SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL

Emmanuel Nkemjika NKEMJIKA EMMANUEL 51 PAGES (8782 WORDS) Project
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SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL

 

A RESEARCH PROJECT

BY

 

NKEMJIKA, EMMANUEL EKE

12/SC/CH/256

 

SUBMITTED TO

 

DEPARTMENT OF CHEMISTRY

FACULTY OF SCIENCE

UNIVERSITY OF UYO, UYO

AKWA IBOM STATE

 

 

 

IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE AWARD OF BACHELOR OF SCIENCE (B.Sc.) DEGREE IN CHEMISTRY

                                         

 

 

  DECEMBER 2016

 

CERTIFICATION

          This is to certify that this project is an authentic record of work carried out by Nkemjika, Emmanuel Eke (12/SC/CH/256) of the Department of Chemistry, Faculty of Science, University of Uyo.

 

 

…………………………….                                                                       ……………………

      V. N. Mkpenie                                                                                        Date

         Supervisor

 

 

 

.............................................                                                                   ……………………….

    Dr. O. U. Abakedi                                                                                     Date

          Co-ordinator

 

 

 

……………………………….                                                                    ……………………

      Dr. A. U. Israel                                                                                                    Date

   Head of Department

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

DEDICATION

          This work is dedicated to my Mother Mrs. Ada Nkemjika from whom I have learned so much about the importance of love and family.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

ACKNOWLEDGEMENTS

            I wish to express my sincere gratitude to the Almighty God for His immense love, care, provision and protection all through the period of my study in school and the successful completion of my first degree programme.

I am grateful to my supervisor, V. N. Mkpenie for his good will and effort he put through to guide me specifically on the course of this project work. May God bless you and your family tremendously. I also acknowledge Dr.(Mrs.) A. S. Johnson, Dr. S. Simon and my lecturers Dr. B. I. Antia, Dr Akpan, and many of them who have been epitome of knowledge and being their student was an opportunity to learn from them not just academically but in character also. God bless you.

I would like to acknowledge my parent Mr./Mrs, Nkemjika Eke and my uncle Dr. M. Eke for their moral and financial support, they are the back bone behind my success. I pray God to continually Bless and sustain them to live and reap the fruits for the labour of love.

                       

 

 

 

 

 

 

 

 

 

 

 

ABSTRACT

The mixed ligand complex of Cobalt(II) and Iron(II) derived from 2-[(Z)-(2-hydroxybenzylidene)amino]phenol and 1-{(2E)-2-[(Z)-(2-hydroxyphenyl)imino]ethyl}-2-naphthol was synthesized and characterized based on the 1HNMR spectral studies and elemental analysis. The results of elemental analyses indicate a 1:1:1 stoichiometry of the ligands and the metal in the respective complexes. The 1HNMR spectra indicate the deprotonation of one of the two hydroxyl group on each ligand to form a mixed ligand complex with the metal ions.

 

 

Keywords: Mixed ligands, 1HNMR, Complex, Salicylaldehyde, 2-Hydroxy-1-                      naphthaldehyde, Schiff base.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

TABLE OF CONTENTS

                                                                                                                                                  Page

TITLE PAGE-  -           -           -           -           -           -           -           -           -           -           i

CERTIFICATION -      -           -           -           -           -           -           -           -           -           ii

DEDICATION -           -           -           -           -           -           -           -           -           -           iii

ACKNOWLEDGEMENTS-     -           -           -           -           -           -           -           -           iv

ABSTRACT-   -           -           -           -           -           -           -           -           -           -           v

TABLE OF CONTENTS-         -           -           -           -           -           -           -           -           vi

LIST OF TABLES-      -           -           -           -           -           -           -           -           -           ix

LIST OF FIGURES-     -           -           -           -           -           -           -           -           -           x

 

CHAPTER ONE

1.0         INTRODUCTION-                 -           -           -           -           -           -           -           1

1.1       Complexes-                 -           -           -           -           -           -           -           -           2

1.1.1    Tetrahedral complexes-           -           -           -           -           -           -           -           -           2

1.1.2    Octahedral complexes-            -           -           -           -           -           -           -           -           3

1.2       Ligands-           -           -           -           -           -           -           -           -           -           3

1.2.1    2-Hydroxy-1-naphthaldehyde derivatives-                  -           -           -           -           4

1.2.2    Salicylaldehyde derivatives-    -           -           -           -           -           -           -           4

1.3       Complexes of iron-      -           -           -           -           -           -           -           -           5

1.4       Complexes of cobalt-  -           -           -           -           -           -           -           -           6

1.5       Nuclear magnetic resonance (NMR) spectrometry-      -           -           -           -           7

1.6       Elemental analysis-      -           -           -           -           -           -           -           -           8

1.7       Aim and objectives of this research-    -           -           -           -           -           -           8

1.7.1    Aim of this research-   -           -           -           -           -           -           -           -           8

1.7.2    Objectives of this research-                 -           -           -           -           -           -           8

 

 

CHAPTER TWO

2.0         LITERATURE REVIEW-       -           -           -           -           -           -           -           10

CHAPTER THREE

3.0       MATERIALS AND METHODS-         -           -           -           -           -           -           17

3.1       Materials-         -           -           -           -           -           -           -           -           -           17

3.1.1    Apparatus-       -           -           -           -           -           -           -           -           -           17

3.1.2    Regents-           -           -           -           -           -           -           -           -           -           17

