Evaluation of Lead Ion in the Wastewater of the Lifting and Treatment Stations Using ICP-MS and CPE Methods


Mohammed Nasser Hussain(1), Ahmed Fadhil Khudhair(2*), Hussain Jawad Ahmed(3)

(1) Department of Chemistry, College of Science, University of Kerbala, Karbala 56001, Iraq
(2) Department of Chemistry, College of Science, University of Kerbala, Karbala 56001, Iraq
(3) Department of Chemistry, College of Science, University of Kerbala, Karbala 56001, Iraq
(*) Corresponding Author


To pre-concentrate trace amounts of lead before determining it by UV-vis spectrophotometer, a new method for micelle-mediated phase separation has been created. The process depends on the extraction of lead from iodine media using Triton X-114 in the cloud point extraction method without the need for any chelating agents, where the optimal conditions for the method were achieved, which temperature 50 °C, pH 4, and 30 mmol L−1 concentration of KI, 0.3 mL of 2% (v/v) Triton X-114, and time of 10 min in the water bath. Linearity was followed between 1 and 16 µg/mL of lead concentration. The method's lead detection limit is 0.1 µg/mL and %RSD 3.633. Additionally, the interference impact of certain cations was evaluated. The proposed technique was successfully applied to determine the lead ion in the wastewater in ten different stations in the center and district of Al-Hur in Karbala City. The lead ion of the wastewater of the stations under study was also determined directly using inductively coupled plasma-mass spectrometry (ICP-MS) technology comparing its results with the new method and performing the statistical analysis of both methods. The p-value was less than 0.05, showing significant differences between both methods.


chemical pollutants; cloud point extraction method; ICP-MS; lead ion; wastewater

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[1] Ibrahem, S., Hassan, M., Ibraheem, Q., and Arif, K., 2020, Genotoxic effect of lead and cadmium on workers at wastewater plant in Iraq, J. Environ. Public Health, 2020, 9171027.

[2] Azimi, A., Azari, A., Rezakazemi, M., and Ansarpour, M., 2017, Removal of heavy metals from industrial wastewaters: A review, ChemBioEng Rev., 4 (1), 37–59.

[3] Yang, X., Liu, Y., Hu, S., Yu, F., He, Z., Zeng, G., Feng, Z., and Sengupta, A., 2021, Construction of Fe3O4@MXene composite nanofiltration membrane for heavy metal ions removal from wastewater Xiaojun, Polym. Adv. Technol., 32 (3), 1000–1010.

[4] Castro-Muñoz, R., Barragán-Huerta, B.E., Fíla, V., Denis, P.C., and Ruby-Figueroa, R., 2018, Current role of membrane technology: From the treatment of agro-industrial by-products up to the valorization of valuable compounds, Waste Biomass Valorization, 9 (4), 513–529.

[5] Bhuyan, M.M., Adala, O.B., Okabe, H., Hidaka, Y., and Hara, K, 2019, Selective adsorption of trivalent metal ions from multielement solution by using gamma radiation-induced pectin-acrylamide-(2-Acrylamido-2-methyl-1-propanesulfonic acid) hydrogel, J. Environ. Chem. Eng., 7 (1), 102844.

[6] Sadee, B.A., and Ali, R.J., 2022, Determination of essential and trace elements in various vegetables using ICP-MS, Baghdad Sci. J., 20, 715–725.

[7] Castro-Muñoz, R., Gontarek, E., and Figoli, A., 2020, “Chapter 7- Membranes for toxic- and heavy-metal removal” in Current Trends and Future Developments on (Bio-) Membranes, Eds. Figoli, A., Li, Y., and Basile, A., Elsevier, Amsterdam, Netherlands, 125–149.

[8] Natrayan, L., Kaliappan, S., Dheeraj Kumar Reddy, C.N., Karthick, M., Sivakumar, N.S., Patil, P.P., Sekar, S., and Thanappan, S., 2022, Development and characterization of carbon-based adsorbents derived from agricultural wastes and their effectiveness in adsorption of heavy metals in wastewater, Bioinorg. Chem. Appl., 2022, 1659855.

[9] Utami, U., Harianie, L., Dunyana, N.R., and Romaidi, R., 2020, Lead-resistant bacteria isolated from oil wastewater sample for bioremediation of lead, Water Sci. Technol., 81 (10), 2244–2249.

[10] Kamel, A.H., Amr, A.E.G.E., Al-Omar, M.A., and Elsayed, E.A., 2019, Pre-concentration based on cloud point extraction for ultra-trace monitoring of lead(II) using flame atomic absorption spectrometry, Appl. Sci., 9 (22), 4752.

[11] Saleh, M.G., Badawy, A.A., and Ghanem, A.F., 2019, Using of titanate nanowires in removal of lead ions from wastewater and its biological activity, Inorg. Chem. Commun, 108, 107508.

[12] Mortada, W.I., Kenawy, I.M.M., Abou El-Reash, Y.G., and Mousa, A.A., 2017, Microwave assisted modification of cellulose by gallic acid and its application for removal of aluminium from real samples, Int. J. Biol. Macromol., 101, 490–501.

