This is an open access article under the CC BY license: Al-Khwarizmi Engineering Journal Al-Khwarizmi Engineering Journal ISSN (printed): 1818 – 1171, ISSN (online): 2312 – 0789 Vol. 20, No. 1, March, (2024), P. P. 1- 16 Modification, Characterization of Tea Residue-derived Activated Carbon, and Ciprofloxacin Adsorption Alaa Kareem Mohammed* Israa M. Rashid** Nadya Hussin AL Sbani*** Wan Nor Roslam Wan Isaha**** *,**Department of Biochemical Engineering / Al-Khwarizmi College of Engineering/ University of Baghdad/ Baghdad / Iraq ***Department of Chemical Engineering/ Faculty of Oil and Gas Engineering/ Al Zawia University/ Libya ****Department of Chemical and Process Engineering/ Faculty of Engineering and Built Environment/ Universiti Kebangsaan Malaysia/ 43600 UKM Bangi/ Selangor/ Malaysia Corresponding Author*Email: dr.alaa@kecbu.uobaghdad.edu.iq **Email: israa msc2018@kecbu.uobaghdad.edu.iq ***Email: n.alsbani@zu.edu.ly ****Email: wannorroslam@ukm.edu.my (Received 29 August 2023; Accepted 6 November 2023; Published 1 March 2024) https://doi.org/10.22153/kej.2024.11.001 Abstract Tea residue was used for preparing activated carbon (AC) which was used as an adsorbent to remove Ciprofloxacin (CIP) from synthetic contaminated water. This study investigates the physicochemical properties and adsorption efficiency of the prepared activated carbon. The activated carbon was prepared via two steps: Activation step using phosphoric acid (H3PO4) followed by carbonization at a temperature of 450 °C. Different factors were investigated to show their effects on the adsorption efficiency of (CIP). These factors were initial concentration of (CIP), pH, Absorption time, and adsorbent dosage. The maximum adsorption efficiency was 94.4% which was obtained when pH=8.75, contact time =454 min, adsorbent dosage =0.194 g/ 25 ml, and initial concentration of 200 ppm. The prepared activated carbon was characterized using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET). The prepared activated carbon was found to have a specific surface area of 774 m2/g. It was found that the Langmuir model well fit the adsorption isotherm of (CIP) on the prepared activated carbon. The produced activated carbon can adsorb Ciprofloxacin, with a maximum adsorption capacity of 256.41 mg g-1. A pseudo-second-order reaction model is effective at describing the kinetics of adsorption. The examination of adsorption thermodynamics reveals that the process of CIP adsorption on TAC is characterized by being both endothermic and spontaneous. Keywords: Adsorption, Tea residue, Active carbon, Ciprofloxacin, adsorption kinetics, adsorption thermodynamics. 1. Introduction Water is essential to human life and the health of the environment. Its existence is described as a limiting factor for human development. The growing population demands more water for a wide range of uses while water resources are limited. In addition to that, the rapid increase in industrial and human activities produces increasing amounts of waste matter as well as a higher spread of environmental water pollution [1]. Pollution, in its broadest sense, includes all changes that restrict natural functions and exert damaging effects on life [2]. Water pollution is the undesired change in water quality that leads to an unfavorable alteration of the physical, chemical, and biological properties of water that prevents domestic, commercial, industrial, agricultural, recreational, and other beneficial uses of water [3], [4]. There are various types of water pollutants; they are mainly mailto:dr.alaa@kecbu.uobaghdad.edu.iq mailto:israa%20msc2018@kecbu.uobaghdad.edu.iq mailto:n.alsbani@zu.edu.ly mailto:wannorroslam@ukm.edu.my mailto:wannorroslam@ukm.edu.my https://doi.org/10.22153/kej.2024.11.001 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 2 categorized into organic pollutants (e.g., petroleum hydrocarbons, aromatic hydrocarbons, organic halides, oils, dyes, etc.), and inorganic compounds (e.g., mineral acids, inorganic salts, trace elements, metal compounds, cyanides, sulfate, heavy