17 : - | OF 1 ORNL P s1603 EEEEE MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS - 1963 i VER. T . ORNC-p-1603 Conf-650918-7 . 2 1965 QCT 6 UNEXPECTED RATE EFFECTS IN THE EXTRACTION OF RARE EARTHS BY DI(2-ETHYLHEXYL) PHOSPHORIC ACID* D. J. Crouse D. E. Horner Oak Ridge National Laboratory Oak Ridge, Tennessee -LEGAL NOTICE The report we prepared M M of Governo poucored wort. Metoher the Bund mate, we the C incton, more porno settes au boht of the Countetan: A. Yan ay warranty of ro t ation, an d or implied, a roupast to the acor- they, w picture, a wote now the formation owned in the report, or that the man a nagy formation, Apparatus, method. * proces theolood in this report may not fuering Mit went or - 3. Assumos sky liabilities with respect to the use of, or for damages resulting from the wo of any information, apparamo, wood, « mon drolourd to the reports dow n the home, porta notte an holl of the Countwater" Inchen myne na tretur dhe Count, or play on otrotor, at det helt piesne o santractor of the Coundation, or player of wel contractor nepares, him, w ho , latina pro Merlot « contrat via the Countdown, or woonplegue with me onatriotar. To be presented at the INTERNATIONAL CONFERENCE ON THE CHEMISTRY OF THE SOLVENT EXTRACTION OF METALS on September 27-29, 1965; Harwell, England RELEASED FOR ANNOUNCEMENT IN NUCLEAR SCIENCE ABSTRACTS Research sponsored by the U. S. Atomic Energy Commission under contract with the Union Carbide Corporation. UNEXPECTED RATE EFFECTS IN THE EXTRACTION OF RARE EARTHS BY DI(2-ETHYLHEXYL) PHOSPHORIC ACID* D. J. Crouse D. E. Horner Oak Ridge National Laboratory Oak Ridge, Tennessee ABSTRACT In extraction of fission product rare earths with di(2-ethylhexyl) phosphoric acid from tartrate- (or citrate-) complexed waste liquors (275), the rates of extraction are decreased by the presence of certain metal ion contaminants, such as iron, aluminum, and particularly chro- mium. Apparently, these metal ions react with the rare earths ions and tartrate in the aqueous phase to form non-extractable complexes that are slow to dissociate. The magnitude of the effect is different with each interfering metal ion and also for the different rare earths. Increasing the tartrate concentration increases the rates of extraction. *Research sponsored by the U. S. Atomic Energy Commission under contract with the Union Carbide Corporation. ty TERRA UNEXPECTED RATE EFFECTS IN THE EXTRACTION OF RARE EARTHS BY DI(2-ETHYLHEXYL) PHOSPHORIC ACID* D. J. Crouse D. E. Horner Oak Ridge National Laboratory Oak Ridge, Tennessee INTRODUCTION The efficiency of metal recovery by solvent extraction methods is sometimes adversely affected by metal contaminants in the aqueous phase which themselves are extracted and thereby decrease the amount of ex- tractant available for recovery of the wanted metal. In addition, ani- onic constituents in the aqueous phase often decrease the extraction efficiency by complexing the metal value in the aqueous phase. In this paper we will describe a system wherein interference occurs through still a different mechanism in which metal contaminants apparently a880- ciate in the aqueous phase with the metal value and interfere with ex- traction. In the processes, developed for recovering fission products from reactor fuel reprocessing wastes, strontium and mixed rare earths are co-extracted with di(2-ethylhexyl) phosphoric acid (D2EHPA) from tartrate- (or citrate-) complexed solutions at a pH of about 5. The complexing agent is added to