Skip to main content
SpringerLink
Log in

Solid phase extraction and preconcentration of trace mercury(II) from aqueous solution using magnetic nanoparticles doped with 1,5-diphenylcarbazide

  • Original Paper
  • Published:
Microchimica Acta Aims and scope Submit manuscript

Abstract

A new method for solid-phase extraction and preconcentration of trace mercury(II) from aqueous solution was developed using 1,5-diphenylcarbazide doped magnetic Fe3O4 nanoparticles as extractant. The surface treatment did not result in the phase change of Fe3O4. Various factors which influenced the recovery of the analyte were investigated using model solutions and batch equilibrium technique. The maximum adsorption occurred at pH > 6, and equilibrium was achieved within 5 min. Without filtration or centrifugation, these mercury loaded nanoparticles could be separated easily from the aqueous solution by simply applying an external magnetic field. At optimal conditions, the maximum adsorption capacity was 220 μmol g−1. The mercury ions can be eluted from the composite magnetic particles using 0.5 mol L−1 HNO3 as a desorption reagent. The detection limit of the method (3σ) was 0.16 μg L−1 for cold vapor atomic absorption spectrometry, and the relative standard deviation was 2.2%. The method was validated by the analysis of a certified reference material with the results being in agreement with those quoted by manufactures. The method was applied to the preconcentration and determination of trace inorganic mercury(II) in natural water and plant samples with satisfactory results.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6

Similar content being viewed by others

References

  1. Aravindhan R, Madhan B, Rao J (2004) Bioaccumulation of chromium from tannary wastewater: an approach for chrome recovery and reuse. Environ Sci Technol 38:300

    Article  CAS  Google Scholar 

  2. Ayuso E, Sanchez A, Querol X (2003) Purification of metal electroplating waste waters using zeolites. Water Res 37:4855

    Article  Google Scholar 

  3. Thurman EM, Mills MS (1998) Solid-phase extraction: principles and practice. Wiley, New York, p 98

    Google Scholar 

  4. Fang G, Tan J, Yan X (2005) An ion-imprinted functionalized silica fel aorbent prepared by a surface imprinting technique combined with a sol-gel process for selective solid-phase extraction of cadmium(II). Anal Chem 77:1734

    Article  CAS  Google Scholar 

  5. Mohamed EM (1999) Selective solid phase extraction of mercury(II) by silica gel immobilized dithiocarbamate derivatives. Anal Chim Acta 398:297

    Article  Google Scholar 

  6. Emteborg H, Baxter DC, Frech W (1993) Speciation of mercury in natural water by capillary gas chromatography with a microwave-induced plasma emission detector following preconcentration using a dithiocarbamate resin microcolumn installed in a closed flow injection system. Analyst 118:1007

    Article  CAS  Google Scholar 

  7. Matilde FG, Rosario PG, Nerea BG, Alfredo SM (1994) On-line preconcentration of inorganic mercury and methylmercury in sea-water by sorbent-extraction and total mercury determination by cold vapour atomic absorption spectrometry. Talanta 41:1833

    Article  Google Scholar 

  8. Elamahadi HAM, Greenway GM (1993) Immobilized cysteine as a reagent for preconcentration of trace metals prior to determination by atomic absorption spectrometry. J Anal At Spectrom 8:1011

    Article  Google Scholar 

  9. Zhai Y, Chang X, Cui Y, Lia N, Lai S (2006) Selective determination of trace mercury(II) after preconcentration with 4-(2-pyridylazo)-resorcinol-modified nanometer-sized SiO2 particles from sample solutions. Microchim Acta 154:253

    Article  CAS  Google Scholar 

  10. Mohamed EM, Maher MO, Mohamed EA (2000) Selective pre-concentration and solid phase extraction of mercury(II) from natural water by silica gel-loaded dithizone phases. Anal Chim Acta 415:33

    Article  Google Scholar 

  11. Mohamed EM, Gamal AG (2000) Silica gel-immobilized-dithioacetal derivatives as potential solid phase extractors for mercury(II). Talanta 51:77

