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1 Chapter IV Studies on the adsorption of metal ions and dyes The presence of heavy metals/dyes in the aquatic environment can be detrimental to a variety of living species. Therefore, elimination of heavy metals/dyes from water and waste water is important to protect public health. The adsorption phenomenon under-welldesigned conditions have a definite edge over other methods used for the separation and recovery of heavy metal ions/dyes. In view of the potential pollution hazard caused by heavy metals/dyes, adsorption onto low cost adsorbents, which is characterized by simplicity, selectively and efficiency, is a feasible technique of extensive interest. The present investigation deals with the development of chemically modified low cost adsorbents, its characterization and its potential for removal of heavy metal ions/dyes from aqueous solutions. This chapter reports the results and discussions of the investigations on the equilibrium, kinetic and thermodynamic aspects on the adsorption of Fe(II), Cu(II) ions and malachite green, Rhodamine B onto BBC, MCC and PDC low cost activated carbons. 65

2 4.1 Adsorption of ferrous ion by BBC Effect of carbon mass: The amount of ferrous ion adsorption increased with the increase in carbon dose and reached a maximum value after a particular dose (Figure.4.1). Taken an initial metal ion concentration of 20 mg/l, complete ferrous ion removal was obtained at a maximum carbon dose of 100 mg. The increase in the adsorption of ferrous ion with carbon dose was due to the introduction of more binding sites for adsorption and the availability more surface area 23,70, Effect of agitation time and initial Ferrous ion concentration: The equilibrium data were collected in Table 4.1 reveals that, percent adsorption decreased with increase in initial ferrous ion concentration, but the actual amount of metal ion adsorbed per unit mass of carbon increased with increase in metal ion concentration. It means that the adsorption is highly dependent on initial concentration of ferrous ion. It is because of that at lower concentration, the ratio of the initial number of metal ions to the available surface area is low subsequently the fractional adsorption becomes independent of initial concentration. However, at high concentration the available sites of adsorption becomes fewer and hence the percentage removal of ferrous ion is dependent upon initial concentration. Equilibrium have established at 20 minutes for all concentrations. Figure 4.2 reveals that the curves are single, smooth, and continuous, leading to saturation, suggesting the possible monolayer coverage of the ferrous ion on the carbon Adsorption isotherms. The experimental data are analyzed according to the linear from of the Langumuir 141 and Freundlich 142 isotherms (Eqn.3.1 and 3.2). A plot of Ce/Qe versus Ce at different initial temperatures for all the metal ions is linear and a representative plot is given in Figure 4.3. Linearity of the plots suggests the applicability of the Langmuir isotherm. The statistical parameters along with Langmuir constants are collected in table 66

3 4.2. From the results, it is clear that the value of adsorption efficiency Qm and adsorption energy b increases on increasing the temperature. This is because of the fact that the maximum adsorption corresponds to a saturated monolayer of adsorbate molecules on adsorbent surface 22,24. Further, such a variation confirms the endothermic nature of the adsorption processes involved in the system 41. The favorability of the adsorption process is confirmed by the separation factor, RL. The calculated values of the separation factor are presented in table 4.3. The values are found to be between 0 and 1 confirming that the ongoing adsorption process is favorable 41,54,77. The Freundlich equation is also employed for the adsorption of ferrous ions onto BBC The plot of log Qe versus log Ce is linear for the metal ion at all the temperatures investigated showing that the adsorption of metal ion follows the Freundlich isotherm. A plot is shown in Figure 4.4. The computed values of Freundlich constants K and n given in Table 4.4, indicate that the adsorption is favorable under the experimental conditions. This may be due to the fact that, the increase of negative charge on the surface that enhances the electrostatic force like van der Waal s forces between the carbon surface and metal ion which makes the adsorption fesaible 40. The intensity of adsorption is indicative of the bond energies between metal ion and adsorbent. Hence, in the present study the adsorption of ferrous ion onto BBC may be through physisorption 44,48. Further, the values of n are greater than one which indicates the adsorption as favorable 49,59, Kinetics of adsorption. The solute uptake rate, which governs the residence time of sorption reaction, is described by kinetic studies. In the present study, the kinetics of the metal ion removal is studied using Natarajan and Khalaf equation. The plots of log Co/Ct versus t for different concentrations and temperatures are linear and the linearity of these plots indicates that the adsorption of metal ions from aqueous solution follows reversible first order kinetics. From the slope of these plots the rate constant for adsorption, k ad, and 67

