DOCTOR OF PHILOSOPHY IN CHEMISTRY

Transcription

1 STUDIES ON NEW REAGENTS FOR THE SPECTROPHOTOMETRIC DETERMINATION OF ANIONS, METAL IONS AND DRUGS A THESIS SUBMITTED FOR THE DEGREE OF DOCTOR OF PHILOSOPHY IN CHEMISTRY TO THE FACULTY OF SCIENCE AND TECHNOLOGY OF MANGALORE UNIVERSITY BY Mr. CHAND PASHA DEPARTMENT OF POST- GRADUATE STUDIES AND RESEARCH IN CHEMISTRY MANGALORE UNIVERSITY MANGALAGANGOTHRI INDIA September

2 TO MY BELOVED PARENTS, BROTHERS, SISTERS, WIFE, SUFI & MAHIN 2

3 CONTENTS Page No DECLARATION i CERTIFICATE ii ACKNOWLEDGEMENT iii SUMMARY vi CHAPTER 1: INTRODUCTION TO SPECTROPHOTOMETRY 14 CHAPTER 2: SPECTROPHOTOMETRIC DETERMINATION OF IODATE 32 IN IODIZED TABLE SALT AND SEA WATER SAMPLES CHAPTER 3: SPECTROPHOTOMETRIC DETERMINATION OF 61 HYPOCHLORITE IN ENVIRONMENTAL SAMPLES CHAPTER 4: NEW REAGENTS FOR THE SPECTROPHOTOMETRIC 85 DETERMINATION OF VANADIUM IN ALLOYS, SYNTHETIC AND PHARMACEUTICAL SAMPLES CHAPTER 5: SPECTROPHOTOMETRIC DETERMINATION OF CHROMIUM 123 USING TOLUIDINE BLUE AND SAFRANINE O AS NEW REAGENTS CHAPTER 6: SPECTROPHOTOMETRIC DETERMINATION OF ARSENIC 158 IN ENVIRONMENTAL AND BIOLOGICAL SAMPLES 3

4 CHAPTER 7: SPECTROPHOTOMETRIC DETERMINATION OF SELENIUM 186 IN ENVIRONMENTAL, BIOLOGICAL AND PHARMACEUTICAL SAMPLES. CHAPTER 8: SPECTROPHOTOMETRIC DETERMINATION OF 213 CEPHALOSPORINS IN PHARMACEUTICAL SAMPLES CHAPTER 9: SPECTROPHOTOMETRIC DETERMINATION OF MOSAPRIDE 247 BY DIAZOTIZATION METHOD LIST OF PUBLICATIONS 4

5 DECLARATION I hereby declare that the matter presented in this thesis is the result of investigations carried out by me in the Department of Post-Graduate Studies and Research in Chemistry, Mangalore University, Mangalagangothri , Karnataka, India, under the guidance of Dr. B. Narayana, Professor of Chemistry, Mangalore University and the same has not previously formed the basis for the award of any degree or diploma. Whenever the work described is based on the findings of other researchers, due acknowledgement is made in keeping with the general practice of reporting scientific observations. However, errors and unintentional oversights, if any are regretted. Place: Mangalore University Date: 23 rd September 2008 Chand Pasha 5

6 MANGALORE UNIVERSITY DEPARTMENT OF CHEMISTRY [Post- Graduate Studies and Research] Phone: (O) MANGALAGANGOTHRI Fax : KARNATAKA, INDIA nbadiadka@yahoo.co.uk Dr. B. Narayana Ref. MU/CHEM/BN/ Professor of Chemistry Date: September 2008 CERTIFICATE This is to certify that this thesis entitled STUDIES ON NEW REAGENTS FOR THE SPECTROPHOTOMETRIC DETERMINATION OF ANIONS, METAL IONS AND DRUGS submitted by Sri. Chand Pasha to the Faculty of Science and Technology of Mangalore University for the award of the degree of Doctor of Philosophy in Chemistry is the result of bona fide research work carried out by him in the Department of Post Graduate Studies and Research in Chemistry, Mangalore University under my guidance and direct supervision. I further certify that this thesis or part thereof has not previously formed the basis for the award of any degree, diploma, associate ship of any other University or Institution. Dr. B. Narayana 6

