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Pour the solution through a Teflon column, 4 X 0.62 cm anion exchange resin AG l-x8 (Cl-: 0.297 to 0.144 mm) previously waahed with 10 ml of 9 N HC1. Adjust — the flow rate to 2 ml/ min. Wash the column with 15 ml of 9 ~ HC1. Elute with 30 ml of 6 — N HC1-O.2 — N HF. Collect the eluate in a Teflon beaker which contains 15 mg of NaC1. Evaporate to drynese, Dissolve the salt in concentrated HN03 and transfer to glass. Add 3 ml of HC104, 2 ml of H2S04J and heat to dryness. Dissolve the salt in 1 ml of water and transfer to the electrodeposition cell fitted with a tantalum disk. Add 4 ml of 6 N NH4C1 solution and 2 drops of concentrated — HC1. Electrodeposit at 2.5 to 3.0 A for 20 min. Quench the cell with 1 ml of concentrated NH40H. Wash the solution from the cell with distilled water and dry the tantalum disk on a hot plate. Alpha count. 165
Procedure 25. Determination of Plutonium in Urine and Bone Ash by Extraction with Primary Amines F. W. Bruenger, B. J. Stover, and D. R. Atherton (Ref. 61) Outline of Method Concentrated urine, or a solution of bone ash is made 1 M in H2S04 and — Pu is extracted by a mixture of highly branched primary alkyl amines. The Pu is then back-extracted with 8 ~ HC1 and counted. Reagents and Equipment The a-detection instrument is a 27r proportional counter of conventional design capable of accepting 2-in. stainless steel planchettes; counter performance is checked with a U308 standard supplied by the National Bureau of Standards. Prirnene J.M- T, a mixture of tert-alkyl primary amines, 5 ~. by volume in xylene, was purchased from Rohm and Haas, Philadelphia, Pa. The Prirnene solution is washed with half its volume of 1 ~ H2S04 before use. Procedure Urine analysis. Urine is collected in polyethylene bottles over 10 ml of concentrated formic acid to avoid excessive hydrolysis of urea, which would render the specimen basic and could result in loss of Pu by adsorption on the wall of the con- tainer. An aliquot of urine is transferred to a Kjeldahl flask containing enough 5 ~ H2S04 to attain an acid concentration of 2 ~ in the final sample. The solution is boiled without charring for about 1 hr. Thus far, volumes up to 500 ml have been extracted. For larger volumes, amounts of reagents are increased proportionally. The following amounts of reagents are used for 100-rnl aliquots. The sample is filtered through borosilicate glass wool into a separator funnel and is allowed to cool to room temperature. Twenty ml of a 57’. solution of Primene JM-T in xylene is added to the sample and the mixture is shaken for 15 min. After separation of the two phases, the aqueous phase is put aside for a second extraction. The organic phase is washed twice with 25 ml of 1 g H2S04. Pu is removed from the organic phase with two 20-ml portions of 8 y HCL The aqueous phase is again extracted with 20 ml of 5~. Primene, and Pu is back-extracted from the Prirnene with 20 ml of 8 M HC1. The — combined HC1 fractions are dried under a heat lamp and then the organic contaminants are destroyed by heating over an open flame or in a furnace at 5000C. The Pu residue is dissolved in concentrated HN03 and transferred to a Z-in. -diameter stainless steel planchette for a counting, Bone analysis. Bone is ashed for 4 hr at 600°C and, after cooling, is dissolved in as little HN03 as possible and diluted with H20 to a known volume. and a suitable aliquot of this solution is taken for analysis, The. amount of bone ash should not exceed 250 mg for every 75-ml volume of the aqueous phase. The aliquots are evaporated to dryness under a heat lamp to minimize the amount of HN03 and then put in solution with 4 ml of concentrated HCOOH, and a 6O-ml portion of 2.5 ~ H2S04 is added. This solution is heated in a water bath until it is clear, and then transferred to a separator funnel. Transfer is completed with a 10-ml rinse of distilled water. Any CaS04 that forms does not interfere. Pu is extracted as described above. 166
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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
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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
Page 51 and 52:
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
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
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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
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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.
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2 d 1.0 I I I 1 I I 1 ,, , , I II r
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X“ 104 , 1 1 1 1 1 .— .-. I Ioa
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200 100 50 20 I O.10 ~ $ NPIX PUIIT
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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
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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 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: Procedure 24. Determination of Plut
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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