This study investigated the removal of phosphate (PO4 3- ) from disodium hydrogen phosphate (Na2HPO4) solution using Iron-loaded pomegranate peel (IL-PP) as a bio-adsorbent. The full factorial design using Minitab19 software was applied to analyze the effects of influencing parameters and their interactions and derive the equation that adequately describe PO4 3- removal by IL-PP. Effective PO4 3- removal up to 90% was achieved within 60 min, at pH 9 and 25 °C temperature using a 150 mg dose of IL-PP

Bellahsen Naoufal

Hodúr Cecília

Kertész Szabolcs

English

University of Szeged

27th International Symposium on Analytical and Environmental Problems  15  FACTORIAL DESIGN ANALYSIS OF PHOSPHATE REMOVAL FROM MODEL SOLUTION BY IRON-LOADED POMRGRANATE PEEL  Naoufal Bellahsen1, Szabolcs Kertész2, Cecilia Hodúr2  1Materials and Solutions Structure Research Group, University of Szeged, H-6720 Szeged, Dóm tér 8, Hungary 2Department of Process Engineering, Faculty of Engineering, University of Szeged, Moszkvai krt. 9, 6725 Szeged, Hungary e-mail: naoufal.bel@hotmail.com  Abstract This study investigated the removal of phosphate (PO43-) from disodium hydrogen phosphate (Na2HPO4) solution using Iron-loaded pomegranate peel (IL-PP) as a bio-adsorbent. The full factorial design using Minitab19 software was applied to analyze the effects of influencing parameters and their interactions and derive the equation that adequately describe PO43- removal  by IL-PP. Effective PO43- removal up to 90% was achieved within 60 min, at pH 9 and 25 °C temperature using a 150 mg dose of IL-PP.   Introduction Excess release of phosphorus is the main culprit for the eutrophication of freshwater and marine ecosystems [1]. Furthermore, phosphorus which is a critical element for plant growth is threaten by exhaustion [2]. Therefore the recovery of phosphate from wastewater is highly required protect the ecosystem and sustain the environment. Biosorption process using agricultural and food waste (AFW) presents several advantages such as simplicity, cost-effectiveness, and wide availability of potential bio-adsorbents that can be further applied to soil as fertilizer after adsorption of phosphate. Pomegranate peel (PP) is among the widely abundant AFW [3]. Valorization of PP as bio-adsorbent for heavy metals, dyes and other contaminants removal was investigated in several studies and it showed promising adsorptive characteristics in both raw and activated forms or even as active carbon [4–6]. The present study investigated the efficiency of IL-PP at PO43- removal from Na2HPO4 model solution using factorial design methodology in order to prove the performance of IL-PP as an alternative to conventional phosphate adsorbents.  Experimental PO43− removal rate was calculated as follows: 𝐑𝐞𝐦𝐨𝐯𝐚𝐥 % =  𝐂𝐢−𝐂𝐟𝐂𝐢. 𝟏𝟎𝟎    Where Ci (mg·L−1) and Cf (mg·L−1) are the initial and final PO4-P concentrations, respectively. 23 full factorial design was used to evaluate the effect of pH, adsorbent dose, temperature and their interactions on PO43- removal by IL-PP. Factorial design plots such as plots for the main effects and interactions, Pareto chart, and normal plot for the standardized effects describe how the effect of one factor varies with the level of the other factors. This technique investigates all possible combinations and verifies the accuracy of the obtained mathematical model through the analysis of variance (ANOVA) to achieve optimum removal of PO43−. Parameters such as initial PO4-P concentration (40 mg.L-1), contact time (60 min) and stirring speed (150 rpm) were kept constant and the three factors pH, adsorbent dose, and temperature of solution were varied at two levels as given in (Table 1). A centre point was duplicated and added to matrix in order to verify the curvature of the studied model. 27th International Symposium on Analytical and Environmental Problems  16  Table 1. Factors and levels used in the factorial design for PO43- removal by IL-PP Factor Symbol Low level (-1) High level (+1) Centre point (0, 0, 0) pH Adsorbent dose Temperature A B C 3 100 25 9 150 45 6 125 35  Results and discussion The mean of the experimental results for the respective high and low levels of pH, adsorbent dose and temperature are shown in Figure 1.   