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Analytical Report
I
Fluorochemical Characterization of Filter Samples
_
Particle Size Distribution Study 3/04
|
Exygen Research Laboratory Report No. L0002178
[
Testing Laboratory
=
Exygen Research
[
3058 Research Drive
State College, PA 16801
F
Requester
Michael D. Aucoin
URS Corporation
|
Barley Mill Plaza
Bldg 27 Room 1260
[5
Lancaster Pike and Rt 141
(
Wilmington, DE 19805
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1 Introduction
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presents resus assigned o Exygen Research study number LODO2178.
|
Speci fluorochemical characterization by uid chromatograph/y tandem mass spectrometry
(LCMSMMS) was requested for all samples. A total of 29 samples were received for analysis.
I
Thesampleswerepreparedandanalyzedby LC/MSMSfo the following stof uorocherricas
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+ Table 1:TargetAnalysis
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2 Sample Receipt
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3 Holding Times
--~
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witin 14 days of colecton.
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4 Methods - Analytical and Preparatory
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41 LC/MSIMS
41.1 Sample Preparation for LC/MS/MS Analysis
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PFOA was extracted from he fterbyshaking ovemight wih 40 mL of reagent grade viter.
.
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methanol was colected for analysis by LOMSMS. This treatment resuted in anaightfod
`concentration of the samples prior to analysis.
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|
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412 Sample AnalbyyLsOiSsS
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an(aSlRyMt)i.caldSaatmaplceasnbweefre eoxtrianucAtetdancohnmde4/n3t0D4. and analyzed between 44/04 and 477/04. Faw
5 Analysis
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|-
51 ACa6l-ipboriantciaolnbration curve was analyzed at the beginning of the analycal sequence and
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fCoarfstarmaptloens.standards for MS/MSanalysiswereprepausrinegthde same SPE procedure used
For the resus reported hero, callration criteria wor me.
| -
52 ExeBtxrltaraaccnttikioosnnbbllaannkkssswheoruedpnrootphaarveedaannydtaarngaeltyzaendawlyitehsepverreyseexntartacotriaobnobvaettchheofcosnacmenptlreast.ioTnhoof
he low-evol calbraton standard. For these samples, ha extraction banks were compiant
|
hlIeanvvsetelrcuaamnlebynrtattbairloganentksstaaninnadltayhrtede,sfoaprnrmdoesfaefncttlreaaktnnoomrwetnahbahoinvgohel-ltsehovelevlelsnoatwmAwpaleveresol.aclasAlogbaraiannta,lotynhzeesdtbaaanndfatkrrsde.svheroFyuorlhitnghohet-
samples prosented heretheinstrument baarnecomkpliasnt.
|
53 `SSuurrrrogoagteastpieksesarenotacompoofthneLeGMSnIMtS analyical metho.
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5.4 spMMaaktterirdxixsaptiSk2pelseivwkeelers/esannlodatabnporarelapyatzroeerddyffoCorrotnPhFteOrsAoe.lsAaSmcapclomeppsi;laehbolswoervero, tcwo bowlaenrkvefseeertaprtap7a0ir-s1w3se0r%e
|
Sampo recoveries wers win the acceptable range. Matix spike recoveries are given i
:
Attachment B.
55 SDaumplpicdauptleiscateswerenot perforfomrhedsstudy.
Pacesoes n0579
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56
`STawomapnlaleytoRaellrauntsewdeCroopmemrfeonrtmsefdo ualtycontrolnarrativefo each un.
compthleseamtplee
analysis.
The
foloiwsaibnrigef
f "AnalRuy n Numt ber i Sampc lesAa nalyl zed Comments
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6 Data Summary
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25Plauags/afslcreats PaFOcA hAfmoraedentated ising ofthe analytical esuls. Al resus are reported
|
_
Pace ors
cnnsse
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|-
7 Data/Sample Retention
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8 Attachments
[
81 AtactAmRoesnutts
82 AttBa:Mac trih xSpim keRe ecovn erit es:
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83 AtachmentC: Chan of Custody
84 Atachment: LOMSMS RawAnalytoal Data
[
85 tachment: Sandrcs Data
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9 Signatures
|
|
MF
7fd
Rnery, Operations Manager
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Kevin J Lioyd, Vice President
|| Other Lab MembersContributto Diantga
Karen Smit
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ND <L0D <NO<10Q =
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Attachment B: LC/MS/MSLaboratory Spike Recovery
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LC/MS/MS SYSTEM AND OPERATING CONDITIONS
|
`SponsorProtocolNo:NA
Exveen Study No: 12178
.
