Statistical Analysis of Congo Red Dye Removal Using Sawdust Activated Carbon

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1 Statistical Analysis of Congo Red Dye Removal Using Sawdust Activated Carbon M.Srinivas Kini*, K.Balakrishna Prabhu, Ankit Gundecha and Devika.U Department of Chemical Engineering, Manipal Institute of Technology, Manipal, Karnataka , India. *Orcid ID: , (*Corresponding author) Abstract In the present study, an adsorbent was prepared from Ben Teak sawdust by chemically treating and carbonizing with phosphoric acid. Using Design Experts software, 2 level factorial studies and Response surface methodology studies using Box-Benkhen design model were carried out and a relationship between Q e and ph, temperature, concentration of dye, amount of adsorbent, agitation speed were derived for Congo red- Saw Dust Carbon(SDC). Maximum Congo-red removal of % and adsorption capacity of mg/g was found at ph 2, 30 C, 125 rpm, 150 mg/l and 1gram/L of reaction mixture for an optimum contact time of 2.5 hours. Adsorption isotherm obtained fitted well into both Freundlich and Langmuir equation but Freundlich isotherm fits better with 1/n ranging from to and R 2 ranging from to The q max from Langmuir isotherm was established to be mg/g. Keyword: Sawdust Carbon, Congo red, Box-Benkhen, Response surface methodology, Langmuir The freshwater is consumed in mainly three segments like agricultural, industrial and domestic segments and this has led to the production of large amounts of wastewater comprising innumerous pollutants. One of the main type of the contaminants is dyes. Dye pollution has become a significant problem. The release of dye-bearing wastewater into water bodies from different industries poses problems as these dyes are toxic in nature causing damage to the natural surroundings and disrupting the life of aquatic beings. Dyes are toxic and concentration as low as 0.005mg/L is visible which captures the attention of both public and authorities. Currently, there are more than 100,000 marketable dyes and the annual production of these dyes is assessed to be tonnes per year [1]. It is established that 10-15% of the used dyes enter the environs through waste [2]. The main end users of dyes are textile, dyeing, paper and pulp, tannery and paint industry. Hence the wastewater of these industries in addition to those from plant producing dyes tend to contain dyes in adequate amount. Various methods that have been adopted for dye removal over the years are microbial degradation, precipitation, membrane filtration, electrochemical destruction, ozonation, photochemical process, Ion exchange and reverse osmosis. Adsorption is a familiar separation technique and preferred method for dye elimination from wastewater [3]. Adsorption has been found to be successful technique over other treatment methods due to its less first cost, greater flexibility, ease of design and operation, insensitivity to toxic dyes. Though adsorption on commercially activated carbon (AC) is preferred in most of the industries for effluent treatment but issues like losses during regeneration and high cost limit their use. In this context, an earnest effort is made to present an inexpensive adsorbent for dye removal. The study involves preparation of Ben Teak sawdust carbon (SDC) as an adsorbent for elimination of Congo red(cr) dye. Batch studies incuded parameters such as ph, adsorbent concentration, initial CR concentration, temperature and agitation rpm. The influence of these parameters on adsorption capacity was examined using 2 Level factorial and Response Surface Methodology (RSM) studies employing Design Expert software. The adsorption data were fitted using suitable isotherm. MATERIALS & METHODS Preparation of the adsorbate Congo red dye solution of 1000mg/L was prepared by dissolving 1 g of CR powder in 1L standard flask using distilled water. Figure 1: Chemical structure of Congo-Red 8788

