Microchimica Acta

, Volume 171, Issue 3–4, pp 313–319 | Cite as

Determination of trace mercury in environmental samples by cold vapor atomic fluorescence spectrometry after cloud point extraction

Original Paper

Abstract

A sensitive method is presented for the determination of ultra-trace levels of mercury using cold vapor atomic fluorescence spectrometry along with cloud point extraction. Preconcentration is based on the complexation of Hg(II) by dithizone, followed by micelle-mediated extraction of the complex using the surfactant Triton X-114. Foaming, which is always observed when generating vapor mercury in the presence of surfactant, was strongly reduced by using SnCl2 as a reducing reagent, and a homemade gas–liquid separator. Variables that affect the assay were optimized. These included pH value, concentration of chelating reagent, concentration of Triton X-114, equilibration temperature and time. The preconcentration of a 45-mL sample gave an enhancement factor of 29. The calibration graph is linear in the range from 0.05 to 5.0 ng mL−1 with a correlation coefficient of 0.9991. The limit of detection (3δ) obtained under the optimal conditions is 5 pg mL−1. The relative standard deviation for seven replicate determinations at 0.5 ng mL−1 level is 5.2%. The method was successfully applied to the determination of Hg in real samples.

Keywords

Cloud point extraction Mercury Atomic fluorescence spectrometry 

Notes

Acknowledgement

This work was kindly co-funded by State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (KF2008-01), the Fundamental Research Funds for the Central Universities (10ZG01), the Program for New Century Excellent Talents in University (NCET-10-0341), the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry ([2009]1001) and the Natural Science Foundation of Hebei Province (B2010001676).

