European Journal of Chemistry

Evaluation of the effects of significant factors and interactions on the enrichment of arsenic and chromium by pipette tip solid phase extraction using novel P-ZrO2CeO2ZnO nanoparticles/alginate beads


Main Article Content

Nichodimus Hokonya
Courtie Mahamadi
Netai Mukaratirwa Muchanyereyi
Timothy Gutu


The study seeks to determine the most significant factors affecting arsenic and chromium enrichment using novel P-ZrO2CeO2ZnO nanoparticles/alginate beads in order to minimize the total number of runs needed to successfully run the experiment. The effects of interactions between factors were also evaluated so that the optimum conditions which are not affected by the other factors are chosen for the experiments. The most significant factors on arsenic and chromium enrichment were screened for by using a half-factorial design, followed by the optimization of significant factors using the full-factorial design, and the interaction between factors was determined using ANOVA and interaction plots. The most significant factors for chromium recovery were sample volume, eluent flow rate, and sorbent dosage. For both chromium and arsenic recovery, interactions occurred between sample volume, dosage, and pH. The optimum conditions chosen for the experiment that gave favourable results for both metal ions were sample volume 5 mL, dosage 40 mg, pH = 7 and eluent flow rate 1 mL/min. This study showed that a preliminary screening step for the most significant factors for arsenic and chromium enrichment helps to reduce the number of total runs, and for the same experiment interactions between factors were present; hence, it is necessary to take this into account during the experimental design.

icon graph This Abstract was viewed 321 times | icon graph Article PDF downloaded 223 times

How to Cite
Hokonya, N.; Mahamadi, C.; Muchanyereyi, N. M.; Gutu, T. Evaluation of the Effects of Significant Factors and Interactions on the Enrichment of Arsenic and Chromium by Pipette Tip Solid Phase Extraction Using Novel P-ZrO2CeO2ZnO Nanoparticles Alginate Beads. Eur. J. Chem. 2022, 13, 327-336.

Article Details

Crossref - Scopus - Google - European PMC

[1]. Rasool, A.; Farooqi, A.; Xiao, T.; Masood, S.; Kamran, M. A.; Bibi, S. Elevated levels of arsenic and trace metals in drinking water of Tehsil Mailsi, Punjab, Pakistan. J. Geochem. Explor. 2016, 169, 89-99.

[2]. Raj, K.; Sardar, U. R.; Bhargavi, E.; Devi, I.; Bhunia, B.; Tiwari, O. N. Advances in exopolysaccharides based bioremediation of heavy metals in soil and water: A critical review. Carbohydr. Polym. 2018, 199, 353-364.

[3]. Genthe, B.; Kapwata, T.; Le Roux, W.; Chamier, J.; Wright, C. Y. The reach of human health risks associated with metals/metalloids in water and vegetables along a contaminated river catchment: South Africa and Mozambique. Chemosphere 2018, 199, 1-9.

[4]. Singh, R.; Singh, S.; Parihar, P.; Singh, V. P.; Prasad, S. M. Arsenic contamination, consequences and remediation techniques: a review. Ecotoxicol. Environ. Saf. 2015, 112, 247-270.

[5]. Masindi, V.; Gitari, W. M. Removal of arsenic from wastewaters by cryptocrystalline magnesite: complimenting experimental results with modelling. J. Clean. Prod. 2016, 113, 318-324.

[6]. Amran, M. B.; Aminah, S.; Rusli, H.; Buchari, B. Bentonite-based functional material as preconcentration system for determination of chromium species in water by flow injection analysis technique. Heliyon 2020, 6, e04051.

[7]. Yao, L.; Zhu, Y.; Xu, W.; Wang, H.; Wang, X.; Zhang, J.; Liu, H.; Lin, C. Combination of dispersive solid phase extraction with dispersive liquid-liquid microextraction for the sequential speciation and preconcentration of Cr(III) and Cr(VI) in water samples prior to graphite furnace atomic absorption spectrometry determination. J. Ind. Eng. Chem. 2019, 72, 189-195.

[8]. Sahayam, A. C.; Venkateswarlu, G.; Chaurasia, S. C. Determination of Cr(VI) in potable water samples after selective preconcentration on oxalate form of Dowex-1 and electro thermal atomic absorption spectrometric determination. Anal. Chim. Acta 2005, 537, 267-270.

[9]. Ahsan, M. A.; Katla, S. K.; Islam, M. T.; Hernandez-Viezcas, J. A.; Martinez, L. M.; Díaz-Moreno, C. A.; Lopez, J.; Singamaneni, S. R.; Banuelos, J.; Gardea-Torresdey, J.; Noveron, J. C. Adsorptive removal of methylene blue, tetracycline and Cr(VI) from water using sulfonated tea waste. Environ. technol. innov. 2018, 11, 23-40.

