.. . . - TOF I ORNL P 1968 .1" comm . jina . 1 - 1 2. 1 : . . 14 ... LA 21 11:13:333 . MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS 1963 Wah..... - - . - - - -:: .. . . TNY LE S " . T !.. . , it 1SN 11 FEB 2 8866 - - . ,!" 1. i LEGAL NOTICE . . . . - - Asya the Y ' . s I . - . ::: .. ..... .. in mammohan sitten consente artiklareamentin mentine warm W sva This report was prepared i m account of Governance, sponsored wort, Matthes the United States, nor the Commission, nor any person acting on behalf of the Commission: A. Maka may warranty or representation, aproved or implied, with respect to the norte racy, completeness, or usefulness of the tutormation sontatud ta this report, or that the wo of any information, apparatus, method, or process dirobored in this report my not intringe privately owned nehte; or B. Asramow my latilities with respect to the won of, or for damage rooting Breas the w of any information, apparte, method, or process dinclound la tuo report the .. As und in the above, "perro acting on behalf of the Commission" taludos m ployee or contractor of the Commission, or saplogue of mich austruotos, to the action that muck employee or contractor of the Commission, or sployw a mucha contractor properes, dissentrates, or provides access to any information purnannt to be sployment or contract with the Commission, or kin omployment with such contractor. : -..-...--. man - a i i . + + + rmers with r - ... . ,. .. . .. ... - ... - . . , in ::... ............ -... 1 .:- * . . . .. ostaviti cui considered as the inter ed winkelm TA a . nd waters of thir with the Union Carbide Corporation. *Research sponsored by the U. 8. Atomic Energy Commission under contract t and Application of Radioisotopes, " Augusta, Ga., March 20-23, 1966. For review in the ANS National Topical Meeting, "Large-Scale Production ! Oak Ridge, Tennessee Oak Ridge National Laboratory Chemical Technology Division . R. D. Baybarz V. C. A. Vaughen ORNG P-1968 CONF-660305113 by CURIUM PROCESSING EXPERIENCE* 18VT. IN MUCLEAR SCIENCE ABSTRACIE - RELEAŞIDID FOR ANNOUNCEMENT -; U - -. . . . - mid mais bien skaisista tai labai tinka audience then sectionalidades de la morte del mondo interno .'m.. - - .*'*".'..." SS. option ' momething to make center on and on a Satamist ..-.non m ir.. . . .. . - - -- .' . . - M e - - . . , . . . met oa yapmany more than . - > INTRODUCTION . . ...n .. *** -- -- .-.' i.. virrini .......... . - .. . - - -. , -. :,: The recovery of curium and americium is part of the larger trans- uranium element program at the Oak Ridge National Laboratory. Towards the goal of producing 1 g of californium-252 per year, targets of plutonium-239 were irradiated in a production reactor at the Savannah River Plant. The purpose was to convert the plutonium-239 to plutonium- 242, a better target isotope for use in the High Flux Isotope Reactor. Significant quantities of americium-243 and curium-244 were also pro- duced. Slightly more than a kilogram of higher actinides survived this initial irradiation, yielding about 550 grams of plutonium-242, about 300 g of americium-243, and about 300 g of curium-244. The Americivn, curium and rare-earth fission-product concentrates were transferred to ORNL for recovery and purification of the actinides. The bulk of these will be used as HFIR feed materials, while portions will be distributed for basic research programs. About 35 g each of americium and curium have been recovered to date. A second program recovered curium-242 and americium-241 from irradiated