Document nNdRVjL5aN1K2pg5roQvj46bm

NORTHERN KENTUCKY OFFICE TAFT, STETTINIUS & HOLLISTER LLP -A R a OR 6 p.1 ~~56",v CLEVELAND, OHIO OFFICE 1717 SUITE 340 3500 BP TOWER 425 WALNUT STREET, SUITE 1800 COVINGTON, KIEVNT4U1C0K 1Y 1-4704 606-331-283 6 200 PUBLIC SQUARE CLEVELAND, OHIO 44114-2302 i~ PP 513-381-2838 216-241-2838 CINCINNATI, OHIO 45202-3957 FAX : 513-381-6613 FAX: 216-241-3707 COLUMBUS, OHIO OFFIC E DAYTON, OHIO OFFICE 513-381-2838 21 EAST STATE STREET 110S NU OR IT THEMA 9I0 N 0 STC RE O ET LF U AM X : 5B 13-38U 1-02S 05 , OHIO 43215-4221 DAYTON, OHIO 45402-1786 937-228-2838 www FAX: 937-228-2816 .taftlaw.com FAX614-221-2838 :614-221-2007 ROBERT A . BILOTT (513) 357-963 8 bilott@taftlaw .com October 20, 2005 FEDERAL EXPRES S Dr. Charles M . Auer Mary Dominiak USEPA USEPA 1201 Constitution Avenue, N .W . 1201 Constitution Avenue, N.W. Room 3166A Room 4410 S Washington, DC 20004 Washington, DC 20004 Jennifer Seed James Kelly, M.S. USEPA Health Assessor 1201 Constitution Avenue, N .W . Site Assessment and Consultation Unit Room 6334A Environmental Health Division Washington, DC 20004 Minnesota Department of Healt h 121 E. 7th Place, Suite 360 St. Paul, MN 55164 0 David Douglas Donald Kriens Remediation Division Industrial Division ....:. ~ ~-, Superfund & Emergency Response Section Land & Water Quality Section Minnesota Pollution Control Agency Minnesota Pollution Control Agenc y 520 Lafayette Road North 520 Lafayette Road North 90 St. Paul, MN 55155 St. Paul, MN 55155 0 co Re : Perfluorochemical Residential Exposure Data For Washington Countv Minnesot a 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 . Aue r 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 .1 p. 3 Dr . Charles M. Auer Jennifer Seed Mary Dominiak James 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) )2~ . 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 . Z/ 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 . Aue r Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 4 CHART A - OAKDALE CITY WATER CUSTOMERS YEARS ON PFOA PFOS TOTAL SEX AGE WATER (nnb)/DuL. (ppb)/Dup . PFCs(ppb)* M 41-50 N/A 121 .0 109 .0 267 .12 F 51-60 >30 117 .0 91 .8 240 .06 M >70 >30 105 .0 113 .0 241 .45 M 51-60 20-30 104 .0/103 .0 70 .3/72.7 192 .44/195.54 M 61-70 20-30 100 .00 131 .0 293 .08 F 51-60 20-30 96 .1 67 .8 180 .2 F 41-50 <10 95 .1/89 .1 85 .9/79.8 200.71/186 .15 M 51-60 20-30 86.8 125 .0 248.01 M >70 N/A 82 .3 118 .0 221 .79 F 61-70 20-30 80 .5 163 .0 212 .40 M >70 >30 78 .6 112 .0 210 .63 F 41-50 N/A 77 .5 78 .4 178 .51 F 51-60 20-30 74 .9 61 .1 152 .72 M 31-40 10-20 74 .6 91 .0 182 .36 F >70 >30 69 .3 102 .0 191 .84 F 41-50 N/A 69 .0 77.2 163 .79 M <18 <10 68 .3 50 .1 134 .12 M 41-50 10-20 63 .3 76 .7 158 .88 W0537662 .1 p. 5 Dr. Charles M . Aue r Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 5 YEARS ON PFOA PFOS TOTAL SEX AGE WATER (ppb)/DuP. (ppb )/DWL. PFCs(ppb)* F 41-50 <10 63 .3 73 .1 150 .11 F 61-70 N/A 59 .9 71 .0 145 .61 F 61-70 >30 58 .7 73 .4 149 .48 M 61-70 <10 58 .7 61 .7 134 .64 F 61-70 20-30 58 .3 68 .1 154 .95 F 41-50 20-30 57 .8 70 .4 146 .46 F 31-40 10-20 48 .4 71 .9 132 .83 M 51-60 10-20 44 .6 60 .4 115 .40 M 41-50 <10 44 .1 55 .2 114 .29 M 18-30 10-20 43 .5 54.4 107 .12 M <18 10-20 42 .4 51 .1 107 .84 M 61-70 20-30 39 .8 46 .5 104 .37 F 18-30 20-30 38 .8 47 .6 96 .33 M 51-60 >30 37 .1 51 .1 102 .01 F 51-60 10-20 33 .2 59 .5 105 .24 F 41-50 <10 32 .7 41 .5 89.66 M 41-50 10-20 32 .1 57 .6 103 .35 F <10 <10 30 .7 56 .8 99 .11 F <10 <10 27 .5 62 .0 98 .63 W0537662 .1 p. 6 Dr . Charles M . Auer Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 6 YEARS ON PFOA SEX AGE WATER (ppb)/Dup . PFOS TOTAL (ppb)/Dup . PFCs(anb )* 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 availabl e *Total of detected levels of PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFBS, PFHxS, PFOS, and PFOSA in the blood sampl e 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 YEARS PFOA PFOS PPB PPB TOTAL ON (ppb)/ (ppb) PFOA IN PFOS IN PFCs SEX AGE WATER Dup . /Dup . WATER WATER (ppbl * 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 . Aue r Jennifer Seed Mary Dominiak James Kelly David Douglas Donald Kriens October 20, 2005 Page 8 YEARS PFOA PFOS PPB PPB TOTAL ON (ppb)/ (ppb) PFOA IN PFOS IN PFCs SEX AGE WATER Dup . /Dup . WATER WATER (ppb)* M 61-70 >30 6 .1 43 .7 N/A N/A 54 .19 F 51-60 10-20 5 .92 29.5 ND ND 41.26 M 51-60 N/A 5.35 20.4 N/A N/A 29 .02 F 41-50 N/A 3 .14 11 .2 N/A N/A 16 .29 F 18-30 <10 2.63 17.4 N/A N/A 26 .09 F 61-70 >30 2 .4 12.0 N/A N/A 17 .91 N/A=data not availabl e ND= not detected above repo rted detection limits *Total of detected levels of PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFBS, PFHxS, PFOS, and PFOSA in the blood sample ?ery ly yours RAB/mdm Enclosure s obert A. Bilo tt L W0537662 .1 p. 9 Dr . Charles M . Aue r 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 encls.) Stephen J . Randall, Esq . (w/o encls .) Rhon E. Jones, Esq . (w/o encls.) J . Mark Englehart, Esq . (w/o encls .) David B . Byrne III, Esq . (w/o encls .) R . Edison Hill, Esq . (w/o encls .) Larry A . Winter, Esq . (w/o encls .) Gerald J . Rapien, Esq . (w/o encls .) W0537662 .1 zg>g 10 s, . ~ q c uY co Co W) qo r c K ~ ~ Z o 0 w 0 0 = N O O Z Z N O V Z Z r o z z U) o z q a co to > H O Z Z O C Q N M w 0 U- 9 '^ O m Q V! a "; a z z z 0 0 N 41 Q z Z o Z Q R p = = C o IZ & O m q C, a CD v1 b r~. m g ! N C; Z 0 C; N = Q ^ c q ~ a a 0 LL ,0 0 h to co N p Z Z p z A Q n o m MO cs M o Z Z O Z E ~ ~ m ~ 00 m E C a L 0 G CD 40 N os A; >h va g~~a CO E 0 to l0 a 7 0 r~ ~ 3 J }( W j5 c m a m fi N S a a m m' z c~ ro co ~ _~ g m E ~ b m m~ o m a~ Sa3 c a n w cc 0 yp 0 O Z vm o O~ Z Zn i i~ p . 11 3MA00402756 g Ai 2 Analytical Results From Oakdale Combined Effluent Discharge (ug/L) Date PFOA PFOS FOSA PFBS PFHS 8/11/04 66.1 30 .1 ND 4 .0 7 .6 9/17/04 53 .1 28 .2 ND 8 .8 8 . 1 Analytical Results From Woodbury Pumpout System ( ug/L) PFOA PFOS FOSA PFBS PFH S Result 2 .2 0.8 ND 2 .4 7 .8 Du 1 2 .4 0_9 ND 2 .6 8 .1 IF ~Gc.GILP df /4~ ~C ryn ~~n f'~WIfGG~+~l~ ~~ 4' 41A -F Y_!` p .13 3MA00402704 i3 Re - Fwd- Other FCs (in addition to F-8) In Washington Closed Landfill p. 1 4 Page 1 F rom : Virginia Yingling To: James Kelly; Paul Swedenborg Date: 3I912005 12:14 :10 P M Subject: Re : Fwd: Other FCs (in addition to F-8) in Washington Closed Landfill Hi Paul : Jim mentioned that you were looking at C4 and C6 acids in samples to test the standards and me thods . 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 interes ting are : Sample No . Sample Location 208450 Larson (collected Monday) W0020112 Eldredge (collected Monday) 82W01047 Lindblom (collected Tuesday) 82W01038 Conlin (this one is being collected today ) 413551 Loetscher ( this one is being collected today) Thanks . Ginny Ginny Yingfmg virginia.yingling @ heafth .state.mn.us ph - 651-215-091 7 fax - 651-215-0 97 5 >>> James Kelly 03/0910511 :42 AM >> > FYI . . . .3M will supply some standards, and it looks l ike the lab has found low levels of C4 and C6 acids in some Oakdale samples. Jim James Kelly, M .S . Health Assessor Site Assessment & Consultation Unit Environmental Health Division Minnesota Dept. of Health (651) 215-091 3 lames. kelly fthea fth . state . mn, u s >>> 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 pu rity and by-products would be useful as well . Have them please ship the chemicals directly to me. My address should be in the signature below . They are welcome to contact me if they have questions. FYI . We have been screening samples for PFBA, PFPeA, PFHxA, and PFHpA We are seeing the C4 and C6 in some of the Oakdale samples at low levels . Th anks again . Paul. Paul Swedenborg (Organic Unit Supervisor) MN Department of Health Public Heal th Laboratory Division t4 p . 15 lames Kelly - RE : Other FCs in addition to F-8 in W ton ClosedLand6N EM 1 1 From: "Oliaei. Fard'+n" <Fardin .Oliaei@state.mn .us> To: "Oliaei, Fardin" <Fardin .Otiaei@state .mn .us>, "Helen Goeden" <HeIen.GoedenQstate.mn.us>, <Fardin .Oliaei cQstate .mn .us>. <James.Kelly@state.mn .us>, <Laura .Solem@state .mn. us > Date: 2/28/2005 2:35 :07 PM Subject: RE : Other FCs (in addition to F-8) in Washington ClosedLandfrll Helen , I am not sure why 1 can not insert the attached memo. Here, l just copied the entire memo and sending it to you again . Please let me know if you will receive it. If not 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 OGaei Date : February 25, 200 5 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 (G4) perfluorobutane sulfonate (PFBS) compound, and serve as substitutes for the 8 carbon chain pettiuorinated 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 the environment in the areas of partitioning behavior. degradation, chronic toxicity an d b'paocumulation, 3M conducted some 40 toxicity and other tests to demonstrate the relative non-toxicity of these PFBS-based fluorochemicals . 