SavedAdd your journal

Journals / Muş Alparslan Üniversitesi Fen Bilimleri Dergisi / 2025 / Cilt: 13 Sayı: 2

Solid Phase Extraction of Pb²⁺ and Cd²⁺ from Tigris River Water Using an AmideFunctionalized Silica Sorbent and ICP-OES Determination

Amid Fonksiyonlu Silika Sorbent Kullanılarak Dicle Nehri Suyundan Pb²⁺ ve Cd²⁺'nin Katı Faz Ekstraksiyonu ve ICP-OES Tayini

Hayriye Aral(BATMAN ÜNİVERSİTESİ)0000-0001-7673-5108
Uyan Yüksel(SİİRT ÜNİVERSİTESİ)0000-0003-0498-9277
Pages
205–213
Publication Date
2025-12-24
🏛️Bibliographic metadata and full text access for this article are provided via DergiPark.
DergiPark Record ↗
✨

AI Summary & Key Takeaways

AI Insight
⚡ TL;DR(Too Long; Didn't Read)

The method was validated using NIST 1643e and successfully applied to Dicle River water samples.

📌 3 Key Takeaways

🎯
Objective & Hypothesis:In this study, the preconcentration, separation, and simultaneous determination of Pb²⁺ and Cd²⁺ ions in water samples were carried out using solid-phase extraction with a silica-gel–based mixed-mode HPLC stationary phase synthesized in our previous work.
📊
Key Findings & Data:This phase had previously shown strong performance in separating various polar and nonpolar compounds, prompting its evaluation for metal ion enrichment.
💡
Conclusion & Impact:The method was validated using NIST 1643e and successfully applied to Dicle River water samples.
🔬Design:Araştırma Makalesi
📍Scope:Comprehensive Sample
⚙️Variables:Ağır metaller · katı faz ekstraksiyonu · ICP-OES

Abstract

In this study, the preconcentration, separation, and simultaneous determination of Pb²⁺ and Cd²⁺ ions in water samples were carried out using solid-phase extraction with a silica-gel–based mixed-mode HPLC stationary phase synthesized in our previous work. This phase had previously shown strong performance in separating various polar and nonpolar compounds, prompting its evaluation for metal ion enrichment. Solutions containing Pb²⁺ and Cd²⁺ were passed through the column, eluted with 7 mL of 1 mol L⁻¹ HNO₃, and analyzed by ICP-OES. Parameters such as pH, sorbent amount, eluent type and volume, flow rates, sample volume, and foreign ion effects were examined. The optimum pH was found to be 6, with detection limits of 0.15 µg L⁻¹ for Pb and 0.1 µg L⁻¹ for Cd. The enrichment factor was 71.4 for both ions. The method was validated using NIST 1643e and successfully applied to Dicle River water samples.

Özet

Bu çalışmada, su örneklerindeki Pb²⁺ ve Cd²⁺ iyonlarının ön deriştirilmesi, ayrılması ve eşzamanlı analizi, önceki çalışmamızda sentezlenen silika-jel bazlı karışık mod HPLC sabit fazı kullanılarak katı faz ekstraksiyonuyla gerçekleştirilmiştir. Bu sabit fazın daha önce farklı polar ve apolar bileşiklerin ayrılmasında başarılı olması, metal iyonlarına yönelik uygulanabilirliğini araştırmamıza olanak sağlamıştır. Pb²⁺ ve Cd²⁺ içeren çözeltiler kolondan geçirilmiş, elüsyon için 7 mL 1 mol L⁻¹ HNO₃ kullanılmış ve ICP-OES ile analiz edilmiştir. pH, sorbent miktarı, elüsyon tipi ve hacmi, akış hızları ve yabancı iyonların etkisi değerlendirilmiştir. Optimum pH 6 bulunmuş; tespit limitleri Pb için 0.15 µg L⁻¹, Cd için 0.1 µg L⁻¹ olarak belirlenmiştir. Her iki iyon için zenginleştirme faktörü 71.4’tür. Yöntem NIST 1643e ile doğrulanmış ve Dicle Nehri su örneklerinde başarıyla uygulanmıştır.

