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CHEMICAL EFFECTS of the RADIOACTIVE DECAY 76>77Kr

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CHEMICAL EFFECTS of the RADIOACTIVE DECAY 76>77Kr INIS-mf—8579 I I CHEMICAL EFFECTS OF THE RADIOACTIVE DECAY 76> 77Kr-*-76- 77Br REACTIONS OF RECOIL BROMINE IN THE GAS PHASE door Dirk de Jong t CHEMICAL EFFECTS OF THE RADIOACTIVE DECAY 76'77Kr •-»• 76/77Br REACTIONS OF RECOIL BROMINE IN THE GAS PHASE ACADEMISCH PROEFSCHRIFT TER VERKRIJGING VAN DE GRAAD VAN DOCTOR IN DE WISKUNDE EN NATUURWETENSCHAPPEN AAN DE UNIVER- SITEIT VAN AMSTERDAM OP GEZAG VAN DE RECTOR MAGNIFICUS DR. D.W. BRESTERS, HOOGLERAAR IN DE FACULTEIT DER WISKUNDE EN NATUURWETENSCHAPPEN, IN HET OPENBAAR TE VERDEDIGEN IN DE AULA DER UNIVERSITEIT (TIJDELIJK IN DE LUTHERSE KERK, INGANG SINGEL 411, HOEK SPUI) OP WOENSDAG 29 SEPTEMBER 1982 DES NAMIDDAGS TE 16.00 UUR DOOR DIRK DE JONG GEBOREN TE GRAFT 1982 Promotor : Professor Dr. D. Apers Co-referent: Professor Dr. N.M.M. Nibbering ISBN 90 6488 006 9 This work is part of the. research program of the National Institute for Nuclear Physics and High Energy Physics (NIKHEF, section K), made possible by financial support from the Founda- tion for Fundamental Research on Matter (FOM) and the Nether- lands Organisation for the Advancement of Pure Research (ZWO). Dankzij de medewerking van erg veel mensen is dit boekje met de daarin beschreven experimenten, gereed gekomen. Ik wil op deze plaats iedereen bedanken voor zijn enthousiasme, zijn inzet en zijn gastvrijheid gedurende de jaren, waarin dit onderzoek is verricht. CONTENTS CHAPTER I INTRODUCTION . 1 1.1 General introduction; Chemical effects of nuclear transformations 1 1.1.1 Chemical effects of radioactive decay 2 1.1.2 Generation of energetic bromine species . 3 1.2 Reactions of energetic species 7 1.3 Charge and kinetic energy of recoil ' Br species generated by decay of • ' Kr 9 1.4 Ion-molecule reactions in the gas phase, introduction 17 1.4.1 Charge exchange reactions 20 1.4.2 Clustering or solvation reactions 23 1.4.3 Proton transfer reactions 26 1.4.4 Nucleophilic substitution reactions 26 1.5 Purpose of the present investigation 27 CHAPTER II PRODUCTION OF RADIOISOTOPES AND EXPERIMENTAL PROCEDURES 29 2.1 Production of radioisotopes 29 2.1.1 Production of 76'77Kr 30 2.1.2 Preparation of CF3 Br of high specific activity 44 2.1.3 Production of krypton and bromine isotopes with the MEA linear accelerator 52 2.2 Preparation of the gas-mixtures and analysis 56 CHAPTER III THE- DECAY OF 76Kr AND 77Kr IN GASEOUS HALO- METHANES I; THE FORMATION OF CH3Br* Bf REACTION 76 77 OF Br AND Br WITH CH3Br AND CH3I 69 3.1 Introduction 69 3.2 Pure gaseous methyl bromide 69 ii 3.2.1 Results 69 3.2.2 Discussion 73 3.2.3 Additional evidence for the SN9 mechanism 77 3.3 Influence of n-donor bases on the CH^Br yields 80 3.3.1 H2S 80 3.3.1.1 Results 80 3.3.1.2 Discussion 83 3.3.2 CH3SH 89 3.3.3 CH3SCH3 91 3.3.4 H2Se 93 3.3.5 CH3OH 96 3.3.6 CH3OCH3 97 3.3.7 Influence of the glass wall on the exchange reaction with CH3Br 99 3.4 Influence of ir electron donor bases on the