Document zQkEqn1N5aawk9Nz3ZkgOaZ26

I K } NORTHERN KENTUCKY OFFICE SUITE 340 1717 DIXIE HIGHWAY COVINGTON, KENTUCKY 41011-4704 () Y rP 606-331-2838 513-381-2838 FAX: 513-381 -6 6 13 DAYTON, OHIO OFFICE SUITE 900 110 NORTH MAIN STREET DAYTON, OHIO 45402-1786 937-228-2838 FAX: 937-228-2816 Ro b e r t a . Bilott (513) 357-9638 bilott@taftlaw.com TAFT, STETTINIUS & HOLLISTER LLP 425 WALNUT STREET, SUITE 1800 CINCINNATI, OHIO 45202-3957 513-381-2838 FAX: 513-381-0205 www.taftlaw.com CLEVELAND, OHIO OFFICE 3500 BP TOWER 200 PUBLIC SQUARE CLEVELAND, OHIO 44114-2302 216-241-2838 FAX: 216-241-3707 COLUMBUS, OHIO OFFICE 21 EAST STATE STREET COLUMBUS, OHIO 43215-4221 614-221-2838 FAX:614-221-2007 October 20, 2005 FEDERAL EXPRESS Dr. Charles M. Auer USEPA 1201 Constitution Avenue, N.W. Room 3166A Washington, DC 20004 Jennifer Seed USEPA 1201 Constitution Avenue, N.W. Room 6334A Washington, DC 20004 David Douglas Remediation Division Superfund & Emergency Response Section Minnesota Pollution Control Agency 520 Lafayette Road North St. Paul, MN 55155 Mary Dominiak USEPA 1201 Constitution Avenue, N.W. Room 441OS Washington, DC 20004 James Kelly, M.S. Health Assessor Site Assessment and Consultation Unit Environmental Health Division Minnesota Department of Health 121 E. 7th Place, Suite 360 St. Paul, MN 55164 N> C=> cOn Donald Kriens O Industrial Division Land & Water Quality Section --- CO Minnesota Pollution Control Agency 520 Lafayette Road North St. Paul, MN 55155 op o CO "o m --" O* O*t"i -- Re: Perfluorochemical Residential Exposure Data For Washington County. Minnesota Ladies and Gentlemen: In a letter dated May 12, 2005, we provided information regarding levels of various perfluorochemicals, including PFOA and PFOS, detected in blood, soil, and water in the vicinity of 3M's perfluorochemical operations in Minnesota. Since that submission, we have arranged for additional blood samples of individuals residing in communities that may have been impacted W0537662.1 I P-2 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 2 from perfluorochemical wastes attributable to 3M's Minnesota operations. In recognition of the potential threat to human health and the environment revealed by this data, and in response to USEPA's prior public requests for perfluorochemical monitoring data, we are providing copies of this additional data to you for inclusion in USEPA's Administrative Record 226 and OPPT2003-0012. The perfluorochemical (including PFOS and PFOA) results for serum samples collected and analyzed on behalf of Plaintiffs are summarized below. Please note that all results were provided by Axys Analytical Services LTD in Canada and were obtained, arranged for, and paid for without any involvement by 3M. In our May 12, 2005, letter, we presented charts summarizing the PFOA and PFOS serum and whole blood data collected from residents of Washington County, Minnesota, with the data organized by drinking water source. Since our May 12, 2005, submission, additional blood data has been collected from individuals consuming water provided by the City of Oakdale, Minnesota, where testing of the City's water supply wells has, on occasion, confirmed PFOS in levels exceeding the State of Minnesota's recommended Health Based Value ("HBV") of 1 part per billion (1 ppb), and levels of PFOA just below 1 ppb. (See AR-226-1929, 1933, and 1935) 3M also has reported detecting PFOS in tap samples from Oakdale as high as 0.95 ppb and PFOA as high as 0.71 ppb, indicating that the combined level of PFOS and PFOA in Oakdale water has exceeded the State's Hazard Index ("HI") of 1 for drinking water containing both PFOS and PFOA. (See AR-226-2737-39; AR-226-1945-46; Exhibit A (3M's HI calculations)) As 3M explained in its June 14, 2005, letter to USEPA, such cumulative amounts of PFCs in tap water exceeding the HI of 1 represent a level of PFCs that also exceeds the State's current, recommended HBVs, which the State uses to assess whether there is an unreasonable risk to human health. (See id.) There are now also data suggesting the possibility of additional perfluorochemicals, including PFBS (C-4) (a chemical 3M uses in on-going manufacturing processes), in the water near the impacted public water supplies. The presence of these other perfluorochemicals in water already contaminated with both PFOS and PFOA contributes to the threat of even greater cumulative toxicity concerns. (See Exhibit B) Some of these other PFCs, including PFBS (C-4), already have been detected in the blood of area residents, leading to very high cumulative PFC levels in their blood. (See Exhibit D; May 12, 2005, Letter (attached lab sheets)) Chart A below W0537662.I P-3 Dr. Charles M. Auer Jennifer Seed Mary Dominiak Janies Kelly David Douglas Donald Kriens October 20, 2005 Page 3 includes all of the original and new blood data for City of Oakdale water customers, including the cumulative, total amount of various pefluorochemicals detected in the blood samples.- The new data are in bold type. In our May 12, 2005, submission, we also provided data regarding the level of perfluorochemicals found in the blood of individuals consuming drinking water from private wells in the area of 3M's Minnesota operations. Since that submission, we have collected additional blood data from private well users in the Lake Elmo, Minnesota, area and have obtained some additional information from 3M and MDH regarding the level of PFOS and PFOA in some of those wells. (See Exhibit C (Excerpts from 3M's September 2,2005, Answers to Plaintiffs' Interrogatories) Chart B below provides a summary of all of the original Lake Elmo area private well blood and water data (now with cumulative totals for the perfluorochemical blood data), plus the new data obtained since May 12, 2005. The new data is in bold type. In order to avoid identification of individual identities, we have provided available private water well PFC data in a general range, as opposed to specific results. The lab results for the blood results are attached at Exhibit D. For privacy reasons, the names, addresses, and specific ages of each of those sampled are omitted from this submission. - Although the individual blood test result sheets attached to our May 12, 2005, letter referenced the levels of various perfluorochemicals detected in the individual blood samples, we did not include the cumulative totals in the charts set forth in our original, May 12, 2005, letter. We have now included the cumulative total PFC results from those lab sheets in the current charts. - The Minnesota Department of Health is currently using detection/reporting limits of 0.5 ppb and 1.0 ppb for PFOS and PFOA, respectively. (See Exhibit C ) W0537662.1 P-4 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 4 CHART A - OAKDALE CITY WATER CUSTOMERS SEX AGE YEARS ON PFOA PFOS TOTAL WATER iDDbVDllD. innbl/Dun. PFCslDDbl* M F M M M F F M M F M F F M F F M M W0537662.1 41-50 51-60 >70 51-60 61-70 51-60 41-50 51-60 >70 61-70 >70 41-50 51-60 31-40 >70 41-50 <18 41-50 N/A >30 >30 20-30 20-30 20-30 <10 20-30 N/A 20-30 >30 N/A 20-30 10-20 >30 N/A <10 10-20 121.0 117.0 105.0 104.0/103.0 100.00 96.1 95.1/89.1 86.8 82.3 80.5 78.6 77.5 74.9 74.6 69.3 69.0 68.3 63.3 109.0 91.8 113.0 70.3/72.7 131.0 67.8 85.9/79.8 125.0 118.0 163.0 112.0 78.4 61.1 91.0 102.0 77.2 50.1 76.7 267.12 240.06 241.45 192.44/195.54 293.08 180.2 200.71/186.15 248.01 221.79 212.40 210.63 178.51 152.72 182.36 191.84 163.79 134.12 158.88 P-5 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 5 SEX F F F M F F F M M M M M F M F F M F F W0537662.1 AGE 41-50 61-70 61-70 61-70 61-70 41-50 31-40 51-60 41-50 18-30 <18 61-70 18-30 51-60 51-60 41-50 41-50 <10 <10 YEARS ON PFOA PFOS TOTAL WATER (DDbVDllD. (nnbl/Dun. PFCslDDbV <10 63.3 73.1 150.11 N/A 59.9 71.0 145.61 >30 58.7 73.4 149.48 <10 58.7 61.7 134.64 20-30 58.3 68.1 154.95 20-30 57.8 70.4 146.46 10-20 48.4 71.9 132.83 10-20 44.6 60.4 115.40 <10 44.1 55.2 114.29 10-20 43.5 54.4 107.12 10-20 42.4 51.1 107.84 20-30 39.8 46.5 104.37 20-30 38.8 47.6 96.33 >30 37.1 51.1 102.01 10-20 33.2 59.5 105.24 <10 32.7 41.5 89.66 10-20 32.1 57.6 103.35 <10 30.7 56.8 99.11 <10 27.5 62.0 98.63 P-6 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 6 SEX AGE YEARS ON PFOA PFOS TOTAL WATER (DDbVDup. (nnbVDup. PFCstnnbV M 51-60 10-20 24.5 37.2 69.72 F 18-30 20-30 23.1 29.2 59.83 F 51-60 20-30 22.2 46.1 74.88 F 31-40 N/A 21.1/19.6 12.8/8.81 29.64/36.80 F <18 10-20 19.1 42.9 71.21 F <18 <10 17.1 20.1 43.08 M 31-40 <10 15.5 12.7 29.31 M 41-50 <10 14.6 30.8 49.49 F 18-30 <10 13.3 12.3 27.14 F 18-30 <10 10.7 23.1 35.87 M >70 20-30 10.2 24.2 35.31 F 18-30 <10 7.35 10.5 19.39 M 51-60 <10 7.21 38.9 57.56 F 61-70 >30 6.96 22.6 36.00 F 18-30 10-20 6.09 17.7 26.79 N/A=data not available *Total of detected levels of PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFBS, PFHxS, PFOS, and PFOSA in the blood sample W0537662.1 P-7 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 7 CHART B - LAKE ELMO AREA PRIVATE WELL USERS SEX AGE YEARS PFOA ON (ppb)/ WATER Dud. PFOS (ppb) /Dud. PPB PPB TOTAL PFOA IN PFOS IN PFCs WATER WATER (ppb)* F <18 <10 110.0 111.0 1.0-1.4 0.5-0.9 247.19 F 41-50 10-20 72.9 87.6 1.0-1.4 0.5-0.9 175.25 F <18 10-20 55.4 60.0 1.0-1.4 0.5-0.9 124.35 M 41-50 20-30 45.7 19.7 ND ND 72.11 F 61-70 20-30 30.9 88.6 0.5-0.9 ND 128.93 M 51-60 10-20 27.0/26.7 28.5/32.7 1.0-1.4 0.5-0.9 62.32/65.74 M 61-70 20-30 24.2 38.0 0.5-0.9 ND 69.91 F 51-60 >30 24.0 17.0 ND ND 50.96 M N/A N/A 16.4 22.1 ND ND 44.43 F 41-50 10-20 15.7 9.27 N/A N/A 27.68 F >70 >30 14.3 8.90 ND ND 26.27 M 61-70 >30 12.1 9.78 ND ND 24.89 M 41-50 10-20 9.66 26.6 ND ND 42.51 F 41-50 <10 9.25 28.4 N/A N/A 41.58 M 18-30 20-30 7.56 17.3 N/A N/A 33.70 M 61-70 20-30 6.95 43.1 N/A N/A 55.00 M 51-60 20-30 6.78 21.0 N/A N/A 36.91 W0537662.1 p .8 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 8 SEX AGE YEARS ON WATER PFOA (p p b )/ D ud. PFOS (p p b) /D u d . PPB PPB PFOA IN PFOS IN WATER WATER TOTAL PFCs (D D b l* M 61-70 >30 6.1 43.7 N/A N/A F 51-60 1 0 -2 0 5.92 29.5 ND ND M 51-60 N/A 5.35 20.4 N/A N/A F 41-50 N/A 3.14 11.2 N/A N/A F 18-30 < 1 0 2.63 17.4 N/A N/A F 61-70 >30 2.4 12.0 N/A N/A N/A=data not available ND= not detected above reported detection limits *Total of detected levels of PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFBS, PFHxS, PFOS, and PFOSA in the blood sample 54.19 41.26 29.02 16.29 26.09 17.91 RAB/mdm Enclosures Lobert A. Bilott W0537662.1 Dr. Charles M. Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 9 cc: Timothy J. Keane, Esq. (w/ encls.)(City of Oakdale Counsel) Jerome P. Filla, Esq. (w/ encls.)(City of Lake Elmo Counsel) Gale D. Pearson, Esq. (w/o ends.) Stephen J. Randall, Esq. (w/o ends.) Rhon E. Jones, Esq. (w/o ends.) J. Mark Englehart, Esq. (w/o ends.) David B. Byrne III, Esq. (w/o ends.) R. Edison Hill, Esq. (w/o ends.) Larry A. Winter, Esq. (w/o ends.) Gerald J. Rapien, Esq. (w/o ends.) P-9 W0537662.1 Exhibit A SB* C> Analytical work by Exygen Research. All results in ug /l (ppb), averages of sample and duplicate NS Not sampled. NO Not detected at or above 0.025 ug/l. *NQ - Not quantifiable s Measured at concentration between 0.025 u g /l & the lim it of Quantitation (LOO) of 0.050 ug/l. Pump capacity values from MOH database. Sum of all wells * 9010 gpm p. 11 3MA00402756 Exhibit B Analytical Results From Oakdale Combined Effluent Discharge (ug/L) Date 8/11/04 9/17/04 PFOA 66.1 53.1 PFOS 30.1 28.2 FOSA ND ND PFBS 4.0 8.8 PFHS 7.6 8.1 Ajialytical Results From Woodbury Pumpout System (ug/L) Result Dupl PFOA 2.2 2.4 PFOS 0.8 0.9 FOSA ND ND PFBS 2.4 2.6 PFHS 7.8 8.1 W /Sfavf 'TfiV'yfal fa in fy iS -y , fa u v fU -C t 7*1/ fa jS ) S fa '*?l)ufaj' if 1 dtv* 7fa\, fiXf 4 fa*yf fa dl'-ft 4 S S li faiY H fa /IjitJ v U.I. f i {/,! 7 vf*kf 3MA00402704 I James Kelly - Re- Fwd Other FCs (in addition to F-8) in Washington Closed Landfill Page 11 From : To: D ate: S ubject: Hi Paul: Virginia Yingling James Kelly; Paul Swedenborg 3/9/2005 12:14:10 PM Re: Fwd: Other FCs (in addition to F-8) in Washington Closed Landfill Jim mentioned that you were looking at C4 and C6 acids in samples to test the standards and methods. If you're looking for others to check, we just brought in about 28 samples and a few more are coming today, tomorrow, and next week. If they haven't already been run, the ones that might be interesting are: * Sam ple No. 208450 W 0020112 82W 01047 82W 01038 413551 Sample Location Larson (collected Monday) Eldredge (collected Monday) Lindblom (collected Tuesday) Conlin (this one is being collected today) Loetscher (this one is being collected today) Thanks. Ginny Ginny Yingling viiginia.yinglingigihealth.state.m n.us ph - 651-215-0917 fa x -651-215-0975 > Jam es Kelly 03/09/05 11:42 AM > FY I....3M will supply some standards, and it looks like the lab has found low levels o f C 4 and C 6 acids in som e O akdale samples. Jim Jam es Kelly, M.S. Health Assessor Site Assessment & Consultation Unit Environmental Health Division Minnesota Oept. of Health (651) 215-0913 iames.kellv@ heaHh.state.mn.us > Paul Swedenborg 03/09/05 11:19 AM > Jim, It would be great if we could receive PFBS and PFHS in the 1 to 5 gram category. Any information on purity and by-products would be useful as well. Have them please ship the chemicals directly to m e. My address should be in the signature below. They are welcom e to contact m e if they have questions. FYI. W e have been screening samples for PFBA, PFPeA, PFHxA, and PFHpA. W e are seeing the C4 and C 6 in some of the Oakdale samples at low levels. Thanks again. Paul. Paul Swedenborg (Organic Unit Supervisor) MN Departm ent of Health Public Health Laboratory Division ' p am es Kelty - RE: Other FCs (in addition to F -8) in Washington CtosedLandfitl From : "Oliaei, Fardin" <Fardin.Oliaei@ state.mn.us> To: "Oliaei, Fardin" <Fardin.Oliaei@ state.mn.us>, "Helen Goeden" <Helen.Goeden@ state.mn.us>, <Fardin.Oliaei@statB.mn.us>. <James.Kelly@ state.mn.us>, <Laura.Solem @ state.m n.us> D ate: S u b je c t: 2/28/2005 2:35:07 PM RE: Other