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Preparation of electrochemically treated nanoporous pencil-graphite electrodes for the simultaneous determination of Pb and Cd in water samples

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Abstract

A simple and rapid analytical method of determining Pb2+ and Cd2+ in water samples using an electrochemically pretreated pencil-graphite electrode (EP-PGE) is proposed for the first time in the literature. An electrochemically pretreated pencil-graphite electrode was prepared by performing potential cycling between −0.3 V and 2.0 V in 0.1 mol L−1 H3PO4 solution to improve its ability to electrochemically sense Pb2+ and Cd2+ ions. Square-wave anodic stripping voltammetry (SWASV) was used as the electroanalytical method. The electroanalytical parameters that influence the stripping determination of Pb2+ and Cd2+ were optimized based on experimental results. The magnitude of the peak oxidation current was adjusted in order to optimize the value of each parameter. Applying the resulting disposable electrode under the optimized conditions led to good selectivity and sensitivity in the determination of Pb2+ and Cd2+ ions. Interference from coexisting ions was also investigated. The resulting sensor was successfully tested by applying it to a standard reference water sample. Under the optimized conditions, the limits of detection were 0.46 μg L−1 for Pb2+ and 1.11 μg L−1 for Cd2+ using the electrode. Relative standard deviations (%RSD) were 2.76 for Pb2+ and 2.85 for Cd2+. The linear working ranges of the electrode for Pb2+ and Cd2+ ion detection were 5–45 μg L−1 and 10–40 μg L−1, respectively.

Preparation of nanoporous pencil-graphite electrode by cyclic voltammetry and stripping voltammetric screening of Pb and Cd

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References

  1. World Health Organization (WHO). Health risks of heavy metals from long-range transboundary air pollution. Joint WHO/Convention Task Force on the Health Aspects of Air Pollution. Copenhagen: WHO; 2007.

  2. Gençten M, Dönmez KB, Sahin Y, Pekmez K, Suvacı E. Voltammetric and electrochemical impedimetric behavior of silica-based gel electrolyte for valve-regulated lead-acid battery. J Solid State Electrochem. 2014;18:2469. doi:10.1007/s100080142507-y.

  3. Dönmez KB, Gençten M, Şahin Y. A novel polysiloxane-based polymer as a gel agent for gel–VRLA batteries. Ionics. 2017; doi:10.1007/s115810172040-y.

  4. Seiler HG, Sigel H, Sigel A. Handbook on toxicity of inorganic compounds. New York: Marcel Dekker; 1988.

    Google Scholar 

  5. Demetriades D, Economou A, Voulgaropoulos A. A study of pencil-lead bismuth-film electrodes for the determination of trace metals by anodic stripping voltammetry. Anal Chim Acta. 2004;519:167–72.

    Article  CAS  Google Scholar 

  6. Farghaly OA, Ghandour MA. Square-wave stripping voltammetry for direct determination of eight heavy metals in soil and indoor-airborne particulate matter. Environ Res. 2005;97:229–35.

  7. Nedeltcheva T, Atanassova M, Dimitrov J, Stainislavova L. Determination of mobile form contents of Zn, Cd, Pb and Cu in soil extracts by combined stripping voltammetry. Anal Chim Acta. 2005;528:143–6.

  8. Farghaly OA. Direct and simultaneous voltammetric analysis of heavy metals in tap water samples at Assiut City: an approach to improve the analysis time for nickel and cobalt determination at mercury film electrode. Microchem J. 2003;75:119–31.

  9. Reddy SJ, Valenta P, Nürnberg HW, Fresenius Z. Simultaneous determination of toxic metals Cd, Cu, Pb and Zn in soils by differential pulse anodic stripping voltammetry. Anal Chem. 1982;313:390–4.

  10. Li Y, Wahdat F, Neeb R. Digestion-free determination of heavy metals (Pb, Cd, Cu) in honey using anodic stripping differential pulse voltammetry and potentiometric stripping analysis. Fresenius J Anal Chem. 1995;351:678–82.

  11. Legeai S, Soropogui K, Cretinon M, Vittori O, Oliveira AHD, Barbier F, et al. Economic bismuth-film microsensor for anodic stripping analysis of trace heavy metals using differential pulse voltammetry. Anal Bioanal Chem. 2005;383:839–47.

  12. Intarakamhang S, Schuhmann W, Schulte A. Robotic heavy metal anodic stripping voltammetry: ease and efficacy for trace lead and cadmium electroanalysis. J Solid State Electrochem. 2013;17:1535. doi:10.1007/s1000801320182.

  13. Injang U, Noyrod P, Siangproh W, Dungchai W, Motomizu S, Chailapakul O. Determination of trace heavy metals in herbs by sequential injection analysis–anodic stripping voltammetry using screen-printed carbon nanotubes electrodes. Anal Chim Acta. 2010;668:54–60.

