Adsorptive Separation of Lead (Pb2+) from Aqueous Solution Using

Article pubs.acs.org/jced

Adsorptive Separation of Lead (Pb2+) from Aqueous Solution Using Tri‑n‑octylamine Supported Montmorillonite Dipaloy Datta† and Hasan Uslu*,‡,§ †

Department of Chemical Engineering, Malaviya National Institute of Technology (MNIT), Jaipur, Rajasthan 302017, India Engineering and Architecture Faculty, Industrial Engineering Department, Iṡ tanbul Esenyurt University, Esenyurt 34510, Iṡ tanbul, Turkey § Chemical and Materials Engineering Department, Faculty of Engineering, King Abdulaziz University, Jeddah 21589, Saudi Arabia ‡

ABSTRACT: Divalent lead present in the water stream was removed by using adsorption techniques with montmorillonite clay (Mt) modified with tri-n-octylamine (Mt-TOA). Batch adsorption data at equilibrium were determined with different initial Pb2+ ions concentration (8, 10, 12, 14, and 16 mg·L−1) in the aqueous solution at 298 K, and these results were correlated by using three different isotherm models, for instance, the Langmuir, the Freundlich, and the Temkin. The twoparameter Langmuir model was the best fit to the equilibrium data with a coefficient (R2) greater than 0.99. The maximum capacities for monolayer adsorption of Mt and Mt-TOA were determined to be 3.37 mg·g−1 and 33.1 mg·g−1, respectively, as estimated from Langmuir. Also, experimental values were generated to evaluate the influence of adsorbent amount (w, 0.05−0.3 g for Mt, 0.01−0.06 g for Mt-TOA), starting Pb2+ ion concentration (C0, 8 mg·L−1 to 16 mg·L−1), pH (between 1 and 9), and contact period (t, from 10 to 110 min) on the removal effectiveness and adsorption capability of Mt and Mt-TOA adsorbents. In respect to kinetic studies, the removal efficiency of Pb2+ ion reached to a fixed value of 81.42% with Mt (0.1 g) and 80.67% by Mt-TOA (0.01 g) next 100 and 80 min, respectively. Pseudo-first order, pseudo-second order, and intraparticle diffusion models were studied to obtain the kinetic parameters of the adsorption practice. It is observed that the rate of mass transfer of Pb2+ ions was mainly governed by the intraparticle diffusion mechanism. retrieval of heavy metal ions from the water stream.11−16 Among all of these, adsorption is a widely accepted and applied technique for the effective removal of heavy metal ions. The process is uncomplicated as it uses simple equipment and easy operation. Moreover, the solid adsorbent may be used in more number of adsorption cycles without compromising on the metal-adsorption capacity of adsorbent. Therefore, tremendous effort has been devoted to research and characterize new adsorbents for the specific metal ion removal with a high adsorption capacity. It is very much essential to study the adsorption equilibrium isotherms and kinetics for the design and operation of adsorbers for the treatment of wastewater containing toxic pollutants. In the current study, equilibrium isotherms such as Langmuir, Freundlich, and Temkin and kinetic models such as the pseudo-first-order, pseudo-second-order, and intraparticle diffusion have been applied to illustrate or predict the adsorption mechanism of the adsorbent, respectively. The aim of the study is to carry out the adsorptive removal of Pb2+ ions from the water solution onto Montmorillonite (Mt) and its modified version by using tri-n-octylamine, an aminic solvent (Mt-TOA). The effect of important design variables such as the adsorbent amount, concentration of Pb2+ ions, pH, and contact

1. INTRODUCTION The appearance of heavy metal ions in the aqueous bodies has become a serious concern for the society and environment due to their increased discharge.1,2 Metal ions like chromium (Cr), manganese (Mn), arsenic (As), lead (Pb), copper (Cu), cadmium (Cd), nickel (Ni), and mercury (Hg), zinc (Zn), and so forth, are mostly nonbiodegradable and toxic in nature. Processing industries like metal coating and dying, acid batteryoperated industrial, reproduction, explosive manufacturing, photographic materials, and tetraethyl lead industrial, and ceramic-glass manufacturing use lead, and the effluent wastewater streams of these industries are the primary source of lead in the aquatic environment. Lead ion poisons humans, causing severe harm to the nervous system, reproductive system, kidney, liver, and brain, causing serious illness, or finally leading to death. Further, acute reactions to lead ions may be associated with abortion, barrenness, miscarriages, and neonatal death.3−6 Lead ions found in the industrial wastewater streams are high in concentration (200−500 mg·dm−3). The US Environmental Protection Agency (EPA) limits 0.05 mg·dm−3 of lead in the drinking water, and hence, even a small concentration of lead in the aqueous stream will be very toxic.7−10 Many separation methods like filtration, chemical precipitation, electrodeposition, reverse osmosis, evaporation, membranes, solvent extraction, ion-exchange adsorption, and so forth, have been tried and developed for the separation and © XXXX American Chemical Society

