Removal of Methylene Blue, Methyl Violet, Acid Blue and Acid Violet Dyes using Blue-Green Algae by Adsorption Technique

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1 Removal of Methylene Blue, Methyl Violet, Acid Blue and Acid Violet Dyes using Blue-Green Algae by Adsorption Technique By J. Krishnaveni Supervisor Dr. N. Renugadevi Thesis Submitted to Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore In Partial Fulfilment of the Requirements for the Degree of Doctor of Philosophy in Chemistry August 2014

4 Acknowledgement I owe my sincere thanks to ALMIGHTY for showering His generous blessings upon me in all my endeavors. I extend my profound gratitude to Dr. T.S.K. Meenakshisundaram, M.A., M.Phil., Ph.D., Chancellor, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for providing the conducive infrastructure to undertake this research study. I express my sincere thanks to Dr. (Mrs.) Sheela Ramachandran, M.Sc., P.G. Dip., Ph.D., Vice Chancellor, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for granting permission to carry out this work. I extend my grateful thanks to Dr. (Mrs.) Gowri Ramakrishnan, M.Sc., M.Phil., Ph.D., Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for providing all the administrative support and help required to carry out this work. I place a deep sense of gratitude to Dr. (Mrs.) G.P. Jeyanthi, M.Sc., M.Phil., Ph.D., Controller of Examination, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for providing necessary facilities for the completion of the study. I express my sincere thanks and deep sense of gratitude to Dr. (Mrs.) A. Parvathi, M.Sc., Dip.Ed., M.Phil., Ph.D., Dean, Faculty of Science, Avinashilingam Institute for Home Science and Higher Education for women, Coimbatore, for inspiring me to complete the research work successfully. I whole heartedly thank Dr. (Mrs.) R. Shyamala, M.Sc., Dip.Ed., M.Phil., Ph.D., Professor and Head of the Department of Chemistry, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for her valuable advice and generous help.

5 My deepest appreciation and gratitude to my supervisor, Dr. (Mrs.) N. Renugadevi, M.Sc., M.Phil., Ph.D., Professor, Department of Chemistry, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for her constructive criticism, valuable guidance, meticulous care and constant support throughout my research work. She has been very kind and patient in clarifying my doubts during the period of my study. I extend my thanks to all the Faculty Members and Research Scholars, Department of Chemistry, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for their valuable ideas, comments and constant encouragement throughout the research work. I express my thanks to the non teaching staff, Department of Chemistry, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore, for their help throughout the period of my study. I articulate my profound sense of indebtedness to Dr. K. Kadirvelu, M.Sc., Ph.D., Joint Director, DRDO, Bharathiar University Campus, Coimbatore, for providing necessary facilities in recording SEM images. I thank Mr. Murugan, Manager, Quality Control of Dyeing Industries, Tiruppur, for providing Industrial Effluents needed for this work. I express my gratitude to the Chairman, Secretary, Principal and Chief Operation, Tamilnadu College of Engineering, Coimbatore, for granting permission and their tremendous support to carry out this research work. I wish to thank the HOD and my colleagues, Tamilnadu College of Engineering, Coimbatore, for their valuable advice and encouragement. I truly obliged to my family for their uninterrupted love, patience and encouragement that made possible, with whole dedication towards the present study. J. Krishnaveni

6 Contents 1. Introduction Review of Literature 4 3. Materials and Methods Results and Discussion Characteristics of the Adsorbent Effect of Initial Concentration of Dye Solution on Dye Removal Effect of ph on Dye Removal Effect of Adsorbent Dosage on Dye Removal Effect of Temperature on Dye Removal Adsorption of Dyes from Dyeing Industrial Effluent Efficiency of Blue-Green Algae in the Removal of Dyes by Adsorption Kinetics of Adsorption Adsorption Isotherms Thermodynamic Studies Scanning Electron Microscope and FTIR Spectral Analysis 160 Summary and Conclusion. 171 References. 174 Appendices Publications