americium-241 targets, using processes similar to those used in the curium-244 program. Nearly 12 g of curium- 242 have been prepared. The curium produced has several end uses. Curium-244 is being used in basic nuclear research and as a target material for nuclear bombard- ment for the production of higher isotopes. It is also being tested for use as an isotopic heat source. The curium-242 program was initiated to provide material to test the SNAP-11 and SNAP-13 concepts for isotopic *** power generating devices. The processing was carried out in the Curium Recovery Facility. This hot-cell facility is equipped with tantalum, Zircaloy -2, and glass- lined equipment and can process acid nitrate and chl.oride (mixed) solutions through one or more cycles of solvent extraction in mixer settlers. The three primary goals of the Facility have been to test design and equipment concepts, to develop acceptable chemical processing, flowsheets for the Transuranium Processing Plant, and to recover curium Isotopes. Sometim inted to . i Oby, rimmi.ee, .. in:4. TL ...::: : * Priemerom hi , -7.** , . , . . * mesi...nisam n . 1 ci. Wi.. 4- : L-12 ! .. .. Seti * : ;.! . - ... . nings... vi mene : . . . . Mij . . . ... . i .................................... ............... amma - - - - - - - - - - - - -. -. vor . The basic separation step 18 the Tramex cycle, in which the actinides, in 11 M Lic.l, are preferentially extracted into a tertiary amine while the lanthanides remain in the 11 M Lici raffinate. But, since nitrate seriously reduces the separation factors, and, in addition, since sodium and aluminum chlorides have low solubilities in the prepared Teed, feed materials containing significant amounts of these ions must be pretreated to remove them before the feed moves on to the Tramex step. T!e clanex cycle was chosen for this pretreatment because it uses the same amine for a solvent and has similar stripping-bank conditions. This auxiliary flowsheet will be discussed are fully later. The programs represent a joint effort on the part of the Chemical Technology Division and the Isotopes Development Center and were given strong supporting work by members of the Analytical Chemistry Division. . . - ** Carmen de Processing The scope of the processing done at the Curium Recovery Facility is shown in Fig. 1. The two types of feed materials are the Savannah River Plant (SRP) concentrate in nitric acid solution, and irradiated americium- 241 targets. The targets are dissolved in hydrochloric acid at the facility. When the targets have a weight ratio of aluminum to curium less than about 50, the feed volume is limited by activity level; at greater ratios, the volume is limited by aluminum solubility. The product from the Clanex cycle is boiled down with Lic1 and put through the Tramex .cycle. Product solutions of curium-242 destined for source fabrication were converted to nitric acid solutions. . Curium-244 products were highly purified before separating the americium and curium. - - -- - Clanex Process: The Conversion to Chloride System and Removal of Aluminum •; As already mentioned, the feed material for the curium-244 programa is a nitric acid solution. It contains about 0.1 g of Cm and 10 g.of mixed lanthanide elements per liter of solution. Since the basic lantha- nide actinide separation process, Tramex, is a chloride system, pre- processing was necessary to convert the nitrate solution to a chloride solution. The method chosen was an amine extraction of the nitrate from - . 