Received: August 10, 2016 Accepted: November 16, 2016

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DOI: 10.1021/acs.jced.6b00716 J. Chem. Eng. Data XXXX, XXX, XXX−XXX

Journal of Chemical & Engineering Data

Article

adsorption process provides very significant and fundamental information which are required to evaluate the capacity or affinity of an adsorbent used. The study is also important as it helps in selecting a suitable adsorbent. Therefore, the results obtained for the adsorption of Pb2+ ion were analyzed by different thermodynamic equilibria and kinetic models as given in Table 1.18−25

time was evaluated on the adsorption capacity of Montmorillonite.

2. MATERIALS AND METHODS 2.1. Materials. Montmorillonite, procured from Resadiye/ Tokat, Turkey was used for the adsorptive removal of Pb2+ ions from aqueous solution. The clay material is a soft phyllosilicate group of minerals present in its microscopic crystal form and has an elemental composition of the form: [Al1·47Fe0.29Mg0.23][Al0.076Si3.29]O10(OH)2 as provided by the supplier. The aqueous solution of Pb2+ ions was made by dissolving lead nitrate [Pb(NO3)2; Sigma-Aldrich, purity: 99 wt %] in distilled water. Trin-octylamine (TOA, purity: 98 wt %) was obtained from Sigma-Aldrich. 2.2. Impregnation of TOA into Montmorillonite. The montmorillonite clay received was first grinded in a laboratory type ball-mill (FRITSCH, Pulverisette 5 model). The screening of particles was done with a ASTM sieve of 100 mesh, and the undersized particles were collected and used as adsorbent. The impregnation of tri-n-octylamine solvent (1 mL per 3 g of MM) into the montmorillonite clay was performed as per the procedure explained by Ahmad et al.17 The characterization of modified clay was also done and presented in somewhere else.15−17 2.3. Methods. To perform the equilibrium experiments on adsorption, an Erlenmeyer flask of 100 mL volume was used, and 25 mL of aqueous solution of Pb2+ with an appropriate amount of adsorbent was placed in it. This solution was kept in a thermostatic shaker at 298 K for 2 h (determined by preliminary tests) until equilibrium was achieved. In the adsorption kinetics, batch experiments were conducted in a 100 mL conical flask with 0.1 g of Mt and 0.01 g of Mt-TOA and 12 mg·L−1 concentration of Pb2+ ion in the aqueous solution. This flask was shaken at 120 rpm at 298 K, and at a regular interval of time, samples were collected to analyze the amount of Pb2+ ion remaining in the aqueous phase. Pb2+ ion concentration after adsorption was measured by using atomic absorption spectrophotometer (Perking Elmer). From the mass balance, the amount of Pb2+ ion transferred to the solid phase was calculated. The quantity of lead (Pb2+) ion adsorbed per unit mass of the clay was calculated by using eq 1. qe or qt =

⎛ C0 − Ce ⎞ ⎜ ⎟ × V ⎝ w ⎠

Table 1. Equilibrium and Kinetic Models sl no.

ref.

qmKLCe

1.

Langmuir

qe =

2.

Freundlich

qe = KFCe1/ n

19

Temkin

qe = qm ln(K TCe)

20

qt = qm(1 − e−k1t )

21, 22

3.

1 + KLCe

18

Kinetic 4.

Pseudo-first order (PFO)

k 2qm2t

5.

Pseudo-second order (PSO)

qt =

6.

