As a part of the Agency's programme to promote regional and international exchange of informations, a Study Group Meeting on Radioisotope Production

Transcripción

1 F O R E W O R D As a part of the Agency's programme to promote regional and international exchange of informations, a Study Group Meeting on Radioisotope Production for the Latin-American Region was held in Sao Paulo, Brazil, on 6-10 October 1969» by

2 ALL PLEASE BE AWARE THAT

3 W.K. Eister and P. Richards: Radi pharmaceutical* and Short-Liv - - isotopes (U.S.A.)... "... *" l6l...

4 CONTENTS FOREWORD... Ill I. RADIOISOTOPE PRODUCTION PROGRAMMES W.C. Parker, W.J. Rose and G. Chuchani: The Radiochemistry Programmes at the Instituto Venezolano

5 RADIOISOTOPE PRODUCTION PROGRAMMES

6 THE RADIOCHEHISTRY PROGRAMMES AT TÍIE INSTITUTO VENEZOLANO DE INVESTIGACIONES CIENTÍFICAS* W. C. Parker**, W. J. Ross and G. Chuchani Química Nuclear Sección Química Instituto Venezolano

7 (5) Future Programmes. Major efforts

8 1. INTRODUCTION; The nuclear chemistry department, IVIC, comprises three laboratories, namely, radiochemistry, activation analysis and radiocarbon dating.

9

10 activity

11 a period of four to five weeks. to study For this reason it was decided

12 of electron spin resonance, x-ray diffraction and I. R. spectrometry. Although

13 the influence

14 E. Elcctrodcposition of The electrodeposition of 252 Cf is also the subject of investigation based on the sane lines as for 237 Np. Obviously, the economic preparation of thin layers of tms material will make possible many interesting experiments. This work will

15 charged with the parent material, the eluant passes through two bacteriological filters (size 0.22 y), the first above and the second below the column packing material, thus eluting a sterile daughter product. The effectiveness of the device was tested using a carrier-free activity of 99 Mo, obtained by recoil enrichment method.

16 demico".

17 Another phase of this iodine-deficient problem has been investigated

18 initiated with the researchers in the Physics Section of IVIC. These investigators

19 adsorption

20 vents

21 from

22 storage period should

23 of

24 At this time, the Directive Council of IVIC is negociating with the appropriate governmental authorities for official recognition of IVIC as an institution capable of granting advanced degrees and diplomas. FIGURE CAPTIONS Fig.

25 /' ^i5s ii 55, 1'"^?i;^.í I'^EV, " : - ".!,'. '».''«'.? ''.''.. ' ',./.-';{.. v?fr : 'íií?.^-' l^' ^^'/V u '^i.' '" $, ^>K, > '..i;..?.'.jk&:'.*"" '-. :\. to to

26 * * * to CO Fig *

27 Pig. 3

28 TABLE

29 TABLE II ACETA?IIDE PROPONAMIDE MALONAMIDE UREA N- METHYL N-N 1 -DIMETHYL UREA TABLE III Indicator Type 43 C

30 All APPENDIX I

31 Three - glove boxes (S-35, P-32/33 and Cf-252)..

32 1. M. Colonomos PUBLICATIONS PRESENT

33 6. H. Groning, W. Parker, J. Pérez-Alarcón and O. Linde. STUDIES

34 11.

35 ?KGGRA.»A DE PHwJUCCiON b na2;ioióo A Xf > U > ^.K K.&1CO A. h. ;w.íu'lf<w K.-

36 z6

37 agregados marcados

38

39 Potasio

40 Kriptón - 83m Blanco; Se0 2 B.Á. Tiempo de irradiación; 1 hora Flujo; V x n/'cm 2 seg Áct. específica; ^ 1 mci/gr Se Planes futuros:- üns vez i ue les instalación- s de procssamien. to estén terminadas, se planea llevar al cuo la producción de los siguien^&s radioisótopos; ^8Au coloidal, ^ho, * ría, K, 82 Br, 51er, 6* Cu y

41 ^ «*<* tof>0«> i

42 lí It "* *«c.s su: ráíico U

43 c; «\ 1 a?. 41 c-vño

44 RADIOISOTOPE PRODUCTION

45 areas is relatively well established. However, there is much work yet to be done to adapt these products to the developing applications; and this work is expected to continue at an increasing pace for many years. While neutron products

46 containing about

47 from Hanford graphite reactors.

48 secondary reaction

49 greatest interest today is that regarding radiopharmaceuticals. While to date in the United States this has been controlled in part by the Atomic Energy Commission, in time the Food and Drug Administration will assume this responsibility. Since this has been anticipated for many years, there should

50

51 Table

52 Table ORNL CYCLOTRON PRODUCTS Nucí id Estimated Yicló

53 Table

54 LA EXPERIENCIA ARGENTINA

55 en nuestros laboratorios.