🔖

Cite This Article

Aral, H., Yüksel, U. (2025). Solid Phase Extraction of Pb²⁺ and Cd²⁺ from Tigris River Water Using an AmideFunctionalized Silica Sorbent and ICP-OES Determination. Muş Alparslan Üniversitesi Fen Bilimleri Dergisi, Cilt: 13 Sayı: 2, 205–213. https://doi.org/10.18586/msufbd.1654901

📄 Full Text PDF Viewer

📄

PDF görüntüleyici hazırlanıyor...

References (52)

  1. Shmeis R.M.A. Nanotechnology in wastewater treatment, Comprehensive Analytical Chemistry, 99, 105-134, 2022. doi: 10.1016/bs.coac.2021.11.002.
  2. Ge F., Li M.M., Ye H., Zhao B.X. Effective removal of heavy metal ions Cd²⁺, Zn²⁺, Pb²⁺, Cu²⁺ from aqueous solution by polymer-modified magnetic nanoparticles, J. Hazard. Mater., 211, 366-372, 2012. doi: 10.1016/j.jhazmat.2011.12.013.
  3. Jang S.H., Min B.G., Jeong Y.G., Lyoo W.S., Lee S.C. Removal of lead ions in aqueous solution by hydroxyapatite/polyurethane composite foams, J. Hazard. Mater., 152, 1285-1292, 2008. doi: 10.1016/j.jhazmat.2007.08.003.
  4. Murata I., Hirono T., Saeki Y., Nakagawa S. Cadmium enteropathy, renal osteomalacia ("Itai Itai" disease in Japan), Bull. Soc. Int. Chir., 29, 34-42, 1970. PMID: 5510186.
  5. Kumar N.S., Dharmendra V., Sreenivasulu V., Asif M., Ibrahim A.A., Balaram V. Separation and pre-concentration of Pb and Cd in water samples using 3-(2-hydroxyphenyl)-1H-1,2,4-triazole-5(4H)-thione (HTT) and their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES), Metals, 7, 240, 2017. doi: 10.3390/met7070240.
  6. Pereira M.D., Arruda M.A.Z. Trends in preconcentration procedures for metal determination using atomic spectrometry techniques, Microchim. Acta, 141, 115-131, 2003. doi: 10.1007/s00604-002-0941-5.
  7. Ghaedi M., Fathi M.R., Shokrollahi A., Shajarat F. Highly selective and sensitive preconcentration of mercury ion and determination by cold vapor atomic absorption spectroscopy, Anal. Lett., 39, 1171-1185, 2012. doi: 10.1080/00032719.2012.658764.
  8. Mashhadizadeh M.H., Pesteh M., Talakesh M., Sheikhshoaie I., Ardakani M.M., Karimi M.A. Solid phase extraction of copper (II) by sorption on octadecyl silica membrane disk modified with a new Schiff base and determination with atomic absorption spectrometry, Spectrochim. Acta Part B: Atomic Spectroscopy, 63, 885-888, 2008. doi: 10.1016/j.sab.2008.03.018.
  9. Manjusha R., Dash K., Karunasagar D. UV-photolysis assisted digestion of food samples for the determination of selenium by electrothermal atomic absorption spectrometry (ETAAS), Food Chem., 105, 260-265, 2007. doi: 10.1016/j.foodchem.2006.11.011.
  10. Lemos V.A., DaSilva D.G., DeCarvalho A.L., Santana D.D., Novaes G.D., DosPassos A.S. Synthesis of amberlite XAD-2-PC resin for preconcentration and determination of trace elements in food samples by flame atomic absorption spectrometry, Microchem. J., 84, 14-21, 2006. doi: 10.1016/j.microc.2006.03.006.
  11. Da-Col J.A., Domene S.M.A., Pereira-Filho E.R. Fast determination of Cd, Fe, Pb, and Zn in food using AAS, Food Anal. Methods, 2, 110-115, 2009. doi: 10.1007/S12161-008-9041-4.
