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3 0R1\IL ISOTOPES DIVISION 1'. B. O r r OAK RIDGE l'tational TJUOlUTORY Oak Ridge, Tennessee ogerated by UNiON C B I D E CORPOIUTION for t h e u ss ATOKiC ETrnGY C O ~ a s S I O T J S b

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5 n A B S T ~... ~T T~~OUUCTION lwsuiim OF m TABORATORY worn UESCRZPTION OF WORK WITH FISSION PRODUCTS... TUBORATORY EXPERDENTS WI ITX STABLE2 ET;EtIENTS. Page I ~ROCEI)T CONCLUSIONS AND I ~ C O ~ ~ N D ~ I O N S ACrnOVT;DGrn~ T METHODS OF KNALYSIS... DISCUSSZON... 6

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7 a c 4 Based on 8, h a l f - l i f e of years, a cal-cul-ated weight of g of L9n$/'703 i z i 9 g of fission-produced raree a r t h and- <americium oxides i m s s e p a r a t e d i n two rims by c a t i o n exchange (Dowex 501J-X4 r e s i n, 80 mesh), w i t h die&li.yylen?tria.minepentaacetic a c i d s o l u t i o n as t h e elmixi;. Prom.ethium, compu.ted as the element, was p r e s e n t Lo Yne e x t x n t of aboul 23.5 wt; $ i n?ne s'c,:x-t;ingmixture xnd was i n c r e a s e d t o 98 w t $ i n t h e firs-t; run and t o 99 w t $ Ln the second, w i t h y i e l d s of 58.2 w t $I and 61.8 w t $ r e s p e c t i v e l y. A decofitaxination f a c - t o r of 2.7 X l o 9 w a s r e a l i z e d i n t h e r e moval o americium from t h e product. This i s t h e highes-i;decontamination f a c t o r yeti achieved f o r t h i s s e p a r a t i o n, whichw i. 1 1 be used. a t ORNL. Procedures, 3 modified e l u t i o n cixve, methods of a a a l y s i s, losses, m a t e r i a l balaoces, and a d e s c r i p t i o n of t h e equipment a r e gi-ven. In a d d i t i o n, a possibl-e col.ori:atetric a n a l y s i s scheme ( q u a l i t a t i v e ) i s given f o r deterxkuiag t h e p r o p o r t i o n s of neodymium and p r o n e t h i m in a ~01uLio1i. INTRODUCTION I n 1-959t h e I s o t o p e s D i v i s i o n of ORHL used a n i o n exchange procedure t o produce about 20 k i l o c u r i e s of c i, t r i c : a c i d a t ph 3 was t h e eluant.' and Nd.203, about 3%; h$4103r & m a activity. a p p m x L m t e l y 65% p w e ; 0.2 M - The b p u x ' i t i e s rermining were S ~ 0 3 about 5 to a$; and about 40 mc of Eu With i n t e r e s t s t i m u l a t e d i n t h e use o f Pap703 i n x-ray sources, work was s t a r t e d a t ORNL toward developing ne7w and more e f f i c i e n t i o n exchange processes for t h e p u r i f i c a t i o n of prometiziwn. Expei-hents were done with st;a?ule r a r e e a r t h s, using as f e e d approxirnat&ly equal m i x t u r e s of 14 rare earths and yttrium. The c o n c e n t r a t i o n of each rare e a r t h w a s about '7 w-t; This work l e d t o t h e p i l o t - p l a n t process d e s c r i b e d i n tliis r e p o r t. IR. S. P r e s s l y e t al., P u r i f i c a t i o n of K i l o c u r i e Q u a n t i t i e s of Ym'"' by I o n ~ e h a n g e, O R N L - ~ C(JULY ~ ~ ~5, XI). I - $*