[13] Sulaiman, R., Adeyemi, I., Abraham, S.R., Hasan, S.W., and Al-Nashef, I.M., 2019, Liquid-liquid extraction of chlorophenols from wastewater using hydrophobic ionic liquids, J. Mol. Liq., 294, 111680.

[14] Santana-Viera, S., Padrón, M.E.T., Sosa-Ferrera, Z., and Santana-Rodríguez, J.J., 2020, Quantification of cytostatic platinum compounds in wastewater by inductively coupled plasma mass spectrometry after ion exchange extraction, Microchem. J., 157, 104862.

[15] Arslan, Z., Oymak, T., and White, J., 2018, Triethylamine-assisted Mg(OH)2 coprecipitation/preconcentration for determination of trace metals and rare earth elements in seawater by inductively coupled plasma mass spectrometry (ICP-MS), Anal. Chim. Acta, 1008, 18–28.

[16] Dhahir, S.A., Kadhim, E.A., and AL-Gani, R.H.A., 2019, Micro spectrophotometric determination and cloud point extraction of sulphadimidine sodium in pure form and pharmaceutical drug, Baghdad Sci. J., 16 (2), 332–344.

[17] Ojeda, C.B., Rojas, F.S., and Pavón, J.M.C., 2010, Preconcentration of cadmium in environmental samples by cloud point extraction and determination by FAAS, Am. J. Anal. Chem., 1 (3), 127–134.

[18] Khudhair, A.F., Hassan, M.K., Alesary, H.F., and Abbas, A.S., 2019, A simple pre-concentration method for the determination of nickel(II) in urine samples using UV-vis spectrophotometry and flame atomic absorption spectrometry techniques, Indones. J. Chem., 19 (3), 638–649.

[19] Azooz, E.A., Ridha, R.K., and Abdulridha, H.A., 2021, The fundamentals and recent applications of micellar system extraction for nanoparticles and bioactive molecules: A review, Nano Biomed. Eng., 13 (3), 264–278.

[20] Al-ward, H.S., Al-Abachi, M.Q., and Ahmed, M.R., 2023, Spectrophotometric analysis of vancomycin hydrochloride in pure and pharmaceutical injections via batch and cloud point extraction techniques, Baghdad Sci. J., 20 (2), 409–419.

[21] Benabdallah, N., Hadj Youcef, M., Reffas, H., and Bendraoua, A., 2021, Evaluation and optimization of mixed-micelle mediated cloud point extraction of nickel(II) from concentrated chloride medium with Triton X-114-amphiphilic Schiff bases, Sep. Sci. Technol., 56 (14), 2407–2425.

[22] Awual, M.R., and Hasan, M.M., 2019, A ligand based innovative composite material for selective lead(II) capturing from wastewater, J. Mol. Liq., 294, 111679.

[23] Awual, M.R., 2019, Innovative composite material for efficient and highly selective Pb(II) ion capturing from wastewater, J. Mol. Liq., 284, 502–510.

[24] Awual, M.R., 2019, Mesoporous composite material for efficient lead(II) detection and removal from aqueous media, J. Environ. Chem. Eng., 7 (3), 103124.

[25] Awual, M.R., 2019, An efficient composite material for selective lead(II) monitoring and removal from wastewater, J. Environ. Chem. Eng., 7 (3), 103087.

[26] Awual, M.R., Hasan, M.M., Iqbal, J., Islam, A., Islam, M.A., Asiri, A.M., and Rahman, M.M., 2020, Naked-eye lead(II) capturing from contaminated water using innovative large-pore facial composite materials, Microchem. J., 154, 104585.

[27] Boudias, M., Gourgiotis, A., Montavon, G., Cazala, C., Pichon, V., and Delaunay, N., 2022, 226Ra and 137Cs determination by inductively coupled plasma mass spectrometry: State of the art and perspectives including sample pretreatment and separation steps, J. Environ. Radioact., 244-245, 106812.

[28] Hong, Y.S., Choi, J.Y., Nho, E.Y., Hwang, I.M., Khan, N., Jamila, N., and Kim, K.S., 2019, Determination of macro, micro and trace elements in citrus fruits by inductively coupled plasma–optical emission spectrometry (ICP-OES), ICP–mass spectrometry and direct mercury analyzer, J. Sci. Food Agric., 99 (4), 1870–1879.

[29] Zhang, X., Bai, J., Wang, R., Wei, X., Chen, M., Yang, T., and Wang, J.‏, 2023, Biological elemental analysis: A cute-meet of microfluidic device to inductively coupled plasma mass spectrometry, VIEW, 4 (1), 20220035.

[30] Mohammed Nawi, A., Chin, S.F., and Jamal, R., 2020, Simultaneous analysis of 25 trace elements in micro volume of human serum by inductively coupled plasma mass spectrometry (ICP-MS), Pract. Lab. Med., 18, e00142.

