scholarly journals THE OPTIMATION SIMULTANEUOS DETERMINATION OF LEAD(II) AND CADMIUM(II) BY ADSORPTIVE STRIPPING VOLTAMMETRY (ADSV)

2012 ◽  
Vol 5 (2) ◽  
pp. 100
Author(s):  
Deswati ◽  
Hamzar Suyani ◽  
Umiati Loekman ◽  
Nilam Sari

A selective and sensitive adsorptive stripping voltammetric (AdSV) method for simultaneous determination of lead(II) and cadmium(II) were proposed. The aim of this study was to get the optimum condition for simultaneuos determination of lead(II) and cadmium(II). The parameters were studied such as: variation of accumulation potential, accumulation time, pH, and variation ofcalcon concentration. In this case, the optimum conditions were reached at accumulation potential –0.7 V, accumulation time 80 s, concentration of 0.12 mM calcon, and pH 7.0. At the optimumconditions the relative standard deviation were 2.90% and 1.46% for Pb(II) and Cd(II) respectively for eight replicates (n = 8) measurements. The method was applied for the direct determination of Pb(II) and Cd(II) in sea water around Bungus, Padang City. Concentration Pb(II) and Cd(II) insample were 9.918 μg/L – 27.320 μg/L for Pb(II) and 7.997 μg/L - 32.521 μg/L for Cd(II), with recovery of 99.48%, and 103.28 for Pb(II), and Cd(II) respectively.

2015 ◽  
Vol 3 (1) ◽  
pp. 22
Author(s):  
Deswati ◽  
Hamzar Suryani ◽  
Imelda ◽  
Yulia

 ABSTRACT Study of optimation chromium (VI) in sea water by adsorptive stripping voltammetry has been done. The aim of this method to get optimum conditions for determination of Cr(VI). Adsorptive stripping voltammetry (AdSV) has been used for the ultra trace determination of chromium using 2,2’- bipyridin as ligand. Parameters were done, like accumulation time, concentration of ligand, pH, accumulation potential, electrolyte concentration and catalyst concentration. In this case, the optimum conditions were reached in accumulation time 80 second, pH 5.0, concentration of 2,2’- bipyridin 10 μM, accumulation potential -0,6 Volt and electrolyte concentration (NH4Cl) 0,1 M. In the optimum conditions, a linear calibration graph was obtained with correlation coefficient of 0.9971, the relative standard deviation was 15.06 % for eight replicates (n = 8) measurements of 10 μg/L of Cr(VI). The detection limit method was 0.1692 μg/L. The method was applied to the direct determination of Cr(VI) in sea water around Muara Padang water. Concentration Cr(VI) in sample was equal to 0.9684 μg/L with recovery of 90.23 %. Keywords : optimation, chromium, adsorptive, stripping, voltammetry


2015 ◽  
Vol 3 (2) ◽  
pp. 122
Author(s):  
Deswati Deswati ◽  
Hamzar Suyani ◽  
Citra Buhatika

  ABSTRACT Study of optimation cadmium(II) by adsorptive stripping voltammetry has been done. The aim of this study to get optimum conditions for determination of Cd(II). Parameters were done : potential accumulation, time accumulation, pH, supporting electrolite concentration and optimum of complex concentration. In this case, the optimum conditions were reached in potential accumulation -0.7 V, time accumulation 60 second, pH 7.0, NH4Cl 0.12 M, calcon concentration 0.12 mM. In the optimum condition was obtained with the relative standard deviation was 4.61% for eight replicates, measurements of 0.01 ppm. The method was applied to the direct determination of Cd(II) in water around Batang Air Dingin Lubuk Minturun and Muara Padang. Concentration Cd(II) in sample was equal to 7.359 μg/L and 3.659 μg/L with recovery of 99.04%. Keywords: cadmiun, adsorptive, stripping, voltammetry


2013 ◽  
Vol 13 (3) ◽  
pp. 236-241 ◽  
Author(s):  
Deswati Deswati ◽  
Hamzar Suyani ◽  
Safni Safni ◽  
Umiati Loekman ◽  
Hilfi Pardi

