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Lalzawnpuia (Chemistry).Pdf ION PAIR AND TRIPLE ION FORMATIONS OF SOME SELECTED COMPOUNDS IN AQUEOUS AND BINARY SOLUTIONS AT DIFFERENT TEMPERATURES A Thesis submitted in partial fulfilment of the requirements for the Degree of Doctor of Philosophy in Chemistry By LALZAWNPUIA Regd. No. : MZU/Ph.D./468 of 15/05/2012 DEPARTMENT OF CHEMISTRY SCHOOL OF PHYSICAL SCIENCES MIZORAM UNIVERSITY TANHRIL, AIZAWL- 796004 September, 2016 ION PAIR AND TRIPLE ION FORMATIONS OF SOME SELECTED COMPOUNDS IN AQUEOUS AND BINARY SOLUTIONS AT DIFFERENT TEMPERATURES A Thesis submitted in partial fulfilment of the requirements for the Degree of Doctor of Philosophy in Chemistry By LALZAWNPUIA Regd. No. : MZU/Ph.D./468 of 15/05/2012 DEPARTMENT OF CHEMISTRY SCHOOL OF PHYSICAL SCIENCES MIZORAM UNIVERSITY TANHRIL, AIZAWL- 796004 September, 2016 i MIZORAM UNIVERSITY (A central University under the Act of Parliament) Department of Chemistry School of Physical Sciences Tanhril Campus, Aizawl-796004, Mizoram Dr. N. Mohondas Singh Assistant Professor CERTIFICATE This is to certify that the thesis entitled “Ion pair and triple ion formations of some selected compounds in aqueous and binary solutions at different temperatures ” submitted by Mr.Lalzawnpuia , (Regd. No. : MZU/Ph.D./468 of 15/05/2012), for the degree of Doctor of Philosophy in Mizoram University, Aizawl, Mizoram, embodies the record of original investigations carried out by him under my supervision. He has been duly registered and the thesis presented is worthy of being considered for the award of the Ph.D. degree. This work has not been submitted for any degree in any other university. Dated: _________________ (N.MOHONDAS SINGH) Supervisor India: Ph. 0389-2330832 (0): Cell: 09612163894 Fax: 0389-2330834: Email: [email protected] ii Declaration of the Candidate Mizoram University September, 2016 I, Lalzawnpuia, hereby declare that the subject matter of this thesis is the record of work done by me, that the contents of this thesis did not form basis of the award of any previous degree to me or to do the best of my knowledge to anybody else, and that the thesis has not been submitted by me for any research degree in any other University/Institute. This is being submitted to the Mizoram University for the degree of Doctor of Philosophy in Chemistry. (LALZAWNPUIA) Candidate (PROF. DIWAKAR TIWARI) (Dr. N. MOHONDAS SINGH) Head Supervisor iii ACKNOWLEDGEMENT At first I feel tremendously excited and fortunate enough while expressing my deepest sense of gratitude and inner sentiments to my teacher and supervisor, Dr. N. Mohondas Singh, Assistant Professor, Department of Chemistry, Mizoram University. He deserves my thanks because he has not only guided me during the completion of research work but also motivated me, encouraged me and for his being dynamic and mesmerizing one. He gave me the freedom to pursue an interesting research as well as trusted me often times more than myself and never let me out of his office without a positive thought. Without his loving care, scrupulous guidance and precious supervision, it would not have been possible for me to bring the present contour to this thesis. I would like to convey my heartfelt thanks to Prof. Mahendranath Roy , Department of Chemistry, North Bengal University, India for giving me chance to visit and provided me with the necessary facilities, and thanks to his research group members for their kind help, valuable assistance and whole-hearted co-operation during my research work in North Bengal. I convey my heartfelt thanks to Mr. Lalhmingliana Hnamte , Department of Chemistry, Gov,t Zirtiri Residential Science college, Aizawl, Mizoram, and Dr. Muthukumaran R , former Head, Department of Chemistry, Mizoram University, for their immense advice, lucid explanation during consultation and continual inspiration during the course of my research work. My sincere gratitude to Prof. Diwakar Tiwari, Head, Department of Chemistry for the timely support and guidance throughout my course and providing research facilities for completion my research. I also express my profound sense of gratitude to all the teaching staff, Dr. Zodinpuia Pachuau, Dr. Raj Kumar Mishra, Dr.Ved Prakash singh, Dr. A. Bimolini iv Devi and non-teaching staff, Department of Chemistry, Mizoram University, for their helpful assistance and continual inspiration during the course of my research work. I express my gratitude to University Grant Commission (UGC) for providing financial support from ‘MZU-UGC Fellowship’ during the course of this research work. The encouragement, motivation and support given by Prof. R.C. Tiwari, Dean, School of Physical Sciences, Mizoram University is greatly acknowledged. My heartfelt thanks to my colleagues and friends, Mr. Lalrosanga, Ms. R. Lawmzuali, Mr.Premjit Singh, Ms. Olivia Lalmuanzuali, and others for their valuable co-operation and being a great source of help. My deepest gratitude to my family, Dad