Cloud Point Extraction of Copper, Lead, Cadmium, and Iron Using 2,6-Diamino-4-Phenyl-1,3,5-Triazine and Nonionic Surfactant, and Their Flame Atomic Absorption Spectrometric Determination in Water and Canned Food Samples

2012 ◽  
Vol 95 (4) ◽  
pp. 1170-1175 ◽  
Author(s):  
Demirhan Citak ◽  
Mustafa Tuzen

Abstract A cloud point extraction procedure was optimized for the separation and preconcentration of lead(II), cadmium(II), copper(II), and iron(III) ions in various water and canned food samples. The metal ions formed complexes with 2,6-diamino-4-phenyl- 1,3,5-triazine that were extracted by surfactant-rich phases in the nonionic surfactant Triton X-114. The surfactant-rich phase was diluted with 1 M HNO3 in methanol prior to its analysis by flame atomic absorption spectrometry. The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, surfactant concentration, temperature, and incubation time, were optimized. LOD values based on three times the SD of the blank (3Sb) were 0.38, 0.48, 1.33, and 1.85 μg/L for cadmium(II), copper(II), lead(II), and iron(III) ions, respectively. The precision (RSD) of the method was in the 1.86–3.06% range (n = 7). Validation of the procedure was carried out by analysis of National Institute of Standards and Technology Standard Reference Material (NIST-SRM) 1568a Rice Flour and GBW 07605 Tea. The method was applied to water and canned food samples for determination of metal ions.

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.


2015 ◽  
Vol 52 (3) ◽  
pp. 178-186 ◽  
Author(s):  
Cennet Karadaş

A sensitive and simple cloud point extraction method was developed for simultaneous separation and preconcentration of cadmium and copper prior to their determination by flame atomic absorption spectrometry. 4-phenyl-3-thiosemicarbazide was used as complexing agent and the cadmium and copper complexes were extracted from the aqueous phase by Triton X-114 surfactant. The effects of parameters such as sample pH, ligand amount, concentration of surfactant, incubation temperature and time were optimized. For 20 mL of preconcentrated solution, the detection limits (3σ) were 0.20 and 0.49 μg L−1, and the enrichment factors were 20.7 and 19.9 for Cd(II) and Cu(II), respectively. In order to verify the accuracy of the developed method, certified reference materials (SLRS-5 river water and SPS-SW2 Batch 127 surface water) were analysed. Results obtained were in good agreement with the certified values. The proposed method was applied to tap water, river water and seawater samples with satisfactory results.


2012 ◽  
Vol 95 (6) ◽  
pp. 1797-1802 ◽  
Author(s):  
Mustafa Soylak ◽  
Erkan Yilmaz ◽  
Mehrorang Ghaedi ◽  
Mortaza Montazerozohori ◽  
Marjan Sheibani

Abstract A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2-(1E,1′E)-1,1′-(2,2′-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters—including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time—were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples.


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