scholarly journals Optimization of cloud point extraction procedure with response surface methodology for quantification of iron by means of flame atomic absorption spectrometry

2013 ◽  
Vol 78 (1) ◽  
pp. 115-127 ◽  
Author(s):  
Hossein Abdolmohammad-Zadeh ◽  
Abdolhossein Naseri ◽  
Golamhossein Sadeghi

A simple micelle-mediated phase separation method has been developed for the pre-concentration of trace levels of iron as a prior step to determination by flame atomic absorption spectrometry (FAAS). The method is based on the cloud point extraction (CPE) of iron using non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5) without adding any chelating agent. Several variables affecting the extraction efficiency were studied and optimized utilizing central composite design (CCD) and three levels full factorial design. Under the optimum conditions, the limit of detection (LOD), limit of quantification (LOQ) and pre-concentration factor were 1.5 ?g L-1, 5.0 ?g L-1 and 100, respectively. The relative standard deviation (RSD) for six replicate determinations at 50 ?g L?1 Fe(III) level was 1.97%. The calibration graph was linear in the rage of 5-100 ?g L-1, with a correlation coefficient of 0.9921. The developed method was validated by the analysis of two certified reference materials and applied successfully to the determination of trace amounts of Fe(III) in water and rice samples.

2014 ◽  
Vol 70 (4) ◽  
pp. 605-611 ◽  
Author(s):  
Jinyan Ning ◽  
Yang Jiao ◽  
Jiao Zhao ◽  
Lifen Meng ◽  
Yaling Yang

A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium (Cd) as a prior step to its determination by flame atomic absorption spectrometry has been developed. Cadmium reacted with 8-hydroxyquinoline to form hydrophobic chelates, which were extracted into the micelles of nonionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) in an alkaline medium. Octanol was used to depress the cloud point of Genapol X-080 in the extraction process. The chemical variables that affect the CPE, such as pH of complexation reaction, amount of chelating agent, Genapol X-080 and octanol were evaluated and optimized. Under optimized conditions, linearity was obeyed in the range of 10–500 μg/L, with the correlation coefficient of 0.9993. For 5 mL of sample solution, the enhancement factor was about 20. The limit of detection and limit of quantification of the method were 0.21 and 0.63 μg/L, respectively. The relative standard deviations (n = 6) was 3.2% for a solution containing 100 μg/L of Cd. The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. Recoveries of spiked samples varied in the range of 94.1–103.8%.


2014 ◽  
Vol 70 (12) ◽  
pp. 1913-1918 ◽  
Author(s):  
Lifen Meng ◽  
Jinyan Ning ◽  
Yaling Yang

A sensitive and simple method for flame atomic absorption spectrometry determination of traces of cadmium and chromium(III) species in water samples after preconcentration by cloud point extraction has been developed. A novel complex agent of alizarin complexone with cadmium (Cd) and chromium (Cr(III)) was quantitatively extracted in surface primary alcohol ethoxylate-rich phase at 33 °C. The effects of experimental conditions including pH of sample solution, concentration of chelating agent and salt, equilibration temperature and time, and foreign ions were evaluated in order to enhance sensitivity of the method. Under optimal conditions, the low limit detections were 6.7 and 3.2 μg/L, and the enrichment factors were 24 and 20 for Cd and Cr(III), respectively. The relative standard deviations were 3.8 and 2.5% for Cd and Cr(II), respectively (n = 11). The high recoveries of the spiked Cd and Cr(III) ions were obtained in the range of 90–116%. The proposed method has been successfully applied for the determination of Cd and Cr(III) in water samples.


2019 ◽  
Vol 9 (22) ◽  
pp. 4752 ◽  
Author(s):  
Ayman H. Kamel ◽  
Abd El-Galil E. Amr ◽  
Mohamed A. Al-Omar ◽  
Elsayed A. Elsayed

The cloud point extraction (CPE) method was successfully used for the isolation and pre-concentration of ultra-low concentration of Pb prior to its determination by flame atomic absorption spectrometry (FAAS). Lead(II) reacts with methyl 4,20-diisobutyl-2,5,8,16,19,22- hexaoxo-7,17-dipropyl-3,6,9,15,18,21-hexaaza-1(2,6)-pyridinacyclo-docosaphane-10-carboxylate (DLNL) as chelating agent in the presence of octylphenoxypolyethoxyethanol (Triton X-114) as a nonionic surfactant giving a surfactant-rich phase chelate which could be used for CPE. Factors affecting the CPE such as solution pH, concentrations of the chelating ligand and surfactant, temperature of equilibration, and time were optimized. The efficacy features of the proposed protocol such as linear range, lower limit of detection, pre-concentration, and progress factors were evaluated. The method revealed a wide linear range in the range of 7–250 ng/mL of Pb2+ with a limit of detection of 5 ng/mL using FAAS. Validation of the presented protocol revealed good performance characteristics including high between-batch repeatability, high precision, wide linear range, low limit of detection, and acceptable accuracy. The presented procedure was successfully introduced for the separation and quantification of lead (II) in wastewater samples with acceptable results.


2010 ◽  
Vol 7 (3) ◽  
pp. 278-283
Author(s):  
F. Ahmadia ◽  
A. Khanmohammadi ◽  
A. Malekpour

A cloud point extraction method was presented for preconcentration of copper in various samples. After complexation with 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP) or N-Benzoyl-N-phenylhydroxylamine (BPA)  in water, analyte ions are quantitatively extracted to the phase rich in Triton X-114 after centrifugation. 2.0 mol L-1 HNO3 solution in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for ADPP, Triton X-114, HNO3 and parameters such as bath temperature, centrifuge rate and time were optimized. Detection limits (3SDb/m) of 1.3 and 1.9 ng mL-1 for ADPP and BPA along with enrichment factors of 30 and 38 for ADPP and BPA were achieved. The high efficiency of cloud point extraction to carry out the determination of analyte in complex matrices was demonstrated. The proposed method was applied to the analysis of biological, industrial, natural and wastewater, soil and blood samples.   Keywords: 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP), N-Benzoyl-N-phenylhydroxylamine (BPA) ,   Cloud Point Extraction, Triton X-114, Flame Atomic Absorption Spectrometry.


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