K.B.R.Bantawa, mom N.T.Sangpari, brothers Lallawmthanga (died in 17.05.16) & Vanlalhmingsanga, sisters Dr. Jessy Ngurthantluangi & Zonunsiami, wife Ramengliani Colney, daughter Lalengpuii and son Stefan Lalhriatzuala for their ceaseless inspiration, sincere help, constructive suggestion and whole-hearted cooperation, great forbearance, understanding, moral support and sacrifice in shapingmy Ph.D. thesis in the present form. Above all, I would like to acknowledge my heartiest thanks to the almighty God, who blessed, protected and guided me to overcome the problems and difficulties to complete this research work. (LALZAWNPUIA) v CONTENTS Title of the Thesis i Certificate ii Declaration of the Candidate iii Acknowledgement iv Contents vi CHAPTER-1. INTRODUCTION 1 1.1. Definition of ion-pairs and triple ions 2 1.2. Various types of interactions 4 1.3. Concept of ion pair and triple ion formation 6 1.4. Effect of shape and size 16 1.5. Solvation number 17 1.6. Limiting equivalent conductance and walden product 18 1.7. Limitation of the concept of ion pairs and triple ions 21 1.8. Scope of the study 22 CHAPTER-2. REVIEW 24 2.1. Conductometric method 24 2.2. Ion pair and triple ion formation in 2:1 complexes and 1:1 complexes 25 2.3. Solvent mixtures 37 2.4. Effects of pressure on the electrolytic conductance 39 2.5. Spectrophotometric/Spectroscopic method 40 CHAPTER-3. METHODOLOGY 46 3.1. Methods 46 3.2. Evaluation of limiting molar conductance ( Λ0) and association constant (K A) of electrolytic salts by Shedlovsky technique 47 3.3. Evaluation of limiting molar conductance ( Λ0) and association constant (K A) of electrolytic salts by Fuoss technique 49 T 3.4. Evaluation of limiting molar conductance of triple ion ( Λ0 ) and triple ion formation constant (K T) of electrolytic salts by Fuoss-Kraus technique 51 3.5. Evaluation of thermodynamic parameters 52 3.6. Calculation of walden product 53 3.7. Calculation of solvation number 54 3.8. Calculation of diffusion coefficient 55 3.9. Physical Measurements 55 3.9.1. Conductance measurements 55 3.9.2. Temperature control 55 3.9.3. Measurement of weights 55 3.9.4. Computations 56 3.10. Materials 57 3.10.1. Ligands 57 3.10.2. Preparation of compounds/ complexes 59 3.11. Elemental analysis of few complexes 63 CHAPTER-4. RESULTS AND DISCUSSIONS 64 4.1. Ion association of copper complexes in aqueous medium at different temperature: A conductance method. 64 4.1.1. Introduction 64 4.1.2. Experimental 65 4.1.2.1. Preparation of ligands and compounds 65 4.1.2.2. Conductivity measurements 65 4.1.3. Evaluation of limiting molar conductance and association constant 67 4.1.4. Evaluation of thermodynamic parameters 71 4.2. Study of N-[(benzoyl-amino)-thioxomethyl]-cystein metal (II) chloride complexes in aqueous medium at different temperatures. 73 4.2.1. Introduction 73 4.2.2. Experimental 74 4.2.2.1. Preparation of ligands and compounds 74 4.2.2.2. Conductivity measurements 74 4.2.3. Evaluation of limiting molar conductance and association constant 77 4.2.4. Evaluation of Thermodynamic parameters 80 4.3. Physico-chemical studies of some transition metal (II) chlorides in pure methanol and water and their binaries at different temperatures 83 4.3.1. Introduction 83 4.3.2. Experimental 84 4.3.2.1. Preparation of ligands and compounds 84 4.3.2.2. Conductivity measurements 84 4.3.3. Evaluation of limiting molar conductance, association constant, walden product and effective radius 92 4.3.4. Evaluation of Thermodynamic parameters 98 4.4. Ion Association and Solvation Behavior of Metal (II) Chlorides in Binary Mixtures of Methanol + Water: A Conductance Method 105 4.4.1. Introduction 105 4.4.2. Experimental 106 4.4.2.1. Preparation of ligands and compounds 106 4.4.2.2. Conductivity measurements 106 4.4.3. Evaluation of limiting molar conductance, association constant, walden product and effective radius 118 4.4.4. Evaluation of thermodynamic parameters 123 4.5. Association constant of 1-butyl-4-methylpyridinium hexafluorophosphate in binary solvent of methanol, acetonitrile and dimethylsulphoxide at different temperatures. 133 4.5.1. Introduction 133 4.5.2. Experimental 134 4.5.3. Evaluation of limiting molar conductance and association constant 141 4.5.4. Calculation of walden product 146 4.5.5. Evaluation of thermodynamic parameters 149 4.5.6. Evaluation of bond length, surface of electron density and electrostatic potential by using a computational software Gaussian 09W, Revision A.02 155 4.6. Association and solvation behavior of some ionic liquids ([emim]NO 3, [emim]CH 3SO 3, [emim]Tos) in pure and aqueous- tetrahydrofuran solutions at T = 298.15, 303.15 and 308.15K by physicochemical approach. 158 4.6.1. Introduction 158 4.6.2. Experimental 159 4.6.3. Evaluation of limiting molar conductivity ( Λ0), the association constant (KA), the distance of closest approach of ions (R),walden product ( Λ0η0) and Gibb’s energy change (∆G0).
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