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TITLE
CERTIFICATE
ACKNOWLEDGEMENT
CONTENTS
PREFACE
LIST OF NOTATIONS AND ABBREVIATIONS
LIST OF TABLES
LIST OF FIGURES
1. INTRODUCTION AND SCOPE OF THE PRESENT INVESTIGATION
1.1 General Remarks on Yttrium and Lanthanides
1.2 Yttrium Among Lanthanides
1.3 Chemistry of Lanthanides
1.4 Coordination Chemistry of Lanthanides
Table 1.1 Comparison of transition metal ions and lanthanide ions.
1.5 Stereochemistry and Coordination Polyhedra
Fig. 1.1 Ideal polyhedra for various high coordination numbers.
1.6 Bonding in Lanthanide Complexes
1.7 Application of Complexes of Yttrium and the Lanthanides
1.8 Schiff base Complexes of Yttrium and Lanthanides: A Review
2. REAGENTS AND PROCEDURAL DETAILS
2.1 Reagents
2.1.1 Lanthanide oxides
2.1.2 Lanthanide salts
2.1.3 Solvents
2.1.4 The ligands
Fig. 2.1 4-N- (2-furfurylidene) aminoantipyrine.
Fig. 2.2 4-N- (2-thienylidene) aminoantipyrine.
2.1.5 Other reagents
Fig. 2.3 4-N- (5-nitro-2-thienylidene) aminoantipyrine.
2.2 Analysis of the Complexes
2.2.1 Estimation of the metal content
2.2.2 Estimation of the perchlorate content
2.2.3 Estimation of the iodide content
2.3 Physicochemical Methods Employed for the Characterization of the Complexes
2.3.1 Electrolytic conductance
Table 2.1 Molar conductance in some selected solvents.
2.3.2 Magnetic susceptibility
2.3.3 Electronic spectra
2.3.4 Infrared spectra
Nature of coordination of perchlorate ion
Fig. 2.4 Vibrations of perchlorate group as a function of symmetry.
Nature of coordination of the nitrate ion
Nature of coordination of iodide ion
2.3.5 Nuclear magnetic resonance spectra
2.3.6 Thermal studies
3. STUDIES ON YTTRIUM AND LANTHANIDE COMPLEXES OF 4-N-- (2-FURFURYLIDENE) AMINOANTIPYRINE
Fig. 3.1 4-N- (2-furfurylidene) aminoantipyrine.
EXPERIMENTAL
3.1 Preparation of Complexes
3.1.1 Yttrium and lanthanide perchlorate complexes of FAA
3.1.2 Yttrium and lanthanide nitrate complexes of FAA
3.1.3 Yttrium and lanthanide iodide complexes of FAA
3.2 Results and Discussion
3.2.1 Electrolytic conductance
3.2.2 Magnetic susceptibility
3.2.3 Infrared spectra
Perchlorate complexes
Nitrate complexes
Iodide complexes
3.2.4 Proton NMR spectra
3.2.5 Electronic spectra
3.3 Summary and Conclusion
Perchlorate complexes
Fig. 3.2 Tentative structure of lanthanide perchlorate complexes of FAA.
Nitrate complexes
Fig. 3.3 Tentative structure of lanthanide nitrate complexes of FAA.
Iodide complexes
Fig. 3.4 Tentative structure of lanthanide iodide complexes of FAA.
4. STUDIES ON YTTRIUM AND LANTHANIDE COMPLEXES OF 4-N- (2-THIENYLIDENE) AMINOANTIPYRINE
Fig. 4.1 4-N- (2-thienylidene) aminoantipyrine.
EXPERIMENTAL
4.1 Preparation of Complexes
4.2 Results and Discussion
4.2.1 Electrolytic conductance
4.2.2 Magnetic susceptibility
4.2.3 Infrared spectra
4.2.4 Proton NMR spectra
4.2.5 Electronic spectra
4.3 Summary and Conclusion
Fig. 4.2 Tentative structure of lanthanide perchlorate complexes of TAA.
5. STUDIES ON YTTRIUM AND LANTHANIDE COMPLEXES OF 4-N- (5-NITRO-2-THIENYLIDENE) AMINOANTIPYRINE
Fig. 5.1 4-N- (5-nitro-2-thienylidene) aminoantipyrine.
