Microchimica Acta

, Volume 181, Issue 9–10, pp 1035–1040 | Cite as

Preconcentration of trace lead via formation of the bis(2,2-bipyridyl) complex and its adsorption on oxidized multiwalled carbon nanotubes

Original Paper


A solid phase extraction method is presented for the preconcentration of trace lead ions on oxidized multiwalled carbon nanotubes (ox-MWCNTs). In the first step, the cationic Pb(II) complex of 2,2-bipyridyl is formed which, in a second step, is adsorbed on ox-MWCNTs mainly due to electrostatic and van der Waals interactions. The Pb(II) ions were then eluted with dilute nitric acid and quantified by FAAS. The effects of pH value, mass of sorbent, concentration of 2,2-bipyridyl, stirring time, of type, concentration and volume of eluent, of eluent flow rate and sample volume were examined. Most other ions do not affect the recovery of Pb(II). The limits of detection are 240 and 60 ng L−1 for sample volumes of 100 and 400 mL, respectively. The recovery and relative standard deviation are >95 % and 2.4 %, respectively. Other figures of merit include a preconcentration factor of 160 and a maximum adsorption capacity of 165 mg g−1. The method was successfully applied to the determination of Pb(II) in spiked tap water samples. The accuracy of the method was verified by correctly analyzing a certified reference material (NCS ZC85006; lead in tomatoes).


A solid phase extraction method is presented for the preconcentration of trace lead ions on oxidized multiwalled carbon nanotubes (ox-MWCNTs). Most other ions do not affect the recovery of Pb(II).


Multiwalled carbon nanotubes 2,2-bipyridyl Flame atomic absorption spectrometry Trace amounts of lead Selectivity 

Supplementary material

604_2014_1210_MOESM1_ESM.pdf (265 kb)
ESM 1 (PDF 265 kb)