Intraparticle diffusion

qt = k int 0.5 + c

1 + k 2qmt

22, 23 24, 25

4. RESULTS AND DISCUSSION Batch adsorption experiments at equilibrium were performed for the removal of Pb2+ ion from the aqueous solutions by using montmorillonite (Mt) and by tri-n-octylamine (Mt-TOA) solvent modified montmorillonite (Mt-TOA). The operating parameters like adsorbent amount (w, g), pH, the initial concentration of Pb2+ ion (C0, mg·L−1), and the contact time (t, min) are the significant variables to be considered for designing an adsorber for Pb2+ ion separation from the aqueous solution. Their effect is studied on the capacity of adsorption of both the adsorbents in the current study. 4.1. Effect of Adsorbent Amount (w). To evaluate how the adsorption capacity gets affected by changing the amount of both the adsorbents (Mt and Mt-TOA) for Pb2+ ion separation, the equilibrium batch experiments were carried out with 12 mg·L−1 of initial Pb2+ ion solution at 298 K. The results are shown in Table 2. With an increase in the adsorbent amount, the adsorption

(1)

or

equation Equilibrium

Table 2. Effect of Amount of Mt and Mt-TOA on the Adsorption of Pb2+ Ion (Co = 12 mg·L−1) at 298 K

where C0 (mg·L−1) is the initial Pb2+ ion concentration, and Ce (mg·L−1) is the Pb2+ ion concentration at equilibrium. qe (mg·g−1) and qt (mg·g−1) represent the adsorption capacities of adsorbent at equilibrium, and at time, t, respectively. V is the volume of aqueous solution in L, and w is the mass of adsorbent in g. The removal efficiency of metal ion was determined by using eq 2. ⎛ C − Ce ⎞ % removal = ⎜ 0 ⎟ × 100 ⎝ C0 ⎠

model

adsorbent Mt

⎛ C0 − Ct ⎞ ⎜ ⎟ × 100 ⎝ C0 ⎠

Mt-TOA

(2)

3. MATHEMATICAL MODELS The experimental data were validated using three different isotherm (Langmuir, Freundlich, and Temkin), and three different kinetic (pseudo-first order, pseudo-second order, and intraparticle diffusion) models. An equilibrium study of an

Ce (mg·L−1)

adsorbent dosage (g)

qe (mg·g−1)

% removal

2.43 2.23 2.11 1.98 1.85 1.75 2.32 2.15 1.96 1.80 1.75 1.66

0.05 0.10 0.15 0.20 0.25 0.30 0.01 0.02 0.03 0.04 0.05 0.06

4.79 2.44 1.65 1.25 1.02 0.85 24.20 12.31 8.37 6.38 5.13 4.31

79.75 81.42 82.42 83.50 84.58 85.42 80.67 82.08 83.67 85.00 85.42 86.17

capacity of both the adsorbents for Pb2+ ion removal was found to decrease. The adsorbent capacity for Pb2+ ion removal was B



Figure 1. Equilibrium isotherms for the removal of Pb (0.1 g) and (b) Mt-TOA (0.01 g) at T = 298 K.

Article

2+

Figure 2. Kinetic model for the removal of Pb2+ by (a) Mt (0.1 g) and (b) Mt-TOA (0.01 g) at T = 298 K.

by (a) Mt

active sites are available for the adsorption of lead ions. As seen from Table 2, the highest adsorption capacity was achieved as 4.79 mg·g−1 with 0.05 g of Mt and 24.20 mg·g−1 with 0.01 g of Mt-TOA. The impregnation of TOA molecules into the clay has increased the adsorption sites in the modified version of montmorillonite (Mt-TOA) which definitely increased the metal intake capacity of the clay material. In addition to physical adsorption, there is possibility of ion-pair formation of Pb2+ molecules with TOA molecules. 4.2. Effect of Initial Pb2+ Ion Concentration (C0). The initial Pb2+ ion concentration in the aqueous solution was changed from 8 to 16 mg·L−1 to examine the effect of initial Pb2+ ion concentration on the uptake capacity of Mt and Mt-TOA. The equilibrium isotherms between the concentration of Pb2+ ions in the solid phase and aqueous phase are shown in Figure 1a and b for Mt and Mt-TOA, respectively. As seen from Figure 1, by increasing the initial concentration of Pb2+ ion from 8 mg·L−1 to 16 mg·L−1 in the aqueous solution, the intake capacity of Mt and Mt-TOA was increased from 1.79 mg·L−1 to 2.85 mg·L−1 and 17.60 mg·L−1 to 27.83 mg·L−1, respectively. The separation efficiency (a ratio of the quantity of Pb2+ ion adsorbed to the initial concentration of Pb2+ ion in the aqueous solution) was found to decrease from 89.38% to

Table 3. Effect of pH on Pb2+ Ion (Co = 12 mg·L−1) Adsorption with Mt (0.1 g) and Mt-TOA (0.01 g) at 298 K adsorbent Mt

