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Research Sponsored by the U.S. Atomic Energy Commission Under Contract with the Union Carbide Corporation, Oak Ridge, Tennessee 37830

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Research Sponsored by the U.S. Atomic Energy Commission Under Contract with the Union Carbide Corporation, Oak Ridge, Tennessee 37830 159 PREPARATION OF ISOTOP1 CAI.LY F.NRJCtiLD SAMPLES OF IRID1UM, OSMIUM, PALLADIUM, AND 1'LATINUM FOR RESEARCH USE K. W. McDaniel, L. 0. Love, V. !'. Prater, R. L. Bailey Oak Ridge National Laboratory Oak Ridge, Tennessee 37330 Abst me i The .'\ ;:;'.' i fluorination technique, which is currently be ins; employed at Oak Piiire National Laboratory for enriching the stable isotopes of iridium, osmium, palla- dium, and platinum in electromagnetic isotope separators, is de-scribed. Ion-source modifications and safe-handl i .nj.; procedures for usinj; chlorine trifluor- iue (the fluorinating agent), both necessary for successful separation, are given in some detail. It is suggested that the internal fluorination method might be used in smaller lab- oratory separators for target making by depositional methods. Simple chemical recovery and purification schemes are i'.iven for each of the four elements, along wi'\ some of the current uses of the nuclides in research and me d i c i n e . -A Research sponsored by the U.S. Atomic Energy Commission under contract with the Union Carbide Corporation, Oak Ridge, Tennessee 37830. 100 !'Ki-.!'ARAno.\ OF 1 HIM <)VICAi.i.Y I.'-Kl''.'. ••'. !' :.A!'.:'i.!..; OF I "., i'.T.'-'.I 1,'M , i'Ai.i.Ai)! L'M, ,Vsi) i'i.ATlNCy. i '•; Ki:Si.Aj<:Gi i:Si. i\a' :.:i: •.' ' ..si's Liu ft1 has r>;isU:J a need I'M' separated .iscti 'pc.-^ o'. the p S it L; ,ui" ;. - s-._ > i i •. i ••! , indents, e,pedal ly I'or tiie study o! v.ii:ii-i;: inrit.ij- ;r porties. L'J.LIJ <a.:ite iv: int I y , p r"i-i ;:. i n;-. el' Mro.se eli-iieiils in e 1 L--. i r< : ;.i/.:ie i j c .-;•_• j"-.i r..jL' r:s '.-.as d';'iciiil .m J ti.:.t- i •..'•.iSiiii'i n;' due to Liu- tact tiiaL the lack of a suitably stable an.i volaij le char.c <:. »r j|! ^;i a l LI no- ••.-;:; i t at e d hi ;-u-t el'pe ral UIC i n:! st.crccs . apanie o: v.i; •.; i i ;• i ;:.: the nie! alii' I >• rr.i "I i he e I ei:-en I. Th is i • i.n i •.;(».•, ' ..';u,:.; si/i i:ia.s:'ii i i: :•;. l.ii ni ii>; ;-n.l •!]>; ( a 1 ! y •. iiriciicd iwciii.u- • s "I iridi".:;., ;•., i ; aa i ;:;.,, ..r.ii p ! ,n : nu;:. (ii^::i- i.::. •.!.!.-. !;:••;!. ,c ;ia r a! a ii 11 •. i i.. •, I '• 11 • 1.1 r.:>:i i!c) , ri~ii;:!n. u ::•:'! •, i;aa ; i I i t-s. "I m.ii.. •- lia] '.•.