EXPERIMENTAL
5.1 Preparation of Complexes
5.2 Results and Discussion
5.2.1 Molar conductance
5.2.2 Magnetic susceptibility
5.2.3 Infrared spectra
5.2.4 Proton NMR spectra
5.2.5 Electronic spectra
5.3 Summary and Conclusion
Fig. 5.2 Tentative structure of lanthanide perchlorate complexes of NTA.
6. THERMAL STUDIES OF YTTRIUM AND LANTHANIDE COMPLEXES OF SOME SCHIFF BASES
6.1 Introduction
Thermogravimetry (TG)
Differential Thermal Analysis (DTA)
(a) Phenomenological aspects
(b) Kinetic aspects
(c) Mechanistic studies
Table 6. 1 commonly used ?? forms solid state reactions. reactions.
6.2 Experimental
6.2.1 Preparation of the ligand and complexes
6.2.2 Instrumentation
6.3 Results and Discussion
6.3.1 Phenomenological aspects
Yttrium and lanthanide perchlorate complexes of FAA
Yttrium and lanthanide nitrate complexes of FAA
Yttrium and lanthanide iodide complexes of FAA
Yttrium and lanthanide perchlorate complexes of TAA
Yttrium and lanthanide perchlorate complexes of NTA
Comparison of the thermal behaviour of the three series of complexes of FAA
Comparison of the perchlorate complexes of FAA, TAAand NTA
6.3.2 Kinetic studies
Yttrium and lanthanide perchlorate complexes of FAA
Yttrium and lanthanide nitrate complexes of FAA
Yttrium and lanthanide iodide complexes of FAA
Yttrium and lanthanide perchlorate complexes of TAA
Yttrium and lanthanide perchlorate complexes of NTA
6.3.3 Mechanism of the thermal decomposition reaction
6.3.4 Summary and Conclusion
7. SUMMARY
TABLES AND FIGURES
Table 3.1 Analytical data of yttrium and lanthanide perchlorate complexes of FAA.
Table 3.2 Analytical data of yttrium and lanthanide nitrate complexes of FAA.
Table 3.3 Analytical data of yttrium and lanthanide iodide complexes of FAA.
Table 3.4 Molar conductance and magnetic moment data of yttrium and lanthanide perchlorate complexes of FAA.
Table 3.5 Molar conductance data of yttrium and lanthanide nitrate complexes of FAA.
Table 3.6 Molar conductance and magnetic moment data of yttrium and lanthanide iodide complexes of FAA.
Table 3.7 Magnetic data of the yttrium and lanthanide nitrate complexes of FAA.
Table 3.8 Important infrared spectral bands of FAA and its yttrium and lanthanide perchlorate complexes.
Table 3.9 Important infrared spectral bands of FAA and its yttrium and lanthanide nitrate complexes.
Table 3.10 Important infrared spectral bands of FAA and its yttrium and lanthanide iodide complexes.
Table 3.10a Electronic spectral bands of FAA and its yttrium and lanthanide perchlorate complexes
Table 3.11 Electronic spectral bands of FAA and itsyttrium and lanthanide nitrate complexes
Table 3.12 Electronic spectral bands of FAA and its yttrium and lanthanide iodide complexes.
Table 3.13 Important proton NMR bands of the perchlorate complexes of yttrium and lanthanides with FAA.
Table 3.14 Important proton NMR bands of the nitrate complexes of yttrium and lanthanides with FAA.
Table 3.15 Important proton NMR bands of the iodide complexes of yttrium and lanthanides with FAA.
Table 4.1 Analytical data of yttrium and lanthanide perchlorate complexes of TAA.
Table 4.2 Molar conductance data of yttrium and lanthanide perchlorate complexes of TAA.
Table 4.3 Important infrared spectral bands of TAA and its yttrium and lanthanide perchlorate complexes.
Table 4.4 Electronic spectral bands of TAA and its yttrium and lanthanide perchlorate complexes.
Table 4.5 Important proton NMR bands of the perchlorate complexes of yttrium and lanthanides with TAA.
