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The Chemistry of Tributyl Phosphate at Elevated Fapact Temperatures in the Plutonium Finishing Plant Process Uc- Leve T S Q Vessels

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The Chemistry of Tributyl Phosphate at Elevated Fapact Temperatures in the Plutonium Finishing Plant Process Uc- Leve T S Q Vessels WHC-EP-0737 c The Chemistry of Tributyl I Phospha Approved for Public Release DISTRIBtmON OF THlS 00CUME:hn IS UNLIM[TED e LEGAL DISCLAIMER - This report has been reproduced Available in paper copy and micr P.O. Box 62 Oak Ridge, TN 37831 (615) 576-8401 Printed m *e United Wtes d Am I MSCUI-1.CHP (1.01) 1 . DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied. or assumes any legal liabiiity or rcspnsibility for the accuracy, completeness, or use- fulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any spe- cific commercial product, process, or service by trade name, trademark, manufac- tuum, or otherwise dots not necessarily constitute or imply its endorsement. ream- mendation. or favoring by the United State Government or any agency thereof. The views and opinions of authors exprrssed herein do not necessarily state or reflect thwe of the United States Government or any agency thereof. *- DISCLAIMER Portions- -__ of this document may be illegible in electronic image products. Images are produced from the best availabIe original document. fl Full Paper W TeduricalReport . U Manual t] Abstract a BmchunlFDer t] VtrwlAld fl Softwam/lJatabase Date Release Required fl SpeakenBuraau fl ContmlledDofumsnt [I Pocter&sslon fl Vldaotape a octwr March 11, 1994 Unclassified Category Title The Chemistry of Tributyl Phosphate at Elevated fapact Temperatures in the Plutonium Finishing Plant Process uc- Leve t S Q Vessels. lnformatlon received from others in aontidenw, wch as proprietary data, NOW or novel (patentable) wbjeot mattar? [XI NO [ ]YE8 If 'Yes'. ha8 diCdo8~r0been wbmitted bv WHC or other company? trade wcnt8, dlorinventions? [] No [] YE8 DlSdo8UM NO(.). [x] No []Yes IMemffy) Tndemarlrs? Copyrlghtc? [XI No [I Yes If 'Yes'. has written permission been granted? [XI No [I YeS(Id~nEifv1 [] No [I Yes(AttachPermis&n) I Date(s) of Conference or neeting I Wilpmwedhgebepublished? 51 Yes 51 NO I I Will materid be handed out? 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Sutter c Date Cancelled I Date Disapproved ED-7600-062 (08/91) LIEF074 ' Part 1 WHC-EP-0737 The Chemistry of Tributyl Phosphate at Elevated Temperatures in the Plutonium F nishing Plant Process Vessels. Prepared for the U.S. Department of Energy Off ice of Environmental Restoration and c Waste Management ,WC-EP-0737 * Document Title: The Chemistry Of Tributyl Phosphate At Elevated Temperatures InThe Plutonium Finishing Plant Process Vessels Prepared by : Date Fellow Scientist Reviewed by: Approved by : Approved by : Quali ty Assurance Engineer mc-EP-0737 THE CHEMISTRY OF TRIBUTYL PHOSPHATE AT ELEVATED TEMPERA'IlJRE INTHEpLuToMuMFI"INGPLANTPR0CESSvEssELs GoSo Barney ToDo Cooper ABSTRACT Potentia@ violent chemhl reactions ofthe tribwylp?wsphae solvent used by the Plutonium Finishing Phat the HimfZorrd Site were investigated. *re is a small probability that a signijicant Qumrtity of &is solvent cod be acci&nt&y trm$erred to heated process vesseli and react there with ninic crcid or plutonium nitrate also pment in the solvent tmmction process. 23re remlrs oflabotatory studies of the reactions show that exo~m*c oxi&ion of triburyl phosph by eizher nitric acid or actin& nitrates is slow at temperawes expected in the heated vessels. Less thun four percent of the tibutyl phospbe will be oxidized in these vented vessek at temperatures bewen 125 'C and 250 'C because the axidant will be lostjhrn the vessels by vaporitarion or decomposition before the tribwyl phosphate can be extensively midized. lk net amounts of heat generated by axidation with concentrated nirric acid and with thoriMI nitrate (a stand-in for plutonium nitrate) were detemined to be abow -150 and -220 joules per grmn of rn3uyl phosphate initially present, respectively. This is not enough heat to cause violent reactions in the vesseli. prt.olysis of the tributylphosphae occurred in these mirtures at temperatures of IIO'C to 270'C and produced mainly I-butene gas, water, andpyrophosphoric acid. Butene gas generation is slow at expectedpmess vessel temperatures, but the rate is fater at higher temperatures. iv WHC-mm7 At 252'C the rate @butene gas generated was 0.33 g butene/min/g of tributyl phosp?uue present. l%e metrnrred heat absorbed by the pyrolysis reaction was 228 J/g of tribuzyl phosphate lniriauy present (or 14.5 kcalhole of nibutyl phosphate). Release offrcmunablc butene gas into process areas where it wuU ignite appears to be the most seriotls s@eq coltsidetotin for ttre Plutonium Finishing Ph. This page intentionally left blank. vi WHC-EP-0737 TABLE OF CONTENTS 1;O INTRODUCI'ION ......................................... 