'I 1 ... S : . ORNL Dwg 65-11022 1,- . ii.. 1 "2 .. - . . : : Fig. 1. . OUTLINE OF PROCESSING DONE AT THE CURIUM RECOVERY FACILITY SRP 241Am TARGETS CONCENTRATE DISSOLVED IN HCI Am, Cm IN HNO3| ing's T CLANEX CYCLE NITRATE AND - ALUMINUM REMOVAL STEP : LOW Al/Cm RATIO If in. : , Y . 1 , TRAMEX CYCLE ACTINIDE RECOVERY FROM TIM LICI . .' . .- ... im . ---- . .: b, PRODUCT CONVERSION SHIP AS |_ SOLUTION :: . . -- ! PURIFICATION | AND SEPARATION STEPS ISHNO . . T '' 11 Y . :: ; . - SMS . 4 erry . . R . . 1 971 :::. 2 . 1 . 5 concentrated LiNO, solution. This process was termed the Clanex process, an acronym signifying the Co-Lanthanide-Actinide-Nitrate Extraction. ! Nitrate ion is preferentially extracted by amines, thus, a simple strip with dilute hydrochloric acid provided the chloride product containing the mixed rare earths and actinides. Feed adjustment for the Clanex cycle consisted in boildown with the addition of Lino, for salting and the addition of aluminum dihydroxy nitrate (DIBAN) to reduce the acidity. The Clanex flowsheet is shown in Fig. 2. The important variables in the feed were the nitrate concentra- tion of 7.0 M and the free nitric acid concentration of about 0.05 M. Note that the rare-earth concentration was 0.18 M. The extractant was a mixed &- and 10-carbon tertiary amine hydrochloride (0.6 m in diethyl- benzene) containing a slight excess of acid. The pregnant solvent was stripped with 1 M HC1. The product was washed with two reagents. The first, a more concentrated form of the extractant, provided the extra amine sites required to exchange chloride for the nitrate ions associated. with large quantities of the stripped metal salts. The second wash, di-2-ethylhexyl phosphoric acid in kerosene, removed some corrosion. products and fission-product zirconium from the product. . ... Tramex Process: Separation of Actiaides from Lanthanides - - The Tramex solvent extraction flowsheet is based on the preferential extraction et trivalent actinide chlorides from lanthanides by a tertiary amine extractant. The Tramex feed adjustment was made by a simple boil- down of the Clanex product with sufficient Licl io make the resulting volution 11 M in Lici. The flowsheet is shown in Fig. 3. The feed is 11 M in Licl and 0.25 M in free HC1, plus a holding reductant, Snci,. The Snci, prevents the cerous ion from being oxidized to the extractable ceric form by the radiolysis of chloride ion. This use of Snci, was first demonstrated in laboratory studies at the "Savannah River Laboratory. The Tramex cycle uses the same extractant as the Clanex. The pregnant solvent 18 scrubbed with 11 M Licl and then stripped with 1 M HC1. Wash I 18 the nitrite form of the amine extractant to aid in ruthenium decontamination. The zirconium removal step is the same as I before. In! W .'' WA . SCRUB 170.2 M LINOZ 0.22 +0.02M LICI 0.0250.005 MHCI . i. ORNL Dug 65-3157: FEED :- ** EXTRACTANT 5M LINO 0.65 0.025 M Adogen-HCI SO.18 M RENOZ 0.03 0.01 M HCl in ~0.25 g/liter 244cm Diethyl Benzene. 0.67 M AI(NO3)3 0.05 0.025 M HNO3 NOTE: Total Nitrate=7.0:0.2M. EXTRACTANT, 30. : FEED 1 . . . . SCRUB EXTRACTION - - - - . . 1 -165 RAFFINATE . - 1 M . .. 11 1 . STRIP 1.0 3.0.1 M HCI WASH TI IM Adogen-HCI in Diethyl Benzene WASH TI 0.5 10.025 M D2EHPA in Amsco . QED . . -- - . r . 540 ::::: : A* 1 3 . STRIPPING NO. - Το WASTE . . . . . - IT BACKWASH BACKWASH II .. . 1 . . . . . A -.'.- - " .. * 17 .. .. . . . . . .. .', 1. / :: ;, . . . . K , . - . Hi -"- - -- . 10 . : TE VI. T! . : . ST . y .. . 1 . *** 1L . * 4 . ill PRODUCT -209/liter RE 0.209 liter 244cm . . : | . . 