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Preparation HF: cone. HF-HN03: equal volumes of 2 M solutions — H3B03: saturated solution NH20H. HC1: 35~o by weight in H20 Solution I: 0.1 ml cone. HN03 per 15 ml cone. HC1 Dowex A-1 (10% cross-link, Nalcite SBR) anion resin slurry in H20, The 200-400 mesh moist solid is washed about three times with successive portions of water and cone, HC1. After each wash the resin is allowed to settle and the liquid decanted by siphoning or by means of a vacuum pipet. The resin is then stirred thoroughly with several times its volume of water in a large graduated cylinder, and the following fractions are withdrawn on the basis of sedimentation rates: < (1 cm/min,
Procedure m. Pipet tie samples (2~in HC1 or HN03) into 40-ml long taper conical centrifuge tubes. (1 -ml aliquots are used if possible. although aliquots as large as 25 ml can be taken if necessary). If tracer or spike is added to 1 or 2 of ~ the samples, make the others up to the same volume with a solution of acid strength identical to that of the tracer or spike. Stir. =. Add 1-2 drops of La carrier ad then 2-4 drops of NH20H” HC1 per ml of solution. Make the solution at least 2.5 ~ in HF by addition of cone. reagent (Note 1). Agitate the solution and permit to stand for 5 min after the addition of each of the above reagents. =. Centrifuge and discard the supernate. Step 4. Wash the precipitate with about 0.5 ml of 2 ~ HF-2 ~ HN03 solution. Stir, centrifuge and discard the supernate. Step 5. Dissolve the LaF3 precipitate by adding 1 drop of saturated H3B03 solution, stirring, and then adding cone. HC1 to a volume of 1.5- 2.0 ml. The solution may be warmed if necessary. =. Transfer the solution to a 5-cm Dowex A-1 resin column (see Note 4 of Np procedure) which has been washed with 1-2 column volumes (Note 2) of Solution I (Note 3). Wash the centrifuge tube with two 1-ml’ aliquots of Solution I. The washes may be driven through the column with air pressure if so desired. The effluent solutions from these washes may be used for the Am and Cm determinations; if not to be so used the washes are discarded. Step 7. Wash the sides of the centrifuge tube with 1.5 ml of cone. HC1, wash and remove the Pt stirring rods, centrifuge and pass the solution through the column with the use of pressure. =. Add a few cryst~s of ~20H” HC1 direc~y to the top of the resin column. (This helps to prevent immediate oxidation of the HI solution by any traces of HN03 remaining on the column. ) Wash the centrifuge tube with 1.5 ml of cone. HC1, transfer the washings to the column, and permit them to pass through. The column should not be permitted to run dry while air pressure is being applied to it, since air bubbles will be forced into the column and channeling and erratic elution of activity may occur, &I& 1-2 ml of tie HI-HC1 elutriant is put on the top of the col~n and no pressure is applied during elution. The dark band of the elutriant may be seen migrating down the column. The activity appears to be concentrated about the lower edge of the elutriant band and most of it comes off in a 6- to 8-drop peak. However, to obtain quantitative yields, drop collection is begun on a 2-in. Pt disk when the band is about 0.8 cm from the end of the column, and collection is continued for 10-15 drops after the band has reached the end of the column. This allows for possible irregularities in the band or misjudgements regarding its position. The drops taken before the band reaches the end of the column are arranged on the periphery of the Pt disk, and those which are expected to contain most of the activity are collected near the center. The drops are not permitted to run together. 120
Page 1 and 2:
1National Academy of Sciences Natio
Page 3 and 4:
The Radiochemistry of Plutonium. Ge
Page 5 and 6:
PREFACE This report has been prepar
Page 7 and 8:
Procedures (Continued) CONTENTS (Co
Page 9 and 10:
IL GENEWL REVDZWS OF THE RADIWHEMIS
Page 11 and 12:
IV. CHEMISTRY OF PLUTONIUM OF SPECI
Page 13 and 14:
Solution TABLE IV-2. Behavior of PU
Page 15 and 16:
* Compiled primarily from the revie
Page 17 and 18:
TABLE IV-6. Oxidation-Reduction Rea
Page 19 and 20:
c.. Pu(IV)+ Pu(VI) Reagents Solutio
Page 21 and 22:
Concentration Equilibrium Constant
Page 23 and 24:
PU+4 has approximately the same ten
Page 25 and 26:
TABLE IV- 9. Ionic Potential of Plu
Page 27 and 28:
TABLE IV- 11. Stabflity Conetants o
Page 29 and 30:
TABLE IV- 12. Stability Constants o
Page 31 and 32:
D. 1 Co-precipitation and Precipita
Page 33 and 34:
is first oxidized to Pu(VI) with so
Page 35 and 36:
oxygen in the ratio 1:3. If an exce
Page 37 and 38:
the TBP cone entration. Solovkin 39
Page 39 and 40:
D, l? D Ic n. 0 5 10 Concentration
Page 41 and 42:
D 103 ~ ,.2 _ 10 I H ,0-1 ~ / P / P
Page 43 and 44:
100( I0( 1( D 1.( 0. 0.0 0.00 Nltrl
Page 45 and 46:
Table IV- 16. (Continued) Extractan
Page 47 and 48:
Table IV-16. (Continued) Extr actan
Page 49 and 50:
In this equation, HA represents any
Page 51 and 52:
X[N05] = [HN03] ‘( ~ ~[N03] = HN0
Page 53 and 54:
Di-acidic compounds. Mono-2- ethylh
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A may be either a simple anion or t
Page 57 and 58:
n 104 d Id 10 I 10-1 , a ,,81 0.1 M
Page 59 and 60:
The fact that Pu(III) does not extr
Page 61 and 62:
Fig. 25. Extraction of elements as
Page 63 and 64:
TABLE IV- 19. Distribution Coeffici
Page 65 and 66:
10~ I ~ 0.01~ D 0.001 : 0,0001 . La
Page 67 and 68:
loi- 1“’’’’’’’”1
Page 69 and 70:
TABLE IV- 22. Extraction of Plutoni
Page 71 and 72:
m * Amideb N, N-Dihexylformamide N,
Page 73 and 74:
dependence on the TTA concentration
Page 75 and 76: 1.0 D 0.1 —--L~,20 HNOO; CO&NT R
Page 77 and 78: cupferron, followed by back extract
Page 79 and 80: . more. Siekierski and Taube, 381 a
Page 81 and 82: TABLE IV- 27. Slope of the Dependen
Page 83 and 84: polymerization of the resin to prov
Page 85 and 86: co ; n 1000L z - 100 z o ~ m oL x z
Page 87 and 88: Volume distribution coefficient of
Page 89 and 90: affinity of several ions was Th(IV)
Page 91 and 92: 95% of Pu(IV) was removed from a 0.
Page 93 and 94: 2 d 1.0 I I I 1 I I 1 ,, , , I II r
Page 95 and 96: X“ 104 , 1 1 1 1 1 .— .-. I Ioa
Page 97 and 98: 200 100 50 20 I O.10 ~ $ NPIX PUIIT
Page 99 and 100: Fig. 54. Adsorption of the elements
Page 101 and 102: Toribara et al. 403 used a liquid s
Page 103 and 104: V. DISSOLUTION OF PLUTON17JM SAMPLE
Page 105 and 106: m m TABLE VI- 30. Source Preparatio
Page 107 and 108: o 0 TAIIT.E VI-31. Techniques for M
Page 109 and 110: Solvent extraction of Pu into a liq
Page 111 and 112: TABLE VII-33. Basic Data for Critic
Page 113 and 114: Procedure No. 6. 7. 8. 9a, 9b , Aut
Page 115 and 116: Procedure 1. Determination of Pu in
Page 117 and 118: (e) (f) (g) (h) Where C v E The pre
Page 119 and 120: Procedure 2. Separation and determi
Page 121 and 122: Procedure 3. Separation and determi
Page 123 and 124: Procedure 4. Plutonium R. J. Morrow
Page 125: Procedure 5. Plutonium D. C, Hoffma
Page 129 and 130: Procedure 6. Separation of Plutoniu
Page 131 and 132: Procedure 7. Determination of Pu (R
Page 133 and 134: Procedure 8. Uranium and Plutonium
Page 135 and 136: 15. Add 3 drops of HC1 and 1 drop o
Page 137 and 138: Procedure 9b. Separation of Plutoni
Page 139 and 140: Procedure 11. Uranium and Plutonium
Page 141 and 142: Procedure 12. Plutonium from Enviro
Page 143 and 144: 9. 10. 11. 12. 13. 14. 15. 16. 17.
Page 145 and 146: 10. 11. 12. 13. 14. 15. 16. 17. 16.
Page 147 and 148: Procedure 14. Separation of Plutoni
Page 149 and 150: Procedure 15. Separation of Pu befo
Page 151 and 152: Procedure 16. Separation of Plutoni
Page 153 and 154: Appendix (m) (n) (o) (P) Purificati
Page 155 and 156: Procedure 17. Separation of Np and
Page 157 and 158: Procedure 19. Determination of Plut
Page 159 and 160: NOTE: Reporting Results Results are
Page 161 and 162: Notes .. 1. 2. 3. The element prase
Page 163 and 164: 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13
Page 165 and 166: Procedure 22. Determination of Amer
Page 167 and 168: concentrated nitric acid in a block
Page 169 and 170: Preparation of Sample The 24-hr or
Page 175 and 176: “The Actinide Elements” (McGraw
Page 177 and 178:
48. D. H. Boase, J. K. Foreman, and
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108. 109. 110. 111. 112. 113, 114.
Page 181 and 182:
159. 160. 161. 162. 163. 164. 165.
Page 183 and 184:
217. W. E. Keder, J. Inorg. Nucl. C
Page 185 and 186:
279. 280. 281. 282. 283. 284. 285.
Page 187 and 188:
339. 340. 341. 342. 343. 344. 345.
Page 189 and 190:
397. 398. 399. 400. 401. 402. 403.
Page 191 and 192:
451. C. E. Honey, Jr., R. N. R. Mul
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