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Procedure Author No. (principal) 21. Everett 22. Bokowski 23. 24. 25. Campbell Weiss Bruenger Title or method Determination of Pu in urine (LaF3 precipitation, TTA extraction) Determimtion of Am in urine in the presence of Pu (BiP04 precipitation, LaF 3 precipitation extraction of Pu into di - (2- ethylhexyl) phosphoric acid Determination of Pu in urine (alkaline earth phosphate precipitation, anion exchange 161 Determination of Pu in urine (co-crystal- 166 lization with potassium rhodizonate, LaFs precipitation, anion exchange) Determination of Pu in urine and bone ash (extraction by primary amines from H2S04 solution) 107 164
Procedure 1. Determination of Pu in solutions containing large amounts of Fe and Cr. G. A. Welch ~. (Ref. 446). — Outline of Method Hydroxylamine is added to the sample to reduce plutonium and chromium to the trivalent state. The acidity of the solution is adjusted and lanthanum nitrate carrier added. Lanthanum fluoride is precipitated by adding a limited amount of ammonium fluoride and carries the plutonium with it. By strictly controlling the amount of fluoride added the precipitation of iron and chromium is prevented. The precipitate is separated by centrifuging, washed and mounted on a flat stainless-steel counting tray, and the a -activity measured with a scintillation counter calibrated against standard sources. Reagents All reagents are analytical reagent quality where available. 1. 2. 3. 4. 5. 6. 7. Equipment Ammonium hydroxide, 9~ Nitric acid, 2~ Hydroxylamine hydrockiloride, 5!70 w/v Lanthanum nitrate solution, 5 mg La/ml. Dissolve 7. Elg of lanthanum hyxahydrate in 500 ml of distilled water. Ammonium fluoride solution, 12-57. wfv Store in a polythene bottle. Cellulose lacquer. Dilute “ZAPON” lacquer with amyl acetate. Standard Pu solution, 0-5 ~g/ml. Dilute a solution of known Pu concentration. The exact Pu concentration of the diluted solution need not be known, but the isotopic constitution should be essentially the same as that of the samples requiring analysis. 1. a - scintillation equipment. Type 1093A or B scintillation unit with associated equipment. 2. Counting trays. Stainless steel, flat, mirror finish, 1-1/16 in, diameter. Prepare for use by heating in a flame until the surface Allow to cool and paint a ring of cellulose lacquer round the edge. to dry and store the pr:epared trays in a closed container. Procedure 1. Transfer a suitable portion of the sample to a 3 ml is straw coloured. Allow the lacquer @ass centrifuge tube. Wash out the pipette with 2~ nitric acid and add the washings to the tube. [ Note (a)]. I 08
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1National Academy of Sciences Natio
Page 3 and 4:
The Radiochemistry of Plutonium. Ge
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PREFACE This report has been prepar
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Procedures (Continued) CONTENTS (Co
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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
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the TBP cone entration. Solovkin 39
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D, l? D Ic n. 0 5 10 Concentration
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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
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Table IV- 16. (Continued) Extractan
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Table IV-16. (Continued) Extr actan
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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
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: Procedure No. 6. 7. 8. 9a, 9b , Aut
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 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 171 and 172:
Procedure 24. Determination of Plut
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Procedure 25. Determination of Plut
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
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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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