•:!;: i I-^L1 r-t aaii-av.'rave- i :.DL"; . i a purities. ;...•.-.' ti ;a:iicjuv du vv i u[)i.' J !"!.-'< t'I;/. !y a; i •]•:'.';., pat t''i':;i ..i a] L .. r tia. \'.\.-: -:. i .ia a ua'1 .^! i--11-:..<.•]; J a r .' i iLiorJiiL'" and iJiv.i.'.i i::-.'-- ij: v.Li ., ut i 1 i /..v; f. i i" . (..! i\ icl witii a;:d uraa^pi ia piatinui;; and p lal i luini-^r^ap niclais d i iv t 1', iat- tau i on i zaL Loii rL-'i'Mi •.'1 tin.- i .-.! lit. ri);: i uii suurcc. iaiD:parud Lu tin- •.- U c 1 ron-a<:%harU:-,ia: t ':; ,;a -Cfi:.peraL i:rc :::''liiod a 1 :u.'parat iai'.- p laL i nai;!-;!!*.1 La Is i L-L-L i>p<> , i.i-- -:-u r'tv-n t L--. '•; i: \/.] uu has r.. v j ] u- I i oiii Zi.'ci i.lu- saparat. i ens oi Liu- p 1 ;;t i i'.uir.-i'.v i. i! is.-Lipas (u:;pi.'c !.••'! Lv i r i d i una in ; • I'I • ail !ia t aad i s ; t • > p i c put: i Ly . (Ire a L ca" o '• • a'- : : ; 11!:> •-1 : r i a i nr , isri ur:, j\:: ; a a i m~., .•HI'.; p!ati;:nni .na- ,-•: i-r-.1 »t ly fcr SDI.II iili ;U') a.-.: i ! .I'.I I ^ it IIIV/HT ist't.pi.' parity ! :i-.iu L ia'ii^a t ! ^a.M ;: ]L i 'a.1-, i a ,i;:.;ri [ i ;:;L- ,I^;I> . ia1 ; I i;a if L nat i ;a; :\L- t. aad in :a • i ii;' aSL- d in p raaiK L i L;II- t. vp./ s^: p ;rat > a ^. ; jr t iir rurov- ci'v i I /. r.in ipian t i 1-ias ui must, DI' Lin.- :su'i'[v-i; ;n)Wc\-L-;', ti'^iv appears [.;"•• bu no r ^ •.!,-•• = 3; '.vir: : iu- t t.'i:i; ni-qut' C.MJJ(] not i-u- a.-.t-d , ri :a:^a 1 1 S'.-pjr.itt.'rs v.:a.-r^ L-::;piia.sis is p:a....<j uii dir..'cL Larcrt prudni'L ion. in this vu i n, v.v v.ajvild like t. di-scribu tlie jiiiy:-. i ail i-uadit.ions i'i l';\v .•n'paratiiin in suna- d. • t a i 1 !!"i^u]'!.- 1 is .; Hciiumalie dia- ;-j"ar. i'i Lin l ln..'r i P..IL ion syst'.T 'ur a ralaLrai ion .,ourci-.i . The graphite ion 'ia;ri:c (':-;ii LypvJ v/as mudi.l"ied i ii tin- )'. • i ] uw 1 ny t'ayr.: Lai- .••.t.iinU'Ss steo] timing V a-.t..'d !i'i tiu' ' raiisiii 1 .ss i on J t CC 1;, Lu L i: L c:iar;j.c iujLtiL' -.•.'.'is Vvp I aci-d v/iLh a nickel ! : in lur !iii-: L ranmia s>; i i n at" |_. I 1-', I're:. ,• cvlindar niuuntvd nn the ii i aa-vo] tage tcr- iiiia.ii bo:-: aiia.TLly inLo Liu- '.>.ii-k ui tin.- ar/ ciuiir.iio r wiiii-ii aoiiiaineJ the eJcncnt ( is iiiflal) ;.)i.-in>: p rinL'Ssod; iiccaasi.- <;l IIK1 1~COC L i on be LWI-IMI grap'nite ar.d Clr-j and p. ss i i.. 1<- n-ai.-t i oiis but'.-.'ei.-r. p 1 at i nun-aela J c .or:,;:aa:nds and j-,rapl> i 1 e , a. nirkel liner •-.I.-; i aii i" i ratt-d to cover tiie inside surfaces of the :n"t. chaniber; the nickel linei' •...is ]!i-r! iiiati:i! vitii l/3_!-in. iioJes every i/'-i-in. to providi- a more unilrrn f 1 ..