7 ACKNOWLEDGEMENT It gives me a great pleasure to place on record my deep sense of gratitude and heartfelt thanks to my supervisor Dr. B. Narayana, Professor, Department of Post- Graduate Studies and Research in Chemistry, Mangalore University, Mangalagangothri, who gave me a chance to work with him, extended all facilities, sustained interest in me and provided inspiring guidance for the successful completion of my research work. I deem it as my privilege to work under his able guidance. I ever remain grateful to him. I am thankful to Prof. J. Ishwara Bhat, Chairman, Department of Post Graduate Studies and Research in Chemistry, Mangalore University for providing me an opportunity and making available the department facilities. The inspiration, help and suggestions received from Prof. A. M. Abdul Khader, Prof. B. Thimme Gowda, Prof. Balakrishna Kalluraya, Dr. Suresh P Nayak, Dr. B. Vishalakshi, Dr. Boja Poojary, Dr. Jagadeesh Prasad and all other staff members are beyond evaluation. I wish to express my sincere thanks to my colleague Dr. B. K Sarojini, Professor & Head, Department of Chemistry, P. A. College of Engineering, Nadupadav, Mangalore, for the support and constant encouragement extended throughout the investigations. I am thankful to Prof. Syed Akheel Ahmed, Vice Chancellor, Yenepoya University, Mangalore, Prof. K. Basavaiah, Prof. P. G. Ramappa and the faculty members of the Department of Post Graduate Studies and Research in Chemistry, Mysore University for the moral support and constant encourangement extended throughout the investigation. I also record my appreciation to the senior researchers and fellow researchers of our group, Dr. A. Joseph, Dr. R. A Nazareth, Dr. N. V. Sreekumar, Dr. N. G. Bhat, Dr. Tom Cherian, Dr. M. Mathew, Dr. K. K Vijay Raj, Dr. B. V. 7

8 Ashalatha, Sri. K. Sunil, Smt. K. Veena, Smt. T. V. Sreevidya and Sri. S. Samshuddin for their pleasant association and help in various forms. My thanks are also to Dr. N. S. Rai, Sri. M. Ashok and Sri. V. Prakash for their timely help and association. I remain grateful to the Head, Microtron Centre of Mangalore Univesity for permitting me to use the spectrophotometer and I thank Dr. Ganesh and Sri. Dayanand for providing all the assistance during the spectrophotometric analysis of the metal cations and anions. I was fortunate enough to avail the ungrudging help and assistance from all our laboratory and non-teaching staff particularly, Sri. M. Manohar and Sri. Chitharanjan. I am thankful to the librarian Dr. M. K. Bhandi, Asst. librarian Dr. N. V. Gowda and staff of Mangalore University Library for their valuable co-operation. I express my sincere thanks to the Director of Computer Centre, Mangalore University, and the staff of the computer centre for the computer facilities. I wish to express my heartful thanks to Dr. S. A. Khan, Principal, P. A. College of Engineering, Nadupadav, Mangalore, for his continuous support and constant encourangement extended throughout the investigation. I also wish to express my thanks to my other colleagues Sri Abdulla K. P, Sri. Mohd. Eliyas, Sri. U. Farroq, Smt. Suhana, Sri. Hakeem and Sri. Kiran of P. A. College of Engineering, Nadupadav, Mangalore. I am thankful to Dr. Mohammed Asif, Professor and Head, Department of Biotechnology, P. A. College of Engineering, Nadupadav, Mangalore, for his support and constant encourangement extended throughout the investigation. 8

9 I am grateful to Sri. Saleem Ahmed (Gust Faculty, CPDM, I.I.Sc. Bangalore), Sri. Abhishek, Sri. Wilson (J. H. Bio, Bangalore), Smt. Sunitha (Delnet, Delhi) and Staffs of I.I.Sc. Library, Bangalore for their support I received at various stages of the investigations. I also thank to my Brothers (Sri. Ghaffar Jan, Aleem Pasha and Afsar Nadeem) for their special interest, love and affection. At this juncture I think of my Parents, Brothers and Sisters with profound sense of gratitude whose selfless sacrifice and their great efforts with pain and tears and unceasing prayers has enabled me to reach the present position in life, I express my sincere thanks to my beloved wife Mrs. Shabreen Taj and little darlings Mohd. Sufiyan Pasha and Noor Maheen Taj, who have been a source of inspiration to me. Her loving concern, care, understanding and sacrifice made my task much easier. Words fail me to express the sort of heavenly benediction they have been to me. Finally I thank all those who have helped me directly or indirectly in the successful completion of my thesis. Above all I humbly thank God Almighty, whose sustaining grace has been sufficient for me to complete this endeavor. CHAND PASHA 9