Instrument:
Micromass Quatio Ultima (LC/MS/MS Unit #7)
|
Computer
COMPAQProfessionalWorkstation AP200
|e
Software:
MMiiccrroosmoafstsWLiinmditoewd:s NMTa:ssVeLrysnixon3.44BBuuiilldd 1030814: Service Pack 5
|
HPLC Equipment: HeHwHlPePtBtAiuPnoacsPkauammrpdple(HrP) Series 1100HHPP CVoalcuumunmODveegnasser
|
HPLC Column: Genesis C-8, Som x 2.1mm id. x 4 (Exygen ID: MAI3296)
(JONESCHROMATOGRAPHY:Part No. FK5962EJ)
Mobile Phase (A): 2 mM Ammonium Acetate in Type I Water
|
Mobile Phase (B): Methanol
6)ot oX
|-
Analyst:
KE3a0vr3re8naReRsiosehaaarchtDrive, State College, PA 16501
Phone: (814) 272-1039 FAX: (14) 231-1580
L
NOTE: The next 3 pages are computer generated printouts from
the masslynx software program. The pages contain the
|
instrument settings used for the analysis of this data set.
|
All Handwritten Peak ID's by: 2 los et
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In order to verify mass resolution, a calibration check is performed on the mass spectrometer using a Nal/Rb/Cs tuning solution. The tuning solution is infused
|
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|
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Page 1
Sample List: P:\Data\LCMSHS?\Masalynx\008 APFO.PRONSampleD\O40304A Filter paper
| _ HLLeaatssnttodmmsooddiiffiieedd:: TMFiuo\enDaMAtaparr\L20C35HS01H60S::?4584\::N23a42ssl22y00n00x44\008 APFO.PRO\MOtEDB\031704 PFO &
|
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Page 2
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| HLlaaatsshttodmm:ooddiiffiieedd:: MTouAneDaANEpaarr\L02C53NS01M60S::745\84H::2a34s2s12200y00n48x\008 APFO.PRO\NGEEDB\031704 PFOA
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|
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04-Apr-2004 09:59:4
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| ||
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1.00
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| Sxygen Reseaxch, 3059 Ressarch Drive. State College, 7A 16601 l
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Sample List: P:\Data\LCMSMST\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper
| HeLLaatsshttodmm:ooddiiffiieedd:: MPTu7oe\nDMaAaLprar\L025C3NS01H60S::?45\84H::a2342ssl22y000n04x4\008 APFO.PRO\NGEDB\031704 PFOA
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Page 28
|
Sample List: NLoatshtodm:odified:
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v073
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||
qStuuadnytiNfoy.:SLa2m1p7l8e, ReSpetorNto.:040304A, Ext.Date:04/03/04, Analyst:K.Risha
Page 35
Sample List: P:\Data\LCSHST\asalynx\003 APFO.PRO\SampleDB\040304A Filter paper
| HLLoaatsshttodmm:ooddiiffiieedd:: PTM:uo\enDaMAtaparr\L023C5NS10H06S::754\48N::a3224ssl22y00n00x44\008 APFO.PRO\NethDB\031704 PFOA
[ ----domcoder--------
Printed: Mon ApE 05 07:35:10 2004
|| NTaamxe:: 040304A-1035
| 1: ern
_
| . 1217817
04030441035 Sm (Mn, 262)
[fe11
|
%
| oC 100 200 3.00