prevent precipitation of hydrolyzable metals at this low acidity where extractions of strontium are optimum. Rare earths are extracted slowly in this system. It was noticed in process studies at Hanford Atomic Products Operation that cerium extractions with D2EHPA Research sponsored by the U. S. Atomic Energy Commission under contract with the Union Carbide Corporation. from citrate-complexed solutions were sensitive to the presence of chromium in the feed solutions, and this effect was subsequently inves- tigated further at Hanford. This paper describes studies at the Oak Ridge National Laboratory of the effect of chromium and other metals on rare earths extraction from tartrate-complexed solutions. EXPERIMENTAL MATERIALS AND TECHNIQUES The organic and aqueous phases were contacted by mixing vigorously in an open separatory funnel with a high speed interface stirrer. Most of the studies were with simulated Purex IWW waste, similar in composi- tion to that produced until recently at the Hanford plant.5 Prior to the extraction tests, sodium tartrate was added to the solution and it was ad justed to the desired pH and simultaneously diluted 3-fold with sodium hydroxide solution. Appropriate radioisotope tracers were added as an analytical aid. The approxima te composition of the adjusted feed and of other aqueous solutions used are listed with the data for each experiment. In all tests the organic solvent was 0.2M D2EHPA-0.1M NaD2EHP-0.15M TBP in Amsco 125-82 diluent. This D2EHPA/NAD2EHP ratio provides a buffered solvent that minimizes Na*-** transfer between the organic phase-and the low-acid aqueous 'phase and simplifies maintaining the pH at about 5. EXTRACTION OF RARE EARTHS Extractions of rare earths with D2EHPA from acidic nitrate solu- tions are rapid. The distribution coefficients increase with increasing atomic number and differ for adjacent rare earths by a factor of about 2.5.16) In extractions from tartrate-complexed Purex IWW waste solu- tions at pH 5 (Figure 1), however, extractions are relatively slow and the order of extractability, at least up to 30 min contact time, 18 exactly opposite, 1.e., Ce > Pr > Nd > Pm > Eu, to that obtained from simple nitrate solutions. Ageing the ad justed aqueous feed prior to extraction decreases the rare earth distribution coefficients, probably because of slow forma- tion of aqueous complexes. In extraction of europium and cerium from tartrate-complexed feeds, this effect was small for ageing periods in the range of 1 to 24 hr (Figure 2). Cerium distribution coefficients decreased markedly when the ageing time was extended to 8 days. A much larger effect of feed ageing time on europium extraction has been observed for citrate-complexed feeds.? In all the tests described sub- sequently, the adjusted feed was aged for 1 hr prior to extraction. Effect of Individual Metal Contaminants Experiments in which metal contaminants were added one at a time to a nitrate-sulfate-tartrate solution showed that iron, aluminum, and chromium, particularly the last, depressed the rare earths extraction rates (Figure 3). Extractions of chromium and aluminum in these tests were negligible (Table 1). Although some iron was extracted, the amounts, at least for contact times up to 5 min, were not large enough to repre- gent significant competition for the D2EHPA extractant. With 0.003M chromium in the aqueous phase, cerium distribution coefficients were 8.5, 25, and 120 for contact times of 1, 10, and 30 min, respectively. By contrast, cerium