  12. Hammer D., Nicolas M., Andrey D. Improved chromium determination in various food matrices using dynamic reaction cell ICP-MS, Atom. Spectrosc., 26, 203-208, 2005. doi: 10.46770/AS.2005.06.001.
  13. Nardi E.P., Evangelista F.S., Tormen L., Pierre T.D.S., Curtius A.J., De-Souza S.S., Barbosa F. The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples, Food Chem., 112, 727-732, 2009. doi:10.1016/j.foodchem.2008.06.010.
  14. He Q., Chang X.J., Huang X.P., Hu Z. 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, 147-152, 2008. doi: 10.1007/s00604-007-0823-y.
  15. Balaram V. Developments and trends in inductively coupled plasma mass spectrometry and its influence on the recent advances in trace element analysis, Curr. Sci., 69, 640-649, 1995.
  16. Balaram V., Anjaiah K.V., Reddy M.R.P. Comparative study on the trace and rare earth element analysis of an Indian polymetallic nodule reference sample by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry, Analyst, 120, 1401-1406, 1995. doi: 10.1039/AN9952001401.
  17. Kamboh M.A., Solangi I.B., Sherazi S.T.H., Memon S. Synthesis and application of calix[4]arene based resin for the removal of azo dyes, J. Hazard. Mater., 172, 234-239, 2009. doi: 10.1016/j.jhazmat.2009.06.165.
  18. Karadaş C., Kara D. On-line preconcentration and determination of trace elements in waters and reference cereal materials by flow injection – FAAS using newly synthesized 8-hydroxy-2-quinoline carboxaldehyde functionalized Amberlite XAD-4, Journal of Food Composition and Analysis, 32, 90-98, 2013. doi: 10.1016/j.jfca.2013.07.003.
  19. Farajzadeh M.A., Bahram M., Zorita S., Mehr B.G. Optimization and application of homogeneous liquid–liquid extraction in preconcentration of copper (II) in a ternary solvent system, J. Hazard. Mater., 161, 1535-1543, 2009. doi: 10.1016/j.jhazmat.2008.05.041.
  20. Atanassova D., Stefanova V., Russeva E. Co-precipitative pre-concentration with sodium diethyldithiocarbamate and ICP-AES determination of Se, Cu, Pb, Zn, Fe, Co, Ni, Mn, Cr and Cd in water, Talanta, 47, 1237-1243, 1998. doi: 10.1016/S0039-9140(98)00211-2.
  21. Kuroda R., Hayashibe Y., Oguma K., Kurosu K. Anion-exchange enrichment and spectrophotometric determination of traces of uranium in sea water, Fresenius' Zeitschrift für analytische Chemie, 335, 404, 1989. doi: 10.1007/BF00482110.
  22. Yan H., Xu Y.C., Lu Y., Xing W. Reduced graphene oxide-based solid-phase extraction for the enrichment and detection of microRNA, Anal. Chem., 89, 10137-10140, 2017. doi: 10.1021/acs.analchem.7b03138.
  23. Vergara-Barberán M., Lerma-García M.J., Simó-Alfonso E.F., Herrero Martínez J.M. Polymeric sorbents modified with gold and silver nanoparticles for solid-phase extraction of proteins followed by MALDI-TOF analysis, Microchim. Acta, 184, 1683-1690, 2017. doi: 10.1007/s00604-017-2168-5.
  24. Liu H., Yu H., Jin P., Jiang M., Zhu G., Duan Y., Yang Z., Qiu H. Preparation of mesoporous silica materials functionalized with various amino-ligands and investigation of adsorption performances on aromatic acids, Chemical Engineering Journal, 379, 122405, 2020. doi: 10.1016/j.cej.2019.122405.
