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AR 226 = 0875 ACUTE TOXICITY TO FISH (FATHEAD MINNOW) JTESTSU~ B~ S~ TANC 000E Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-7808B. (1- Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was 2. The test sample is FC7808, identified by the laboratory as "3M Sample 1-3". Current information indicates it is a mixtureof 0.58% PFOS, 14% diethylene glycol monobutyl ether, 76.7% water, 5.5% urea, 1.17% Hydroxy foamer, 1.15% sodium octyl sulfate, 0.8% polyoxyethylene monooctylphenyl ether, 0.05% sodium lauryl sulfate, and 0.05% benzotriazole. The following summary applies to a mixture with incompletely characterized concentrationsof impurities. Data may not accurately reflect toxicityofthe fluorochemical component of the test sample. METHOD: Method: Methods for Acute Toxicity Tests with Fish, Macroinvertebrates and Amphibians, EPA-660/3-75-009, 1975. Type: Acute flow-through GLP: No Year completed: 1980 Species: Pimephales promelas Supplier: Fattig Fish Hatchery, Brady, NE. Analytical monitoring: Dissolved oxygen, pH, ammonia, and temperature. Exposure period: 96-hours Statistical methods: LCs values and 95% confidence intervals calculated using a computer program by Stephan, et al. 1978. Test fish age: Juveniles Length and weight: Average length = 27 mm Average weight = 0.34 g (wet) - Loading: Not given. Pretreatment: None. Test conditions: Dilution water: Filtered well water Dilution water chemistry: Hardness: 255 mg/L as CaCO; Alkalinity: 368 mg/L as CaCOs --- PH: 78 Conductivity: 50 pmhos/cm Lighting: A daily photoperiod of 16 hours light and 8 hours darkwas maintained throughout the testing period. 002569 Stock and test deionized water solution preparation: The on a volume/volume basis. stock solution was prepared in F2l4ohwo-utrhs.rough rate: Approximately seven volume exchanges of water every Stability of the test chemical solutions: Not noted ENxpousurmoefvrbeespslee ilcsa:tresG:las1 s aquaria containing 30 L of test solution. Numberoffish per replicate: 20 WNautmebrecrhoefmicsotnrcyendturraitnigontsh:e sfitvuedypl:us a blank control pH range (0-96 hours): 7.98.2 (control exposure) 8.08.1 (1500 mg/L exposure) Temperature range (0-96 hours): 21-22 C (control exposure) 21-22 C (1500 mg/L exposure) Dissolved oxygen range (0-96 hours): 7.99.1 mgiL (control exposure) 7.986 mg/L (1500 mg/L exposure) R0 Esw0 ts00000000000 Nominal concentrations: Blank control, 90, 200, 380, 770, and 1500 mg/L. Element values: 96-hour LCso = >1500 mg/L 96-hour NOEC = 380 mg/L. Element values based on nominal concentrations SRuebmsatraknsc:e TReesmtianrgkwsafsielcdo. nTduhcetevadlounestrheepmoirxtteudraepapslydteosctrhiabtemdixitnutrhee aTnedstnot the fluorochemical proportion alone. conclusions 000000000 The test sample 96-hour LCso for fathead minnow was determined to be >381050m0glmLg./L. The 96-hour No Observed Effect Concentration (NOEC) was `The 1500 mg/L concentration resulted in a 15% mortality. Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. _ Paul, Minnesota, 55133 pataQuAalTY Reliability: Kiimisch ranking = 2. The study meets the criteria for quality testing. However, the sample purity was not properly characterized and the 002570 study lacks analytical confirmation of the amount of fluorochemical proportion in the solution. R0 EFE0 RENC0 ES 0000000000 `This study was conducted by Analytical BioChemistry Laboratories, Inc., Columbia, MO at the request of the 3M Company, St. Paul, MN, 1980. oTWeR Last changed: 6/28/00 O00 002571 AP.NOA.LYBToIxCA1L097BIO CCoHluEmMbIiaS,TRMYO L6A5B2O0R5AT=OR(I31E4S),47I4N.G8570 SM) Dynanic Acut12e62B0i1oassay Report Subitted To: 3AttnC:onpHarn.y Moe Elnsbaravy E93n5viBruosnhmen-taBlldgL.ab2-3 - St. Paul, Minnesota 55144 "gol we to FaDthyenaadmiHcionf9a6o-3wHHsouSra(aPApiclmueetpeh1a-l3Teosxipcriotvyelas) Septeaber 29, 1980 002572 BEST copy AVAILABLE Subaitted By: A77n2-a00l0.ytEiaBcsoatxlA1B0BC8i7oCLahneeaistry Laboratories, Tac. . CGortuiabieai, -Msisssouri 65205 Prepared By: C Matio c STuopseb rsvisorleoo . ot = Aopvaaiti,c )fBloorltoFsgiostk BFoiPuollooBgnoiutsdtreRnosndranns fez a(B2pit0e/p80 2 YoSeotfeso IT3atoef0 Aoproved By: QuphiPtylanteAagueance Officer LiiibooratorSyotaHasneangel slDatse _ -Ba3t0e -8 002573 TAOFBCOL NTEE NTS Page Yo. LIST OF TABLES. .....euueeereerrnereeeinaeneeeneaaeseeeeeeeeenseenodd INTRODUCTION. +s eee ee eeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeannaaeens2 To TeSt FAshueerrruunniieaaiaiiiisesiaiieeenieeieeansaeaeeaaeaeenese2 II. TestSYStem........iseiiiieiiiiiiiiiiiiimeeiieie eee? III.Test COMPOUDd.+rvvvvvvnnssssssnsssssssensenissnnessensanaaanaannsd IV. Test Procedure-Biological......e.trrrirerrrrrrrrerrrrerereenisssssd V. TestProcedanudPhrysie cal.-...C ....h...e ..ccmeeei ieec eeeeaennl nnd LITERATURE CITED......ssunnsnesessssesesssseeeseeasaneeeneessnenesesensd QUALITYASSURANCE STATEMENT..........errrreressssrssssssssrsnsssnsnnessd APPENDIIX RAWDATA 002574 LIST OF TABLES Table Page He No. 1 Tfhoer tehsetim9a6t-ehdourLCgfoathveaalduemsinwniotwh tthoexiircit9y5%stcuodnyfiodfenc3e Slaimnpiltes 2 CcThnoeel.moigcya(LlAaLLbcohraanaratalocyrtsyeersoifcpsAenroaffloyrtmwieecdlalblywBaAitBoeCCrhLeamatibsatt)hre.y-AL.qa.ub.ao.triractroorTriosexrsi,-erers.5 . 