4 that for the forward (k 1 ) and reverse (k 2 ) processes of the equilibrium are calculated using Eqn. 3.5 and are collected in Table 4.5. It is evident from the results that the forward rate constant is much higher than the backward rate constant suggesting that the rate of adsorption is clearly dominant 62,80. The overall rate constant for the adsorption, k ad increases with increase in temperature indicating the endothermic nature of the adsorption process. Further, the k ad values decrease with increase in initial concentration of the ferrous ion. This is due to the fact that in cases of strict surface adsorption a variation of rate should be proportional to the first power of concentration. However, when pore diffusion limits the adsorption process, the relationship between initial metal ion concentration and rate of reaction will not be liner. It shows that pore diffusion limits the over all rate of ferrous ion adsorption 33,44, Intra particle diffusion studies. The possibility of the existence of intra-particle diffusion is tested by plotting a graph between the amount of ferrous ions adsorbed and square root of time. The rate constant for intra-particle diffusion, K p, for the metal ions is determined from slopes of linear portion of above plots using Eqn.3.6 the values of K p ( mg g -1 min -0.5 ) are shown in the table 4.6. It is interesting to note that the percentages of uptakes of ferrous ion are also observed to be in the same order. Thus, the intra-particle diffusion is the rate determining step in the adsorption process under investigation. Further, the linear portions of the curves do not pass the origin which indicates that the mechanism of metal ion adsorption onto BBC may be a complex process in which both the surface adsorption and intra-particle diffusion contributes the rate-determining step 69, Effect of temperature. The equilibrium constant, K o for the adsorption of malachite green at four different temperatures were computed by the method described in literature 56,135,147. The values are given in Table 4.7 from the temperatures dependence of 68

5 the equilibrium constant, The adsorption capacity of the carbon increased with increase of the temperature in the system from 30 to 60 C. Thermodynamic parameters such as change in free energy ( G ) (kj/mol), enthalpy ( H )(kj/mol) and entropy ( S )(J/K/mol) were determined using the following equations 3.7 to The H and S values obtained from the slope and intercept of Van t Hoff plots have been presented in Table 4.7. The values H in the range of 1 to 93 KJ/mol indicates the physisorption. From the results we could make out that physisorption is much more favorable for the adsorption of malachite green. The positive values of H show the endothermic nature of adsorption which governs the possibility of physical adsorption 147. Because in the case of physical adsorption, while increasing the temperature of the system, the extent of dye adsorption increases, this rules out the possibility of chemisorption 139,152. The low H value depicts dye is physisorbed onto adsorbent BBC. The negative values of G (Table 4.7) show that the adsorption is highly favorable and spontaneous. The positive values of S (Table 4.7) show the increased disorder and randomness at the solid solution interface of malachite green with BBC adsorbent. The enhancement of adsorption capacity of the activated carbon at higher temperatures was attributed to the enlargement of pore size and activation of the adsorbent surface 146, Effect of ph. The experiments carried out at different initial ph show that the adsorption percentage increase with increase in initial ph of the medium in the range studied i.e. 3 to 9 as depicted in the figure 4.5. this behavior can be explained using ph zpc of the adsorbent. In the present study the ph zpc of BBC is At any ph below ph zpc, the surface of adsorbent is positively charged and at ph above ph zpc the surface is negative 20,32. When the solution ph exceeded ph zpc the metal species are more easily attracted by the negatively charged surface of adsorbent, favoring accumulation of metal species on the surface and thus promoting adsorption 35,43. In addition the increase is partially attributed to 69

6 the formation of different hydroxo species with rise in solution ph 51,58. The decrease in adsorption of metal ions at low and high ph can be attributed to the competition between H + and OH - with ferrous ions. It is thus clear from figure 4.6 that at lower ph, the adsorption of metal ions studied is drastically reduced. This observation was made use of to desorb the metal ions from the adsorbed material 20, Effect of co-ions. The effect of added chloride and calcium ions, taken in the form of NaCl and CaSO 4, on the adsorption of ferrous ions onto BBC is shown in figure 4.6. It is observed that the adsorption of ferrous ions from aqueous solution decreased with increase in concentration of chloride and calcium ions. This may be due to the fact that, at high ionic strength, the increased amount of NaCl and CaSO 4 can swamp the surface of the carbon, which decreases the metal ions access to the carbon surface for adsorption. The cation competition and modification of metal ion speciation are less important factors since NaCl and CaSO 4 is used as the source of chloride and calcium ions ions 20,30. The observed interference is due to increasing ionic radii, that is their decreasing hydrated ionic radii. The smaller the hydrated ionic radius, the greater is the efficiency of an ion to bind to the active sites of the adsorbent. This suggests that the energy required in the dehydration of the metal ions, in order that they could occupy a site in the adsorbent, plays an important role in determining the selectivity 52, Analytical evidenced for adsorption. The FT-IR spectra of the raw BBC and ferrous ion loaded BBC is recorded with an aim to understand the nature of adsorption. A representative spectrum is shown in Figure 4.7 a and b.it is evident from the spectra that the positions of the peaks remain unaltered after adsorption of metal ion indicating that the chemical nature of the adsorbent remains unaffected. Thus, the adsorption of metal ions on the adsorbent is by physical forces but not by chemical forces which might alter the chemical nature of the adsorbent and consequently the position of the peaks 40,134 70