56 Queda claro entonces que la etapa en la que nos encontramos compromete seriamente la actividad de todo el grupo de producción, tanto la del personal dedicado

57 En cuanto

58 en forma rutinaria. En un pafs como el nuestro, donde las distancias entre el centro de producción o distribución y los centros de uso son muy grandes, la posibilidad

59 u» oe Consumo total

60 Radioisótopos

61 mci J jjjjj >' ';! Envíos locates Envíos O5 o U00_ _ 800_

62 nistpiri irion

63 INSTITUTO DE ENERGÍA ATÓMICA I. E. A. CIDADE TJN1VERS1TAWA CX POSTAL Pinhriroi

64

65 Bromine-82 Target: NH^Br. Irradiation time: three hours Thermal neutron flux:

66 step on the cationic ion-exchanger contains Zr-95, Nb-95 and Ru This effluent is percolated through an anionic ion-exchanger conditioned with oxalic acid. Zirconium-95, followed

67 Number Tables I to VIII

68 TABLE II YEAR * ** 0,1 to mci 5 to

69 TABLE III 24 Na mci YEAR 0,1 to 5 5 to to * ** * From 1964 on, first column is 1 to 5 mci, ** Extrapolated to December. TABLE IV 35_ roci YEAR 1 to 5 5 to to * * Extrapolated to December.. 73

70 TABLE V 82 Br mci YEAR * 1 to to

71 TABLE

72 QUALITY CONTROL Radioactive Impurity - Some radioactive species» other than the one which is the radioisotope to be produced, may appear in the matrix as consequence of secondary nuclear reactions or as consequence of thermal neutrons absorption by impurities existing in the matrix. Detection

73 BIOLOGICAL ASSAY Radioisótopos

74 THE RADIOCHEMISTRY DIVISION OF THE "INSTITUTO DE ENERGÍA ATÓMICA".

75 already been discussed,

76 With the creation of a Chemical Engineering Division many of the classical chemical service functions of the Radiochemistry Division were allocated to that Division. Even so, some of ancient service functions still remained under

77 REFERENCES 1. F.W.Lima, Chemical Problems Arising in the Operation of a Swimming Pool Reactor and Uses of The Reactor in Chemistry, Proceedings of the Symposium

78 PAPERS PUBLISHED

79 9. G.Vicentini, M.Perrier, F.W.Lima and E.Giesbrecht, On the Use of Sodium Triphosphate for the Separation of Zirconium from Hafnium. Paper presented at the Third Inter-American Symposium on the Peaceful Application of Nuclear Energy, Petropolis, Brazil, July 16-23, (IEA-n9 25). 10. F.W.Lima, A Versatile and Inexpensive Pippeting Device for Radioactive and Other Dangerous Liquids. (IEA-n9 36). 11. F.W.Lima, A.Abrao and L.T.Atalla, Production of Carrier-Free PhcBphorus-32 by Using Sulphates

80

81

82 34. A.Abrao, M.J.C.Nastasi and A.A.Laranja, Application of Ion Exchange Resins to the Separation of Carrier Free Fission Products.Presented at the XVII Annual Meeting the Brazilian Association for Advancement of Science, Belo Horizonte, July (IEA-n9 101). 32

83

84 49. F.U.Lima and C.M.Silva, Activation Analysis of Chromium in Water Matrix» J.Radioanal.Ch m. U 147 (1968). (IEA-n9 160).

85 58. F.W.Lima, "Analise por Ativagio e suas Possibilidades ñas Ciencias Biológicas", Presented

86 II IRRADIATION AND PROCESSING TECHNIQUES

87 ISOTOPE PRODUCTION ORGANIZATION AND FACILITIES Atomic Energy

88 INTRODUCTION Atomic Energy

89 PRODUCTION ORGANIZATION

90 3. Production Engineering (6P, 14T) The process systems and equipments used in our production operations are largely the result of the efforts of this branch. This is a close support group which combines the multi-disciplined engineering staff with a shop which specializes in the prototyping, construction,

91 half lives less than 24 hours, this distance, requiring two to three hours road transport, does not cause a serious delay. Since on-site handling would be required in any case, off-site handling in approved bulk containers on company vehicles adds little to the cost. Finally, and most important, Ottawa is the closest major airport to Chalk River and most of the on-going shipments after processing are sent by air throughout Canada, the U.S. and overseas. ISOTOPE PROCESSING AND HANDLING FACILITIES Our processes and equipment have evolved over a period of 10 to 15 years. Generally speaking chis evolution