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 the environment since they are relatively non-biodegradable, and it is anticipated that concentrations of PFBS will 'accumulate" in blood of humans. Although not bioaccumutafive, the PFBS levels in blood are expected in part due to the ubiquitous nature of the PFBS based fluorochemical products and also likely due to a relatively higher volatility versus PFOS. PFOA, etc. There is some information that suggests that the half life of shorter perfluorinated compounds i s longer than C-8 based compounds in humans_ Although a very brief review of tests completed by 3M appears to demonstrate the relativ e non-toxicity of PFBS, the kxig term effects of these new fluonochemicals are of course unknown . Because of the heightened sensitivity and awareness of the toxicities associated with PFOS, PFOA, and related higher chain fluorochemicat compounds it may be prudent to begin some evaluation of the new C-4 PFB S chemicals, in order to respond in an informed fashion to inquiries . In part this also appears reasonable simply because PFBS is a short chain James Ke - RE Other FCs (in addition to F-8) p. 1 6 Wa on ClosedLandfU P 2 halogenated organic, and nume rous other sho rt chain halogenated compounds have known problems. It seems probable that the public or others may ask about the safety of the new C-4 based fiuorochemicals. Therefore, at some point we may want to consider the folbwing potential evaluations: 1 . Conduct a literature review of all studies conducted for PFBS regarding toxicity, degradation, etc, in order to p rovide informed answers to any ques tions on this issue that may arise . 2. Evaluate the disposition of PFBS regarding air, water, and solid waste media at the 3M Cottage Grove plant Disc uss whether monitoring should be required by 3M for PFBS and related C-4 FC compounds in the water discharge, sludges generated, and air emissions . 3. Determine whether any additional studies should be required of 3M regarding aquat ic toxicity. Are the present studies adequate con cerning poten tially affe cted species in the receiving water. Involve wate r 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, ar e the studies completed adequate to assess long term impacts, if any . 6 . Is there adequate informa tion developed to assess the distribution of PFBS to the environment and potential impacts, if any. Is there adequate information regarding breakdown products and poten tial impacts, if any . (As a separate note we found PFBS at high concentrations in the pumpout water and standing water at the Washington County Landfill. ) These evaluations w ould primarily be conducted to assure that we may answer questions related to PFBS in the Minnesota envi ronment, and do not necessarily presume a problem wi th PFBS. However, I believe it would be appropriate to be prepared to assure that studies to date are adequate for envi ronmental protection, and so that we may respond to any inquiries in an informed fashion . --Original MessageFrom : OGaei, Fardin Sent Monday, February 28, 2005 2:28 PM To : 'Helen Goeden; 'Faniin .Oliaei@state .mn .us; 'James.[Celly@state.mn .us; 'l.aura .Solem @state.mn.us' Cc: 'Lar ry Gust' ; 'Rita Messing'; 'Cart.Herbrandson(Qstate.mn .us'; 'DougIas .Day@state .mn.us' ; ` H i1ary.Carpenter@state .mn.us'; 'Ingrid_Verhagen@state.mn.us ; 'Joseph.JulikCstafie.mn.us' ; 'Paui.Slwedenborg @stabe_mn.us' Subject RE: Other FCs (in addition to F-8) in Washington ClosedLandfid Hi Helen , I am sorry for not attaching the memo. Here is a copy of the memo. Please feet free to revise and complement this memo as you see it best fit with your position at the MDH on this is sues . Th anks for your time , 1'6 James Kelly -RE : Other FCs bn addition to F-8 in Washi ton ClosedLandfat Fardi n --Original MessageFrom : Helen Goeden [maitto:Hefen.Goeden@slate.mn .usI Sent: Monday, February 28 . 