2 Preparation of the adsorbent Saw dust of Ben Teak wood was dried at 105 C in a drier for 5 hours to minimize moisture content. The dried saw dust was mixed thoroughly with 88% ortho-phosphoric acid. The mixture was then carbonized in a muffle furnace at 300 C for 3 hours. The carbonized sample was first washed with water followed by 2% of sodium bicarbonate (NaHCO 3) to neutralize the ph. The washed sample was dried at 110 C in a drier for 24 hours. The dried sample was grinded and sieved through a mesh size of 150 µm. From the BET studies the surface area of SDC was m 2 /g and the pore volume was cc/g. LEVEL FACTORIAL AND RSM STUDIES Factorial and RSM studies were carried out by analysing the process of adsorption for 100mL of reaction mixture according to the change in ph, temperature, amount of adsorbent, concentration of dye and agitation speed. The range of these parameters is as follows: a) ph 2 to 9 b) Temperature 30 C to 50 C c) Amount of adsorbent 0.1 to 2 g d) Concentration of dye 25 mg/l to 150 mg/l e) Agitation speed 125 rpm to 200 rpm A table of experiments was created using the design expert software. The factorial and RSM studies were carried out by varying 5 parameters. Hence, a table of 32 (2 5 ) experiments was created. Box-Benkhen design was employed for the RSM studies. The experiments were carried out according to the table for a preliminary contact time of 6 hours in 250mL conical flask containing 100mL of reaction mixture. The filtrate from each experiment was analysed using the UV spectrophotometer and corresponding Q e, percentage removal values were calculated using the following equations. Boehm Titration [4] For Boehm titration, 1.0 g of the SDC was mixed with 15mL solution of Sodium bicarbonate (0.1M), Sodium carbonate (0.05M) and Sodium hydroxide (0.1M) for determining acidic groups and 0.1M Hydrochloric acid for determining basic groups/sites respectively at 32 o C for more than 48 hours with intermittent swirling. Consequently, the aqueous mixture were back titrated with Hydrochloric acid(0.1m) for acidic and Sodium hydroxide (0.1M) for basic groups. The quantity and nature of acidic groups were calculated by considering that Sodium hydroxide neutralises carboxylic, lactonic and phenolic groups, sodium carbonate neutralises carboxylic and lactonic groups and that sodium bicarbonate neutralises only carboxylic groups. Neutralisation points were known using ph indicator of phenolphthalein solution. Fourier transform infra-red (FTIR) Studies The FTIR analysis was carried out in a FTIR spectrophotometer 8400S manufactured by Shimadzu having a wavenumber range of cm -1. In this study, the adsorbent is first mixed with KBr (about 10 times the weight of the sample) in a mortar at ambient temperature. The mixture is then placed in a hydrostatic pressure (pressure of 5 tonnes is applied) to make a thin transparent pellet. The pellet is then transferred to the FTIR spectrophotometer for analysis Adsorption Isotherms Langmuir and Freundlich, were used to fit the experimental data points for Congo-Red adsorption on absorbent at three temperatures, 30, 40 and 50 C. 100mL of dye with concentrations of 25, 50, 75, 100 and 150mg/L were used at each temperature and 0.1gram of adsorbent was added at ph 3.3. The agitation speed of 125rpm was maintained for all experiments. Where, Co Initial conc. in mg/l Ct Final conc. in mg/l And, V Volume of CR solution in L M Amount of adsorbent in g RESULT AND DISCUSSION Calibration Curve of Congo-red The calibration curve provided with the relationship between the measured absorbance and the CR concentration of the dye at λ max = 499nm. 8789

3 Figure 2: Calibration Curve of Congo-red Table 1: Boehm Titration Results Groups Before adsorption of congo-red After adsorption of congored Carboxylic groups (mmol/g) Phenolic groups (mmol/g) Lactonic groups (mmol/g) 0 0 Basic groups (mmol/g) From the above table we can infer that, predominantly carboxylic and phenolic groups existing on the exterior of the adsorbent are responsible for the adsorption of congo-red. FTIR Studies Figure 3: FTIR before adsorption of CR on SDC 8790