1.* *. . . . . Lorcatica . . ' . TOP . . UN . ' i * 74 "' ' . omni. ?'.. . 5 riit : .. . !" yi. . . . i, V1 ' " 2. : Home . " . "; . . ' f . . ni . . TH . . 1 . '. . . '. SZE 1:19: . LE . i . . LIM HCL . . i ', Dr.,: . . ,* . . 4 . . ..:: CSERE LIM . K .. NET 3 . Krite " - > TV Sil! : . L . . 174 * L mi . Sr. SP. 1113 LY . . TEL . T / .' .. ! ..VO .. w . . . . .! . . SY Wic C . f. H y Fig. 2. CURIUM RECOVERY FLOWSHEET, CLANEX-B- 3 * VY . 4 . 1, . Y , " . SOY . LA ya NIUM YTI * 4 . ' . ! . .. . 3.3 Det . A . * T. Mr. 71 ' * , . . 1 .. .. . . ", . . A A 1 i ? TOR . N2 * sto . .A . '. 1. . . - . . VAN . ! ir !' . - * 1 .! . 2, ". 11: . .. , . iun . S **. y 2 Y. in ! * 1' .. . . . ti . . . ! S , ' . . . ." . . STI! 79 . ." . , i " Ha - V .: . . . 2 + . . ..: . V .. ... mark AS . . . . . . .! . . . 1 :.? . - . 4 1- - . : . . . - .1 . . . - S. . NL12 ter, X I - :- CU . 1 ily .4 . i . . . -, S . ,4 . . . - - - - PE ! v . - . * , - + : . . DXC ,- 'T . ; -, ', ::::: :: . . . # 3 . . . - . . . ( . !. . . • r im : '... s. . y ' 1 - -- . I. 1 - . T PT. ' P " . + - - .. . . . :. r. - - :: ... . i S. .." . . . . . . * . -. . . SCRUB 11.0.1 M. LICI 0.03 0.01 M HCI FEED". II $0.2 M. LICI. 0.14 M RECI: 0.2 g/liter 244 cm 0.25 +0.05 M HCI C.I M SnCl2 . is..VI M NO3 : ORNL. Owg 65=4771 EXTRACTANT : 10.6 2 0.025 M Adogen-HCI 0.03 0.01 M HCI in * Diethyl Benzene. NOTE::. EXTRACTANT 1.24 FEED + SCRUBSC 365 - (70 Oo . .. - - SCRUB EXTRACTION . 1 DRAFFINATE ...-..- .• " 1 . STRIP 1.0 : 0.1 M HCI WASH I 0.6 M Adogen-HNO2 in Diethyl Benzene, cold WASH T 0.5 20.025 M DZEHPA in Amsco__ 60 io . -575 575 (575) - STRIPPING .. BACKWASH | BACKWASH . . . WASTE .. 150 .. . . . . . - - - wat WASTE TO WASTE PRODUCT_ ORGANIC :: STORAGE :: 0.13 g/liter 244 Cm LIM HCI -Fig. 3. CURIUM RECOVERY FLOWSHEET; TRAMEX-B • • -.- - - -- - - - - . 1 . . i 1 - ..8 :: 11. . mult nieminin on .. . na . . . " in we mieristici . ...... :-, V 1. !--: resursa painamminant kanaganoret motorn - Purification of 244cm - 243 Am Product The Tramex product is further separated from fission products and other contaminant ions by small-scale separations in laboratory glass- ware. Nickel, cobalt, and copper are removed by precipitating the curium wi.th excess ammonium hydroxide. These contaminants remain in the filtrate. During a later precipitation, chromium, as the soluble chromate, is sept qarated from the curium-americlum hydroxides, which are precipitated by sodium hydroxide. The other ionic impurities, as well as residual fission products, were removed by a Licl anion exchange step using a resin column - chemically very similar to the Tramex process. Separation of 243Americium and 244curium In the curiun-244 program, the ameicium and curium are separated by oxidizing the americium from the trivalent to the pentavalent state with sodium hypochlorite or potassium persulfate. The oxidized americium precipitates in carbonate solution as the potassium americyl double carbonate (K,Amo (co)n) and is easily removed by filtration. About 99.5% of the americium was removed from solution, with about 1% of the curium remaining with the precipitate. The curium content was reduced to 0.02% by & second oxidation and precipitation step. -- - ;......... i. . ." . - o n . ::. . . ... :: isan. . - 1.