BNMBE 22 PPT presented by Dr. Arvind Kumar.pptx

32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology &
Environmental Sciences (BNMBE-22)

1. O ptimization studies for 2-C hlorophenol removal by walnut shell activated carbon ( WAC) using T aguchi's experimental design Speaker Dr. Arvind Kumar, Asst. Professor Dept. of Chemical Engineering NIT, Rourkela, India, 769008 E-Mail: [email protected] Presented at 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences (BNMBE-22) Dec. 21-23, 2022 Bangkok, Thailand 18-02-2023 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand 1

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6. Introduction 2-Chlorophenol (2-CP) is a chlorinated phenol and has catastrophic effects towards aquatic ecosystem [1] . Physicochemical properties of 2-CP [2] Parameter Value CAS ID 95-57-8 Formula C 6 H 5 OCl Mol. wt. (g mol -1 ) 128.56 Boiling pt. ( o C) 174.9 Melting pt. ( o C) 9.3 Solubility (g L -1 ) 28 pK a 8.56 Density (g cm -3 ) 1.26 Health hazards of 2-chlorophenol [3] 2-CP has several detrimental health hazards. Health hazards Compromised immunity due to lymphocyte disruption Genetic disorders because of the defects in DNA strands Cancer Failure of vital organ systems : endocrine system, respiratory system, cardiac system, and digestive system Industrial application of 2-CP and sources of its introduction into ecosystem [4] Industrial applications Pesticide Wood preservation Plastic Petrochemicals Pharmaceuticals Textiles Effluent sources Industrial effluents Agricultural runoffs Sewage 2-CP has been adjudged as a priority pollutant by USEPA and EU. As per USEPA the maximum concentration of 2-CP in effluent and water should be as low as 2 and 0.1 µg L -1 , respectively [5] . 18-02-2023 6 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

7. Methods of 2-CP removal from aqueous environment and their cons [6] Adsorption and its pros Statistical optimization using Taguchi’s experimental design [7] The Taguchi’s design was proposed by Genichi Taguchi The design of experiments ensure bare minimum experimental runs required for achieving the optimization The multivariate approach helps in simultaneous exploration of the effects of all variables at once The Signal-to-noise (S/N) ratio and analysis of variance (ANOVA) are the decisive parameters to adjudge the most influential and significant parameters, respectively. Minitab statistical software package [version 14.12.0.1, Minitab Inc., USA ] was used. 18-02-2023 7 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

8. Materials and Methods Adsorbent and Adsorbate Walnut shell activated carbons (WAC) were prepared via thermochemical route with ZnCl 2 as impregnating agent in the (w/w) ratio of 6:1 for walnut shells : ZnCl 2 2-CP solutions were prepared by dissolving appropriate quantity of the solute in double distilled water Analysis of 2-CP samples [8] The 2-CP samples were analyzed using UV-Vis Spectrophotometer (UV-1800, Shimadzu) at  max = 273 nm The adsorption performance was determined on the basis of adsorption capacity ( q e ) Adsorption capacity = (1) Where X o is the initial concentration X e is the equilibrium concentration (mg L -1 ) of 2-CP at equilibrium w is the mass (g) of WAC V is the volume (mL) of the 2-CP solution taken. 18-02-2023 8 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

9. Taguchi’s Experimental design: Orthogonal array [7, 9] A L 9 orthogonal array was chosen for optimizing the 2-CP adsorption onto WAC Four parameters namely pH , contact time (min) , 2-CP concentration (mg L -1 ) and temperature ( o C) were taken into consideration for optimization. The degree of freedom (DOF) for any parameter = [levels of variation-1] (2) Based on Eq. 2, total degrees of freedom of the parameters = 4(3-1) = 8 Table 1. Chosen parameters and their three level variations. Parameters Level-1 Level-2 Level-3 pH 6 8 10 Contact time (t) 60 120 180 Concentration (X o ) 50 100 150 Temperature (T) 30 40 50 18-02-2023 9 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

10. Results and Discussions The design matrix of L 9 orthogonal array The highlighted section is the design matrix for L 9 orthogonal array used in this study. It has 9 rows depicting the 9 sets of experiments set by Taguchi’s design, and 4 columns, those depict the parameter combinations for experimental run. Run pH t X o T q t,WAC S/N ratio 1 6 60 50 30 22 31 2 6 120 100 40 27 34 3 6 180 150 50 38 38 4 8 60 100 50 29 41 5 8 120 150 30 106 113 6 8 180 50 40 29 29 7 10 60 150 40 19 27 8 10 120 50 50 5.2 12.9 9 10 180 100 30 16 20 Table 2. Design matrix of L 9 orthogonal array with corresponding adsorption capacity and S/N ratio. 18-02-2023 10 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

11. S/N ratio analysis [10] The S/N ratio predicts the desirability index of any parameter. Practically three different characteristics of S/N ratio exists. The-minima-the-better (TMTB ) = (3) The-maxima-the-better (TMB) = (4) The-nominal-the-better (TNB) = (5) In this study the TMB approach was chosen, since maximum 2-CP removal was desirable . Table 3. S/N ratio response matrix of different parameters for 2CP adsorption by WAC . 18-02-2023 11 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