  1. 1.
    Mohammadia SZ, Afzali D, Baghelan YM (2009) Ligandless-dispersive liquid-liquid microextraction of trace amount of copper ions. Anal Chim Acta 653:173–177CrossRefGoogle Scholar
  2. 2.
    Khari R, Shemirani F, Majdi B (2011) Combination of dispersive liquid-liquid microextraction and flame atomic spectrometry for preconcentration and determination of copper in water samples. Desalination 266:238–243CrossRefGoogle Scholar
  3. 3.
    Lemos VA, Silva da Franca R, Moreira BO (2007) Cloud point extraction for Co and Ni determination in water samples by flame atomic absorption spectrometry. Sep Purif Technol 54:349–354CrossRefGoogle Scholar
  4. 4.
    Candira S, Narinb I, Soylak M (2008) Ligandless cloud point extraction of Cr(III), Pb(II), Cu(II), Ni(II), Bi(III), and Cd(II) ions in environmental samples with Tween 80 and flame atomic absorption spectrometric determination. Talanta 77:289–293CrossRefGoogle Scholar
  5. 5.
    Tokalıoglu S, Dasdelen O (2011) Coprecipitation with Cu(II)-4-(2-pyridylazo)- resorcinol for separation and preconcentration of Fe(III) and Ni(II) in water and food samples. Clean Soil Air, Water 39:296–300CrossRefGoogle Scholar
  6. 6.
    Duran C, Ozdes D, Sahin D, Bulut VN, Gundogdu A, Soylak M (2011) Preconcentration of Cd(II) and Cu(II) ions by coprecipitation without any carrier element in some food and water samples. Microchem J 98:317–322CrossRefGoogle Scholar
  7. 7.
    Pohl P, Prusisz B (2007) Fractionation analysis of manganese and zinc in tea infusions by two-column solid phase extraction and flame atomic absorption spectrometry. Food Chem 102:1415–1424CrossRefGoogle Scholar
  8. 8.
    Gurnani V, Singh AK, Venkataramani B (2003) Cellulose functionalized with 8-hydroxyquinoline: new method of synthesis and applications as a solid phase extractant in the determination of metal ions by flame atomic absorption spectrometry. Anal Chim Acta 485:221–232CrossRefGoogle Scholar
  9. 9.
    Xie F, Lin X, Wu X, Xie Z (2008) Solid phase extraction of lead (II), copper (II), cadmium (II) and nickel (II) using gallic acid-modified silica gel prior to determination by flame atomic absorption spectrometry. Talanta 74:836–843CrossRefGoogle Scholar
  10. 10.
    Shamspur T, Sheikhshoaie I, Mashhadizadeh MH (2005) Flame atomic absorption spectroscopy (FAAS) determination of iron(III) after preconcentration on to modified analcime zeolite with 5-((4-nitrophenylazo)-N-(20,40-dimethoxyphenyl))salicylaldimine by column metod. J Anal At Spectrom 20:476–478CrossRefGoogle Scholar
  11. 11.
    Huang LH, Sun YY, Yang T, Li L (2011) Adsorption behavior of Ni (II) on lotus stalks derived active carbon by phosphoric acid activation. Desalination 268:12–19CrossRefGoogle Scholar
  12. 12.
    Zhanga L, Li Z, Dud X, Li R, Chang X (2012) Simultaneous separation and preconcentration of Cr(III), Cu(II), Cd(II) and Pb(II) from environmental samples prior to inductively coupled plasma optical emission spectrometric determination. Spectrochim Acta Part A 86:443–448CrossRefGoogle Scholar
  13. 13.
    Afkhami A, Saber-Tehrani M, Bagheri H, Madrakian T (2011) Flame atomic absorption spectrometric determination of trace amounts of Pb(II) and Cr(III) in biological, food and environmental samples after preconcentration by modified nano-alumina. Microchim Acta 172:125–136CrossRefGoogle Scholar
  14. 14.
    Sohrabi MR, Matbouie Z, Asgharinezhad AA, Dehghani A (2013) Solid phase extraction of Cd(II) and Pb(II) using a magnetic metal-organic framework, and their determination by FAAS. Microchim Acta 180:589–597CrossRefGoogle Scholar
  15. 15.
    Perez-Lopez B, Merkoci A (2012) Carbon nanotubes and graphene in analytical sciences. Microchim Acta 179:1–16CrossRefGoogle Scholar
  16. 16.
    Soylak M, Unsal YE (2009) Simultaneous enrichment-separation of metal ions from environmental samples by solid-phase extraction using double-walled carbon nanotubes. J AOAC Int 92:1219–1224Google Scholar
  17. 17.
    Liang P, Liu Y, Guo L, Zeng J, Lu H (2004) Multiwalled carbon nanotubes as solid-phase extraction adsorbent for the preconcentration of trace metal ions and their determination by inductively coupled plasma atomic emission spectrometry. J Anal At Spectrom 19:1489–1492CrossRefGoogle Scholar
  18. 18.
    Sitko R, Zawisza B, Malicka E (2012) Modification of carbon nanotubes for preconcentration, separation and determination of trace-metal ions. Trends Anal Chem 37:22–31CrossRefGoogle Scholar
  19. 19.
    Tajik S, Taher MA (2011) A new sorbent of modified MWCNTs for column preconcentration of ultra trace amounts of zinc in biological and water samples. Desalination 278:57–64CrossRefGoogle Scholar
  20. 20.
    Mohammadi SZ, Afzali D, Pourtalebi D (2010) Flame atomic absorption spectrometric determination of trace amounts of lead, cadmium and nickel in different matrixes after solid phase extraction on modified multiwalled carbon nanotubes. Cent Eur J Chem 8:662–668CrossRefGoogle Scholar
  21. 21.
    Vellaichamy S, Palanivelu K (2011) Preconcentration and separation of copper, nickel and zinc in aqueous samples by flame atomic absorption spectrometry after column solid-phase extraction onto MWCNTs impregnated with D2EHPA-TOPO mixture. J Hazard Mater 185:1131–1139CrossRefGoogle Scholar
  22. 22.
    Durana A, Tuzena M, Soylak M (2009) Preconcentration of some trace elements via using multiwalled carbon nanotubes as solid phase extraction adsorbent. J Hazard Mater 169:466–471CrossRefGoogle Scholar
  23. 23.
    Tuzen M, Saygi KO, Soylak M (2008) Solid phase extraction of heavy metal ions in environmental samples on multiwalled carbon nanotubes. J Hazard Mater 152:632–639CrossRefGoogle Scholar
  24. 24.
    Ruijun L, Xijun C, Zhenhua L, Zhipeng Z, Zheng H, Dandan L, Zhifeng T (2011) Multiwalled carbon nanotubes modified with 2-aminobenzothiazole modified for uniquely selective solid-phase extraction and determination of Pb(II) ion in water Samales. Microchim Acta 172:269–276CrossRefGoogle Scholar
  25. 25.
    Zang Z, Hu Z, Li Z, He Q, Chang X (2009) Synthesis, characterization and application of ethylenediamine-modified multiwalled carbon nanotubes for selective solid-phase extraction and preconcentration of metal ions. J Hazard Mater 172:958–963CrossRefGoogle Scholar
  26. 26.
    Yang C, Shan L, Zhang-Jun H, Xiang-Hu L, Hong-Wen G (2011) Solid-phase extraction of lead(II) ions using multiwalled carbon nanotubes grafted with tris(2-aminoethyl)amine. Microchim Acta 174:107–113CrossRefGoogle Scholar
  27. 27.
    Nabida MR, Sedghia R, Bagheria A, Behbahania M, Taghizadeha M, Oskooieb HA, Heravi MM (2012) Preparation and application of poly(2-amino thiophenol)/MWCNTs nanocomposite for adsorption and separation of cadmium and lead ions via solid phase extraction. J Hazard Mater 203–204:93–100CrossRefGoogle Scholar
  28. 28.
    Tavallali H, Abdardideh D, Aalaei M, Zahmatkesh S (2012) New application of chemically modified multiwalled carbon nanotubes with thiosemicarbazide as a sorbent for separation and preconcentration of trace amounts of Co(II), Cd(II), Cu(II), and Zn(II) in environmental and biological samples prior to determination by flame atomic absorption spectrometry. J Chin Chem Soc 59:114–121CrossRefGoogle Scholar
  29. 29.
    Xiaowei Z, Naizhong S, Qiong J, Weihong Z (2009) Determination of Cu, Zn, Mn, and Pb by microcolumn packed with multiwalled carbon nanotubes on-line coupled with flame atomic absorption spectrometry. Microchim Acta 166:329–335CrossRefGoogle Scholar
  30. 30.
    Stafiej A, Pyrzynska K (2008) Solid phase extraction of metal ions using carbon nanotubes. Microchem J 89:29–33CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Wien 2014

Authors and Affiliations

  1. 1.Department of Analytical Chemistry, Institute of ChemistryUniversity of SilesiaKatowicePoland

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