- . : : : :* ini . YTM - N . ! Curium-242 Processing Curium-242 processing differed from the previous work in two main categories. First, the source of feed material was irradiated americium- 241 oxide, canned in aluminum. It was not necessary to perform a Clanex cycle to remove nitrate with this material. However, the large amount of aluminum was most easily removed by processing through the clanex cycle. The second major difference was the high activity levels encountered. Curiun-242 has a specific activity of 3.83 x 1012 counts minimg., or a heat evolution rate of about 120 w/g compared to curium-244 which has a rate of only about 3.W/8. Radiolysis and acid loss from Iramex feed was ** about 0.7 meq/whr, corresponding to a G value of about 1.9. In other. words, all acid in the curium-242 feed (about 6.3 M) could be consumed in about 24 hr. At first, it was necessary to make frequent acid additions to maintain a stable feedo Later, an acid holding solution was devised. , .. } ...un 1 19 - ...: ::;; - 3 - 4- ' . " W ... . - M . . Another effect of the high radiation levels was the increased rate at which oxidizing materials formed in the feed. The net effect was the early depletion of the Snci, reductant, which resulted in a strong cerium breakthrough to the product. In a second framex cycle, care was taken to limit the adjusted feed batch size to prevent an accumulated exposure of greater than 600 wnr per equivalent of tin. Another reductant, hydroxyl- amine hydrochloride, shows promise as a nonextracting reductant that can be added "on the fly," just before the fled reaches the mixer-settlers. The highest feeâ concentration used in Clanex processing was about 18 w/liter, with no indications of difficulty. The highest feed concen- tration demonstrated successfully in the Tramex process was 6 w/liter. It is hoped that this may be raised to about 10 w/liter by the continuous addition of reductant. Recoveries averaged from several runs are shown in Fig. 4. These are 98% for the Clanex process and 97% for the Tramex. Purity of the Product As to purity of the product, the feed material for the curium-244 program had about 100 g of rare earths per gram of curium of which 30 were fission products. · A gamma scan of this material is shown in Fig. 5. Plotted on the ordinate are the relative Intensities of the beta-gamna activity associated with about 0.7 ug of curium-244. The 'abscissa repre- sents the energy of the gamma emitters. The low-energy (but high intensity) beta-gamma radiation 18 filtered out by a 2-cm cadmium shield. The peaks are identified in the figure. For comparison, the purified, separated curium-244 gamma spectrum is shown in Fig. 6. The coordinates are the same as before, and the sample contained 120 ug of curium-244, an increase in curium content of about 170 over the previous figure. The only identifiable peaks are at about 0.3 and 0.6 Mev - resulting from durium-243 and cúrium-242. The curium-242 product after one Clanex cycle and two Tramex cycles was also quite pure radiochemically (Fig. 7). Estimates of the contributions of the contaminant ions are shown as shaded areas. This second-cycle Tramex product met the purity require. ments for source fabrication. “ ** Decontamination factors during the curium-24's solvent extraction processing were about 500 overall for gross gamma, and about 2000 and . . . . . . . . - *..., . . ... - .. VI. .... . cu . - *** 1.! . . - : . . . ... . . .. en ". * ** V - : : - ' . - . . ". . ORNL Dng 65-8872 . www........ about S . .. . ) 1 Fig. 4. 242 Cm MATERIAL BALANCE (%) . . . . . 1. ... - . *** * . FLOW- SHEET RUNS ORIG. IN LOSSES : ADJUSTED RAFFI- WASTE MATERIAL: 1 FEED NATE ORGANIC MISC PRODUCT | BALANCE 10 11 . I . . CLANEX : 100 <0.01 0.4 98.5 .. <0.1 | 0.1 98.0 97.0.1 071" TRAMEX 100 1.2 0.5 98.8 . - - , . 