and europium coefficients were TABLE 1. EXTRACTION OF CONTAMINANT METALS (Additional data for tests described in Figure 3) Contact · Time (min) Fe Organic Phase Analysis (3/1) A1 0.21 < 0.001 <0.04 < 0.04 < 0.001 0.41 0.44 <0.04 1.2 <0.04 < 0.04 < 0.001 < 0.001 <0.001 2.9 5 , higher than 700 in l-min extractions from solutions of similar composi- tion but containing no contaminant metal ions or containing only nickel (0.003M). The magnitude of the effect of each interfering metal was different for the different rare earths. Iron. depressed extraction of europium and neodymium more than extraction of cerium, while chrc- mium depressed extraction of cerium more than extraction of europium. In extractions of europium from a solution containing 0.0014 Eu, the distribution coefficient (3 min contact) was > 1000 with no chro- mium present but decreased to 88, 32, and 12 on addition of 0.001M, 0.002M, and 0.01M chromium, respectively (Figure 4). Ageing the Aqueous Phase Between Extraction Contacts The slow extraction of the rare earths is due to slow read justments y to equilibrium in the aqueous phase after the system has been distur.bed. This was demonstrated by batch extracting tartrate-complexed Purex IWW waste (pH 5) for 1 min and ageing the raffinate for various periods be- fore contacting again for 1 min with fresh solvent. The europium dis- tribution coefficient in the second contact was 5 with 6 hours between contacts compared with only 0.37 with 2 min between contacts (Figure 5). The total amounts of europium extracted in two contacts were 97.6% and 88.8%, respectively, for these two conditions. Effect of Tartrate Concentration The adverse effect of the offending metals on extraction of the rare earths can be partially overcome by increasing the amount of ex- cess tartrate in the solution. For example, increasing the tartrate concentration in ad justed Purex IWW from 0.27M to 0.5M increased the europium distribution coefficients (5-10 min contact time) by a factor of about 10 (Figure 6). Effect of Temperature As would be expected, the rare earths extraction rates increase with an increase in temperature. In extractions from tartrate-complexed, simulated Purex [WW solution at pH 5, europium distribution coefficients were a factor of 2 to 3 higher at 45°C than at 25°C for contact times in the range of 3 to 10 minutes (Table 2). At 45°C extractions dropped off rapidly for contact times longer than 10 min because of excessive iron extraction. DISCUSSION While the mechanism of the rate effect has not yet been investi- gated, some speculation may be appropriate. Remembering that the rare earths are extracted here as cations, we may expect maximum extraction when they are present as the uncomplexed +3 cations. Tartrate complex- ing should be expected to lower the extraction (whether of +3 cation or of +2 or +1 complex cation), but it is found to be still high and rapid with up to 0.5M tartrate. We suggest that in the presence of chromium (and similarly, with certa in other metal cations) a double chromium-rare earth-tartrate complex 18 formed, which 18 slow to dissociate and thus slows the extraction. Then, if increasing tartrate concentration favors forming chromium-tartrate complexes, this will decrease the amount of the double complex and free some rare earth again for more rapid extrac- tion. TABLE 2. EFECT OF TEMPERATURE ON EUROPIUM EXTRACTION RATE Organic phase:. 