7 List of Tables Table 1 Dyes used in this Study 26 Table 2 Characteristics of the Adsorbent BGA 33 Table 3 with Variation of Initial Concentration of Methylene Blue Dye Solution 36 Table 4 with Variation of Initial Concentration of Methyl Violet Dye Solution 37 Table 5 Adsorption of Acid Blue Dye from Aqueous Solution with Variation of Initial Concentration of Acid Blue Dye Solution 38 Table 6 Adsorption of Acid Violet Dye from Aqueous Solution with Variation of Initial Concentration of Acid Violet Dye Solution 39 Table 7 Adsorption of Methylene Blue Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Methylene Blue Dye Solution 42 Table 8 Adsorption of Methyl Violet Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Methyl Violet Dye Solution 43 Table 9 Adsorption of Acid Blue Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Acid Blue Dye Solution 44 Table 10 Adsorption of Acid Violet Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Acid Violet Dye Solution 45 Table 11 with ph Variation 50 Table 12 Adsorption of Acid Violet Dye from Aqueous Solution with ph Variation 51 Table 13 with ph Variation 53

8 Table 14 Adsorption of Acid Blue Dye from Aqueous Solution with ph Variation 54 Table 15 with Adsorbent Dosage Variation 57 Table 16 with Adsorbent Dosage Variation 58 Table 17 Adsorption of Acid Blue Dye from Aqueous Solution with Adsorbent Dosage Variation 59 Table 18 Adsorption of Acid Violet Dye from Aqueous Solution with Adsorbent Dosage Variation 60 Table 19 with Temperature Variation 64 Table 20 with Temperature Variation 65 Table 21 Adsorption of Acid Blue Dye from Aqueous Solution with Temperature Variation 66 Table 22 Adsorption of Acid Violet Dye from Aqueous Solution with Temperature Variation 67 Table 23 and from Dyeing Industrial Effluent using Blue-Green Algae and Commercial Activated Carbon 73 Table 24 and from Dyeing Industrial Effluent using Blue-Green Algae and Commercial Activated Carbon 74 Table 25 Adsorption of Acid Blue Dye from Aqueous Solution and from Dyeing Industrial Effluent using Blue-Green Algae and Commercial Activated Carbon 75 Table 26 Adsorption of Acid Violet Dye from Aqueous Solution and from Dyeing Industrial Effluent using Blue-Green Algae and Commercial Activated Carbon 76 Table 27 Lagergren Rate Equation for the Adsorption of Methylene Blue 81

9 Table 28 Lagergren Rate Equation for the Adsorption of Methyl Violet 82 Table 29 Lagergren Rate Equation for the Adsorption of Acid Blue 83 Table 30 Lagergren Rate Equation for the Adsorption of Acid Violet 84 Table 31 Lagergren Rate Equation for the Adsorption of Methylene Blue 87 Table 32 Lagergren Rate Equation for the Adsorption of Methyl Violet 88 Table 33 Lagergren Rate Equation for the Adsorption of Acid Blue 89 Table 34 Lagergren Rate Equation for the Adsorption of Acid Violet 90 Table 35 Methylene Blue 94 Table 36 Methyl Violet 95 Table 37 Acid Blue 96 Table 38 Acid Violet 97 Table 39 Methylene Blue Dye from Dyeing Industrial Effluent onto BGA 100 Table 40 Methyl Violet Dye from Dyeing Industrial Effluent onto BGA 101 Table 41 Acid Blue 102 Table 42 Acid Violet 103 Table 43 Elovich Rate Equation for the Adsorption of Methylene Blue 107 Table 44 Elovich Rate Equation for the Adsorption of Methyl Violet 108

10 Table 45 Elovich Rate Equation for the Adsorption of Acid Blue 109 Table 46 Elovich Rate Equation for the Adsorption of Acid Violet 110 Table 47 Elovich Rate Equation for the Adsorption of Methylene Blue 113 Table 48 Elovich Rate Equation for the Adsorption of Methyl Violet 114 Table 49 Elovich Rate Equation for the Adsorption of Acid Blue 115 Table 50 Elovich Rate Equation for the Adsorption of Acid Violet 116 Table 51 Langmuir Isotherm for the Adsorption of Methylene Blue 122 Table 52 Langmuir Isotherm for the Adsorption of Methyl Violet 124 Table 53 Langmuir Isotherm for the Adsorption of Acid Blue Dye 126 Table 54 Langmuir Isotherm for the Adsorption of Acid Violet Dye 128 Table 55 Langmuir Isotherm for the Adsorption of Methylene Blue 130 Table 56 Langmuir Isotherm for the Adsorption of Methyl Violet 132 Table 57 Langmuir Isotherm for the Adsorption of Acid Blue Dye 134 Table 58 Langmuir Isotherm for the Adsorption of Acid Violet Dye 136 Table 59 Freundlich Isotherm for the Adsorption of Methylene Blue 140 Table 60 Freundlich Isotherm for the Adsorption of Methyl Violet 142