12. Fig 2. Graphical representation of S/N ratio for 2CP adsorption onto WAC. Analysis of Variance (ANOVA) The ANOVA helps in evaluating the significant parameters among the parameters used for optimization [9, 10] Table 4. The ANOVA results based on the Fisher test and the sum of squares. Parameters DOF Seq. Sum of squares Adj. Sum of squares Adj. Mean square F (Denominator of F-test is zero) P Remarks pH 2 2839.82 2839.82 1447.29 Very high <0.0001 Significant t 2 1054.48 1054.48 523.16 Very high <0.0001 Significant X o 2 1233.27 1233.27 607.34 Very high <0.0001 Significant T 2 2407.67 2407.67 1205.17 Very high <0.0001 Significant Error 0.00 0.00 0.00 <0.0001 Total 8 7535.24 18-02-2023 12 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

13. Validation of the Taguchi’s design predicted parameters This step is a confirmatory step for the Taguchi’s design predicted parameters Table 5. Outcomes of experimental validation run based on Taguchi's design . pH t X o T q e,WAC S/N ratio Taguchi model predicted optimized combination of parameters 6 120 150 30 205 256 Result obtained from experimental run 6 120 150 30 206.17 256±1 18-02-2023 13 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

14. Conclusions The S/N ratio analysis has revealed that the pH of the adsorption environment had the highest impact , whereas the contact time has the least impact on 2-CP adsorption. The ANOVA analysis has revealed that pH, contact time, 2-CP concentration and temperature all four parameters were significant in the course of optimization process. Based on the validation experimental run, the L 9 orthogonal array based on Taguchi's design of experiments has successfully optimized the adsorption of 2-CP onto WAC . 18-02-2023 14 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

15. References A.O. Olaniran, E.O. Igbinosa, Chlorophenols and other related derivatives of environmental concern: Properties, distribution and microbial degradation processes, Chemosphere . 83 (2011) 1297–1306. doi:10.1016/j.chemosphere.2011.04.009. T. Ge, J. Han, Y. Qi, X. Gu, L. Ma, C. Zhang, S. Naeem, D. Huang, The toxic effects of chlorophenols and associated mechanisms in fish, Aquat Toxicol. 184 (2017) 78–93. doi:10.1016/j.aquatox.2017.01.005. Substance Priority List (SPL) Resource Page, CERCLA priority list of hazardous substances: Agency for Toxic Substances and Disease Registry, Buford Hwy NE Atlanta (US). https://www.atsdr.cdc.gov/spl/previous/07list.html , 2007 (accessed 20 Aug 2021). E.O. Igbinosa, E.E. Odjadjare, V.N. Chigor, I.H. Igbinosa, A.O. Emoghene, F.O. Ekhaise, N.O. Igiehon, O.G. Idemudia, Toxicological Profile of Chlorophenols and Their Derivatives in the Environment: The Public Health Perspective, The Scientific World Journal, (2013) 1  11. doi : 10.1155/2013/460215. Ambient Water Quality Criteria for 2-chlorophenol, United States Environmental Protection Agency, Office of Water Regulations and Standards Criteria and Standards Division Washington DC (US) 20460. https://www.epa.gov/sites/default/files/2018-12/documents/ambient-wqc-2chlorophenol.pdf , (accessed 10 Oct 2022). Z.N. Garba, W. Zhou, I. Lawan, W. Xiao, M. Zhang, L. Wang et al., An overview of chlorophenols as contaminants and their removal from wastewater by adsorption: A review, J. Environ Manage . 241 (2019) 59–75. doi: 10.1016/j.jenvman.2019.04.004. M.K. Mahapatra, A. Kumar, Taguchi Optimization Studies for Abatement of 2-Chlorophenol Using Neem Seed Activated Carbon, Chem. Eng. Technol. 45 (2022) 641-648. doi:10.1002/ceat.202100427 . M.K. Mahapatra, A. Kumar , Studies on the Adsorption of 2-Chlorophenol onto Rice Straw Activated Carbon from Aqueous Solution and its Regeneration, Chem. Biochem. Eng. Q., 36 (2022) 51–65. doi:10.15255/CABEQ.2021.2004. V.C. Srivastava, I.D. Mall, I.M. Mishra, Optimization of parameters for adsorption of metal ions onto rice husk ash using Taguchi's experimental design methodology, Chem. Eng. J. 140 (2007) 136–144. doi:10.1016/j.cej.2007.09.030. A.S. Yusuff, O.A. Ajayi, L.T. Popoola, Application of Taguchi design approach to parametric optimization of adsorption of crystal violet dye by activated carbon from poultry litter, Sci. Afr. 13 (2021) 113. doi:10.1016/j.sciaf.2021.e00850. 18-02-2023 15 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

16. Acknowledgements I am very much thankful to the organizers of the International Conference on Nanotechnology, Materials, Biotechnology and Environmental Sciences (BNMBE-22) for providing an opportunity to present our research work. I am also thankful to my Ph.D. research scholar and co-author of this presented study Mr. Manoj Kumar Mahapatra, for carrying out the necessary research work in the laboratory . I want to convey a token of gratitude to the National Institute of Technology (NIT) Rourkela administration, for providing the necessary facilities for carrying out this research work and facilitating the requirements for attending this conference. 18-02-2023 16 32nd BANGKOK International Conference on Nanotechnology, Materials, Biotechnology & Environmental Sciences ( BNMBE-22), Dec . 21-23, 2022, Bangkok , Thailand

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