2005 2:09 PM To : Fardin.Otiaei@state.mn.us; Helen .Goeden @state.mn .us ; James .KeBy@~state .mn .us ; LauraSolen>@state .mn.us Cc: Lar ry Gust; Rita Messing ; Carl .Herbrandson@state.mn.us; Douglas .Day@state.mn.us; Hi11ary.Carpenter@state .mn .us; Ingrid.VerhagenQstafie.rnn.us; Joseph.Julik@state.mn.us; Paul . Swedenborg@slate .mn .u s Subject RE Other FCs ( in addition to F-8) in Washington CtosedLand filt Fardin , Jim and I will be coordinating a response from our units to your questions. The copy of your memo to Paul Hoff was not attached to the e-mail_ Could you forward a copy of the memo to us? Thanks. Helen Helen Goeden, Ph .D. Minnesota Department of Health P .O . Box 64975 St Paul, MN 55164-0975 (651)215-0874 helen.goeden@health .state-mn.us >>> "O6aei, Fardin" <Faradin.OUaei@state_mn.us> 02/28/051 :04 PM > > Dear Helen . Laura, and Jim . > > Now that I submitted a copy of the following preliminary data for 3M > to review, I should also share them with you for your review- The > following data are on the levels of FCs in the Washington County's > contaminated well (V2), clean, reference well (J), and two surface > water samples (created with the V2 being sprayed over the surface area > of the dosed landfill). > > I am concern. Specially. with the high con ce ntrations of G4 > compounds. Let me know what you think . Based on the ongoing EPA > SAB panel dim=ion on cancer classification for PFOA, are we going > to revise the MOH HRV values for PFOS/PFOS? Is there sufficient data > to develop toxicity values for C-4 . C-5, and C-6 Fluorinate d > compounds? > > I also attac hed a copy of a memo that I put together far my > supervisor, Paul Hoff per his request on this issue . In my view, this > memo needs to be expanded, suggesting a comprehensive enviro nmental > monitoring (conducted by MPCA), and bio monitoring (conducted by MDH) > for a period of five year (financially supported by 3M) . > ~7 p . 1 7 Pap 3 James Ke - RE' Other FCs in addition to F-8 'an Wash jNn Ctosedlandfi ll > File: Paul-PFBS .doc > The following are the prelimina ry data on c ontaminated well (V2), > clean and reference well (J), and two samples of the surface water > (where the V2 is being sprayed over the dosed landfill) . I need to > explain more about these data. > > CLIENT 10 Wash-CL (surface water#1) Wash-CL (surface water#2) > Wash-CL (clean Well J) Wash-CL(polluted Well V2 ) > > UNITS ng/mL ng/mL > nglmL ng/m L > PFBA 371 352 > <0.190 1170 (F-4 ) > (this high conc . Is my concern, and it is a substitute for F-8!) > PFPeA 7 .98 > <0.0205 43.1 (F-5) > 6.89 PFHxA 3.36 > <0.0037 15.6 (F-6) > 3.28 PFHpA 0 .582 0 .659 > <0.0044 2.38 (F-7) > PFOA 10 .9 15.2 > <0.0027 41 .6 (F-8) > PFNA 0 .009 > 0_001 0 .01 2 0 . 006 > PFDA <0 .0156 0.027 > <0 .0015 0.006 > PFUnA <0.0068 > <0.0009 <0 .0039 > 0.016 PFDoA <0.0142 0.016 > 0.002 <0 .0032 > PFTA <0.0202 <0.0103 > <0.0005 <0 .0020 > PFBS <0 .333 <0 .252 > <0.0201 1 .3 1 > PFHxS <0 .422 > <0.0257 1_77 (F-6 ) > PFOS 1 .35 > <0.0030 2.69(F-8) >(oNy PFOA and PFOS are being reported by MDH) > <0.300 1 .67 > Thanks for your ti7ne, Fardin > > Fardin Obaei, Ph-D . > Research Scientist I N > Emerging Contaminants Coordirkitor > Minnesota Pollution Control Agency (MPCA) > > E-mail : faniin.oiiaei ftca .state .mn .us > Phone: (651) 296-796 7 > 18 p . 18 Page 4 J James - RE: Other FCs in addition to F In V1/ash Closedt Im p .19 Page 51 > > <<File : Paul-PFt3S.doc CC: "Larry Gust" <Lany.Gust(dlstate.mn.us>, "Rita Messing' <Rita.Messing@state .mn .us>, <Carl .Hertxandsontbstate.mn_us>, <Douglas.lray cGDstate.mn .us>, <Hdlary.Carpenter@state.mn.us>, <Ingrid.Verhagen @state.mn .us>, < loseph.Jufdc@state.mn.us>, <Paul .Swedenborg @state.mn .us> Groundwater Monitoring Network around Washington Cou Landfill %AK* r?~yi V~ Ir e GW* ~a ~3 B3 ~ p . 20 ~-- Dv wca Eo s r~ ~r~ I~t' tt YV ~ Jr ~~. ; 14,. ~ ~~3. ~3 PF~~,~yl~ ~lY Monitoring Wells (s in street s Z <0 Landfill outlined in red 900 Meters 40 ~ n 91 , , .> p m v~ OnCQ mZO=2m m -n23 r fp ytnD6 DD>DDD f m D ~~ ~~ v C 'D iaiw o~o r p oo(w,,10v ~C O r A ,~SOooooo+o~ ~ NOOON Q 0~i~7 Cs~ IV+ voo'n ~3 +~pr~ 2S ooSooooooooog g'pv ~ o 43 0 N ++ O O S O O j N+++~ E+D (~~) V~~ tl J+ N 0 N kD C1 in Or33r M T6 9 00000oooooFiso ~ op O O O O ~ + S SO q Os 40/ fOd V OJ V N !-, 3 p WO O 0000000ooooow ~ o~~m~ g9 P5,~~ So ~ ~ Q rn tA V JGa~J. W sb~~p f11 A OOO O # o OOOOOa~+pONQ N~p A pOU V Op .1~ C~bp Lt e 0000000o o o o oop ~~$ 88~88~~0 3~ $~~ , e Z : 22 p . 