Mt-TOA

pH

Ce (mg·L−1)

qe (mg·g−1)

% removal

1 3 5 7 9 1 3 5 7 9

12.00 11.32 3.15 1.69 2.82 12.00 11.45 3.17 1.76 2.85

0.00 0.17 2.21 2.58 2.30 0.00 1.38 22.08 25.60 22.88

0.00 5.67 73.75 85.92 76.50 0.00 4.58 73.58 85.33 76.25

decreased from 4.79 mg·g−1 to 0.85 mg·g−1 for Mt and from 24.20 mg·g−1 to 4.31 mg·g−1 for Mt-TOA. It was found that the removal of Pb2+ ion by Mt (79.75−85.42%) and Mt-TOA (80.67−86.17%) increased by increasing the amount of Mt or Mt-TOA. The fall in the value of the adsorption capacity (qe) of both adsorbents refers to the fact that there are sufficient number of C



Article

water was more because of the presence of a large number of active vacant sites available on the adsorbent surface. With the time, the repulsive force between the Pb2+ ions already adsorbed on the adsorbent surface and in the bulk aqueous phase increases which makes difficult for the Pb2+ ions to get attached to the vacant sites. The content of separation of Pb2+ ion remains almost fixed and approaches a value of 81.42% with Mt (0.1 g) after 100 min and 80.67% with Mt-TOA (0.01 g) after 80 min. With this finding, a steady-state condition was approximated, and a quasi-equilibrium situation was considered. 4.5. Comparison of Models. 4.5.1. Equilibrium Models. The equilibrium results on the adsorption of Pb2+ ions using Mt and Mt-TOA as adsorbents were fitted with the Langmuir, Freundlich, and Temkin isotherms.18−20 The values of model parameters with R2 are presented in Table 4. It is found that a good fit to the equilibrium data was provided by the Langmuir (R2 = 0.9968 for Mt and 0.9976 for Mt-TOA) isotherm model. The predicted values of adsorption capacity (qe) with these three models are plotted in Figure 1a for Mt and Figure 1b for Mt-TOA. A nondimensional term called the equilibrium 1 parameter, RL (= 1 + C K ) is defined to represent the essential

71.19% with 0.1 g of Mt and 88.00% to 69.56% with 0.01 g of Mt-TOA. This may be due to the saturation of probable exchangeable sites present on both Mt and Mt-TOA. 4.3. Effect of pH. pH of the aqueous solution is an important parameter which decides the separation efficiency of heavy metal ions by adsorption method. Generally, Pb2+ ions compete with the protons present in the aqueous solution at low pH values. The results by varying pH and its effect on the uptake capacity of adsorbent is shown in Table 3. It is observed that the separation of Pb2+ ion from the aqueous solution was almost nil at lower and at higher pH values. The highest separation of Pb2+ ions was achieved to be 85.92% with Mt and 85.33% with Mt-TOA at a pH of 7. 4.4. Effect of Contact Time (t). The effect of contact time for the separation of Pb2+ ion onto Mt and Mt-TOA is shown in Figure 2. The experiments were conducted with no pH adjustments. From Figure 2, it may be seen that at the initial stage of adsorption the rate of separation of Pb2+ ion from Table 4. Equilibrium Isotherm Model Parameters for the Adsorption of the Pb2+ Ion with Mt and Mt-TOA at 298 K adsorbent isotherm

0 L

Mt

Mt-TOA

3.37 1.19 0.9968 0.0284

33.10 1.13 0.9976 0.0026

1.88 3.43

18.08 3.37

characteristics of the Langmuir isotherm.18 The values of RL indicate the characteristics and the nature of adsorption mechanism and also predict the feasibility of the adsorption process [irreversible (RL = 0), favorable (0 < RL < 1), linear (RL = 1), and unfavorable (RL > 1)]. In the current study, the RL values were determined and obtained in the range of 0.049− 0.095 for Mt and 0.052−0.099 for Mt-TOA, showing the feasibility of Pb2+ ion adsorption on these adsorbents. The prepared montmorillonite modified with tri-n-octylamine for the separation of Pb2+ ions from aqueous solution is compared with other adsorbents in terms of the maximum uptake capacity (qm) of different adsorbents as reported in Table 5.10,11,26−41 From these data, it is obvious that the uptake capacity of the prepared Mt-TOA is comparable with most of the adsorbents studied as cited in the literature. 4.5.2. Kinetic Models. Three different kinetic models (pseudofirst order, pseudo-second order, and intraparticle diffusion) were