FCs fin addition to F-8) in Washington ClosedLandfill H elen , I am not sure why I can not insert the attached memo. Here, I just copied the entire memo and sending it to you again. Please let me know if you will receive it. If n o t I can just fax it to you. I am not sure what the problem is. Did you get the data in a readable format? Thanks, Fardin To: Paul Hoff From: Fardin Oliaei Date: February 25, 2005 Re: Lower Fluorinated Organic Compounds (3M ) As you know 3M received EPA approval for, and is manufacturing, 18 new fluorochemicals. These new fluorinated compounds are based on the 4 carbon (C -4) perfluorobutane sulfonate (P F 8S ) compound, and serve as substitute* for the 8 carbon chain perfluorinated chemicals associated with PFOS. PFOA. etc. for which 3M terminated production. Although there are significant uncertainties surrounding the behavior of fluorocarbon compounds in general in foe environment in foe areas of partitioning behavior, degradation, chronic toxicity and bioaccumulation, 3M conducted some 40 toxicity and other tests to dem onstrate foe relative non-toxicity of these PFBS-based fluorochem icals PFBS does not significantly bioaccumulate and, based on the testing completed to date, does appear to be relatively non-toxic. However, PFBS and related C -4 fluorochemicals will remain very persistent in foe environment since they are relatively non-biodegradable, and it is anticipated that concentrations of PFBS wifl "accumulate" in blood of humans. Although not bioaccum iiative, the PFBS levels in blood are expected in part due to foe ubiquitous nature of foe PFBS based fluorochemical products and also likely due to a relatively higher volatility versus PFO S. PFOA, etc. There is some information that suggests that foe half life o f shorter perfluorinated compounds is longer than C -8 based compounds in humans. Although a very brief review o f tests completed by 3M appears to demonstrate the relative non-toxicity of PFBS, the long term effects o f these new fluorochemicals are o f course unknown. Because of the heightened sensitivity and awareness of the toxicides associated with PFOS, PFOA, and related higher chain fluorochemical compounds it may be prudent to begin some evaluation of the new C-4 PFBS chemicals, in order to respond in an informed fashion to inquiries. In part this also appears reasonable simply because PFBS is a short chain Pagg i I [Jam sKelty - RE Other FCs (in addition to F-B) In Washington ClosedLandfi haiogenated organic, and numerous other short chain halogenated compounds have known problems. It seem s probable that the public or others may ask about the safety of the new C -4 based fluorochemicals. Therefore, at som e point we may want to consider the following potential evaluations: 1. Conduct a literature review of all studies conducted for PFBS regarding toxicity, degradation, etc, in order to provide informed answers to any questions on this issue that may arise. 2. Evaluate the disposition of PFBS regarding air, water, and solid waste media a t die 3M Cottage Grove p lant Discuss whether monitoring should be required by 3M for PFBS and related C -4 FC compounds in the w ater discharge, sludges generated, and air emissions. 3. Determine whether any additional studies should be required o f 3M regarding aquatic toxicity. Are the present studies adequate concerning potentially affected species in the receiving water. Involve water quality staff in this effort 4. Evaluate the mammalian toxicity studies. Is any health risk assessment needed with respect to drinking water. 5. Since the PFBS and related C -4 compounds are expected to be widely distributed in human blood, are the studies completed adequate to assess long term im parts, if any. 6. Is there adequate information developed to assess the distribution of PFBS to the environment and potential impacts, if any. Is there adequate information regarding breakdown products and potential impacts, if any. (As a separate note w e found PFBS at high concentrations in the pumpout w ater and standing w ater at the Washington County Landfill.} These evaluations would primarily be conducted to assure feat we may answ er questions related to PFBS in the Minnesota environm ent and do not necessarily presume a problem with PFBS. However, I believe it would be appropriate to be prepared to assure that studies to date are adequate for environmental protection, and so that we may respond to any inquiries in an informed fashion. ----- Original Message-----From: Ofiaei, Fardin S e n t Monday, February 28. 2005 2:28 PM To: 'Helen Goeden'; 'Fardin.Oliaei@ state.m n.us'; 'James.Kelly@ state.mn.us1; laura.Sotem @ state.m n.us* Cc: 'Larry Gust*; 'Rita Messing*; 'Cari.Herbrandson@ state.mn.us'; 'Douglas.Day@ state.mn.us'; 'HiBary.Carpenter@state.mn.us'; 'Ingrid.Verhagen@ state.mn.us'; 'JosephJulikQstate.m n.us'; 'Paul.Swedenboig@ state.mn.us' S ubject RE: Other FCs (in addition to F -8) in Washington CtosedLandfiU Hi Helen, I am sorry for not attaching the memo. H ere is a copy of Ihe memo. Please feel free to revise and complement this memo as you see it best lit with your position at the M DH on this issues. Thanks for your time. _______ _____________________________ ___________ ___________ _______________________________ p. 17 I Janrfes Kelly - RE: Other FCs (In addition to F-8) in Washington CtosedLandfitl ........... Page 3 j Fardin ----- Original Message-----From: Helen Goeden [mailto:Helen.Goeden@ state.mn.us] Sent: Monday, February 2 8 .2 0 0 5 2:09 PM To: Fardin.Oliaei@ state.m n.us; Helen Goeden@ state.mn.us; James.Kelfy@ state.mn.us, Laura.Solem@ state.mn us Cc: Larry Gust; Rita Messing; C arl Herbrandson@state.mn.us; Dougtes.Oay@ state.m aus; Hillary.Carpenter@ state.mn.us; Ingrid.Verhagen@ state.m n.us; Joseph.Julik@ state.mn.us; Paul.Swedenborg@ state.mn.us Subject RE: Other FCs (in addition to F-8) in Washington ClosedLandfai Fardin, Jim and I will be coordinating a response from our units to your questions. The copy o f your m em o to Paul Hoff was not attached to the e-m ail. Could you forward a copy of the memo to us? Thanks. H elen Helen Goeden, Ph.D. Minnesota Department o f Health P.O . Box 64975 SL Paul, MN 55164-0975 (651)215-0874 heien.goeden@ health.state.m n.us > "Oliaei, Fardin" <Fardin.OIteei@ state.mn.us> 02/28/05 1:04 PM > > D ear Helen, Laura, and Jim, > > Now that I submitted a copy o f the foilowing preliminary data for 3M > to review, I should also share them with you for your review. The > following data are on the levels o f FCs in the Washington County's > contaminated well (V 2), d ean , reference well (J), and two surface > w ater samples (created with the V2 being sprayed over the surface area > o f the closed landfill). > > I am concern. Specially, with the high concentrations of C -4 > compounds. Let m e know what you think. Based on the ongoing EPA > SAB panel discussion on cancer dassification for PFOA, are w e going > to revise toe M DH H R V values for PFOS/PFO S? Is there suffiderrt data > to develop toxidty values for C -4, C -5. and C -6 Fluorinated > compounds? > > I also attached a copy of a memo that I put together for my > supervisor. Paul Hoff per his request on this issue. In my view, this > mem o needs to be expanded, suggesting a comprehensive environmental > monitoring (conducted by M PCA), and bio monitoring (conducted by MDH) > for a period o f five year (financially supported by 3M). (7 j James Kelly - RE: Other FCs (in addition to F-8) in Washington ClosedLandfiH > File: Paul-PFBS.doc > The following are the preliminary data on contaminated well (V 2), > d ean and reference well (J), and two samples of the surface water > (where the V 2 is being sprayed over the dosed landfill). I need to > explain more about these data. > > C LIEN T ID W ash-C L (surface water#1) W ash-CL (surface water#2) > W ash-CL (dean W ell J) Wash-CL(polluted W ell V 2) > > U N ITS > ng/mL ng/m L ng/mL ng/mL > PFBA > < 0.1 10 371 1170 (F-4) 352 > (this high cone. Is my concern, and it is a substitute for F-8!) PFPeA > <0.0205 > PFHxA > <0.0037 > PFHpA > <0.0044 > PFOA > <0.0027 > PFNA > 0 .0 01 > PFDA > <0.0015 > PFUnA > 0 .0 0 0 9 > PFDoA > 0 .0 0 2 > PFTA > 0 .0 0 0 5 > PFBS > 0 .0 2 0 1 7 .9 8 43.1 (F-5) 3.36 15.6 (F-6) 0 .5 8 2 2.38 (F-7) 10.9 41.6 (F-8) 0 .0 0 9 0 .0 1 2 <0.0156 0 .0 0 6 <0.0068 <0.0039 <0.0142 <0.0032 <0.0202 <0.0020 <0.333 1.31 6 .8 9 3.28 0.659 15.2 0.006 0.027 0.016 0.016 <0.0103 <0.252 PFHxS > 0 .0 2 5 7 > PFOS > <0.0030 <0.422 1.77 (F-6) 1.35 2 .6 9 (F -8 ) > (only PFOA and PFO S are being reported by M DH) > > Thanks for your time, Fardin > > Fardin O iaei, Ph.D. > Research Scientist III > Emerging Contaminants Coordinator > Minnesota Pollution Control Agency (M PCA) > > E-m ail. fardin.o)iaei@ pca.state.m n.us > Phone: (651 ) 296-7967 <0.300 1.67 . r* Page4j |tomes Kefly - RE: Other FC s (in addition lo F-8) tei Washington GtosedLandfg p. 19________ Page5| > > File: Paul-PFBS.doc CC: "Larry Gust' <Lany.Gust@ state.mn.us>, "Rita Messing* <Rita.Messing@state.mn.u$>, <Car1.Herbrandson@ state.mn.us>, <Douglas.Day@ state.mn.us>, <Hinary.Carpenter@state.mn.us>, <lngrid.Verhagen@ state.m n.us>, <Joseph.Jufik@ state.mn.us>. <PauLSwedenborg@state mn.us> Groundwater Monitoring Network around Washington County Landfill p. 20 IRWtN 37TH 3TTH 4t / 7 m ht iu & -G -llfi amiwatch P *l(4f Monitoring Weils -------- streets Landfill outlined in red O /t'f 900 DMeters C? CLIENT ID Axy ID WORKGROUP Simple Size UNITS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS With -Cl-witenU L7419-1R WG14680 9.09 mL ng/mL 371 7.98 3.36 0.982 10.9 0.009 <0.0196 <0.0066 <0.0142 <0.0202 <0.333 <0.422 1.39 WutvCL-witer #2 L7419-2R WG14660 6.12 ml ng/mL 392 6.89 3.28 0.659 19.2 0.006 0.027 0.016 0.016 <0.0103 <0.292 <0.300 1.67 WuhingtonCo. Wet J L7419-3 WG14980 90.2 mL ng/mL <0.110 <0.0209 <0.0037 <0.0044 <0.0027 0.001 <0.0019 <0.0009 0.002 <0.0006 <0.0201 <0.0257 <0.0030 Washington Co. WashingtonCo. Well WelV2 LABBUNK LABBLANK SPIKEDMATRIX V2 (DUPLICATE) L7419-4 WG14580-101 WG14560-101 WG14580-102 WG14680-103 WG14580 49.3 mL WQ14580 WG14680 50.0mL 6.00mL WG14680 WG14560 4.97 mL ng/mL ng/mL ng/mL %REC ng/mL 1170 <0.166 <1.68 122 1260 43.1 <0.0216 <0.216 128 26.6 15.6 <0.0042 <0.0418 111 10.6 2.36 <0.0017 <0.0169 101 1.96 41.6 <0.0027 <0.0271 109 36.6 0.012 <0.0016 <0.0175 103 0.014 0.006 0.003 0.026 114 <0.0145 <0.0038 0.003 0.031 104 0.019 <0.0032 0.006 0.063 106 0.017 <0.0020 <0.0006 <0.0069 107 <0.0052 1.31 <0.0031 <0.0307 97 0.548 1.77 <0.0069 <0.0390 <1.46 2.69 <0.0030 <0.0303 106 2.61 Washington Co, Well (DUPLICATE) WG14680-104 WG14580 50.2 mL ng/mL <0.134 <0.0301 <0.0041 <0.0041 <0.0024 0.003 <0.0024 0.003 0.002 <0.0007 <0.0167 <0.0204 <0.0049 Exhibit C INTERROGATORY NO. 3: Identify each human drinking water supply in Minnesota or Wisconsin where any PFCs have ever been detected, specifying the dates of each such detection for each such water supply, the level and/or concentration of each PFC detected, and the identity of the entity(s) who conducted and/or arranged for the sampling and analysis. ANSWER: Subject to and without waiving its general objections and the objections to this interrogatory stated below, 3M states as follows: The following water supplies have been tested and showed no detectable PFOA or PFOS: the City of Cottage Grove, the City of Hastings, 13 3 p. 24 V__ / the City of Woodbury, the City of Lake Elmo, the City of North St. Paul, Whispering Oaks mobile home park water supply, Cimarron Park public water supply wells in Lake Elmo, private wells near the eastern side of the Cottage Grove facility, private wells in Woodbury , and many private wells in Lake Elmo. 3M is aware of PFOA or PFOS being detected in the following water supplies: City of Oakdale water wells and Oakdale City tap water in two buildings in Oakdale, one private well in Oakdale, and certain Lake Elmo private wells. 3M's Cottage Grove plant also has had detectable levels in drinking water. 3M notes, however, that the mere detection of these compounds at part per billion or part per trillion levels does not indicate a potential for adverse health effects. Even detections above the MDH Health Based Values, which comprise a small subset of the findings, do not mean there are adverse health effects in humans. The MDH Health Based Values of 1 ppb for PFOS and 7 ppb for PFOA incorporate substantial safety factors compared to the levels of exposure that cause effects in a laboratory study of monkeys. The Health Based Value for PFOS 24 includes a safety factor of 1,000 and the Health Based Value for PFOA includes a safety factor of 3,000. Moreover, these values are intended to be protective for lifetime exposure. Much of the drinking water data has been collected by the Minnesota Department of Health (MDH). In addition to documents 3M will produce in connection with this interrogatory response, 3M refers Plaintiffs to data available from MDH or the relevant local governmental entities. . Oakdale 3M and the State have been analyzing split samples taken from Oakdale municipal wells since December 2004. The Minnesota Department of Health conducted all of the State's analyses of these samples. Exygen Research conducted 3M's analyses of these samples through May 2005. From June 2005 forward, 3M's in-house environmental laboratory analyzed 3M's split samples. The following tables summarize the results of 3M's and the State's sampling. 45 Municipal Wells Oakdale December 22, 2005 Sampling Results (ug/L) Well Number 1 2 3 5 7 8 Exygen Result NA NA NA 0.747 0.258 0.539 Exygen Duplicate NA NA NA 0.718 0.268 0.452 PFOA Exygen Average MDH Measured Value NA NA NA 0.733 0.263 0.496 ND ND ND 0.7067 0.2458 0.4248 MDH Measured Value Duplicate NA NA NA 0.7402 NA NA MDH Average NC NC NC 0.7235 NC NC NC 9 0.727 0.772 0.750 0.7781 NA Well Number PFOS Exygen Exygen Exygen MJJri MDH Measured MDH Result Duplicate Average Value Average Duplicate 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 1.13 1.10 1.12 1.0884 1.2332 1.1608 7 0.259 0.267 0.263 0.1918 NA NC 8 0.794 0.692 0.743 0.7335 NA NC 9 0.63 0.666 0.648 0.5087 NA NC All results in ug/L (parts per billion or ppb). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L and the Limit of Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. 26 Oakdale January 25, 2005 Sampling Results (ug/L) PFOA Well Number Exygen Result Exygen Duplicate Exygen Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 0.0746 0.0790 0.0768 ND NA NC 2 0.0773 0.0750 0.0762 ND NA NC 3 ND ND ND ND NA NC 5 0.821 0.736 0.779 0.799 NA NC 7 0.285 0.274 0.280 0.211 0.235 0.223 8 0.668 0.647 0.658 0.628 NA NC 9 Well Number 0.825 Exygen Result 0.892 Exygen Duplicate 0.859 0.737 PFOS Exygen Average MDH Measured Value NA MDH Measured Value Duplicate NC MDH Average 1 NQ 0.0514 NC ND NA NC 2 NQ ND NC ND NA NC 3 ND ND ND ND NA NC 5 1.12 1.01 1.07 1.125 NA NC 7 0.276 0.269 0.273 0.187 0.117 0.152 8 1.02 0.977 0.999 0.936 NA NC 9 0.583 0.653 0.618 0.613 NA NC All results in ug/L (parts per billion). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit of Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. Oakdale February 28,2005 Sampling Results (ug/L) PFOA Well Number 1 2 3 5 7 8 9 Oakdale Exygen Result 0.0892 0.0807 ND 0.714 0.274 0.523 NS Exygen Exygen Duplicate Average 0.0852 0.0871 ND 0.761 0.305 0.503 NS 0.0872 0.0839 ND 0.738 0.290 0.513 NS MDH Measured Value ND ND ND 0.693 0.214 0.423 NS MDH Measured Value Duplicate NA NA NA 0.727 NA NA NS MDH Average NC NC NC 0.710 NC NC NC Public Works Bldg. Lunch 0.687 0.709 0.698 0.624 NA NC Room Sink Well Number PFOS 1 2 3 5 7 8 9 Oakdale Exygen Result 0.0516 NQ ND 0.889 0.238 0.687 NS Exygen Duplicate 0.0541 NQ ND 0.968 0.273 0.662 NS Exygen Average 0.0529 NQ ND 0.929 0.256 0.675 NS MDH Measured Value ND ND ND 1.054 0.242 0.693 NS MDH Measured Value Duplicate NA NA NA 1.004 NA NA NS MDH Average NC NC NC 1.029 NC NC NS Public Works Bldg. Lunch 0.872 0.949 0.911 0.947 NA NC Room Sink All results in ug/L (parts per billion). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit of Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. as Oakdale March 29, 2005 Sampling Results (ug/L) PFOA Well Number 1 2 3 5 7 8 9 Well Number Exygen Result 0.0887 0.0823 ND 0.779 NS 0.503 0.813 Exygen Duplicate 0.0939 0.0817 ND 0.710 NS 0.457 0.763 Exygen Average MDH Measured Value 0.0913 ND 0.0820 ND ND ND 0.745 0.5281 NS NS 0.480 ND 0.788 0.8650 PFOS MDH Measured Value Duplicate NA NA NA NA NS NA 0.7575 MDH Average NC NC NC NC NS NC 0.8113 Exygen Exygen Result Duplicate 1 0.0619 0.0609 2 NQ NQ 3 ND ND 5 1.14 0.941 7 NS NS 8 0.704 0.551 9 0.58 0.502 All results in ug/L (parts per billion or ppb). NS - Not sampled. ND - Not detected. Exygen Average 0.0614 NC ND 1.04 NS 0.628 0.541 MDH Measured Value ND ND ND 0.9007 NS 0.8500 0.7147 MDH Measured Value Duplicate NA NA NA NA NS NA 0.5727 MDH Average NC NC NC NC NS NC 0.6437 NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit of Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. Oakdale April 2005 Sampling Results (ug/L) PFOA Well Number 1 2 3 5 7 8 9 Well Number Exygen Result ND ND ND 0.528 NS ND 0.865 Exygen Duplicate NS NS NS NS NS NS 0.758 Exygen Average MDH Measured Value NC NC NC NC NC NC 0.812 * * * * * * * PFOS MDH Measured Value Duplicate * * * * * * * MDH Average * * * * * * * Exygen Result Exygen Duplicate Exygen Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 ND NS NC * ** 2 ND NS NC * ** 3 ND NS NC * ** 5 0.901 NS NC * ** 7 NS NS NC * ** 8 0.850 NS NC * ** 9 0.715 0.573 0.644 * ** *3M does not have any MDH sampling data from April, and believes MDH did not sample in April. All results in ug/L (parts per billion or ppb). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit of Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. Oakdale May 18,2005 Sampling Results (ug/L) P FOA Well Number 1 2 3 5 7 8 9 Well Number Exygen Result NA NA NA NA NA NA NA Exygen Duplicate NA NA NA NA NA NA NA Exygen Average MDH Measured Value MDH Measured Value Duplicate NA ND NA NA ND NA NA ND NA NA NS NS NA 0.3184 NA NA 0.5594 ' 0.5195 NA 0.7740 NA PFOS MDH Average NC NC NC NS NC 0.5395 NC Exygen Exygen Result Duplicate 1 NA NA 2 NA NA 3 NA NA 5 NA NA 7 NA NA 8 NA NA .......... 9 NA NA All results in ug/L (parts per billion or ppb). NS - Not sampled. Exygen Average NA NA NA NA NA NA NA MDH Measured Value ND ND ND NS ND 0.7409 0.6539 MDH Measured Value Duplicate NA NA NA NS NA 0.6620 NA MDH Average NC NC NC NS NC 0.7015 NC ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L (25 parts per trillion). NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit o f Quantitation (LOQ) o f 0.050 ug/L (50 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. _ 3' Oakdale June 16, 2005 Sampling Results (ug/L) PFOA Well Number 3M Env Lab Result 3M Env Lab Duplicate 3M Env Lab Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 2 3 5 7 8 9 Well Number NA NA NA 0.887 NA 0.472 * NA NA NA 0.948 NA 0.506 * NA ND NA ND NA ND 0.918 0.9195 NA 0.3057 0.489 0.5390 0.923 0.8605 PFOS NA NA NA NA NA NA 0.9686 ' NC NC NC NC NC NC 0.9146 3M bnv LTaoUk Result 3M Env Lab Duplicate 3M Env Lab Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 1.16 1.20 1.18 1.1482 NA NC 7 NA NA NA 0.1937 NA NC 8 0.698 0.709 0.704 0.5303 NA NC 9 0.872 0.945 0.909 0.6474 0.5513 0.5994 All results in ue>/T. narts npr hil NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: Lower limit o f quantitation (LOQ) for PFOA for two extraction sets were 0.00492 ug/L (4.92 parts per trillion) and 0.00738 ug/L (7.38 parts per trillion). Lower limit o f quantitation (LOQ) for PFOS for two extraction sets were 0.00496 ug/L (4 96 parts per trillion) and 0.00992 ug/L (9.92 parts per trillion) For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. * Sample and duplicate were run for two separate extractions with the following four results- 0 967 0 938 0.881,0.906 ug/L. '' ' ' i2 Oakdale July 13, 2005 Sampling Results (ug/L) PIFOA Well Number 3M Env Lab Result 3M Env Lab Duplicate 3M Env Lab Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 0.747 0.718 0.733 0.7067 0.7402 0.7235 7 0.258 0.268 0.263 0.2458 NA NC 8 0.539 0.452 0.496 0.4248 NA NC 9 0.727 0.772 0.750 0.7781 NA NC Well Number P] ?OS 3M Env Lab Result 3M Env Lab Duplicate 3M Env Lab Average MDH Measured Value MDH Measured Value Duplicate MDH Average 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 1.13 1.10 1.12 1.0884 1.2332 1.1608 7 0.259 0.267 0.263 0.1918 NA NC 8 0.794 0.692 0.743 0.7335 NA NC 9 0.63 0.666 0.648 0.5087 NA NC All results in ug/L (parts per billion or ppb). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: Lower limit of quantitation (LOQ) for PFOA for two extraction sets were 0.00492 ug/L (4.92 parts per trillion) and 0.00738 ug/L (7.38 parts per trillion). Lower limit o f quantitation (LOQ) for PFOS for two extraction sets were 0.00496 ug/L (4.96 parts per trillion) and 0.00992 ug/L (9.92 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. Oakdale August 12,2005 Sampling Results (ug/L) PFOA 3M Well Number Pnv 3M Env 3M Env MDH MDH t nU Lab Lab Measured Mf asured MDH 1 2 3 5 7 8 9 Well Number Result * * * * * * * DuPllcate * * * * * * * Average Value * * * * * * * ND ND ND 0.9350 0.5344 0.6903 ND PI^OS ^ Value Duplicate NA NA NA NA 0.4720 NA NA AveraSe NC NC NC NC 0.5032 NC NC 3M P 3M Env 3M Env MDH MDH Lab Result Lab DuPlicate Lab Average Measured Value Mf af red TM Ue Duplicate MDH Average 1 * * * ND NA NC 2 * * * ND NA NC 3 * * * ND NA NC 5 * * * 1.1630 NA NC 7 8 * * * * * * 0.6302 0.6903 0.6471 0.6387 NA NC 9 * * * ND NA NC All results in ug/L (parts per billion or ppb). * - 3M results not yet available. NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: Lower limit o f quantitation (LOQ) for PFOA for two extraction sets were 0.00492 ug/L (4.92 parts per trillion) and 0.00738 ug/L (7.38 parts per trillion). Lower limit o f quantitation (LOQ) for PFOS for two extraction sets were 0.00496 ug/L (4.96 parts per trillion) and 0.00992 ug/L (9.92 parts per trillion). For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. MDH has also tested a public water supply at Whispering Oaks mobile home park sampled on January 25, 2005, and found no detectable levels of PFOS or PFOA. 3M sampled water at the office building occupied by its subsidiary Dyneon in Oakdale on January 4, 2005, with the following results: Dyneon Oakdale Building Samples (ug/L or parts per billion) E05-0007-77781 Reception area rest room E05-0007-77782 Reception area rest room Dup E05-0007-77785 Ctr office rest m fin E05-0007-77786 Ctr office rest rm fin Dup E05-0007-77789 Break room sink E05-0007-77790 Break room sink Dup E05-0007-77793 Utility room janitor sink E05-0007-77794 Utility room janitor sink Dup PFO A (ug/L) 0.75 0.66 0.18 0.19 0.14 0.14 0.67 0.71 P F O S (ug/L) 0.86 0.86 0.14 0.16 0.18 0.15 0.84 0.88 MDH collected samples from the Oakdale Public Works Building on February 28, 2005. February 28,2005 Sampling Results (ug/L or parts per billion) PFOA Location Oakdale Public Works Bldg. Lunch Room Sink Exygen Result 0.687 Exygen Duplicate 0.709 Exygen Average 0.698 MDH Measured Value 0.624 MDH Measured Value Duplicate NA MDH Average NC PFOS Oakdale Public Works Bldg. Lunch Room Sink 0.872 0.949 0.911 0.947 NA NC All results in ug/L (ppb). NS - Not sampled. ND - Not detected. NC - Not calculated. NA - Not analyzed. For Exygen data: ND - Not detected at or above 0.025 ug/L. NQ - Not quantifiable = Measured at concentration between 0.025 ug/L & the Limit o f Quantitation (LOQ) o f 0.050 ug/L. For MDH data: Report level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. Where data is reported at less than these values, it represents Measured Values. Private Wells in Oakdale In March 2005, MDH analyzed samples collected from several private wells located in or around Oakdale: Oakdale Private Wells OAKDALE W82W0020113 unk W 82W 0020112 unk unk 174298 unk Street No. Street Name 3465 3445 3315 3307 3301 7641 1 00 -ao Geneva Ave. N Geneva Ave. N Geneva Ave. N Geneva Ave. N Geneva Ave. N 7287 Stillwater Blvd. N Sample Date 3/7/2005 3/7/2005 3/7/2005 3/7/2005 3/8/2005 3/7/2005 3/7/2005 PFOS PFOA ND ND ND ND ND ND ND ND ND ND ND ND 0.662 ug/L ND orppb Lake Elmo Public Water Supplies MDH tested municipal drinking water from well number 1 in the City of Lake Elmo municipal water supply, sampled January 26, 2005, and found no detectable PFOS or PFOA. MDH testing of wells #1 and 2 of the public water supply in Cimarron Park in Lake Elmo sampled on January 26, 2005 showed no detectable levels of PFOS or PFOA. Private Wells Between April 2005 and July 2005, MDH collected and analyzed water samples from private wells located in Lake Elmo. MDH has provided 3M with the following data: Lake Elmo Private Wells (ug/L or parts per billion) LAKE ELMO 82W01045 404104 Street No. Street Name 4111 4077 Isle Ave. N Isle Ave. N 82W01033 ! 8830 42nd St. N 82W01022 82W01018 82W01014 82W01026 493185 82W01015 82W01016 439126 539248 3490 3508 3509 3533 3551 3567 3597 3681 3691 Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. Kelvin Ave. N. 82W01044 134754 3322 3240 Ideal Ave. N Ideal Ave. N 710053 670792 710051 82W01034 82W01035 89318945 89718975 89818985 8611 8633 34th St. N. 34th St. N. 34th St. N. 413596 82W01021 82W01017 10120 10174 10212 Stillwater Lane Stillwater Lane Stillwater Lane Sample Date 4/13/2005 4/13/2005 3/7/2005 6/21/2004 6/21/2004 6/21/2004 6/21/2004 6/21/2004 6/21/2004 6/21/2004 6/21/2004 6/21/2004 3/8/2005 3/8/2005 PFOS PFOA ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 4/13/2005; VOCs ND ND 3/8/2005 3/8/2005 6/21/2004 6/21/2004 6/21/2004 ND ND ND ND ND ND ND ND ' ND ND 670770 82W01003 9018 9038 31st St. N. 31st St. N. 82W01004 9046 31st St. N. 82W01047 82W01029 604274 9051 9066 9077 31st St. N. 31st St. N. 31st St. N. 6/22/2004 6/22/2004 7/20/2004 4/27/2005 6/22/2004 7/20/2004 4/27/2005 4/13/2005 7/20/2004 4/27/2005 7/20/2004 4/27/2005 ND ND ND ND ND ND ND ND ND ND ND 1 ND ND 0.5 0.4 0.5 0.4 0.2 0.6 ND 0.3 0.3 0.6 p. 38 O 82W01019 82W01005 82 WO1024 82W01006 82W01007 82W01008 82W01028 82W01023 616698 82W01009 82W01020 82W01200 82W01133 82W01134 82W01135 208450 536672 413551 82W01048 82W01050 604259 82W01136 82W01137 82W01138 82W01122 82W01139 82W01140 82W01141 493576 82W01142 451602 82W01124 82WO1123 110523 82W01037 82W01064 82W01038 82W01063 583343 9078 31st St. N. 9095 9098 9141 9148 9181 9198 9202 9260 9343 9345 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 31st St. N. 3030 3010 2990 2950 Janero Ave. N. Janero Ave. N. Janero Ave. N. Janero Ave. N. 3052 3014 3053 3023 2991 2994 2970 2940 2935 2959 2909 2904 2877 2850 2809 2805 2798 2751 Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. Jamley Ave. N. 2819 Ivy Ave N. 8866 8863 8740 8707 8680 Stillwater Blvd Stillwater Blvd. Stillwater Blvd Stillwater Blvd. Stillwater Blvd 6/22/2004 7/20/2004 4/27/2005 6/22/2004 6/22/2004 6/22/2004 6/22/2004 6/22/2004 7/20/2004 6/21/2004 7/20/2004 4/27/2005 6/21/2004 6/21/2004 4/27/2005 ND 0.4 ND 0.2 ND 0.5 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 0.1 ND 0.3 ND ND ND 0.9 ND 1 6/13/2005 6/13/2005 6/13/2005 6/13/2005 ND ND ND 0.2 ND 0.2 ND ND 3/7/2005 3/17/2005 3/9/2005 4/13/2005 4/13/2005 4/13/2005 6/13/2005 6/13/2005 6/13/2005 5/16/2005 6/13/2005 6/13/2005 6/13/2005 ND ND ND 0.647 ND ND ND ND ND ND ND ND ND 0.4 ND 0.3 ND ND ND 0.7 ND ND ND 0.3 ND ND 6/13/2005 6/13/2005 5/16/2005 5/16/2005 ND 0.2 ND ND ND ND ND ND 4/18/2005 ND ND 3/8/2005 4/18/2005 3/9/2005 4/13/2005; VOCs 3/7/2005 7/22/2005 - GAC ND ND ND 0.178 2.2 ND ND ND ND ND 1.5 ND 38 82W01062 676479 82W01061 558222 82W01060 82W01059 82W01058 82W01057 82W01056 82W01055 82W01054 82W01053 599973 82W01039 154476 634270 82 WO 1132 82W01025 82W01010 539268 151756 569744 687850 613401 622211 82W01065 154443 156421 121060 440560 437308 428479 82W01067 82W01068 82W01069 82W01130 82W01131 8659 8643 8627 8620 Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd 8583 8567 8511 8488 8464 8428 8404 8384 8364 8308 Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd 8282 Stillwater Blvd 8268 8255 9517 9521 9524 10240 Stillwater Blvd Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. Stillwater Blvd. 3082 Inwood Ave. N 3077 Inwood Ave. N 3036 Inwood Ave. N 3033 Inwood Ave. N 2961 2915 2895 2875 2856 Inwood Ave. N. Inwood Ave. N. Inwood Ave. N. Inwood Ave. N. Inwood Ave. N. 2816 2796 2793 2773 Inwood Ave. N Inwood Ave. N Inwood Ave. N. Inwood Ave. N. 2731 2298 2038 Inwood Ave. N. Inwood Ave. N. Inwood Ave. N. 4/18/2005 4/15/2005 3/7/2005 6/21/2005-GAC 4/15/2005 4/13/2005; VOCs 4/13/2005 4/15/2005 4/15/2005 4/13/2005; VOCs 4/13/2005 4/13/2005; VOCs 4/13/2005 3/7/2005 6/13/2005 - GAC 3/7/2005 6/13/2005 - GAC 3/7/2005 4/18/2005 6/21/2004 6/21/2004 6/21/2004 6/21/2004 1.876 0.233 0.3 1.4 ND ND 0.155 ND ND ND ND ND ND 0.398 1.4 ND 1.2 ND ND ND ND ND ND ND 1.72 0.423 0.5 1.7 ND ND ND ND ND 0.793 ND ND ND ND 1 ND 0.6 ND 0.48 ND ND ND ND ND 3/7/2005 7/22/2005 - GAC 3/10/2005 6/13/2005-GAC 3/7/2005 7/13/2005 -GAC 3/10/2005 6/24/2005 - GAC 4/13/2005 4/13/2005 4/18/2005 4/13/2005 4/15/2005 7/13/2005 3/7/2005 3/8/2005 4/15/2005 4/15/2005 7/13/2005 4/14/2005 5/18/2005 5/23/2005 3.3 ND 1.4 ND 1.4 ND 1.4 ND ND ND ND ND 0.694 1 0.285 ND ND 0.629 0.7 ND ND ND 3 ND 1.3 ND 1 ND 1.8 ND ND ND ND ND 0.868 0.8 0.426 ND ND 1.006 0.7 ND ND ND p p. 40 82W01073 471065 428478 82W01070 440566 82W01072 82W01071 453245 519084 82WO1129 82W01074 82W01075 82W01076 82W01077 82W01078 82W01079 82W01080 82W01081 82W01082 82W01083 424136 82W01084 82W01085 82W01086 82W01087 82W01088 82W01089 82W01090 110434 82W01091 82W01092 82 WO1093 82W01094 82W01095 82W01096 82W01097 671999 82W01099 2965 2960 Innsdale Ave. N. Innsdale Ave. N. 2935 2930 2906 2895 2876 2655 2626 2621 Innsdale Ave N Innsdale Ave. N. Innsdale Ave N Innsdale Ave. N. Innsdale Ave. N. Innsdale Ave. N. Innsdale Ave. N. Innsdale Ave. N. 8520 Ironwood Trl. N. 8521 8540 Ironwood Trl. N. Ironwood Trl. N. 8549 Ironwood Trl. N. 8580 Ironwood Trl. N. 8592 8603 8618 8628 8633 8650 8652 8657 8674 8690 8695 8702 8716 8722 8725 8748 8772 8775 8780 8785 Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. Ironwood Trl. N. 2811 2770 2759 Irish Ave. N. Irish Ave. N. Irish Ave. N. 4/18/2005 4/13/2005 6/22/2005 - GAC 3/7/2005 4/13/2005 3/9/2005 4/18/2005 4/13/2005 5/16/2005 5/16/2005 5/16/2005 0.177 0.804 ND ND ND ND ND ND ND ND ND ND 1.245 ND ND ND ND ND ND ND ND ND 4/15/2005 7/13/2005 4/15/2005 4/15/2005 7/13/2005 4/15/2005 7/13/2005 4/18/2005 7/13/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 3/8/2005 4/15/2005 4/14/2005 4/14/2005 4/15/2005 (inside) 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/14/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 0.791 0.8 ND 0.692 0.9 0.676 0.6 0.644 0.9 ND ND ND 0.408 ND 0.296 ND ND ND 0.833 1.7 0.791 1.095 0.7 1.004 0.4 0.93 0.7 ND ND ND 0.746 ND 0.302 ND ND ND ND 0.545 0.402 0.286 0.513 ND ND 0.482 ND ND ND ND 0.86 0.693 0.668 0.858 ND ND 0.713 ND ND ND 4/15/2005 4/15/2005 4/15/2005 7/13/2005 ND ND 0.143 0.2 ND ND ND 0.3 p. 41 585145 575148 588139 576160 614269 609537 598819 617699 678196 606937 607488 569982 554316 569782 569978 82W01100 82W01101 82WO1102 82W01103 446288 82W01125 82 WO1126 82W01127 82W01128 511739 457680 465954 440589 196939 442140 82W01104 440577 503288 453250 670740 700594 670739 679966 82 WO 1106 82W01107 82W01108 2895 2890 2850 2841 2769 2760 2811 2696 2699 2677 2678 2655 2656 2618 2580 Imperial Ave. N Imperial Ave. N. Imperial Ave. N. Imperial Ave. N Imperial Ave. N. Imperial Ave. N. Imperial Ave. N. Imperial Ave, N. Imperial Ave. N. Imperial Ave. N. Imperial Ave. N. Imperial Ave. N. Imperial Ave. N. Imperial Ave. N Imperial Ave. N. 3/8/2005 4/13/2005 4/13/2005 3/8/2005 4/13/2005 4/13/2005 4/13/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 3/8/2005 5/16/2005 0.257 ND ND 0.351 ND ND 0.264 ND 0.2 ND ND ND ND ND ND 0.323 ND ND ND ND ND ND ND ND ND ND ND ND ND ND 8623 8643 8648 8687 9043 9049 9065 9079 9155 28th St. N. 28th St. N. 28th St. N. 28th St. N. 28th St. N. 28th St. N. 28th St. N. 28th St. N. 28th St. N. 4/15/2005 5/16/2005 4/14/2005 4/15/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 ND ND 0.2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 8244 8247 8282 8301 8310 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 8341 8352 8375 8478 8483 8555 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 8570 8605 27th St. N. 27th St. N. 8623 8639 8644 8650 27th St. N. 27th St. N. 27th St. N. 27th St. N. 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 7/13/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 4/15/2005 7/13/2005 -GAC 4/14/2005 4/14/2005 6/23/2005 4/15/2005 4/14/2005 4/14/2005 4/14/2005 7/13/2005 ND ND ND ND 0.733 0.3 ND ND ND ND ND 0.857 ND ND 0.899 ND ND ND 0.416 0.813 0.9 ND ND ND ND 0.863 0.2 ND ND ND ND ND 1.232 ND ND 1.052 ND ND ND 0.686 0.884 0.7 41 p. 42 82 WO 1109 82W01110 82W01111 82W01112 82W01113 415659 176046 194159 176036 174267 82W01114 82W01115 173927 176020 82W01117 176049 182679 173925 185945 162931 187000 173938 182731 577036 616945 554311 598818 590036 577037 588140 569984 582669 587849 590079 656705 597121 641705 641458 633298 637433 8655 8656 8685 8709 8715 8735 8755 8785 8815 8845 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 27th St. N. 8875 8905 8925 27th St. N. 27th St. N. 27th St. N. 8770 8780 8790 8800 8810 8820 8830 27th St. Ct. N. 27th St. Ct. N. 27th St. Ct. N. 27th St. Ct. N. 27th St. Ct. N. 27th St. Ct. N. 27th St. Ct. N. 8840 8850 27th St. Ct. N. 27th St. Ct. N. 8860 27th St. Ct. N. 8119 8154 8165 8215 8281 8284 8364 8367 8454 8457 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 26th St. N. 8042 8125 8382 8414 22nd St. Ct. N. 22nd St. N. 22nd St. N 22nd St. N 1873 1849 1827 Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. 4/22/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 7/13/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/14/2005 4/15/2005 7/13/2005 4/14/2005 4/18/2005 7/13/2005 4/14/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/23/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 3/7/2005 3/8/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 5/16/2005 0.214 ND ND ND 0.356 ND ND ND 0.386 0.709 0.7 0.414 0.488 0.454 ND ND ND ND 0.675 ND ND ND ND 0.708 0.4 0.582 ND ND ND ND ND 0.301 ND 0.357 0.727 1.2 0.608 0.711 0.5 0.65 ND ND ND ND ND ND 0.697 0.5 ND 0.887 0.6 ND ND ND ND ND ND ND ND ND ND ND ND ND 0.2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 42 633269 633266 628276 622311 623865 633264 645610 628279 633276 637406 615494 658982 82W01147 672580 658960 1805 1779 1757 1743 1709 1694 1697 1680 1681 1668 1663 Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. Ivory Ave. N. 1696 1683 1665 1634 Ivy Ave. N. Ivy Ave. N. Ivy Ave. N. Ivy Ave. N. 5/16/2005 5/16/2005 5/16/2005 5/16/2005 6/13/2005 6/13/2005 6/13/2005 6/13/2005 6/13/2005 6/13/2005 6/13/2005 5/16/2005 6/13/2005 6/13/2005 6/13/2005 ND ND ND ND ND ND ND ND 0.2 0.2 ND ND ND ND ND ND ND ND ND ND ND ND 0.2 ND ND ND ND ND ND ND 478956 512491 8281 8280 15th St. N. 15th St. N. 3/8/2005 3/8/2005 ND ND ND ND 3M Cottage Grove Plant Both the State and 3M have sampled the water supply to Building 116 at the Cottage Grove facility, which comes from site groundwater wells. Exygen conducted the fluorochemical analysis for 3M, and MDH conducted the analysis for the State. Building 116 Sampling Results for May 16, 2003 Exygen Results Sample ID PFOS (ug/L or parts per billion) PFOA (ug/L or parts per billion) Bldg 116 Outlet 0.596 5.29 Bldg 116 Outlet* 0.517 5.58 ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) *Laboratory Duplicate p. 44 O Building 116 Sampling Results for December 7, 2004 Exygen Results Sample ID PFOS (ug/L or parts per billion) PFOA (ug/L or parts per billion) Effluent ND ND Effluent* ND ND Effluent Dup ND ND ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) laboratory Duplicate Building 116 Sampling Results for February 14, 2005 MDH Results, ug/L or parts per billion PFOS Sample ID Field ID Measured ' Reported Value Level 200502990 05-173 final (ug/L) (ug/L) 0.0 <0.5 Note: The reporting level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. PFOA Measured Reported Value Level (ug/L) (ug/L) 0.0 <1.0 Building 116 Sampling Results for June 6, 2005 Exygen Results ug/L or parts per billion Sample ID PFOS (ug/L) PFOA (ug/L) Effluent , ND ND Effluent* ND ND Effluent Dup ND ND ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) *Laboratory Duplicate 3M has tested a well at the site of a Trap Range on the Cottage Grove site which may occasionally have been used for drinking water. Results from August 17, 2001 sampling showed 4-4 p. 45 'o non-quantifiable levels of PFOS at a limit of quantitation of 0.025 ug/L. PFOA was measured at 0.541 ug/L (parts per billion), with 0.0565 ug/L in the laboratory duplicate and 0.0571 ug/L in the field duplicate. Private Wells Near Cottage Grove Facility MDH also sampled several private wells east of the 3M Cottage Grove facility. This work was done by MDH and is referenced in its Site Consultation Report concerning the facility. 3M has not located any copy of the MDH data; however, the Site Consultation Report (which Plaintiffs have) at page 17 indicates that neither PFOA nor PFOS was detected in those wells. Woodbury MDH tested Woodbury municipal wells numbers 10-15 sampled on January 27, 2005, and found no detectable PFOS or PFOA. MDH sampled a number of private wells in Woodbury and provided 3M with the following results: Woodbury June 15-16,2005 Sampling Results ug/L or parts per billion Sample ID Field ID 200515731 200515732 200515733 200515734 200515735 233142 408198 406171 151763 440575 PFOS Measured Value Reported Value ... (PP*>) 0.0000 <0.5 0.0000 <0.5 0.0000 <0.5 0.0000 <0.5 0.0000 <0.5 PFOA Measured Value 0.0000 Reported Value (PPb) <1.0 0.0000 0.0000 <1.0 <1.0 0.0000 <1.0 0.0000 <1.0 p. 46 200515736 200515737 200515738 200515739 200515740 200515741 200515742 200515743 200515744 200515745 200515746 (duplicate) Note: 544438 641472 TB ISW001 427043 471471 460152 402592 698214 109708 109738 162915 trip blank 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 <0.5 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 <1.0 <1.0 <1.0 <1.0 <1.0 < 1.0 <1.0 <1.0 <1.0 < 1.0 <1.0 1. The reporting level is 0.5 ppb for PFOS and 1.0 ppb for PFOA. 2. One sample (200515746) is measured twice and performed duplicate matrix spike measurement. City of Hastings 3M analyzed a number of samples from the municipal wells of the City of Hastings and found no measurable levels of PFOA or PFOS. Hastings December 22, 2004 Sampling Results ug/L or parts per billion Sample ID PFOS (ug/L) PFOA (ug/L) H-W6-207643 NO ND H-W6-207643* NQ ND H-W4-207993 ND ND H-W4-207993* ND ND H-W5-207639 ND ND H-W5-207639* ND ND H-W3-206333 ND ND H-W3-206333* ND ND H-W7-509053 ND ND H-W7-509053* ND ND ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) *Laboratory Duplicate 46 o p. 47 Hastings February 28,2005 Sampling Results ug/L or parts per billion Sample ID PFOS (ug/L) PFOA (ug/L) H-W6-207643 ND ND H-W6-207643* ND ND ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) "Laboratory Duplicate City of Cottage Grove 3M analyzed a number of samples from the municipal wells of the City of Cottage Grove and found no detectable levels of PFOA or PFOS. Cottage Grove December 22 and 29,2004 Sampling Results ug/L or parts per billion Sample ID CG-W6-201238 CG-W6-201238* CG-W9-165602 CG-W9-165602* CG-W5-208806 CG-W5-208806* CG-W3-208807 CG-W3-208807* CG-W7-201227 CG-W7-201227* CG-W8-110464 CG-W8-110464* CG-W 11-655944 CG-W11-655944* CG-W10-191904 CG-W 10-191904* CG-W2-208809 PFOS (ug/L) ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND PFOA (ug/L) ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND V p. 48 CG-W2-208809* ND ND CG-W1-208808 ND ND CG-W1-208808* ND ND ND = Not detected = Response between 0 and 0.025 ug/L NQ = Not quantifiable = Response between 0.025 ug/L and LOQ (0.050 ug/L) *Laboratory Duplicate City of North St. Paul MDH has informed 3M of the results of MDH samples collected from the City of North St. Paul on January 27, 2005. The analyses show no detectable PFOA or PFOS. North St. Paul January 27, 2005 Sampling Results ug/L or parts per billion Objections: Sample ID PFOS (ug/L) 200501452 (Well 3) 200501453 (Well 4) ND = < 0.5 ug/L ND ND PFOA (ug/L) ND ND 3M objects to Interrogatory No. 3 as overly broad and not reasonably calculated to lead to the discovery of admissible evidence to the extent it seeks information about drinking water supplies in Wisconsin or PFCs other than PFOA and PFOS. Exhibit D AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 16-Jun-2005 18:15 Contract No.: 4191 Matrix: N/A Sample Receipt date: 22-Jun-2005 Extraction Date: 06-Sep-2005 Analysis Date: 13-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 8:38:26 Lab Sample ID: L7909-1 Y2 Sample Size: 1.00 Initial Calibration Date: 13-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: Blank Data Filename: FC5G168S017 FC5G_168S015 Cal. Ver. Data Filename: CAL VER ID: FC5G_168S010 PFC-LIN-048CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION LIMIT U u 0.410 u u u u u 0.291 u u u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 0.254 0.255 0.258 0.250 RETENTION TIME 4 27 3.77 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected (2) R (% ) = Percent recovery 16814PFD3_2.xIs, S4 Approved by: CONC. FOUND (ng) 3.99 6.03 4.77 10.7 R (%)2 RETENTION TIME 33.2 50.3 39.7 88.9 4.70 5.56 5.56 5.41 _QA/QC Chemist 11-10-2005 dd-mm-yyyy > V X V S A N A L Y T I C A L S E R V I C E S L T D p.o. BOX22I9,2045MILLStD. WEST, SIDNEY, B.C.. CANADAV8t 3S8 TEL (250) 655-5800 FAX (250) 655-58)1 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1AI2 PERFLUORINATED ORGANICS ANALYSIS REPORT CUENT ID: Sample Collection; 28-Jun-2005 10:27 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-1 Matrix: SERUM Sample Size: 1.00 , Sample Receipt Date: 29-Jun-2005 Initial Calibration Date: 05-Aug-2005 Extraction Date: 04-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 