metals, etc. [5], [6]. Veterinary medicine, human medicine, and the pharmaceutical industries are the principal contributors of pharmaceutical residues to the environment. In addition, when therapeutic compounds are discharged from factories, hospitals, and private homes or when unwanted pharmaceuticals are improperly disposed of, surface water and groundwater are contaminated, and drinking water is contaminated as a result. This poses a potential health risk to humans [7]. As a result, many treatment technologies have been proposed to treat this type of wastewater, such as reverse osmosis, ion exchange, adsorption, and nanofiltration [8]. Among these methods, the adsorption process is regarded as a promising method for the removal of micropollutants because of its simple design, low cost, high efficiency, and low production of toxic intermediates [9]. Due to antibiotics' toxicological effects on aquatic species and the resistance they can create in some bacterial strains, even at low concentrations, the presence of antibiotics in surface water and wastewater has been regularly reported and is growing in importance. [10]. Ciprofloxacin (CIP; C17H18O3N3F) is efficient against several different Gram-negative and Gram- positive bacteria [11]. CIP is frequently detected in groundwater and polluted wastewater as a result of its widespread use to treat several human and animal illnesses. [12]. Figure 1 shows the basic structure of CIP. Fig. 1. Structure of Ciprofloxacin. Several adsorbents, as cheap and efficient alternate materials, have been used, such as activated carbon, graphene, and silica, for water purification [13], [13]. A wide range of inorganic and organic pollutants are removed from the aquatic environment and industrial wastewater using activated carbon as an efficient adsorbent due to its high surface area, porosity structure, the presence of a broad spectrum of surface functional groups, and the capability of pollutant distributed on the high internal surface [14]. Activated carbon is widely used as an adsorbent due to its features such as low cost, availability, and surface heterogeneity [15]. Therefore, the practical usage of AC is restricted by the price of precursors and relatively high preparation costs [16]. Biomass waste as a renewable resource has attracted widespread attention. Aiming to reduce the total cost regarding the preparation of AC, using biomass waste as a precursor of AC, including groundnut husks [17], sugarcane bagasse [18], coconut shells [19], and tea residue [20], [21], is a viable option. Apart from the precursors, the physicochemical property of AC is also associated with the preparation method. The preparation of AC is divided into the following two methods, i.e., chemical activation and physical activation [22]. Typically, the activation temperature for lignocelluloses, precursors of AC, is between 800 and 1000 °C. During the chemical activation stage, acid, alkali, and salt, such as phosphoric acid (H3PO4) [20], potassium hydroxide (KOH) [15], and zinc chloride (ZnCl2) [23], are often employed as activating agents. Activating temperature, impregnation ratio, and activation time[24], [25] are some of the factors that affect the physicochemical properties of AC during the chemical activation process. This study was concerned with the feasibility of using tea residue as a low-cost and readily available sorbent material for the removal of Ciprofloxacin from aqueous solutions in batch mode. Tea residue was selected as a precursor to prepare activated carbon using chemical activation with H3PO4. The adsorption of Ciprofloxacin was also looked at to find out about the adsorption equilibrium, kinetics, and thermodynamics of the AC sample that was made. 2. Materials and Methods 2.1 Materials The tea residue was collected locally from leftover tea used in homes. Ciprofloxacin (CIP) was chosen as the target adsorbate and supplied by the Ministry of Health, Iraq. Ciprofloxacin was directly used without any further treatment. Phosphoric acid (H3PO4), used as the activating agent, was purchased from Himedia, India. Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 3 2.2 Preparation of activated carbon The waste tea was boiled with distilled water for 2 hours to remove water-soluble materials and then washed with distilled water until the washing water was colorless. The decolorized waste tea was dried in a drying oven at 110 °C for 10 hours. Before activation, the waste tea was fully mixed with a 60% (by wt) H3PO4 solution at an impregnation ratio of 1:2.5 (g waste tea /g H3PO4) at room temperature for 12 hours. The mixture was then filtered. After pretreatment, the raw material was placed in a closed steel crucible for carbonization in a furnace at 450 °C for 1 hour with nitrogen. The N2 flow is 150 cm3/min. After cooling to room temperature, the activated carbon was washed with distilled water (DW) until pH equaled seven. Then the carbons were dried at 110 °C for 6 hours. The product (TAC) was ground with mortar and sieved to obtain a particle size equal to or less than 350 µm then preserved in a desiccator for the upcoming batch trials. 2.3 Activated Carbon Characteristics Various characterizations were performed to describe the adsorbent produced. Scanning electron microscopy (SEM) was used to analyze the surface morphologies (JOEL, JSM-7600 F, Tokyo, Japan). Fourier transform infrared spectroscopy (FTIR 8400s Shimadzu) was used to study the functional groups on the adsorbent surface using KBr pellets in the (4000-400 cm-1) range. X-ray diffraction (XRD) was used to determine the crystalline phase (type Shimadzu XRD 6000 / Japan). The elemental composition of the absorbent was studied using EDX (JOEL, JSM- 7600 F, Tokyo, Japan). The Brunauer-Emmett- Teller (BET) analysis (HORIBA, SA-900 series, USA), to determine the surface area and porous structure of activated carbon. 2.4 Ciprofloxacin Adsorption on TAC At room temperature, batch adsorption experiments with 50 ml of Ciprofloxacin (CIP) solution were carried out at different initial concentrations (100–500 mg/l), pH (2–11), contact time (15-600 min), and active carbon (TAC) dosage (0.025–0.25 g/25 ml) at a constant speed of agitation (150 rpm). In the Erlenmeyer flask (250 ml), 50 ml of CIP solution of the specified initial concentration was put in. The TAC was added with a known quantity and mixed well at 150 rpm using an orbital shaker(Edmund Buhler SM25, German). After that, the adsorbent was removed from the aqueous solution using filter paper (Whatman). The final CIP concentration was measured using a double-beam UV-visible spectrophotometer (PG Instruments, Model UV T80, England). The CIP has a wavelength of 272.5 nm. The proportion of CIP removed by the prepared activated carbon (TAC) was calculated using Eq. (1) [26]. 𝑹 % = [ 𝑪₀ − 𝑪𝒆 𝑪₀ ] ∗ 𝟏𝟎𝟎% … (𝟏) Where R represents the removal percentage, 𝐶𝑜 & 𝐶𝑒 are initial and equilibrium concentrations of CIP (mg/l) respectively. The adsorption capacity at equilibrium qₑ was calculated using Eq.(2) [27], [28]. 𝒒ₑ = (𝑪₀ − 𝑪𝒆)𝑽 𝒎 … (𝟐) Where V(ml) is the sample volume and m (g)is the adsorbent quantity. 2.5 Design of an Adsorption Experiment The central composite Design (CCD) was used in the experimental design with four variables at five levels. These variables were: Adsorption time, solution acidity pH, adsorbent dosage, and CIP initial concentration Co. These variables were studied to investigate their impact on the adsorption efficiency of CIP. To design, analyze, and optimize the influencing parameters as well as to create an empirical model illustrating the CIP's adsorption efficiency, experimental design software (CCD) was employed. The independent factors, with their actual levels and coding chosen for process optimization, are shown in Table 1. Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 4 Table 1, Adsorption experimental design following CCD The effects of the parameter on CIP sorption were modeled and designed using the CCD method, as illustrated in Table 1. The time for absorption (𝑋1), pH (𝑋2), dose of the adsorbent (𝑋3), and CIP's initial concentration (𝑋4) were used to optimize the response removal of CIP (R%). The value of the coefficient of determination R2 was used to assess the fit of the regression, Eq. (3), and it was found to be 0.9997, approving the model's accuracy. 