7 A representative X-ray diffraction (XRD) pattern of BBC before and after adsorption of Fe(II) ins is shown in Fig.4.8 a and b. In Fig.4.8 a, the intense peaks show the presence of highly organized crystalline structure of raw activated carbon, after the adsorption of metal ions, the intensity of the highly organized peaks were slightly diminished (Fig.4.8 b).however, there is no change in the 2 theta values. This has been attributed to the adsorption of metal ion on the upper layer of the crystalline structure of the carbon surface by means of physisorption 134, Desorption studies. The effect of various reagents used for desorption of the spent BBC is shown in Figure 4.9. All the reagents employed are of 0.2 M. The results indicate that hydrochloric acid is a better reagent for desorption because it could remove more than 90% of adsorbed ferrous ion. The reversibility of adsorbed metal ion in mineral acid is in agreement with the ph dependent results obtained. Desorption of the ferrous ions by mineral acids indicates that the metal ions were adsorbed on to the activated carbon through physisorption mechanism 24,38,52. 71

8 Table 4.1 Equilibrium parameters for the adsorption of ferrous ion on to acid activated Carbon (Temperature 0 C) Ferrous ion (mg/l) C e (mg /l) Q e (mg/g) Ferrous ion Removed (%)

9 Table 4.2 Langmuir isotherm results (Ferrous ion) Temp Statistical parameters/constants ( C) r 2 Q m b Ferrous ion adsorption

10 Table 4.3 Dimensionless separation factor (R L ) Ferrous ion (mg/l) Temperature ( C)

11 Table 4.4 Freundlich isotherm results (metal ion) Temp Statistical parameters/constants ( C) K r 2 f n Ferrous ion adsorption

12 Table 4.5 Rate constants for the adsorption of ferrous ion (10 3 k ad, min -1 ) and the constants for forward (10 3 K 1, min -1 ) and reverse (10 3 K 2, min -1 ) process Temperature ( C) Ferrous ion (mg/l) K ad k 1 k 2 k 1 k 2 k 1 k 2 k 1 k

13 Table 4.6 Intraparticle diffusion (K p ) Ferrous ion (mg/l) Temperature (30 C) r 2 K p

14 Table 4.7 Equilibrium constant and thermodynamic parameters for the adsorption of ferrous ion onto acid activated carbon K o G [Ferrous on] (mg/l) 30 C 40 C 50 C 60 C 30 C 40 C 50 C 60 C H S

15 percentage removal of metal ion Adsorbent dose in mg Fig.4.1 Effect of dosage on the removal of metal ion with initial concentration 20 mg/l 79

16 percentage removal of metal ion Contact time in min Fig.4.2 Effect of contact time with the initial concentration of 20 mg/l of Ferrous ion 80

17 C e /Q e C 40 0 C 50 0 C 60 0 C C e Fig.4.3 Langmuir isotherm for the adsorption of Ferrous ion onto carbon 81

18 logqe C 40 0 C 50 0 C 60 0 C logce Fig.4.4 Freundlich isotherm for the adsorption of Ferrous ion 82

19 percentage removal of metal ion ph Fig.4.5 Effect of ph on the removal of metal ion 83

20 percentage removal of metal ion Ca 2+ Cl Concentration of other ions (mg/l) Fig.4.6.Effect other ions on the removal of metal ion with with initial concentration of 20 mg/l 84

21 Fig.4.7a. FT-IR Spectrum of BBC before adsorption Fig 4.7b FT-IR Spectrum of BBC after adsorption of ferrous ion 85

22 percentage removal of metal ion Reagents Fig.4.9 Regeneration pattern (1.Hydrochloric acid, 2.Sulphuric acid, 3.Nitric acid,4.sodium chloride, 5.Sodium chloride+water) 86

23 4.2 Adsorption studies of copper ion by BBC Effect of carbon concentration: The adsorption of the metal ion on carbon was studied by varying the carbon concentration (10-100mg/50ml) for Copper ion concentration of 20mg/L. The percentage of adsorption increased with increase in the carbon concentration (Figure 4.10). This has attributed to increased carbon surface area and availability of more adsorption sites 23, Effect of contact time and initial copper ion concentration: The experimental results of adsorptions of Copper ion on the activated carbon at various concentrations (5, 10, 15, 20, 25 and 30mg/L) with contact time are shown in Figure The equilibrium data were collected in Table 4.8 reveals that, percent adsorption decreased with increase in initial metal ion concentration, but the actual amount of metal ion adsorbed per unit mass of carbon increased with increase in metal ion concentration. It means that the adsorption is highly dependent on initial concentration of metal ion. It is because of that at lower concentration, the ratio of the initial number of metal ion to the available surface area is low subsequently the fractional adsorption becomes independent of initial concentration 21,70,154. However, at high concentration the available sites of adsorption becomes fewer and hence the percentage removal of metal ion is dependent upon initial concentration. Equilibrium have established at 40 minutes for all concentrations. Figure 4.11 reveals that the curves are single, smooth, and continuous, leading to saturation, suggesting the possible monolayer coverage of the copper ion on the carbon surface 21,70, Adsorption isotherm: The experimental data analyzed according to the linear form of the Langmuir 141 and Freundlich 142 isotherms (Eqn 2.1 and 2.2). The linear plots of C e/ Q e 87

