was carried out by using acetate solution as buffer (pH 4.6) with a sweep rate of 0.06 V/sec and pulse amplitude 0.05 V by HMDE by standard addition method. The minimum level of Zn, Cd, Pb and Cu should also be near to zero and the concentration found in the ground water sample of Hapur (India) as analyzed 2.1834, 0.0509, 0.0116 and 0.0331mg/L-1 respectively.


2010 ◽  
Vol 6 (1) ◽  
pp. 855-860
Author(s):  
Tarik Attar ◽  
Nouria Dennouni Medjati ◽  
Yahia Harek ◽  
Lahcene Larabi

An electroanalytical method has been developed for the determination of zinc in whole blood by differential pulse anodic stripping voltammetry (DPASV) on a hanging mercury drop electrode (HMDE). The best conditions were found to be electrolyte support perchloric acid 0.02M, an accumulation potential of -1150 mV, and an accumulation time of 60 s. The optimum value of stirring rate was determined to be 400 rpm. The correlation coefficient and relative standard deviation were 0.9999 and 3.96% respectively with a detection limit of 0.86 µg L-1. Zinc levels in whole blood samples of 53 healthy subjects living in Tlemcen (west Algeria).


2019 ◽  
Vol 2019 ◽  
pp. 1-11 ◽  
Author(s):  
Nguyen Mau Thanh ◽  
Nguyen Van Hop ◽  
Nguyen Dinh Luyen ◽  
Nguyen Hai Phong ◽  
Tran Thanh Tam Toan

The simultaneous electrochemical determination of Zn(II), Cd(II), Pb(II), and Cu(II) in the aqueous solution has been developed on the basis of the bismuth film glassy carbon electrode (GCE) using differential pulse anodic stripping voltammetry (DP-ASV). The bismuth film electrode (BiFE) was prepared by adding 500 ppb bismuth(III) directly to the sample solution and simultaneously depositing bismuth and the metal analytes on GCE. The optimal operational parameters, namely, accumulation potential (–1.6 V), accumulation time (110 s), pulsed amplitude (0.07 V), and scan rate (0.021 V·s−1), were found using a Box–Behnken design. Under the optimum conditions, a linear relationship exists between the current and the concentration of Zn(II), Cd(II), Pb(II), and Cu(II) in the range between 5.0 ppb and 110.0 ppb with the detection limits of 1.07 for Zn(II), 0.93 ppb for Cd(II), 0.65 ppb for Pb(II), and 0.94 ppb for Cu(II) calculated on the basis of a signal-to-noise ratio equal to 3 (S/N = 3). The interference experiments show that Co(II), Ni(II), and Fe(III) have a little influence on the DP-ASV signals of Zn(II), Cd(II), Pb(II), and Cu(II). In addition, a high reproducibility was indicated from small relative standard deviations (1.03%, 1.74%, 1.32%, and 4.74%) for 25 repeated measurements of 15 ppb copper, lead, cadmium, and zinc solutions. BiFE was successfully applied to determine Zn(II), Cd(II), Pb(II), and Cu(II) in river samples, and the results are in a good agreement with those determined with graphite furnace atomic absorption spectrometry (GF-AAS).


1984 ◽  
Vol 49 (1) ◽  
pp. 45-50 ◽  
Author(s):  
Alireza Aliakbar ◽  
Milan Popl

The use of differential pulse anodic stripping voltammetry in the determination of heavy metals (Cd, Pb, Cu, As) in foodstuffs was studied. Preconcentrating from solutions and dissolution took place on a thin film mercury electrode. A factorial experiment served to determine the effects of variable parameters of the apparatus, a polarographic analyzer: pulse amplitude, pulse period, and potential scan of the working electrode during dissolution. The first two parameters are significant but the scan rate is not. The apparatus parameters were optimized further by the method of response surface fitting near optimum.


2010 ◽  
Vol 9 (2) ◽  
pp. 243-246
Author(s):  
Saryati Saryati

The direct determination of some metals impurity in uranium by using differential pulse anodic stripping voltammetry (DPASV) method at a hanging mercury drop electrode and in a carbonate buffer media was developed. It was found that the carbonate buffer show the strongest affinity for uranium and gives the best separation between the DPASV peaks of heavy metals impurities. The carbonate concentration markedly affects the oxidation and reduction the major and the minor constituents of the uranium samples. In 0.1 M carbonate buffer solution pH 10, copper, bismuth, thalium, lead, cadmium, zinc, could be determined without the removal of the uranium matrix. Recovery and relative standard deviation (RSD) of this method was in the range of 174% - 85.2% for recovery and 36.8% - 1.2% for RSD. The larger error of analytical result was obtained for Zn at low concentration. In general, the analytic results error and RSD decreased with increasing metals concentration.   Keywords: heavy metal determination, differential pulse anodic stripping voltammetry, uranium


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