Langmuir qm (mg·g−1) KL (L·mg−1) R2 SD Freundlich KF [(mg·g−1) (L·g−1)1/n] n qm (mg·g−1) R2 SD

0.9775 0.0331

0.9681 0.0391

0.67 16.70 0.9795 0.0721

6.67 14.68 0.9761 0.7531

Temkin qm (mg·g−1) KT (L·mg−1) R2 SD

Table 5. Comparison of the Maximum Adsorption Capacity of Different Adsorbents for the Removal of Pb2+ adsorbent

maximum adsorption capacity, qm (mg·g−1)

ref.

Mt-TOA montmorillonite−illite Ca-montmorillonite Mn−Fe/MnO2 magnetic nanoparticles clay/poly(methoxyethyl)acrylamide 8-hydroxy quinoline-immobilized bentonite natural clay, collected from the Gabes area, southern Tunisia (Early Cretaceous) chitosan immobilized on bentonite Turkish kaolinite clay conjugate adsorbent limestone illite zirconium silicate paper sludge nanoadsorbent redox polymer zeolite−kaolin−bentonite sepiolite montmorillonite

33.10 52.00 13.65 261.10 81.02 142.94 86.40 28.00 31.75 195.31 0.0167 25.44 186.30 103.50 169.34 21.99 108.70 30.50 37.16

present study 26 27 28 29 10 11 30 31 32 33 34 35 36 37 38 39 40 41

D



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ORCID

Table 6. Kinetic Model Parameters for the Adsorption of the Pb2+ Ion with Mt and Mt-TOA at 298 K

Hasan Uslu: 0000-0002-4985-7246 Notes

adsorbent kinetic model qm (mg·g−1) k1 (min−1) R2 SD qm (mg·g−1) k2 (g·mg−1·min−1) R2 SD qm (mg·g−1) kin (g·mg−1·min−1) c R2 SD

Mt PFO 2.19 0.0422 0.9820 0.3433 PSO 3.24 9.74 × 10−3 0.9861 1.0705 Intraparticle Diffusion 2.75 0.28 −0.17 0.9141 0.2116

The authors declare no competing financial interest.

Mt-TOA

■

21.22 0.04021 0.9631 0.3801 38.91 5.2 × 10−4 0.9728 0.1017 27.87 3.67 −7.02 0.9802 1.1208

applied to describe the kinetic behavior of the adsorption process. The values of rate constants along with other parameters and linear correlation coefficient (R2) obtained from fitting are listed in Table 6. The pseudo-second order model (R2 = 0.9861 for Mt and 0.9728 for Mt-TOA) yielded a better fit to the kinetic data with both Mt and Mt-TOA. Also, the qt values are predicted by three kinetic models for both the adsorbents and are plotted in Figure 2 as lines. The trend lines showed that the rate of Pb2+ ion adsorption onto Mt-TOA is higher than Mt at any particular time which is very much important for application purpose. Therefore, the solvent (TOA) modified form of montmorillonite clay could be a suitable choice for the separation of Pb2+ ion from the wastewater streams in the industrial effluents.

5. CONCLUSIONS Montmorillonite, a natural clay material, and its modified version were used for the removal of Pb2+ ion from industrial wastewater. The montmorillonite which was chemically modified by trin-octylamine showed good efficiency for removing the Pb2+ ion from aqueous solutions by adsorption. A better removal of Pb2+ was found with 12 g·L−1 and 2.4 g·L−1 of Mt and Mt-TOA, respectively. A pH value of 7 will provide better conditions for effective Pb2+ ion removal. The data of equilibrium adsorption were evaluated by using three isotherm models, and the data fit well to the Langmuir isotherm model. The highest uptake capacities for the separation of Pb2+ ion from water phase were found (estimated by the Langmuir model) to be 3.37 mg·g−1 and 33.10 mg·g−1 with Mt and Mt-TOA, respectively. Three kinetic models were used to explain the kinetic behavior of the adsorption. Among them, the pseudo-second order model was able to explain the rates of the adsorption process. The proposed modified form of montmorillonite clay with tri-n-octylamine could be successfully applied for the adsorption of heavy metals like lead from the effluents of industrial wastewater streams.

■

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Adsorptive Separation of Lead (Pb2+) from Aqueous Solution Using

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