24 versus C e suggest the applicability of the Langmuir isotherms (Figure 4.12). Langmuir constants related to adsorption efficiency and energy of adsorption, respectively. Values of Q m and b were determined from slope and intercepts of the plots and are presented in Table 4.9. From the results, it is clear that the value of adsorption efficiency Q m and adsorption energy b of the carbon increases on increasing the temperature. From the values we can conclude that the maximum adsorption corresponds to a saturated monolayer of adsorbate molecules on adsorbent surface with constant energy and no transmission of adsorbate in the plane of the adsorbent surface 22,24. The trend shows that the adsorbent prefers to bind acidic ions and that speciation predominates on sorbent characteristics, when ion exchange is the predominant mechanism. Further, it confirms the endothermic nature of the processes involved in the system. To confirm the adorability of the adsorption process, the separation factor (R L ) has calculated and presented in Table The values were found to be between 0 and 1 and confirm that the ongoing adsorption process is favourable 41,54,156 The Freundlich equation have also employed for the adsorption of Copper ion on the adsorbent. Linear plot of log Q e versus log C e shows that the adsorption of Copper ion follows the Freundlich isotherm (Figure 4.13). The K f and n are constants incorporating all factors affecting the adsorption capacity and intensity of adsorption, respectively. Values of K f and n were found and given in the Table 4.11 shows the increase of negative charge on the surface that enhances the electrostatic force like vanderwaal s between the carbon surface and metal ion, which increases the adsorption of Copper ion. The values clearly show that dominance in adsorption capacity. The intensity of adsorption is an indicative of the bond energies between metal ion and adsorbent and the possibility of slight chemisorptions rather than physisorption. The possibility of multilayer adsorption of metal ion through the 88

25 percolation process cannot be ruled out. However, the values of n is greater than one indicating the adsorption is much more favourable 41, Kinetics of adsorption. The overall rate constant, K for the adsorption of metal ions at different temperatures are calculated from the slopes of the linear Natarajan-Khalaf plots. The rate constant (k) increases with increase in temperature suggesting that the adsorption process is endothermic in nature. Further, k values decrease with increase in initial concentration of the metal ion. In cases of strict surface adsorption a variation of rate should be proportional to the first power of concentration. However, when pore diffusion limits the adsorption process, the relationship between initial metal ion concentration and rate of reaction will not be linear. Thus, in the present study pore diffusion limits the overall rate of metal ion adsorption. The over all rate of adsorption is separated into the rate of forward and reverse reactions using Eqn.2.5. The rate constants for the forward and reverse processes are also collected in Table The results indicate that, at all initial concentrations and temperatures, the forward rate constant is much higher than the reverse rate constant suggesting that the rate of adsorption is clearly dominant 133,157, Intra particle diffusion studies. In adsorption studies, it is necessary to determine the rate-determining step. Therefore, the results obtained from the equilibrium experiments were used to study rate-limiting step. Since the particles were vigorously agitated during the experiment, it is reasonable to assume that the mass transfer from the bulk liquid to the particle external surface did not limit the rate. One might then postulate that the rate limiting step might be film or intra particle diffusion 47,69,80. 89

26 Hence, in this study, the possibility of existence of intra-particle diffusion is tested by plotting a graph between the amount of metal ion adsorbed and square root of time.the double nature of these plots may be explained as: the initial curve portions are attributed to boundary layer diffusion effect and flat portion indicates the intra-particle diffusion effect The rate constant for intra-particle diffusion, Kp, for the metal ion are determined from the slopes of the linear portions of these curves. The values of Kp(mg g -1 min -0.5 ) are shown in table Indicates the percentage uptake of the metal ions is in increasing order. Thus the intra-particle diffusion limits the rate of adsorption process. Further, the linear portions of the curves do not pass the origin. This indicates that mechanism of metal ion removal by the adsorbent is complex and both surface adsorption and intra-particle diffusion may contribute to the rate-determining step 139, Effect of temperature. At equilibrium, the rate is the ratio of the concentration of adsorbate in adsorbent and in aqueous solution is given by equilibrium of adsorbate in adsorbent and in aqueous solution is given by equilibrium constant, K 25,37,146. The values of K are calculated from the equilibrium concentrations and are presented in Table The results indicate that K value increase with increase in temperature indicating the endothermic nature of the adsorption process. From the dependence of K with temperature the thermodynamic parameters such as change in free energy ( G ), enthalpy ( H ) and entropy ( S ) are determined by employing vant t Hoff equation (Eqn.3.7 and 3.11) 37,61,147. For the metal ions at different initial concentrations the van t Hoff plots are found to be linear (r>0.99). The thermodynamic parameters for the uptake of copper ions by BBC are collected in Table The positive values of H indicate the endothermic nature of the adsorption. 90