11 Table 61 Freundlich Isotherm for the Adsorption of Acid Blue Dye 144 Table 62 Freundlich Isotherm for the Adsorption of Acid Violet Dye 146 Table 63 Freundlich Isotherm for the Adsorption of Methylene Blue 148 Table 64 Freundlich Isotherm for the Adsorption of Methyl Violet 150 Table 65 Freundlich Isotherm for the Adsorption of Acid Blue Dye 152 Table 66 Freundlich Isotherm for the Adsorption of Acid Violet Dye 154 Table 67 Thermodynamic Parameters for the Removal of from Aqueous Solution 158 Dyes

12 List of Figures Figure 1. with Variation of Initial Concentration of Methylene Blue Dye Solution 40 Figure 2. with Variation of Initial Concentration of Methyl Violet Dye Solution 40 Figure 3. Adsorption of Acid Blue Dye from Aqueous Solution with Variation of Initial Concentration of Acid Blue Dye Solution 41 Figure 4. Adsorption of Acid Violet Dye from Aqueous Solution with Variation of Initial Concentration of Acid Violet Dye Solution 41 Figure 5. Adsorption of Methylene Blue Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Methylene Blue Dye Solution 46 Figure 6. Adsorption of Methyl Violet Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Methyl Violet Dye Solution 46 Figure 7. Adsorption of Acid Blue Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Acid Blue Dye Solution 47 Figure 8. Adsorption of Acid Violet Dye from Dyeing Industrial Effluent with Variation of Initial Concentration of Acid Violet Dye Solution 47 Figure 9. with ph Variation 52 Figure 10. Adsorption of Acid Violet Dye from Aqueous Solution with ph Variation 52 Figure 11. with ph Variation 55 Figure 12. Adsorption of Acid Blue Dye from Aqueous Solution with ph Variation 55 Figure 13. with Adsorbent Dosage Variation 61 Figure 14. with Adsorbent Dosage Variation 61

13 Figure 15. Adsorption of Acid Blue Dye from Aqueous Solution with Adsorbent Dosage Variation 62 Figure 16. Adsorption of Acid Violet Dye from Aqueous Solution with Adsorbent Dosage Variation 62 Figure 17. with Temperature Variation 68 Figure 18. with Temperature Variation 68 Figure 19. Adsorption of Acid Blue Dye from Aqueous Solution with Temperature Variation 69 Figure 20. Adsorption of Acid Violet Dye from Aqueous Solution with Temperature Variation 69 Figure 21. and from Dyeing Industrial Effluent using BGA 70 Figure 22. and from Dyeing Industrial Effluent using BGA 71 Figure 23. Adsorption of Acid Blue Dye from Aqueous Solution and from Dyeing Industrial Effluent using BGA 71 Figure 24. Adsorption of Acid Violet Dye from Aqueous Solution and from Dyeing Industrial Effluent using BGA 72 Figure 25. Removal of Dyes from Aqueous Solution using BGA 77 Figure 26. Removal of Dyes from Aqueous Solution using CAC 77 Figure 27. Removal of Dyes from Dyeing Industrial Effluent using BGA 78 Figure 28. Removal of Dyes from Dyeing Industrial Effluent using CAC 78 Figure 29. Lagergren Rate Equation for the Adsorption of Methylene Blue 85 Figure 30. Lagergren Rate Equation for the Adsorption of Methyl Violet 85 Figure 31. Lagergren Rate Equation for the Adsorption of Acid Blue 86

14 Figure 32. Lagergren Rate Equation for the Adsorption of Acid Violet 86 Figure 33. Lagergren Rate Equation for the Adsorption of Methylene Blue 91 Figure 34. Lagergren Rate Equation for the Adsorption of Methyl Violet 91 Figure 35. Lagergren Rate Equation for the Adsorption of Acid Blue 92 Figure 36. Lagergren Rate Equation for the Adsorption of Acid Violet 92 Figure 37. Methylene Blue 98 Figure 38. Methyl Violet 98 Figure 39. Acid Blue 99 Figure 40. Acid Violet 99 Figure 41. Methylene Blue Dye from Dyeing Industrial Effluent onto BGA 104 Figure 42. Methyl Violet 104 Figure 43. Acid Blue 105 Figure 44. Acid Violet 105 Figure 45. Elovich Rate Equation for the Adsorption of Methylene Blue 111 Figure 46. Elovich Rate Equation for the Adsorption of Methyl Violet 111 Figure 47. Elovich Rate Equation for the Adsorption of Acid Blue Dye 112