co ---------------- 04-Apr-2L0C0I4M1S7I:4M7S:5#1) MRM of 1 Channel ES-
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| QSutatndtyiNfoy.:SLa3m1p7l3e, ReSpeotrtNo.:040304A, Ext.Date:04/03/04, Analyst:X.Risha
Page 36
|
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oPn:\Dhapta\0L5QH0S6M:S475\:M2a4ss2l0y0n8x\008 7 i\Data\L\MCagHsLSynHx\S00T8
APFO.PRO\SampleDB\010304A Filter APFO.PRO\NOthDE\031704 PFOA
paper
----JoLbas-tcomotdeirfiad: Tue Mar 23 10:54:32 2004
Text:
| L21e7e8-r18
104030441036 Sm (Min, 2:2) 100;7
[=i
| - Od1er |
100 | 2.00
04-Apr-2004 18:04:27
LCIMSIMS#7
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MRM of 1 Cha4n1ne3"l>13E34S66-08)
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. u075
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MoNnonAEpE Er 05 06:4E8:n 2L4 E20E048an o9r8oPsaOaNnaSnAoSsSAO31Pier
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Page 38
|
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MBPoRrnD\DAeaptraL\0L5\CH0LS6H:SG47\8\M:HHa2as4sEssl2lNy0yn0nx4xS\\00T0088
APFO.PRO\SampleDB\040304A Filter APFO.PRO\MetHDE\031704 PFO
paper
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Mon Apr 05 07:35:10 2004
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Page 39
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HE Seatmnpolde:L List:
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APFO.PRO\SspleDE\GA0I04R Filter APFO.PRO\NSCHDS\G31704 PFOA
paper
coYagst emodnifited::TTuona tMaart 33 1T03:1540:333 2004
----
| eTemnetrs cassoancsons
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|~
L2178-21
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04-Apr-2004 18:54:41 LC/MS/MS #:
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| | . \ : \ Sxygen Research, 3058 Ressarch Drive, State College, PA 16601
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| | ouncssE y sampE le Reporrte. c040304A, Bxt.Date:08/03/04, AnalystiK.Risha
Page 40
sample List: Pr\Data\LCMSST\Masslynx\008 APFO.PRO\SampleDB\O40304A Filter paper
F1| | SMeeLatishtodma:ostdsiicftiioeeadr::sTMP:uo\snDaWAtaparr\L20C95MS10N06S1:754s\48M1:ea3234srsl22ey00n00x44\008
APFO.PRO\MethDB\031704
PFOA
--
| pwrmae:t osos0sn-r000 | Coen Xcus2s044, 250 ngiL standard
|040304A-10S4m0 (Mn, 2:2)
|: | "
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04-Apr-2004 19:11:28) MRMofL1CCIhMaSn1nI3eM>lS3E#6S79-))|
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|
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QSuvaanrtiHtby. s2a0m7pl3e, ReSuprorMto.1040304, Bxt.Dater04/03/04, Amalyst:K.Risha
Page 41
Sample List: P:\Date\LCHNMS?\Masslymc\0DS ARFO.PRO\SSEplsDE\G40304A Filter paper
| -SaMLLneaatasshttnodmmasooeddii,tffiiieeeddd:: TMPTouooesnnrAWtaeparrr\0359L01m60C:145084H:1ua23s43Ss122y00H0a044r\--0S08 APFO.PROVMLADE\031704 FOR
pred 1. pron
|
L2178-22
[of [. a040030)4A-1041 Sm (Mn, 2x2)
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04-Apr-2004 19:28:16