CH3Br* yield 100 3.4.1 Results 100 3.4.2 Discussion 107 3.4.3 Isotopic ratio in CH3Br* 113 3.5 Pure gaseous methyl iodide 114 76 77 3.5.1 The CH3 ' Br yield in pure gaseous methyl iodide 114 ?6 77 3.5.2 Effect of H2S on the CH3 ' Br yield in methyl iodide 117 123 3.6 Decay of Xe in gaseous methyl bromide and methyl iodide 118 CHAPTER IV THE DECAY OF 76Kr AND 77Kr IN GASEOUS HALOMETHANES 121 4.1 Introduction 121 82 80 4.2 Reactions of ' Br with halomethanes, a literature survey 121 76 77 4.3 Reactions of ' Br with fluoromethanes (CH3F, CH2F2, CHF3, CF4) 127 4.3.1 Results 127 4.3.2 Discussion 127 iii 76 77 4.4 Reactions of ' Br with CH3F: effects of scavengers and moderators 145 i 4.4.1 Results 145 i i 4.4.2 Discussion 154 76 77 4.5 Reactions of ' Br with CH3C1 165 4.5.1 Results 165 4.5.2 Discussion • 168 77 4.6 Hydrogen substitution by ' Br in CH3Br 173 4.6.1 Results 174 4.6.2 Discussion 174 4.7 Reactions of 76'77Br with the monohalo- methanes; general remarks 178 4.8 Reactions of 6f77Br in trifluoromethanes (CF4, CF3C1, CF3Br) 183 4.9 Influence of the storage temperature on the CH3Br* yield in CH3Br, CH3C1 and CH3F 187 4.10 Inorganic yield in 76'77Kr - 76'77Br decay experiments 189 80m 80 4.11 Decay of Br to Br in CH3F and CH3C1 193 ,: 4.11.1 Introduction 193 4.11.2 Results 194 4.11.3 Discussion 195 : CHAPTER V REACTIONS OF 76f77Br WITH PROPANE AND CYCLOPROPANE 198 5.1 Reactions of 76'77Br with propane 198 5.1.1 Introduction 198 5.1.2 Results 198 5.1.3 Discussion 200 5.2 Reactions of ' Br with cyclopropane 207 5.2.1 Introduction 207 5.2.2 Results 208 : 5.2.3 Discussion 212 iv 7fi 77 ft9 CHAPTER VI REACTIONS OP ENERGETIC /o'"'ö*Br ATOMS, PRODUCED VIA PROTON ACTIVATION OF GASEOUS SELENIUM COMPOUNDS 226 6.1 Introduction 226 6.2 Experimental procedures 228 6.3 Choice of the selenium target compound 231 6.4 76 77 82 Reactions of ' ' Br recoil atoms in halomethanes 235 6.4.1 Results 235 6.4.2 Discussion 241 CHAPTER VII EXCITATION LABELING OF SIMPLE ORGANIC MOLECULES WITH 76Br AND 77Br 245 REFERENCES 250 SUMMARY 265 SAMENVATTING 269 STELLINGEN 1. Het verschil in stabiliteit van de koolstof- halogeen binding in een met jodium of broom ge- merkte verbinding wordt,onder Min vivo" omstandig- heden niet alleen bepaald door het verschil in dissociatie energie. Stöoklin, G., Int. J. Appl. Rad. Isot. 28,131(1977) 2. De bepaling van het doorbraakvolume van adsorptie- buisjes door middel van de experimenteel te bepalen chromatografische parameters retentievolume en piekbreedte, leidt vaak tot een overschatting van dit doorbraakvolume bij luchtbemonstering. Namiesnik, J.t KozZowski, E., Fresenius. Zeitschr. Anal. Chemie 311,581(1982) Bertoni, G., Bruner, F., Libevti, A.t Perrinoa C.9 J. of Chrom. 