𝑅 = 80 + 3.11 𝑋1 + 0.3846 𝑋2 + 2.94𝑋3 − 3.2 𝑋4 + 1.22 𝑋1𝑋2 − 0.6994 𝑋1𝑋3 − 1.66 𝑋1𝑋4 − 0.1394 𝑋2𝑋3 − 1.44 𝑋2𝑋4 + 0.1069 𝑋3𝑋4 + 0.7178 𝑋1 2 + 0.2216 𝑋2 2 + 0.3016 𝑋3 2 + 0.1628 𝑋4 2 … (3) Figure 2 plots the predicted vs. observed values of removal percent content in the five-factor CCD analysis. The predicted responses from the empirical function are almost identical to the measured values, where all points are close to the line in the range of the operating factors. Fig. 2. Predicted vs. actual values of the percentage removal of CIP adsorption. 3. Results and Discussion 3.1 Characterization of the activated carbon 3.1.1 Characterization using FT-IR The chemical structure of the carbon substance is revealed through infrared spectroscopy. Figure 3 60 65 70 75 80 85 90 95 100 60 65 70 75 80 85 90 95 100P re d ic te d R em o v al % Actual Removal % Run X1: Adsorption time (min) X2: pH X3: Dosage (g/25ml) X4:sa Initial Conc. (mg/L) R% (Experimental) R% Predicted Residuals 1 307.5 6.5 0.1375 100 86.86 87.05 -0.1854 2 161.25 8.75 0.08125 200 77.1 77.05 0.0529 3 453.75 8.75 0.08125 400 77.6 77.61 -0.0137 4 161.25 4.25 0.19375 200 83 82.91 0.0913 5 307.5 6.5 0.1375 300 80 80 0 6 307.5 6.5 0.1375 500 74.2 74.26 -0.0571 7 161.25 8.75 0.19375 400 78 78.09 -0.0887 8 161.25 4.25 0.19375 400 83 82.92 0.0792 9 453.75 4.25 0.08125 400 77 77 -0.0008 10 453.75 4.25 0.19375 400 82 81.98 0.0246 11 307.5 6.5 0.25 300 87 87.09 -0.0871 12 161.25 4.25 0.08125 200 75.6 75.56 0.0358 13 307.5 2 0.1375 300 80 80.12 -0.1171 14 15 6.5 0.1375 300 76.5 76.66 -0.1604 15 161.25 8.75 0.19375 200 84 83.83 0.1658 16 453.75 8.75 0.19375 400 82.16 82.03 0.1292 17 161.25 8.75 0.08125 400 71.03 70.87 0.1558 18 453.75 8.75 0.08125 200 90.5 90.41 0.0858 19 600 6.5 0.1375 300 89 89.08 -0.0821 20 307.5 6.5 0.025 300 75.17 75.33 -0.1554 21 453.75 8.75 0.19375 200 94.4 94.41 0.0063 22 161.25 4.25 0.08125 400 75.22 75.15 0.0713 23 453.75 4.25 0.19375 200 88.6 88.59 0.0092 24 453.75 4.25 0.08125 200 84.21 84.04 0.1663 25 307.5 6.5 0.1375 300 80 80 0 26 307.5 6.5 0.1375 300 80 80 0 27 307.5 11 0.1375 300 81.53 81.66 -0.1254 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 5 shows the FTIR spectra of the synthetic carbons obtained by phosphoric acid activation at different concentrations. A broad transmittance band is visible in all spectra between 3200 and 3600 cm-1, with maxima at roughly 3420 to 3440 cm-1. The O- H stretching mode of the hydroxyl groups and the adsorbed water can be attributed to this band. All carbons' spectra have a faint, acute transmittance band between 2921 and 2855 cm-1, which decreases when carbons are exposed to high concentrations of H3PO4 [29]. The spectral bands shown in Figure 3 at wavenumbers 885, 840, and 775 cm-1 can be attributed to the out-of-plane deformation mode of the C-H bonds in different substituted benzene rings. The spectral feature observed at approximately 1700 cm-1 is commonly attributed to the stretching vibrations of C-O bonds in ketones, aldehydes, lactones, or carboxyl groups. The activated carbons that were synthesized exhibit a prominent spectral feature in the range of 1600- 1580 cm-1, which can be attributed to the vibrations of carbon-carbon bonds inside aromatic rings. The spectral peak observed at the wavenumber range of 1190-1200 cm-1 has been attributed to the stretching mode of hydrogen-bonded P=O, as well as the stretching vibrations of O-C bonds in P-O-C (aromatic) linkages. Additionally, this peak is also associated with the presence of P=OOH. This assignment is supported by reference [30]. In summary, the analysis of impregnation in infrared spectroscopy (IR) reveals significant alterations, notably the introduction of phosphorous groups (at a wavenumber of 1100 cm- 1) and the emergence of C-H vibrations. The latter can be attributed to the depletion of oxygen