92 COMISIÓN NACIONAL ATÓMICA FACULTAD

93 xuüunuuxuaj'üb ae PXOU.UUU.LUU Los fotones

94 <^? v '.. u»*; 45 Ti 3,08h 13,3 ^^^^^^ 49 6r 42n 12, p e 58n co 5 7?ri 62 cu 8,51n 9,15h 36, Oh 9,76n 13,3 10,44 11,9 10,9 18,3 18,75 18,5 17, Zn 38, 4n 11,6 18, Ge 83n 9,6 79n Se 3,9n 9,8 78 Br 6,411 10,8( $ Br 17,6n 10, BT 39m Zr 4,4h 4,2n 11 12, Zr 78, 4h 11, Mo 15, 5n 13,2 18, Ag 24ri 9,5 16,5 108 Ag 2,4m 9,3 16,5 320 l20 Sb 15,9n 9,3 14, P2a Sb 4,2u :22 Sb 2,8d 9, I 13,2d 9,14 15, Os 6,58". 9,11 ^^^B^^!37 Ba 2,6a 9,3 ^^^^ lc0^ta 8,1h 7, Th ^7U 25, 6h 6,75d 6,0 6,0 14,2 13, Tal cono e e ve en le. Disna tabl&, nunerosos radioisótopos dtí corto período

95 107

96 . 13 )» oomiii.tia jeiic introducir el '.tizfcarsxj^ á.^irr^diar den-t. tro del 1aabü"del' 'óefetrón 'justo detras del.blancojdo»*» 7; inciden ^csve].ecl;r^nés..jsl flujo 'es allí especialmente alto por.lo que. % con*es1;& técnica se obtienen las üós altas actividades específicas. En nuestro caso

97 Ya sea q,uo 83 utilice el breñastrahlun producido internamente

98 Tratamientos del blanco irradiado En numerosos casos oí blanco irradiado puede ser usado directamente. Ello ocurre cuando

99

100 Henos comenzado a estudiar algunos sistanas de irri.dic.cion con miras

101 Conclusiones

102 Merecen sor citadas las reacciones ('V. r O con el 5 Cr,y. l Ni daj^lugar, luego do la enisión de post tronos,a los radioisótopos y 5 'Co respectivamente. En nuestro caso no se logró" activar oí Cr por requerirse fotones de nayor energía, la disponibilidad do fjtones ñas energéticas posibilita la obtención do actividad "oxtra" por la roducción, adei..ás,de la reacción

103 J4» I fut Hit

104 COMISIÓN NACIONAL

105 ÍNTRODUCCTON; Actualmente la producción de radioisótopos puede dividirse en tres grandes ramas:

106 También puede producirse Ge-68 irradiando germanio con neutrones de elevada energía (n,xn), siendo esta vía menos apropiada pues el rendimiento es menor y se ob.tiene un producto con portador, lo que implicaría generadores de mayor tamaño y eluciones de Oa-6S con me-

107 La resolución del detector utilizado

108 7. manera

109 K> 3 6 CmbJ '** I..J..1 («.2») = = 5«. «o^l, rnncioncs do e:ccitaci ór> pe -a la obtención Ge-68, i rrc.dic.njo zinc co pni'ti citlnfa al "ot.

110 Ci Figura

111 Ill RADIOISÜTÜFE GENERATORS

112 I.A.E.A. STUDY GROUP MEETING

113 Radiopharmaceutical i " m Tc serumalbumin -^""TC macroaggregates Na I5I I ^

114 t=... \2 -Xl in where X j = -2fcS2.. and A T I T 2 T, being the half life of the parent.. Tp being the half life of the daughter. Ap andao are tne respective decay constants. A number

115 Parent Half life 58 S 2,9 h IIJ Ag

116 As short lived radioisótopos

117 Table Radiopharmaceutical Pertechnetate Scintigraphy Use Colloidal sulfide Labelled human serum albumin Labelled macroaggregates Iron ascorbic acid Complex

118 Mineral adsorbents such as alumina for the couples I52 Te - I52 I, 99 Mo - " m Tc, 68 Ge - 68 Ga, hydratea zirconium oxide for the couple

119 The main disadvantage is the relative short half life

120 Several kits have been prepared by the French Atomic Energy Commissariat and presented in a manner which makes their handling easy and secure (4). 5.1.

121 5.6.

122 Generators

123 1. - WINSCHE W.E., STANG L.G., TUCKER W.D., Nucleonics 1951, 8, (3), p

124 RADIO ISOTOPE GENERATOR DEVELOPMENT IN AMERICA Warren K. Eister U.S. Atomic Energy Commission and Louis G. Stang, Jr. Brookhaven National Laboratory Radioisotope generators provide to those without immediate access to nuclear reactors and/or accelerators

125 to apply to those systems of radioactive nuclides in which the half life

126

127

128 Table

129 Table 2 - Nucllde Ag-109m Al-28 Cs-128 Pr Sb-118ra Pr-144 Pm-141 Nd-141 Ag-112 Te-127g Cs-131 Te-125m Product Half Life 40 s RADIOISOTOPE EXPERIMENTAL