203,263(1981) 3. Omdat de m-halogeen gesubstitueerde benzoëzuren en de hiervan afgeleide methylesters niet als een homologe reeks beschouwd kunnen worden, is de door Shiue et al. gegeven identifikatie van het m- astato gesubstitueerde benzoëzuur en het hiervan afgeleide methylester aan twijfel onderhevig. Shiue, G.Y., Meyer, G.J., Ruth, T.J., Wolf, A.P., J. of Lab. Comp. 18,1039(1980) 4. Het is onjuist de toepassing van kortlevende radio- nukliden niet te noemen in een leerboek over de toepassingen van kernfysika in de geneeskunde, dat anno 1981 werd gepubliceerd. Dyson, N.A. in "Introduction to nuclear* physios with application in medicine and biology" (1981) 5. De grote verschillen, welke gevonden zijn voor reakties van "thermische" Br ionen, gevormd via verval van mBr of via verval van Kr, met aro- maten in de gas fase, rechtvaardigen een nader onderzoek naar de invloed van CH,Br, dat in de ft Om Br experimenten in hoge percentages aanwezig is in het reaktiemengsel. Knust, E.J., Rep. KFA Jülich (Jül-1168), Ph.D. Thesis, Ch. 3.1 - 3.3 (1975) Coenen, H.H. Rep. KFA-Jülich (Jül-1950), Ph.D. Thesis, Ch. 3.4 (1979) 6. De identifikatie van radiolyse produkten - verkregen via radiolyse van verbindingen als haloalkenen en haloaromaten - welke alleen gebaseerd is op een retentietijd bepaald van een gaschromatografische analyse op een gepakte kolom, is absoluut onvol- doende; kombinatie met massaspektrometrie cjeeft vaak de vereiste aanvullende informatie. Pauwels, E.K.J, Ph.D. Thesis, Ch. 3.4 (1971) Linde, K.D. van der, Spoelstra-van Balen, S., Kaspersen, F.M., Louwrier, P.W.F., Lindner, L., Radioahimiaa Aota 24_,U7(1977) This work, Chapter VI 7. Bij de scheiding van organische arainen met behulp van reversed phase ionenpaar vloeistof chromato- grafie kan de daarbij dikwijls voorkomende aanzien- lijke piekassymetrie sterk gereduceerd worden door toevoeging van een alkylamine of een alkylammonium zout aan de mobiele fase. Op grond van het mechanisme voorgesteld door Sokolowski en Wahlund is echter erg moeilijkste verklaren, dat zowel tertiaire amines als guaternaire ammoniumzouten dit effekt teweeg zouden brengen. Sokolowski, A., Wahlund, K.G., J. Chrom. 189,299(1980) 8. Bij de bepaling van deuterium isotoop effekten in pyridines met behulp van pKa metingen houden Balaban et al. onvoldoende rekening met het feit dat de verontreinigingen in gedeutereerde en niet gedeute- reerde verbindingen kunnen verschillen. Balaban, A.T., Bota, A., Onioiu, B.C., Klatte, G., Eoussel, C, Metzger, J., J. Chem. Res. 44 (1982) 9. De formule, welke door Pilling/ Rice en Butler wordt gebruikt ter berekening van de afstand afhankelijkheid van de potentiële energie bij elektrontunneling is onjuist. Pilling, M.J., Rice, S.A., J. Phye. Chem 79,3035(1975) Butler, P.R., Pilling, M.J., Disc. Farad. Soa. 63,38 (1977) D. de JONG 1982 CHAPTER I INTRODUCTION 1.1 General Introduction Chemical effects of nuclear transformations Nuclear transformations as a consequence of particle or photon activation or radioactive decay, generally lead to product nuclei, which possess an excess of kinetic or recoil energy and which may be charged. The chemistry of such recoil species will often be Influenced to a large extent by these charge and energy effects. The recoil energy of the product nuclei arises from the emission of particles or photons from an excited nucleus and Its value Is determined by the laws of conservation of energy and momentum.
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