1.1 2.0 PROCESSING ENTS INVOLVING HEATED TBP SOLVENTS ........2.1 '2.1 TNX EVAPORATORINCIDENT AT SAVANNAH RIVER PLANT .....2.1 2.2 TBE 1953 "FORD SlTE CONCENTRATOR INCIDENT ......... -2-1 2.3 THE 1975 SAVANNAH RIVER DENITRATOR INCIDENT ..........2.2 2.4 THERUSSIANTOMSKINCIDENT . i ....................... 2.3 3.0 CONDlTIONS Y REACTIONS INPROCESS VESSELS . 3.1 3.1 SEALED VERSUS VENTED SYSTEMS ...................... 3.1 3.2 HEATING AND COOLING RATES ...... ..................3.2 3.3 SPECIFICACCIDENTS~ARIOS ..... ..................3.2 4.0 EXPERIMENTAL .............. ..................e1 4.1 MATERIALS AND EQUXE'MENT ............................ 4.1 4.2 METHODS ................; ......................... 4-2 5.0 RESULTS AND DIS ..........................5. 1 5.1 TRIBU'I'YL PHOSPHATE'REACTIONS WITH NITRIC ACID .........5.1 5.2 TRIBUTYL PHOSPHATE REAWONS N" PLUTONIUM NITRATE . 5-15 5.3 THERMAL DECOMPOSITiON REACTIONS OF TBP ..............5-20 6.0 CONUUSIONS. ......................................... ~1 7.0 FUTUREWORK ......................................... 7.1 8.0 REFERENCES ............ .................... 8.1 . 1 .. .. LIST OF FTGURES Fv 5-1. TG (..) and DTA (J Curves far 231.7 mg of 20% TBP in Carbon Tetrachloride Saturated with Concentrated Nitric Acid (31.4 mg TBP, 191 mg CQ, and 9.3 mg ENO, + H20). Atmosphere = Argon, Flow Rate = 100 Cdmin, Heating ............ ..............5-2 . Figure 5-2. TG (..) and 138.0 mg of Mixture of TBP (Previously Saturated with Concentrated Nitric Acid) and Concentrated Nitric Acid (66.9 mg TBP, and 71.1 mg +GO). Atxnosphexe Rate = 100 cc/min, Heating 'C/miIi. ........ Figure 5-3. Mass Intensity Curves D&g Thermal Analysis of 138 mg of Mixture of TBP (Previously Saturated with Concentrated Nitric Acid) and Concenated Nitric Acid (66.9 mg TBP, and 71.1 mg HNQ + H20). Atmosphere = Argon, Flow Rate = 100 dmin, Heating Rate = 3.0 'C/plin. (A) Mass 12 (,* Mass 44 (..), and Mass 56 (-). (B) Mass 28 (J, Mass 30 (..), and Mass 46 (J ....5-5 Figure 5-4. Mass Intensity Curves During "hemal Analysis of 138 mg of Mixture of TBP (Previously Saturated with Concentrated Nitric Acid) and Concentrated Nitric Acid (66.9 mg TBP, and 71.1 mg HNO, + H20). Atmosphem = Argon, Flow Rate = 100 dmin, Heating Rate = 3.0 'C/min. Mass 18 (J, Mass 27 (..),and Mass 29 (0) ..................................... .5-6 Figure 5-5. Mass Spectra of Pure TBP Heated to 251'C (A) and Pure 1-Butene ReferenceGas(33). ....................................... 5-7 Figure 5-6. Mass Spectra of TBP Saturated with.Concentrated Nitric Acid EMto 144'C (A) and Pure Concentrated Nitric Acid Reference Liquid at 128'C (B). ...5-8 Figure 5-7. Comparison of DTA Curves for Mixtures Containing Different Ratios of TBPNitric Acid. (J 39.9 mg TBP + 14.8 mg HNO,, (..) 33.1 mg TBP + 104.9 mg HNO,, and (-) 29.9 mg TBP + 169.6 mg "0,. Atmosphere = Argon, Flow Rate = 100 dmin, Heating Rate = 3.0 'C/min. ............5-9 Figure 5-8. Comparison of TG Curves for TBP Equilibrated with Various Aqueous Concentrations of Nitric Acid. (J 15.7 M HNQ, (..) 12.0 HN03, (-) 8.0 MENa,aIId(..J3.OMENO3. ............................. -5-10 Figure 5-9. Effect of Air Atxnospheze on DTA (A) and TG (B) Curves for TBP Saturated with Concentrated Nitric Acid. (J 80.4 mg TBP + 29.7 mg HNQ in Argon and (..) 73.7 mg TBP + 38.0 mg HNO, in Air. ..............5-11 Figure 5-10. Effect of Heating Rate on DTA (A) and TG (B) Curves for TBP Saturated with Concentrated Nitric Acid. (J 37.6 mg TBP + 20.3 mg HNG, 5 'C/&, (..) 39.9 mg TBP + 14.8 mg HNG, 3 'amin; (-) 38.9 mg TBP + 21.9 mg ENG, 2 'Cl&, and.(-.) 37.6 mg TBP + 21.1 mg "Os, 1 'C/min. 5-13 Figure 5-11. TG (..) and DTA (-) Curves for TBP Saturated with Thorium Nitrate and Concentrated Nitric Acid (39.6 mg TBP, 41.8 mg ThO,, and 25.0 mg "0, + H20). Atmosphere = Argon, Flow Rate =-100 dmin, Heating Rate . =3.0*C/min. .. .......................... ......... .5-16 Figure 5-12. Mass Spectrum of TBP Satuated with Thorium Nitrate and Concentrated Nit& Acid Heat& toJ61'C (A) and 245'C (B). .................... 5-17 Figure 5-13. Mass Spectrum of TBP Saturated with Thorium Nitrate and Concentrated Nitric Acid Heated to 302'C.
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