23 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 ,23 p . 24 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 PFO S 34 p . 25 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 p . 26 Municipal Well s Oakdale December 22, 2005 Sampling Results (ug/L) PFOA MD H MDH Well Number Exygen Exygen Exygen Me d Measured MDH asu e Result Duplicate Average Value 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 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 N C NC 9 0 .727 0.772 0.750 0 .7781 N A Well Number PFOS MDH Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average MVeaaluseured Value Average Duplicat e 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 (pa rts 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) of 0 .050 ug/L (50 pa rts per trillion) . For MDH data : Repo rt level is 0 .5 ppb for PFOS and 1 .0 ppb for PFOA . Where data is repo rted at less than these values, it represents Measured Values . 26 p . 27 Oakdale Janua ry 25, 2005 Sampling Results (ug/L) PFOA MDH Well Number Exygen Exygen Exygen MDH Me asured MDH Result Duplicate Average Measured Value Average Value Duplicat e 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 7 8 9 0.821 0.736 0 .779 0 .799 NA NC 0 .285 0 .274 0.280 0 .211 0.235 0 .223 0 .668 0 .647 0 .658 0 .628 NA NC 0 .825 0 .892 0.859 0 .737 NA NC Well Number PFOS MDH Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average MeVasaulureed Value Average Duplicat e 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 (pa rts 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) of 0 .050 ug/L ( 50 parts per tri llion) . For MDH data : Repo rt level is 0.5 ppb for PFOS and 1 .0 ppb for PFOA . Where data is repo rt ed at less than these values, it represents Measured Values . A7 p . 28 Oakdale February 28, 2005 Sampling Results (ug/L ) PFOA Well Number MD H MDH Exygen Exygen Exygen Measured Measured MDH Result Duplicate Average Value Value Average Duplicate 1 0.0892 0 .0852 0 .0872 ND NA NC 2 0 .0807 0 .0871 0 .0839 ND NA NC 3 ND ND ND ND NA NC 5 7 8 0.714 0.761 0.738 0 .693 0.727 0 .710 0.274 0 .305 0.290 0 .214 NA NC 0.523 0.503 0 .513 0.423 NA NC 9 NS NS NS NS NS NC Oakdal e Public Works 0 Bldg . Lunc h .687 0.709 0 .698 0 .624 NA NC Room Sink Well Number PFOS MDH Exygen Exygen Exygen MDH Measured MDH 1 Result Duplicate Average Measured Value Average Value Duplicate 0.0516 0 .0541 0.0529 ND NA NC 2 NQ NQ NQ ND NA NC 3 ND ND ND ND NA NC 5 0.889 0.968 0 .929 1 .054 1 .004 1 .029 7 0.238 0.273 0 .256 0 .242 NA NC 8 0.687 0.662 0 .675 0 .693 NA NC 9 NS NS NS NS NS NS Oakdal e Public Works 0 Bldg . Lunc h .872 0.949 0.911 0 .947 NA NC Room Sin k 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) of 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 . .2 8 p . 29 Oakdale March 29, 2005 Sampling Results (ug/L ) PFOA MDH Well Number Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average Measured Value Average Value Duplicat e 1 0.0887 0 .0939 0 .0913 ND NA NC 2 0 .0823 0 .0817 0.0820 ND NA NC 3 ND ND ND ND NA NC 5 0.779 0 .710 0.745 0 .5281 NA NC 7 NS NS NS NS NS NS 8 0.503 0.457 0 .480 ND NA NC 9 0 .813 0.763 0.788 0 .8650 0.7575 0 .8113 Well Number PFOS 1 MDH Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average Measured Value Averag e Value Duplicat e 0 .0619 0 .0609 0 .0614 ND NA NC 2 NQ NQ NC ND NA NC 3 ND ND ND ND NA NC 5 1 .14 0 .941 1 .04 0 .9007 NA NC 7 NS NS NS NS NS NS 8 0 .704 0 .551 0 .628 0 .8500 NA NC 9 0 .58 0 .502 0 .541 0 .7147 0 .5727 0 .6437 All results in ug/L (pa rts 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 quanti fiable = Measured at concentration between 0 .025 ug/L & the Limit of Quantitation (LOQ) of 0 .050 ug/L (50 pa rts 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 . 29 ~' ` ~,,,,,~ p . 