8 2 The systems dcscribed.. belotvrhad thc followi.ng condiiions i n common: 1. The r e s i n volume of' t h e column was 1800 ml 'l'hc flow r a t e was about 1 l i L e r / h r * 'The r a c e - e a r t h loadlng was one-tnird of the r e s i n volume. A b r i e f d e s c r i p t i o n of t h e e l u a n t s and t h e r e s i n s follows; a l l col- UjiJflS were operated a t 75"~.Imporiant observations are a l s o included: 1. One-half perc e n t diethyl.enetriaminepen-ta,ace t i c a c i d (DYPA} s o l u t i o n a-l p l 7.5; 1.2% cross-linked hydrogen-form Dowex r e s i n, 60 mesh. 2. One-half percent UTPA sol-ution a t ph 7.5; 4% cross-linked, hydrogenform Dowex 50W. A b c t t e r separatioii i m s obkiined w i t h t h e charge in r e s i n, apparently due t o l e s s r e s i n d l f f u s i o n One-half percent DTPA s o l u t i o n a t pli 5.5; form Dowex 5014, 60 mesh. 4. 4% cross-linked, hydrogen- One-half percent e t h y l r n e d i. ~ ~ i n e t e t r a a c e t iacc i d (bdta) solution a t I+$ cross-linked Dowex 50W r e s i n, 60 mesh, copper foim. ph '7.5; 5. C i t r i c acid. sol.ution, 0.2 l4, pii 2.9; 4$ cross-linked, hyds-ogen-form Dowex SOW r e s i n, 60 mesh. 6. percent c i t r i c a c j d s o l u t i o n a t pii 4-5; 476 cross-linked, in]d.i-ugen-form Dowex 50W r e s i n, 60 mesh. Accorilling t o resu.l.ts obtained from t h e use of systems 1-3, i t w a s determined t h a t E'TPA changes t h e ordinary order of e l u t i o n o f t h e r a r e earths. By u s e of c i L r i c acid., t h e y arc e l u t e d i n t h e reverse order of atomic number, lutetium corning o f f first; and y t t r i u m havia5 an apparent aloruic nurfl'ber of 65.5, e1ul;in.g between tci-bium and dysprosium. 'i'he f o l - lowing i s a l i s t of t h e e l u t i o n order f o r a DTPA system:. Lute tiwr? 1 Dysprosium 6 2. iiohxl1.m. 7. 'Terbium 3. Erbium 8. Europium 4. Thulium 9. Gadolinium 14. Cerium 5. YGLerbium S&rn3L"irn 15. Lanthanum II LO. 1.1c Yttri1m 12. Neodymiw 1..3, P r a e s e o ~. i i m F o r system 5, extrme1.y 5ood results were obiained a t t h e l i s h i end, with complzte breaks between Sm and Nd, P r and Ce, :e and ia. 'R. D. iiansen and. Stanley Chaberek,.Io Excharge Separation of Y-Ltrium fi:(x R a r e Earths w-i.lii U s... e t h y l e n e t r i ~ ~. n e p e n t a a c e t ", Acid lc._ I- D O C ~ n e i z a l. Co

