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AR 286 -- 1274 DRAFT TELOMER RESEARCH PROGRAM LC/MS/MS Analysis of Articles and Products: Samples and Suggested Sampling Procedures Marilyn A. Stadalius, Ph.D. February 12,2003 I. Preliminary Study = Samples for Method Development and Extraction Efficiency eDfufriicniegntchyedcatoaurosne tohfrteheismaptrreilciemsin--arcayrsptetu,dyt,extthielecaonntdrapcatfpaecri--liatywtihlrleededivfefleorpenetxctornaccetnitornations: t1hpepcbo,nt1r0acptplbabanndee1d0s0ipndpibvifdouralarltyicplreespoanrleyd. coInntorrodlesrintotdheoftohlatlowwoirnkg,quwaentihtayv:e determined that Product Matrix Untreated Shaved Carpet [Nylon Untreated Textile [Pobvester Number | Approx. wiof Requested_| cach sample 15a" Tograms | 15a" Tograms | Total pieces: 162 #18ofeach of these 54 untreated samples are required/requested for method development. 11. Trea`tNeudmbaenrdofSUantmrpelaetsedRAerqtuiicrleeds for Analysis FOR CARPET RNeuqumebsetred Aepapcrhoxs.amwptleof Each Treated Shaved Carpet__ |" Each Untreated Shaved CarpetTM | 16 14 [Togams 10grams Used overly extraction cin 11 pyb. 10570 andT00 py. a wel 2sconor | | We plan on having three different carpet samples. g 52 5on3 2 35 > &% 58 5 Towed Samples [6 "Te -- (On1v8esaarmpeldeSsaamnpallyezsed[4 Ta 30 total treated and untreated articles T a FOR TEXTILES [ene [wen | Number | Approx. wi of Treated Textile |YT UUnsterdeatevdeTreyxetxivlaeci|on STACYa T1po4. 10 ps 7 100 7b.[2 grwealmls5 coma SLiCmAplSeMnSdASunggaestloedyfASsnamiipclesisngaPnrdoPcreodduurcets DRAFT FMaerbirluyanryA,12S.t20a0d3e, PD. We plan on having seven textile samples [Text Text [Textll[TexIV |TexV_[TexVi [Texvii| Treated fmoeee T[ FF F 7] 4Te2xtsialmeples analyzed 70 total treated and untreated articles [em[en |J,[my FOR PAPER Requested | each sample [TrestedPaper [1To6 gams | [UntCcreedattoevderPiatypeexvra|cion ciency 11p1p4bTO and OOFbo,gsrewaemlsarr| We plan on having two trated paper products analyzed. [r[ esidPaper [6TPapert [UnPatperr[4eat [e 4d ] 2102 tsoatmalplterseaatendalaynzdeduntreated articles 111. Pr`oNduumcbterFoorfmSualmaptlieosnsReSqaumiprleedsfor Analysis Approx. vol of Formulation] 40m Formulation 11 [FormulationIIT] 40 mL 40 mL FFoorrmmuullaattiioonn VV-T 1] 7 40 mL d40ommLi [FormulationVit 1 Formulation VIL dom. ome [FX oFromrmuutlaattiioonn X I 1 ET E dAommL_____| Formulation XI[v1 40 mL [Formulation Xi dom. 2 9 NSLaOmiMplSneIsMAaSnSdASiudgganes.teoPsdfASDva,imycpleisnsagnPdroPcreodduurcets oRAFT Fabry 12,2003 IV. Procedure for Preparing Samples ox"Tfihtishsesftpourrdetylhiesmhaionnuaallrdyysisbsteuovdfiyehiwesetdeosudtessamuobsnscstrteaernncaietnigtnhsectausrdupyiet.tab(Cisulihrtaryveoinfntgltsyh),e,aetvxeaxitlsiitldieanstgaeLdndOmMepatSpheIordM.oSlTomhgeeytpdhuoorgdpsotnsooet analyze the test substance inyour matrices. A report detailing the methodology used to abtain 70-10% extraction efficiencies