[10]. Akhtar, A.; Kazi, T. G.; Afridi, H. I.; Baig, J. A.; Khan, M. Simultaneous preconcentration of toxic elements in eye makeup products through single drop ionic liquid based non-dispersive microextraction method using narrow glass column: Multivariate application. Microchem. J. 2020, 157, 104963.

[11]. Molaei, K.; Bagheri, H.; Asgharinezhad, A. A.; Ebrahimzadeh, H.; Shamsipur, M. SiO 2 -coated magnetic graphene oxide modified with polypyrrole-polythiophene: A novel and efficient nanocomposite for solid phase extraction of trace amounts of heavy metals. Talanta 2017, 167, 607-616.

[12]. Yavuz, E.; Tokalıoğlu, Ş.; Şahan, H.; Patat, Ş. Nanosized spongelike Mn3O4 as an adsorbent for preconcentration by vortex assisted solid phase extraction of copper and lead in various food and herb samples. Food Chem. 2016, 194, 463-469.

[13]. Mandlate, J. S.; Soares, B. M.; Seeger, T. S.; Vecchia, P. D.; Mello, P. A.; Flores, E. M. M.; Duarte, F. A. Determination of cadmium and lead at sub-ppt level in soft drinks: An efficient combination between dispersive liquid-liquid microextraction and graphite furnace atomic absorption spectrometry. Food Chem. 2017, 221, 907-912.

[14]. Özzeybek, G.; Şahin, İ.; Erarpat, S.; Bakirdere, S. Reverse phase dispersive liquid-liquid microextraction coupled to slotted quartz tube flame atomic absorption spectrometry as a new analytical strategy for trace determination of cadmium in fish and olive oil samples. J. Food Compost. Anal. 2020, 90, 103486.

[15]. Blanchet-Chouinard, G.; Larivière, D. Determination of Pb in environmental samples after cloud point extraction using crown ether. Talanta 2018, 179, 300-306.

[16]. Arslan, Z.; Oymak, T.; White, J. 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 2018, 1008, 18-28.

[17]. Kim, E. J.; Baek, K. Enhanced reductive extraction of arsenic from contaminated soils by a combination of dithionite and oxalate. J. Hazard. Mater. 2015, 284, 19-26.

[18]. Najafi, N. M.; Eidizadeh, M.; Seidi, S.; Ghasemi, E.; Alizadeh, R. Developing electrodeposition techniques for preconcentration of ultra-traces of Ni, Cr and Pb prior to arc-atomic emission spectrometry determination. Microchem. J. 2009, 93, 159-163.

[19]. Płotka-Wasylka, J.; Szczepańska, N.; Owczarek, K.; Namieśnik, J. Miniaturized Solid Phase Extraction. In Comprehensive Analytical Chemistry; Elsevier, 2017; pp. 279-318.

[20]. Calderilla, C.; Maya, F.; Leal, L. O.; Cerdà, V. Recent advances in flow-based automated solid-phase extraction. Trends Analyt. Chem. 2018, 108, 370-380.

[21]. Dimpe, K. M.; Ngila, J. C.; Nomngongo, P. N. Preparation and application of a tyre-based activated carbon solid phase extraction of heavy metals in wastewater samples. Phys. Chem. Earth (2002) 2018, 105, 161-169.

[22]. Chen, S.; Wang, C.; Yan, J.; Lu, D. Use of fibrous TiO2@graphitic carbon nitride nanocomposites in dispersive micro-solid phase extraction for arsenic species before inductively coupled plasma mass spectrometry determination. Microchem. J. 2020, 158, 105211.

[23]. Ghazaghi, M.; Mousavi, H. Z.; Rashidi, A. M.; Shirkhanloo, H.; Rahighi, R. Graphene-silica hybrid in efficient preconcentration of heavy metal ions via novel single-step method of moderate centrifugation-assisted dispersive micro solid phase extraction. Talanta 2016, 150, 476-484.

[24]. Barciela-Alonso, M. C.; Plata-García, V.; Rouco-López, A.; Moreda-Piñeiro, A.; Bermejo-Barrera, P. Ionic imprinted polymer based solid phase extraction for cadmium and lead pre-concentration/determination in seafood. Microchem. J. 2014, 114, 106-110.

[25]. He, M.; Huang, L.; Zhao, B.; Chen, B.; Hu, B. Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review. Anal. Chim. Acta 2017, 973, 1-24.

[26]. Alipanahpour Dil, E.; Ghaedi, M.; Asfaram, A.; Mehrabi, F.; Bazrafshan, A. A. Optimization of process parameters for determination of trace Hazardous dyes from industrial wastewaters based on nanostructures materials under ultrasound energy. Ultrason. Sonochem. 2018, 40, 238-248.