9 d 3 h "he r e s u l t s of t h e work w i t h s t a b l e r a r e eal-ths inhicxled t h e f o l - l o w i n g: 1. Promethi-im of high puri.l;y could possribly be obtained f r o m low- c o n c e n t r a t i o n f e e d (less than 1.76 promethium) i n f x o passes, by t h e fol- loiring procedure : ( a ) One-half p e r c e n t UTPA solu-lion a t ph 5.5; 4% cross-linked, hydrogen-forin ow ex 5 0 r~e s i n ; co1umn temperature, 7 5 t o 80'~ By t h i s process, 3+i.trium w i l l b e e l u t e d between -tro.ukleson?e eu.e ropium and prornetnium. This add-ittonal element Ehoid.d pejlrnrit a l l t h e europium and mosi; of t h e s,.tmarium Lu be eliijged b e f o r e t h e promethium s t a r t s t o el_urte. A shaq s e p a r a t i o n of promethium and neod.ymim should also be mad.e. P (b) 2. A secon.d. pass Lhrough the c o l ~ ~ m ( a.f t e r. reconverting t o t h e hydrogen f o r m ), wit'n 0.2 M c i t r i c acid at pii 2.9 -to 3.0 and 45 c r o s s - l i n k e d Dowex 50M r e s i n a-i; 7 5 t o 80 C, should remove tne y t t r i u m and mos-l of t h e remaining scmmriurfland neodymium, From t h e renxxhder of -the 20 kil-ocixies of promethium produced II 1-959,? promethium of high p u r i t y should be ohtaified iil one pass tnrough an i o n exchaogc:. resin.,w i t h t h e DT'PA solutj-on. a t ph 5.5 and a temperature of 70 t o mot. Since t'ae or&er of e l u t i o n of yttrium and t h e o t h e r r a r e earths was changed i n t h e DTPA system, it i s hoped tinat t h e e l u t i o n o r d e r of Am2" i n t h e promethium feed sol.i.xt3.on w i l l. be changed a l s o. DESCRlPTION OF WOiX WITH FISSION PIiODUCTS D e s c r i p t i o n of Equipment. - With t h e exception of the preheaters and the c o n t a i n e r f o r the eluant, s o l u t i o n, all t h e equipment was i n s i d e a s h i e l d e d manipulator c e l l. Eluant Container. l i n e was used. -A Prelneater f o r Elua,nt l i t e r polyethylene b o t t l e w i t h bottom d r a i n -A g1a,ss t u b e (SO i n. long, w i t h a n i n s i d e diameter of 20 mi) was w e d w i t h a draw-off l i n e 26 i n. from t h e bottom. A 1 - l i t e r expansion f l a s k was l o c a t e d a t tine top, and a n i n l e t l i n z w a s Located a t t h e bottom. r i n g s and had tixi Tlie bottom h a l f of t h e t u b e w a s f i l l e d w i t h Raschig e l - e c t r i c a l h e a t i n g element wound on t h e 0iirtsi.de.

10 4 Vessel f o r Providing t h e Column Head. - A 500-mL round f l a s k with one t o a vacuum l i n e, a second t o t h e crude fin203 t h r e e o u t l e t s was used: dissol-ver f l a s k, and a t h i r d Lo t h e i o n exchange column. This f l a s k was used as a v e s s e l f o r t h e f e e d s o l u t i o n and as a vacuum t r a n s f e r v e s s e l from t h e d i s s o l v e r f l a s k. Ion Exchange Column. -A diameter of 1 5 rm was used. supported t h e r e s i n bed. jacketed c o l m i 4 f-i; 10% wi-ui a n i n s i d e A coarse, s l i i t e r e d - f i l t e r disk. a t t h e bottom I'he c o l m i has a capacity of 200 m l of hydrogen- form Dovex 5Od-X4. r e s i n, which was di-;--classlfied on an. 80-mesh screen. Flow r a t e of t h e e l u a n t w a s s e t a t about 200 r l / h r by use of a stop- cock on t h e column discharge. means of h o t water. The 'iempei-ature was held t o about 75 C by Dissolver Flask f o r t h e Cru.d.e Pm A 500-rd Erlenmeyer f l a s k. was used t o d i s s o l v e the crude oxide i n aqueous IiicI.. PROCEDURE A flow diagram f o r t h e process i s shown i n F i g. 1. Feed m a t e r i a l f o r t h e col-wnn w a s a p o r t i o n of t h e T%2O3 s e p a r a t e d at OFUL i n 1959 and was processed i n iwo runs. originally Analysis of t h e f e e d rm,terial i s shown below: ilpproxinmte Activi 'iy E Lcment pm '76 m e / d Am ~ About 6 rnc ~ c... X 10' ml_-' coimnts min"" Tihe rela'irivr r a r e - z a r t h and a ~ n e r i e i u ~ contents i f o r t h e iwo runs a r e sho>/ir ' ~ J c ~ o w : ---.I Fm203 b? 0 3 SmzO3, Ed203 Ru.n 1. ~. 22.6% g 22.6% 5.9$ g 5.9$ 71.2% g 4.00c Q Run %.. I g g g p