at the carbon material's surface. Fig. 3. FTIR spectra of the raw material, tea residue, and tea active carbon TAC. 3.1.2 Characterization using SEM The prepared active carbon's ( TAC ) form and surface morphology were investigated using SEM and EDX analysis, as illustrated in Figure 4. Figure 4a which illustrates the micro-surface morphologies of (TAC). The activated carbon depressions exhibit internal structures characterized by the presence of cavities and cracks on their external surfaces. The presence of holes on carbon surfaces can be attributed to the evaporation of the activating agent, phosphoric acid, during the carbonization process. This evaporation leads to the creation of voids in the areas formerly occupied by the agent. [31]. The H3PO4 impregnation, followed by a heat treatment in an inert environment, affects the microstructure of activated carbon. These effects will break down many of the bonds within the material and thus lose many of the components that make up the material, which will lead to an increase in pores within the material. The elemental analysis of activated carbon was conducted using energy-dispersive X- ray spectroscopy (EDX), as shown in Figure 4b, and indicates the existence of carbon at 69.66 %, oxygen at 16.89%, nitrogen at 12.06 %, and phosphorus at 1.48% Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 6 Fig. 4. (a) SEM image of Active carbon, (b) EDS spectra of TAC. 3.1.3 Surface Area and Pore Structure The results of the Brunauer-Emmett-Teller (BET) research revealed that the activated carbon derived from tea residue (TAC) exhibited a specific surface area of 774 m2/g and an average pore volume of 0.563 cm3/g. These results are consistent with the findings of Tao et al. [15] who prepared activated carbon from tea residue and found the surface area and pore size fall in the range of 503- 1337 m2/g and 0.353-0.817 cm3/g, respectively. Also, Tuli et al. [32] found that the surface area and pore size of the activated carbon were 850.58 cm3/g and 0.67 cm3/g, respectively. 3.2 ANOVA analysis Table 2 presents the empirical outcomes of the analysis of variance (ANOVA) assessments. The statistical significance of a parameter is indicated by its corresponding p-value. The model's F-value of 2592.2 and p-value of less than 0.0001 indicate that the model is statistically significant. In this case, 𝑋1, 𝑋2, 𝑋3, 𝑋4, 𝑋1 𝑋2, 𝑋1 𝑋3, 𝑋1 𝑋4, 𝑋2𝑋3, 𝑋2𝑋4, 𝑋3𝑋4, 𝑋1 2, 𝑋2 2, 𝑋3 2, and 𝑋4 2 are significant model terms. Values greater than 0.05 indicate the model terms are not significant. The analysis results in Table 2 indicate the significant effect of each variable in the model on removal efficiency. It can be observed that the initial concentration Co parameter in the linear form 𝑋4 (F-value = 11012.55) has the most significant effect on removal efficiency, followed by the linear term of the mixing time 𝑋1 (F-value = 10390.10). In interactive terms, the most significant effective parameters are pH and initial concentration 𝑋2𝑋4 (F-value = 1488.12), and the other is mixing time and initial concentration 𝑋1𝑋4 (F-value = 1971.82), as well as mixing time and dosage 𝑋1𝑋3 (F-value = 1072.36). Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 7 Table 2, ANOVA Results of CIP Adsorption Findings. An analysis of variance (ANOVA) was employed to evaluate the appropriateness of the model. The quadratic model was found to be very significant, with the values of R-squared, adjusted R-squared, and predicted R-squared correlation coefficients equal to 0.9997, 0.9993, and 0.9981, respectively. This value indicates the proportionality of the experimental values and the predicted adsorption removal values. The ANOVA analysis of CIP adsorption nearly agrees with that of [7], who studied the removal of diclofenac from aqueous solution on apricot seeds using activated carbon synthesized by pyrocarbonic acid microwave and analyzed the results using the Response Surface Methodology method. 