130 Table

131 Table

132 Table

133 Table 6 RADIOISOTOPE GENERATORS WITH FUTURE POSSIBLE INTEREST (PARENT HALF LIFE Product Radionuclide -GREATER THAN P-32 Co-60m Nb-93m Sb-126m Tl-202 Tl-206

134 IV LABELLED COMPOUNDS

135 . (fx) Gladi N.E- do Salas, Hernán Casanova*

136 (0.4mg/ml)0.05ml de ioduro de potasio (2mg/ml), 0.05ml de iodato de potasio (2mg/ml), Yoduro

137

138 -4-4 Influencia de la Iluminación y Temperatura Las mismas experiencias que se realizan con luz de incandescencia común (150W)

139 Translated from Portuguese PL-363 PREPARATION OP I 2,6-DIIODO-4-NITROPHENOL (DISOPHENOL, DISOPHENE) José Carlos Barbarie Radiobiology Division, Atomic Energy Institute Sao Paulo 1. INTRODUCTION Disophenol, also known as disophene, is 2,6-diiodo-4-nitrophenol (formula CKI.NO-) with the following structure : Its molecular weight is $}1 and its melting point 157 C. The salt is yellow in colour, has very little solubility in water and alcohol "but is more readily soluble in alkaline solutions. This drug has been used successfully in veterinary therapeutics because

140 2. EXPERIMENTAL PABT 2.1. Labelling In a centrifuge vial we dissolved 100 mg of disophenol in 0.5 carbowax 400 and 1.0 ml of distilled water. The ph was brought to 5«"5 with the subsequent addition of I sodium iodide, free from carrier and reducing agents (1-10 mci), after vrhich two drops of chloramine T ">1 of (3*5 rog/ml) were added. The vial was closed with a stopper secured with adhesive tape.

141 (c) Thin-layer chromatography Stationary phase: Silica

142 p_h Yield, 13 min 30 niin » Influence

143

144 ~I REFERENCES

145 LABELING ORGANIC COMPOUNDS WIT» TRITIUM US INC.

146 Introduction: Some kinds

147 of the two compounds in question and exposing same to cobalt-60 radiation. The results of these experiments have been so successful that this preliminary communication is considered justified. Experimental; In the work to be described the two compounds in question, malonamidc

148 The paper chromatograph strips were scanned

149 TABLE I. MALONAMIDE UREA IMPURITY GLICINE A:R f B:R f C:R f A: n-butanol-ethanol-\vater (4:1:1). SOLVENTS ÍB: n-butanol-acetic acid-water (4:1:2). >C: ethanol-methanol-water (3:1:1). Rr

150 pounds

151 RADIOPHARKACEUTICALS AND SHORT-LIVED RADIOISOTOPES (USA) Warren K. Eister U.S. Atomic Energy Commission and Powell Richards Brookhaven National Laboratory

152 of Iodine-131

153 Improved Product Forms OUT most recent work in this area has been primarily concerned with technetium-99m and silver-109m. Technetium-99m, like iodine-131, appears to lend itself

154

155 Table I NUCLEAR MEDICAL PROCEDURES PERFORMED IN 1966 Procedure In vitro In vivo Patient Applications Number 1,040, Medical Function Scanning Research Subtotal Radiopharmacoutica1 Therapy Brachytherapy Teletherapy Therapy Research TOTAL Subtotal 930, , OOP 60,000 88,000 3,390, ' -'lj_-b _ ^ '^ MORP 68-10, Radionuclidcs

156 Table 2 RADIOACTIVA PHARMAaiUTICALS/AJ-JC APKUWíá PRODUCrS Radioisótopo Au Agent Fona

157 Table 3 RADIOACTIVE PHARMACSUTICALS. ABC APPROVED PROCEDURES Xedical Diagnostic Function Bono scans (patients with diagnosed cancer) metastases therapy* Brain tumor localization scan Radioisótopo Sr 85 Agent Form Nitrate Cardiac scans scans (for pericardial effusions) dysfunction* Circulatory studies blood and plasma volume red cell studies pernicious anemia polycythemia vera* leukemia*

158 Table 3 (Cont.) Medical Diagnosei Function Radioisótopo. Gastrointestinal protein loss Kidney function scan

159 Table

160 Table A NUCLEAR jledical FUNCTION PROCEDURES Radtonuclide Form

161 Table

162 Table

163 Table 8 BRACHYTHERAPY PROCEDURES (1966) Radionuclide Form Ra-226 Sealed sources 31.6 Plaques

164 Table 9 NUCLEAR MEDICAL DIAGNOSTIC PROCEDURES COMPARISON BETWEEN 1959 AND 1966 Half Life Tc-99m Co-60 Co d 60.2 d 6.0 h 5.26 y Hg-203 Hg-197 P-32 Au-198 Cr-51 Fe-59 K-42 Br-82 H-3 C-14 Se-75 In-113m ^ Others J Patient Administrations