for 1 ppb, 10 ppb and 100 ppb test substance in each of these eotalhrcoehgeyamtwait1lrlpipbcbee,sdew1it0lelprpmbibenaaevndadibly1a0be0lxetptrpoabaclotlniTn6tRgwPounmsteurmcacbteecsrdssi.avretidTcahlyeess.a(cecuucrhacoyfcaanrdpepr,ecpiaspieornoafndthteextmielte)hodOnce validated and verified for accuracy and precision, this method will be used to analyze our stnaaokmwepnl1i2ngtgrpeeranoteecrdeadatuartreiecrlseesup.rseesIdenntotoargtdieevrneetrsoaamtmipntlhieemsifeozresactmahcpehlvearsraibtaebeiddliotacrytuiimcnleesn.atmeIptdliiasnngid,mpriotertitasaiknneetdyhitanhtasttohsuetrepsstubdey records A. TextileSamplingProcedure 1. Determine the sizeof a2-gram sampleofpaper 2. Suggested sampling approach TreatedSamplesfromRollofFabric: sf"Iwrfaottmhechtht0er.ev5aetrmeydeotsuaetmsplioldneegoifsftrthoaekmetnrohleflre-onmdeqaoufitrovhlalel,efnritroslt0doifastcfaalrebdarsitcaomneinwirmaupm tofhe1 mteakteeraofffulalbwriidcth Create a grid with pencil on the treated fabric, eliminating 3-5 cm from the fabric edges. a`Trheeasgrwihdesrheoyulodu bweilcloamkpeosoende sofasmpilxe.equDiivvaliednetcbalcohcoksf.thTehelsaregesibxlobclkosckisntroepsrmeaslelnetrthe six `ablglleonctekhrsea,tSesmoaltlihesatrtobcflaorcchaknssduiobnm-ebalnocuchmkbleairsrgseeqrbuibelvtoawcleke.ennt UtI soaean&d2-rtgharenadnmoumsmabnmepurlmeb.ofesrmSyagsletnleeemrraattbiolcroacl(kilsny Einnxuccmaebclehrto slaarmgpelreloicnkc.achUsleargtehre bflirosctk.six numbers to select the six locations ofthe tested article "If cach discrete squareof treated fabric is small enough to generate one to sixsamples, dtteaaskkieegoonnneecorrnaacennpddtoommdesssaacmrmippblleeedfarboomve.eacThhedrisecfroertee,sfqruoamresoifxtdriesactreetdefsaqburiacreussionfgrteheebdlofcakbric, intrested Fabric Samples `Uanvtoriedactoendtafmaibrniactisoanm;plseusppclaynfboeurtauknternerataenddosammlpylefsr.om untreated fabric - avoid edges -- 3 10 . _ SLaCmMplSeIsMaSndASnuaggleysstieodsf SAaimplleisnganPdroPcreodduurcets DRAFT MFeabnriuyanryA12t.o20d0a3s, PhD 3. Document the sampling approach. B. PaperSamplingProcedure 1. Determine the size of 2-gram sample ofpaper. 2. Suggested sampling approach: "ITfrteraetaetdeSdasmapmlpelsefsrotmakReolnlforfomPaapeolrl, first discard a minimum of | mete ofpaper fswraotmcthhe0.v5ermyetoeurtsliodnegoffrtohme trohlele-nedoqufivtahleenotll0ofapalpeaesrt oinnethwerlaopt s-atmhpelne.take a full-width Crriedastheoaulgdribdewciotmhppoesnceidloofnstihxeepqaupievra,leenltimbiloncaktsi.ngT3h-e5scemsifxrbolmoctkhse praepperrseendtgetsh.e sTihxe ablroccakssw,hSeorethaytoucawcihllsutbak-eblooncek siasmepqluei.valDeinvtidteo aca2c-hgorfatmhseamlparlgee.blSoycsktsemianttiocaslmlayllneurmber agelntehreatSemaalllisetrobflorcaknsdionmeancuhmblearrgserbbeltowceke.n U1 sanead rthaendnoummbneurmbofersmgalelneerrbaltoc(okirsn einxccealc)hto slaarmgpelreblioncke.achUsleartghere bfilrostcksix numbers to select the six locations of the