Figure 1. Cube plots for PO43- removal by IL-PP Table 2 presents the main effects and interactions, model coefficients, standard deviation of each coefficient, standard errors, Fisher test value (F-value), and probability value (P-value).  Table 2. Estimated effects and coefficients for PO43- removal by IL-PP Term Effect Coef SE coef t-value p-value VIF Constant  71.195 0.125 569.56 0.001  pH (A) 12.650 6.325 0.125 50.60 0.013 1.00 Adsorbent dose (B) 32.565 16.282 0.125 130.26 0.005 1.00 Temperature (C) 5.440 2.720 0.125 21.76 0.029 1.00 A*B −6.855 −3.428 0.125 −27.42 0.023 1.00 A*C −1.480 −0.740 0.125 −5.92 0.107 1.00 B*C −2.145 −1.072 0.125 −8.58 0.074 1.00 A*B*C −1.065 −0.533 0.125 −4.26 0.147 1.00 Ct Pt  0.055 0.280 0.2 0.876 1.00 S 0.135015 R2 100.00% R2 (Adj) 99.96%  The effects of pH (A), adsorbent dose (B), temperature (C), and the interaction (A*B) were significant at a 5% probability level (P < 0.05). However the effects of interactions (A*C), (B *C) and (A*B *C) were not significant (P > 0.05). Furthermore, the adjusted square correlation coefficient R2 (adj) had a value of 99.96%, which indicates that the presented model perfectly fit the statistical model [7].  In this way, PO43- removal by IL-PP could be expressed using Eq. (1). 27th International Symposium on Analytical and Environmental Problems  17  Phosphate removal% =  71.195 + 6.325 𝐴 + 16.282 𝐵 + 2.720 𝐶 − 3.428 𝐴 ∙ 𝐵 +0.740 𝐴 ∙ 𝐶 − 1.072 𝐵 ∙ 𝐶 − 0.533 𝐴 ∙ 𝐵 ∙ 𝐶 + 0.055 𝐶𝑡 𝑃𝑡                                           (1) where: A (pH), B (adsorbent dose), C (temperature), AB, AC and BC (their 2- way interaction) and ABC (their 3-way interaction). (3< pH <9, 100 mg< Adsorbent dose < 150 mg, 25 °C < temperature < 45°C). ANOVA was performed to investigate the significance of parameters affecting PO43− removal to ensure the accuracy of the model. Table 3 presents the sum of the squares used to estimate the effect of factors, the F-ratio (i.e., the ratio of individual mean square effects to the mean square error) and the P-value (i.e., the level of significance leading to the rejection of the null hypothesis). The results showed are in accordance with the estimated effects shown in Table 2 and thus confirm the accuracy of the factorial design model. Table 3. ANOVA for PO43- removal by IL-PP Source DF Adj SS Adj MS F-Value P-Value Model 8 2610.03 1118,32 2610.03 0.015 Linear 3 2500.19 2499.60 6667.18 0.009 pH (A) 1 320.05 959.50 2560.36 0.013 Adsorbent dose (B) 1 2120.96 6361.90 16967.67 0.005 Temperature (C) 1 59.19 177.40 473.50 0.029 2-Way Interactions 3 107.56 107.54 286.84 0.043 A*B 1 93.98 281.88 751.86 0.023 A*C 1 4.38 13.13 35.05 0.107 B*C 1 9.20 27.63 73.62 0.074 3-Way Interactions 1 2.27 6.77 18.15 0.147 A*B*C 1 2.27 6.77 18.15 0.147 Curvature 1 0.00 0.00 0.04 0.876 Error 1 0.13 0.02   Total 9 2610.15     Figure 2 shows the main effects of each parameter on PO43− removal by IL-PP and thus helps to identify which parameters affect the response variable the most. A larger deviation is synonymous with a large effect [8]. Accordingly, adsorbent dose appears to have the greater effect on PO43- removal by IL-PP, followed by pH and then temperature that has a negligible effect.   Figure 2. Main effects plot for PO43- removal by IL-PP 27th International Symposium on Analytical and Environmental Problems  18  Figure 3 plots the interactions of the studied parameters. If the interaction lines are not parallel, this implies that the interaction has a strong effect, whereas parallel interaction lines indicate a weak effect Interpretation of interaction plot implies that if the interactions lines are not parallel, the interaction under control is strong and vice versa [9]. The most important interaction for PO43− removal by IL-PP appears to be (pH × adsorbent dose), followed by (adsorbent dose × temperature). The least important interaction was (pH × temperature), which had almost parallel interaction lines.   