Table 5.1 Analytical data of yttrium and lanthanide perchlorate complexes of NTA.
Table 5.2 Molar conductance and magnetic moment data of yttrium and lanthanide perchlorate complexes of NTA.
Table 5.3 Important infrared spectral bands of NTA and its yttrium and lanthanide perchlorate complexes.
Table 5.4 Electronic spectral bands of NTA and its yttrium and lanthanide perchlorate complexes.
Table 5.5 Important proton NMR bands of the perchlorate complexesof yttrium and lanthanum with NTA (in 6 scale w.r. to TMS)
Table 6.2 Phenomenological data for the thermal decomposition of the perchlorate complexes of FAA.
Table 6.3 Phenomenological data for the thermal decomposition of the nitrate complexes of FAA.
Table 6.4 Phenomenological data for the thermal decomposition of the iodide complexes of FAA.
Table 6.5 Phenomenological data for the thermal decomposition of the first and second stages of the perchlorate complexes of TAA.
Table 6.6 Phenomenological data for the thermal decomposition of important stage of the perchlorate complexes of NTA.
Table 6.7 Correlation coefficients computed using the nine forms of g (a) for yttrium and lanthanide perchlorate complexes of FAA.
Table 6.8 Correlation coefficients computed using the nine forms of g (a) for yttrium and lanthanide nitrate complexes of FAA.
Table 6.9 Correlation coefficients computed using the nine forms of g (a) for yttrium and lanthanide iodide complexes of FAA.
Table 6.10 Correlation coefficients computed using the nine forms of g (a) for the first stage of the yttrium and lanthanide perchlorate complexes of TAA.
Table 6.11 Correlation coefficients computed using the nine forms of g (a) for the second stage of the yttrium and lanthanide perchlorate complexes of TAA.
Table 6.12 Correlation coefficients computed using a nine forms of g () for yttrium and lanthanide perchlorate complexes of NTA
Table 6.13 Kinetic parameters of the first stage thermal decomposition of yttrium and lanthanide perchlorate complexes of FAA
Table 6.14 Kinetic parameters of the (first stage) thermal decomposition of yttrium and lanthanide nitrate complexes of FAA.
Table 6.15 Kinetic parameters of the (first stage) thermal decomposition of yttrium and lanthanide iodide complexes of FAA.
Table 6.16 Kinetic parameters of the (first stage) thermal decomposition of yttrium and lanthanide perchlorate complexes of TAA.
Table 6.17 Kinetic parameters of the (first stage) thermal decomposition of yttrium and lanthanide perchlorate complexes of NTA.
Fig. 6.1 TG and DTG curves of [Ln (FAA) 3 (CIO4) 2] (CIO4) complex
Fig. 6.11 TG and DTG curves of [Ln (FAA) (N03) 2] (NO3) to 6.20
Fig. 6.21 IG and DTG curves of [Ln (FAA) 312]I. to 6.30
Fig. 6.31 TG and DTG curves of [Ln (TAA) 3 (C104) ] (C104) 2 to 6.40
Fig. 6.51 log (g (a) /T2] Vs 1000/T plots for the to 6.60 thermal decomposition of the first stage of (tn (FAA) 3 (C104) 2] (C104)
Fig. 6.61 log[g (a) /T2] Vs 1000/T plots for the to 6.70 thermal decomposition of the first stage of [Ln (FAA) (N03) 2] (N03)
Fig. 6.71 log[g (a) /T2] Vs 1000/T plots for the to 6.80 thermal decomposition of the first stage of [Ln (FAA) 312]1
Fig. 6.81 log[g (a) /T2] Vs 1000/T plots for the to 6.90 thermal decomposition of the first stage of [tn (TAA) 3 (C104) ] (C104) 2
Fig. 6.91 log[g (a) /T2] Vs 1000/T plots for the to 6.100 thermal decomposition of the second stage of [Ln (TAA) 3 (C104) ] (C104) 2
Fig. 6.101 log[g (a) /T2] Vs 1000/T plots for the to 6.110 thermal decomposition of the first stage of [Ln (NTA) 2 (C104) 2] (C104)
REFERENCES