trated article "TIrfeeaatcehdSSaqmuparleeosffdriosmcDrietsecrtreetaetSeqdupaarpeesroifs sPmaapllerenough to gencrate one 10 six samples, dteaskceroinbeedraabnodvoe.m saThmeprleefofrre,omfreoamchsisxqudairsceoreftetrseqautaerdespoafpetrreuastiendgptahpeerb,loackkedeosniegnracnondcoempt sample. Collect ix samples. "UUnnitreeeaatteeddPsaapmeprlSeasmcpalnesbe taken randomly from untreatedpaper -- avoid edges - avoid contamination; supply four untreated samples. 3. Document your sampling approach. C. CarpetSampling Procedure s1.haDveintgesr.mine the sizeof carpet that will produce approximately 10-grammsof carpet 2. Suggested sampling approach: `ISFacmaplcehsfdirsocrmeDtiesscercettieoSne/csqtuiaornesooftfrCeaartpedetcarpet can generate one to six samples, take. odensecrriabneddoambsovaempfloer fterxotimleeaacnhd speacpteiro.noTfherreeaftoerde,cafrrpoemt suisxindgistchreetbelsockqduesioagfntrrceoeantcseedpt carpet take one random sample. 4 1 - -- SLaCm/pMlSes/ManSdASnuaglgyessitseodfSAamrpcliengaPnrdoPcreodduurcets DRAFT FMeabrriuyarnyA.12S,t2ad0a0l3is, PhD. ~frWohmenthesacmaprlpeetlboaccatkiionng.is Sihdeenatriffiiebde,rsusaes hcaliorseshteoacrasrptoetrebamcokviencgaarspeptossshiabvlie.ngsIt(ifsibers) recommended to clear contaminated with the the test hair shears substance. with cheesecloth, as cheesecloth should not be Untreated SamplesofCarpet ~Unaivroeiadtecdonstaammpilneastoiofn;casruppeptlcyanfobuer ntiakreenatreadndsoammlpylefsroofmcuanrtpreetatsehdavcianrgsp.et -avoid edges 3. Document your sampling approach. V. Sample Packing Procedure A. Aticles Triple wrap foil that s at each least sample with 25-cm long. aFlouldmifnoiulmatfotihl.e mFiodra-p1o0i-oncftm tshqeualernegtsha.mplPel,acceutaratipclieecien of the pocket. crimp tight. Fold-up Repeat about I cm on with two more epaicecheseodgfe.alFuomlidnuupmafnoiol.thePrlaccmeoifn zciapc-hloccdkgeb. aT-ghen remove air from bag and scal. nPluamcbeerisn oanseocuosniddezoifplsoecckonbadg.plaPsltiaccebapgr.ovSidaemdplleabeslhsouwlidthbesalmapbleleedidweinttihfiPcraotjieocnt cNluemarbleyrs,taSteaimfsplaempIldeentiisfitcraetaitoend Norumunbtererataend.d sCaommpplleettyepe.SamSpulmeplIedelnatbieflicsahtoiuonldShaseoe.t for the study records ~Sample shipped oindeFnteibfriucaartiyon13n,u2m0b0e3r.s have been provided in excel spreadsheet. Labels will be "Pack untreated sample separately from treated samples. Includae chain-of-custody form in cach package. Follow shipping procedure. B. Products s- hPilpamceent4.0 mDLouboflep-rboadgucctacfhorsmaumlpatlieo,nuussinegd z1i0pt-rleoactkarptliacslteicinbatghse. apPplraocperilaatbeelcwointthaisnaermsplfeor biadge.niiIfinccaltuidoen cnhuamibne-orf,-cpruosjteocdtynfuomrbmearndanmdodsiafmipelde MloSt DnuSmbinebrooxncoounttsaiidneionfgsfeocromunldatpleadstic `pCroomdpulcettseaSmpalmepsl.e SIhdienptipfriocdauticotnsSsheepeatraftoerlythferostmuadrytircleecso.rdsF.ollow shipment procedures. 12 5