3 Wsattuedry qofual3iMtySammepalseure1m-e3nttso dfuartihnegsdthmeiam9o6v-shou(rPinteopxhiaclietsy PT TO RRS Sn soveserere NUIT 4 cPeenrtcreanttiomnortoaflit3yM oSfamfpaltehea1d-3midmuuroiwnsg e8xpo9s6e-dhotuor ftiovexicciont-y 5 002575 SupaRY acuteA tdoyxniacmiitcy 96o-fhou3r toSxaimcpiltey s1t-3udytowasfactohnedaudctemdinntoowsdet(ePrimnienpehaltehse pMreotmheoldass)f.or TThoeximceitthyodsTeesmtpslowyietdhveArqeuattihcoseOroguatnliisnmesd (b2y).theVaCtoemritqtueaeliotny puraerdamettherrosughoofuttetmhpeertaetsutrea,nddivsesroelvweidthioxnygaecnc,eptpaHblsendliammimtosn.ia were meas constAantflotwe-stthrcooungchenptrroaptoirotniso.nalNodmiilnuatlerexspyosstuerme wcaosncuesnetdrattioonmsaiwnetraei:n 90, 200, 380, 770 and 1,500 mg/1. referAesncea cqoumiploiutnyd, chAenctki,myctihne Af.atheTahde moibnsneorwvsedwe9r6e-BcohuarllLeCnsgoed anwdith95a% confidence limits (C.1.) were within the 95% confidence limits reported io the literature (5), indicating that the fish were in good condition. matedThLe0sqobvsaelruveesd. mortality data for the study gave the following esti- TABLE 1: TLhienitesstfiomrattehde L9i6g-ohovuarlufeasthweiatdhmtinhneoiwr t9o5x%icciotnyfidsetnucdey of 3M Sample 1-3. Hours of Exposure "2 on 96 3 Semple 915-3% C(oangf/1i)dence Ls Linits >>11550000 e--n-- >1500 ---- 21500 ----- 96-houIra, andodiotbisoenrvetdo etfhfeect`abcoovneceLaCtgroativoanluoefs,380thmeg/lr.esults indicated a - 002576 INTRODUCTION BioCh3e1miCsotmrpyanLyabcoornattroarciteesd, thIenc.A,quattoiccoTnodxuicctoloagyfiDviev-icsoinocnenotfraAtniaolnytipclauls Scaomnptlroel,1-396t-ohofura,thefaldowm-itohnroowusgh(PBiimoeapshsaalyestoprodmeetlearsm)i.ne Tthhee ptroixmiacriytyoobfjec3dteitveernoifnitohge tshteudmyedwiaasn tloetdheaflinceontcheentarcauttieonstox(iLcCistey's)ofdu3rinSgamptlhee c1-o3urbsey Coofmpathney, teisat.a prTohteocosltuddyatevdasSeaputtehmobreirze1d5, by198M0r. (AHpopeendEilxnaIb)araawnyd, va3sH conducted fron September 25 to September 29, 1980. SampleThe1-t3ercmauLsCignog a5s0%usemdortianlitthyis afrteeprorta isspetchiaftiecdonceexnptorsautrieonperoifo3d. Ttheicshnirceaplortappprreosaecnhtsusetdhetoremseuelttsthoef ptrhoejetcoxticoibtjyectsitvuedsy. and describes the METHODS AND MATERIALS test Tahree bbiaosliocgailclayl thmoestehoddsescursiebdedfoirn tShtean9d6a-rhdouHrethfloodws-tfhorroutghhe Etxoaxmiicniat-y wtiitohn oFifshW,atHearcraonidaWvaesrtteewbartaeters a(n1d) AandnMp etho(h d2s).oi f ATchbuetesitTouxdiys citvyan s Tecs sotns ducted pendix If)o.llowing the procedures outlined in ABC Protocol No. 8007 (Ap- I. Test Fish Fish THhaetcfhaetrhyeadinmiBnrnaodwys, usNeedbrianskat.he teTshte wfeirseh obwtearieneiddefnrtoimfiFeadttitgo sfpieschievseruesihnegldthien tcauxlotnuormeictaknekyss odnevael1o6p-ehdoubry dEadydlyig(h3t).phoAtLoLpertieosdt atnedchnoibqsueersvewderfeorbaasticlaelalsytth1o4sedadyesscprriiboerd tboy tBersatuinng.et.Fials.h c(4u)l.turAe wdiatihly prreocpohrydlacotficfisahndobtsheerrvaapteiuotnisc dduirsienagsethterehaotlmdeinntgs,perisiodi,ncsliuodnegd sintanAdpapredndcioxmmIe.rciaDlurfiinsgh tfhoeod h(oRladnignegn'sp8e)riodda,ilythien afnisahmoruencteievqeudivaafeldentdurtoing3 tpheercaecnctliomfattihoeniranbdodtyeswteipgehrti.odsT.he Ttheestfaftihsehadwemriennomwost ~ ussteadndafrodr