05-Aug-2005 Time: 21:17:29 LC Column ID: C18, Zorbax XDB Extract Volume (mL): 2 Sample data Filename: FC5G_131S040 Injection Volume (pL): 30.0 Blank data Filename: FC5G_131S024 Dilution Factor: Concentration Units : N/A ng/mL Cal. Ver. data Filename: CAL VER ID: FC5GJ31S037 PFC-LIN-039CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u u 30.9 2.60 0.510 0.290 u u 6.03 88.6 u 0.638 0.620 0.251 0.247 0.268 0.259 0.256 0.255 0.254 0.255 0.258 0.250 4.70 5.07 5.38 5.67 4.90 5.50 LABELED COMPOUND 13C-PFOA 13C-PFDA LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 CONC. FOUND (ng) 7.69 10.3 R (V.)2 RETENTION TIME 64.1 85.8 4.70 5.34 (1) U = not detected (2 ) R (% ) = Percent recovery 16535p f D2_2.xis, S2 A pproved by: Q A /Q C Chemist 11-10-2005 dd-m/n*yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2045 MIUS RD. WEST, SIDNEY, B.C, CANADAV813S8 TCI (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 P F 0 S _ S 1_D 12 Form 1A/2 " " PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 28-Jun-2005 10.30 Lah Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-2 Matrix: SERUM Sample Size: 1.00 Sample Receipt Date: 29-Jun-2005 Initial Calibration Date: 05-Aug-2005 Extraction Date: 04-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 05-Aug-2005 Time: 21:42:08 LC Column ID: C18, Zorbax XDB Extract Volume (mL): 2 Sample Datafile: FC5G_131S042 Injection Volum e (pL): 30.0 Blank Data Filename: FC5G_131S024 Dilution Factor: Concentration Units : N/A ng/mL Cal. Ver. Data Filename: CAL VER ID: FC5G_131S037 PFC-LIN-039CS-F COMPOUND LAB FLAG ' CONIC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u u 24.2 1.48 u u u u 6.23 38.0 u 0.638 0.620 0.251 0.247 0.268 0.259 0.256 0.255 0.254 0.255 0.258 0.250 4.70 5.07 4.90 5.50 LABELED COMPOUND 13C-PFOA 13C-PFDA LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 CONC. FOUND (ng) 8.09 11.2 R (%)2 R E T E N T IO N T IM E 67.4 93.0 4.70 5.34 (1) U = not detected (2) R (%) = Percent recovery i6535PFD2_2.xfs. S4 Approved b y : .QA/QC Chemist 11-10-2005 dd-mm-yyyy A X Y S A N A L Y T I C A L . S E R V I C E S L T D P.0. BOX 22J9, 2045 MILLS RO. WEST, SIDNEY, B.C., CANADA 81 3S8 TEL (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 p fo s si_oi2 Form 1A/2 " PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 01-Jul-2005 13:03 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-4 Matrix: SERUM Sample Size: 1.00 Sample Receipt Date: 06-Jul-2005 Extraction Date: 04-Aug-2005 Anaiysis Date: 05-Aug-2005 Extract Volume (raL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 21:54:26 Initial Calibration Date: 05-Aug-2005 Instrument ID: LC-MS/MS LC Column ID; C18, ZorbaxXDB Sample Datafile: FC5G_131S043 Blank Data Filename: FC5GJ31S024 Cal. Ver. Data Filename: FC5G_131S037 CAL VER ID: PFC-LIN-039CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u u 9.25 1.40 u u u u 2.53 28.4 u 0.638 0.620 0.251 0.247 0.268 0.259 0.256 0.255 0.254 0.255 0.258 0.250 4.66 5.01 4.90 5.50 LABELED COMPOUND 13C-PFOA 13C-PFDA LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 CONC. FOUND (ng) 8.14 10.7 R (%)* RETENTION TIME 67.9 88.8 4.66 5.34 (1 ) U = n o t d e tected (2 ) R (% ) = Percent recovery i6535PFD2_2.xls, S5 A p p ro v e d by:. Q A /Q C Chemist 11-10-2005 dd-mm-yyyy A X Y S AP'vLA.LVTICA.L SERN/'ICTES L T D P.0. BOX 221?. 2045 ILLS RO. WEST, SIDNEY, B.C., CANADA V813S8 TEI (250) 455-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 08-Aug-2005 11:41 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 18:50:23 Lab Sample ID: L7932-16 Y2 (A) Sample Size: 1.00 Initiai Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S033 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-N-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U u 0.753 E 0.967 0.417 0.273 U u 17.3 85.9 u 0.256 0.248 0.251 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.22 5.05 5.41 5.70 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG 1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 11.3 12.8 11.9 12.0 (1) U = not detected; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery R (%)2 RETENTION TIME 94.5 4.70 107 5.56 99.2 5.56 100 5.36 16755PF_D1_2.xls, S4 Approved by: .QA/QC Chemist 11-10-05 dd-mm-yyyy )][@A X Y S -A.INd>KL>rTICZA.L S E R V I C E S ETC) PO. BOX 22I9, 2045 MILLS Ml. WEST, SIDNEY, B.C., CANADAV8L 3S8 TEL (250) 55-5800 FAX (250) 455-5811 AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: ' Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 09-Aug-2005 11:41 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration U n its: ng/mL Time: 19:04:39 Lab Sample ID: Sample Size: WG16755-104 Y2 (DUP L7932-16) 1.00 mL Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S034 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB FLAG1 CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u 0.945 E 1.37 0.439 U U u 14.5 79.8 u 0.256 0.248 0.251 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 4.22 5.05 5.36 4.87 5.51 LABELED COMPOUND 1 3 C 2 -P F O A 13C4-PFOS(80) 1 3 C 4 -P F O S (9 9 ) 13C2-PFDA LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 11.7 14.2 13.7 14.3 (1) U = nol detected; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery R (%)2 R E T E N T IO N T IM E 97.7 4.70 118 5.56 114 5.56 119 5.36 16755PF_D1_2.xls. S5 Approved by:. - ________ q a/QC Chemist 11-10-05 dc-mm-yyyy ][(A X Y S ^ M Y X I L S T T I O X L S E R V I C E S L T D f.o. BOX 2219, 2045 MIUS RD. WEST, SIDNEY, B.C., CANADAV8L3S8TEI (250) <55-5800 FAX (250) <55-5811 AXYS METHOD MLA-042 Rev 02 PFOS_st_oi2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: " Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 08-Aug-2005 11:41 Contract No.: 4191 Matrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 13-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration U n its: ng/mL Time: 1:43:59 Lab Sample ID: Sample Size: WG16755-104 Y2i (DUP L7932-16 Y2i (A)) 1.00 mL Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S062 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S059 CAL VER ID: PFC-UN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFIlnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT D 89.1 0.741 RETENTION TIME 4.70 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG 1 D SPIKE CONC. (ng) 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.xls, S3 Approved by: ^4 CONC. FOUND (ng) 11.5 R(%)2 RETENTION TIME 95.8 4.70 QA/C5C Chemist 11-10-05 dd-mm-yyyy A X Y S / X M X X L Y T I O X L S E R V I C E S L T D P.0. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADAV8L 3S8 TEL (250) <55-5800 FAX (250) <55-5811 AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction datae: 29-Aug-2005 Analysis datae: 13-Sep-2005 Time: 1:29:43 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Sample Collection: 08-Aug-2005 11:41 Lab Sample ID: L7932-16 Y2i (A) Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample data Filename: FC5G_167S061 Blank data Filename: FC5G_167S031 Cal. Ver. data Filename: FC5G 167S059 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT D 95.1 0.741 RETENTION TIME 4.70 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG 1 D SPIKE CONC. (ng) 12.0 (1) U = not detected; D = dilution data (2) R {%) = Percent recovery 16755PF_D3_Zxts, S2 Approved by:_ CONC. FOUND (ng) 9.79 R(%)2 RETENTION TIME 81.6 4.70 .QA/QC Chemist 11-10-05 (id-mm-yyyy ][C9 A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2045 M itts RO. WEST, SIDNEY, B.C., CANADAV813S8TEI (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 p f o s _ s i _ D 12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID' Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 08-Aug-2005 13:31 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 19:18:55 Lab Sample ID: L7932-17 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S035 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S027 CALVER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT U U 0.367 42.4 1.07 U u u u 12.9 51.1 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.22 4.70 5.05 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 i6755PF_Di_2.xls. S6 Approved by:. CONC. FOUND (ng) 10.8 11.5 12.5 12.8 R (%)2 RETENTION TIME 90.2 4.70 95.7 5.56 104 5.56 107 5.41 QAYQC Chemist 11-10-05 dd-mm-yyyy I( A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 221?, 2045 MlltS RD. WEST. SIDNEY, B.C, CANADAMl 358 TEI (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 2p f o s _s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 19:47:27 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Sample Collection: 08-Aug-2005 13:17 Lab Sample ID: L7932-19 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S037 Blank Data Filename: FC5GJ67S031 Cal. Ver. Data Filename: FC5G 167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB CONC FLAG12 FOUND DETECTION LIMIT U u 0.276 43.5 1.03 0.315 u u u 10.6 51.4 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.22 4.70 5.05 5.41 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS{99) 13C2-PFDA (1) U = not detected (2) R {%) = Percent recovery LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 10.1 12.2 12.0 12.3 R (%)J RETENTION T IM E 84.1 102 99.8 103 4.70 5.56 5.56 5.41 167S5PF_D1_2.)ds, 58 Approved by:. / y <Z. -- QA/QC Chemist 11-10-05 dd-mm-yyyy @][(A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2015 MltiS 0, WEST, SIDNEY, B.C., CANADAV8L 3S8 TEI (250) 55-5800 FAX (250) 455-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID` Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 08-Aug-2005 13:10 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor N/A Concentration Units : ng/mL Time: 20:01:42 Lab Sample ID: L7932-20 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S038 Blank Data Filename: FC5G167S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION LIMIT U U u 63.3 1.55 0.331 u u u 17.0 76.7 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.70 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB F LA G 12 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 1675SPF_D1_2jds, S9 Approved by: CONC. FOUND (ng) 10.3 10.8 11.5 11.1 R (%)2 RETENTION TIME 85.6 89.8 95.6 92.3 4.70 5.56 5.56 5.36 .QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D BO. BOX 2219, 2045 Milts (D. WEST, SIDNEY, B.C., CANADA V8L 3S8 Iti (250) 55-5800 FAX (250) 55-5811 AXYS METHOD MLA-042 Rev 02 pfos_s i_d i2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 20:15:59 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration U n its: ng/mL Sample Collection: 08-Aug-2005 13:14 Lab Sample ID: L7932-21 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S039 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U U u 48.4 0.626 u u u u 11.9 71.9 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.70 5.05 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R {%) = Percent recovery LAB FLAG' SPIKE CONC. (ng> 12.0 12.0 12.0 12.0 16755PF_D1_2.xls, S10 Approved by:_ CONC. FOUND (ng) 10.9 14.0 12.9 14.6 R(%)12 RETENTION TIME 90.7 4.70 117 5.56 108 5.56 122 5.41 QA/QC Chemist 11-10-05 dd-mm-yyyy I# A X Y S /Xl^JyXI Y T I C A L S E R V I C E S L T D POI. BOX 22IP, 2045 MIUS 80. WEST, SIDNEY, B.C, CANADAV81.3S8 TEI (250) 855-5800 FAX (250) 855-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 1 1 -Aug-2005 10:56 Contract No.: 4191 Matrix: SERUM Sample Receipt date: 12-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration U n its: ng/mL Time: 20:44:30 Lab Sample ID: L7932-24 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_16TS041 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5GJ67S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION LIMIT U u 0.321 10.7 0.877 0.458 0.415 u u u 23.1 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.22 4.70 5.05 5.36 5.70 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG' SPIKE CONC. <ng) 12.0 12.0 12.0 12.0 i6 7S 5P F_oi_2.xls, S1 2 Approved by:. CONC. FOUND (ng) 10.9 12.3 13.0 12.4 R (%)2 RETENTION TIME 90.5 4.70 103 5.56 108 5.56 103 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy I(A X Y S A N A L Y T I C A L S E R V I C E S L T D BO. BOX 2219, 2045 MILLS BO. WEST. SIDNEY, B.C., CANADAV8L 3SB TEL (250) <55-5800 FAX (250) <55-5811 p. 63 AXYS METHOD MLA-042 Rev 02 PFOS_S1_D12 FoiTO 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 12-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 20:58:46 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Sample Collection: 11-Aug-2005 10:59 Lab Sample ID: L7932-25 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5GJI67S042 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-UN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT U u 0.373 17.1 0.848 0.498 0.398 u u 3.76 20.1 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.22 4.70 5.05 5.36 5.70 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_01_2.xls. S13 Approved by: CONC. FOUND ("9) 10.1 11.9 13.6 12.5 R (%)2 RETENTION T IM E 84.2 98.9 114 104 4.70 5.56 5.51 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy JJP A X Y S A N A L Y T I C A L SERX/ICTES L T D P.0. BOX 2219, 2045 MILLS SD. WEST, SIDNEY, B.C., CANADA V8L3S8 Ifl (250) 55-5000 FAX (250) 655-5811 63 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 11-Aug-2005 12:31 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 12-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 20:30:13 Lab Sample ID: L7932-23 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S040 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G 167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U u 0.711 E 1.46 0.376 U u u 20.9 E u 0.256 0.248 0.251 0.268 0.259 0.257 0.255 2.54 2.55 0.250 RETENTION TIME 4.22 5.05 5.36 4.87 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 12.3 15.5 13.7 15.2 (1) U = not detected; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery R(%)12 RETENTION TIME 103 4.70 129 5.56 114 5.56 126 5.36 16755PF_D1_2jds, S11 Approved by:_ QA/QC Chemist 11-10-05 dd-mm-yyyy ][C A X Y S x x r v j / \ L > m o x L s e r v i c e s l t d p.o. box2 2 1 ?, 20 4 5 mus no. west, sioney, b.c., can * vslssstel(2soi ss-s&oofax2 so sss-sbii AXYS METHOD MLA-042 Rev 02 p f o s _s i _012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 1 1 -Aug-2005 12:31 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 12-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 13-Sep-2005 Time: 2:12:31 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor 3 . Concentration U n its: ng/mL Lab Sample ID: L7932-23 Y2i Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S064 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S059 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT D 105 0.741 RETENTION TIME 4.70 D 113 0.774 5.56 LABELED COMPOUND 1 3C 2 -P FO A 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 D D SPIKE CONC. (ng) 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.xls. S5 Approved by: CONC. FOUND (ng) 13.3 11.6 R (%)2 RETENTION T IM E 111 4.70 96.4 5.56 QA/QC Chemist 11-10-05 dd-m m -yyyy )][(A X Y S A.rsl>\LVTICZA.L S E R V I C E S L T D RO. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA V8L 3S8 TEL (250) 655-5800 FAX (250) 655-5811 p. 66 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID' Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 11 -Aug-2005 12:33 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 12-Aug-2005 Extraction datae: 29-Aug-2005 Analysis datae: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 21:55:49 Lab Sample ID: L7932-26 Y4 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample data Filename: FC5G_167S046 Blank data Filename: FC5G_167S031 Cal. Ver. data Filename: FC5G 167S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U U 0.665 58.7 1.74 0.670 U U U 14.3 73.4 U 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.23 4.70 5.05 5.41 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_D2_2.xls. S2 Approved by:_ CONC. FOUND (ng) 10.2 12.3 10.4 11.0 R(%)12 RETENTION TIME 84.9 4.70 102 5.56 87.0 5.56 92.0 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy )][(& A X Y S A N A L Y T I C A L S E R V IC E S L T D P.O.BOX2219, 2045IOSD. WEST,SIDNEY,B.C., CANADAV813S8TEL(250) 655-5800FAX(250) 655-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 15-Aug-2005 13:54 Contract No.: 4191 Matrix: SERUM Sample Receipt date: 17-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 22:10:04 Lab Sample ID: L7932-28 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S047 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5GJ67S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U u u 5.92 1.32 0.486 0.272 u u 3.76 29.5 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.70 5.05 5.41 5.75 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG' SPIKE CONC. <ng) 12.0 12.0 12.0 12.0 16755PF_D2_2.xls, S3 Approved by:. CONC. FOUND (ng) 10.5 11.3 10.4 13.6 R (% )12 RETENTION TIME 87.2 4.70 94.4 5.56 86.4 5.56 113 5.41 QA/QC Chemist 11-10-05 dd-mm-yyyy )][(A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 22I9,2045 MIUS RD. WEST, SIDNEY, B.C., CANADA V8L 3S8 TEL (25G) 55-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 P F 0S _ S 1_ D 12 Form 1A/2 PERFLUOR1NATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 1 6-Aug-2005 09:43 Contract No.: 4191 Matrix: SERUM Sample Receipt date: 17-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration U n its: ng/mL Time: 22:24:21 Lab Sample ID: L7932-29 Y4 Sample Size: 1.00 Initial Calibration Date: Instrument ID: 12-Sep-2005 LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S048 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5GJ67S044 CAL VER ID: PFC-N-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U U 1.16 30.7 2.96 0.362 u u u 7.13 56.8 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.23 4.70 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 10.5 11.9 13.7 13.4 (1) U = not detected (2) R (%) = Percent recovery 16755PF_D2_2.xls, S4 Approved by: r/r*~*<? R (%)2 RETENTION TIME 87.8 4.70 99.0 5.56 114 5.56 112 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy C A X Y S A N A L Y T I C M S E R V I C E S L T D P.0. BOX 221?, 2045 MIUS BO. WEST, SIDNEY, B.C., CANADAY8L 358 TEL (250) 55-5800 FAX (250) 55-5811 AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 17-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 22:38:38 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Sample Collection: 16-Aug-2005 09:40 Lab Sample ID: L7932-30 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S049 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G 167S044 CAL VER ID: PFC-UN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG 1 CONC FOUND DETECTION LIMIT U U 1.06 27.5 2.60 0.430 u u u 5.04 62.0 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.23 4.70 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_02_2jds, S5 Approved by:. CONC. FOUND (ng) 10.3 13.1 12.2 13.7 R (%)2 RETENTION TIME 86.2 4.70 109 5.56 101 5.56 115 5.36 .QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2045 M ilts JO. WEST,SIDNEY, B.C, CANADAV8L3S8TEI (250) 455-5800FAX(250) 455-581 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 17-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 22:52:53 Extract Volume (mL): 2 Injection Volume (pL): 30.0 D ilution Factor: N/A Concentration U n its: ng/mL Sample Collection: 16-Aug-2005 09:37 Lab Sample ID: L7932-32 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S050 Blank Data Filename: FC5GJ67S031 Cal. Ver. Data Filename: FC5G_167S044 CALVER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U u 0.253 13.3 1.02 0.265 u u u u 12.3 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.23 4.70 5.05 5.36 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_D2_Zxls, S6 Approved by:_ CONC. FOUND (ng) 8.70 12.6 13.7 11.2 R (%)2 RETENTION TIME 72.5 4.70 105 5.56 114 5.56 93.7 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy ^ A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2045 MILLS Ml. WEST, SIDNEY, B.C, CANADA V813S8 TEL (250) 655-5800 FAX (250) 655-5811 p . 71 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 16-Aug-2005 09:35 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 17-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 23:07:08 Lab Sample ID: L7932-33 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S051 Blank Data Filename: FC5G167S031 Cal. Ver. Data Filename: FC5G 167S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB FLAG1 CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u 0.454 15.5 0.660 u u u u u 12.7 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 4.23 4.70 5.05 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_D2_2.xls, S7 Approved by. CONC. FOUND (ng) 10.7 14.0 15.2 14.1 R (%)2 RETENTION TIME 89.1 4.70 116 5.56 126 5.56 118 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy )][C A X Y S A N A L Y T I C A L S E R V IC E S L T D P.0. BOX2219, 2045MltlS RO.WEST, SIDNEY,B.C., CANADAV8L3S8IEI (250) <55-5800FAX(250) <55-5811 'll AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUOR1NATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Matrix: SERUM Sample Receipt date: 19-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Time: 23:21:23 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Sample Collection: 1 7-Aug-2005 18:11 Lab Sample ID: L7932-35 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S0S2 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT U u 0.352 74.6 2.16 0.466 0.384 u u 13.4 91.0 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.23 4.70 5.05 5.36 5.70 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(8Q) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 9.13 11.3 11.3 11.6 (1) U = not detected (2) R (%) = Percent recovery 16755PF_D2_2jds, SB Approved by: G- R(% )2 RETENTION TIME 76.0 94.3 94.6 96.5 4.70 5.56 5.56 5.36 QA/QC Chemist 11-10-05 dd-fnm-yyyy IC9A X Y S A N A L Y T I C A L S E R V I C E S L T D F.O. BOX 2219, 2045 WILIS RO. WEST, SIDNEY, B.C., CANADAV8L3S8 TEL (250) 655-5800 TAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 18-Aug-2005 18:15 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 23-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 13-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration U n its: ng/mL Time: 0:18:25 Lab Sample ID: L7932-39 Y4 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S056 Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S044 CALVER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG U u u u u u u CONC FOUND 9.66 1.35 0.375 4.52 26.6 DETECTION LIMIT 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION TIME 4.70 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 16755PF_D2_2jds, S12 Approved by:_ CONC. FOUND (ng) 9.15 13.8 12.8 12.8 R (%)2 RETENTION TIME 76.2 4.70 115 5.56 107 5.56 106 5.36 .CWQC Chemist 11-10-05 dd-mm-yyyy C( A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0.BOX 2219. 2045 MltlSRD. WEST, SIDNEY. B.C., CANADA VBl 3S8TEL {2S0) 655-5800 X 250) 655-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 23-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 13-Sep-2005 Time: 3:09:35 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Sample Collection: 18-Aug-2005 18:17 Lab Sample ID: Sample Size: WG16755-105 Y2i (DUP L7932-37 Y2i (A)) 1.00 mL Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S06fi Blank Data Filename: FC5G_167S031 Cal. Ver. Data Filename: FC5G_167S059 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT D 103 0.741 RETENTION TIME 4.70 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG' D SPIKE CONC. (ng> 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.xls. S9 Approved by: CONC. FOUND ("9) 9.66 R (%)12 RETENTION TIME 80.5 4.70 QA/QC Chemist 11-10-05 dd-mm-yyyy 1CA X Y S A N A L Y T I C A L S E R V I C E S L T D P.O. BOX 221?. 2045 MIUS HO. WtST, SIDNEY, B.C., CANADAY813S8 TEI (250) 55-5800 FAX (250) 455-581) AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 18-Aug-2005 18:17 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: M atrix: 4191 SERUM Lab Sample ID: Sample Size: WG16755-105 Y2 (DUP L7932-37 Y2) 1.00 mL Sample Receipt date: 23-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 12-Sep-2005 Time: 23:49:55 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_167S054 Injection Volume (pL): 30.0 Blank Data Filename: FC5GJ67S031 Dilution Factor: Concentration Units : N/A ng/mL Cal. Ver. Data Filename: FC5G_167S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u 2.62 E 1.83 0.894 U u u 14.5 72.7 u 0.256 0.248 0.251 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 4.18 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 10.2 14.5 13.2 15.0 (1) U = not detected; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery R (%)12 RETENTION T IM E 85.0 121 110 125 4.70 5.51 5.51 5.36 16755PF_02_2 xls. S10 Approved by:. .QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S /\IS>J>VIJVXICZA.L S E R V I C E S L T D PO. BOX 2219, 2045 MIUS BO. WEST, SIDNEY, B.C, CANADA V813S8 TEI (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 18-Aug-2005 18:17 Contract No.: 4191 Matrix: SERUM Sample Receipt date: 23-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 23:35:39 Lab Sample ID: L7932-37 Y2 Sample Size: 1.00 Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S053 Blank Data Filename: FC5GJ67S031 Cal. Ver. Data Filename: FC5G 167S044 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION L IM IT U u 2.08 E 1.75 0.910 U u u 13.4 70.3 u 0.256 0.248 0.251 0.268 0.259 0.257 0.255 2.54 2.55 0.258 0.250 RETENTION T IM E 4.23 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 1 3 C 4 -P F O S (8 0 ) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 9.98 13.5 13.0 13.7 (1) U = not detected; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery R (%)2 RETENTION T IM E 83.1 112 108 114 4.70 5.51 5.51 5.36 16755PF_02_2xls, S9 Approved by:_ QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.O.BOX2219, 2045MUIS80. WEST, SIDNEY. B.C.CMWD*V813S8JH(250)855-5800 FAX(250) 455-5811 p. 77 AXYS METHOD MLA-042 Rev 02 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 18-Aug-2005 18:17 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-37 Y2i (A) M atrix: SERUM Sample Size: 1.00 : Sample Receipt date: 23-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 13-Sep-2005 Time: 2:55:19 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_167S067 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_167S031 Dilution Factor Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_167S059 CALVER ID: PFC-LIN-044CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 104 0.741 4.70 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 D SPIKE CONC. (ng) 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.xls, S8 Approved by: CONC. FOUND (ng) 9.67 R (%)2 RETENTION TIME 80.6 4.70 QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S /X I^ J X X L Y T IC /X L S E R V IC E S L T D P.0. BOX2219, 2045MILLSRD.WEST, SIDNEY,8.C., (MIAO*V8L3S8TEL(250) 55-5800FAX(250) 55-5811 77 AXYS METHOD MLA-042 Rev 02 P F 0S _ S 1_D 12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CUENT ID: Sample Collection : 18-Aug-2005 18:11 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-38 Y2i Matrix: SERUM Sample Size: 1.00 Sample Receipt date: 23-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 13-Sep-2005 Time: 3:23:49 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_167S069 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_167S031 Dilution Factor: Concentration U n its: 3 ng/mL Cal. Ver. Data Filename: FC5G 167S059 CALVER ID: PFC-LIN-044CS-F COMPOUND LAB CONC FLAG12 FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 96.1 UD UD UD UD UD D 16.3 D 67.8 UD 0.767 0.744 0.753 0.741 0.804 0.777 0.770 0.765 7.62 7.65 0.774 0.750 4.70 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13 C 4 -P F O S (8 0 ) 13C4-PFOS(99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected: D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.jds, S10 Approved by:. CONC. FOUND (ng) 11.4 12.1 11.1 9.86 R (%)* R E T E N T IO N T IM E 94.7 101 92.7 82.2 4.70 5.56 5.56 5.41 .QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R