[27]. Asfaram, A.; Ghaedi, M.; Goudarzi, A. Optimization of ultrasound-assisted dispersive solid-phase microextraction based on nanoparticles followed by spectrophotometry for the simultaneous determination of dyes using experimental design. Ultrason. Sonochem. 2016, 32, 407-417.

[28]. Jain, A.; Wadhawan, S.; Kumar, V.; Mehta, S. K. Colorimetric sensing of Fe3+ ions in aqueous solution using magnesium oxide nanoparticles synthesized using green approach. Chem. Phys. Lett. 2018, 706, 53-61.

[29]. Sharma, G.; Bhogal, S.; Naushad, M.; Inamuddin; Kumar, A.; Stadler, F. J. Microwave assisted fabrication of La/Cu/Zr/carbon dots trimetallic nanocomposites with their adsorptional vs photocatalytic efficiency for remediation of persistent organic pollutants. J. Photochem. Photobiol. A Chem. 2017, 347, 235-243.

[30]. Bayat, M.; Javanbakht, V.; Esmaili, J. Synthesis of zeolite/nickel ferrite/sodium alginate bionanocomposite via a co-precipitation technique for efficient removal of water-soluble methylene blue dye. Int. J. Biol. Macromol. 2018, 116, 607-619.

[31]. Shah, J.; Kumar Kotnala, R. Rapid green synthesis of ZnO nanoparticles using a hydroelectric cell without an electrolyte. J. Phys. Chem. Solids 2017, 108, 15-20.

[32]. Gnanamoorthi, K.; Balakrishnan, M.; Mariappan, R.; Ranjith Kumar, E. Effect of Ce doping on microstructural, morphological and optical properties of ZrO2 nanoparticles. Mater. Sci. Semicond. Process. 2015, 30, 518-526.

[33]. Thommes, M.; Kaneko, K.; Neimark, A. V.; Olivier, J. P.; Rodriguez-Reinoso, F.; Rouquerol, J.; Sing, K. S. W. Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report). Pure Appl. Chem. 2015, 87, 1051-1069.

[34]. Khazaeli, E.; Haddadi, H.; Zargar, B.; Hatamie, A. Response surface methodology based on central composite design as a chemometric tool for optimizing dispersive liquid-liquid microextraction for determining ultra-trace amounts of zinc in oil and water samples. Anal. Methods 2016, 8, 5101-5110.

[35]. Abbaspour, M.; Makhmalzadeh, B. S.; Arastoo, Z.; Jahangiri, A.; Shiralipour, R. Effect of anionic polymers on drug loading and release from clindamycin phosphate solid lipid nanoparticles. Trop. J. Pharm. Res. 2013, 12, 477-482.

[36]. Serkan Yalçın, M.; Kılınç, E.; Özdemir, S.; Yüksel, U.; Soylak, M. Phallus impudicus loaded with γ-Fe2O3 as solid phase bioextractor for the preconcentrations of Zn(II) and Cr(III) from water and food samples. Process Biochem. 2020, 92, 149-155.

[37]. Baranik, A.; Gagor, A.; Queralt, I.; Marguí, E.; Sitko, R.; Zawisza, B. Determination and speciation of ultratrace arsenic and chromium species using aluminium oxide supported on graphene oxide. Talanta 2018, 185, 264-274.

[38]. Ghorbani, Y. A.; Ghoreishi, S. M.; Ghani, M. Derived N-doped carbon through core-shell structured metal-organic frameworks as a novel sorbent for dispersive solid phase extraction of Cr(III) and Pb(II) from water samples followed by quantitation through flame atomic absorption spectrometry. Microchem. J. 2020, 155, 104786.

[39]. Zhang, Y.; Wang, W.; Li, L.; Huang, Y.; Cao, J. Eggshell membrane-based solid-phase extraction combined with hydride generation atomic fluorescence spectrometry for trace arsenic(V) in environmental water samples. Talanta 2010, 80, 1907-1912.

Most read articles by the same author(s)

Dimensions - Altmetric - scite_ - PlumX

Downloads and views


Download data is not yet available.


Metrics Loading ...
License Terms

License Terms


Copyright © 2024 by Authors. This work is published and licensed by Atlanta Publishing House LLC, Atlanta, GA, USA. The full terms of this license are available at and incorporate the Creative Commons Attribution-Non Commercial (CC BY NC) (International, v4.0) License ( By accessing the work, you hereby accept the Terms. This is an open access article distributed under the terms and conditions of the CC BY NC License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited without any further permission from Atlanta Publishing House LLC (European Journal of Chemistry). No use, distribution, or reproduction is permitted which does not comply with these terms. Permissions for commercial use of this work beyond the scope of the License ( are administered by Atlanta Publishing House LLC (European Journal of Chemistry).