27 Further, the low values of enthalpy change suggest that the adsorption is governed mainly by physical forces i.e. the copper ions are physisorbed on the adsorbent surface 139. Hence, the increase in percentage of adsorption with increase in temperature may be due to enlargement of the pore size at higher temperature. As the rate of the adsorption process depends on the intra-particle diffusion, increase in pore size would lead to increased uptake of the copper ions Effect of ph: The experiments carried out at different ph shows that there was a change in the percent removal of metal ion over the entire ph range of 3 to 9 shown in the Figure 4.14, This indicates the strong force of interaction between the metal ion and the activated carbon that, either H + or OH - ions could influence the adsorption capacity. Here the interaction is more at ph 6, the competence of acidic H+ ion with metal cation for the sorption sites. The percentage of sorption increased at the above ph value is due to the presence of ionic COOH groups. The adsorption of metal ion on the activated carbon does involve ion exchange mechanism. Due to the adsorption of metal ion through ion exchange mechanism by the adsorbent, there should be an influence on the metal ion adsorption while varying the ph. This observation is in line with the type I isotherm shown in Figure 4.12 and The positive H value obtained, which indicates irreversible adsorption probably due to polar interaction 35,43,51, Effect of co-ions. The effect of other ions like Ca 2+ and Cl - on the adsorption process studied at different concentrations. The ions added to 20mg/L of metal ion solutions and the contents were agitated for 60 min at 30 C. The results had shown in the Figure 4.15 reveals that low concentration of Cl - does not affect the percentage of adsorption of metal ion on activated carbon, because the interaction of Cl- at available sites of adsorbent through 91

28 competitive adsorption is not so effective. While the concentration of other ion Ca 2+ increases, the interference of these ions at available surface sites of the sorbent through competitive adsorption increases that, decreases the percentage adsorption. The interference was more in the presence of Ca 2+ compared with Cl - ion. This is so because ions with smaller hydrated radii decrease the swelling pressure with in the sorbent and increase the affinity of the sorbent for such ions 20,36, Spectral evidences for adsorption. The FT-IR spectra of the raw BBC and copper ion loaded BBC is recorded with an aim to understand the nature of adsorption. Representative FT-IR spectra are shown in Fig. 4.16a and b. It could be seen that the position of the peaks remains unaltered after adsorption of metal ion indicates that the adsorbent remains unaffected. Thus, the adsorption of metal ions on the adsorbent is by physical forces but not by chemical combination 134. The representative XRD patterns of BBC before and after adsorption of Cu(II) ions are shown in Fig 4.17a and b. The intense peaks show the presence of highly organized crystalline structure or raw achieved carbon, after the adsorption of metal ions, the intensity of the highly organized peak s were slightly diminished. However, there is no change in the 2 theta values. This has been attributed to the adsorption of metal ion on the upper layer of the crystalline structure of the carbon surface by means of bhysisorption1 34, Desorption studies. This study helps to elucidate the nature of adsorption and recycling of the spent adsorbent and the metal ion. The effect of various reagents used for desorption studies are shown in Figure The results indicate that hydrochloric acid is a better reagent for desorption, because we could get more than 90% removal of adsorbed metal 92

29 ion. The reversibility of adsorbed metal ion in mineral acid or base is in agreement with the ph dependent results obtained. The desorption of metal ion by mineral acids and alkaline medium indicates that the metal ion was adsorbed onto the activated carbon through by physisorption mechanisms 38,53,85. 93

30 Table 4.8 Equilibrium parameters for the adsorption of copper ion onto BBC activated Carbon [M] 0 C e (mg/l) Q e (mg/g) Metal ion removed (%) Temperature (C) 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o

31 Table 4.9 Langmuir isotherm results Metal ion Temp Statistical parameters/constants 0 C r 2 Q m B Copper ion Table 4.10 Dimensionless Separation factor (R L ) Temperature ( 0 C) [M] (mg/l)

32 Table 4.11 Freundlich isotherm results Metal ion Temp Statistical parameters/constants 0 C r 2 K f N Copper ion

33 Table 4.12 Rate constants for the adsorption of copper ion (10 3 k ad, min -1 ) and the constants for forward (10 3 k 1, min -1 )and reverse (10 3 k 2, min -1 ) process Temperature ( 0 C) k ad [Cu] o 40 o 50 o 60 o k 1 k 2 k 1 k 2 k 1 k 2 k 1 k

34 Table 4.13 Intraparticle diffusion (K p ) (Copper ion) (mg/l) r 2 K p

35 Table 4.14 Equilibrium constant and thermodynamic parameters for the adsorption of copper ion onto BBC carbon [Cu] 0 K 0 G o H o S o Temperature ( 0 C) 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o

36 percentage removal of metal ion carbon dosage in mg Figure 4.10 Effect of carbon dosage on the removal of metal ion with the concentration of 20 mg/l 95

37 percentage removal of metal ion contact time in min Figure 4.11 Effect contact time on the removal of copper ion with the initial concentration of 20 mg/l 95

