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OS AR226-2660 RESEARCH Precise Research. \ Proven Results. AR226-2660 Analytical Report Air Sampling Fluorochemical Report DuPont Washington Works - Air Sampling Program Round 4 Exygen Research Report No. L0001359 Testing Laboratory Exygen Research . 3058 Research Drive State College, PA 16801 Requester Michael D Aueoin URS Corporation Barley Mill Plaza Building 27 Room 1260 Lancaster Pike and Rt 141 Wilmington, DE, 19805 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Pae 1 of 7 3058 Research Drive State College, PA 16801, USA T: 800.281.3219 F: 814.272.1019 exvgen.com Summary '.'.!;::'.'". '. '''/"'"\- '. ".'/-' ',..; .'.' . Seven solid media samples were received by Centre Analytical Laboratories, Inc. (dba Exygen Research) (Exygen) from DuPont Corporation. The media represent samples of air collected on OVS tubes. Please see Table 1 for a completed listing of samples received and field air volumes collected. : , , ? ' . -:;' ' . ' '.. ' . ' ,. ' '' : ' ' . " . . .. The samples were analyzed for Perfluorooctanoic Acid (C8 Acid) using liquid chromatography / mass spectrometry (LCMS). The method employed is entitled "Method of Analysis for the Determination of Perfluorooctanoic Acid (PFOA) in OVS Airtubes by LCMS" (James Miller, Exygen Research, February 17, 2003). The OVS tubes were separated into three fractions for specific fluorochemical analysis. Fraction A consisted of the filter, backing material and plastic ring. Fraction B contained the first bed of XAD resin and the PUF backing. Fraction C contained the second bed of XAD resin and PUF backing. Fractions A and B were extracted with 1 mL of methanol. Fraction C |||| was not analyzed but saved for possible future analysis. Perfluorodecanoic Acid (C10 Acid) J*''/was added as a surrogate spike to each fraction prior to extraction. Sample WWK-A-AMS6-E4 was not analyzed as per client request. ' I ' ' ' ' ' ' ; .' - ' ' ' . ^.'.''' ' .-'' ^ ',' .' . . . . . , I ., Instrument operating conditions can be found at the beginning of each analytical run. Raw instrument data is given in Appendix A. Chain-of-custody information can be found in I AppendixB.. ; ALL DATA" CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 2 of 7 Results Summary Request # . WWK-A-AMS1-E4A WWK-A-AMS1-E4B , . , WWK-A-AMS1-E4C WWK-A-AMS1-E4 (Total) Air Volume Sampied(L) 1432 : ' -" . . 1432 1432 C8Acid . (mfl/m3) < 0.00.007 < 0.00007 NA < 0.00014 WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B WWK-A-AMS2-E4 C WWK-A-AMS2-E4 (Total) 1458 : 1458 1458 0.0002 <0.00007 NA 0.0002 WWK-A-AMS3-E4 A : WWK-A-AMS3-E4 B WWK-A-EMS3-E4 C WWK-A-EMS3-E4 (Total) 1468 1468 1468 0.0002 < 0.00007 NA 0.0002- WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B " WWK-A-AMS4-E4 C WWK-A-AMS4-E4 (Total) , 1421 : : .. ' .'1421' . . 1421 ' : , . WWK-A-AMS5-E4 A ': '.. . WWK-A-AMS5-E4 B WWK-A-AMS5-E4 C . WWK-A-AMS5-E24(Total) 1435 1435 . 1435 <0.00007 < 0.00007 NA < 0.00014 < 0.00007 < 0.00007 NA <0.00014 NA - Not Analyzed. Fraction B was below the quantitation limit, therefore the backup fraction does not require analysis. 1. ."<" is defined as not detected at or above the reported level. 2. .Sample results have not been corrected for blank results or control spike recoveries. 3. Please note the following descriptions of the OVS sample tube fractions: Fraction Fraction Description Frit Extract 1st set beads extract 2nd set beads extract (not analyzed) ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Paae3of7 'i^^^' QC Data LCS Please note: One control sample was spiked with each perfluorooctanoic acid to give a final concentration of 500 pp through the tube at a rate of 1-liter per minute for one hour (60 liters of air). The fractions were separated and analy acceptable range for control recovery is 75-125%. Request # Control 1 C8 Acid (amount spiked - ppb) 500 CSAcid (amount recovered 499 ppb) CSAcid (percent recovery 100 Blanks Request # WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B Vol. Of Air {L) 0 .: -1 . ' ' '0 .'