15 Figure 48. Elovich Rate Equation for the Adsorption of Acid Violet Dye 112 Figure 49. Elovich Rate Equation for the Adsorption of Methylene Blue 117 Figure 50. Elovich Rate Equation for the Adsorption of Methyl Violet 117 Figure 51. Elovich Rate Equation for the Adsorption of Acid Blue Dye 118 Figure 52. Elovich Rate Equation for the Adsorption of Acid Violet Dye 118 Figure 53. Langmuir Isotherm for the Adsorption of Methylene Blue 123 Figure 54. Langmuir Isotherm for the Adsorption of Methyl Violet Dye 125 Figure 55. Langmuir Isotherm for the Adsorption of Acid Blue Dye 127 Figure 56. Langmuir Isotherm for the Adsorption of Acid Violet Dye 129 Figure 57. Langmuir Isotherm for the Adsorption of Methylene Blue 131 Figure 58. Langmuir Isotherm for the Adsorption of Methyl Violet Dye 133 Figure 59. Langmuir Isotherm for the Adsorption of Acid Blue Dye 135 Figure 60. Langmuir Isotherm for the Adsorption of Acid Violet Dye 137 Figure 61. Freundlich Isotherm for the Adsorption of Methylene Blue 141 Figure 62. Freundlich Isotherm for the Adsorption of Methyl Violet 143

16 Figure 63. Freundlich Isotherm for the Adsorption of Acid Blue Dye 145 Figure 64. Freundlich Isotherm for the Adsorption of Acid Violet Dye 147 Figure 65. Freundlich Isotherm for the Adsorption of Methylene Blue 149 Figure 66. Freundlich Isotherm for the Adsorption of Methyl Violet 151 Figure 67. Freundlich Isotherm for the Adsorption of Acid Blue Dye 153 Figure 68. Freundlich Isotherm for the Adsorption of Acid Violet Dye 155 Figure 69. Vant Hoff s Plot for the Removal of Methylene Blue Dye from Aqueous Solution 159 Figure 70. Vant Hoff s Plot for the Removal of Methyl Violet Dye from Aqueous Solution 159 Figure 71. Vant Hoff s Plot for the Removal of Acid Blue Dye from Aqueous Solution 159 Figure 72. Vant Hoff s Plot for the Removal of Acid Violet Dye from Aqueous Solution 159 Figure 73. FTIR Spectrum of the Adsorbent BGA 166

17 List of Abbreviations BGA - Blue-Green Algae CAC - Commercial Activated Carbon MB - Methylene Blue MV - Methyl Violet AB - Acid Blue AV - Acid Violet TSS - Total Suspended Solids TDS - Total Dissolved Salts BOD - Biological Oxygen Demand mg - milligram g - gram ml - milliliter K - Kelvin C - Degree Centigrade C.I - Colour Index ZnO - Zinc Oxide TiO2 - Titanium dioxide PAC - Powdered Activated Carbon GAC - Granular Activated Carbon SEM - Scanning Electron Microscope FTIR - Fourier Transform Infrared spectroscopy rpm - rotation per minute H2SO4 - Sulphuric acid NaOH - Sodium Hydroxide NO32- - Nitrate ion SO42- - Sulphate ion PO42- - Phosphate ion Cl- - Chloride ion

18 kjmol-1 - KiloJoule per mole Jmol-1K-1 - Joule per mole per Kelvin ΔG - Free Energy Change ΔH - Heat Energy Change ΔS - Entropy Change λ max - Wavelength CAS - Chemical Abstracts Service Sec - Second BET - Brunauer-Emmett-Teller nm - Nanometer µm - micrometer cm-1 - per centimeter mol-1 - per mole K - Kelvin Temperature kj - Kilo Joule KBr - Potassium Bromide m2 - Square meter mg/l - milligram per litre mg/g - milligram per gram 2 m /g - Square meter per gram N - Normality min-1 - per minute mm - millimeter

Equilibrium and Kinetics of Adsorption of Cationic Dyes by STISHOVITE Clay TiO2 Nanocomposite

Vol.2, Issue.6, Nov-Dec. 2012 pp-3989-3995 ISSN: 2249-6645 Equilibrium and Kinetics of Adsorption of Cationic Dyes by STISHOVITE Clay TiO2 Nanocomposite Venkateswaran Vinayagam 1, Priya Thangaraju 2 1