1. - .. . . . Sii ' . ;.. i . ' * i . ' . 1 : * . ' . 1 . 11 1 1.: -- - . 7.15., : : . . . - - . . 2). iinin 1 1. , . . : . . .. . . - - - - , ii por parte pommes from Ti. : *:: Martinica :: New St. ORNL Om Serama - -- - - ....... S01 0.7 GRAM 244 cm + CADMIUM FILTER ws on ropes pridonismo; inom "sti imoriad . perly the the entrih room's nie's vie RELATIVE IN . . Y. 1.0 0.8 . 1.2 1.4 M. E.V. . i.'!.. Fig. 5. 244 Cm FEED SOLUTION . . town . LE int . . : & M T. : 1 1. :: ** . *7'. - .- .. . . . . - Li - !! . it ; * * * 1 . Rivilih... ! . .) . C . . 1 . .. S . V . ." f 1. - , i.ir 2 . . .. TV l A KA > . .. - ' - . P . -": . . . - 1 1 .. 1 ... M mingly Fig. 6. PURE 244 cm 1 ........ . 1 . - .' MiEV I . - 17. T . . .. .:: ., .. , .. . . . ... . . . :... ... . . Lii! - . - - - Sie :- * RELATIVE INTENSITY . watch online translation entertainment -- ia.de ...... *--. . .. .. .... . ORNL Dug. 69-4154 somn .' ' # . Y 1 imti..... om m a n intense on.co..maaaminimo mechaniniamencienc .re. -. :! !.. 12re . . .. . ... . ... diese r .. ....... .. wjetozar Motonta a meg . . .. . . ... vv. :-*. ..- .. - - - ... - ... . 1 :.', ...: sos: ... ..... . .. . ORAL Ong • :... . 103 _103R -242CM 4141ce and 242 Cm FILTERED OUT. . ... ..: '.. . ....... ..rec .. 144cm RELATIVE I DUE TO: ONTANEOUS FI OF 242 144 1.0 : 1.5 M.E.V. myshirw ... sive Fig. 7. Gamma-ray Spectrum of 242cm Product.. .. : .nem . . bi men in ..1 1 1. . YA ... ... 24 . merimarnice ... ... 1 . .... . us. - .. --- . ..... :, .: mri: . il kos. name . .'... . : .'. . - - ; - *.- 3000 for certain gamma fission product emitters. Decontamination factors for the curium-242 program are listed in Fig. 8. A zirconium decontami. nation factor of about 300 was attained on the Clanex cycle and, as je expected, no decontamination from lanthanum or cerium. The first Tramex cycle was ineffective for cerium decontamination because of the 1088 of reductant through radiolysis, however lanthanum-140 decontamination was > 1800. The second cycle demonstrated the effectiveness of the stannous chloride reductant. Overall decontamination fac'cors are given at the bottom of the figure and vary from about 200 for cerium to better than 20,000 for ruthenium. Ionic purity specifications were very tight. Since large volumes of solutions were accumulated and concentrated by boiling down to a small volume in the solvent extraction processing, the incoming solutions had to be very pure. Typical product compositions and specifications for source fabrication are given in Fig. 9. The principle impurities found in the product were lithium, nickel, zirconium, iron, and calcium, la that order. The separated americium and curium products had less than 0.1 wt % impurities. These were predominantly alkali-metal salts. Radiation Effects Several interesting alpha-radiation effects were noteå. Cerium oxidation and acid loss have already been mentioned. Closely akin to these was gassing or fizzing. Nitric acid or pure nitrate solutions did ; not gas appréciably even up to concentrations as high as 200 w/liter. However, hydrochloric acid solutions gassed continuously, like ginger ale or worse. Methanol effectively reduced gassing in hydrochloric acid solutions containing pure curium-244, but it did not inhibit acid loss from lithium chloride solutions (Tramex feed) containing sonic impurities, such as iron, chromium, nickel, and tin, the reductant. However, a mix ture of methanol and formaldehyde was successful in holding the acidity for up to one week, if added at the proper time. Heat evolution and violent gassing were experienced when chlorides and nitrates containing large amounts of alpha emitters were mixed. Another interesting phenomenon was alpha-induced corrosion. For example, purified curium-244 (equivalent to 200 w/liter, 10 2 M HNOZ) ... " www.wan i .:7;, tel : . TE . $ .. :: . .. i . . . . . . .. . . . " ':. . * . . ** - I i e. t ,.. meie tee ---- - - - : 0 . :ORNL Dwg 65-8873 Fig. 8. 