. 11" ': CSAcid (ug/fraction) <0.10 . <0.10 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 4 of 7 Surrogates . : . .'. :. A surrogate spike (C10 Acid) was added to all OVS tubes to give a final concentration of 500 ppb in the extract. Surrogate spike recoveries are given in the following table.. There are no set criteria for surrogate spike recoveries. Advisory ranges are 75-125%. Sample # Amount Spiked (PPb) . ,Amount Recovered (PPb) Percent Recovery (%) WWK-A-AMSFBLK-E4 A 500 931 186* WWK-A-AMSFBLK-E4 B WWK-A-AMS1-E4A 500 500 443 " . 946 89 .. .: 189* . WWK-A-AMS1-E4B 500 - 465 93 WWK-A-AMS2-E4 A 500 : WWK-A-AMS2-E4 B : 500 ' . 802 :- < 498 ,: 161*100 WWK-A-AMS3-E4 A 500 797 159* WWK-A-AMS3-E4 B WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS5-E4 A WWK-A-AMS5-E4 B Control Spike A Control Spike B 500 ,' 500 500 ^ 500 500 ^ 500 500 474 794 471 : 804 ^ 424 '889 412 ,95 : 159* .94 161* : 85. - 178* 82 '''.' '''. * Surrogate recovery outside of advisory range. tl!^.i&ls's;* ' - ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 5 of 7 ; Calculations Request # WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMS1-E4A WWK-A-AMS1-E4B -WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS5-E4 A WWK-A-AMS5-E4 B Control Spike A Control Spike B Vol. Of Air (L) 0 0 1432 1432 1458 1458 1468 1468 1421 1421 1435 1435 0 0 C8 Acid (raw-ppb) <10 <10 <10 <10 311 <10 314 ' <10 <10 <10 <10 <10 499 <10 :C8Add (ug/fraction) <0.10 <0.10 <0.10 <0.10 0.31 <0.10 ,0.31 <0.10 <0.10 <0.10 <0.10 <0.10 0.50 <0.10 C8Acid (mg/m3) < 0.00007 < 0.00007 0.0002 < 0.00007 0.0002 < 0.00007 < 0.00007 < 0.00007 < 0.00007 < 0.00007 ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Page 6 of 7 Example Calculation For sample WWK-A-AMS2-E4 A C8 Acid, :. , . ; ' , .: = [311ng/mlofC8Acidx(lml)x(lug/1000ng)x(lmg/1000ug)] / [(1458 L)x (lm3 / 1000L)] . -, 0.0002 me / m3 Signatures Paul Connolly, LCMS Team Leader; aLmfUJ^ ' y/<<ffoohhnnMM, .Flaherty, Vice^resident Other Lab Members Contributing to Data James Miller ALL DATA CONTAINED IN THIS REPORT WAS GENERATED BY EXYGEN RESEARCH Pare 7 of 7 Table 1. Login Information / Field Data Sample ID Exygen LabID WWK-A-AM8FBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMSFBLK-E4 C WWK-A-AMS1-E4A WWK-A-AMS1-E4B WWK-A-AMS1-E4C WWK-A-AMS2-E4 A WWK-A-AMS2-E4B WWK-A-AMS2-E4 C WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS3-E4 C WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS4-E4 C WWK-A-AMS5-E4 A WWK-AAMS5-E4B WWK-A-AMS5-E4 C Control Spike A Control Spike B Control Spike C L0001359-1 L0001359-2 L0001359-3 L0001359-4 L0001359-5 L0001359-6 L0001359-7 L0001359-8 L0001359-9 L0001359-10 L0001359-11 L0001359-12 L0001359-13 L0001359-14 L0001359-15 L0001359-16 L0001359-17 L0001359-18 L0001359-19 L0001359-20 L0001359-21 Date Received Description 11/25/03' 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1st set beads extract 2nd set beads extract Frit extract 1 st set beads extract 2nd set beads extract Air Volume Sampled (L) ! ... ! .: '!1 : Q . .' .. 0 ' 0 . . . . '': /:' ,.. ' " ' ' . U32 ; . 1432 - 1432 1458 1458 1458 1468 1468 ; 1468 ' : , , . 1421 . ' ',' ., ,1421. '.:'.', .' 1421 . ; ^1435 - . . . ' 1435' 1435 ' '.' ' ' '0 ,'1 / ' ! ' 0' . - . , , . 