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| Sxygen Research, 3058 Ressarch Drive, State Colleg"e, PA 16801 C2456ubol
SQueaanytitNoy.1s2a2m3p7l8e, ReSpetortMo.:040304A, Ext.Date:04/03/04, Analyst:X.Risha
sage 42
|
pSamrplee sListt:o Method:
7sPornA\DDhartaak\oLFaCcH\SeNLStTCr\MiMHaiasdsSss10lNyydnnSXx\\T0000\88
APFO.PRO\SempleDB\040304A Filter APFO.PRO\HOtHDB\031704 POM
paper
| lamsetemdodtified: Tue Nar 2 23 10:54:32 2004 -
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| : L2178-23 040304A-1042 Sm (Mn, 2x2) |":
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Page 44
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MBBoi\n\oDAapatraL\0L5aCH\0S6HL:S4TC8\H:UMa2as4Esss12Nly0ym0Smx8\\T0000\88
APFO.7RO\SaapleDS\040304A Filter APFO.PRO\NSERDB\031704 PFO
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Page 45
| mSaamplmeodLiifsit:ca: woPnr\Dhaotra\oLbCHoScNsStTe\iMiaissal0y0ntx\008 APFO.PRO\SaspleDS\040304A Filter paper
MaLatshtodm:odifisd: TPuAePWAaLr\L3C3HS1N0S:75\4N:a3s2s210y0n4x\008 APFO.PRO\MGEDE\031704 PFOA
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Page 47
| - SLaasmtplmeodLiifsit:ed: MPo:n\DAaDtEa\0L5CH0S6M:S4?8\:M2a4ss2l0y0n4x\008 APFO.PRO\SampleDB\040304A Filter paper
| dLoatshtodm:odified: \TuDeatMaa\rLC2H3SI1S07:\54K:a3s2s12y0n0x8\008 APFO.PRO\MethDB\G31704 PFOA --gebeoder
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rage 48
Sample List: P:\Data\LCMSHS?\Masslynx\008 APFO.PRO\SampleDB\040304A Filter paper | MLeatshtodmsodified: MPo:n \ApDr a05ta06\:4\L8:aC2s4HsL2Sy0n0Hx4\S00?8 APFO.PRO\NGthDB\031704 PFOA ~ JLasot mbodcifi--oed:dTeus rMar 23 10:54:32 T2004
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Page 49
Sample List: P:\Data\LCHSMST\Masslynx\008 APFO.PRO\SampleDB\O40304A Filter paper | NLoatshtodm:odified: MPo:n\DaAtpar\L0C5HS0H6S:T48\:a2s4s12y0n0x4\008 APFO.PRO\MethDB\03L704 PFOA ~--sLbasotomotdiefised--: ~ Tue Mar~ 23 10:5P 4:32M2004
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04-Apr-2004 21:41. 4
LC/MS/MS #:
040304A-1049 Sm (Mn, 2x2)
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84523521
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LC/MS/MS SYSTEM AND OPERATING CONDITIONS
Sponsor Protocol No: NA
Exuen Study No: 12178
Instrument compen Software:
MicromassQuatzo Ultima (LCMSAMS Unit #7) coMPAQProesioml WorksaiAonPO
Microsoft Windows NT: Vers4iBuoilnd 1381: Service Pack
Micromass Limited: MassLynx 3.4 Build 004
HPLC Equipment:
Hewlett Packard (HP) Series 1100
HP Bin Pump
HP Vacuum Degasser
HP Autosampler
HP Column Oven
HPLC Column:
G(eJneOsiNsEC-S8,CSHcRmOxM2.A1 TmOmGi.Rd.AxPP4aHptYN(Eo:x,ygFeRnSI9D6:2MEA)13296)
Mobile Phas (A): 2mMAmmonium Acetate in TypWateer
ol
Mobile Phase (B): ~~ Methanol
Yule?
Avalyst
KarenRisha
E3Ph0xo3yn8gee:Rne(sR5ee1as4re)cah2rc7Dh2r1i0v,39StFatAeXC.ol(l5e1g4e), 2P3A1.116558001
NOTE: The next 3 pages are computer generated printouts from the masslynx software program. The pages contain the
instrument settings used for the analysis of this data set.
