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UNCLASSIFIED a *.** 9 -.” . APPROVED FOR PULBIC RELEASE a UNCLASSIFIED 9: ● *.** ● ● ●:0: ●:0:.e●9** . LIA-Z1Q3L CW14 REP*T GOUHION Copy No. a, ~ 6?EPRODLICTION Cig COPY AECRESEARCHANDDEVELOPMENTREPORT LOS ALAMOS SCIENTIFIC LABORATORY OF THE UNIVERSITYOF CALIFORNIAo LOSALAMOS NEW MEXICO PYROMETALLURGY EXPERIMENTS ON PLUTONIUM-RICH REACTOR FUELS (Project Status Report as of March 31, 195’7) UNCLASSIFIED ,- -. .--— .-—. ——-—. ----- . -.. —.-, -- m –—e= = .–— =-– ..=– -—=- -. ..~. r .- ~.——.- .-- .-. -------.. -.—--—.-— ------ -.--- —.. ..— .—— — -.=— ... --.=. .- ..__ .:. -.. .. ... —_*~08e 6.*. -*. .? ● — ._ -:. —. _-. — .. .._ ___ .=. -——— -—-_ —__ - —.-—. — . —----- .. -.-— --——= .— - APPROVED● e FOR PUBLIC RELEASE .. APPROVED FOR PULBIC RELEASE . ● e ● 00 ● 00 ● e* ● 9* be ‘ ● .00: : .:0. ● m ● *m ● m : : : :0 ● * ●0: ● 90 ● ● 00 ● LEGAL NOTICE This report was prepared as an account of Govern- ment sponsored work, Neither the United States, nor the Commission, nor any person acting on behalf of the Com- mission: A. Makes Wy warraqty or representation, express or implied, with respect to the accuracy, completeness, or Usefqlne>s of the information contained in this report, or that tfie U$e ,“oj’ any information, apparatus, method, or process disclosed’ in this report may not infringe privately owned ,rights; or B. Assure-es any liabilities with respect to the use of, or for dam ages,, resulting from the use of any infor- m ation, appar&s, method, or process disclosed in this report. AS used intheabove,‘personacting on behalf of the Commission “ includes any employee or contractor of the Commission to the extent that such employee or contrac- tor prepares, handles or distributes, or provides access to, any information pursuant to his employment or con- tract with the Commission.. Printed in USA. Charge 35 cents. Available from the U. S. Atomic Energy Commission, Technical Information Service Extension, P. O. Box 1001, Oak Ridge, Tennessee. Please direct to the same address inquiries covering the procurement of other classified AEC reports, * APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE 99*O ● *** ● 0 :0 ● * ● : ● 0 ● ●:0 : ●:0 :8* ● * UNCLASSIFIED LA-2132 C-16, CHEMISTRY--TRANSURANfC ELEMENTS (M-3679, 20th cd.) This document consists of 29 pages No. f 197 copies, Series A m LOS ALAMOS SCIENTIFIC LABORATORY OFTHEUNIVERSITYOFCALIFORNIALOSALAMOS NEWMEXICO REPORT WRITTEN: May 8, 1957 REPORT DISTRIBUTED: September 16, 1957 CIas by ~uthoritY PYROMETALLURGY EXPERIMENTS ON PLUTONIUM-RICH REACTOR FUELS (Project Status Report as of March 31, 1957) Classification changed to UNCLASSIFIED by authority of the U. S. hiu~tic Ihergy Commisaiom / . By REPORT LIBfMRY / Work done by: Report written by: JUL 2 ~ 1959 J. A. Leary J. A. Leary W. J. Maraman R. Benz Contract W-7405 -ENG. 36 with the U. S. Atomic Energy Commission ● *9 a ::0 ● *. ●b* ● .0 .04.. ● ● :0. : ● 0 ● 0 :: 9*. APPROVED FOR PUBLIC: RELEASE9* G ● * ● 00 ● 9* . :.. .. .— — <k’ *<f. ..’.”.. APPROVED FOR PULBIC RELEASE ● . ‘= i!!R!!P—. UNCLASSIFIED UNCLASSIFIED ‘“ ., . ... ‘, , . v 9* ..* ● .* ● ● -0 ● . ...-* .po.::: :.:. ● *. APPROVED FOR PUBLIC RELEASE APPROVED● 0 FOR● 9*. .PULBIC..