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procedure untfi all fines are removed. Use 3 ml wet resin in a 6-mm bore silica column fitted with a quartz wool plug. (See Fig. 60). for dimensions. ) (d) (e) (f) (g) (h) (i) At this stage the color changes from blue to green. Condition the columns immediately before use by allowing 10 ml 8 ~ HN03 to run through them. This solution contains the impurities free from Pu. This solution is ready for analysis by the polythene funnel method. Collect the washings and transfer to the appropriate e residue bottle. Add about 10 ml 8 ~ HN03 and stir the resin with a pointed l/8-in. perspex rod until it is in suspension and all air bubbles have been removed. Allow to settle for 10 tin and decant off any resin still in suspension. Add fresh resin to bring the total resin volume to 3 ml. I: --- 1.5cm SORE 4cm --- 4cm SORE 0 cm -- 6mm BORE 20 cm QUARTZ WOOL PLUG --- Fig. 60. Ion exchange column. 143
Procedure 16. Separation of Plutonium Before Spectro~aphic Analysis of Impurities. Extraction Chromatography Method Using TBP F. Trowell (Ref. 405) Outline of Method Pu in 8 ~ HN03 solution is adsorbed on a KelF/ TBP chromatographic column and the impurities eluted with 8~ HN03. Sc is added as an internal standard to the eluted solution which is then concentrated by evaporation and analyzed by the graphite spark technique for Al, Co, Cr, Fe, Ga, Mn, Ni, and Ti. Applicability. This method is intended for the analysis of high-purity Pu. The concentration range covered is from 0.5 to 10 ppm. The lower limit of analysis may be restricted by the reagent blank. Equipment Reagents 1. Column (for dimensions and preparation see Appendix). 1. 2. 3. 4. 5. 6. 7. Procedure 1. 2. 3. 4. 5. 6. 6 ~ HC1. Note (a). 16 ~ HN03. Note (b). 8 ~ HN03. 0,32 ~HN03. 2 ~HF. Note (c). CC14. Note (d). Tri-n-butyl phosphate. Note (e). KelF. Note (f). Grease solution. Note (g). Weigh 2 g of Pu and dissolve by tipping into silica beaker. Cover with a clock glass and When all traces of the metal have dissolved, 5 ml 6 ~ HC1 in a 50-ml warm. Note (h). rinse and remove the clock glass, rtise down the sides of the beaker, and evaporate the solution to dryness. Cool (Note (i)), add 5 ml 16 ~ HN03, warm and add 5 drops 2 ~ HF to ensure complete solution. Evaporate to a moist residue. Note (j). Redissolve this residue in 10 ml 8 ~ HN03, warming to ensure complete solution. Transfer the solution to the KelF / TBP column using the minimum volume of 8 M HN03 to rinse out the beaker. — Note (k). Place a 50-ml tall-form silica beaker containing 1 ml 20 pg/ ml Sc solution under the column. Note (l). 144
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
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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
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c.. Pu(IV)+ Pu(VI) Reagents Solutio
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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
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TABLE IV- 12. Stability Constants o
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D. 1 Co-precipitation and Precipita
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is first oxidized to Pu(VI) with so
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oxygen in the ratio 1:3. If an exce
Page 37 and 38:
the TBP cone entration. Solovkin 39
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D, l? D Ic n. 0 5 10 Concentration
Page 41 and 42:
D 103 ~ ,.2 _ 10 I H ,0-1 ~ / P / P
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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
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X[N05] = [HN03] ‘( ~ ~[N03] = HN0
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Di-acidic compounds. Mono-2- ethylh
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A may be either a simple anion or t
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n 104 d Id 10 I 10-1 , a ,,81 0.1 M
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The fact that Pu(III) does not extr
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Fig. 25. Extraction of elements as
Page 63 and 64:
TABLE IV- 19. Distribution Coeffici
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10~ I ~ 0.01~ D 0.001 : 0,0001 . La
Page 67 and 68:
loi- 1“’’’’’’’”1
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TABLE IV- 22. Extraction of Plutoni
Page 71 and 72:
m * Amideb N, N-Dihexylformamide N,
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dependence on the TTA concentration
Page 75 and 76:
1.0 D 0.1 —--L~,20 HNOO; CO&NT R
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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
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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 and 126: Procedure 5. Plutonium D. C, Hoffma
Page 127 and 128: Procedure m. Pipet tie samples (2~i
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: Procedure 15. Separation of Pu befo
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
Page 179 and 180: 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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