11 ITER EXPANSION FLASK i MOP1 IPU I..?'<TORC E L L Ei l l 4 N T PREH EATER, 50in. X 20 mrrl ID COLLUMkl ELIJEMT (DTPA) FEED, U T E R VESSEL I WAY STOPCOCK HEAT1 RIG COI 1- I O, 200-mlVOCUMC TO 110-v VARlAC H 2 0 IN --HOT ION CHAMi3Eil DISSOLVER FLASK F i g. 1. Flowsheet f o r 1k?47 P u r i f i c a t i o n rrom AUI*";. The crude oxide was d i s s o l v e d i n a 500-ml Erlenmeyer fl.ask i n su fi- c i e n t IICL t o bring t h e c o n c e n t r a t i o n of H C l i n t.he f i n a l solution t o l e s s t h a n 0.1.N. I The a c i d c o n c e n t r a t i o n was kept low i n order to rainimzze the s p r e a d of the rare-earth band during adsorption on the r e s i n. A f t e r dissolution., the crude proaethiuin solution was t r a n s f e r r e d Lo tlie column-head. vessel- by vacu-lun and t h e n adsorbed ora the hydrogen-form Dowex 5GW-X4 r e s i n i n khe coli.mn a t f u l l column flow (abou.t 250 ml/hr). The c o l i m w a s tineil washed with abou% 250 irnl of ws-ler t o remove excess a c i d from the system. E l x t i o n was done w i t h 0.5$ DTPA, the p H having been a d - j u s t e d t u 5.0 w-ith NHc,OH. Flow rate.was set at 200 n f l / l i n r ~ The discharge l i n e of the c o l m was a small-bore Tygon t u b e whjch penetrated an i o n chanber, TwhiCIi, i n t u r n, was connected i n t o an el.ec'r,r.ometer-recor~~r system to i n d i c a t e

12 6 and record any a c t i v i t j - e s as they were e l u t e d. Collecbion of 100-ml f r a c - t i o n s w a s begun when t h e electrometer f i r s t i n d i c a t e d a r i s e i n radioac- (This w a s due t o E I J. ' ~ ~ - ~ ~ '.. ) tivity. Each 100-ml f r a c t i o n w a s analyzed Tor Am241, Tpni147, 'When t h e a n d. i;;u peak was reached, samples of Lhe f i r s t and l a s t f r a c t i o n s of 1;he peak were analyzed spectrographically, by use of a containmeilt technique developed at, OKNL by t h e s t a f f of t h e Analy'iical Chemistry Di- All frac-lions w i t h promethium p u r i t y above 99% were combined as one product. another product. F r a c t i o n s of approximately 80% p u r i t y were combined as Each 100-rl frac-llon w a s a c i d i f i e d w i t h l.5 m l of concentrated HCJ., t o brzak t h e DTPA com-piex and was t h e n passed t b r o w h d r y - c l a s s i f i e d 60- mesh Dowex 50N-X4 r e s i n i n a column 10 i n. long and 20 m i n insid.e aneter. dj- Whcn a l l f r a c t i o n s were thus adso?-bed, t h e coluinn was washed with 300 ml. of d.isti?.l.ed w a k r t o remove excess DTPA and. H C 1, The promethi.im band w a s s t r i p p c d from t h e resin with 1 l i t e r o f 6 11 I HC1; t h i s was followed by a 200-ml-water wash. T'ne PmC1..3 so?_if,ion was t h e n evaporated- t o dryriess on a hot p l a t e and fumed w i t h 50 ml. o f 70% HN03 and s m a l l amoimts of 820;? t o d e s t r o y fiiies from 'ihe r e s i n. 'The residue, P m ( N O 3 ) 3, was filmed twice %-it11 50 irzl of concentlated i i C 1 i.n order t o reconveri it to PmCJ.3. Then it was dil-uted t o 500 rial approximately 1 N HCI., in wii."ch form t h e product was ready f o r s a l e. c iii Ana-, l y s i s of the two products from run 2 i s given below: Percei11;age of Fm Percentage of Sm 99 < Percentage of Nd I'e Y C e n tage of S t a r t i n g Ma, t e r i.a1 Am2 4.1 ~ l ~ Content, Content < 1-6.l. 8 Nil Nil Nil Nil 1- Promethiuml[+-_? T h i s i s o t o p e was d e t e mimd by l i q u i d - sc i n t i l l a t i o n b e t a counting an.d. end-window f l o w 4 y p e p r o p o r t i o n a l counting. ~ ~~ 3J. A. Norris, 'ThP <b-al_ysisof Promethiimi-lA7, 26, 1961). AnaJ.ysis 01th~Cli ( A p r. p