242 Cm DECONTAMINATION FACTORS 9521 95Nb103Ru 140La 144ce 500 CLANEX 300 TRAMEX: Ist CYCLE 180° =1800 smallb * 2nd CYCLE - 84 160 ... OVERALL 1 >9x103 >500 >2x104 >1800 -200 - NOT DETERMINED a. Zr-ND REDISSOLVED FROM DISSOLVER VESSEL DURING REPEATED FEED ADJUSTMENT. • b. SnCl2 WAS DEPLETED BEFORE RUN WAS COMPLETED. (>600 w-hr/equiv.). Dwg 65-4774 + + + 2 A Fig. 9. PRODUCT PURITY RUN ELEMENT SPECIFICATION TR-2(A) TR-2(B) TR-3 Ni (gliter) 1.0 0.2 0.24 0.8 Total Bi, Pb, Ca, Si, Mn, 1g/g cm) 0.05 0.02 0.02 0.02 Total Al, Mg, Cu, Fe, Zr, Cr, Co, Mo (g/liter) ; : 0.10 0.06 0.69 Total Li, No (g/liter) 10.0 19.2 . 7.0 13.1 :: Cm (g/liter) 0.951 0.994 3.74 2 in is. .. . ::: 1 . .. I - ' ::. . . . - .. re . . 11 . . , - A y 1ii! . . A : - 2. . 1 + . ET 1: . . . * . + . 1X 1 . 1 ::. LA 4 ' L Desa - . . .. S. . -- . .. Y . . 7 .. . .. 1 : ...: 5 : ë. . . .:- iei - . . 1 " 73 . - - - - - . . 27 . .. was stored for six weeks in glass. About 100 cc of granular silica accumulated due to alpha-particle attack of the glass walls. The silica was easily removed by filtration. Pentavalent americium-243 proved to be suprisingly stable in nitric acid solution. Spectrophometric examination of 1 M HNO, solutions in- dicated a half-life of 18 days for Am>* at 25°C. This stability seri. ously inhibited oxalate precipitation of the americium; in fact, only about a third of the americium precipitated following the addition of oxalic acid to a nitric acid solution, and the precipitate that formed was lemon yellow, not the reddish tan of Am»* oxalate. The americium remaining in solution was colorless and was stable for days. It was finally reduced and precipitated by adding NH,OH •HC1 and heating. The concentrated curium-244 solution had a reddish glow as seen in Fig. 10. The solution (30 w/liter) glowed strongly enough to allow an auto photograph through 4 ft of lead glass window. wani, ..... .. . .. - -- " . ::. .. CONCLUSIONS In conclusion, about 35 g each of curium-244 and americium-243 have been prepared in pure form. About 12 g of curium-242 have also been prepared. Processes have been demonstrated to yield recoveries of about 95% across the two-cycle (Clanex-Tramex) process, with demonstrated decontamination factors of up to 500 for gross gamma, 2000 for ruthenium- 106 and europium-154, and 3000 for cerium-144. Ionic purity was suitable for source fabrication. Final purification and separation of curium-244 from americium-243 yielded an americium product of better than 99.9% purity and a curium product containing about 0.5 wt% americium. Beta- sauma emitting contaminants were below detectable limits. . :.: .:. . . .,.: :.::;"..., :.:.:.: : .. - . . . "-:.."* ... - . . . ... .. .. .. . . . .. .. .. . . . i . . . . . . MONI A LANN IMA " - t t- .. . . . - . , 4 业 ​11 , l ) 14 . , : 4 - B . :, il: : *」 :: : : .F sr 1 | 11. , * try A ” 、 。 * ” * |- - - . ·中 ​. ORNL PHOTO 68542 . . EAT 「. ,在​”, . " 直 ​: HEY: 得到更 ​41 11 . 「. . 年 ​垂直 ​。 了 ​1, 在19 . | 年11:11 | | 14 | , . | | 11 Tai11111) i 出​:44 · tar, A 「是 ​, 」! Niki ve, 事 ​, F1 th, .. { .msi :19 :s . 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