    Article  Google Scholar 

  12. Ezzat MS, Mohamed BS, Salwa AA (2004) New solid phase extractors for selective separation and preconcentration of mercury(II) based on silica gel immobilized aliphatic amines 2-thiophenecarboxaldehyde Schiff’s bases. Anal Chim Acta 523:133

    Article  Google Scholar 

  13. He Q, Chang X, Huang X, Hu Z (2008) Determination of trace elements in food samples by ICP-AES after preconcentration with p-toluenesulfonylamide immobilized on silica gel and nanometer SiO2. Microchim Acta 160:147

    Article  CAS  Google Scholar 

  14. Hadjiivanov K, Klissurski K, Kantcheva M, Davydov A (1991) State and localization of cobalt, nickel and copper ions adsorbed on titania (anatase). J Chem Soc Faraday Trans 87:907

    Article  CAS  Google Scholar 

  15. Lian N, Chang X, Zheng H, Wang S, Cui Y, Zhai Y (2005) Application of dithizone-modified TiO2 nanoparticles in the preconcentration of trace chromium and lead from sample solution and determination by inductively coupled plasma atomic emission spectrometry. Microchim Acta 151:81

    Article  CAS  Google Scholar 

  16. Bolis V, Fubini B, Giamello E (1991) Effect of form on the surface chemistry of finely divided solids. Mater Chem Phys 29:153

    Article  CAS  Google Scholar 

  17. Cui Y, Chang X, Zhai Y, Zhu X, Zheng H, Lian N (2006) ICP-AES determination of trace elements after preconcentrated with p-dimethylaminobenzaldehyde-modified nanometer SiO2 from sample solution. Microchem J 83:35

    Article  CAS  Google Scholar 

  18. Ji Y, Liu X, Guan M, Zhao C, Huang H, Zhang H (2009) Preparation of functionalized magnetic nanoparticulate sorbents for rapid extraction of biphenolic pollutants from environmental samples. J Sep Sci 32:2139

    Article  CAS  Google Scholar 

  19. Tsai HY, Hsu CF, Chiu IW, Bor Fuh C (2007) Detection of C-reactive protein based on immunoassay using antibody-conjugated magnetic nanoparticles. Anal Chem 79:8416

    Article  CAS  Google Scholar 

  20. Shin S, Jang J (2007) Thiol containing polymer encapsulated magnetic nanoparticles as reusable and efficiently separable adsorbent for heavy metal ions. Chem Comm 4230

  21. Hu J, Chen G, Irene MC (2005) Removal and recovery of Cr(VI) from wastewater by maghemite nanoparticles. Water Res 39:4528

    Article  CAS  Google Scholar 

  22. Huang C, Hu B (2008) Silica-coated magnetic nanoparticles modified with γ-mercaptopropyltrimethoxysilane for fast and selective solid phase extraction of trace amounts of Cd, Cu, Hg, and Pb in environmental and biological samples prior to their determination by inductively coupled plasma mass spectrometry. Spectrochim Acta B 63:437

    Article  Google Scholar 

  23. Huang C, Hu B (2008) Speciation of inorganic tellurium from seawater by ICP-MS following magnetic SPE separation and preconcentration. J Sep Sci 31:760

    Article  CAS  Google Scholar 

  24. Banerjee S, Chen D (2007) Fast removal of copper ions by gum arabic modified magnetic nano-adsorbent. J Hazard Mater 147:792

    Article  CAS  Google Scholar 

  25. Ngomsik A, Bee A, Siaugue J, Cabuil V, Cote G (2006) Nickel adsorption by magnetic alginate microcapsules containing an extractant. Water Res 40:1848

    Article  CAS  Google Scholar 

  26. Takafuji M, Ide S, Ihara H, Xu Z (2004) Preparation of poly(1-vinylimidazole)-grafted magnetic nanoparticles and their application for removal of metal ions. Chem Mater 16:1977

