Document GKMnJag4BX0jjayo1boDOne5v
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
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Formulation VIL
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Formulation XI[v1
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[Formulation Xi
dom.
2 9
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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,
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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.
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~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.
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