[31] Michalke, B., 2020, Review about powerful combinations of advanced and hyphenated sample introduction techniques with inductively coupled plasma-mass spectrometry (ICP-MS) for elucidating trace element species in pathologic conditions on a molecular level, Int. J. Mol. Sci., 23 (11), 6109.

[32] Rocha, F.S., Gomes, A.J., Lunardi, C.N., Kaliaguine, S., and Patience, G.S., 2018, Experimental methods in chemical engineering: Ultraviolet visible spectroscopy UV-vis, Can. J. Chem. Eng., 96 (12), 2512–2517.

[33] Azooz, E.A., Al-Wani, H.S.A., Gburi, M.S., and Al-Muhanna, E.H.B., 2022, Recent modified air-assisted liquid–liquid microextraction applications for medicines and organic compounds in various samples: A review, Open Chem., 20 (1), 525–540.

[34] Sheikh, M.C., Hasan, M.M., Hasan, M.N., Salman, M.S., Kubra, K.T., Awual, M.E., Waliullah, R.M., Rasee, A.I., Rehan, A.I., Hossain, M.S., Marwani, H.M., Islam, A., Khaleque, M.A., and Awual, M.R., 2023, Toxic cadmium(II) monitoring and removal from aqueous solution using ligand-based facial composite adsorbent, Liq. J. Mol., 389, 122854.

[35] Hamran, B.N., Khudhair, A.F., and Marhoon, A.A., 2020, Cloud point extraction of paracetamol in pharmaceutical formation coupling with spectrophotometric method, AIP Conf. Proc., 2213 (1), 020320.

[36] Mortada, W.I., Kenawy, I.M.M., Abdel-Rhman, M.H., El-Gamal, G.G., and Moalla, S.M.N., 2017, A new thiourea derivative [2-(3-ethylthioureido) benzoic acid] for cloud point extraction of some trace metals in water, biological and food samples, J. Trace Elem. Med. Biol., 44, 266–273.

[37] Ng, D.Q., and Lin, Y.P., 2015, Effects of pH value, chloride, and sulfate concentrations on galvanic corrosion between lead and copper in drinking water, Environ. Chem., 13 (4), 602–610.‏

[38] Khalifa, M.E., Mortada, W.I., El-defrawy, M.M., and Awad, A.A., 2019, Selective separation of gadolinium from a series of f-block elements by cloud point extraction and its application for analysis of real samples, Microchem. J., 151, 104214.

[39] Waliullah, R.M., Rehan, A.I., Awual, M.E., Rasee, A.I., Sheikh, M.C., Salman, M.S., Hossain, M.S., Hasan, M.M., Kubra, K.T., Hasan, M.N., Marwani, H.M., Islam, A., Rahman, M.M., Khaleque, M.A., and Awual, M.R., 2023, Optimization of toxic dye removal from contaminated water using chitosan-grafted novel nanocomposite adsorbent, J. Mol. Liq., 388, 122763.

[40] Zheng, H., Hong, J., Luo, X., Li, S., Wang, M., Yang, B., and Wang, M., 2019, Combination of sequential cloud point extraction and hydride generation atomic fluorescence spectrometry for preconcentration and determination of inorganic and methyl mercury in water samples, Microchem. J., 145, 806–812.

[41] Travičić, V., Cvanić, T., Šovljanski, O., Erceg, T., Perović, M., Stupar, A., and Ćetković, G., 2024, Updating the status quo on the eco-friendly approach for antioxidants recovered from plant matrices using cloud point extraction, Antioxidants, 13 (3), 280.

[42] Nikam, B.K., Jadhav, V.B., and Borse, M.S., 2022, Influence of alcohols on the lower consolute behavior and thermodynamic approach of Triton X-114 aqueous two-phase systems, J. Indian Chem. Soc., 99 (8), 100572.

[43] Adnan Azooz, E., Abd Wannas, F., Kadhim Ridha, R., Kadhim Jawad, S., and Al-Mulla, E.A.J., 2022, A Green approach for micro determination of silver(I) in water and soil samples using vitamin C, Anal. Bioanal. Chem. Res., 9 (2), 133–140.

[44] Gao, Y., Wu, P., Li, W., Xuan, Y., and Hou, X., 2010, Simultaneous and selective preconcentration of trace Cu and Ag by one-step displacement cloud point extraction for FAAS determination, Talanta, 81 (1-2), 586–590.

[45] Kachangoon, R., Vichapong, J., Santaladchaiyakit, Y., and Srijaranai, S., 2020, Cloud-point extraction coupled to in-situ metathesis reaction of deep eutectic solvents for preconcentration and liquid chromatographic analysis of neonicotinoid insecticide residues in water, soil and urine samples, Microchem. J., 152, 104377.

[46] Broadhurst, D., Goodacre, R., Reinke, S.N., Kuligowski, J., Wilson, I.D., Lewis, M.R., Dunn, W.B., 2018, Guidelines and considerations for the use of system suitability and quality control samples in mass spectrometry assays applied in untargeted clinical metabolomic studies, Metabolomics, 14 (6), 72.

DOI: https://doi.org/10.22146/ijc.87545

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