165 Table 10 RADIOPHARMACEUTICAL THERAPY PROCEDURES COMPARISON BETWEEN 1959 AND 1966 " P-32 Co-60 Au-198 Patient Administrations % , % ,000 MORP 68-10, Radtpnuclides in Medicine. Williams and Sutton. 175

166 Table II NEW MEDICAL ISOTOPES Nucíid e. Cu-67 Zn-69m Fe-52 Ga-68 In-Ill Half Life 61.0 h 14.0 h 8.3 h 68.0 m 2.8 d 13.0

167 Translated from Portuguese PREPARATION OP I MONOIODOBENZENE Maria Apparecida T. Marcilio and José Carlos Barbé rio Radiobiology Division, Atomic Energy Institute, Sao Paulo SUMMARY

168 Sodium thiosulphate, lofo solution in distilled water. Sodium sulphite, 2$ solution

169 Oxidizing^ agent Table II

170 Table

171 easy to perform, gives a good yield and permits efficient purification, and second, because n-hexane has a low boiling point and is easy to evaporate, a property which facilitates its removal before the I monoiodobenzene is used for the purposes for which it is intended. In addition, it proved to be a good stabilizing agent

172 PREPARACJOK DB INSUIJNA I e I 131 DB ALTA ACTIVIDAD._BSPBCIPICA

173 biológica

174 6) O,5 ml de una solución de albúmina humana al 1% en buffer de veronal-veronal sódico de ph 8,6 (l,85g de veronal y 1O,3mg

175 c) Controles v jiá leu lo de Inactividad especifica De cada uno de los eluídos que contienen la insulina no dañada se toman 2 microunidades; se introducen en un tubo de Khan con O,9ml

176 i i ; ' ^J

177

178 CO^PORTAMISgfO TIjMUjrOLOglCO Técnica TécniCK tío Harbort I "o «O -T- TÍ r-

179 3I3LI03RAPIA 1- Proom A.- J. Path. 5ach. 5_5, 419 (1943)

180 30- ísitta A, 5. A. y Peña Iva K.J.- Informe N» 135 C. N.3. A. (1955 ) 31- Graig L.3. Biochem Wassington,

181 PREPARACIÓN

182

183 INTRODUCCIÓN Los radioisótopos naturales y los artificiales, hasta 1946 sólo hablan sido utilizados

184 enviado por el Organismo Internacional de Energía Atómica, puso, con demostraciones prácticas 1, a profesionales de la C.N.E.A. al corriente de los procedimientos a emplear* Los métodos dejados por el Dr.Veall fueron complementados en el transcurso de 1962 con el añadido de nuevas técnicas de control indicadas por el Df.ilanuel Tubis del Vereran's "ospital de los Angeles, California,

185 Uruguay, Bolivia, Paraguay, Chile, Perú

186 CUADRO

187 Cantidad f CUADRO I (3onxinuación)

188 CUADRO

189 CUADRO f

190 .12& Cantidad de productos marcados con I * e I (en milicuriea) que la C.N«B.A. suministró a ios Centros de Estudios locales o

191 .12& Cantidad de productos marcados con I * e I (en milicuriea) que la C.N«B.A. suministró a ios Centros de Estudios locales y del exterior 6. PRODUCTOS 30 «Rosa 125 o

192 '

193 Cantidad

194 mg h , GRÁFICO 200O * to ' o CO Lcoo

195 Total CUADRO II *

196 CUADRO II (continuación) to o 01

197 II (continuación) CHILE Yodoalbdmina 131

198 ESTOPO DE PREPARACIÓN A continuación oe deocriben somernmeite los métodos de marcación. precedidos de breve mención do sus aplicaciones. 13' 5 Yodo Albúmina

199 grafía (35), Este procedimiento constituye una apreciable simplificación del método do Tubis y col (3) y al de Mitta y col (4) que

200 todo (12) que permite obtener un rendimiento radiactivo de 1OO% en sólo unos mr.nv.too K Controles: cromatografía

201 anhidro durante 3O minutos. S e evapora oí solvente, se toma el residuo

202 <3e

203 trifuga y redieaelve a pk 7-7,5 con hidróxido de sodio. Rendimiento radioquímicoí 98#«Controles: esterilidad, pirógenos, electroforesis (34,35,41). 131 Albúmina coloidal I Se utiliza para centellografía de corazón.hígado,bazo,estómafo

204 Se marca triyodotironina y tetrayodotironina en medio ter-bu- 131 taño previo ajuste

205 lodoformo 1 T ^

206 B I B L I O G R A F Í A l.mc FÁRLANE,S. Nature 182, 53 (1953) 2.SALAS,G.6.de y I1ITTA, A.B.A., Presentado al I"*" Congreso Latinoamericano

207 -9.TAXKB,J.J. y KBSTSKS, P. J - Gun, Chem.Acta 8,3O2/4 (1968).