30 Oakdale April 2005 Sampling Results (ug/L) PFOA MD H Well Number Exygen Exygen Exygen MDH Me asured MDH Result Duplicate Average Measured Value Average Value Duplicat e 1 ND NS NC * * * 2 ND NS NC * * * 3 ND NS NC * * * 5 0.528 NS NC * * * 7 NS NS NC * * * 8 ND NS NC * * * 9 0.865 0 .758 0 .812 * * * Well Number PFOS I 2 MDH Exygen Exygen Exygen MDH Measured MDH Result Dup licate Average MVeaaluseured Value Averag e Duplicat e ND NS NC * * * 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 ( part s 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 pa rts per trillion) . NQ - Not quanti fi able = Measured at concentration between 0 .025 ug/L & the Limit of Quantitation ( LOQ) of 0 .050 ug/L (50 pa rts per trillion) . For MDH data : Report level is 0 .5 ppb for PFOS and 1 .0 ppb for PFOA . Where data is report ed at less than these values, it represents Measured Values . 30 p .31 Oakdale May 18, 2005 Sampling Results (ug/L ) PFOA MDH Well Number Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average Measured Value Average Value Duplicate 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 NA NA NA NS NS NS 7 NA NA NA 0 .3184 NA NC 8 NA NA NA 0 .5594 0.5195 0 .5395 9 NA NA NA 0.7740 NA NC Well Number PFOS MDH Exygen Exygen Exygen MDH Measured MDH Result Duplicate Average Measured Value Value Averag e Duplicat e I NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 NA NA NA NS NS NS 7 NA NA NA ND NA NC 8 NA NA NA 0 .7409 0 .6620 0 .7015 9 NA NA NA 0 .6539 NA NC All results in ug/L (pa rts 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) of 0 .050 ug/L (50 pa rt s per trillion) . For MDH data : Repo rt level is 0 .5 ppb for PFOS and 1 .0 ppb for PFOA . Where data is repo rt ed at less than these values, it represents Measured Values . 31 p . 32 Oakdale June 16, 2005 Sampling Results (ug/L ) PFOA Well Number 3M 3M Env 3M Env MDH MD H E Lan b v LaM b Le ab asu Merase ured d MDH Duplicate Average Value Value Average Result Duplicate 1 NA NA NA ND NA NC 2 NA NA NA ND NA NC 3 NA NA NA ND NA NC 5 0.887 0.948 0 .918 0 .9195 NA NC 7 NA NA NA 0.3057 NA NC 8 0 .472 0 .506 0 .489 0 .5390 NA NC 9 * * 0.923 0 .8605 0 .9686 0 .9146 Well Number PFO S 3M 3M Env 3M Env MDH MDH Env Lab Lab Measured Measured MDH RLesaulbt Duplicate Average Value Value Average Duplicat e 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 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 pa rt s per trillion) and 0 .00738 ug/L (7 .38 pa rt s per trillion) . Lower limit of 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 . 32 `~.. . ~....' p . 33 Oakdale July 13, 2005 Sampling Results (ug/L) PFOA Well Number 3M 3M Env 3M Env MDH Measured MD H Lab Lab Measure d Lab Duplicate Average Value Value Average Result Duplicate I 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 PFOS Env 3M Env 3M Env MDH Measured MDH Lab Lab Measure d Lab Duplicate Average Value Value Average Result Duplicate I 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 of 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 : Repo rt 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 . 33 . .~, p . 34 ,Oakdale August 12, 2005 Sampling Results (ug/L ) PFOA Well Number 3M 3M Env 3M Env MDH MD H E Lan b v LaM b Le ab asu Merasuered d MDH Result Duplicate Average Value Value Average Duplicate 1 * * * ND NA NC 2 * * * ND NA NC 3 ~` * * ND NA NC 5 * * * 0 .9350 NA NC 7 8 * * * * * * 0.5344 0 .4720 0 .5032 0.6903 NA NC 9 * * * ND NA NC Well Number PFO S 3M 3M Env 3M Env MDH MD H Env Lab Lab Measured Measured MDH Lab Duplicate Average Value Value Average Result Duplicat e I * * * ND NA NC 2 * * * ND NA NC 3 * * * ND NA NC 5 7 8 * * * * * * * * * 1 .1630 NA NC' 0 .6302 0.6471 0 .6387 0 .6903 NA NC 9 * * * ND All results in ug/L (parts per billion or ppb) . * - 3M results not yet available . NA NC 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 pa rt s per trillion). Lower limit of 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 pa rts per t ri llion) . For MDH data : Report level is 0 .5 ppb for PFOS and 1 .0 ppb for PFOA . Where data is repo rted at less than these values, it represents Measured Values . 34 p . 35 MDH has also tested a public water supply at Whispering Oaks mobile home par k 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) PFOA (ug/L) E05-0007-77781 Reception area rest room 0 .75 E05-0007-77782 Reception area rest room Dup 0 .66 E05-0007-77785 Ctr office rest m fin 0.18 E05-0007-77786 Ctr office rest rm fln Dup 0 .19 E05-0007-77789 Break room sink 0 .14 E05-0007-77790 Break room sink Dup 0 .14 E05-0007-77793 Utility room janitor sink 0 .67 E05-0007-77794 Utility room janitor sink Dup 0 .71 PFOS (ug/L) 0 .86 0 .86 0 .14 0 .16 0 .18 0 .15 0 .84 0 .88 1 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 MDH Exygen Exygen Exygen ~H Measured MDH Result Duplicate Average Measured Value Average Value Duplicate Oakdale Public Works 0 Bldg . Lunch Room Sink .687 0 .709 0 .698 0 .624 NA NC PFOS Oakdale Public Works 0 Bldg . Lunch Room Sink .