A selective and sensitive adsorptive stripping voltammetric (AdSV) procedure for the simultaneous determination of cadmium, copper and lead in the sea water was conducted. The aim of this research is to get optimum condition for simultaneous determination of cadmium, copper and lead. Adsorptive stripping voltammetry has been used for determination of trace amount of Cd(II), Cu(II) and Pb (II) by using calcon as a complexing agent. The parameters studied were variation of calcon concentration, pH, accumulation potential and accumulation time. In this study, the optimum conditions were calcon concentration of 0.6 mM, pH = 4.0, accumulation potential of -0.7 V and accumulation time of 80 sec. At the optimum conditions, the relative standard deviation were 8.78%, 3.12%, and 4.02% for Cd(II), Cu(II) and Pb(II) respectively for eight replicates (n = 8) measurements of 10 μg/L mixed standard solution of Cd(II), Cu(II) and Pb(II). The method was applied to the direct simultaneous determination of Cd(II), Cu(II) and Pb(II) in sea water around Bungus, Padang City. Concentration of Cd(II), Cu(II) and Pb(II) in samples were equal to 1.8 μg/L for Cd(II), 38.6 μg/L for Cu(II) and 0.7 μg/L for Pb(II) with recovery of 87.03%, 98.80%, and 95.73%, respectively.


2012 ◽  
Vol 12 (1) ◽  
pp. 20-27 ◽  
Author(s):  
Deswati Deswati ◽  
Hamzar Suyani ◽  
Safni Safni

A sensitive and selective absorptive stripping voltammetric (AdSV) method to determine Cd(II), Cu(II), Pb(II) and Zn(II) in sea water is proposed. The aim of this study was to get optimum condition for the determination of Cd(II), Cu(II), Pb(II) and Zn(II). Absorptive stripping voltammetry has been used for ultra trace determination of Cd(II), Cu(II), Pb(II) and Zn(II) using calcon as a complexing agent (ligand). In this case, the optimum conditions were reached at 0.1 M KCl supporting electrolyte, concentration of 0.5 mM calcon for Cd(II), Cu(II) 0.3 mM while 0.7 mM for Pb(II) and Zn(II), pH 6 for Cu(II) and pH 7 for Cd(II), Pb(II) and Zn(II), accumulation potential -0.5 V for Cu(II) and Pb(II) and -0.6 V for Cd(II) and Zn(II) and accumulation time 70 sec for Cd(II), 90 sec for Cu(II) and Pb (II) while 50 s for Zn(II). At the optimum condition the relative standard deviations were 7.80%, 4.25%, 8.70% and 0.86% for Cd(II), Cu(II), Pb(II) and Zn(II) respectively for eight replicates (n = 8) measurements of 10 μg/L Cd(II), Cu(II), Pb(II) and Zn(II). The method was applied for the direct determination of Cd(II), Cu(II), Pb(II) and Zn(II) in sea water around Bungus, Padang City. Concentration Cd(II), Cu(II), Pb(II) and Zn(II) in sample were 13.200 μg /L for Cd(II), 17.200 μg/L for Cu(II), 0.089 μg/L for Pb(II) and 62.000 μg/L for Zn(II) with recovery of 98.68%, 97.99%, 96.17% and 99.96% for Cd(II), Cu(II), Pb(II) and Zn(II), respectively.


2021 ◽  
Vol 324 ◽  
pp. 01001
Author(s):  
Hilfi Pardi ◽  
Friska S Silitonga ◽  
Eka P Ramdhani ◽  
Dina Fitriyah

The research on the determination of Cd(II) metal in river and seawater samples using the Adsortive Cathodic Stripping Voltammetry (AdCSV) method has been done. In order to increase the sensitivity and selectivity of Cd(II) measurement, it is necessary to determine the optimum condition for the variation of potential ligand accumulation, accumulation time, pH and optimum ligand concentration. It is also determined the accuracy and precision of the method used by determining the value of the relative standard deviation (SDR), as well as the recovery value. The result obtained is chalcone as the optimum ligand, the optimum accumulation potential is -0.1 V, the optimum accumulation time is 60 seconds, the optimum solution pH is 6, and the optimum chalcone concentration is 0.5 mM. The relative standard deviation value is 4.27%, the recovery value is 98.31%. The application of the VSAd method to water sample results the concentration of Cu(II) metal in the sample of Bangek river, Indonesia is 4.778 g/L and seawater in Teluk Kabung, Indonesia is 5.189 g/L.