38 C e /Q e C 40 0 C 50 0 C 60 0 C C e Figure 4.12.Langmuir isotherm for the adsorption of copper ion 95

39 logq e C 40 0 C 50 0 C 60 0 C logc e Figure 4.13 Freundlich isotherm for the adsorption of copper ion 95

40 percentage removal of metal ion ph Figure 4.14 Effect of ph on the removal of copper ion with the initial concentration of 20 mg/l 95

41 percentage removal of metal ion concentration of other ions in mg/l Cl - Ca 2+ Figure 4.15 Effect of chloride and calcium ion on the removal of copper with the initial concentration of 20mg/L 95

42 Fig 4.16a FT-IR Spectrum of BBC before adsorption Fig.4.16b. FT-IR Spectrum of BBC after adsorption of copper ion 95

43 Counts outside work2_ Position [ 2Theta] Fig 4.17b, XRD pattern of BBC after adsorption of copper ion 95

44 Percentage removal of metal ion HCl 2.HNO 3 3.H 2 SO 4 4.NaCl 5.NaCl + H 2 O Reagents Figure 4.18 Regeneration pattern 95

45 4.3 Adsorption studies of Malachite green by BBC Effect of carbon dose: The adsorption of the malachite green dye on carbon was studied by varying the carbon dose ( mg/50ml) for 40 mg/l of dye concentration. The percentage of adsorption increased with increase in the carbon concentration (Figure 4.19). This was attributed to increased carbon surface area and availability of more adsorption sites 139,151. Hence the entire studies were carried out with 100 mg of adsorbent /50 ml of the varying adsorbate solutions Effect of agitation time and initial concentration: The experimental results of adsorptions at various concentrations (10, 20,30,40,50 and 60 mg/l) was collected in Table 4.15 reveals that, percent adsorption decreased with increase in initial dye concentration, but the actual amount of dye adsorbed per unit mass of carbon increased with increase in dye concentration. It means that the adsorption is highly dependent on initial concentration of dye. At lower concentration, the ratio of the initial number of dye molecules to the available surface area is low subsequently the fractional adsorption becomes independent of initial concentration. However, at high concentration the available sites of adsorption becomes fewer and hence the percentage removal of dye is dependent upon initial concentration Equilibriums have been established at 40 minutes for all concentrations. Figure 4.20 reveals that the curves are single, smooth, and continuous, leading to saturation, suggesting the possible monolayer coverage of the dyes on the carbon surface Adsorption isotherms: The experimental data s are analyzed by the linear form of the Langmuir and Freundlich isotherms 141,142.. The linear plots of C e/ Q e versus C e suggest the applicability of the Langmuir isotherms (Figure 4.21). The values of Q m and b were determined from slope and intercepts of the plots and are presented in Table The Q m 95

46 and b is Langmuir constants related to adsorption efficiency and energy of adsorption, respectively From the results, it is clear that the value of adsorption efficiency Q m and adsorption energy b of the carbon decreases on increasing the temperature suggests that the maximum adsorption corresponds to a saturated monolayer of adsorbate molecules on adsorbent surface and endothermic nature of adsorption 145,147,154. The favorability of the adsorption process was calculated from dimensionless separation factor (R L ) which was found between 0 and 1 confirms the ongoing adsorption of malachite green 147,154. The values were shown in Table The Freundlich equation was employed for the adsorption of Malachite green dye on the adsorbent. Linear plots of log Q e versus log C e shows that the adsorption of malachite green dye obeys the Freundlich adsorption isotherm (Figure 4.22). The K f and n are constants incorporating the factors affecting the adsorption capacity and intensity of adsorption, respectively The values of K f and n given in the Table 4.18 show that the increase of negative charges on the adsorbent surface makes electrostatic force like Vanderwaal s between the carbon surface and dye ion. The molecular weight and size either limit or increase the possibility of the adsorption of the dye onto adsorbent. However, the values clearly show the dominance in adsorption capacity. The intensity of adsorption is an indication of the bond energies between dye and adsorbent and the possibility of slight chemisorptions rather than physisorption 139,160. However, the multilayer adsorption of malachite green through the percolation process may be possible. The values of n are less than one indicating the physisorption is much more favorable 139, Kinetic of adsorption. In the present study, the kinetics of malachite green removal has been carried out understands the behavior of the adsorbent employed. The Natarajan and Khalaf kinetic plots for different concentrations and temperature are found to be 95