  25. Liu H.M., Zhang M.L., Guo Y., Qiu H.D. Solid-phase extraction of flavonoids in honey samples using carbamate-embedded triacontyl-modified silica sorbent, Food Chem., 204, 56-61, 2016. doi: 10.1016/j.foodchem.2016.02.102.
  26. Chigome S., Torto N. Electrospun nanofiber-based solid-phase extraction, Trends Anal. Chem., 38, 21-31, 2012. doi: 10.1016/j.trac.2012.04.011.
  27. Zygler A., Wasik A., Namieśnik J. Retention behaviour of some high-intensity sweeteners on different SPE sorbents, Talanta, 82, 1742-1748, 2010. doi: 10.1016/j.talanta.2010.07.070.
  28. Huang X., Chang X., He Q., Cui Y., Zhai Y., Jiang N. Tris(2-aminoethyl) amine functionalized silica gel for solid-phase extraction and preconcentration of Cr(III), Cd(II) and Pb(II) from waters, Journal of Hazardous Materials, 157, 154-160, 2008. doi: 10.1016/j.jhazmat.2007.12.113.
  29. Alghanmi R.M. ICP-OES determination of trace metal ions after preconcentration using silica gel modified with 1,2-dihydroxyanthraquinone, Journal of Chemistry, 9, 1007, 2012. doi: 10.1155/2012/279628.
  30. Camel V. Solid phase extraction of trace elements, Spectrochimica Acta-Part B: Atomic Spectroscopy, 58, 1177-1233, 2003. doi: 10.1016/S0584-8547(03)00072-7.
  31. Cui Y., Chang X., Zhu X., Luo H., Hu Z., Zou X., He Q. Chemically modified silica gel with p-dimethylaminobenzaldehyde for selective solid-phase extraction and preconcentration of Cr(II), Cu(II), Ni(II), Pb(II) and Zn(II) by ICP-OES, Microchemical Journal, 87, 20-26, 2007. doi: 10.1016/j.microc.2007.04.004.
  32. Dakova I., Vasileva P., Karadjova I., Karadjova M., Slaveykova V. Solid phase extraction and diffusive gradients in thin films techniques for determination of total and labile concentrations of Cd(II), Cu(II), Ni(II) and Pb(II) in Black Sea water, Int. J. Environ. Anal. Chem., 91, 62-73, 2011. doi: 10.1080/03067310903195011
  33. Aydin F.A., Soylak M. A novel multi-element coprecipitation technique for separation and enrichment of metal ions in environmental samples, Talanta, 73, 134-141, 2007. doi: 10.1016/j.talanta.2007.03.007.
  34. Haginaka J. Selectivity of affinity media in solid-phase extraction of analytes, Trends Anal. Chem., 24, 407-415, 2005. doi: 10.1016/j.trac.2004.12.005.
  35. Lemos V.A., Santos J.S., Baliza P.X. Synthesis of α-Nitroso-β-Naphthol Modified Amberlite XAD-2 Resin and its Application in On-Line Solid Phase Extraction System for Cobalt Preconcentration, Sep. Sci. Technol., 39, 3317-3330, 2004. doi: 10.1081/SS-200027351.
  36. Narin I., Soylak M., Kayakirilmaz K., Elci L., Dogan M. Preparation of a Chelating Resin by Immobilizing 1-(2-Pyridylazo) 2-Naphtol on Amberlite XAD-16 and Its Application of Solid Phase Extraction of Ni(II), Cd(II), Co(II), Cu(II), Pb(II), and Cr(III) in Natural Water Samples, Anal. Lett., 36, 641-658, 2003. doi: 10.1081/AL-120018254.
  37. Ramesh A., Mohan K.R., Seshaiah K. Preconcentration of trace metals on Amberlite XAD-4 resin coated with dithiocarbamates and determination by inductively coupled plasma-atomic emission spectrometry in saline matrices, Talanta, 57, 243-252, 2002. doi: 10.1016/s0039-9140(02)00033-4.
