Cloud point extraction for preconcentration of Pb II , Fe III , Cr III and determination by flame atomic absorption spectrometry

Abstract

Acloud point extraction CPE method for preconcentration of Pb II , Fe III and Cr III has been established. This is based on the complexation of the metal ions with p-nitrophenylazoresorcinol Magneson I at pH 6.5 in the presence of non-ionic surfactant of octylphenoxy polyethoxyethanol Triton X-114 , prior to their determination by flame atomic absorption spectrometry FAAS . The main factors affecting CPE efficiency, such as sample pH, complexing agent concentration, Triton X-114 concentration, temperature and incubation time were investigated. Under the optimized conditions, the detection limits 3s, n = 10 of Pb II , Cr III and Fe III were 2.5, 2.3 and 1.9 μg L-1, respectively. The relative standard deviation for ten replicate determinations of the analytes was less than 2.4%. The validation of the procedure was carried out by analysis of certified reference materials. The proposed method has been applied to the determination of lead, chromium and iron in tap water and some food samples.

Keywords

• cloud point extraction,preconcentration of lead,iron,chromium,FAAS

Pb II , Fe III , Cr III ’ün önderiştirilmesi için bulutlanma noktası ekstraksiyonu ve alevli atomik absorpsiyon spektrometresi ile tayini

Abstract

P b II , Fe III ve Cr III ’ün önderiştirilmesi için bulutlanma noktası ekstraksiyonu CPE yöntemi geliştirilmiştir. Bu yöntem, alevli atomik absorpsiyon spektrometresi FAAS ile metal iyonlarının tayininden önce, non-iyonik yüzey aktif madde Triton X-114 varlığında, pH 6.5 de, metal iyonlarının p-nitrofenilazoresorsinol Magneson I ile kompleks oluşturması temeline dayanmaktadır. CPE verimini etkileyen pH, kompleksleştirici madde derişimi, Triton X-114 derişimi, sıcaklık ve inkübasyon süresi gibi temel etkenler incelenmiştir. Optimum koşullarda, Pb II , Cr III ve Fe III için gözlenebilme sınırı 3s, n = 10 sırasıyla 2.5, 2.3 ve 1.9 µg L-1 dir. On tekrarlı ölçümlere ait bağıl standart sapma %2.4 den daha düşüktür. Yöntemin doğruluğunun belirlenmesi için sertifikalı referans maddelerin analizi yapılmıştır. Önerilen yöntem, musluk suyu ve bazı gıda numunelerinde kurşun, krom ve demir tayini için uygulanmıştır

Keywords

• Bulutlanma noktası ekstraksiyonu,kurşun,demir,krom önderiştirilmesi,FAAS

References

1. I. Jaric, Z.V. Jeftic, G. Cvijanovic, Z. Gacic, L. Jovanovic, S. Skoric, M. Lenhardt, Determination of differential heavy metal and trace element accumulation in liver, gills, intestine and muscle of sterlet (acipenser ruthenus) from the Danube river in serbia by ICP-OES, Microchemical Journal, 98 (2011) 77.
2. P.T. Lieu, M. Heiskala, P.A. Peterson, Y. Yang, The roles of iron in health and disease, Molecular Aspects of Medicine, 22 (2001) 1.
3. WHO (World Health Organization), http://www.who. int/water_sanitation_health/dwq/chemicals/iron.pdf, Accessed 15.04.13,2008, 2.
4. T. Oymak, Ş. Tokalıoğlu, V. Yılmaz, Ş. Kartal, D. Aydın, Determination of lead and cadmium in food samples by the coprecipitation method, Food Chemistry, 113 (2009) 1314.
5. S.G. Özcan, N. Şatiroğlu, M. Soylak, Column solid phase extraction of iron(III), copper(II), manganese(II) and lead(II) ions food and water samples on multi-walled carbon nanotubes, Food and Chemical Toxicology, 48 (2010) 2401.
6. S. Saçmacı, S. Kartal, M. Saçmacı, Selective separation and preconcentration of Fe(III) and Zn(II) ions by solvent extraction using a new triketone reagent, Clean - Soil, Air, Water, 39 (2011) 584.
7. J. Chen, K.C. Teo, Determination of cadmium, copper, lead and zinc in water samples by flame atomic absorption spectrometry after cloud point extraction, Analytica Chimica Acta, 450 (2001) 215. J.L.
8. Manzoori, A.B. Tabrizi, Cloud point preconcentration and flame atomic absorption spectrometric determination of Cd and Pb in human hair, Analytica Chimica Acta, 470 (2002) 215.