N / I C E S L T D P.0. BOX 2219, 2045 MILLS RD. WEST, SIDNEY. B.C., CANADA V8L 3S8 TEL (250) 655-5800 FAX (250) 5S-5811 AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 22-Aug-2005 16:20 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Matrix: SERUM Sample Receipt date: 24-Aug-2005 Extraction datae: 06-Sep-2005 Analysis datae: 16-Sep-2005 Time: 13:23:23 Extract Volume (mL): 2 Injection Volume (|iL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Lab Sample ID: L7932-41 Y4 (A) Sample Size: 1.00 Initial Calibration Date: 15-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample data Filename: FC5G_176S011 Blank data Filename: FC5G_159S016 Cal. Ver. data Filename: CALVER ID: FC5G_176S008 PFC-LIN-048CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 19.6 D 1.78 D 0.952 UD UD UD D 5.56 D 8.91 UD 0.638 0.620 0.628 0.618 0.670 0.648 0.640 0.638 0.635 0.638 2.58 0.625 4.70 5.12 5.46 4.93 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (% ) = Percent recovery 16814PFD5_2.xIs , S2 Approved by: CONC. FOUND ("9) 11.1 11.3 13.6 11.7 R (%)2 RETENTION TIME 92.9 94.3 113 97.6 4.70 5.56 5.56 5.41 QA/QC Chemist 11-10-2005 dd-mm-yyyy A X Y S /Xr^JYXLYTIOVL S E R V I C E S L T D P.0. BOX 221?, 2045 MlUS RD. WEST, SIDNEY, B.C, UNAM V8L 3S8 TEL (250) 655-5800 FAX (250) 655-5811 77 AXYS METHOD MLA-042 Rev 03 PF0S_S1 D12 Form 1A/2 " PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection: CLIENT ID: 22-Aug-2005 16:20 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Matrix: Sample Receipt date: SERUM 24-Aug-2005 Extraction Date: Analysis Date: 06-Sep-2005 16-Sep-2005 Time: 0:08:02 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Lab Sample ID: WG16814-104 Y3 Sample Size: 1.00 i Initial Calibration Date: 15-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_175S013 Blank Data Filename: FC5G_159S016 Cal. Ver. Data Filename: CAL VER ID: FC5GJ75S010 PFC-LIN-048CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 21.1 D 1.56 D 1.00 UD UD UD D 2.62 D 12.8 UD 0.638 0.620 0.628 0.618 0.670 0.648 0.640 0.638 0.635 0.638 2.58 0.625 4.70 5,05 5.41 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery i68i4PFD4_2.xte, S3 Approved by: CONC. FOUND (ng) 13.4 14.7 12.2 13.8 R (%)2 RETENTION TIME 112 4.70 122 5.56 102 5.56 115 5.41 QA/QC Chemist 11-10-2005 dd-mm-yyyy >)][(A X Y S /MVlyALYTICZAL S E R V I C E S L T D P.0. BOX 221 9,20 45 MILLS ID. WEST, SIDNEY, B .t, CANADA8L 3S8 TEL (250) 555-5800 FAX (250) 655-5811 p. 81 AXYS METHOD MLA-042 Rev 03 pfos_s i D12 Form 1A/2 " PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection: CLIENT ID: 24-Aug-2005 17:18 Lab Name: A X Y S ANALYTICAL SERVICES Contract No.: Matrix: Sample Receipt date: 4191 SERUM 26-Aug-2005 Extraction Date: Analysis Date: 06-Sep-2005 16-Sep-2005 Time: 0:36:32 Extract Volume |mL): 2 Injection Volume (pL): Dilution Factor: 10.0 3 Concentration Units : ng/mL Lab Sample ID: L7932-44 Y3 Sample Size: 1.00 I Initial Calibration Date: 15-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_175S015 Blank Data Filename: FC5G_159S016 Cal. Ver. Data Filename: CAL VER ID: FC5G_175S010 PFC-LIN-048CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 32.7 D 0.963 UD UD UD UD D 14.5 D 41.5 UD 0.638 0.620 0.628 0.618 0.670 0.648 0.640 0.638 0.635 0.638 2.58 0.625 4.70 5.05 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1 ) U = not detected; D = dilution data (2) R (% ) = Percent recovery i68l4PFD4_2.xls, S5 Approved by:. CONC. FOUND (ng) 15.1 14.2 14.4 14.2 R (%)2 RETENTION TIME 126 4.70 118 5.56 120 5.56 118 5.41 QA/QC Chemist 11-10-2005 dd-mm-yyyy T O A X Y S / \ r v l> \ L V T I O M _ S E R V IC E S L T D P.0. BOX2219, 2045MILLSRD.WEST.SIDNET,8.C. CANADAV813S8IEI (250) 655-5800FAX(250) 455-5811 SI AXYS METHOD MLA-042 Rev 03 p f o s S 1_ D 12 Form 1A/2 " PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 25-Aug-2005 10:45 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: M atrix: Sample Receipt date: Extraction Date: Analysis Date: Extract Volume (raL): 4191 SERUM 26-Aug-2005 06-Sep-2005 16-Sep-2005 2 Time: 0:22:18 Lab Sample ID: Sample Size: Initial Calibration Date: Instrument ID: LC Column ID: Sample Datafile: L7932-43 Y3 1.00 15-Sep-2005 LC-MS/MS C18 FC5G_175S014 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_159S016 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_175S010 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 10.2 UD UD UD UD UD D 0.905 D 24.2 UD 0.638 0.620 0.628 0.618 0.670 0.648 0.640 0.638 0.635 0.638 2.58 0.625 4.70 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (% ) = Percent recovery 16814PFD4_2.xIs, S4 Approved by: CONC. FOUND (ng) 12.7 11.2 14.5 14.2 R (%)2 RETENTION TIME 106 4.70 92.9 5.56 121 5.56 118 5.41 QA/QC Chemist 11-10-2005 dd-mm-yyyy ][($ A X Y S / N . r v l y N . L Y T I C A . L S E R V I C E S L T D P.0. BOX 2219, 2045 MILLS HD. WESI. SIDNEY, B.C.. CANADAV8L 3S8 TEL (250) <55-5800 FAX (250) 55-5811 AXYS METHOD MLA-042 Rev 03 p f o s _s i _d i 2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 25-Aug-2005 10:48 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-45 Y2 Matrix: SERUM Sample Size: 1.00 Sample Receipt date: 26-Aug-2005 Initial Calibration Date: 13-Sep-2005 Extraction Date: 06-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 13-Sep-2005 Time: 10:03:59 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_168S023 Injection Volume (pL): 30.0 Blank Data Filename: FC5G_168S015 Dilution Factor: Concentration Units : N/A ng/mL Cal. Ver. Data Filename: FC5G_168S010 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U u 0.401 80.5 1.77 0.841 0.343 u u 49.4 E u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 0.254 0.255 0.250 4.18 4.70 5.05 5.36 5.70 4.87 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 11.5 10.3 12.7 12.6 (1) U = not detected; E = exceeds calibrated linear range, see dilution data (2) R (% ) = Percent recovery 16ai4PFD3_Zxls, S10 Approved by:_ R{%)12 RETENTI TIME 95.9 4.70 86.0 5.56 106 5.56 105 5.36 Q A /Q C Chemist 11-10-2005 dd-mm-yyyy )][@A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 20<5 MILLS RD. WEST. SIDNEY, B.C., CANADAV8L 3S8 TEL (250) 455-5800 FAX (250) 655-581 i AXYS METHOD MLA-042 Rev 03 pfos_s i_d i2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 25-Aug-2005 10:48 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-45 Y2i M atrix: Sample Receipt date: SERUM 26-Aug-2005 Sample Size: Initial Calibration Date: 1.00 13-Sep-2005 mL Extraction Date: 06-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 13-Sep-2005 Time: 11:29:32 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_168S029 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_168S015 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_168S010 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION UMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA X X X X X X X X X X D 163 X 0.645 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' X X D X SPIKE CONC. (ng) 12.0 (1) D = dilution data; X = results reported separately (2) R (%} = Percent recovery 16814PFD3_2xls, S15 Approved by:_ CONC. FOUND (ng) R (%)12 RETENTION TIME 10.7 89.0 5.56 QA/QC Chemist 11-10-2005 dd-mm-yyyy [0A X Y S /\rsJ/M_YTIOK.L S E R V I C E S L T D P.0. BOX 2219, 2045 MIUS 80. WEST, SIDNEY, I.C, CANADA VBL 3SS TEl (250) 55-5800 FAX (250! 55-5811 AXYS METHOD MLA-042 Rev 03 pfos_s i_d i2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 25-Aug-2005 18:35 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: M atrix: 4191 SERUM Lab Sample ID: Sample Size: L7932-47 Y2i 1.00 Sample Receipt date: Extraction Date: 31-Aug-2005 06-Sep-2005 Initial Calibration Date: Instrument ID: 13-Sep-2005 LC-MS/MS Analysis Date: 13-Sep-2005 Time: 11:43:48 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_168S030 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_168S015 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_168S010 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 63.3 D 1.03 D 0.775 UD UD UD D 11.9 D 73.1 UD 0.638 0.620 0.627 0.617 0.670 0.647 0.641 0.637 0.635 0.637 0.645 0.625 4.70 5.05 5.36 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (% ) = Percent recovery i63l4PFD3_2.xis, S16 Approved by: CONC. FOUND (ng) 13.4 13.4 12.1 11.4 R (%)2 RETENTION TIME 112 4.70 111 5.56 101 5.56 95.2 5.41 QA/QC Chemist 11-10-2005 dd-mm-yyyy )X(9 A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219. 20X5 Hills (O. WEST, SIDHEY, B.C.. CANADA V813S8 TEl (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CUENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 25-Aug-2005 18:39 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 31-Aug-2005 Extraction Date: 06-Sep-2005 Analysis Date: 13-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 10:32:29 Lab Sample ID: L7932-48 Y1 Sample Size: Initial Calibration Date: 1.00 13-Sep-2005 mL Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_168S025 Blank Data Filename: FC5G_168S015 Cal. Ver. Data Filename: FC5G_168S010 CALVER ID: PFC-LIN-048CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U u u 14.6 1.49 0.312 u u u 2.29 30.8 u 0.256 0.248 0.251 0.247 0.268 0.259 0.257 0.255 0.254 0.255 0.258 0.250 RETENTION TIME 4.70 5.05 5.36 4.87 5.51 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG 1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected (2) R {% ) = Percent recovery i68l4PFD3_2.xls. S12 A pproved by:. CONC. FOUND (ng) 12.0 15.7 15.9 16.2 R (%)2 RETENTION TIME 99.8 4.70 131 5.51 133 5.51 135 5.36 Q A /Q C Chemist 11-10-2005 dd-mm-yyyy A X Y S / W I A L Y T I C A . L S E R V I C E S L T D P.0. BOX 2219,2015 MIUS (0. WEST, SIDNEY, B.C., CANADAV8t 3S8 TEL (250) 455-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 29-Aug-2005 09:59 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: 17932-49 Y3 M atrix: SERUM Sample Size: 1.00 Sample Receipt date: 31-Aug-2005 Initial Calibration Date: 15-Sep-2005 Extraction Date: 06-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 16-Sep-2005 Time: 0:50:49 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_175S016 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_159S016 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_175S010 CAL VER ID: PFC-LJN-048CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 7.21 D 1.30 D 0.650 UD UD UD D 9.50 D 38.9 UD 0.638 0.620 0.628 0.618 0.670 0.648 0.640 0.638 0.635 0.638 2.58 0.625 4.70 5.05 5.41 4.87 5.56 LABELED COMPOUND 13C2-PFOA 13C4-PFOS{80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG ' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1 ) U = not detected: D = dilution data (2) R (% ) = Percent recovery 16814PFD4_2.xIs , ss Approved by: CONC. FOUND (ng) 10.9 11.9 10.7 10.8 R {%f RETENTION TIME 91.0 4.70 99.4 5.56 89.2 5.56 89.7 5.41 Q A IQ C Chemist 11-10-2005 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0.80X 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA V8L 3S8 TEL (250) 455-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 31-Aug-2005 09:56 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: WG16982-104 i Matrix: SERUM Sample Size: 1.00 Sample Receipt date: 01-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 0:41:20 LC Column ID: C18 Extract Volume (raL): 2 Sample Datafile: FC5G_181S054 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor: Concentration U n its: 3 ng/mL Cal. Ver. Data Filename: FC5G_181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG1 CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 26.7 D 1.00 UD UD UD UD D 5.34 D 32.7 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.65 5.05 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 2PFD1 2 x1s. S4 Approved bv: jA CONC. FOUND <ng) 12.3 12.4 11.6 10.5 R (%)2 RETENTION TIME 103 4.65 103 5.46 97.0 5.46 87.3 5.36 '-- . QA/QC Chemist 11-10-05 dd-mm-yyyy ^)][(A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219, 2045 ttIUS RD.WEST, SIDNEY, B.C., CANADAV8L 3S8IE I (250) 455-5800 FAX (250) 455-5811 AXYS METHOD MLA-042 Rev 03 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 31-Aug-2005 09:56 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-51 I (A) M atrix: SERUM Sample Size: 1.00 Sample Receipt date: 01-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 0:27:07 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_181S053 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor: Concentration U n its: 3 ng/mL Cal. Ver. Data Filename: FC5G_181S048 CALVER ID: PFC-LIN-055CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT UD UD UD D 27.0 D 1.55 UD UD UD UD D 5.27 D 28.5 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 RETENTION TIME 4.65 4.99 4.80 5.46 LABELED COMPOUND -I3C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2.xls, S3 Approved by:_ CONC. FOUND (ng) 11.4 14.6 13.5 10.1 R (%)12 RETENTION TIME 94.9 4.65 122 5.46 113 5.46 83.8 5.36 _QA/QC Chemist 11-10-05 dd-mm-yyyy )][(9A X Y S / `K h s l ^ L ' Y T I C Z A . L S E R V I C E S L T D P.0. BOX 2219, 2045 MILLS RO. WEST, SIDNEY, B.C, CANADA813S8 TEL (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 03 p f o s _ S 1_ d i 2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 31-Aug-2005 10:03 Contract No.: 4191 Lab Sample ID: L7932-52 i M atrix: SERUM Sample Size: 1.00 Sample Receipt date: Extraction Date: Analysis Date: 01-Sep-2005 21-Sep-2005 23-Sep-2005 Time: 0:55:34 Initial Calibration Date: Instrument ID: LC Column ID: 22-Sep-2005 LC-MS/MS C18 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Sample Datafile: FC5G_181S055 Blank Data Filename: FC5GJ181S070 Cal. Ver. Data Filename: FC5G_181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION LIMIT UD UD UD D 72.9 D 1.51 D 0.739 UD UD UD D 12.5 D 87.6 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 RETENTION TIME 4.65 4.99 5.36 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 CONC. FOUND (ng) 12.2 12.9 13.2 10.3 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2.rts, S5 Approved by:. :/ivi C? R (%)2 RETENTION TIME 102 4.65 108 5.46 110 5.46 85.6 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D PO. BOX 2219, 2015 MIUS RD. WEST, SIDNEY, B.C., CANADAV8L 3S8 TEL (250) 655-5800 FAX (250) 655-58) 1 AXYS METHOD MLA-042 Rev 03 p f o s s i 012 Form 1A/2 ~~ PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 31-Aug-2005 10:32 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-53 i M atrix: SERUM Sample Size: 1.00 ; Sample Receipt date: 01-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 1:09:49 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_181S056 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G 181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD D 1.95 D 110 D 2.92 D 1.32 UD UD UD D 20.0 D 111 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.18 4.65 5.05 5.36 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG' D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2jds, S6 Approved by: CONC. FOUND (ng) 12.1 12.0 12.7 10.8 R (%)12 RETENTION TIM E 101 4.65 99.6 5.46 106 5.46 90.0 5.36 .QA/QC Chemist 11-10-05 cd-mm-yyyy A X Y S / X . r v J A L V T I O V L S E R V I C E S L T T D P.0. BOX 2219, 2045 MILLS HI. WEST, SIDNEY, 8.C., CANADA 81 358 TEl (250) 655-5800 FAX (250) 655-5811 AXYS METHOD MLA-042 Rev 03 2p f o s _ s i _ d i Form 1A/2 ~ PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 31-Aug-2005 10:30 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-54 i M atrix: SERUM Sample Size: 1.00 Sample Receipt date: 01-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 1:24:02 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_181S057 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G 181S048 CALVER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG1 CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 55.4 D 2.36 UD UD UD UD D 6.59 D 60.0 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.65 5.05 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2.x!s, S7 Approved by:. CONC. FOUND (ng) 11.8 15.0 13.4 10.1 R (%)2 RETENTION TIME 98.2 4.65 125 5.51 112 5.46 84.4 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219. 