scholarly journals Preconcentration and Spectrophotometric Determination of Copper and Nickel in some Medicinal PlantsafterCloud Point Extraction

Author(s):  
Azhar A Ghali ◽  
Ashwoq S Hussein

In this work,Cloud point extraction (CPE) methodology as an one green chemistry method is used for extraction, enrichment and determination ofNi (II) and Cu (II) in the somemedicinal plants,by use organic reagent2-[ (6-Methyl-2-Benzothiazolyl)azo]-4-Chloro Phenol (6-MeBTAClP) for formationthe extracted complexes into micelles of Triton X-114 as a mediated extractant at65,70 C0 respectively. The extracted product in densityhigh (cloud point layer )is separated from the aqueous layer by centrifugation for 15 min and dissolved in 0.5 mLfrom ethanol followed the determination of Ni (II) and Cu (II)by using spectrophotometry at a wavelength maximum of 644 and 598 nm respectively. The optimum conditions established as pH, The linear range of Ni (II) and Cu (II)along with limit of detection,precision expressed as relative standard deviation for seven replication measurements and the recovery range were obtained for Ni (II) and Cu (II) ions,respectively. The complex s identified by UV-Visible and IR spectra. The mole ratio method and continuous variation method (Job’s method)also investigated.

2016 ◽  
Vol 13 (2) ◽  
pp. 426-439
Author(s):  
Baghdad Science Journal

In this study, cloud point extraction combined with molecular spectrometry as an eco-friendly method is used for extraction, enrichment and determination of bendiocarb (BC) insecticide in different complex matrices. The method involved an alkaline hydrolysis of BC followed Emerson reaction in which the resultant phenol is reacted with 4-aminoantipyrene(4-AAP) in the presence of an alkaline oxidant of potassium ferric cyanide to form red colored product which then extracted into micelles of Triton X-114 as a mediated extractant at room temperature. The extracted product in cloud point layer is separated from the aqueous layer by centrifugation for 20 min and dissolved in a minimum amount of a mixture ethanol: water (1:1) followed the determination of BC by using spectrophotometry at a wavelength maximum of 470 nm. The most important parameters affecting the extraction and determination of BC are conducted via a classical optimization. Under the optimum conditions established , Beer’s law is obeyed in the range of 0.1-4 µg mL-1 while the optimum concentration ranges estimated by Ringbom’s plot was of 0.4-2.12 µg mL-1. The enrichment factor was of 59.87 fold leading to achieve the limit of detection of 0.076 ?g mL-1. The proposed method gives superior sensitivity in terms of the molar absorptivity of 1.99x105 L mol-1 cm-1 and extraction efficiency of 98.0%. The established method is applied in the analysis of the spiked vegetables, orange, soil and water samples with appropriate concentration with BC standard.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Mohammad Reza Jamali ◽  
Mohammad Gholinezhad ◽  
Saiedeh Balarostaghi ◽  
Reyhaneh Rahnama ◽  
Seyed Hojjat Allah Rahimi

A new, simple, and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of cobalt. The cobalt ions in the initial aqueous solution were complexed with 4-Benzylpiperidinedithiocarbamate, and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the cobalt content was measured by flame atomic absorption spectrometry. The main factors affecting CPE procedure, such as pH, concentration of ligand, amount of Triton X-114, equilibrium temperature, and incubation time were investigated and optimized. Under the optimal conditions, the limit of detection (LOD) for cobalt was 0.5 μg L-1, with sensitivity enhancement factor (EF) of 67. Calibration curve was linear in the range of 2–150 μg L-1, and relative standard deviation was 3.2% (c=100 μg L-1;n=10). The proposed method was applied to the determination of trace cobalt in real water samples with satisfactory analytical results.


2018 ◽  
Vol 5 (4) ◽  
pp. 171500 ◽  
Author(s):  
N. I. Mohd ◽  
N. N. M. Zain ◽  
M. Raoov ◽  
S. Mohamad

A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient ( R 2 ) in the range of 0.991–0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l −1 (atrazine) and 1.22 µg l −1 (propazine), and the limit of quantitation was 3.54 µg l −1 (atrazine) and 4.07 µg l −1 (propazine). Satisfactory recoveries in the range of 81–108% were determined in milk samples at 5 and 1000 µg l −1 , respectively, with low relative standard deviation, n  = 3 of 0.301–7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.


2013 ◽  
Vol 830 ◽  
pp. 345-348
Author(s):  
Lin Gao ◽  
Sheng Jie Chen ◽  
Fang Chen ◽  
Wen Hong Zhou ◽  
Jun Long Yao

A simple, sensitive, green and low cost detection method based on the cloud point extraction (CPE) separation and spectrophotometry was proposed for the determination of lead. In pH=9.0 H3BO3 buffer solution, Pb(II) reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) in the presence of Triton X-100 yielding a hydrophobic complex, which then is extracted into micro-volume surfactant-rich phase. The calibration graph was linear in the range of 20-400 µg/L (at 560 nm). Under the optimized conditions, the detection limits of 10.94 µg/L and the relative standard deviations(RSD) of 2.0% (n=5) for Lead(II) were found, respectively. The sensitivity and absorbance of this method are at least five times higher when compared with that of usual 5-Br-PADAP spectrophotometry without CPE, and the proposed method has been applied to the determination of Lead in environment water samples with satisfactory results.


