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Download (7MB) https://theses.gla.ac.uk/ Theses Digitisation: https://www.gla.ac.uk/myglasgow/research/enlighten/theses/digitisation/ This is a digitised version of the original print thesis. Copyright and moral rights for this work are retained by the author A copy can be downloaded for personal non-commercial research or study, without prior permission or charge This work cannot be reproduced or quoted extensively from without first obtaining permission in writing from the author The content must not be changed in any way or sold commercially in any format or medium without the formal permission of the author When referring to this work, full bibliographic details including the author, title, awarding institution and date of the thesis must be given Enlighten: Theses https://theses.gla.ac.uk/ [email protected] RADIOTRACER STUDIES OF THE FLUORINE BOND LABILITY OF SOME BINARY FLUORIDES. Thesis submitted to the University of Glasgow in fulfilment of the requirement of the degree of Doctor of Philosophy. by MOHAMMED FOUZI GHORAB M.Sc. Department of Chemistry University of Glasgow September, 19S8. ProQuest Number: 10998195 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest ProQuest 10998195 Published by ProQuest LLC(2018). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 4 8 1 0 6 - 1346 To my mother and father. ACKNOWLEDGEMENTS. I would like to thank my supervisor Dr. J.M. Winfield for all bis help and guidance during the course of this work. I would also like to thank my colleagues of the Fluorine Chemistry Group for their helpful discussions, Messrs. R.R. Spence and L. McGhee for their technical assistance, Messrs. W. McCormack and R. Wilson of the glass blowing workshop and Mrs. F. Lawrie and Mr. G. McCulloch of the infrared service for their cooperation. Many thanks are due to Mrs. L. Hughes for her efficient typing of this thesis. The nuclear facilities provided by Dr. J.E. Whitley and his colleagues at the Scottish Universities Research and Reactor Centre, East Kilbride, without which the present work would have been a much more difficult task, are gratefully acknowledged. My very special thanks go to my parents for their support and encouragement and my friends for their good company. Finally, I would like to acknowledge the financial support granted to me by the Ministry of Higher Education (M.E .S ) , Algeria. CONTENTS page ACKNOWLEDGEMENTS SUMMARY (i CHAPTER 1. INTRODUCTION 1 1.1 Preparation and Physical Properties of the 4 Hexafluorides of Molybdenum, Tungsten and Uranium. 1.2 Chemical Reactivity of the Hexafluorides of 5 Molybdenum Tungsten and Uranium. 1.3 Preparation of the Hepta-and Octa-fluoroanions 7 of Molybenum, Tungsten and Uranium. 1.4 Structures of the Hepta- and Octa-fluoroanions 7 of Molybdenum, Tungsten and Uranium. 1.5 Fluorine Bond Lability of the Hexafluorides of 11 Molybdenum, Tungsten, Uranium and their Derivatives. 1.6 Chemistry of Boron Trifluoride and the Penta- 14 Fluorides of Phosphorus and Arsenic. 1.7 Chemistry of Antimony Pentafluoride 17 1.8 Chemistry of the Pentafluorides of Niobium and 19 Tantalum 1.9 Lewis Acidity Order of Binary Fluorides 20 1.9.1 General Definitions 20 1.9.2 Lewis Acid-Base Definition 21 1.9.3 Lewis Acidity Order 22 CHAPTER 2 EXPERIMENTAL 2. 1 Equipment 25 2.1.1 Vacuum Line 25 2.1.2 Inert Atmosphere 25 2.1.3 Vibrational Spectroscopy 25 2.2 Preparation and Purification of Reagents 26 2.2.1 Purification of Acetonitrile 26 2.2.2 Purification of Diethylether 27 2.2.3 Preparation and Purification of Molybdenum 27 Hexafluoride 2.2.4 Preparation and Purification of Dinitrogen 28 Tetroxide 2.2.5 Preparation of Nitrosyl Fluoride 29 2.2.6 Preparation of Tris(dimethylamine)sulphonium 30 Difluorotrimethylsilicate 2.2.7 Preparation of Trimethylfluorosilane 31 2.2.8 Purification of the Pentafluorides of Niobium 31 and Tantalum 2.2.9 Preparation of Arsenic Pentafluoride- 32 Acetonitrile Adduct. 