3.3 Interactions of Adsorption Parameters 3.3.1 pH and initial concentration of CIP Figure 5 shows the 3D response surface and contours of how the most important factors, pH and the initial concentration of CIP, interact. The p- value and F-value are indicators of these outcomes, as shown in Table 2. Figure 5 shows that the initial concentration is the most important factor in the adsorption process. In the range of the initial concentration of CIP (Co) between 100 and 500 ppm, the adsorption percentage increased with increasing pH. The observed phenomena can be attributed to the competitive interaction between CIP and H+ ions for adsorption sites, occurring on the surface of the adsorbent under conditions characterized by low pH levels. The adsorbent exhibits a progressive increase in adsorption capacity as the pH level rises, eventually reaching its peak adsorption efficiency of 94.4% at a pH of 8.75 and an initial concentration of 200 ppm. Nevertheless, when the pH is equal to 11, the adsorption capacity of TAC fibers exhibits a little drop. This can be attributed to the weakening of hydrogen bonding caused by the presence of OH-1 ions. This behavior aligns with the findings of Haotian et al., who conducted a study on the adsorption of tetracycline antibiotics. [33]. SOURCE SUM OF SQUARES MEAN SQUARE F-VALUE P-VALUE MODEL 808.4 57.74 2592.2 < 0.0001 significant 𝑿𝟏-TIME 231.45 231.45 10390.1 < 0.0001 significant 𝑿𝟐-PH 3.55 3.55 159.35 < 0.0001 significant 𝑿𝟑-DOSAGE 207.51 207.51 9315.32 < 0.0001 significant 𝑿𝟒-CO 245.31 245.31 11012.55 < 0.0001 significant 𝑿𝟏𝑿𝟐 23.89 23.89 351.32 < 0.0001 significant 𝑿𝟏𝑿𝟑 7.83 7.83 1072.36 < 0.0001 significant 𝑿𝟏𝑿𝟒 43.92 43.92 1971.82 < 0.0001 significant 𝑿𝟐𝑿𝟑 0.3108 0.3108 13.95 0.0028 significant 𝑿𝟐𝑿𝟒 33.15 33.15 1488.12 < 0.0001 significant 𝑿𝟑𝑿𝟒 0.1828 0.1828 8.2 0.0142 significant 𝑿𝟏² 10.99 10.99 493.46 < 0.0001 significant 𝑿𝟐² 1.05 1.05 47.01 < 0.0001 significant 𝑿𝟑² 1.94 1.94 87.09 < 0.0001 significant 𝑿𝟒² 0.5655 0.5655 25.39 0.0003 significant RESIDUAL 0.2673 0.0223 PURE ERROR 0 0 COR TOTAL 808.67 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 8 Fig . 5. Counter plots and 3D of removal percent (%) of CIP as a function of pH and initial concentration of CIP (ppm). 3.3.2 Adsorption time and initial concentration of CIP The influence of adsorption time on the CIP ions adsorbed by TAC was investigated and presented in Figure 6. The P-value and F-value are indicators of these outcomes, as shown in Table 2. Figure 6 shows that the adsorption time is the most important factor in the absorption process. When the initial concentration of CIP (Co) was between 100 and 200 ppm, increasing the adsorption time led to a higher percentage of CIP being removed. When the concentration of CIP is greater than 200 ppm, the adsorption capacity gradually slows down over time. This observation is due to the fact that the increasing concentration requires more time to be adsorbed. This behavior is in agreement with [10]. The optimum values for mixing time and initial concentrations are 454 min and 200 ppm, respectively. Fig. 6. Counter plots and 3D of removal percent (%) of CIP as a function of time (min) and initial concentration of CIP (ppm). 3.3.3 Mixing time and TAC dosage The effects of contact time and TAC dosage on the removal efficiency of CIP using TAC were studied in the ranges 15 - 600 min and 0.025 - 0.25 g / 25ml, respectively. The results are shown in Figure 7. This indicates that the removal efficiency is increased by increasing the contact time and TAC dosage until the values of the removal efficiency become constant. The optimum values for mixing time and TAC dosage are 454 min and 0.194 g / 25ml, respectively. These results are in agreement with the findings of [34]. Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 9 Fig. 7. Counter plots and 3D of removal percent (%) of CIP as a function of time (min) and TAC dosage (g/25ml). 3.4 Optimization of process variable The model accuracy was validated by optimizing the process parameters of the adsorption of CIP on TAC. The experimental result obtained confirmed the validity of the model, as shown in Table 3, with 94% removal. Table 3, Adsorption of CIP on TAC optimization following the designed model. 