ltehaigstheoxfpe2r7immen.t hWaedighat maenadn lweeniggthhtmeofasu0r.e3mengtsanwderae mmeaaden oinncltuhdeedcoinntrAoplpegnrdoiuxp I.of fAissha aqtuatleirtmyincahteicokn, otfhethfeattheesatd amnidnnoawrse wseerrevedch9a6llehonugred 1Cwgiothanad r9e5f%erceonncfeidceonmcpeoulnidm,itsAntwiemryeciwnitAh.in Tthhee 9o5b~% cthoenfifdiesnhceverleimiintsgoroedpocrotnedditiionn.theRelsiutletrsatoufreth(i5s),teisntdiacraetiinngclutdheadt_ in Appendix I. I. Test systea (6), AwitphrotphoertmioodniaflicdaitliuotnesrofsyMsctAelmlidsetsecrriebte.d alb.y (H7o)u,ntvaasndusBerdunfgosr 2 002577 tihneto itnhteermtiestttenatquairnitar.oduAcetriaotnedofwe3ll wSaatmeprle(T1a-b3lean2d) dwialsuednetliwvaerteedr wthoicthhewagslasssufafqiucaireiaat atto areprlaatceeofthe15030all/imtienruttee/satquvaorliuumse,aatnleaamsotunt7 tciimrecsulaitninag 2w6atehrourbaptehrihoedl.d Tahte 2t2esCt (a1qui)riabywesruebmeirmgmeedrsehdeaitninga elements. III. Test Compound in goTohde c3ondSiatmipolne. 1-T3hestsaanmdpalred wuapsonrerceecieviepdt ownasSeopbtseemrbveerd 1t0o, b1e980a,n asmobleurtiloinquviads apnrdepvaarsedstionreddeaitonirzoeodm tweamtpeerraotnurae v(o2l2uCe)/.volTuhee bsatsoicsk aSntdandcaorrdrecwteeidghftosr asnpdecdiifliuctigornavviotlyumteosacwaenigbhet/fvooulnudmeinbasAipspen(dnigx/1)I.. IV. Test Procedure-Biological sigumTehnet otfes2t0 vfaastheianditmiiantaeodwsontoSceapcthemboefrth2e5,3019l8i0t,erbytersatndaoqmuaraisahaofutresr. teTsthe sfoilsuhtiownesre heaxdpobseeedn tfolotwhiengfotlhlroowuignhg ntohmeinaaqluacroinacefnotrra-8 t1i,o5n0s0 omfg/l3. SaTmhpelefi1s-h3:vere90ombgs/elr,ved200fomrg/mlo,rta3l8i0tymg/aln,d 7a7b0normmga/ll aben-d phearviioodr. iniDteiaadlliyndainvdiduoanlcse weevreery re2m4ovehdourast feoarchthoebse9r6v-ahtoiuorn.tesAt ctoompcuatlecruilzaetdeLCtshe prLoCggroamvadleuveeslopaendd bythSetierph9a5n%etc.onafli.de(n8c)e walsimiutsse.d V. Test Procedure-Chemical and Physical and aWmamtoenriaquawleirtey pmaeraasmuerteedrsthorfoutgehmopuetratthuere,tedsitssaonldvedveorxeygewni,thpiin acceptable limits (Table 3). measuTrhiengnopmriendaeltecromnicneendtrdaitliuotnisonosf 3 of Sample 1-3 vere determined a stock Rhodamine B dye. by A bsatnacnedar(dCoclaemlainbraStpieocntrocpuhrvoetomweatsercoMnosdterluc5t5e)d otfo mkenaoswunredilthuetiosnbssoro-f ~ tphreopodryteiontahlatdilburtaecrk.eteTdhethdeiluatbisoonrbfaanccteorvvaalsuedeotbetramiinneedd bfyroimntetrh-e p1o-3latcioonncefnrtormattihoen stdainvdiadredd cbuyrveth(eApdpielnudtiixonI).facTthoer sdteotcekrm3ineSdamptlhee hciaglhceusltatendombiynamlulctoinpcleynitnrgatitohne. higThheestrecmoanicneinntgractoinocnenbtyratthieonpservceernet edxialmuptlei:on (% difference) obtained from the calibration curve. F--or- 631.5G2g1/1 ((dsitlouctkioncofnaccetnotrr)ation) y 4 : , [% daiqluuatriioan#4for] 0 8 [emaiqulareiae#4 etn] 3 002578 mThaennenromvienrael: co9n0c,en2t0r0a,ti3o8n0s, o7f70 