2.2.10 Preparation of Antimony Pentafluoride- 33 Acetonitrile Adduct 2.2.11 Preparation of Acetonitrile Adduct of the 34 Pentafluorides of Niobium and Tantalum 2.2.12 Preparation of Lithium Tetrafluoroborate, 35 Lithium H e x a f luorophosphate and Lithium Hexafluoroarsenate Preparation of Nitrosonium Hexafluoro- 36 phosphate and Nitrosonium Hexafluoroarsenate Preparation of Lithium Hexafluoroantimonate 36 Preparation of Lithium Hexafluoroniobate 37 Lithium Hexafluorotantalate and Copper(II) Hexafluoroniobate Pentakis Acetonitrile Preparation of Copper(II) Heptafluoro- 39 tungstate(VI) Pentakis Acetonitrile Preparation of Thallium(I) Heptafluoro- 39 tungstate(VI) Preparation of Nitrosonium Heptafluoro- AO tungstate(VI) Preparation of Caesium Heptafluorotungstate(VI) A 1 and Caesium Heptafluoromolybdate(VI) Activation of Caesium Fluoride A2 Radiochemical Techniques A3 Isotopic Exchange Reactions AA 1 ft [ F]-Fluorine as Radiotracer A? Counting Apparatus A9 50 Radioactive Decay Background 51 Statistical Errors 51 Radiochemical Balance 53 [18F]-Fluorine Reaction Vessels 55 Single-Limb Vessel 55 56 Double-Limb Vessel 57 Preparation of Radiolabelled Compounds 2.13.1 Preparation of [ 18 F]-Fluorine Labelled Caesium Fluoride 2.13.2 Preparation of [ 18F]-Fluorine Labelled Hexafluorides of Molybdenum, Tungsten and Uranium 18 2.13.3 Preparation of [ F]-Fluorine Labelled Boron Trifluoride Phosphorus Pentafluoride, Arsenic Pentafluoride and Trimethylfluorosilane 2.13.A Preparation of [18F]-Fluorine Labelled Lithium Hexafluorophosphate and Lithium Hexafluoro- arsenate 2.13.5 Preparation of [^8F]-Fluorine Labelled Nitrosyl Fluoride CHAPTER 3 REACTIONS OF THE HEPTAFLUQRQTUNGSTATE(VI) AND HEPTAFLUOROMOLYBDATE(VI) ANIONS WITH [18F]-FLUORINE LABELLED HEXAFLUORIDES OF MOLYBDENUM AND TUNGSTEN. 3.1 Introduction 3.2 Experimental 3.3 Reaction Between Thallium(I) Heptafluoro- 18 tungstate(VI) and [ F]-Fluorine Labelled Tungsten Hexafluoride in Acetonitrile 3.4 Reaction Between Copper(II) Heptafluoro- tungstate(VI) Pentakis Acetonitrile and 18 [ F]-Fluorine-Labelled Tungsten Hexafluoride 1R Reaction Between [ F]-Fluorine Labelled Nitrosonium Heptafluorotungstate(VI) and Tungsten Hexafluoride in Acetonitrile Reaction Between Nitrosonium Heptafluoro- 1R tungstate(VI) and [ F]-Fluorine Labelled Molybdenum Hexafluoride in Acetonitrile Reaction Between Caesium Heptafluoro- 1R tungstate(VI) and [ F]-Fluorine Labelled Molybdenum Hexafluoride in Acetonitrile Evidence For the Formation of Caesium Heptafluoromolybdate and Caesium Hepta- fluorotungstate Reaction Between Caesium Heptafluoro- molybdate (VI) and [^F]-Fluorine ■•Labelled Tungsten Hexafluoride in Acetonitrile Reaction Between Thallium(I) Heptafluoro- 1 Q tungstate(VI) and [ F]-Fluorine Labelled Tungsten Hexafluoride Under Heterogeneous Conditions. Reaction Between Copper(II) Heptafluoro- tungstate(VI) Pentakis Acetonitrile and [1®F]-Fluorine-Labelled Tungsten Hexafluoride Under Heterogeneous Conditions Reaction Between Nitrosonium Heptafluoro- tungstate(VI) and [18F]-Fluorine Labelled Tungsten Hexafluoride Under Heterogeneous Conditions 3.13 Reaction Between [^8 F]-Fluorine Labelled Nitrosonium Heptafluorotungstate(VI) and Tungsten Hexafluoride Under Heterogeneous Conditions. 3.14 Reaction Between Nitrosonium Heptafluoro- tungstate(VI) and [^8F]-Fluorine Labelled Molybdenum Hexafluoride Under Heterogeneous Conditions 3.15 Reaction Between Caesium Heptafluoro- molybdate(VI) and [ ^8F]-Fluorine Labelled Tungsten Hexafluoride Under Heterogeneous Conditions. 3.16 Reaction Between Nitrosonium Heptafluoro- tungstate(VI), Thallium(I) Heptafluoro- 1R tungstate(VI) and [ F]-Fluorine Labelled Uranium Hexafluoride Under Heterogeneous Conditions CHAPTER 4 HETEROGENEOUS REACTIONS BETWEEN ACTIVATED CAESIUM FLUORIDE, COPPER DIFLUORIDE, THALLIUM FLUORIDE AND [18F]-FLUORINE-LABELLED GASEOUS HEXAFLUORIDES OF MOLYBDENUM TUNGSTEN AND URANIUM. 4.1 Introduction 4.2 Experimental 4.3 Reaction Between Activated Caesium Fluoride 1R and [ F]-Fluorine Labelled Tungsten Hexa­ fluoride Under Heterogeneous Conditions Reaction Between Activated Caesium Fluoride 18 and [ F]-Fluorine Labelled Molybdenum Hexa­ fluoride Under Heterogeneous Conditions 4.5 Reaction Between Activated Caesium Fluoride 9 1 18 and [ F]-Fluorine Labelled Uranium Hexa­ fluoride Under Heterogeneous Conditions 4.6 Reaction Between Copper Difluoride and [18F] 93 Fluorine Labelled Hexafluorides of Molybdenum Tungsten and Uranium Under Heterogeneous Conditions. 1 R 4.7 Reaction Between Thallium Fluoride and [ F] 95 Fluorine Labelled Hexafluorides of Molybdenum Tungsten and Uranium Under Heterogeneous Conditions. CHAPTER 5 REACTIONS BETWEEN THE FLUQRQANIONS OF BORON, PHOSPHORUS, ARSENIC, ANTIMONY, NIOBIUM AND TANTALUM AND [18F]-FLUORINE LABELLED HEXAFLUORIDES OF MOLYBDENUM, TUNGSTEN AND URANIUM IN ACETONITRILE 5.1 Introduction q7 5.2 Experimental 99 5.3 Reaction Between Lithium Tetrafluoroborate and 100 1 ft [' F]-Fluorine Labelled Hexafluorides of Molybdenum, Tungsten and Uranium in Acetonitrile. 5.4 Reaction Between Lithium Hexafluorophosphate and 102 1 ft [ °f ]-Fluorine Labelled Hexafluorides of Molybdenum, Tungsten and Uranium in Acetonitrile.
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