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Armento William J 196905 Phd

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Armento William J 196905 Phd In presenting the dissertation as a partial fulfillment of the requirements for an advanced degree from the Georgia Institute of Technology, I agree that the Library of the Institute shall make it available for inspection and circulation in accordance with its regulations governing materials of this type. I agree that permission to copy from, or to publish from, this dissertation may be granted by the professor under whose direction it was written, or, in his absence, by the Dean of the Graduate Division when such copying or publication is solely for scholarly purposes and does not involve potential financial gain. It is under- stood that any copying from, or publication of, this dis- sertation which involves potential financial gain will not be allowed without written permission. 7/25/68 THE CHEMISTRY OF SEVERAL HYDROXOCHLOROPLATINATES(IV) AND THEIR USE IN THE ISOLATION OF CARRIER FREE PT 197 A THESIS Presented to the Faculty of the Graduate Division by W. Joseph Armento In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the School of Chemistry Georgia Institute of Technology May, 1969 THE CHEMISTRY OF SEVERAL HYDROXOCHLOROPLATINATES(IV) AND THEIR USE IN THE ISOLATION OF CARRIER FREE PT 197 Approval and Date Dr. C. E. Lai,-6 n Dr. D. J. Rorer/ -1 r/ (. - L1 Dr. (. C. White Dr. H., Nelcman§11._ Chairman. I wish to dedicate this thesis to my wonderful parents who have made tremendous sacrifices for me and who have worked so hard to see that I was able to reach this final goal. iii ACKNOWLEDGEMENTS This thesis submitted to the Georgia Institute of Technology describes research carried out in the Analytical Division of the Oak Ridge National Laboratory. The research was partially supported by the Oak Ridge Graduate Fellowship Program of the Oak Ridge Institute of Nuclear Studies (Oak Ridge Associated Universities) and was directed by a committee appointed by Dean Mario Goglia of the Georgia Institute of Technology Graduate School which was composed of Drs. H. M. Neumann and D. J. Royer of the School of Chemistry at the Georgia Institute of Technology, Dr. C. E. Larson, President of the Union Carbide Corporation Nuclear Division at the Oak Ridge Gaseous Diffusion Plant, and Dr. J. C. White of the Analytical Division of the Oak Ridge National Laboratory. I am very grateful for the kind and extremely selfless assistance of several people at the Laboratory. In particular I want to thank J. F. Emery who helped me in the use of the pneumatic tube facility at the Oak Ridge Research Reactor. Also I wish to thank W. J. Ross for his assistance in the laboratory which was sincerely appreciated. In addition I wish to include thanks to F. L. Moore whose wisdom 'hath' guided and to Dr. R. L. Hahn for the frequent and very iv enlightening discussions in the field of nuclear chemistry. The neutron generator was available to me mainly through the efforts of J. E. Strain who kept the generator operating through almost impossible situations. Mr. Strain must be thanked for this and even more so for the extra time he put in at the generator for me which was his own time and for which he was not duly compensated. Finally I wish to thank him for the 'morale support' during the bleak times in which accomplishments were nil. Thanks are due to Dr. J. C. White of the Oak Ridge National Laboratory for his valuable help which was often needed. His constant guidance provided the necessary direction for the work to be completed. Special thanks are due Dr. Henry M. Neumann, the Chairman of my Reading Committee, whose constant and continuous forebearance and encouragement coupled with the ablest guidance have helped the author to a final and completed goal. Finally I am grateful for his patience and understanding when progress was at a standstill. Finally I wish to thank the Graduate Division of the Georgia Institute of Technology for granting special permission to use blank pages at the end of chapters, to number pages in the center of the page, and to use figure captions as printed by the computer. V The Oak Ridge National Laboratory is operated by Union Carbide Corporation for the United States Atomic Energy Commission. vii TABLE OF CONTENTS Page ACKNOWLEDGEMENTS iii LIST OF ILLUSTRATIONS ix LIST OF TABLES xiii SUMMARY . xv Chapter I. INTRODUCTION 1 II. SPECIAL APPARATUS AND REAGENTS 9 Reagents Paper Chromatographic Techniques Column Chromatographic Techniques Neutron Irradiations Radiation Detection Apparatus Visible and Ultra - Violet Spectra III. OBSERVATIONS ON PALLADIUM CHEMISTRY 17 IV. OBSERVATIONS ON PLATINUM CHEMISTRY 37 V. SEPARATION OF PLATINUM(IV) COMPLEXES FROM ONE ANOTHER 69 Paper Chromatography Cellulose Column Chromatography VI. NUCLEAR AND RADIOCHEMISTRY OF PLATINUM OBSERVED 89 Irradiation with Thermal Neutrons Irradiation with Fast Neutrons Decay Characteristics of the Pt 197 Isotopes