4. Adsorption Isotherms Adsorption isotherms, which are essential for creating adsorption systems, are calculated using equilibrium data. Figure 8 illustrates how two linearized isotherm models (Langmuir and Freundlich) are used to match the sorption data for CIP. Consequently, the slope and intercept of the linear plot were employed to determine the empirical coefficients presented in Table 4 for each model. Eq. (4) represents the Langmuir isotherm [35]. 𝑞𝑒 = 𝐾𝐿 𝑞𝑚 𝐶𝑒 1 + 𝐾𝐿𝐶𝑒 … (4) The linearized form of Eq. (4) is given by Eq. (5) 1 𝑞𝑒 = 1 𝑞𝑚 + 1 𝑞𝑚𝐾𝐿 1 𝐶𝑒 … (5) Where 𝑞𝑒 adsorption capacity at equilibrium (mg/g). 𝑞𝑚 : Maximum adsorption capacity (mg/g). 𝐾𝐿 : Constant (L/mg). 𝐶𝑒 : The equilibrium concentration of the (mg/L). Equation (5) can be used to determine both 𝐾𝐿 and 𝑞𝑚. The Freundlich model is based on the assumption of multi-layer adsorption and heterogeneous surface energies. Equation (6) represents the Freundlich isotherm [23]. 𝑞𝑒 = 𝐾𝐹𝐶𝑒 1 𝑛 … (6) Eq. (7) represents the linearization form of the Freundlich model ln(𝑞𝑒) = ln(𝐾𝐹) + 1 𝑛 ln(𝐶𝑒) … (7) The parameters 𝑛 and 𝐾𝐹 are Freundlich constants, which represent the adsorption intensity and the adsorption capacity, respectively. Equation (7) is used to determine the values of 𝑛 and 𝐾𝐹. Figure (8) shows the fitting of both models Langmuir and Freundlich. Process Parameters (Coded) Time pH Dosage Co Predicted R2 Actual R2 Error % Optimal Values 454 8.75 0.194 200 0.9993 0.9981 0.0012 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 10 Fig. 8. Linear form of the Freundlich and Langmuir isotherm models for the sorption of CIP onto TAC. Table 4 shows the parameters of both models Langmuir and Freundlich as well as the correlation coefficient (𝑅2). Table 4, Parameters of Langmuir and Freundlich equations According to the correlation coefficient values (𝑅2), the Langmuir model matches the experimental results more closely than the Freundlich model, which predicts a high monomolecular layer on the surface of the TAC. 5. Kinetics Adsorption Two kinetic models were used to analyze the adsorption kinetics of CIP onto TAC to comprehend the regulating mechanism and the adsorption rate: pseudo-first-order and pseudo- second-order as represented by Equations (8) and (9), respectively. [36], [37]. ( 𝑑𝑞𝑡 𝑑𝑡 ) = 𝐾1 (𝑞𝑒 − 𝑞𝑡) … (8) 𝑑𝑞𝑡 𝑑𝑡 = 𝐾2(𝑞𝑒 − 𝑞𝑡)2 … (9) The parameters 𝑞𝑡 and 𝑞𝑒 (mg/g) represent the amounts of the TC adsorbed on the TAC at time t and equilibrium, respectively. 𝐾1(min-1) and 𝐾2(𝑔/ 𝑚𝑔. 𝑚𝑖𝑛) represent the rate constants of the pseudo-first-order and pseudo-second-order kinetics, respectively. Eqs. (10) and (11), respectively, give the linearized forms of the pseudo-first-order and pseudo-second- order [38]. 𝑙𝑛(𝑞𝑒 − 𝑞𝑡) = ln 𝑞𝑒 − 𝐾1𝑡 … (10) 𝑡 𝑞𝑡 = ( 1 𝐾2𝑞𝑒 2) + ( 𝑡 𝑞𝑒 ) … (11) The experimental adsorption data are graphically presented in Figure 9 using the pseudo-first-order and pseudo-second-order kinetics models. Freundlich Langmuir 𝐾𝐹 n 𝑅2 𝐾𝐿 𝑞𝑚 𝑅2 (L/mg) (mg/g) 37.13 2.76 0.859 24.95 256.41 0.9568 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 11 Fig. 9. Kinetics models for adsorption of CIP onto TAC. (a) Pseudo-first-order, (b) Pseudo -second-order reaction model. Table 5, Kinetics parameters of pseudo-first-order and pseudo-second-order adsorption models Table 5 shows that the pseudo-second-order kinetic well fits the experimental data of CIP adsorption on the TAC. 6. Study of Thermodynamics Three thermodynamic parameters, including, entropy change ∆𝑆0 , Gibbs free energy change ∆𝐺0, and enthalpy change ∆𝐻0, were studied to investigate the thermodynamic behavior of the adsorption onto the TAC. The Gibbs free energy change ∆𝐺0, was determined by Eq. (12) [39]. ∆𝐺𝑜 = 𝑅𝑇𝑙𝑛(𝐾𝑐) … (12) Where R is the universal gas constant (𝑅 = 8.314 𝑘𝐽 𝑘𝑚𝑜𝑙. 𝐾⁄ ) and 𝐾𝑐 is the distribution coefficient that can be calculated by Eq. (13) [40]. 