*_ ● — .a—-.-.*e RELEASE ~.o. ● -0-—-9~– ~– . so ● ** ● a* (I*O ● O* ● O ● ● 00 ● ● ● : 0 s:: -.— ~{ ● ..~. ..& , * :0 ● * ● : ● * ● *:. : ●:0 :.* ● c -Z”” UNCLASSIFIED AIXYIRACT Experiments on the purification of plutonium-cobalt and plutonium- iron fuel alloys by pyrometallurgical methods are reported. Oxidative slagging appears to be an effective method for removing essentially all of the rare-earth fission product ele~nts~ whereas z~coni~) ~l-ybde- num, and ruthenium concentrations axe not seriously affected. Other methods, such as liquation, fluoride and carbide slagging, liquid metal extraction, and various fused salt systems are also being studied. ACKNOWLEDGEMENTS All chemical analyses were done by members of Group CMB-1 under the direction of C. F. Metz. Metallography was done by Group CMF-5 under the direction of A. S. Coffinberry. The advice of R. D. Baker on all phases of the project is also gratefully acknowledged. I UNCLASSIFIED ●☛☛$y.1-s ● :09 ● 9* .● . ● : ● ● ● * ● ● * ● :0 : ● * ● 9O . ●:. :00 :. .– ● .—’ —— .— ● ●’* ~ --_. ---- .*.. ● em ● — - “*. .* be . .-. - -:2. .4_c . ..~.-.:” ● . _ _.. —----- .. __ . ..- -- -—- -—B-=”.o ‘.. APPROVED_.. ———0 FOR● ‘—* PUBLIC● ● RELEASE 9* ● ● D9 APPROVED● ●** FOR● ● °9PULBIC● ●*: RELEASE . ● 0 ● ● 00 wki ● ● ● 9 * c :.: .● 0: ● mm ● * ● ● ** ● 0 APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE UNCIAJSIFIED FOREWORD Although considerable work has been reported on the purification of uranium fuels by pyrometallurgical methods, a dearth of information on plutonium-rich fuel systems exists at the present time. However, there appears to be considerable interest in plutonium pyroprocessing methods. It is for this reason that the following status report of current exploratory experiments has been written, rather than waiting to report when various phases of the problem have been completed. Periodic status reports on this project will be published in the future. ulVCfAJJIFIED 5-6 ● APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE TABLE OF CONTENTS Page ABSTRACT. 3 ACKNOWLEDGEMENTS. 0 . 0.......3 FOREWORD. ..o . .. ***~ 5 1. INTRODUCTION. ● . 9 2* EQUIPMENT. ● . ● ● . ● ● ● ● .9 3~ PREPARATION OF ALLOYS. ● . 11 4. LIQUATIONEXPERIMENTS. 16 5* OXIDATIVESIAGGING. 0 ● 19 6. CARBIDE SLAGGING. ● . ● . ● . 0 .27 7. FLUORIDE SIAGGING. 28 8. FUTURE EXPERIMENTAL PROGRAM. 28 ● ● ● ● ● ● ● ● 29 9* REFERENCES. LIST OF FIGURES 1. VACUUM INDUCTION FURNACE. ● . ● . ● 10 2. VACUUM CASTINGSET-UP. ● . .U 3* MAGNESIACRUCIBLE,TYPEA-392. 0 . ...18 4. STANDARD FREE ENERGY OF FORMATION OF THE OXIDES OF SOME TYPICAL FISSION PRODUCT ELEMENTS. ● . 21 LIST OF TABLES 1. COMPOSITION OF FISSIUM ALLOY CASTINGS. 13 2. MATERIAL BALANCE FOR ADDED FISSIUMEIEMENTS. 14 39 COMPOSITION OF IRON-FISSIUM ALJJ)Y.. ● . ● 15 4. EFFECT OF LIQUATION ON THE COMPOSITION OF COBALT FISSIUM. ● . 17 5. EFFECT OF LIQUATION ON THE COMPOSITION OF IRON FISSIUM. 19 6. EFFECT OF OXIDATIVE SLAGGING ON ‘THECOMFOSITION OF COBALTFISSIUM. .22 7 APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE LIST OF TABLES (continued) ~ 7. EFFECT OF OXIDATIVE SIAGGING ON THE COMPOSITION OF lRONFISSIUM . ● 0000. ● ✎✎✎☛✎ . 