3aHndSa1m,p5l0e0 m1g-/3l.calTchuelamtaexdimiunm ttheisst cspoonncseonrt.ration was set at 1,500 mg/l, as requested by the study RESULTS intervTaalbsle fo1r 3p4resSeanmtpsle t1h-e3. preTdhiescetevdalLuCesso wevraeluoebstaainnded 9b5y% emcpolnofyiidnegncea computerized LCso program developed by Stephan et. al. (8). TABLE 1: TLhienitesstfiomrattehde L9C6g-ohovuarlufeasthweiatdhmitnhneoiwr 9to5x%icciotnyfisdetnucdey of 3 Sample 1-3. Hours of Exposure 28 97%2 3 Samlplee 1-2 e (ag/Le eso Limits >>11550000 e--n- >>11550000 ----- 96-houIrn, andoditoibosnervteod etfhefecatbocvoencLeCnstoratviaolnueosf, 3t8h0e mgr/els.ultsMoritnadliictayteddataa is prescated in Table 4. ammonWiaatewrerequmaelaistuyrepdarianmettheersconotfrotle,mpleorwatucroen,cendtirsastoilovnedanodxyhgiegnh, cpoHnceann-d ttiroantsionwhitchhrosutgahyoeudt btehteweteenst85(Taanbdle1030).perTcheentdissastoulrvaetdioonxywegreen ccoonncseindterrae-d aledveeqluat(e9)f.or TtheestipnHg v(a2l)ueasndwearmemoncioansciosntceeanttrwaittihontshewercoentbreollowtthhreoutgohxoiuct the study. PractiTchee stRuedgyulwaatsiocnosndu(c1t0e)d faonldlowtihneg thfeinailntenrtepoorftthweasGoodreLvaibeowreadtorbyy AonrailgyitniaclalrawBidoaCthaemiwsatsryproLveibdoerdattoorie3s4' ComQpuaanlyi,tywiAtshsuarscaocpey Urneitta.inedALaLt Analytical BioChemistry Laboratories. 4 002579 TABLE 2: Chemical characteristics of vell water at ABC's Aquatic Bioassay Laboratory. Parameter Dissolved Oxygen ot Hardness (CaCO3) Alkalinity (Cac0g) Conductivity Total Amonia (H;) Yog- Concentration 9.3 ppm 78 255 ppm 368 ppm 50 pmhos/cm <0.05 ppm 0.15 pra Ortho-Phosphate usin Arsenic Cadatum Chroniun Cobat Copper Iron Lead Mercury Nickel 2ne Mpeeasstuirceiddesorganophosphorus MpeesatsiucrieddesorpglaunsochBlCoBr'isne 0.10 ppm 0.01 ppm <0.001 ppm <0.001 ppm 0.001 ppm <0.001 pp <0.01 ppm 0.012 ppm 0.009 ppm <0.0001 ppm 0.0157 pom <0.01 ppm . . 25ee appendix for individual analyses. - - o 5 002580 THE 5: fWaattheeradqumailnintoywsmea(Fsiumreepmheanltess pdruocsieolsss)t.he 96-houe toxicity study of 3M Seeple 1-3 to HDomuroseoef T0p, 2 um wm nm sm D0c.on+trol Wd7 mA oS mh es 82 os sa sa 16 es 7s ose se e110 7s sa os Lov TeoCm.p. 0Co0nce+ntration mi pC WmGh3 High TeCmCp. mCDooinc+entrmatCion"mxha 2 85 80 10 2 84 80 14 om so 81 13 2 86 81 16 mo sa so oem 8s 80 0&8 om AS 61 os 2 83 80 086 om 77 so osm 19 80 060 "rhigoh ceoncentration vate quality vas detersiaed fa Tak 6 (1500 mg/L 3H Sample 1-3) theoughout Upiasolved oxygen concentrations - TSI Model 54 Dissclved Oeygen ter sad probe. Sp =pI Probe (CorningNadel 476022) usedwith aCorningNodel125 PH andaV meter. 1a0maonamieatecron.centrations - Ammonia Probe (Extech Hodel 8002-8) used viih a Coradag odel 125 pi <g8 a , &g . FIBVTIVAY AOD 1538 TABLE 4: Pfeirvecenctoncmeonrttraaltiitoynsofof f3athSeaamdplmein1n-o3wsduerxipnogsead 9t6o hour toxicity study. 