13 of t h e f l n a l product was done by spectrographic a n a l y s i s, w i t h g r z q h i t e eleeti?od.es. The weighed s~mpl.ewas analyzed f o r sanariixn and neotipium, but n o t for prome-lhium; t h e promethiim was detenxined- by &i.:f%"erence s( - Y'his Promethium-146. i s o t o p e w a s iden:tified by using a milj.ticharuze1 spectrometer, w i - L h t h e 0.46-, a.nd 1.02-Mev 0.'74-,,~~SIZUL"Lrays being iden.- t i f i e d is1 order tv d e t e c t it. The arml.ysis w a s q u a l i t a t i v e. ticha,nnel g m a spectrometer. The 970-kev and Mev :EuL5' gamma, rays ~ u r o p i u t ~ ~ ~TIE. assay for were i d e n t i f i e d. Rmericiun Detem-iix~tionof E ~ Pw a~ s made - -by-~ using ~ a~ m a~ t h i s i s o t o p e ',as mde by means of alpha p r o p o r t i o n a l counting and a multichsnnel gla.rm spectrometer. 60-kev gmmd radiat,ion was i d e n t i f i e d. The DISCIJSSION The DTPA e l u t i o n and t h e use of Dowex 50W-X/* r e s i n (hydrogen form) exceed.ed. expectations f o r t h e s e p a r a t i o n o f americium from prc~~nei't;lliwn. These experiments showed t h a t high-purity promethj.urn can be made a,nd t h a t l i t t l e o r no americium will reimin as a cont,aminarut, The arnericim was s e p a r a t e d from promethium by t h e change i n t h e o r d e r of e l u t i o n of mericium. In 3 system using 0.2 M - c i t r i c acid., the 8 m e r i c i m i s elu-ted. along w i t h t h e proinetixi.un. In.the DTPA system, wi- e r i c i m i s e l u t e d along w i t h t h e europium, which. charges t h e order of e i u - t i o u s o t h a t the americium no longer e l u t e s like el-emeilt 61 b u t Like element 63. A curve showing o d y t h e ord-er of el.ti.tion i s given i n F i g a 2. 'This graph shows only t h e a c t i v i t i e s present; s t a b l e neodpliwn- a.rxi s a a, rium are n o t sho~.rn. It i s hoped t h a t t i e c o s t of s e p a r a t i o n and p u r i f i c a t i o n can be reduc?d 3s a result of t h e s e experiments, s o t n a t large q u a n t i t i e s may be rmde s v a i l a b l e f o r r e s e a r c h on t h e chemistry of promethium as wel.l a s f o r t h e production of large-scale x-ray sources. t h a t adequate m-ount s of h i g h - p i x i t y FYn147 r e s e a r c h on t h e metal. h..rkrierracjre, i.-t; i s hoped rmj~tnus become avail.a''le for

14 ~ 8 UNCLASSIFIED ORNL-LR-DWG i i P_147 I ml FRACT ONS Fig. 2. Curve Showing Only the Order of El-ution of and Fm'-"/. The fol1ovin.g table shows Vile mterhl. balance for run 2. Cu.ri e s Percentage yrnl47 staiiing material Product, 99% pure 552. h Prociuct, 75% pure fiL47 ia 3m fractions Pm147 in Ed fractions Losses ?io d5fficully was encountered with radiation-induced decomposition of the DTPA during processing. Bowever, some high-activiiy Pm''+7 frac- tions were hcld for about two weeks before conversion to the chloride,