9. N. Şatıroğlu, Ç. Arpa, Cloud point extraction for the determination of trace copper in water samples by flame atomic absorption spectrometry, Microchimica Acta, 162 (2008) 107.
10. M. Ghaedi, H. Tavallali, A. Shokrollahi, M. Zahedi, K. Niknam, M. Soylak, Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry, Clean, 37 (2009) 328.
11. D. Citak, M. Tuzen, A novel preconcentration procedure using cloud point extraction for determination of lead, cobalt and copper in water and food samples using flame atomic absorption spectrometry, Food and Chemical Toxicology, 48 (2010) 1399.
12. Z. Wang, F. Zhao, D. Li, Determination of solubilization of phenol at coacervate phase of cloud point extraction, Colloids and Surfaces A, 216 (2003) 207.
13. M. Dakiky, I. Nemcova, Aggregation of o,o- dihydroxy azo dyes III. Efect of cationic, anionic and non-ionic surfactants on the electronic spectra of 2-hydroxy-5- nitrophenylazo- 4-[3-methyl-1-(400-sulfophenyl)-5- pyrazolone, Dyes and Pigments, 44 (2000) 181.
14. M.S. Masoud, H.H. Hammud, H. Beidas, Dissociation constants of eriochrome Black T and eriochromeblue black RC indicators and the formation constants of their complexes with Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II), and Pb(II), under different temperatures and in presence of different solvents, Thermochimica Acta, 381 (2002) 119.
15. A.E. Visser, S.T. Griffin, D.H. Hartman, R.D. Rogers, Naphthol and resorcinol based azo dyes as metal ion complexants in aqueous biphasic systems, Journal of Chromatography B, 743 (2000) 107.
16. R. Carballo, A. Castineiras, B. Covelo, J. Niclos, E.M. Vazquez-Lopez, Synthesis and characterization of a potassium complex of magneson: [K(HL)(OH)] HL=4-(4-nitrophenylazo) resorcinol (magneson)], Polyhedron, 20 (2001) 2415. ¥
17. Z. Marczenko, M. Balcerzak, Separation and spectrophotometric determination of elements, second edition, New York: Elsevier, Chapter 4, 2000.
18. K. Alizadeh, B. Rezaei, B. Maddah, Spectrophotometric determination of aqueous acidity constants of three azo dyes, Central European Journal of Chemistry, 8 (2010) 392.
19. J. Kotas, Z. Stasicka, Chromium occurrence in the environment and methods of its speciation, Environmental Pollution, 107 (2000) 263.
20. H. Filik, B.D. Öztürk, M. Doğutan, G. Gümüş, R. Apak, Separation and preconcentration of iron(II) and iron(III) from natural water on a melamine- formaldehyde resin, Talanta, 44 (1997) 877.
21. M.A. Radwan, A.K. Salama, Market basket survey for some heavy metals in Egyptian fruits and vegetables, Food and Chemical Toxicology, 44 (2006) 1273.
22. Turkish Official Gazette, Regulation of setting maximum levels for certain contaminants in foodstuffs, Iss:24908, October 16, 2002.
23. Ş. Tokalıoğlu, F. Gürbüz, Selective determination of copper and iron in various food samples by the solid phase extraction, Food Chemistry, 123 (2010) 183.
24. S.M. Abdel-Azeem, N.R. Bader, H.M. Kuss, M.F. El- Shahat, Determination of total iron in food samples after flow injection preconcentration on polyurethane foam functionalized with N,N-bis(salicylidene)-1,3- propanediamine, Food Chemistry, 138 (2013) 1641.
25. S. Candir, I. Narin, M. Soylak, Ligandless cloud point extraction of Cr(III), Pb(II), Cu(II), Ni(II), Bi(III), and Cd(II) ions in environmental samples with Tween and flame atomic absorption spectrometric determination, Talanta, 77 (2008) 289.
26. M. Ghaedi, A. Shokrollahi, K. Niknam, E. Niknam, A. Najibi, M. Soylak, Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples, Journal of Hazardous Materials, 168 (2009) 1022.
27. M. Ghaedi, A. Shokrollahi, K. Niknam, M. Soylak, Cloud point extraction of copper, zinc, iron and nickel in biological and environmental samples by flame atomic absorption spectrometry, Separation Science and Technology, 44 (2009) 773.
28. G.D. Matos, E.B. dos Reis, A.C.S. Costa, S.L.C. Ferreira, Speciation of chromium in river water samples contaminated with leather effluents by flame atomic absorption spectrometry after separation/ preconcentration by cloud point extraction, Microchemical Journal, 92 (2009) 135.