0 Table 2. Chain of Custody Sample ID WWK-A-AMSFBLK-E4 A WWK-A-AMSFBLK-E4 B WWK-A-AMSFBLK-E4 C WWK-A-AMS1-E4A WWK-A-AMS1-E4B WWK-A-AMS1-E4C WWK-A-AMS2-E4 A WWK-A-AMS2-E4B WWK-A-AMS2-E4 C WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMS3-E4 C WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B WWK-A-AMS4-E4 C WWK-A-AMS5-E4 A WWK-AAMS5-E4B WWK-A-AMS5-E4 C Control Spike A Control Spike B Control Spike C Date Collected 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03 11/23/03' 11/23/03 11/23/03 NA . NA ' NA Date Received at Exygen 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 , 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 11/25/03 1 NA ;.NA , NA Date Extracted by Exygen Date Analyzed by Exygen 12/3/03 12/3/03 NA 12/3/03 12/3/03 : NA 12/3/03 , 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 . 12/3/03 NA 12/3/03 12/3/03 NA 12/3/03 12/3/03 : NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA , , 12/9-12/10/03 12/9-12/10/03 NA 12/9-12/10/03 12/9-12/10/03 NA 3058 Research Drive State College, PA 16801 EARCH ogin Phone:814-272-1039 Fax:814-231-1580 Login #: Project: L0001359 > 1,469 POOOQ419 ^ . Conform COC Sample: Conform COC: True True Project Storage: Submitted By: Status: ^ Michael D. Aucoin Unreceived Conform Sample: Conform Request: , True True Login Type: ' Started: Date Start: Due Date: Received Date: Received By: Immediate Receipt of Samples ' T '' - '. ' ' 11/25/2003 11:21:1 SAM 12/09/2003 11/25/2003 AMMERMAN, MARK .At^'f^ Spread Sample: Label: Project Title/Type: Analysis of PFOA in OVS Tubes / ROUTINE Login Notes: Conform Notes: As per Mike Aucoin, sample WWK-A-AMS6-E4 Is cancelled. MSA 11/25/03 PK0001939 Carton Mail Date / Condition Packages/Containers ' Shipper /_ID Temp. Control / Temperat. ; ; 11/25/2003 10:50:59AM FEDEX RT Package & Contents Uncompromised 8363913019820200 Direction / Handled By . RECEIVED AMMERMAN, MARK ^^intainer # C0020181 C0020182 C0020183 C0020184 C0020185 C0020186 C0020187 C0020188 C0020189 C0020190 C0020191 C0020192 C0020193 C0020194 C0020195 C0020196 C0020197 C0020198 C0020199 C0020200 C0020201 Gross Weight E" 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g 7.2 g; 7.2g 7.2g 7.1 g 7.1 g 7.1 g 7.2g 7.2g 7.2g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g 7.1 g Container Type Other , Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Other Miscellaneous Item Key None Description Preservative NONE NONE NONE NONE NONE NONE - ' NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE ICOC Mfg.J-ot UU54 11/25/2003 Login.rpt Report Version: Nov 13 2003 4:51 PM Page 1 of 4 Instance: R0074478 R0074478 inIs, Sample ID || 0001359-0001 001359-0002 Lncini'^P-OOOT . L0001359-0004 L000135S-0005 h900-1359-QOS6-" L0001359-0007 L0001359-0008 -L-eee+aS&eeeS-" , L0001359-0010 L0001359-0011 -Loooisso-we- L0001359-0013 L0001359-0014 teooisso oois> L0001359-0016 L0001359-0017 -tSQM 309-0018^ L0001359-0019 L0001359-0020 -t.0001359-0021-- Matrix GAS GAS (-'AC GAS GAS GAS GAS GAS GAS GAS GAS .GAS GAS GAS GAS GAS GAS GAS GAS GAS GAS ogin Fraction OVS Tubes OVSTubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVS Tubes OVSTubes OVS Tubes OVSTubes OVSTubes OVS Tubes OVSTubes OVSTubes OVSTubes OVS Tubes OVS Tubes Samples Sample . WWK-A-AMSFBLK-E4A: \ WWK-A-AMSFBLK-E4 B WWI<-A-AMBrDLK-C4CWWK-A-AMS1-E4A WWK-A-AMS1-E4 B , -WWK-A-AMS-bC^e-- . WWK-A-AMS2-E4 A WWK-A-AMS2-E4 B -\WW-fFfWSZ-E4-G-- . WWK-A-AMS3-E4 A WWK-A-AMS3-E4 B WWK-A-AMGO-E4 fr- WWK-A-AMS4-E4 A WWK-A-AMS4-E4 B VWVK A-AMS4 1:4 C- : WWK-A-AMS5-E4 A ' WWK-A-AMS5-E4 B ': - WW-firWQQ-mC Control 1 A Control 1 B --Contml -t-G-- ; . ? ^ : ^ ' , . . ;' ' ? ' ' Date Sampled Date Received 11/25/2003 11/25/2003 11/25/2003 11/25/2003 . . . 11/25/2003 11/25/2003 . 1.1/25/2003 ;: - 11/25/2003 11725/2003 11/25/2003 ' "11/25/2003 : : , .11/25/2003 . 