47 linear, with correlation coefficients of more than 0.98, indicating the applicability of firstorder reversible kinetics. The values of rate constant of adsorption, k ad are found to increase with increase in the temperature indicating the endothermic nature of the adsorption process. The k ad values decrease with increase in the initial concentration of malachite green. An examination of the effect of malachite green concentrations on the k ad helps to decrease the mechanism of removal which takes place. In cases of strict surface adsorption, a variation of rate should be proportional to the first power of concentration. However, when pore diffusion limits the adsorption process, the relationships between initial solute concentration and the rate of reaction will not be linear. Hence, it seems likely that pore diffusion limits the overall rate of malachite green adsorption 44, 46,145. The forward (k 1 ) and backward (k 2 ) rate constants were calculated (Eqn.2.5) and are summarized in table It is evident from the results, that the forward rate constant is much higher than the backward rate constant suggesting that the rate of adsorption is clearly dominant 139, Intra-particle diffusion studies. The intra-particle diffusion is the most commonly used technique for identifying the adsorption mechanism. Previous studies by various researchers shows that the plot of Qt versus t 0.5 represents multi linearity, which characterizes the two or more steps involved in the sorption process. According to Weber and Morris, an intraparticle diffusion coefficient K p is defined by the equation 2.6. The K p (mg/g min 0.5 ) values of malachite green adsorption is obtained from the slope of the plot of Qt(mg/g) versus t 0.5. The two phases in the intraparticle diffusion plot (Figure 4.23) suggest that the sorption process was succeeded by surface sorption and intraparticle diffusion. The initial curved portion of the plot indicates the boundary layer effect while the second linear portion is due to intraparticle diffusion. The slope of the second linear portion of the plot gives intraparticle diffusion parameter K p (mg/g min 0.5 ). On the other 95

48 hand, the intercept of the plot reflects the boundary layer effect. The larger the intercept, the greater is the contribution of the surface sorption in the rate limiting step. The calculated intraparticle diffusion coefficient K p values are 0.146, 0.146, 0.147, and 0.149mg/g min 0.5 for initial dye concentrations of 10, 20, 30, 40, 50 and 60 mg/l at 30 0 C. This indicates that mechanism of malachite green removal on the adsorbent is complex and both the surface adsorption and intra-particle diffusion may contribute to the ratedetermining step 80, , Thermodynamic parameters. The adsorption capacity of the carbon increased with increase of the temperature in the system from 30 to 60 C. Thermodynamic parameters such as change in free energy ( G ) (kj/mol), enthalpy ( H )(kj/mol) and entropy ( S )(J/K/mol) were determined using the equations 3.7 to The H and S values obtained from the slope and intercept of Van t Hoff plots have been presented in Table The values H in the range of 1 to 93 KJ/mol indicates the physisorption. From the results we could make out that physisorption is much more favorable for the adsorption of malachite green. The positive values of H show the endothermic nature of adsorption which governs the possibility of physical adsorption 147. Because in the case of physical adsorption, while increasing the temperature of the system, the extent of dye adsorption increases, this rules out the possibility of chemisorption 139,152. The low H value depicts dye is physisorbed onto adsorbent BBC. The negative values of G (Table 6) show that the adsorption is highly favorable and spontaneous. The positive values of S (Table 4.20) show the increased disorder and randomness at the solid solution interface of malachite green with BBC adsorbent. The enhancement of adsorption capacity of the activated carbon at higher temperatures was attributed to the enlargement of pore size and activation of the adsorbent surface 146,

49 4.3.7 Effect of ph.. The ph is one of the most important parameter in controlling the adsorption process. The ph of the solution was controlled by the addition of HCl or NaOH. The effect of ph on the adsorption of malachite green ions on BBC was shown in Figure The uptake of malachite green ions at ph 7.5 was minimum and maximum at ph However, when the ph of the solution was increased (more than ph 7), the uptake of malachite green ions was increased. It appears that a change in ph of the solution results in the formation of different ionic species, and different carbon surface charge. When the ph value is lower than 6, the malachite green ions are able to enter into the pore structure. As the ph value is increased to above 7, the zwitter ions form of malachite green in water may raise the aggregation of malachite green to form a bigger molecular form (dimer) and become unable to enter into the pore structure of the carbon surface. The greater aggregation of the zwitter ionic form is due to the attractive electrostatic interaction between the ionic groups of the monomer. At ph value higher than 9, the exisistance of BBC surface OH - creates a competition between ionic dye and decrease the aggregation of malachite green, it also causes an increase in the adsorption of malachite green ions on the carbon surface. The effect of the charge on the carbon surface and the electrostatic force of attraction and repulsion between the carbon surface and the malachite green ions cannot explain the outcome 20,32,43,51, Effect of co-ions. The effect of sodium chloride on the adsorption of malachite green on BBC is shown in Fig The low concentrate NaCl solution had little influence on the adsorption capacity. When the concentration of NaCl increases the ionic strength is raised. At higher ionic strength the adsorption of malachite green will be high owing to the partial neutralization of the positive charge on the carbon surface and a consequent compression of the electrical double layer by the Cl - anion. The chloride ion can also enhances adsorption of malachite green ion by pairing of their charges and hence reducing 95

50 the repulsion between the malachite green molecules adsorbed on the surface. This initiates carbon to adsorb more positive malachite green ions 36,62, FT-IR spectra and XRD studies. The representative FT-IR spectra of BBC before and after adsorption are shows in Fig 4.26a and b. It is evident from the figure that there is no appreciable change in the spectra of the adsorbent after adsorption. This may be due to the fact that the adsorption doesn t alter the chemical nature of the surface of the adsorbent i.e. the adsorption forces in the present case is of physical in nature 53,60,134. The XRD images of the adsorbent before and after adsorption are given in Fig 4.27a and b which supports the adsorption process Regeneration studies Regeneration studies help to elucidate the nature of adsorption and recycling of the spent adsorbent The effect of various reagents used for desorption studies indicate that hydrochloric acid is a better reagent for desorption, sine it desorp 79% of the adsorbed malachite green. The desorption of malachite green dye by dilute mineral acid indicates that the dyes were adsorbed onto the activated carbon through physisorption.n 38-39,52-53,