0.2M D2EHPA-0.1M NaD2EHPA.15M TBP in Amsco 125-82 Aqueous phase: adjusted simulated Purex IWW solution (atia lysis in Fig. 1). Phase ratio: Temperature Contact. Time (min) Fe in Organic Phase (8/1) Europium Distribution Coefficient . 25 8.8 0.57 1.1 1.6 2.1 3.6 . y o ő is w ni oo uwa 45 . . 1:3 2.3 2.8 . 4.0 REFERENCES 1. Wischow, R. P. and Horner, D. E., U. S. Atomic Energy Commission Report, ORNL-3204 (1962). 2. Horner, D. E., Crouse, D. J., Brown, K. B., and Weaver, B., Nucl. Sci. Eng., 11, 234 (1963). Personal Communication with G. L. . Richardson of Hanford Atomic Products Operation (1963). 4. W. W. Schulz, U. S. Atomic Energy Commission Report, HW-79762, Part I (1964). 5. Văn Tuy1, H. H., U. S. Atomic Energy Commission Report, HW-58970 (1959). 6. Peppard, D. F., Mason, G. W., Maier, J. L., and Driscoll, W. J., J. Inorg. Nucl. Chem., 4, 334 (1957). 7. Burns, R. E., Schulz, W. W., and Bray, L. A., Nucl. Sci. Eng. 17, 566 (1963). ** Si * w V W ** • . - T ... . llllllllllllllllllllIIIIIIIIIM UHURUUMUHIMMllllllllllllllllll Inne WINNIWINUlllllllll TAHRAMMIMOHINInom TITUUNNITTEISINI SUINNIWITIIVIUNIT MIINI DIRI •"' . _THUlllllll --.... ITUUT WIN IIIllll MUNDIMIS U nulllll W l Nllllll will IIIIIIIIIIIIIIIIIIIIIIII llllllllll llllllIUM lllllIHIND I OPINITIILIT 1.|||||IIIITT llll .......---- * .. ..''. . . IUNITI MUN ULUI FRII 17 III.1 IllIIT DINTE All ----- voti e ........... ..... 0.17M Fe, 0.2M DZEHPA-1.1M NaD2EHP- 1/1. Extraction of Rare Earths from Tartrate-Complexed Simulated IWW Solution at pH 5. Aqueous phase composition: 0.03M A137, 0.003M Cr3+, 0.003M Ni2+, 0:003M ERE, 2.7M Na, 1.5M NO3, 0.33M 1042, and 0.33M tartrate; adjusted feed aged 1 h prior to extraction. Organic phase: 0.15M TBP in Amsco 125-82. 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Procedure: phases con- tacted for 1 min at a phase ratio of 1/1 and separated (05.7% .7% of the europium was extracted); aqueous phase from this contact a ged for 0.03 to 6 hr before. contacting with fresh solvent for 1 min ac a phase ratio of 1/1. 14 WOLLIDR un ! TII 部 ​S www OUTADIINIDUMIT Dit nii INIIIIIIIIIIIIIIIIIIIII T ingnnmillUUUUUUUIIIIIIIIIII Biwi RM llllllllllUIIUL su Vin DUQIllllIINILI IMNIH OllllllllllIIIIIIIIIIIII i DUIIllIIlIIIIIII OTT: N D UMIINIUINUIUIII Notitilo DININIUMDITULIINIHINIWII 400 ml UMIINIUUUMMUMTUMITI LHDidim luluillAllNmlllIIIIIII JUDINTITULIIlllllIlITITUTI familTION MULTI UUUUUUITTITT in RE ! !! MINIMO M IINUTI LLAAN LI NIIIIINNNNNlllllIlIIT ETA NE INTRdiNJIMUI) LAND VO DO DOMU U tin mutants QUIHUDUMU ON MO DI MAMMINII dinne . ull VILI. IIIIII II LXGA LA MO DE UM umu!!! Jilli 1/1. Effect of Tartrate Concentration on Europium Extraction. Aqueous phase: tartrate-complexed simulated Purex IWW solution (analysis as shown in Fig. 1 but with tartrate concentration varied in the range of 0.27 to 0.5M). Organic phase: 0.2M D2EHPA-0.1M NAD2EHP- Phase ratio: 0.15M TBP. in Amsco 125-82. WUUUUU lllllllllllllllll . UNUIT UlllllIUT HULDU ILUMINA Will W ill VITINIMUI UMIINI! DH! llllllllllllllllll IIIIIII W IDA UQ JUMTIMUNITE! WWWUWWTIMIT Juan MIININIUMINIUI TolllilllUIIIIMITI MUNTIIIIIIIIIIIII LIT DUVAA:1:1:6 Illil! 14:10 !! JHO! .. WIE NI IIIIIII JANTIDIU TIN minium MllllllIIIIMIIIIIII IIIIIIIIIIIIIIIIIIIIII ILL . . UL! UlurumlllUIII AAH!!!!!! TINNIIIIIIIIIIIIIII NullIIIIIIIIIIIIII JUNTA DLANI. Mllll||IIIIIIIIIII MilliNIIIITTI til Low TNTJUT 1.000 410 ! IMIMIIIMIIIMI Innill IIIIIIIIII illiti INITTIIIIII AUWO lillllllIlIlITITITITIT BUDILI MUTITITIU 0. JININMITILI UNIUNIITTITUTI 11.00 HUU! MINUUTISMUL TR ADAnililih unul 01. 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