  38. Cuekicu S.D., Filik H., Apak R. Use of an o-aminobenzoic acid-functionalized XAD-4 copolymer resin for the separation and preconcentration of heavy metal(II) ions, Anal. Chim. Acta., 505, 15-24, 2004. doi: 10.1016/S0003-2670(03)00211-3.
  39. Lemos V.A., Baliza P.X. Amberlite XAD-2 functionalized with 2-aminothiophenol as a new sorbent for on-line preconcentration of cadmium and copper, Talanta, 67, 564-570, 2005. doi: 10.1016/j.talanta.2005.03.012.
  40. Aral H. Synthesis and Characterisation of a New Hydrophilic Interaction/Reversed Phase Mixed-Mode Chromatographic Stationary Phase, Hacettepe Journal of Biology and Chemistry, 46, 43-52, 2018. doi: 10.15671/HJBC.2018.213.
  41. Stumm, W., & Morgan, J. J. (2013). Aquatic chemistry: Chemical equilibria and rates in natural waters (3rd ed.). John Wiley & Sons.
  42. Dzombak, D. A., & Morel, F. M. (1991). Surface complexation modeling: Hydrous ferric oxide. John Wiley & Sons.
  43. Pereira M.D., Arruda M.A.Z. Trends in Preconcentration Procedures for Metal Determination Using Atomic Spectrometry Techniques, Microchim. Acta, 141, 115-131, 2003. doi: 10.1007/s00604-002-0941-5.
  44. North A.E., Sarpong-Kumankomah S., Bellavie A.R., White W.M., Gailer J. Environmentally relevant concentrations of aminopolycarboxylate chelating agents mobilize Cd from humic acid, J. Environ. Sci., 57, 249-257, 2017. doi: 10.1016/j.jes.2017.02.004.
  45. World Health Organization (WHO). Guidelines for drinking-water quality, 4th Edition, Geneva: World Health Organization, 2017. ISBN: 978-92-4-154995-0.
  46. United States Environmental Protection Agency (EPA). National Primary Drinking Water Regulations, U.S. EPA, Washington, D.C., 2022. Available at: https://www.epa.gov/ground-water-and-drinking-water/national-primary-drinking-water-regulations (Accessed: April 2025).
  47. Khan S., Cao Q., Zheng Y.M., Huang Y.Z., Zhu Y.G. Health risks of heavy metals in contaminated soils and food crops irrigated with wastewater in Beijing, China, Environ. Pollut., 152, 686–692, 2008. doi: 10.1016/j.envpol.2007.06.056.
  48. Türkmen M., Ciminli C., Çekin M. Determination of heavy metals in river waters and sediments by FAAS and ICP-OES, Fresenius Environ. Bull., 14(7), 509–513, 2005.
  49. Zhou X., et al. Magnetic solid-phase extraction for heavy metal ions using functionalized graphene oxide: A review, TrAC Trends Anal. Chem., 102, 2018, 280-290. doi: 10.1016/j.trac.2018.02.016.
  50. Li J., et al. Hybrid nanomaterials for solid-phase extraction of heavy metal ions, Anal. Chim. Acta, 1021, 2022, 1-16. doi: 10.1016/j.aca.2022.02.026.
  51. Hou X., et al. Recent advances in ICP techniques for elemental analysis, Anal. Chim. Acta, 1094, 2020, 1-15. doi: 10.1016/j.aca.2019.10.048.
  52. Wang X., et al. Preconcentration and determination of lead and cadmium in environmental samples by solid phase extraction using novel polymer sorbents, J. Hazard. Mater., 384, 2020, 121275. doi: 10.1016/j.jhazmat.2019.121275.