51 Table 4.15 Equilibrium parameters for the adsorption of malachite green onto activated Carbon [MG] 0 C e (mg/l) Q e (mg/g) Dye removed (%) Temperature (C) 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o

52 Table 4.16 Langmuir isotherm results Dye Temp Statistical parameters/constants 0 C r 2 Q m b MG Table 4.17 Dimensionless Separation factor (R L ) Temperature ( 0 C) [MG] (mg/l)

53 Table 4.18 Freundlich isotherm results Dye Temp Statistical parameters/constants 0 C r 2 K f n MG

54 Table 4.19 Rate constants for the adsorption of malachite green dye (10 3 k ad, min -1 ) and the constants for forward (10 3 k 1, min 1 ) and reverse (10 3 k 2, min -1 ) process Temperature ( 0 C) [D] 0 k ad o 40 o 50 o 60 o k 1 k 2 k 1 k 2 k 1 k 2 k 1 k

55 Table 4.20 Equilibrium constant and thermodynamic parameters for the adsorption of malachite green onto carbon [MG] 0 K 0 Temperature ( 0 C) G o H o S o 30 o 40 o 50 o 60 o 30 o 40 o 50 o 60 o

56 % removal of MG Adsorbent dose in mg Fig.4.19 Effect of adsorbent dose on the adsorption of malachite green onto BBC [MG]=40 mg/l;ph=6.5;contact time=60 min 95

57 % removal of MG Contact time in min Fig.4.20 Effect of contact time on the adsorption of malachite green onto BBC [MG]=40 mg/l;ph=6.5;dose=100 mg/50 ml 105

58 Ce/Qe C 40 0 C 50 0 C 60 0 C Ce Fig.4.21 Langmuir adsorption isotherm for the adsorption of MG onto BBC 106

59 logqe C 40 0 C 50 0 C 60 0 C logce Fig.4.22 Freundlich adsorption isotherm for the adsorption of malachite green onto BBC 107

60 Qt time 0.5 in min Fig.4.23 Intraparticle diffusion effect on the adsorption of malachite green onto BBC [MG]=10 mg/l;ph=6.5;dose=100 mg/50 ml 108

61 % removal of MG Initial ph Fig.4.24 Effect of initial ph on the removal of malachite green by BBC [MG]=40 mg/l;dose=100 mg/50 ml;contact time=60 min 109

62 % removal of MG Concentration of chloride ion in mg/l Fig.4.25.Effect of ionic strength on the adsorption of malachite green onto BBC [MG]=40 mg/l;dose=100 mg/50 ml;contact time=60 min 110

63 Fig.4.26a. FT-IR Spectrum of BBC before adsorption Fig.4.26b. FT-IR Spectrum of BBC after adsorption of malachite green 111

64 Counts 1000 outside work2_ Position [ 2Theta] Fig.4.27b.XRD pattern of BBC after adsorption of malachite green 112

65 4.4 Adsorption of Rhodamine B by BBC Effect of carbon concentration: The adsorption of the dyes on carbon was studied by varying the carbon concentration ( mg/50ml) for 40 mg/l of dye concentration. The percent adsorption increased with increase in the carbon concentration (Figure 4.28). This was attributed to increased carbon surface area and availability of more adsorption sites 23,70,89. Hence the remaining parts of the experiments are carried out with the adsorbent dose of 100mg/50 ml Effect of contact time and initial dye concentration: The experimental results of adsorptions of at various concentrations (10, 20,30,40,50 and 60 mg/l) with contact time are shown in representative Figure The equilibrium data were collected in Table 4.21 reveals that, percent adsorption decreased with increase in initial dye concentration, but the actual amount of dye adsorbed per unit mass of carbon increased with increase in dye concentration. It means that the adsorption is highly dependent on initial concentration of dye. It is because of that at lower concentration, the ratio of the initial number of dye molecules to the available surface area is low subsequently the fractional adsorption becomes independent of initial concentration. However, at high concentration the available sites of adsorption becomes fewer and hence the percentage removal of dye is dependent upon initial concentration 21,23,39. Equilibrium have established at 40 minutes for all concentrations. Figure 4.29 reveals that the curves are single, smooth, and continuous, leading to saturation, suggesting the possible monolayer coverage of the dyes on the carbon surface Adsorption isotherm: The experimental data analyzed according to the linear form of the Langmuir and Freundlich isotherms 141,142.. The linear plots of C e/ Q e versus C e suggest the applicability of the Langmuir isotherms (Figure.4.30). The Q m and b is 113

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