𝐾𝑐 = 𝑞𝑒 𝐶𝑒 … (13) The relation between the thermodynamic parameters enthalpy change ∆𝐻𝑜, entropy change ∆𝑆𝑜, and Gibbs free energy change ∆𝐺𝑜is given by Eq. (14) [41]. ∆𝐺𝑜 = ∆𝐻𝑜 − 𝑇∆𝑆𝑜 … (14) Substituting Eq. (14) in Eq. (12) gives ln 𝐾𝑐 = ∆𝑆° 𝑅 − ∆𝐻° 𝑅𝑇 … (15) The values of ln(Kc) were calculated by Eq. (13) at different temperatures. Plotting ln (𝐾𝑐) vs. 1 𝑇 gives a linear relation from which the values of ∆𝐻𝑜 and ∆𝑆𝑜 can be calculated. Figure 9 illustrates a positive correlation between the value of 𝐾𝑐 and temperature, indicating that when the temperature rises, 𝐾𝑐 also increases. Table 6 presents a comprehensive overview of the thermodynamic parameters ∆Go, ∆Ho, and ∆So at various temperatures for the adsorption of CIP onto TAC. Pseudo-first-order Pseudo-second-order 𝐾1 𝑞𝑒 𝑅2 𝐾2 𝑞𝑒 𝑅2 (min-1) (mg/g) (g/mg. min) (mg/g) 0.0003 74.96 0.8999 0.001 51.282 0.9989 Alaa Kareem Mohamme Al-Khwarizmi Engineering Journal, Vol. 20, No. 1, P.P. 1- 16(2024) 12 Fig. 9. 𝐥𝐧 𝑲𝒄 versus 𝟏 𝑻 for the adsorption of CIP on TAC. Table 6, Thermodynamic parameters for the adsorption of CIP by the Active Carbon The presence of negative values for ∆𝐺𝑜 signifies the natural spontaneity of the sorption process. The positive value of ∆Ho suggests the endothermic nature of the adsorption process. The entropy change has a positive sign, which reveals that the randomness at the interface of solid and liquid will increase during the adsorption of CIP [42]. 7. Conclusion In the present study, the conversion of tea residue into activated carbon was accomplished, followed by its utilization for the efficient adsorption of Ciprofloxacin from an aqueous solution. The optimal conditions for the adsorption process, resulting in a maximum removal efficiency of 94.4% for Ciprofloxacin, are as follows: a mixing time of 454 minutes, an acidity pH of 8.75, a dosage of 0.194 g/25 ml of aqueous solution, and an initial Ciprofloxacin concentration of 200 ppm. The BET analysis of the prepared activated carbon shows a surface area value of 774 m2/g and 0.563 cm3/g, respectively. The adsorption of Ciprofloxacin on the active carbon that was synthesized may be effectively described using the Langmuir model, which precisely predicts the equilibrium adsorption behavior. 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(2024) 1-16، صفحة 1، العدد20المجلد جلة الخوارزمي الهندسيةم عالء كريم محمد 16 بقايا الشاي وامتصاص سيبروفلوكساسين تعديل وتوصيف الكربون المنشط المحضر من ***ناديا حسين السباني **إسراء مزاحم رشيد *عالء كريم محمد ****وان نور رسالم وان عيسى حيائية/ كلية الهندسة الخوارزمي/ جامعة بغدادة االقسم الهندسة الكيميائي**،* الكيميائية/ كلية هندسة النفط والغاز/ جامعة الزاوية/ ليبيا*** قسم الهندسة **** قسم الهندسة الكيميائية وهندسة العمليات/ كلية الهندسة والبيئة / جامعة كيبانجسان/ ماليزيا dr.alaa@kecbu.uobaghdad.edu.iq*البريد االلكتروني: kecbu.uobaghdad.edu.iq2018israa_msc@*البريد االلكتروني:* n.alsbani@zu.edu.ly ***البريد االلكتروني: wannorroslam@ukm.edu.my****البريد االلكتروني: الخالصة االمتزاز من بقايا الشاي. تم دراسة الخواص الفيزيائية والكيميائية وكفاءة (AC) في تحضير الكربون المنشط عملةالمست للطريقةتقدم هذه الدراسة وصفا الكربنة عند الثانية و )4PO3H( مض الفوسفوريكاح عمالالتنشيط باستاالولى مرحلتين: على )AC( إنتاج الكربون المنشط تموقد للكربون المنشط المحضر. تشغيلية عدة عوامل ت دراسةتمفقد . (CIP)السيبروفلوكساسينالعقار الدوائي الكربون المنشط لغرض امتصاص عملاستدرجة مئوية. 450درجة حرارة االمتزاز، زمنالممتز، ومستوى الرقم الهيدروجيني، و CIPالتركيز األولي لـ هذه العوامل تشمل كفاءة االمتزاز. فيمعرفة تأثيرها الغرفة لدرجة حرارة ب ، (SEM)اإللكتروني الماسح ، والمجهر (FTIR)التحليل الطيفي لألشعة تحت الحمراء عمالاختبار خصائص الكربون المنشط باستوتم وكمية المادة المازة. هو Langmuirان نموذج وتمت دراسة نمط االمتزاز وتبين . (BET) المساحة السطحية والحجم المسامي بطريقة وحساب، (XRD)وحيود األشعة السينية على امتصاص السيبروفلوكساسين، يتمتع الكربون المنشط المنتج بالقدرةإذ (TAC). على الكربون المنشط بالشاي CIPعملية امتزاز لالموديل المناسب .الدرجة الثانية تمت دراسة حركية االمتزاز وتبين انه يمكن تمثيلها بتفاعل من وقد رام. م/غغمل 256.41قدرة امتصاص قصوى تبلغ ب mailto:dr.alaa@kecbu.uobaghdad.edu.iq mailto:israa_msc2018@kecbu.uobaghdad.edu.iq mailto:n.alsbani@zu.edu.ly mailto:n.alsbani@zu.edu.ly mailto:wannorroslam@ukm.edu.my