Preconcentration and Determination of Lead for Trace Levels in Water and Wastewater Samples by Vortex-Assisted Microextraction Using TPAS as a New Synthetic Complexing Agent with Electrothermal Atomic Absorption Spectroscopy Detection

Document Type: Research Article

Authors

1 Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad, I.R. IRAN

2 Department of Chemistry, Faculty of Samen Hojaj, Technical and Vocational University, Tehran, I.R. IRAN

3 Department of Environmental Protection (DEP) of Razavi Khorasan Province, Mashhad, I.R. IRAN

Abstract

A simple and rapid solidified vortex assisted 1-undecanol based liquid-liquid microextraction technique was proposed for preconcentration of trace levels of lead ions. The extraction solvent (1-undecanol) was dispersed into the aqueous samples by the assistance of vortex agitator. 100 µL of 1-undecanol containing ethyl (2Z)-3-[(5-chloro-7-methyl[1,3]thiazolo[5,4-d]pyrimidin-2-yl)amino]-2-cyano-3-(methylsulfanyl)prop-2-enoate (TPAS) as a new chelating agent (0.1%w/v) was transferred to the water samples containing lead ions. The hydrophobic complex was extracted into 1-undecanol and the sample vial was cooled in an ice bath for 5 min.The solidified extract was transferred into a conical vial where it was melted immediately, and 20 µL of this solution was injected and analyzed by Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Several variables such as sample pH, the concentration of TPAS, volume of 1-undecanol and extraction time were investigated in details and optimum conditions were obtained. Under the optimum conditions, the Limit Of Detection (LOD) was 0.02 µg L-1 for lead and Relative Standard Deviation (RSD %) for five replicate determinations of 1 µg/L of lead was 5.6%. The results for determination of lead in reference material, three samples of wastewater, well, tap, river and aqueduct water demonstrated the accuracy, recovery, and applicability of the presented method.

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[2] Chen J. R., Xiao S.M., Wu X. H., Fang K., Liu W., Determination of Lead in Water Samples by Graphite Furnace Atomic Absorption Spectrometry After Cloud Point Extraction, Talanta., 67, 992-996 (2005). 

[3] Moreira F. R., Borges R. M., Oliveira R. M., Comparison of Two Digestion Procedures for the Determination of Lead in Lichens by Electrothermal Atomic Absorption Spectrometry, Spectrochim. Acta B., 60, 755- 781    (2005).

[4]  Baird C., "Environmental Chemistry", Freeman W. H. and Company, New York (1999).

[6]  Ndungu K., Hibdon S., Flegal A. R., Determination of Lead in Vinegar by ICP-MS and GFAAS: Evaluation of Different Sample Preparation Procedures, Talanta., 64: 258- 263 (2004).

[7]  Dos Santos W. L., Dos Santos C. M. M.,  Costa J. L. O., Andrade H. M. C., Ferreira S. L. C., Multivariate Optimization and Validation Studies in On-Line Pre-Concentration System for Lead Determination in Drinking Water and Saline Waste from Oil Refinery, Microchem. J., 77: 123-129 (2004).

[10] Li Z.J., Tang J., Pan. J.M., The determination of Lead in Preserved Food by Spectrophotometry with Dibromohydroxyphenylporphyrin, Food Control., 15: 565- 570 (2004).

[11] Di Nezio M. S., Palomeque M. E., Fernandez Band B. S., A Sensitive Spectrophotometric Method for Lead Determination by Flow Injection Analysis with On-Line Preconcentration, Talanta., 63: 405-409 (2004).

[12] Liu H.G., Dasgupta P.K., Analytical Chemistry in a Drop, Solvent Extraction in a Microdrop, Analytical Chemistry Anal. Chem., 68: 1817-1825 (1996).

[13] Jeannot M.A., Cantwell F.F., Solvent Microextraction into a Single Drop, Analytical  Chemistry Anal. Chem., 68:  2236-2241 (1996).

[16] Ghiasvand A. R., Shadabi S., Mohagheghzadeh E., Hashemi P., Homogeneous Liquid–Liquid Extraction Method for the Selective Separation and Preconcentration of Ultra Trace Molybdenum, Talanta., 66: 912- 916 (2005).

[18] Rezaee M., Assadi Y., Milani Hosseini M.R., Aghaee E., Ahmadi F., Berijani S., Determination of Organic Compounds in Water Using Dispersive Liquid Liquid Microextraction, J. Chromatogr. A., 1116: 1-9 (2006).

[21] Khalili Zanjani M. R., Yamini Y., Shariati S., Jonsson J. A., A New Liquid-Phase Microextraction Method Based on Solidification of Floating Organic Drop, Anal. Chim. Acta., 585: 286-293 (2007).

[22] Karimian A., Esghi H., Shiri M., Bakavoli A., Heterocycl,commun, 20,p. 275 (2014).

[23] Jones R.G., Reactions of Orthoesters with Active Methylene Compounds, J, Am. Chem. Soc, 74: 4889-4891 (1952).

[27] Cai Y., Jiang G., Liu J., Liang X., Solid Phase Extraction of Trace Amounts of Lead Derivatized with 8-Hydroxyquinoline Using a GC Stationary Phase Mini-Column Packed with Chromosorb 105, At. Spectrosc, 23: 52-61 (2002).

[29] Chen J., Xiao S., Wu X., Fang K., Liu W., Determination of Lead in Water Samples by Graphite Furnace Atomic Absorption Spectrometry After Cloud Point Extraction, Talanta, 67: 992- 996 (2005).