-,<- ii[ ill. tiV'-r Liie netaJ.j tile oven heater was eiini naL.d; ti;ub the i on Lzat ion arc and i.u- < ititrorj drain supply 1 roiu tue sourco were couiitea CMI to- pro\-i(:e sufficient a---.il lor LIIL- iau-r.iicai reaction lietwcL-n tile kll-". .aid meL-.tl . ALuj\e tile vaporization Leiiiperal ure .1 tile metallic fluoride, tile rate of ia.ac.tioii vas , i.;i (. roJ 1 ed largely i.y tile : !. iv rate o! (.IF; which •.-.-, is regulated by a n.eterinj; vaivi outside the ion Al l;:.m,;:i C i F . is toy.ii: and ii az ardous , as a resnl! ef til-.- adu-p t i i in ui a very ri^ : set oi n.uidii n;.', procedu rus , no inei dents have been experienced in tile use of tilis ^ja.s . Figure .1 siiows Liie precautions t aive n durini; rvir. tern: nat i ons , lilese pro- cedures were instituted durin;.!, sliort du ve lopr.ent runs with tiie advice and approval • a tiie i'lant Industrial Hygieni (Iroup. As a further protective me ch,m is:?i as we]] a.-, .u; aid to reducing tank pressures, caiciun; metal was vaporized at tiie rate oi 1-3 :' Ca/br. into l.iie lar^e '.'acaiun sys tei;: vnie.n i'l}\ was beim; used. \ . V . liueiin, !i . V.. C.avr i I ov , ai\d V. :> . Zojotarev, :•'. i •. •': i roaiu^nc t i c Separation of tiie isotopes •:•;.' tiie !' 1 at j nun-!'.!! J adi ur.i Croup, 1 soti.penpra>: i « 7(b): 23d-5 (19 71); i ii loass i ;ii:. 161 HIGH-VOLTAGE TV TERMINAL PI METAL AND/OR SPONGE ION CHAMBER Fig. 1. Fluorination System for Calutron Ion Source. Fig. 2. Precautions Taken During Run Terminations. 162 Table 1 COMPARISON OF ASSAYS USING FJJ:CTRO.\' UUMHARDMJiNT SOURCE AND FLUORINATION WITH GIF, NA "Bombardm ent" "GIF/1 U) (%) C.) :•)• Pt 0.0127 0.76 4 .2 1 !; i't 0.78 n.s 57.3 •'•"•l-t. 32.90 65 .0 93 .9-97.4 i ."Tt 33.80 60.1 9 7.3 : !•• 1>t 2 5 . 30 65.9 9 7.5 - l:i\'t 7.21 60.9 95 .8 XUN DATA: Time 4,769 lir 4,400 hr Recovered 64.9 a 176 .3 !•, ::.!,,. 37.3 9 4.66 9 7.1-9 8.2 i ) .'. | r (.2.7 9 8.7 96.9-99 .4 IUN DATA: Time ..,471 h r 2,600 hr Recovered 2.7 g 151 .0 g i.cule 1 is .i Lable comparing the outputs and purities of the GIF-j system with the electron hiiir.bardment method. Chemical Recovery and Refinement of Enriched Platinum-Metal Isotopes Iridiuni, osmium, palladium, and platinum isotopes are all collected on fabricated, ii iyn-p-.iri Ly graphite receiver pockets (receiver is shown in Figures 3 and 4). The cnriihcd material is recovered in each case by the simple expedient of burning i mlj i' idu.'jl graphite pockets, in oxygen, after removal of any neutral or adjacent- iHoLupe material from the outer surfaces of the pockets.
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