All Handwritten Peak ID's by:
_
||
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|
MS scan from 80 to 1380 amu is performed on both MS1 and MS2. The
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|
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| Last modified: Wed Apr 07 08:02:10 2004
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Sample List: P:\Data\LCMSMS7\Masslynx\00 APFO.PRO\SampleDB\040304AR Filter paper
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paper
L last moL dified: Tue-- Mar 23 10:54:32-- 2004 ----eeee--
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07-Apr-2004 02:17:18
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APFO.PRO\SampleDB\040304AR Filter
APFO.PRO\NOtHDE\031704 PFOA
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i Last modified: Tue Mar 23 10:54:32 20-- 04
| NToamxae:s 040304AR-325
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07-Apr-2004 02:34:03
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Sample List: P:\Data\LCHSHST\Masslynx\008 APFO.PRO\SampleDB\O40304AR Filter paper
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I ~ HSaatmhpolde:List:
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paper
T Tast modified: TuR e Mar 23 10:54:32 2004 ee
_
| NTaemxet:: 040304AR-327
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Page 28
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WPe+d\DAaptra\0L7CM0S8K:S072\:M1a0ss2l0y0n4x\008 Pe\Data\LCMaHssSLNynSx\700\8
APFO.PRO\SampleDB\040304AR Filter APFO.PRO\NethDB\031704 PFOA
paper
oLabstComdodeisfied: Tue Mar 23 10:54:32 2004 ------------------------------
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GTaeskemlodified: TTueaar Mar 73E10l:54o:3i7 2s004a
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| Memtmeeaeified: Tue Mar 23 1015~4132~20~08~
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= Laosttmmaodritfied: Tuoe Mear 23 10:54:32E2004h --
--_--
| NTaemxet:: 040304AR-333 | xeceoorsois,250 ng/L standard
040304AR-333 Sm (Mn, 2x2) | 100
07-Apr-2004 04:47:5:
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| oaosntcomoddiefried: Tue e Mar 2m 3 1054132 2008
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Ext.Date:04/03/04, Analyst:K.Risha
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Sample List: B:\Date\LCHOHS?\Masslymx\008 APFO.SRO\smLeDB\O4DI0ANR Filter paper
| eHLFaae tsthtosmh:oadaitfeieedd:: uWB eod AHparro S03By57u0s180y:in 0o24:+e13a05s22ve 00a00t40\0e0e8ereAePmFmOe.eBeRmOm\eNeArErEDBG3170e8 aPIOmN es
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MLeatshtodm:odified: PT:u\eDaMtaar\L2C3HS1K0S:75\4H:a32ssl2y0n0x4\008 APFO.PRO\NethDB\031704 POA
| --obrracceesmer--wea nor 07 assonsen 2000
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RESEARCH
S3i0t5e8 CReoslelaergcehPDAriv1e6.801 .
SP 3800 PhoFnaec: s81a4:n2712.a10m39
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Exygen Study No: __
FR TANT COMMINCATIINE
Page [of |
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|
Person: _Ken
Company: _Aldrich
|
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Originator: ~~ Exygen __x Sponsor
Date: _12/08/03
Time: _1022
Notes:
Icalled Aldrich tech service at 1-800-231-8327 to ask the shelf life of the PFOA standard
|
Ireceived today. Ken, an Aldrich rep in technical service, toldme that the shelf life is
2 years from the date of receipt stored at room temperature.
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THIS 1S AN EXACT COPY OF
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cram 0150 August 7.20001
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Fax: 814-231-1580
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i PREPARATION OFSTOCKSTANDARDSOLUTION
I Protocol Number: __\[A
BxygenStudy Number: D0B-APED
|
Compound:
FENTAMCAR
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UORDCCTANDICACI,
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LotNumber: 200002.
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Source:CMWENRONS Purity: 47% DateLastCharacterized: s1li5|02
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Date Standard Received: _0M|0A0%
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Net Wt. ofMaterial: 0.61031 _g
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Manufacturer: EM
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Lot Number:_U3238336"
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Storage Conditions for Solution:
|
. FreezerNumber: _T_--_aRdefwrhiigcehroafttohr Naubmobvera:ppe_a2l2, axRooatoomn.Temperature: _~
|
REMARKS:
|| Signature: lo cnavaDaate: [U0125773ly 18,2008
.
3058 Research Drive. Phone: 814-272-1039
State College, PA 16801
Fax: 814-231-1580
RESEARCH
PREPARATIOOFN FORTIFICATION STANDARD SOLUTIONS
-
Exygen Study Project Number:
`Customer Project Number:
!
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Date Prepared:
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REGU Lb
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METHANOL
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