4 Figure 4: FTIR after adsorption of CR on SDC From Figure 3, peaks with wavenumber cm -1 and cm -1 are predominant and from Figure 4., peaks having wavenumber cm -1, cm -1 and cm -1 are predominant. On comparing the two figures, it can be inferred that Alcohol (O-H, stretch, H-bonded), Carbonyl (C=O, stretch) and Nitro (N-O, stretch) functional groups are accountable for the adsorption of congo-red on the exterior of the adsorbent. The results obtained from FTIR analysis are in concordance with Boehm titration results. LEVEL FACTORIAL STUDIES The 2 Level factorial studies were carried out using the Design Expert software. The following table illustrates the results obtained after carrying out each experiment for 6 hours. Std Run Block ph Amt of adsorbent g Table 2: Factorial Studies for adsorption of CR on SDC Conc of dye mg/l Temp Deg C Agitation speed rpm Qe mg/g % removal 6 1 Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block

5 2 16 Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block The results obtained were analysed using ANOVA (Analysis of Variance) and the following results were obtained for adsorption capacity: Table 3: ANOVA Analysis Table - I Source Sum. of Squares df Square of Mean F - Value p-value Prob. > F For Model < significant A-pH B-Conc of Ad < C-Conc of dye < D-Temperature E E-Agitation speed AB AC AD E AE BC < BD E BE DE E ABC ABD E ABE ADE 1.555E E E BDE E ABDE 9.574E E E Residual Cor Total

6 The F-value of obtained from the model implies the it is significant. There is a 0.01% chance that a "Model F-Value" this large could happen due to noise. St. Dev R Mean Adj R The "Pred R-Squared" of agrees with the "Adj R- Squared" of "Adequate Precision" gives the ratio of signal to noise. The desirable ratio should be greater than 4. Adequate Precision of point toward an adequate signal. This model can be used to navigate the design space. CV. % Pred R PRESS Adequate Precision Final Equation with Actual Factors: a) Percentage Removal = (3) * ph * Amt of adsorbent * Conc of dye * Amt of adsorbent * Conc of dye From the above equation we can infer that, percentage removal has a linear relationship with ph, amount of adsorbent and concentration of dye. There is also a significant interaction between amount of adsorbent and concentration of dye. b) Qe = (4) * ph * Conc of Ad * Conc of dye * Temperature * Agitation speed * ph * Conc of Ad * ph * Conc of dye E-00 * ph * Temperature * ph * Agitation speed * Conc of Ad * Conc of dye E-004 * Conc of Ad * Temperature * Conc of Ad * Agitation speed E-005 * Temperature * Agitation speed * ph * Conc of Ad * Conc of dye E-003 * ph * Conc of Ad * Temperature * ph * Conc of Ad * Agitation speed E-006 * ph * Temperature * Agitation speed E-005 * Conc of Ad * Temperature * Agitation speed E-005 * ph * Conc of Ad * Temperature * Agitation speed From the above equation we can infer that, adsorption capacity has a linear, 2 factor interaction and 3 factor interaction with the parameters taken into consideration. Response Surface Methodology (RSM) Studies Adsorption experiments were conducted as per design developed with response surface Box-Benkhen design methodology. The experiments were performed in 250mL conical flasks and 100mL reaction mixture for 6 hours. 8793

7 Std Run Block ph Amt of adsorbent in g Table 4: RSM Studies for adsorption of CR on SDC Conc of dye in mg/l Temp in C Agitation speed in rpm Qe in mg/g % removal 38 1 Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block Block

8 8 41 Block Block Block Block Block Block The following fit summary was obtained for adsorption capacity : Table 5: Fit Summary for adsorption capacity of SDC Source. Sum. of Squares df Square of Mean F- value p-value Prob. > F Mean vs Total Linear vs Mean < Suggested 2FI vs Linear Quadratic vs 2FI Suggested Cubic vs Quadratic Aliased Residual Total The following model summary analysis was obtained for adsorption capacity : Table 6: Model Summary Analysis for adsorption capacity of SDC Source. St. dev R 2 Adjusted R 2 Predicted R 2 PRESS Linear Suggested 2 FI Quadratic Suggested Cubic E+005 Aliased *PRESS Predicted Residual Sum of Sqaures The following fit summary was obtained for percentage removal: Table 7: Fit summary for percentage removal of CR Source. Sum. of Squares df Square of Mean F- value p-value Prob. > F Mean vs Total 3.775E E+005 Linear vs Mean Suggested 2FI vs Linear Quadratic vs 2FI Suggested Cubic vs Quadratic Aliased Residual Total 3.84E