208 37.BARBERIO,J.C.,^:i?vATA,I.S.,NAKAZON3,A. y MITTA, A.E. A. presentado

209 PREPARACIÓN

210 INTRODUCCIÓN La preparación de compuestos marcados con Carbono 14 en nuestro pal comenzó el año 1957, cuando en la División Moléculas Marcadas del Departamento de Química, Gerencia de Investigaciones de la C.N.E.A. se sintetizó algunos ácidos orgánicos marcados en el carboxilo y diferentes compuestos derivados de los mismos. Posteriormente este pequeño número de sustancias se fue ampliando, llegando en la actualidad

211 PREPARACIÓN DE ÁCIDOS ORGÁNICOS MARCADOS

212 r CH'COOM CM,CH"COOH COOH-COOH CM,CH,'coa>

213 derivados, y en la fig.3 el grupo de derivados obtenidos usando como materia prima

214 14 Preparación de ^Am^n o ácidos^ con C^ (4 A partir

215 Pirólj-sisde Sales

216 También se efectuó

217 Pora

218 Hemos terminado el estudio de copoliraerizacióu de nonómeros uti- 14 lizundo sustancias marcadas

219 TRABAJOS REALIZADOS

220 11 BUHLBR,M.F., CASTRILLON,J.P.A. Influencia dol óxido de magnesio sobre la pirólisis de sales do litio de ácidos carboxilicos. DIG N 16 CNBA (no publicado) (1962). 12 BUHLBR.M.F., CASTRILLON,P.J.A. y MERTIG,C.P. Evidencia de la formación cíe hexafeniletano

221 23 3UHLER,M,F., LOPBZ,R.,CASTRILLOK,J.P.A.,MITTA,A.E.A. Preparación de 4-Difenilaminosulfonato

222 r.cooh"cooh.ch,ch»t«>h. CH^MBrtoOH CH/HBrtoOCjH, CHjCHÍCH/COOH, CH,(CH,\C»C 1 COOH I FÍ2.2.-

223 R-CH,! M9 R-CHjMgl 14 CO, HjSO, (MKCM ACUOSf) NaOH R-CH/COONa HO R-CH/OBr Br, R-CHBr-COBr K PURIFICACIÓN R-CHBr-COOC 2 Hb CMH4TOGMFICÁ JÍZ. L»-.- Síutí ís de ést^r^s de ícir'os bromar'oc

224 CH,Br CH? CH 2 KOH Mq CO? H* CH 2 Br CHBr CHMgBr,H CH COOH COOCjH,. i HNHCHO CHj=CH COOC.Hs COOC^HJ \NHCHO COOC 2 H 5 COOH ;HNH, :OOH Fi^.5.- Sintáis

225 co \ «/ co KCN ^CH.Ci, ^ C N -- "to Q 7 \chjboci CH^ y VH^OCHN "to x ca CO

226 HOÍCH^OH SOCU PIRIDINA C^C^SSCH BrMgCjH, CH^^jteCMgBr Nal ACETONA HCHO HOCNa NH 3 CH^CIj^sCCHyOH BfjPPMDINA OVtlilpCCiyr BrMgC=C(C^;t H H' H H HyCsC N&N-DMSO CH,OH\CIH m>4,»>9 IHt t'coíoditnoko K m,7.n octotferarfimwco m:7 n,6

227 RADIOCHEKICAL RESEARCH

228 RADIOCHEMICAL RESEARCH G.B. Cook International Atomic Energy Agency Vienna, Austria

229 the target isotopes

230 Another aspect of isotope product, namely quality control, particularly in respect

231 The Szilard-Chalmers effect

232

233 After radioactive cooling, the ferrocene was volatilised and it was found 59 that

234 I. HOT ATOM CHEMISTRY H. ENERGETIC DECOMPOSITIONS IN HOT ATOM RE ACTIONS. ÜNIMOLECULAR REACTIONS

235

236 n(v) K CHEMICAL REACTIONS IN A MAXWELLIAN SYSTEM to *> H 8" 0.5 n(v)o-(v)v (T(v) 0.01 i i I 10

237 used extensively

238 RADIO

239 more

240 AT FIGURE 3. RADIO GAS CHROMATOGRAM OF RADIOACTIVE PRODUCTS FROM REACTION OF 38 C 1 WITH CH 3 C1. Lower line: Macroscopic Composition; Upper line: Radioactivity to O o: ü CH 3 CI 38 CH 2 CICI 38

241 presence

242 the radioactive' substitution products, CH 3 T

243 SEPARATION

244 detail

245 about

246 are shown in the boxes: Scavenger Radical R H DX RD HD X 2 RX HX When D D 2 DX

