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VIII. COLLECTION <strong>OF</strong> PROCEDURES A. Introduction The literature of Pu is replate with radiochemical and analytical separation procedures. A survey disclosed 54 papers with procedures which were written in enough detail to do justice to the name, and many more methods which could easily be developed into procedures by making the directions quantitative or more complete. Of the 54, 26 survived screening and are included in this collection. The basic criteria for screening were fourfold: (1 ) distinctiveness in chemistry, (2) completeness in detailed instructions, (3 ) generality in application, and (4) utility. In some cases a rather arbitrary choice had to be made between procedures which met these criteria equally well. The procedures are divided into (1) general radiochemical procedures, (2) special purpose separation procedures, and (3) urinalysis procedures. The procedures in the first group are concerned with purifying Pu from other alpha emitters and from fission products sufficiently for the purpose at hand, usually for alpha counting or alpha pulse analysis. The starting materials range from reactor target dissolver solutions of varying ages to fresh samples of nuclear explosion debris to very dilute environmental samples. There are 13 of these procedures included. The second group of procedures is concerned with a specific separation involving Pu. Two examples are the separation of Np and Pu and the removal of Pu before analysis for impurities in Pu metal. Urinalysis is a separate category, primarily because there are so many procedures in the literature, all purporting to do the same thing. The chemistry after the initial separation step is, of course, similar to that in the other categories. The urinalysis procedures included were chosen primarily for distinctiveness of chemistry. General Radiochemical Procedures B. Listing of Contents Procedure Author No. (principal) Title or method m 1. Welch Determination of Pu when large amounts 108 of Fe and Cr are present (LaF3 method) 2. Moore Separation and determimtion of Pu by 112 TTA extraction 3. Maeck Separation and determination of Pu in 114 ~ U-fission product mixtures (extraction of quaternar y alkylammonium - pluton yl nitrate complex into hexone - TTA extraction 4. Morrow 5. Hoffman Plutonium (anion exchange ) 116 Plutonimn (anion exchange) 105 118
Procedure No. 6. 7. 8. 9a, 9b , Author (principal) Hart (No author ) Rider Lingjaerde Rydberg Title or method Separation and determination of Pu from U and fission products in irradiated reactor targets (anion exchange — TBP extraction) U and Pu determination in highly irradiated fuel. (Hexone extraction, TTA extraction) Pu from irradiated U (cation exchange, anion exchange ) Separation of Pu from U and fission products (BiP04 precipitation, TTA extraction) 10. Rydberg Separation of Pu from U and fission products (adsorption of Zr-Nb on silica gel, precipitation of CUSJ TTA extraction) 11. 12. 13. Special Procedures Geiger Sheidhauer Kooi U and Pu from environmental samples of soil, vegetation and water (TBP extraction) Pu from environmental water samples (chemisorption on CaF2, TTA extraction) Pu from environmental water samples (BiP04 precipitation, co-extraction with ferric cupferride) 14. Larsen Separation and spectrophotometeric determination of Pu from U-Pu-fission element alloys (TBP extraction from HC1 solution) 15, Trowell Separation of Pu before spectrographic analysis of impurities in Pu metal (anion exchange 16. Trowell Separation of Pu before spectrographic analysis of impurities in high purity Pu metal (extraction chromatography using TBP) 17. Jackson 18. Zagrai Urimlysis Procedures 124 126 129 131 132 134 137 140 142 144 148 Separation of Np and Pu by anion exchange 149 Separation of Np and Pu by cation exchange 150 chromatography 19. Brooks Determination of Pu in urine (ferric cupferride extraction) 20. Perkins Determination of Pu in urine (PrF3 precipitation, TTA extraction) 106 153 155
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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
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Solution TABLE IV-2. Behavior of PU
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* Compiled primarily from the revie
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TABLE IV-6. Oxidation-Reduction Rea
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c.. Pu(IV)+ Pu(VI) Reagents Solutio
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Concentration Equilibrium Constant
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PU+4 has approximately the same ten
Page 25 and 26:
TABLE IV- 9. Ionic Potential of Plu
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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
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: TABLE VII-33. Basic Data for Critic
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
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Procedure 22. Determination of Amer
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concentrated nitric acid in a block
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Preparation of Sample The 24-hr or
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Procedure 24. Determination of Plut
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Procedure 25. Determination of Plut
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“The Actinide Elements” (McGraw
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48. D. H. Boase, J. K. Foreman, and
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108. 109. 110. 111. 112. 113, 114.
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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.
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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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