2013 ◽  
Vol 699 ◽  
pp. 34-39
Author(s):  
Li Liu ◽  
Xia Shi Zhu

A new Triton X-114 cloud point extraction combined with fluorometry method for analysis of magnolol in drug samples was developed. Under the optimum conditions, the calibration graph was linear in the range of 2.0-150.0ng/mL of magnolol in the initial solution with r = 0.9998. Detection limit (DL) was 0.03ng/mL (S/N=3) and the relative standard deviation (RSD) for 20.0ng/mL of magnolol was 2.79%(n=11). The method was successfully applied for the determination of magnolol in drug samples with satisfactory results.


2021 ◽  
Vol 33 (10) ◽  
pp. 2472-2476
Author(s):  
Rajib Joarder

A simple, sensitive, quick, easy and efficient (SSQuEE) analytical technique based on cloud point extraction (CPE) has been developed for the determination of different pesticides present in soil and water with high performance liquid chromatography separation and ultraviolet detection. The environmentally friendliness surfactant like Triton X -100, compared to Tween series of non-ionic surfactant can effectively extract imidacloprid (insecticide), flusilazole (fungicide) and atrazine (herbicide) at cloud point temperature at 67 ºC, 82 ºC and 62 ºC, respectively. To reach the optimum extraction efficiency, different experimental parameters like surfactant concentration, salt type and its concentration, equilibrium time and temperature, pH were observed. At the optimum conditions, linear regression coefficient of the standard curves was greater than 0.9924. The limit of detection of imidacloprid, flusilazole and atrazine were 0.10 μg L-1, 0.24 μg L-1, 0.15 μg L-1 and recovery percent are 99.71 %, 88.1% and 89.74%, respectively.


2008 ◽  
Vol 59 (1) ◽  
pp. 3-7
Author(s):  
Aurora Reiss ◽  
Mihaela Mureseanu ◽  
Nicolae Muresan

5-Hydroxy-6-mercapto-benzo [a] phenazine (HMBP) is proposed as a sensitive and selective analytical reagent for the extractive spectrophotometric determination of copper (II). Copper reacts with HMBP to give a dark red complex which is soluble in chloroform. The composition of the CuII � HMBP complex is established as 1:2 by Job�s continuous variation method and molar ratio method. The instability constant of the complex calculated by Job�s relation for nonisomolar series is 4.65 . 10-9, at room temperature. The CuII-HMBP complex in chlorophorm shows a maximum absorbance at 495 nm, with molar absorptivity and Sandell�s sensitivity values of 7.39 . 103dm3 mol-1 cm-1 and 0.012 mg cm-2, respectively. Beer�s law is obeyed in the concentration range 0.67 - 26.90 mg mL-1 and the detection limit is 0.59 mg mL-1. A repetition of the method is checked by finding the relative standard deviation (RSD) at 1.00 mg mL-1 CuII of 0.6%. The method is successfully employed for the determination of copper (II) in environmental samples. The reliability of the method is assured by analysing the standard alloys and by inter-comparison of experimental values, using an atomic absorption spectrometer.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Mohammad Hosein Soruraddin ◽  
Rouhollah Heydari ◽  
Morteza Puladvand ◽  
Mir Mehdi Zahedi

A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL-1; the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL-1of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Naghi Saadatjou ◽  
Shahab Shariati ◽  
Mostafa Golshekan

A simple and high sensitive preconcentration method based on micelle-mediated extraction followed by high performance liquid chromatography (LC-UV) was developed for preconcentration and determination of trace amounts of bisphenol A (BPA) in aqueous samples. The BPA was quantitatively extracted from aqueous samples in the presence of Triton X-114 as a nonionic surfactant and preconcentrated into the small volume (about 30 μL) of the surfactant-rich phase. Taguchi method, an orthogonal array design (OA16 (45)), was utilized to optimize the various factors affecting the micellar extraction of BPA. The maximum extraction efficiency of BPA was obtained at pH 3, 0.2% (w/v) Triton X-114, and 0.25 mol L−1 sodium acetate. For the preconcentration, the solutions were incubated in a thermostatic water bath at 50°C for 7 min. After centrifuge and separation of aqueous phase, the surfactant-rich phase was diluted with 100 μL acetone and injected in the chromatographic system. Under the optimum conditions, preconcentration factor of 34.9 was achieved for extraction from 10 mL of sample solution and the relative standard deviation (RSD%) of the method was lower than 6.6%. The calibration curve was linear in the range of 0.5–150 μg L−1 with reasonable linearity (r2>0.9987). The limit of detection (LOD) based on S/N = 3 was 0.13 μg L−1 for 10 mL sample volumes. The limit of quantification (LOQ) based on S/N = 10 was 0.43 μg L−1 for 10 mL sample volumes. Finally, the applicability of the proposed method was evaluated by the extraction and determination of BPA in the real samples, and satisfactory results were obtained.


2012 ◽  
Vol 12 (1) ◽  
pp. 12-19 ◽  
Author(s):  
Dhananjay B Sarode ◽  
Sopan T Ingle ◽  
Sanjay B Attarde

A new method for determination of stoichiometry of colorless complexes by using atomic absorption spectrophotometric technique in continuous variation method and slope ratio method was described here. This method can be used in same manner as that of mole ratio method and slope ratio method. In this method atomic absorption spectroscopy was used instead of UV-Vis spectrophotometry. Atomic absorption spectrophotometric technique is superior to UV-Vis spectrophotometry as it can be applied to colorless soluble complexes. Pb(II) and n-benzoyl-n-phenyl hydroxylamine react to form colorless complex at pH 6.5, which can be easily determined by this method. It was found that Pb(II) forms 1:2 complex with n-benzoyl-n-phenyl hydroxylamine and is quantitatively extracted back to aqueous solution for AAS analysis.


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