3.2       Methods-         -           -           -           -           -           -           -           -           -           17

3.2.1    Synthesis of 2-[(Z)-(2-hydroxybenzylidene) amino] phenol-  -           -           -           17

3.2.2    Synthesis of 1-{(2E)-2-[(Z)-(2-hydroxyphenyl) imino] ethyl}-2-naphthol-     -           18

3.2.3    Synthesis of the metal complex HBAP and HPEN-     -           -           -           -           18

3.6       Solubility test-  -           -           -           -           -           -           -           -           -           19

3.7       Melting point determination-    -           -           -           -           -           -           -           19

3.8       Proton NMR analyses- -           -           -           -           -           -           -           -           19

3.9       Elemental analysis-      -           -           -           -           -           -           -           -           20

CHAPTER FOUR

4.0       RESULTS AND DISCUSSION-           -           -           -           -           -           -           21

4.1       Synthesis of the Schiff bases and metal complexes-    -           -           -           -           21

4.1       Physical properties of the Schiff bases and complexes-          -           -           -           -           22

4.2       Elemental analysis -     -           -           -           -           -           -           -           -           24

4.3       Proton NMR spectra of the Schiff bases and complexes-                    -           -           -           24

CHAPTER FIVE

5.0       CONCLUSION AND RECOMMENDATIONS                       -           -           -           -           31

5.1       Conclusion-     -           -           -           -           -           -           -           -           -           31

5.2       Recommendations-      -           -           -           -           -           -           -           -           31

REFERENCES-            -           -           -           -           -           -           -           -           -           32

APPENDICES -           -           -           -           -           -           -           -           -           -           34

 

 

 

 

 

 

 

 

 

 

 

 

 

LIST OF TABLES

Tables                                                                                                                                   Pages              1.            Elemental analysis/Melting point data-             -           -           -           -           -           12

2.         Solubility data of the compounds-       -           -           -           -           -           -           12

3.         Physical properties of the compounds-            -           -           -           -           -           -           12

4.         Elemental analysis/Physical property of schiff bases L1H,  L2H          -           -           -           13

and their metal complexes

 

 5.        Physical properties of metals complexes and ligands- -           -           -           -           22

6.         Solubility of the metals complex and ligands in different solvents-    -           -           24

 7.        Elemental analysis data of the ligands and metal complexes-            -           -           24

 

 

 

 

 

 

 

 

 

 

 

LIST OF FIGURES

Figures                                                                                                                                           Pages

1.         1HNMR spectra of 2-[(Z)-(2-Hydroxybenzylidene)amino]phenol-    -           -           25

2.         The numbering of protons on 2-[(Z)-(2-Hydroxybenzylidene)amino]phenol-           26

3.         1HNMR spectra of 1-{(2E)-2-[(Z)-(2-hydroxyphenyl)imino]ethyl}-2-naphthol-       2

4.         The numbering of protons on 1-{(2E)-2-[(Z)-(2-hydroxyphenyl)imino]-       -           28

ethyl}-2- naphthol

 

5.         1HNMR spectra of Co(II) complex-   -           -           -           -           -           -           29

6.         The numbering of protons on Co(II) complex-           -           -           -           -           30


 

LIST OF APPENDICES

Appendices                                                                                                                        Pages

A.        Calculations showing how to obtain mass of reacting components-  -           -          35

B.        Elemental analysis calculations           -           -           -           -           -           -          37

C         The AAS spectra report sheet -           -           -           -           -           -           -          39

D.        The light microscope picture of the Schiff bases and the metal complexes   -          40         

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APA

Emmanuel, N (2020). SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL. Afribary.com: Retrieved November 25, 2020, from https://afribary.com/works/synthesis-and-1hnmr-characterization-of-co-ii-and-fe-ii-complexes-of-mixed-schiff-base-ligand-derived-from-salicylaldehyde-and-2-hydroxy-1-naphthaldehyde-with-2-aminophenol

MLA 8th

Nkemjika, Emmanuel. "SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL" Afribary.com. Afribary.com, 18 Jun. 2020, https://afribary.com/works/synthesis-and-1hnmr-characterization-of-co-ii-and-fe-ii-complexes-of-mixed-schiff-base-ligand-derived-from-salicylaldehyde-and-2-hydroxy-1-naphthaldehyde-with-2-aminophenol . Accessed 25 Nov. 2020.

MLA7

Nkemjika, Emmanuel. "SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL". Afribary.com, Afribary.com, 18 Jun. 2020. Web. 25 Nov. 2020. < https://afribary.com/works/synthesis-and-1hnmr-characterization-of-co-ii-and-fe-ii-complexes-of-mixed-schiff-base-ligand-derived-from-salicylaldehyde-and-2-hydroxy-1-naphthaldehyde-with-2-aminophenol >.

Chicago

Nkemjika, Emmanuel. "SYNTHESIS AND 1HNMR CHARACTERIZATION OF Co(II) AND Fe(II) COMPLEXES OF MIXED SCHIFF BASE LIGAND DERIVED FROM SALICYLALDEHYDE AND 2-HYDROXY-1-NAPHTHALDEHYDE WITH 2-AMINOPHENOL" Afribary.com (2020). Accessed November 25, 2020. https://afribary.com/works/synthesis-and-1hnmr-characterization-of-co-ii-and-fe-ii-complexes-of-mixed-schiff-base-ligand-derived-from-salicylaldehyde-and-2-hydroxy-1-naphthaldehyde-with-2-aminophenol