Figure 3. Interaction plot for PO43- removal by IL-PP A Pareto chart can be used to evaluate the significance of effects on the basis of how much they exceed the reference line [10]. Figure 4 shows that (A), (B), their interaction (AB), and (C) had a significant effect because their values exceeded that of the reference line (12.7, in red). However, the effects of interactions  (B × C), (A × C) and (A × B × C) are not significant as their values didn’t exceed the red line.  Figure 4. Pareto chart of the standardized effects for PO43- removal by IL-PP The results of 23 factorial design have showed that pH (A), adsorbent dose (B), their interaction (AB), and temperature (C) are the factors with significant effect on the PO43- removal from Na2HPO4 solution using IL-PP. On the other hand, the effect of temperature between high and low level was very weak and tends to be negligible (0.25%) when using optimum pH (9) and adsorbent dose (150 mg), therefore for technical and cost-effectivity reasons, a reduced model that take in consideration only the significant factors and neglect temperature is suggested. The 27th International Symposium on Analytical and Environmental Problems  19  new model is 22 factorial model with two factors (pH and adsorbent dose) at two levels and can be described using Eq. (2): Phosphate removal% =  71.19 + 6.33 𝐴 + 16.28 𝐵 − 3.43 𝐴 ∙ 𝐵 + 0.06 𝐶𝑡 𝑃𝑡              (2)  Conclusion The efficiency of IL-PP to remove PO43- from aqueous solution was evaluated in this study. Results introduce IL-PP as an efficient bio-adsorbent which could be used in a green technology for wastewater treatment, waste biomass management and phosphate recovery.   Acknowledgements Thanks the support of the János Bolyai Research Scholarship of the Hungarian Academy of Sciences (BO/00576/20/4, (BO/00161/21/4) and the New National Excellence Program of the Ministry of Human Capacities UNKP-21-5-550-SZTE).  References [1] H. Bacelo, A.M.A. Pintor, S.C.R. Santos, R.A.R. Boaventura, C.M.S. Botelho, Performance and prospects of different adsorbents for phosphorus uptake and recovery from water, Chem. Eng. J. 381 (2019) 122566. https://doi.org/10.1016/j.cej.2019.122566. [2] P.M. Melia, A.B. Cundy, S.P. Sohi, P.S. Hooda, R. Busquets, Chemosphere Trends in the recovery of phosphorus in bioavailable forms from wastewater, Chemosphere. 186 (2017) 381–395. https://doi.org/10.1016/j.chemosphere.2017.07.089. [3] N.H. Solangi, J. Kumar, S.A. Mazari, S. Ahmed, N. Fatima, N.M. Mujawar, Development of fruit waste derived bio-adsorbents for wastewater treatment: A review, J. Hazard. Mater. 416 (2021) 125848. https://doi.org/10.1016/j.jhazmat.2021.125848. [4] S. Ben-Ali, I. Jaouali, S. Souissi-Najar, A. Ouederni, Characterization and adsorption capacity of raw pomegranate peel biosorbent for copper removal, J. Clean. Prod. 142 (2016) 3809–3821. https://doi.org/10.1016/j.jclepro.2016.10.081. [5] F. Güzel, Ö. Aksoy, G. Akkaya, Application of Pomegranate (Punica granatum) Pulp as a New Biosorbent for the Removal of a Model Basic Dye (Methylene Blue), World Appl. Sci. J. 20 (2012) 965–975. https://doi.org/10.5829/idosi.wasj.2012.20.07.1609. [6] M. Afsharnia, M. Saeidi, A. Zarei, M.R. Narooie, H. Biglari, Phenol Removal from Aqueous Environment by Adsorption onto Pomegranate Peel Carbon Mojtaba, Electron. Physician. 8 (2016) 3248–3256. https://doi.org/10.19082/3248. [7] F. Geyikçi, H. Büyükgüngör, Factorial experimental design for adsorption silver ions from water onto montmorillonite, Acta Geodyn. Geomater. 10 (2013) 363–370. https://doi.org/10.13168/AGG.2013.0035. [8] A.K. Hegazy, N.T. Abdel-Ghani, G.A. 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Factorial design analysis of phosphate removal from model solution by iron-loaded pomegranate peel

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Factorial design analysis of phosphate removal from model solution by iron-loaded pomegranate peel

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