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 of Quantitation (LOQ) of 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 . 35 p . 36 Private Wells in Oakdal e In March 2005, MDH analyzed samples collected from several private wells located in or around Oakdale : Oakdale Private Wells OAKDAL E Street No . Street Name Sample Date PFOS PFOA W82W0020113 3465 Geneva Ave . N 3/7/2005 ND ND unk 3445 Geneva Ave. N 3/7/2005 ND ND W82W0020112 3315 Geneva Ave . N 3/7/2005 ND ND unk 3307 Geneva Ave . N 3/7/2005 ND ND unk 3301 Geneva Ave . N 3/8/2005 ND ND 174298 7641 10 'h St . N . 3/7/2005 ND N D 0 .662 Stillwater Blvd . ug/L unk 7287 N 3/7/2005 ND or b 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 Elm o 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 : 36  ' ~ p . 37 ~ Lake Elmo Private Wells (ug/L or parts per billion) LAKE ELM O Stree t No . Street Name Sample Date PFOS PFOA 82W01045 4111 Isle Ave. N 4/13/2005 ND ND 404104 4077 Isle Ave . N 4/13/2005 ND ND 82W01033 8830 42nd St. N 3/7/2005 ND ND 82W01022 3490 Kelvin Ave . N . 6/21/2004 ND ND 82W01018 3508 Kelvin Ave . N . 6/21/2004 ND ND 82W01014 3509 Kelvin Ave . N . 6/21/2004 ND ND 82W01026 3533 Kelvin Ave. N. 6/21/2004 ND ND 493185 3551 Kelvin Ave . N . 6/21/2004 ND ND 82W01015 3567 Kelvin Ave . N . 6/21/2004 ND ND 82W01016 3597 Kelvin Ave . N . 6/21/2004 ND ND 439126 3681 Kelvin Ave. N . 6/21/2004 ND ND 539248 3691 Kelvin Ave. N. 6/21/2004 ND ND 82W01044 3322 Ideal Ave . N 3/8/2005 ND ND 134754 3240 Ideal Ave. N 3/8/2005 ND ND 8931- 710053 8945 34th St . N . 8971- 670792 8975 4/13/2005 ; 8981- 710051 898 5 VOCs ND ND 82W01034 8611 34th St . N . 3/8/2005 ND ND 82W01035 8633 34th St . N . 3/8/2005 ND ND 413596 10120 _Stiliwater Lane 6/21/2004 ND N D 82W01021 10174 Stillwater Lane 6/21/2004 ND ND 82W01017 10212 Stillwater Lane 6/21/2004 ND ND 670770 9018 31st St. N . 82W01003 9038 31st St . N . 82W01004 9046 31st St. N. 82W01047 9051 31st St . N . 82W01029 9066 31st St. N . 604274 9077 31st St . N . 6/22/2004 ND ND 6/22/2004 ND 0 .5 7/20/2004 ND 0.4 4/27/2005 ND 0 . 5 6/22/2004 ND 0 .4 7/20/2004 ND 0 .2 4/27/2005 ND 0 . 6 4/13/2005 ND ND 7/20/2004 ND 0 .3 4/27/2005 ND 7/20/2004 ND 0 .3 4/27/2005 ND 0 .6 37 p . 38 82W01019 9078 31st St . N . 6/22/2004 ND 0 . 4 7/20/2004 ND 0 .2 4/27/2005 ND 0.5 82W01005 9095 31st St . N . 6/22/2004 ND ND 82W01024 9098 31st St . N . 6/22/2004 ND ND 82W01006 9141 31st St . N . 6/22/2004 ND ND 82W01007 9148 31st St . N . 6/22/2004 ND ND 82W01008 9181 31st St . N . 6/22/2004 ND ND 82W01028 9198 31st St. N. 7/20/2004 ND ND 82W01023 9202 31st St. N. 616698 9260 31st St . N . 82W01009 9343 31st St . N . 6/21/2004 ND N D 7/20/2004 ND 0 .1 4/27/2005 ND 0 .3 6/21/2004 ND ND 82W01020 9345 31st St . N . 6/21/2004 ND 0 . 9 4/27/2005 ND 1 82W01200 3030 Janero Ave . N. 6/13/2005 ND ND 82W01133 3010 Janero Ave . N. 6/13/2005 ND 0 .2 82W01134 2990 Jan ero Ave . N . 6/13/2005 ND 0 .2 82W01135 2950 Janero Ave . N . 6/13/2005 ND ND 208450 3052 Jan-le Ave . N . 3/7/2005 ND ND 536672 3014 Jan-le Ave . N . 3/17/2005 ND 0 .647 413551 3053 Jamle Ave . N . 3/9/2005 ND ND 82W01048 3023 Janiley Ave . N . 4/13/2005 ND ND 82W01050 2991 Jamley Ave . N . 4/13/2005 ND ND 604259 2994 Jar-le Ave . N. 4/13/2005 ND ND 82W01136 2970 Jamley Ave . N . 6/13/2005 ND 0 .4 82W01137 2940 Jan-le Ave . N . 6/13/2005 ND 0 .3 82W01138 2935 Jamley Ave . N . 6/13/2005 ND ND 82W01122 2959 Jan-le Ave . N . 5/16/2005 ND 0 .7 82W01139 2909 Jamle Ave . N . 6/13/2005 ND ND 82W01140 2904 Jamle Ave . N . 6/13/2005 ND 0 .3 82W01141 2877 lamley Ave . N . 6/13/2005 ND ND 493576 2850 Jamley Ave . N . 82W01142 2809 Jan-le Ave . N. 6/13/2005 ND 0 .2 451602 2805 Jan-le Ave . N . 6/13/2005 ND ND 82W01124 2798 Jamle Ave . N . 5/16/2005 ND ND 82W01123 2751 Jamle Ave . N . 5/16/2005 ND ND 110523 2819 Ivy Ave N . 4/18/2005 ND ND 82W01037 8866 Stillwater Blvd 3/8/2005 ND ND 82W01064 8863 Stillwater Blvd. 4/18/2005 ND ND 82W01038 8740 Stillwater Blvd 3/9/2005 ND ND 82W01063 8707 Stillwater Blvd . 