9 The following model analysis was obtained for pecentage removal: Table 8: Model analysis for percentage removal of CR Source. St. dev R 2 Adjusted R 2 Predicted R 2 PRESS Linear Suggested 2 FI Quadratic Suggested Cubic Aliased From Table 6, it can be concluded that quadratic model gives a better fit for adsorption capacity as the R 2 value is high and adjusted-r 2, predicted-r 2 are in reasonable agreement. Similarly from Table 8, Linear model fits better for percentage removal. Final Equation with actual factors: a) Percentage removal = (5) * ph * Amt of adsorbent * Conc of dye * Temperature * Agitation speed b) Qe = (6) * ph * Amt of adsorbent * Conc of dye * Temperature * Agitation speed * ph * Amt of adsorbent E-004 * ph * Conc of dye E-004 * ph * Temperature E-004 * ph * Agitation speed * Amt of adsorbent * Conc of dye * Amt of adsorbent * Temperature E-003 * Amt of adsorbent * Agitation speed * Conc of dye * Temperature E-006 * Conc of dye * Agitation speed E-004 * Temperature * Agitation speed * ph * Amt of adsorbent E-003 * Conc of dye * Temperature E-003 * Agitation speed

10 Analysis of RSM Studies Figure 5: Effect of amount of SDC and conc. of CR on adsorption capacity of SDC. (ph 2, 30 C, 125 rpm) Figure 6: Effect of ph and amount of SDC on adsorption capacity of SDC. (150 mg/l of CR, 30 C, 125 rpm) Figure 7: Effect of temp. and amount of adsorbent on adsorption capacity of SDC. (150 mg/l of CR, ph 2, 125 rpm) 8797

11 Figure 8: Effect of temp. and agitation rpm on adsorption capacity of SDC. (150 mg/l of CR, 1 g/l of SDC, ph 2) Figure 9: Effect of ph and temp. on adsorption capacity of SDC. (150 mg/l CR, 1 g/l of SDC, 125 rpm) Figure 10: Effect of SDC dosage on percentage CR removal. (150 mg/l of CR, ph 2, 30 C, 125 rpm) 8798

12 Figure 11: Effect of ph on percentage CR removal (150 mg/l of CR, 1g/L of SDC, 30 C, 125 rpm) Figure 12: Effect of temperature on percentage removal of CR. (150 mg/l of CR, 1 g/l of SDC, ph 2, 125 rpm) Figure 13: Effect of agitation rpm on percentage CR removal (150 mg/l of CR, 1 g/l of SDC, ph 2, 30 C) 8799