2008 ◽  
Vol 73 (1) ◽  
pp. 97-106 ◽  
Author(s):  
Ljubiša M. Ignjatović ◽  
Jiří Barek ◽  
Jiří Zima ◽  
Milica C. Stević

The optimum conditions were found for the determination of 1,1-dimethyl-3-phenyltriazene in the concentration range from 1 × 10-4 to 1 × 10-7 mol l-1 by differential pulse voltammetry at a hanging mercury drop electrode. The sensitivity of the determination can be improved by preliminary adsorptive accumulation of the substance on the surface of the hanging mercury drop. Differential pulse adsorptive stripping voltammetry can be used for the purpose in the concentration range from 1 × 10-6 to 1 × 10-9 mol l-1. The determination limit is 1 × 10-9 mol l-1 for a deposition time of 10 min, the relative standard deviation being 5% (n = 10) for a concentration of 2 × 10-9 mol l-1.


2009 ◽  
Vol 74 (4) ◽  
pp. 599-610 ◽  
Author(s):  
Mohammad Bagher Gholivand ◽  
Alireza Pourhossein ◽  
Mohsen Shahlaei

A sensitive and selective procedure is presented for the voltammetric determination of lead. The procedure involves an adsorptive accumulation of lead L-3-(3,4-dihydroxyphenyl)alanine (LDOPA) on a hanging mercury drop electrode, followed by a stripping voltammetric measurement of reduction current of an adsorbed complex at –0.15 V (vs Ag|AgCl). Optimum conditions for lead analysis include pH 8.5, 80 μM LDOPA and accumulation potential –0.15 V (vs Ag|AgCl). The peak currents are proportional to the lead concentration 1–300 nmol l–1 with a detection limit of 0.6 nmol l–1 and accumulation time 60 s. The method was used for the determination of lead in blood, dry tea and also in waters.


1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Sabah Shiri ◽  
Tahere Khezeli ◽  
Shahram Lotfi ◽  
Sina Shiri

A novel, simple, and more sensitive spectrophotometric procedure has been developed for the determination of brilliant blue FCF in water and food samples by an aqueous two-phase system (ATPS). In this method, adequate amount of polyethylene glycol/ sodium carbonate (PEG-4000/Na2CO3) was added to aqueous solution for formation of a homogeneous solution. To the mixture solution, suitable amount ofNa2CO3was added, the mixture solution was shaken until the salt was dissolved, and then it was separated into two clear phases easily and rapidly. The target analyte in the water sample was extracted into the polyethylene glycol phase. After extraction, measuring the absorbance at 634 nm was done. The effects of different parameters such as polyethylene glycol (type and concentration), pH, salt (type and amount), centrifuge time, and temperature on the ATPS of dye was investigated and optimum conditions were established. Linear calibration curves were obtained in the range of 0.25–750 ng/mL for brilliant blue FCF under optimum conditions. Detection limit based on three times the standard deviation of the blank (3Sb) was 0.12 ng/mL. The relative standard deviation (RSD) for 400 ng/mL was 3.14%. The method was successfully applied to the determination of brilliant blue FCF in spiked samples with satisfactory results. The relative recovery was between 96.0 and 102.2%.


2014 ◽  
Vol 1030-1032 ◽  
pp. 301-304 ◽  
Author(s):  
Jian Qi Sun

An novel Lead (II)-dithizone-xylenol orange tenary complex spectrophotometry was developed for the determination of Pb2+ in wastewater. For this purpose, the parameters of spectrophotometry such as the detection wavelength, pH value, the dosage of dithizone-xylenol orange and reaction time were studied and optimized through orthogonal tests. The method was linear in the ranges from 2.1×10-3 to 6.0 μg·mL-1 for Pb2+ with R2≥ 0.999. The procedure allowed efficient recovery of the investigated Pb2+ ranging between 95 % and 103 % with a relative standard deviation (RSD) ≤ 2.1 for actual wastewater samples spiked with 1.00, 2.00 and 3.00 μg·mL-1 of standard Pb2+, respectively. These results show the method can be applied to the direct determination of Pb2+ in wastewater, avoiding the use of toxic extrant (chloroform) and masking reagent (sodium cyanide) in the traditional methods and time-consuming procedures, moreover, the investigated method is simple, accurate, reliable, and inexpensive, which implies the potential of this technique for Pb2+ monitoring in wastewater samples.


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