15 9 and a t.the end of t h i s p e r i o d a p i & p r e c i p i t a t e w8s found. It w a s w r y s o l u b l e in small. <mounts of I-ICl, i n d i c a t i n g that i t w a s n o t a UTPA precipitatee A J - t h o m it was not i n v e s t i g a t e d, the p r e c i p i t a t e may h a v e been a bi3sic s a l t of prorrietbium. T h e procedure f o r s e p a r a t i n g &?47 by use of M1PA elwmt and Dcmex 50d-X4- r e s i n (hydrogen form) resulted i n t h e p r e p a r a t i o n of 99%pure.Pm147. from T h i s process gxve t h e b e s t s e p a r a t i o n to d a t e. During t h e work it was noticed t h a t i n d a y l i g h t t h e purir'ied neo- dymium and promethiwn sol.utfons were lavender-pink from a, mercury-vapor L m p,. Ilowev~er,i n t h e.light; the neodymium soliulion w a s dark blue, w h i l e t h e promethiwn so1irl;ion r e t a i n e d i t s Lavend-er-pink colore This i n f o m a - t i o n may be useful t o -those who need t o q u a l i - b a t i v e l y analyze solukions. tha-t c o n t a i n t h e s e elements. N o work p was charge resic-. done t o determine t h e r a d i a t i o n s t a b i l i t y 09 %he i o n ex- The a u t h o r expresses h i s a p p r e c i a t i o n t o 11. A. Parker arid 3. A. Norcis, of the A n a l y t i c a l Chemistry Division, f o r t h e aimlyt3c:aj work. a

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17 UC-l+ ImEm-liL DISTRIBWL IOW OH31, Chemistry TID4500 ( l / t h e d. ) 1. C. E. L a s o n 83. E. 11. k r e e 2. Biology Library 84. R. E. Bigger:; 3-4. Central Research Library 85. C. E eldman 5. Heactor Division TAbrary 86. Donald Jacobs ,ahoratory Records Department, 87. W. J. Idaxtin 41. Ldboratory Records, ORNL R.C 88. F. L. Moore 4 2. ORNL - Y-12 Techrlical Lri.braZy 13. S. A. Rey-ml..ds Doclummt Reference Section 50. C. U. Su-sano 43. P a t e n t OTi ice (M. J. Skjmier) 91. J. C. V h i t e 44. Laboratory S h i f t Supervisor 92. E. E. Ketcheri 45+A. M. Weinberg E. Lamb 46. J. A. Swartout 95. Boyd Weavqr (Y,12) 47. J. P. Murray (K-25) 96. P. M. Tan-tz 4 8. ii. G. JOT~ZLII(Y-1%) 5 7.$1. J. Martin 4 9. E. H. Taylor 98. G. E. Creek 50. S. C. Lind. 99. B. J. P4assey 51. A. H. S n e l l E. MeHenry 52. A. BolLaender P. R. O r r 53. G. :E. Boyd 112. C. Ta, O t t i ~. g e ~ v 54.. K. Z. Morga;n 113. G. W. Parker 5 5. B. H. Kete1.1.e 114. H. A. Parker 56. A. 13. B r o s i E. E, P i e r c e 5 7. J. A. Morris (Y-12) 11.G. J. C. Posey 5 8. J. IE. Frye, Jr R. S. PressLy 59. J. A. Lane 118. S. J. liinshaw P. S. Baker 119. R. A. Robinson E. E. Beauchamp 120. H. T. R u s s e l l /4. T. A. Dutl-er 121. R. 14. Schaicii 75. F. N. Case F. V. Williams 76. B. F. Early 123. E, 1. Wya;tt E. Ramsey 124. E. G. Af fel J. H. G i l l e t t e 125, K. W. Hoff. 82. J. A. Jones EXTEmAI, DISTRIBUTION 126. Division of Research a n d IIeveI-opment, AEC, OR John I r v i n e, MTT Given d i s t r i b u t i o n a:; shown i n TID-4500 ( 1 7 t h ed. ) und.err Chemi st 1-y c a t e gory

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