2045 MILLS ID. WEST, SIDNEY, B.C., CANADA V813S8IEI (250) 455-5800 FAX (250) 455-581) AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample C ollection: 08-Sep-2005 11:48 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 09-Sep-2005 Extraction Date: 21-Sep-2005 Analysis Date: 23-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Time: 1:38:15 Lab Sample ID: L7932-56 i Sample Size: 1.00 Initial Calibration Date: 22-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_181S058 Blank Data Filename: FC5G_181S070 Cal. Ver. Data Filename: FC5G 181S048 CALVER ID: PFC-LIN-055CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG1 CONC FOUND DETECTION LIMIT UD UD UD D 2.63 D 0.866 UD UD UD UD D 5.19 D 17.4 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 RETENTION TIME 4.65 4.99 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 2PFD1 2.xls. S8 Approved by: CONC. FOUND (ng) 12.9 17.0 14.1 11.5 R (%)2 RETENTION TIME 107 4.65 142 5.46 117 5.46 96.1 5.36 QA/QC Chemist 11-10-05 dd-m m -yyyy A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 221?, 2045 MILLS Ml. WEST, SIDNEY. B.C., CANADA V8L 3S8 TEL (250) <55-5800 FAX (250) 455-5811 p . 94 AXYS METHOD MLA-042 Rev 03 PF0S_S1 D12 Form 1A/2 " ' PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 12-Sep-2005 17:42 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-58 i M atrix: SERUM Sample Size: 1.00 Sample Receipt date: Extraction Date: 14-Sep-2005 21-Sep-2005 Initial Calibration Date: Instrument ID: 22-Sep-2005 LC-MS/MS Analysis Date: 23-Sep-2005 Time: 1:52:30 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5GJ81S059 Injection Volume (pL): 10,0 Blank Data Filename: FC5GJ81S070 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5GJ81S048 CALVER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0.639 UD 0.620 UD 0.628 D 7.35 0.618 . UD 0.670 UD 0.648 UD 0.641 UD 0.638 UD 0.635 D 1.54 0.638 D 10.5 0.645 UD 0.625 4.65 4.87 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1> U = not detected; D = dilution data (2) R (%) = Percent recovery 16982p f d i_2jcIs. S9 Approved by:_ CONC. FOUND (ng) 11.7 15.1 15.2 10.6 R (%)2 RETENTION TIME 97.8 4.65 126 5.46 127 5.46 88.0 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S y\r%J/XI Y T ICA1 S E R V I C E S L T D P.0. BOX2219, 2045Mills tD, WEST, SIDNEY,B.C., CANADAV8L3S8TEL(250) 55-5800FAX(250) 455-5811 m AXYS METHOD MLA-042 Rev 03 2p f o s _s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: 12-Sep-2005 17:46 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: Matrix: 4191 SERUM Lab Sample ID: Sample Size: L7932-59 i 1.00 Sample Receipt date: 14-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 2:06:42 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_181S060 Injection Volume (pL): 10.0 Blank Data Filename: FC5GJ81S070 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG1 CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD D 0.962 D 68.3 D 0.957 UD UD UD UD D 13.8 D 50.1 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.14 4.65 4.99 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2.*ls, S10 Approved by:_ CONC. FOUND (ng) 11.8 15.0 14.1 12.7 R (%)2 RETENTION tm e 98.4 4.65 125 5.46 117 5.46 106 5.36 QA/QC Chemist 11-1005 dd-mm-yyyy A X Y S > \ r v J > M _ V X I C I A . I _ S E R V I C E S L T D P.o. BOX 2219, 2045 MILIS RD. WEST, SIDNEY, B.C, CANA0 V8L 3S8 TEL (250) <55-5800 FAX (250) <55-5811 AXYS METHOD MLA-042 Rev 03 pfos_s i_d i2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection: CLIENT ID: 13-Sep-2005 18:33 Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: SERUM Sample Receipt date: 15-Sep-2005 Extraction Date: Analysis Date: 21-Sep-2005 23-Sep-2005 Time: 2:20:55 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Lab Sample ID: L7932-61 i Sample Size: 1.00 mL Initial Calibration Date: 22-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_181S061 Blank Data Filename: FC5G_181S070 Cal. Ver. Data Filename: FC5G 181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 69.0 D 1.05 D 0.835 UD UD UD D 15.7 D 77.2 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.65 4.99 5.36 4.87 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG 1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected: D = dilution data (2) R (%) = Percent recovery 16982PF01 2.xis, s i 1 Approved b y : CONC. FOUND (ng) 12.1 14.3 14.6 11.0 , _^ R (%)2 RETENTION TIME 101 4.65 119 5.46 122 5.46 91.6 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy 10 A X Y S yAr-vl/VLYriOKI S E R V I C E S L T D P.0.BOX221?,2045MJLISHI.WEST,SIOBET,B.C.,CANADAV8L3S8TEC(250)<55-5800MX(250)<55-58)1 p. 97 AXYS METHOD MLA-042 Rev 03 pfos_s i_d i2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection: 15-Sep-2005 11:03 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 16-Sep-2005 Extraction Date: 21-Sep-2005 Analysis Date: 23-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Time: 2:35:09 Lab Sample ID: L7932-63 i Sample Size: 1.00 Initial Calibration Date: 22-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_181S062 Blank Data Filename: FC5GJ81S70 Cal. Ver. Data Filename: FC5G 181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB CONC FLAG1 FOUND DETECTION LIMIT UD UD D 2.16 D 100 D 1.32 UD UD UD UD D 58.6 D 131 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 RETENTION TIME 4.18 4.65 4.99 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected: D = dilution data (2) R (%) = Percent recovery i6982PFDi_2.xis, S12 Approved by:. CONC. FOUND (ng) 9.60 9.83 9.52 8.67 R (%)2 RETENTION T IM E 80.0 4.65 81.9 5.46 79.3 5.46 72.2 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy [(&A X Y S / M V J A I Y T I O V L S E R V I C F S L T D P.0. BOX 2219, 2045 MILS RO. WIST, SIDNEY, B.C., CANADA Y8L 3S8 TEI (250) 655-5800 FAX (250) 655-5811 V AXYS METHOD MLA-042 Rev 03 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 1 5-Sep-2005 11:05 Contract No.: 4191 M atrix: SERUM Sample Receipt date: 16-Sep-2005 Extraction Date: 21-Sep-2005 Analysis Date: 23-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 10.0 Dilution Factor: 3 Concentration Units : ng/mL Time: 2:49:23 Lab Sample ID: L7932-64 i Sample Size: 1.00 Initial Calibration Date: 22-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_181S063 Blank Data Filename: FC5G_181S070 Cal. Ver. Data Filename: FC5G 181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD UD UD D 86.8 D 1.71 UD UD UD UD D 34.5 D 125 UD 0.639 0.620 0.628 0.618 0.670 0.648 0.641 0.638 0.635 0.638 0.645 0.625 4.65 4.99 4.80 5.46 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG1 D D D D SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16982PFD1_2jds, S13 Approved by: CONC. FOUND (ng) 12.7 16.2 14.0 13.6 R (%)2 RETENTION TIME 106 4.65 135 5.46 116 5.46 113 5.36 QA/QC Chemist 11-10-05 dd*mm-yyyy )][CA X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. BOX 2219. 2045 MOIS RD. WEST, SIDNEY B.C., CANADAV8t 3S8 TEL (250) 55-S800 FAX (250) 655-5811 p. 99 AXYS METHOD MLA-042 Rev 02 pfos_s i_012 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Matrix: Sample Receipt Date: 19-Jul-2005 Extraction Date: 04-Aug-2005 Analysis Date: Extract Volume (mL): 05-Aug-2005 2 Time: 22:43:43 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Sample Collection: N /A Lab Sample ID: Sample Size: Initial Calibration Date: Instrument ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename: CAL VER ID: L7932-12 1.00 mL 05-Aug-2005 LC-MS/MS C18, Zorbax XDB FC5G_131S047 FC5G_131S024 FC5G_131S037 PFC-LIN-039CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG ' CONC FOUND DETECTION LIMIT U 0.638 U 0.620 u 0.251 u 0.247 u 0.268 u 0.259 u 0.256 u 0.255 u 0.254 u 0.255 u 0.258 u 0.250 RETENTIOI TIME LABELED COMPOUND 13C-PFOA 13C-PFDA LAB FLAG ' SPIKE CONC. (ng) 12.0 12.0 CONC. FOUND (ng) 9.16 9.10 R (%)2 RETENTION TIME 76.3 75.8 4.70 5.34 (1) U = not detected (2) R (% ) = Percent recovery l6535PFD2_2.xls. S9 A pproved by: QA/QC Chemist 11-10-2005 dd-mm-yyyy A X Y S A N A L Y T I C A L S E R .N / IC T E S L T D P.0. BO X 2 2 1 ? , 20 45 M IU S CD. WEST, SIONEY, B .C ., CANADA V8 L 3SS T E I (2 5 0 ) i 55-5800 FA X (2 50 ) 45 5 -5 8 11 P- 100 AXYS METHOD MLA-042 Rev 02 PF0S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: N/A Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 M atrix: N/A Sample Receipt date: 10-Aug-2005 Extraction Date: 29-Aug-2005 Analysis Date: 12-Sep-2005 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Time: 19:33:09 Lab Sample ID: L7932-18Y4 Sample Size: 1.00 mL Initial Calibration Date: 12-Sep-2005 Instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_167S036 Blank Data Filename: FC5GJ67S031 Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA LAB FLAG' CONC FOUND DETECTION LIMIT U 0.256 u 0.248 u 0.251 u 0.247 u 0.268 u 0.259 u 0.257 u 0.255 u 2.54 u 2.55 u 0.258 u 0.250 RETENTION TIME LABELED COMPOUND 1 3 C 2 -P F O A 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA (1) U = not detected (2) R (%) = Percent recovery LAB FLAG' SPIKE CONC. (ng) 12.0 12.0 1Z0 12.0 16755PF 01_2.xls. S7 Approved by: CONC. FOUND (ng) 8.36 8.61 9.47 10.2 R (% )12 R E T E N T IO N TIM E 69.7 4.70 71.8 5.56 79.0 5.56 85.0 5.36 QA/QC Chemist 11-10-05 dd-mm-yyyy A X Y S /`\IS'J-AJ_YTICA1_ S E R V I C E S L T D P.0. BOX2219, 20 MIUSD. WEST,SIDNEY,B.C., CANADAVit 3S8TEI (250) 855-5800FAX(250) 855-5811 I DO p. 101 AXYS METHOD MLA-042 Rev 03 pfos_s i _D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection: CLIENT ID: N/A Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Matrix: N/A Sample Receipt date: 31-Aug-2005 Extraction Date: Analysis Date: 06-Sep-2005 13-Sep-2005 Time: 11:01:03 Extract Volume (mL): 2 Injection Volume (pL): 30.0 Dilution Factor: N/A Concentration Units : ng/mL Lab Sample ID: L7932-50 Y2 Sample Size: 1.00 Initial Calibration Date: 13-Sep-2005 instrument ID: LC-MS/MS LC Column ID: C18 Sample Datafile: FC5G_168S027 Blank Data Filename: FC5G_168S015 Cal. Ver. Data Filename: CAL VER ID: FC5G 168S010 PFC-LIN-048CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION UMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U 0.256 u 0.248 u 0.251 u 0.247 u 0.268 u 0.259 u 0.257 u 0.255 u 0.254 u 0.255 u 0.258 u 0.250 LABELED COMPOUND 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA LAB FLAG 1 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected (2) R {% ) = Percent recovery 16814PFD3_2.xIs, S14 A pproved by: CONC. FOUND (ng) 4.15 5.94 4.52 10.7 R (%)2 RETENTION TIME 34.6 49.5 37.6 89.0 4.65 5.51 5.51 5.36 QA/QC Chemist 11-10-2005 dd-mm-yyyy [WA X Y S /\rvly<\LYTIOM- S E R V I C E S L T D RO. BOX 2219, 2 0 MILLS BO. WEST. SIDNEY. B.C., UNADA V8L 3S8 TEL (250) 455-5800 FAX (250) 455-5811 I0l P- 102 AXYS METHOD MLA-042 Rev 03 2p f o s _ s i _ d i Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID: Sample Collection: N/A Lab Name: AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID: L7932-65 i Matrix: N/A Sample Size: 1.00 mL Sample Receipt date: 16-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/MS Analysis Date: 23-Sep-2005 Time: 3:03:37 LC Column ID: C18 Extract Volume (mL): 2 Sample Datafile: FC5G_181S064 Injection Volume (pL): 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor: Concentration Units : 3 ng/mL Cal. Ver. Data Filename: FC5G_181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB FLAG ' CONC FOUND DETECTION LIMIT RETENTION TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0.639 UD 0.620 UD 0.628 UD 0.618 UD 0.670 UD 0.648 UD 0.641 UD 0.638 UD 0.635 UD 0.638 UD 0.645 UD 0.625 LABELED COMPOUND 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA LAB FLAG' D D D D12 SPIKE CONC. (ng) 12.0 12.0 12.0 12.0 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery CONC. FOUND ("9) 12.8 13.6 14.5 15.2 R(%)J RETENTION TIME 107 4.65 114 5.46 121 5.46 127 5.36 16982Pfdi_2.xIs, S14 Approved by: "<g_ -- QA/QC Chemist 11-10-05 dd-mm-yyyy 10 A X Y S XYM>\LYTiCZ/YL S E R V I C E S L T D P.O. BOX 2219, 2045 M ills BO. WEST, SIDNEY, 8.C., CANADA V8L 3S8 TEL (250) 55-5800 FAX (250) 55-5811 101