23 8. EFFECT OF TIME AND TEMPERATURE ON RARE-EARTH REMOVAL BY ● OXIDATIVE SLAGGING . ..0. ● . 24 9* EFFECT OF OXIDATIVE SLAGGING ON CONCENTRATIONS OF RADIOACTIVE FISSION PRODUCTS IN FISSIUM ALLOY ● (Experiment PIF-12). ● 0...0 ● C ✎ . 26 10. SPECIFIC ACTIVITIES OF FISSION PRODUCT ELEMENTS BEFORE AND AFTER OXIDATIVE SLAGGING (Experiment PIF-12) . ✎ ● ● 26 11. EFFECT OF CARBIDE SLAGGING ON THE COMK)SITION OF COBALT FISSIUM (Experiment PCF-8) . ● . 27 12. EFFECT OF FLUORIDE SIAGGING ON THE COMIWITION OF COBALT FISSIUM . 28 8 APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE 1. INTRODUCTION In conjunction with the Jks Alamos Molten Plutonium Reactor Experiment(1) (IAMPRE), a development program has been initiated to study Pyrometallurgical methods of purifying spent plutonium fuel. The relative merits of high-temperature processing have been discussed previously(2-5) and will not be reviewed here. However, certain special features of the proposed IAMPRE fast reactor are pertinent to processing objectives. The loss in fuel reactivity due to dilution by fission products is approximately ten times the loss due to neutron capture by fission ~oducts. Moreover, because the fuel is used in liquid form, it is not necessary to eliminate a high gamma radiation level, as would be required for many cases of solid fuel element fabrication. Thus, the purification problem is essentially one of fission product bulk removal, with no stringent specification on any particular contaminant. At the present time, pyromtallurgy experiments on plutonium-rich systems are being conducted on an 85–g. scale. When the exploratory phases are complete, potential unit operations will be evaluated at the l-kg. scale. Until shielded facilities for handling high-burnup plutonium fuel are available, all experimental work is being conducted with the synthetic spent fuel, “fissium,” similar to that used fm uranium fuel (6) systems at Iowa State College. 2. EQ.UIFMENT The vacuum induction furnace used for alloying, casting, and slagging is shown schematically in Fig. 1. Normally the melt was heated directly by means of a water-cooled current concentrator surrounding the ceramic crucible. In the alloying process, however, the melt was heated indirectly by the containing tantalum crucible. Energy was supplied to the current concentrator by an external water-cooled induction coil. A 3-KVA Ajax spark-gap converter was used to energize the coil. A 100 mm. diameter Pyrex tube with lubricated ground ends was used as the vacuum envelope surrounding the current concentrator. The top of the current concentrator also served as a vacuum wall, while the bottom of the current concentrator and the Pyrex tube were open to the vacuum can which was 9 APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE WATER IN =-’’’’’ATEROIJT I ZzzzLAL/’ /’ #’ /’ 1--”-1 A Tantalum pyrometer tube B Vacuum seal c Pyrex vacuum envelope D Water-cooled inductioncoil E Water-cooled current concentrator F Crucible G Molten alloy H Magnesia pedestal I ToP Of V~ULlm Cm J Neoprene flatgaskets FIG ● 1 ● VACUUM INDUCTION FURNACE 10 APPROVED FOR PUBLIC RELEASE APPROVED FOR PULBIC RELEASE I connected to an oil diffusion pump
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