13 Effect of ph The isoelectric point of congo-red is 3 [5]. At ph below the isoelectric point, CR exists mostly in the molecular form and above the isoelectric point it exists in its dissociated form. By and large the adsorption of an anionic dye drops with increase in ph, due to two reasons (i) the negative charge on the surface of the adsorbent (ii) excess OH - ions in the solution that compete for the adsorption sites. The adsorption of congo-red was studied in the ph range of 2-9 where Q e decreased from mg/g to mg/g and percentage removal decreased from 96.79% to 76% with increase in ph. This behaviour may be due to greater positive charge on the exterior of the SDC. Effect of initial concentration of dye The equilibrium adsorption capacity (Q e) increased from mg/g to mg/g with increase in initial CR concentration from 25 to 150 mg/l due an increase in the mass gradient between the CR solution and the SDC and thus acting as a driving force for the transfer of CR molecules from the bulk to the SDC surface. However the percentage removal decreased from % to % with increase in the initial CR concentration from 25 to 150 mg/l, since the surface area available and the active sites saturate leading to a decrease in percentage decolourization. Effect of temperature Both percentage removal and adsorption capacity increased from % to 96.41% and mg/g to mg/g respectively with rise in temperature from 30 C to 50 C. By increase in temperature, the solubility of the dye decreases which results in greater adsorption. An increase in adsorption may also be due to rise in the movement of the large CR ion with temperature, as many molecules may gain sufficient energy to endure interaction with active sites on the surface of SDC. Effect of SDC dosage Percentage removal of congo-red increased from % to 99.23% with increase in SDC dosage from 0.1 to 2 g whereas Q e decreased from mg/g to mg/g with increase in SDC dosage. Increase in percentage removal can be ascribed to increased SDC surface area and presence of additional adsorption sites. Whereas decrease in adsorption capacity may be due to overlapping of sorption sites as a result of overcrowding of SDC particles.. Isotherm Modelling The optimum conditions in terms of amount of adsorbent (Ben Teak Sawdust), concentration of dye, ph, agitation speed and temperature were maintained throughout to model the optimum isotherm model. The non-linear forms of Langmuir and Freundlich isotherm equations were used and their applicability was determined by comparing the correlation coefficients (R 2 ) and the model with the highest R 2 value is considered as the best fit. Langmuir isotherm theory is based on the assumptions that the surface of the adsorbent is uniform with no interaction of the adsorbed molecules. The entire adsorption happens through the identical mechanism and at the maximum adsorption, only a monolayer is formed. The Langmuir equation can be written in the following form [6] : Where, Qe = equilibrium adsorbent capacity (mg/g) Ce = equilibrium conc. of dye (mg/l) b = constant associated to the affinity of binding sites (L/mg) Qo = Maximum adsorption capacity of adsorbent (mg/g) The Freundlich isotherm is derived by assuming a heterogeneous surface with a non-uniform distribution of heat of adsorption over the surface and is used for dilute solution [7]. The equation is: Where, Qe = KF Ce (1/n) (8) C e= equilibrium conc. in the dye solution (mg/l) Q e = adsorption capacity at equilibrium (mg/g) K F = amount adsorbed at unit concentration n = constant. The following are the graphs obtained through isotherm studies performed at 30 C, 40 C and 50 C. The graphs are obtained by plotting the adsorbent capacity, Qe (mg/g) against the final dye concentration, Ce (mg/l). 8800

14 Figure 14. Langmuir and Freundlich Isotherms at 30 C for adsorption of CR on SDC. (1 g/l of SDC, ph 3.3, 125 rpm) Figure 15. Langmuir and Freundlich Isotherms at 40 C for adsorption of CR on SDC. (1 g/l of SDC, ph 3.3, 125 rpm) 8801

15 Figure 16. Langmuir and Freundlich Isotherms at 50 C for adsorption of CR on SDC. (1 g/l of SDC, ph 3.3, 125 rpm) Table 9. Langmuir and Freundlich isotherm constants at 30 C for CR adsorption on 30 C Langmuir Freundlich Co (mg/l) Qe (mg/gm) RL Qo (mg/gm) b (L/mg) R 2 KF (mg/gm) (L/g) n 1/n R SDC. (1 g/l of SDC, ph 3.3, 125 rpm) Table 10:. Langmuir and Freundlich isotherm constants at 40 C for CR adsorption on SDC. (1 g/l of SDC, ph 3.3, 125 rpm) 40 C Langmuir Freundlich Co (mg/l) Qe (mg/gm) RL Qo (mg/gm) b (L/mg) R 2 KF (mg/gm) (L/gm) n 1/n R