Measurement of the (n,2n) Cross Sections Catcher Foils vi ii VII. SEPARATION OF PT1976 165 VIII. MISCELLANEOUS OBSERVATIONS 181 Analysis for Sodium Nuclear and Radiochemistry of Palladium Iridium Chemistry Analyses of Alkali Metals IX. CONCLUSIONS AND RECOMMENDATIONS 203 Appendix A. PERTINENT DATA AND SAMPLE CALCULATIONS 211 Analyses Cross Sections B. LISTING OF COMPUTER PROGRAMS 227 C. EXAMPLES OF INPUT AND OUTPUT FOR THE COMPUTER PROGRAMS 273 D. DERIVATIONS OF EQUATIONS 299 Derivation of the R f Factor Derivation of the Equations for Calculating Cross Sections Derivation of Growth and Decay Equations Computation of Photopeak Areas Decay and Growth Corrections BIBLIOGRAPHY 323 VITA 331 ix LIST OF ILLUSTRATIONS 1. Cellulose Column Chromatography 13 2. Visible and Ultraviolet Spectrum of Tetrachloro- palladate(II) 21 3. Visible and Ultraviolet Spectrum of Hexachloro- palladate(IV) 22 4. Visible and Ultraviolet Spectrum of Hexahydroxo- palladate(IV) 31 5. Visible and Ultraviolet Spectrum of Tetrachloro- platinate(II) 41 6. Visible and Ultraviolet Spectrum of Hexachloro- platinate(IV) 42 7. Visible and Ultraviolet Spectrum of Hexahydroxo- platinate(IV) 49 8. Visible and Ultraviolet Spectrum of Dihydroxo- tetrachloroplatinate(IV) 50 9. Visible and Ultraviolet Spectrum of Hexachloro- platinate(IV) during Hydrolysis 63 10. Visible and Ultraviolet Spectrum of Tetrahydroxo- dichloroplatinate(IV) 64 11. Elution of Pt* from a Cellulose Column 83 12. Elution of Pt* from a Cellulose Column 84 13. Elution of Pt* from a Cellulose Column 85 x 14. Elution of Pt* from a Cellulose Column 86 15. Decay of Platinum Activity from a Thermal Neutron Irradiation 98 16. Platinum Activity from Thermal Neutrons 99 17. Platinum Activity from Thermal Neutrons 100 18. Platinum Activity from Thermal Neutrons 101 19. Platinum Activity from Thermal Neutrons 102 20. Platinum Activity from Thermal Neutrons 103 21. Platinum Activity from Thermal Neutrons 104 22. Platinum Activity from Thermal Neutrons 105 23. Platinum Activity from Thermal Neutrons 106 24. Platinum Activity from Thermal Neutrons 107 25. Platinum Activity from Thermal Neutrons 108 26. Platinum Activity from Thermal Neutrons 109 27. Platinum Activity from Thermal Neutrons 110 28. Platinum Activity from Thermal Neutrons 111 29. Gold Activity from Platinum 112 30. Gold Activity from Platinum 113 31. Gold Activity from Platinum 114 32.. Decay of Platinum Activity from 14 Mev Neutron Irradiation 118 33. Platinum Activity from 14 Mev Neutrons 119 34. Platinum Activity from 14 Mev Neutrons 120 35. Platinum Activity from 14 Mev Neutrons 121 36. Platinum Beta Activity 125 37. Platinum Beta Activity 126 xi 38. Decay Scheme Ft - Au Mass 197 128 39. Platinum Gamma Decay Plot 133 40. Platinum Gamma Decay Plot 134 41. Platinum Gamma Decay Plot 135 42. Platinum Gamma Decay Plot 136 43. Platinum Gamma Decay Plot 137 44. Gamma Spectrum of Pure Pt 197g Activity 139 45. Gamma Spectrum of Pure Pt197m Activity 140 46. Aluminum Activity from 14 Mev Neutrons 144 47. Aluminum Activity from 14 Mev Neutrons 145 48. Aluminum Beta Activity 147 49. Aluminum Beta Activity 148 50. Platinum 197g Beta Activity Versus Absorber Thickness 150 51. Platinum 197m and 197g Activities Versus Absorber Thickness 151 52. Platinum Foil Showing Mg27 and Na24 160 53. Platinum Foil Showing Na24 161 54. Aluminum Foil Possibly Showing Pt Gammas 162 55. Aluminum Foil Possibly Showing Pt Gammas 163 56. Elution of Gold Complexes from Cellulose Column 167 57. Elution of Pt 197g from Cellulose Column Showing Szilard - Chalmers Products 179 58. Gamma Spectra of Peaks in Figure 53 180 59. Graph of Standard Samples of Sodium Used in Sodium Analyses 183 xii 60. Graph of Standard Samples of Sodium Used in Sodium Analyses 184 61. Spectrum of Palladium Gamma Activity 189 62. Spectrum of Palladium Gamma Activity 190 63. Spectrum of Palladium Gamma Activity 191 64. Spectrum of Palladium Gamma Activity 192 65. Spectrum of Palladium Gamma Activity 193 66. Spectrum of Palladium Gamma Activity 194 67. Spectrum of Silver Activity in Palladium 195 68. Palladium Activity from 14 Mev Neutrons 197 69. Palladium Activity from 14 Mev Neutrons 198 70. Palladium Activity from 14 Mev Neutrons 199 71. Typical Gamma Ray 220 72. Definition of the Rf Factor for a Paper Strip 300 73. Illustration of the R f Factor for a Cellulose Column 302 LIST OF TABLES 1. Palladium Spectral Data 2. Platinum Spectral Data 65 3. Isotopes from the Thermal Neutron Activation of Platinum 92 4. Thermal Neutron Activity of Platinum 94 5. Fast Neutron Activity of Platinum 122 6. Sodium Analysis Data 185 7. Peak Intercepts 222 XV SUMMARY Some of the uses of a Szilard - Chalmers reaction to prepare a carrier free radioisotope or an isotopically enriched radioactive product are well known. The reaction utilizes the energy of a nuclear reaction in one of the atoms of a molecule to break a chemical bond in the molecule thus partially or completely freeing the atom.
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