  14. Hwang GH, Han WK, Park JS, Kang SG. Determination of trace metals by anodic stripping voltammetry using a bismuth-modified carbon nanotube electrode. Talanta. 2008;76:301–8.

    Article  CAS  Google Scholar 

  15. Zhao G, Wang H, Liu G, Wang Z, Cheng J. Simultaneous determination of trace Cd(II) and Pb(II) based on Bi/Nafion/reduced graphene oxide–gold nanoparticle nanoparticle nanocomposite film–modified glassy carbon electrode by one-step electrodeposition. Ionics. 2017;23:767; doi:10.1007/s1158101618436.

  16. Wu Y, Li NB, Luo HQ. Simultaneous measurement of Pb, Cd and Zn using differential pulse anodic stripping voltammetry at a bismuth/poly(p-aminobenzene sulfonic acid) film electrode. Sensors Actuators B Chem. 2008;133:677–81.

  17. Sosa V, Serrano N, Arino C, Diaz-Cruz JM, Esteban M. Sputtered bismuth screen-printed electrode: a promising alternative to other bismuth modifications in the voltammetric determination of Cd(II) and Pb(II) ions in groundwater. Talanta. 2014;119:348–52.

  18. Lezi N, Economou A, Dimovasilis PA, Trikalitis PN, Prodromidis MI. Disposable screen-printed sensors modified with bismuth precursor compounds for the rapid voltammetric screening of trace Pb(II) and Cd(II). Anal Chim Acta. 2012;728:1–8.

  19. Xiao L, Xu H, Zhou S, Song T, Wang H, Li S, et al. Simultaneous detection of Cd(II) and Pb(II) by differential pulse anodic stripping voltammetry at a nitrogen-doped microporous carbon/Nafion/bismuth-film electrode. Electrochim Acta. 2014;143:143–51.

  20. Li X, Zhou H, Fu C, Wang F, Ding Y, Kuang Y. A novel design of engineered multi-walled carbon nanotubes material and its improved performance in simultaneous detection of Cd(II) and Pb(II) by square wave anodic stripping voltammetry. Sensors Actuators B Chem. 2016;236:144–52.

  21. Ozcan A, Sahin Y. Preparation of selective and sensitive electrochemically treated pencil graphite electrodes for the determination of uric acid in urine and blood serum. Biosens Bioelectron. 2010;25:2497–502.

    Article  Google Scholar 

  22. Ozcan A, Sahin Y. A novel approach for the determination of paracetamol based on the reduction of N-acetyl-p-benzoquinoneimine formed on the electrochemically treated pencil graphite electrode. Anal Chim Acta. 2011;685:9–14.

  23. Geremedhin W, Amare M, Admassie S. Electrochemically pretreated glassy carbon electrode for electrochemical detection of fenitrothion in tap water and human urine. Electrochim Acta. 2013;87:749–55.

    Article  CAS  Google Scholar 

  24. Su WY, Wang SM, Cheng SH. Electrochemically pretreated screen-printed carbon electrodes for the simultaneous determination of aminophenol isomers. J Electroanal Chem. 2011;651:166–72.

    Article  CAS  Google Scholar 

  25. Di J, Zhang F. Voltammetry determination of trace manganese with pretreatment glassy carbon electrode by linear sweep voltammetry. Talanta. 2003;60:31–6.

    Article  CAS  Google Scholar 

  26. Sosa E, Carreno G, Ponce-de-Leon C, Oropeza MT, Morales M, Gonzalez I, et al. Lead deposition onto fractured vitreous carbon: influence of electrochemical pretreated electrode. Appl Surf Sci. 2000;153:245–58.

  27. Analytical Methods Committee. Recommendations for the definition, estimation and use of the detection limit. Analyst. 1987;112:199–204.

    Article  Google Scholar 

  28. Zhao G, Wang H, Liu G. Electrochemical determination of trace cadmium in soil by a bismuth film/graphene-β-cyclodextrin-Nafion composite modified electrode. Int J Electrochem Sci. 2016;11:1840–51.

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Acknowledgements

Betül Kahraman, Tuğba Güven, Dilay Ünal, and Dilara Kılıç are kindly acknowledged for fruitful discussions about this topic and for providing us with useful information.

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Correspondence to Ebru Çetinkaya or Yücel Şahin.

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Dönmez, K.B., Çetinkaya, E., Deveci, S. et al. Preparation of electrochemically treated nanoporous pencil-graphite electrodes for the simultaneous determination of Pb and Cd in water samples. Anal Bioanal Chem 409, 4827–4837 (2017). https://doi.org/10.1007/s00216-017-0426-3

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