247 0.07 O.06 CD 3 T OT O Lob. E T (ev) == t 2.5 X

248 can The initial energy of the hydrogen atoms in such experiments

249 MENZINGER t WOLFGANG, 1967 o r> o odc YIELD ENERGY CURVES FROM CYCLOHEXANE + T 4 2O.3% CL to O tu Q. O. U- o 55 D O CYCLOHEXANE-T n-hexane-t HEXENES-T t I I t I I \ I i I- ENERGY. PER TRITIUM NUCLEUS (ev) FIGURE 6: REACTIONS OF T ATOMS FROM T + BEAM 260

250 process, but the beams operate satisfactorily over the whole energy range. The non-zero reaction yields at the lowest energy suggest that some complications still exist

251 JDUJJ3H1 UI U38S JO) p Ol S9Jqi o» e kj <o o "*: o» Lü OL 262

252 tritium systems indicate that

253 Eventually,

254 r-4000 COUNTS PER MINUTE me«o-(chfci) 2 / 'i LIQUID / co O) Ol

255 TABLE 1 Recoil Tritium Reactions with Molecules Containing Asymmetric Carbon Atoms A. Experiments with crystalline materials Ref. 1)

256 at one site does not produce the optical isomer, but forms the djl isomer from the meso.or vice versa. This difference permits

257 600-1 Figure

258 \ result for one such experiment the substitution of T for \ H in CHi, is favored over T for D in CD* by a factor of 1.3Ü.03. Such

259 steadily decreasing ratio: CH*, 7.2; CHjD, 5.6; CH 2 D 2, 3.1;

260 CO -5 RECYCLE SEPARATION

261 FIO. U Figure to -a (S3

262 Figure 12. Moderator Curves for the Reactions of Recoil with CH-jCl, oo ro O ro to -J CO 2-

263 the mass of Ne more closely matches that of Cl than does He. 'the experiments actually involve Since

264 TABLE 2 Relative Yields of HT from Recoil Tritium Reaction with Saturated Hydrocarbons Correlation with Bond Dissociation Energies Hydrocarbon Bond Dissociation Energy [34]

265 However, we have measured the HT yields from some additional molecules, including

266 Figure 4.0 (HT) F -J 2.0 to -o

267 of

268 References 1. "Chemical Effects of Nuclear Transformations," International Atomic Energy Agency, Vienna, 1961.

269 14. A. Kuppexmann and J. M. White, J. Chem. Phys.,,4532 (1966). 15. C. C. Chou and F. S. Rowland, J. Amer. Chem. Soc.,,2616 (1966). 16. C. C. Chou and F. S. Rowland, unpublished experiments.

270

271 II. ENERGETIC DECOMPOSITIONS

272

273 * O 65 O u_ o 60 3tu f 0 2 -SCAVENGED 0 2 -SCAVENGED, MIXTURES WITH CH 4 CYCLO-C 4 H7T YIELD VERSUS PRESSURE (CYCLO-C 4 H 7 T+ C 2 H 3 T«IOO) LIQUID PHASE, WITHOUT SCAVENGER UNSCAVEN6ED, SHORT IRRADIATIONS 55 5C tog (molecules/cm 0 ) I 20 3O 22

274 of the two in equations (5) and (6). Figure 1: Some qualitative conclusions can be drawn from the data of

275 15 14 RICE-MARCUS MODEL log K(E) l3 in Sec' l2 II E+E* ; n»3o THEORETICAL UNIMOLECULAR DECOMPOSITION RATE CONSTANT, K(E)

276 The kinetic energy of the reacting tritium atom is not known in these experiments. However, since

277 N(E) CO 00 CO (a) I (b) > (c) ' Excitation Energy, kcal/mole FIGURE

278 After correction

279 80 70 LEE.ROWLAND, 1963 HOSAKA.ROWLAND 60 to CO L_ 10 J L LOGÍMOLECULES/cm 3 ) ^ «i r-*r *T CM. PRESSURE 22 i LIQ. FIGURE 4: Pressure Dependence of Substitution Reactions of T* with cvclo-c 4 H 8 and cvclo-c 4 n r 4''ij 0 C 4 n

280 from these data:

281 to CO CO RATIO OF PRODUCT YIELDS T*

282 Table 1 Distribution of Radioacitivty Following Recoil Tritium Reactions with Methyl Isocyanide [10]. (Yield of HT - 100) Product CH 2 TNC CH 2 TCN CH 3 T CH 2 TOH C 2 H S T Liquid CH 3 NC Liq.CH 3 NC+I 2

283 energies

284 unavailable CTF.* This reactive chemical species attacks

285 CH,F,

286 I.I 1.0 l-butene> 02 vs. Pressure o 24 C A 25 C x heated after irradiation CO CO CO 0.9 r Q Total Pressure, cm Hg TOO FIGURE 7: Pressure and Vemper.iture Dopondenco of Rocoil Tritium Reactions with I-ruteno.