    Article  CAS  Google Scholar 

  27. Liu H, Zhao X, Chen Y (2007) Preparation and characterization of nano-magnetic Fe3O4-SiO2 composite. Chin Chem Res 18:21

    CAS  Google Scholar 

  28. Khan A, Mahmood F, Khokhar MY, Ahmad S (2006) Functionalized sol-gel material for extraction of mercury(II). React Funct Polym 66:1014

    Article  CAS  Google Scholar 

  29. Burba P, Wilmer PG (1992) Analytical fractionation of labile metals in selected groundwater humic substances by means of chelating ion-exchanger. Fresenius J Anal Chem 342:167

    Article  CAS  Google Scholar 

  30. Guéguen C, Belin C, Thomas BA, Monna F, Favarger PY, Dominik J (1999) The effect of freshwater UV-irradiation prior to resin preconcentration of trace metals. Anal Chim Acta 386:155

    Article  Google Scholar 

  31. Liu Y, Yang D, Chang X, Guo Y, Din B, Meng S (2004) Direct spectrophotometric determination of trace cadmium(II) in food samples with 2-Acetylmercaptophenyldiazoaminoazobenzene (AMPDAA). Microchim Acta 147:265

    CAS  Google Scholar 

  32. Liang X, Wang X, Zhuang J, Chen Y, Wang D (2006) Synthesis of nearly monodisperse iron oxide and oxyhydroxide nanocrystals. Adv Funct Mater 16:1805

    Article  CAS  Google Scholar 

  33. Mondal BC, Das AK (2003) Determination of mercury species with a resin functionalized with a 1, 2-bis(o-aminophenylthio)ethane moiety. Anal Chim Acta 477:73

    Article  CAS  Google Scholar 

  34. Guo Y, Din B, Liu Y, Chang X, Meng S (2004) Preconcentration and determination of trace elements with 2-aminoacetylthiophenol functionalized Amberlite XAD-2 by inductively coupled plasma–atomic emission spectrometry. Talanta 62:207

    Article  Google Scholar 

  35. Chattopadhyay P, Sinha C, Pal DK (1997) Preparation and properties of a new chelating resin containing imidazolyl azo groups. Fresenius J Anal Chem 357:368

    Article  CAS  Google Scholar 

  36. Krishna M, Karunasagar D, Ra SV, Arunachalam J (2005) Preconcentration and speciation of inorganic and methyl mercury in waters using polyaniline and gold trap-CVAAS. Talanta 68:329

    Article  CAS  Google Scholar 

  37. Liu Y, Chang X, Yang D, Guo Y, Meng S (2005) Highly selective determination of inorganic mercury(II) after preconcentration with Hg(II)-imprinted diazoaminobenzene–vinylpyridine copolymers. Anal Chim Acta 538:85

    Article  CAS  Google Scholar 

  38. Wu G, Wang Z, Wang J, Hea C (2007) Hierarchically imprinted organic–inorganic hybrid sorbent for selective separation of mercury ion from aqueous solution. Anal Chim Acta 582:304

    Article  CAS  Google Scholar 

Download references

Acknowledgement

The financial assistance provided by the Grand Science Research Foundation (200902) from Xi’an University of Arts and Science.

Author information

Authors and Affiliations

  1. Department of Chemistry, Xi’an University of Arts and Science, Xi’an, 710065, People’s Republic of China

    Yunhui Zhai, Shu’e Duan, Xiaohui Yang & Quan Han

  2. Department of Chemistry, Lanzhou University, Lanzhou, 730000, People’s Republic of China

    Qun He

Authors
  1. Yunhui Zhai
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Shu’e Duan
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Qun He
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Xiaohui Yang
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Quan Han
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Yunhui Zhai.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Zhai, Y., Duan, S., He, Q. et al. Solid phase extraction and preconcentration of trace mercury(II) from aqueous solution using magnetic nanoparticles doped with 1,5-diphenylcarbazide. Microchim Acta 169, 353–360 (2010). https://doi.org/10.1007/s00604-010-0363-8

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00604-010-0363-8

Keywords

Search

Navigation