16 Table 11: Langmuir and Freundlich isotherm constants at 50 C for CR adsorption on SDC. (1 g/l of SDC, ph 3.3, 125 rpm) Langmuir 50 C Freundlich Co (mg/l) Qe (mg/gm) RL Qo (mg/gm) b (L/mg) R 2 KF (mg/gm) (L/gm) n 1/n R The results show slight deviation from the fitted non-linear equation of Langmuir model as indicated by the high value of R 2 ranging from to The highest R 2 value was obtained at 50 C. From the literature, when the R 2 value is greater than 0.89, the adsorption data follows the Langmuir model. Moreover, the value of Q o of activated Ben Teak wood was calculated to be 209.7mg/g at 50 C and an initial concentration of 150mg/L. The fitting of data to Langmuir model indicates both the homogeneous nature of Ben Teak sawdust surface and the formation of monolayer of Congo- Red dye molecule at its exterior surface. The dimensionless separation factor (R L) indicates a characteristic of Langmuir isotherm. The R L values obtained were in the range of 0 to 1 indicating good adsorption under all temperatures and initial CR concentrations. The non-linear model of Freundlich isotherm was used to find the intercept values of K F and the slope (1/n) together with R 2. The highest value of R 2 obtained using Freundlich model (0.952) was slightly higher than that obtained using Langmuir model. The values of (1/n) obtained were in the range 0 and 1 thus indicating the favourable nature of the process and heterogeneous nature of the adsorbent surface. Therefore, Freundlich model is also well fitted using the data. Hence, it can be conclude that Ben Teak is indeed a good adsorbent of Congo-Red dye using both the Langmuir and Freundlich model. The applicability of both Langmuir and Freundlich model shows that both monolayer adsorption and heterogeneous energy distribution of active sites on the surface of the SDC exist under the experimental conditions employed. CONCLUSION Chemically activated and carbonised ben-teak saw dust can be considered a suitable adsorbent for removal of textile dyes from aqueous solution. The percentage removal/decolourisation increased with (i) increase in SDC mass (ii) decrease in concentration of dye (iii) decrease in ph (iv) increase in temperature and (v) decrease in agitation speed. Whereas, Adsorption capacity increased with (i) decrease in SDC mass (ii) increase in concentration of dye(iii)decrease in ph and (iv) increase in temperature. According to RSM studies, adsorption capacity fitted better in quadratic equation whereas percentage removal fitted better in linear equation. The adsorption isotherm was successfully defined by Freundlich isotherm. ACKNOWLEDGEMENTS Authors gratefully acknowledge assistance received in the form of experimental facilities for conducting this research work from Manipal University, Manipal, India. REFERENCES [1] Husain, Q., 2006, Potential applications of the oxidoreductive enzymes in the decolorization and detoxification of textile and other synthetic dyes from polluted water: a review, Crit. Rev Biotechnol., 26, pp [2] Hai, F. I., Yamamoto, K., Fukushi, K.,2007, Hybrid treatment systems for dye wastewater, Crit. Rev. Env. Sci. Technol., 37, pp [3] Dabrowski A.,2001, Adsorption from theory to practice, Advances in Colloid and Interface Science, 93, pp [4] Ekpete O.A. and Horsfall M.J.N.R., 2011, Preparation and Characterisation of Activated Carbon derived from Fluted Pumpkin Stem Waste, Research Journal of Chemical Sciences, 1(3), pp [5] Zvezdelina Yaneva. and Nedyalka Georgieve, 2012, Insights into Congo Red adsorption on Agro-Industrial Materials Spectral, Equilibrium, Kinetic, Thermodynamic, Dynamic and Desorption Studies. A review, International Review of Chemical Engineering., 4(2), pp [6] Jain, S. and Jayaram, R.V., 2010, Removal of basic dyes from aqueous solution by low cost adsorbent: wood apple shell (Feronia acidissima), Desalination, 250(3), pp

17 [7] Doˇgan M., Abak H. and Alkan M.,2008, Biosorption of methylene blue from aqueous solutions by hazelnut shells: equilibrium, parameters and isotherms, Water, Air, and Soil Pollution, 192(1 4), pp

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