3M NSoammipnlael1-3 co(nceegn/t1r)ation 7 Ho4u8rs of Expos7u2re % Control o o o 90 co 0 200 0 0 RALRi 380 o Th 70 10 10 10 10 1500 15 15 15 15 BEST COPY AVAILABLE Ca ~ 7 002582 LITERATURE CITED (1) AthmeeriEcxaanminPautbiloinc HoefalWtahteArssoacnidatWiaosnt.ewat1e9r7.5. Standard Methods for 14th ed. Washington, D.C. 1193 p. (2) C(Co.mmEi.tteSetepohnan,MeCthhaoidrsmanf)o.r T1o9x7i5c.ityMetTheosdtss fwoirthAcuAtqeuaTtoixciciOtrygaTneisstmss wtietchtioFnisAhg,eaMcayc,roEicaovleorgtiecbarlatReesseaarncdh ASmeprhiiebsiaEnPsA.-66E0n/v3i-r7o5n-m0e09n,talAprPirlo,1975. 61 p. (3) ECdodmyp,anyS,amDuuebl.uque1,96I9A.. T2h8e6 Fpr.eshwater Fishes. 2nd ed. W. C. Brow (4) oBfrauRhens,eaJr.chL.Fiasnhd: R.RaAi.nbSocwhoTertotugte,r.Fat1h9e7a5.d MiAncnqouviss,itCihoannnaenld CCualttfuirseh asnedarcBhluSeegriilelss.EPA-E6n6v0i/r3o-n7m5e-n0t1a1l, MParyo,te1c9t7i5o.n A4g5enpc.y, Ecological Re- (5) BSetrugdeire,s Bo.n AL.n,timRy.ciEn. ALeaasnona FainsdhJ.ToxWi.canHto.gan.U. 1S9.69.DpeaLratbmoernattoorfy Interior, Investigations in Fish Control No. 26. 21 p. (6) Mtouusatf,orDF.isIh. TaonxdicVoW.logA.icaBrlunSgtsu.dies1.967.WatAerSRiemsp.lifi1e:2d1-D2o9s.ing Appara- (7) SMciAmlplliisftieerd, DeW.vicAe.,foJrr.,MetVWe.riLn.gMCahuecmkicaanldsF.inL.InMtaeyremri,ttJern.t-Fl1o9w72.Bio-A assays. Trans. Amer. Fish. Soc. 101:555-557. (8) S1t9e78p.han,A Cc.omEp.u,terK.prAo.grBaumscfho,r R.calScmuiltaht,inJg. aBmurLkCes.andU.R.S.W.EAnnvdirreown.msecnritpatl, PAruogtuesctt,io1n97A8g.ency, Duluth, Minnesota, pre-publication manu- (9) National 1972. U. SA.caDdeepmayrtmoefntScoifenCcoemsm.erce1,97P2B.-236Va1t9e9r. Q5u9a2lipt.y Criteria. (10) FPoroacdticaen.d D2r1ugCFRA,dmPianritst5r8a.tion. Regulations for Good Lsboratory - 8 002583 Q9u6a-lHiotuyr AAcsustueranTcoexicSittayteomfe3nt foSrampflienal1-3reptoortFat#h2e6a2d61Miennntoiwtsled(,Pi"mDeypnhaamliecs promelas)," for Mr. Hoe Elnsbarawy, SM Company, St. Paul, Minnesota. ductedInataccoourrdafnacceiliwtiitehs AaBrCe Ldaebsoirganteodriaensd ifnutnecnttiotnhaitn aclolnfosrtumdainecse cwoint-h 0la0bdoraltaobroyrasttourdyiepsr,acatniciensrpeegcutliaotnioonfs tahned fitnheal prreoptoorctolfsorfo3r iSanmdpilveidu1a-l3 wQuaasl_ictoynduAcstseudranacned fUonuintd. toAnbeinisnpeacntiaocnceopftatbhlee dfaoirlmy bmyoratamleimtbyerraotfeouorf wtehreeteisnt goorogdanhiesamslthprainodr sthooutlhde miontitbiiaatsiontheofobtsheervsetdudmyoritnadliictayteidnththeey s1t9u8d0.y. AAfniniaol-pirnosgpreecstsiosntuodfyalilnsdpaetcatiaonndwraescocrodnsduocnteSdepotnemSbeeprte2m9b,er198206,, ithnedicsattueddy atshaitt tvhaes rceopnodrutctseudbbmiyttAeBdC Ltaoboyroautoirsieasn.accurate reflection of in thSihsousltdatyeomuenthavoer atnhye qfuuenscttiioonns ofreoluartiQnugaltoitythAessiunrfaonrcmeatUinoint,propvliedaesde contact me at your convenience. fistAy.AsAsuulrtance Officer DaSt/e o 9 002584