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 11/25/2003 Date Due 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/2003 12/09/?n03 11/25/2003 Login.rpt U U3 3 Report Version: Nov 132003 4:51 PM Page 2 of 4 Instance: R0074478 R0074478 )001359-0001 Container C0020181 / Other/ NONE L0001359-0002 Container C0020182 /Other /NONE L0001359-0003 Container C0020183/Other/NONE L0001359-0004 Container C0020184 / Other / NONE L0001359-0005 Container C0020185/Other/NONE L0001359-0006 ,(& Container 1 "1020186/Other/NONE L0001359-0007 : Container C0020187 / Other / NONE L0001359-0008 Container C0020188 / Other / NONE L0001359-0009 Container C0020189/Other/NONE L0001359-0010 Container C0020190/Other/NONE L0001359-0011 Container C0020191/Other/NONE IKfcnoi 359-0012 Container 11/25/2003 Login.rpt ogin Bottles Method Method Method Method Method Method a.^ Method Method Method Method Method Method JU56 Report Version: Nov 13 2003 Page 3 of 4 4:51 PM Instance: R0074478 ^ 7433510464 C0020192/ Other /NONE ^001359-0013 y Container ^J020193 /Other /NONE L0001359-0014 . Container C0020194 /Other /NONE L0001359-0015 Container C0020195 /Other /NONE L0001359^0016 Container C0020196/Other/NONE L0001359-0017 Container C0020197 / Other / NONE L0001359-0018 Container ||j||C002019/8Other / NONE Lu001359-0019 Container C0020199 / Other / NONE L0001359-0020 Container C0020200 / Other /NONE L0001359-0021 Container C0020201/Other/NONE Method Method Method Method Method Method Method Method Method 11/25/2003 Login.rpt ^Ub7 Report Version: Nov-132003 4:51PM Page 4 of 4 Instance: R0074478 ^ 29464679 CHAIN OF CUSTODY/ANALYSIS RE RESEARCH ExygenResearchSample Receiving 3117 Research Drive 'State College, PA 16801, US T: 814,231.8032 F: 814.231.1580 exygenresearch.'com PROJECT INFORMATION A fffl^m Client (name & address): ;u\_^m ^ . ^v. Pn^A: ^y^Vum^tovx^LlQr^^ Phone; Fax: Sampler: ?)Ra.v wsi-\wr f<^ L.m^ Please fill out this form completelyto ensure Project Manager (Name & E-mail Address): n^cy-e .(^cjai/^ _ -- -- p - ( \ Project Name.^ r~\ U^ 5^vfW3^o<\ vfn^ixyv^ RO. #: \A 0 Quotation #: correct analysis and proper handling of your samples. Relinquished by % . ^^ua( Date Time l|^'4|o3o%'S>-0 OTHER INFORMATION b \ ^ Cooler ID # _j4Ail^~ Cooler Temp. (C) ^ Receiver by J, /Av. Of^ : 17 ..-.: ..//:. -.7/L--...--..--.,;.--., --.^.'...,'.- LAB USE ONLY Dat^-- P W^A " / 1 . ///2/A? Time ^^^ /,/-a Sampler(s): LK,REK DuPont Washington Works Air Sampling Program FedEx Airbill #: 836391301982 Event Number 669842 669908 669878' 669901 669769 669865 Hours 0 1 2 3 4 Field Blank: AMS-1 AMS-2 AMS-3 AMS-4 AMS-5 AMS-6 Minutes 0 , 60 120 180 240 yes yes or no WWK-A-AMS1-E4 WWK-A-AMS2-E4 WWK-A-AMS3-E4 WWK-A-AMS4-E4 WWK-A-AMS5-E4 WWK-A-AMS6-E4 Hours 5 6 7 8 9, : . WWK-K-AMSFBLK-E4 1.018 1.029 1.028 1.021 1.015 1.014 Minutes 300 360 420 480 540 23-Nov 23-Nov 23-Nov 23-Nov 23-Nov 23-Nov Hours 10 11 12 13 14 6:35 6:30 6:30 6:44 6:09 '6:56 Minutes 600 660 720 780 840 24-Nov 24-Nov 24-Nov 24-Nov 24-Nov 24-Nov Hours 15 16 17 18 19 6:12 6:22 6:22 6:34 6:01 6:45 Minutes 900 960 1020 1080 1140 . Weather; 11/23= 48 degrees andclear, expect temperature to go toupper 60's. , 11/24= 45 degrees and clear, expect rain and drop in temperature to 30's. 1.003 1.008 1.022 0.9668 0.9892 * Hours 20 21 22. 23 24 ! SAFER operational:! yes yes or no Comments: [Total minutes column is the reading from the monitor counter. * The pump for AMS6 was not running when we collected the sample and the counter only read 880 minutes. W get the AMS6 pump to run for Post Calibration even plugged into building outlet. We will replace pump before 11/24/03 11/25/2003 Page 2 of 2 9nn