287 5-10 e.v. range. The best fit to the data of Figure 7 suggests that more than 70% of the tritium atoms reacting by (12) have less than 3 e.v. kinetic energy at reaction [19]. Measurement of the energetics of la P (or 38 C1) substitutions for

288 Chromotoqrams

289 after 10~ 9 seconds,

290 Counts 2 Min o to 22 BACKGROUND Hours 23 SEPARATION

291 is CH

292 decomposition with preferential loss of either the T atom, or an adjacent

293 References, Lecture

294

295 VI QUALITY CONTROL

296 QUALITY CONTROL OP RADIOISOTOPES AND LABELLED COMPOUNDS. by Y ves COHÉN Centre d 1 Etudes Nucléaires de Saclay (France) Quality control

297 the radioisotope which is in that chemical form. The presence of iodate-i-i}! in a solution intended to be entirely iodide-i-i}! is an example of radiochemical impurity in a solution which is radioisotopically pure. The position of a label in a molecule being different might create a radiochemical impurity Chemical_guritjr.

298 Radioisotopes which are prepared by chemical separation from

299 1-4-7.

300 2. - CONTROLS_OP_PHYSICAL_FACTORS. 2-1, Had ioac ti ve _ concentration. Methods of determining the radioactivity,

301 if at least one of the gamma energies of the impurity is higher than the maximum gamma energy of the main product, e.g. in the determination of sodium-24 in potassium-42.

302

303 determination

304 whose shape does

305

306 3-2. Radiochemical^guritj. Radiochemical impurities

307 oxidized during processing or as a consequence of radiation decomposition of the solution (47). Lower valency ions may occur in solutions of iron-59 as ferric chloride and in arsenic-76 solutions as arsenate. Arsenic-74 solutions may also contain traces of cacodylic acid if this material

308 4. - BIOLOGICAL_CONTROLS. Radioactive preparations when used in medical applications must fulfil the general requirements

309 However, much

310 5. - As a summary fo what has been said already, and as a guide to suitable accuracies for the control of medical isotopes,

311 TA3LS I CHROMATOGJMPHIC SEPARATION OP F.A BIOCHEMICAL Zr.iPUIilTIES L\ r ORGANIC RADICPHARJWCSUTICALS '/-I. GO Labeled molecule Support Solvent íyanocobalamln y 53, Co T rt*hatr:an N 4 paper. paper L "oo CO Silica gel G Silica

312 CHROMATOGRAPHIC SEPARATION OF lo - I25 I qi. TABLE I (continued) rifuiutizs HI 0?.GAi;iC \ADICP3AiWiACEuTICALS I LABELLED KOLZCULES. Labeled molecule Support Hippuran Silica Hose bcngal Rose bengal 4 Rose ben^al Rose bensal CO to en

313 :;bclod. Support noleóule 'cohydrln paper "cohycrin paper TAITLS Í (Continued) CKROMATOORAPKIC SEPARATION 0? RADIO COMICAL IKPURITI2S IN ORGANIC RADIOPHARHACEUTICALS. Solvent -c - Kthanol-phosphate ufror p:i 7, 1 * n-'cutanol:r.othanol:aquoous nia (d»0,o3 OR LA33LL3D MOLECULES.

314 O 1 A BLE 2 (continued) ko?«atoqraphic SEPARATION OF SADIOCHEMICAL IMPURITIES IN INORGANIC PHARMACÉUTICALS. pport arid ndi APC Solvent Proportions Duration APC APC TLC APC \PC 5TLC

315 ( TABLE 2 'CHEOKATOGRAPHIC SEPARATION

316 SI '.:ABIE

317 \ Eij:cT:;o?r:cüi:7ic ce'/.r-atzci; o??.".dicc::tjical r-i?ur,i7iss IN OPGAXIC AÍO INORGANIC RADIOPÍIARMACEUTIC/» la'o&ll'jd molecule Pc.pcr Slc.c'*,volytís T.:z of Hc.<Iic chemical Pja

318 tj (continued);- ' '

319 REFERENCES (1) ATO* tic EHJ307 CO.TíICSICII, Radioactive PlvuTnaeeuticcvls (Proc. Syr.p. Cak-hlctge, I9oJ>), CrJc-r\idse Inst. of Mud. studies (1965). (2) V.'OL?, U, TU2I3, H. J. Fharo. So..5, (l#>7) I. 3RL\'CK W.IK, (Synp IS 52) Advances in tr&ccr meth Kcw-Yoi-k. yol> s (KOTJICHILD S. Ed, Plenum Preso, Kew Yortc (1965) 201. GOPAL» fi.g.s., ly/i, V.K., J. Set. Ind. Kca., 2 (ISO

320 -

321 - 5 - (2*)!«C9H13CX, A., J. Chroo&toc. IJ (X $*) (20) CQC&f, *., Prod. Pharre. 16 «* (1961) I. (25) CC:^«y,, j::oifm!d J. A 9/.«9 ft $.L A A XntciTUit. J. Applied (27) KIÍOL;,,