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Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials

School of Chemistry and Chemical Engineering, Henan University of Technology, South Song Shan Road No. 140, Zhengzhou City 450001, PR China.
Journal of hazardous materials (Impact Factor: 4.33). 10/2009; 175(1-3):146-50. DOI: 10.1016/j.jhazmat.2009.09.141
Source: PubMed

ABSTRACT A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by l-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3 sigma) of the proposed method was 0.02 ng mL(-1) for antimony(III), and the relative standard deviation was 7.8% (c=1.0 ng mL(-1), n=7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results.

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    • "Cloud-point extraction (CPE) is an alternative approach that avoids the use of toxic solvents, by exploiting a nonionic surfactant to extract the hydrophobic species incorporated in the micelle aggregates formed when the surfactant is at an appropriate concentration and temperature [3] [19] [20] [21] [22] [23] [24]. To avoiding tedious and time-consuming manual extraction, CPE has been coupled with flow analysis, which improves precision and sample throughput, and minimizes waste generation [20] [25]. "
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    DESCRIPTION: Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H+ followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L−1, described by the equation A=0.137+0.050 CSb (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L−1) and the sampling rate were estimated at 1.8 µg L−1, 1.6% and 16 h−1, respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L−1) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level.
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    • "Cloud-point extraction (CPE) is an alternative approach that avoids the use of toxic solvents, by exploiting a nonionic surfactant to extract the hydrophobic species incorporated in the micelle aggregates formed when the surfactant is at an appropriate concentration and temperature [3] [19] [20] [21] [22] [23] [24]. To avoiding tedious and time-consuming manual extraction, CPE has been coupled with flow analysis, which improves precision and sample throughput, and minimizes waste generation [20] [25]. "
    [Show description] [Hide description]
    DESCRIPTION: Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H+ followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L−1, described by the equation A=0.137+0.050 CSb (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L−1) and the sampling rate were estimated at 1.8 µg L−1, 1.6% and 16 h−1, respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L−1) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level.
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    • "Cloud-point extraction (CPE) is an alternative approach that avoids the use of toxic solvents, by exploiting a nonionic surfactant to extract the hydrophobic species incorporated in the micelle aggregates formed when the surfactant is at an appropriate concentration and temperature [3] [19] [20] [21] [22] [23] [24]. To avoiding tedious and time-consuming manual extraction, CPE has been coupled with flow analysis, which improves precision and sample throughput, and minimizes waste generation [20] [25]. "
    [Show abstract] [Hide abstract]
    ABSTRACT: Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H+ followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 μg L-1, described by the equation A = 0.137 + 0.050 CSb (r = 0.998). The detection limit (99.7% confidence level), the coefficient of variation (n = 5; 15 μg L-1) and the sampling rate were estimated at 1.8 μg L-1, 1.6 % and 16 h-1, respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 μg L-1) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level.
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