References

  1. 1.
    Tan ZQ, Liu JF, Liu R, Yin YG, Jiang GB (2009) Visual and colorimetric detection of Hg2+ by cloud point extraction with functionalized gold nanoparticles as a probe. Chem Commun 45:7030CrossRefGoogle Scholar
  2. 2.
    Chen HT, Chen JG, Jin XZ, Wei DY (2009) Determination of trace mercury species by high performance liquid chromatography–inductively coupled plasma mass spectrometry after cloud point extraction. J Hazard Mater 172:1282CrossRefGoogle Scholar
  3. 3.
    Chen JG, Chen HW, Jin XZ, Chen HT (2009) Determination of ultra-trace amount methyl-, phenyl- and inorganic mercury in environmental and biological samples by liquid chromatography with inductively coupled plasma mass spectrometry after cloud point extraction preconcentration. Talanta 77:1381CrossRefGoogle Scholar
  4. 4.
    Li P, Feng XB, Qiu GL, Shang LH, Li ZG (2009) Mercury pollution in Asia: a review of the contaminated sites. J Hazard Mater 168:591CrossRefGoogle Scholar
  5. 5.
    Liu GL, Cai Y, Philippi T, Kalla P, Scheidt D, Richards J, Scinto L, Appleby C (2008) Distribution of total and methylmercury in different ecosystem compartments in the Everglades: implications for mercury bioaccumulation. Environ Pollut 153:257CrossRefGoogle Scholar
  6. 6.
    Martinis EM, Berton P, Olsina RA, Altamirano JC, Wuilloud RG (2009) Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based preconcentration and flow injection-cold vapor atomic absorption spectrometry. J Hazard Mater 167:475CrossRefGoogle Scholar
  7. 7.
    Rodrigues JL, Torres DP, Souza VCD, Batista BL, de Souza SS, Curtius AJ, Barbosa F (2009) Determination of total and inorganic mercury in whole blood by cold vapor inductively coupled plasma mass spectrometry (CV ICP-MS) with alkaline sample preparation. J Anal At Spectrom 24:1414CrossRefGoogle Scholar
  8. 8.
    Aranda PR, Pacheco PH, Olsina RA, Martinez LD, Gil RA (2009) Total and inorganic mercury determination in biodiesel by emulsion sample introduction and FI-CV-AFS after multivariate optimization. J Anal At Spectrom 24:1441CrossRefGoogle Scholar
  9. 9.
    Pourreza N, Parham H, Kiasat AR, Ghanemi K, Abdollahi N (2009) Solid phase extraction of mercury on sulfur loaded with N-(2-chlorobenzoyl)-N ’-phenylthiourea as a new adsorbent and determination by cold vapor atomic absorption spectrometry. Talanta 78:1293CrossRefGoogle Scholar
  10. 10.
    Bagheri H, Naderi M (2009) Immersed single-drop microextraction–electrothermal vaporization atomic absorption spectroscopy for the trace determination of mercury in water samples. J Hazard Mater 165:353CrossRefGoogle Scholar
  11. 11.
    Leopold K, Foulkes M, Worsfold PJ (2009) Gold-coated silica as a preconcentration phase for the determination of total dissolved mercury in natural waters using atomic fluorescence spectrometry. Anal Chem 81:3421CrossRefGoogle Scholar
  12. 12.
    Bezerra MD, Arruda MAZ, Ferreira SLC (2005) Cloud point extraction as a procedure of separation and pre-concentration for metal determination using spectroanalytical techniques: a review. Appl Spectrosc Rev 40:269CrossRefGoogle Scholar
  13. 13.
    Ojeda CB, Rojas FS (2009) Separation and preconcentration by a cloud point extraction procedure for determination of metals: an overview. Anal Bioanal Chem 394:759CrossRefGoogle Scholar
  14. 14.
    Silva MF, Cerutti ES, Martinez LD (2006) Coupling cloud point extraction to instrumental detection systems for metal analysis. Microchim Acta 155:349CrossRefGoogle Scholar
  15. 15.
    Wang L, Cai YQ, He B, Yuan CG, Shen DZ, Shao J, Jiang GB (2006) Determination of estrogens in water by HPLC-UV using cloud point extraction. Talanta 70:47CrossRefGoogle Scholar
  16. 16.
    Yuan CG, Jiang GB, He B, Liu JF (2005) Preconcentration and determination of tin in water samples by using cloud point extraction and graphite furnace atomic absorption spectrometry. Microchim Acta 150:329CrossRefGoogle Scholar
  17. 17.
    Yuan CG, Jiang GB, Cai YQ, He B, Liu JF (2004) Determination of cadmium at the nanogram per liter level in seawater by graphite furnace AAS using cloud point extraction. At Spectrosc 25:170Google Scholar
  18. 18.
    Zhu X, Zhu X, Wang B (2006) Determination of trace cadmium in water samples by graphite furnace atomic absorption spectrometry after cloud point extraction. Microchim Acta 154:95CrossRefGoogle Scholar
  19. 19.
    Zhu X, Zhu Z, Wu S (2008) Determination of trace vanadium in soil by cloud point extraction and graphite furnace atomic absorption spectroscopy. Microchim Acta 161:143CrossRefGoogle Scholar
  20. 20.
    Liang P, Peng L (2010) Determination of silver(I) ion in water samples by graphite furnace atomic absorption spectrometry after preconcentration with dispersive liquid–liquid microextraction. Microchim Acta 168:45CrossRefGoogle Scholar
  21. 21.
    Bezerra MA, Conceição ALB, Ferreira SLC (2006) A pre-concentration procedure using cloud point extraction for the determination of manganese in saline effluents of a petroleum refinery by flame atomic absorption spectrometry. Microchim Acta 154:149CrossRefGoogle Scholar
  22. 22.
    Niazi A, Momeni-Isfahani T, Ahmari Z (2009) Spectrophotometric determination of mercury in water samples after cloud point extraction using nonionic surfactant Triton X-114. J Hazard Mater 165:1200CrossRefGoogle Scholar
  23. 23.
    Aranda PR, Gil RA, Moyano S, De Vito IE, Martinez LD (2008) Cloud point extraction of mercury with PONPE 7.5 prior to its determination in biological samples by ETAAS. Talanta 75:307CrossRefGoogle Scholar
  24. 24.
    Li YJ, Hu B (2007) Sequential cloud point extraction for the speciation of mercury in seafood by inductively coupled plasma optical emission spectrometry. Spectrochim Acta B 62:1153CrossRefGoogle Scholar
  25. 25.
    Manzoori JL, Abdolmohammad-Zadeh H, Amjadi M (2007) Ultra-trace determination of silver in water samples by electrothermal atomic absorption spectrometry after preconcentration with a ligand-less cloud point extraction methodology. J Hazard Mater 144:458CrossRefGoogle Scholar
  26. 26.
    Afkhami A, Madrakian T, Siampour H (2006) Highly selective determination of trace quantities of mercury in water samples after preconcentration by the cloud-point extraction method. Int J Environ Anal Chem 86:1165CrossRefGoogle Scholar
  27. 27.
    Garrido M, Di Nezio MS, Lista AG, Palomeque M, Band BSF (2004) Cloud-point extraction/preconcentration on-line flow injection method for mercury determination. Anal Chim Acta 502:173CrossRefGoogle Scholar
  28. 28.
    Shokrollahi A, Ghaedi M, Hossaini O, Khanjari N, Soylak M (2008) Cloud point extraction and flame atomic absorption spectrometry combination for copper(II) ion in environmental and biological samples. J Hazard Mater 160:435CrossRefGoogle Scholar
  29. 29.
    Fathi SAM, Yaftian MR (2009) Cloud point extraction and flame atomic absorption spectrometry determination of trace amounts of copper (II) ions in water samples. J Colloid Interface Sci 334:167CrossRefGoogle Scholar
  30. 30.
    Hiemenz PC, Rajagopalan RH (1997) Principles of colloid and surface chemistry, 3rd edn. Marcel Dekker, New York, p 377Google Scholar
  31. 31.
    Clint JH (1992) Surfactant aggregation. Blackie, Glasgow, p 154Google Scholar

Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  1. 1.School of Environmental Science & EngineeringNorth China Electric Power UniversityBaodingChina

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