4/13/2005 ; VOCs 0 .178 ND 583343 8680 Stillwater Blvd 3/7/2005 2 .2 1 .5 7/22/2005 - GAC ND ND 3g p . 39 82W01062 8659 Stillwater Blvd . 4/18/2005 1 .876 1 .72 676479 8643 Stillwater Blvd . 4/15/2005 0.233 0 .423 82W01061 8627 Stillwater Blvd . 0 .3 0 .5 558222 8620 Stillwater Blvd 3/7/2005 1 .4 1 . 7 6/21/2005 - GAC ND ND 82W01060 8583 Stillwater Blvd . 4/15/2005 ND ND 82W01059 8567 Stillwater Blvd. 4/13/2005 ; VOCs 0 .155 ND 82W01058 8511 Stillwater Blvd. 4/13/2005 ND ND 82W01057 8488 Stillwater Blvd . 4/15/2005 ND ND 82W01056 8464 Stillwater Blvd . 4/15/2005 ND 0 .793 82W01055 8428 Stillwater Blvd . 4/13/2005 ; VOCs ND ND 82W01054 8404 Stillwater Blvd . 4/13/2005 ND ND 82W01053 8384 Stillwater Blvd . 4/13/2005 ; VOCs ND N D 599973 8364 Stillwater Blvd. 4/13/2005 0 .398 ND 82W01039 8308 Stillwater Blvd 3/7/2005 1 .4 1 6/13/2005 - GAC ND ND 154476 8282 Stillwater Blvd 3/7/2005 1 .2 0 .6 6/13/2005 - GAC ND ND 634270 8268 82W01132 8255 Stillwater Blvd 3/7/2005 ND 0.4 8 Stillwater Blvd . 4/18/2005 ND ND 82W01025 9517 Stillwater Blvd. 6/21/2004 ND ND 82W01010 9521 Stillwater Blvd. 6/21/2004 ND ND 539268 9524 Stillwater Blvd. 6/21/2004 ND ND 151756 10240 Stillwater Blvd . 6/21/2004 ND ND 569744 3082 Inwood Ave . N 3/7/2005 3 .3 3 7/22/2005 - GAC ND ND 687850 3077 Inwood Ave . N 3/10/2005 1 .4 1 .3 6/13/2005 - GAC ND ND 613401 3036 Inwood Ave. N 3/7/2005 1 .4 1 7/13/2005 - GAC ND ND 622211 3033 Inwood Ave . N 3/10/2005 1 .4 1 . 8 6/24/2005 - GAC ND ND 82W01065 2961 Inwood Ave . N . 4/13/2005 ND ND 154443 2915 Inwood Ave . N . 4/13/2005 ND ND 156421 2895 Inwood Ave . N . 4/18/2005 ND ND 121060 2875 Inwood Ave . N . 4/13/2005 ND ND 440560 2856 Inwood Ave . N . 4/15/2005 0 .694 0 .86 8 7/13/2005 1 0 .8 437308 2816 Inwood Ave . N 3/7/2005 0 .285 0 .426 428479 2796 Inwood Ave . N 3/8/2005 ND N D 82W01067 2793 Inwood Ave . N . 4/15/2005 ND ND 82W01068 2773 Inwood Ave . N . 4/15/2005 0 .629 1 .006 7/13/2005 0 .7 0 . 7 82W01069 2731 Inwood Ave . N . 4/14/2005 ND ND 82W01130 2298 Inwood Ave . N . 5/18/2005 ND ND 82W01131 2038 Inwood Ave . N . 5/23/2005 ND ND 39 p . 40 82W01073 2965 Innsdale Ave . N . 4/18/2005 0.177 ND 471065 2960 Innsdale Ave. N . 4/13/2005 0 .804 1 .245 6/22/2005 - GAC ND ND 428478 2935 Innsdale Ave N 3/7/2005 ND ND 82W01070 2930 Innsdale Ave . N . 4/13/2005 ND ND 440566 2906 Innsdale Ave N 3/9/2005 ND ND 82W01072 2895 Innsdale Ave . N . 4/18/2005 ND ND 82W01071 2876 Innsdale Ave . N . 4/13/2005 ND ND 453245 2655 Innsdale Ave . N . 5/16/2005 ND ND 519084 2626 Innsdale Ave. N . 5/16/2005 ND ND 82W01129 2621 Innsdale Ave . N. 5/16/2005 ND ND 82W01074 8520 Ironwood Trl . N . 4/15/2005 0 .791 0.833 7/13/2005 0 .8 1 .7 82W01075 8521 Ironwood Trl . N . 4/15/2005 ND 0 .791 82W01076 8540 Ironwood Trl. N. 4/15/2005 0 .692 1 .095 7/13/2005 0 .9 0 .7 82W01077 8549 Ironwood Trl . N . 4/15/2005 0 .676 1 .004 7/13/2005 0 .6 0. 4 82W01078 8580 Ironwood Trl . N . 4/18/2005 0 .644 0 .93 7/13/2005 0 .9 0 .7 82W01079 8592 Ironwood Trl. N. 4/15/2005 ND ND 82W01080 8603 Ironwood Trl . N. 4/15/2005 ND ND 82W01081 8618 Ironwood Trl . N . 4/15/2005 ND ND 82W01082 8628 Ironwood Trl . N . 4/15/2005 0.408 0 .746 82W01083 8633 Ironwood Trl . N . 4/15/2005 ND ND 424136 8650 Ironwood Trl . N . 3/8/2005 0 .296 0 .302 82W01084 8652 Ironwood Trl . N . 4/15/2005 ND ND 82W01085 8657 Ironwood Trl. N. 4/14/2005 ND ND 82W01086 8674 Ironwood Trl. N . 4/14/2005 ND ND 82W01087 8690 Ironwood Trl . N . 4/15/2005 (inside) ND ND 82W01088 8695 Ironwood Trl . N . 4/15/2005 0.545 0 .86 82W01089 8702 Ironwood Trl . N . 4/15/2005 0 .402 0 .693 82W01090 8716 Ironwood Trl . N . 4/15/2005 0 .286 0 .66 8 110434 8722 Ironwood Trl . N . 4/15/2005 0 .513 0 .858 82W01091 8725 Ironwood Trl . N . 4/15/2005 ND ND 82W01092 8748 Ironwood Trl . N . 4/14/2005 ND ND 82W01093 8772 Ironwood Trl . N . 4/15/2005 0 .482 0 .713 82W01094 8775 Ironwood Trl . N . 4/15/2005 ND ND 82W01095 8780 Ironwood Trl. N . 4/15/2005 ND ND 82W01096 8785 Ironwood In . N . 4/15/2005 ND ND 82W01097 2811 Irish Ave . N . 4/15/2005 ND ND 67 1 999 2770 Iri sh Ave . N . 4/15/2005 ND ND 82W01099 2759 Irish Ave . N. 4/15/2005 0 .143 ND 7/13/2005 0 .2 0 .3 4' p . 41 585145 2895 575148 2890 588139 2850 576160 2841 614269 2769 609537 2760 598819 2811 617699 2696 678196 2699 606937 2677 607488 2678 569982 2655 554316 2656 569782 2618 569978, 2580 Imperial Ave . N 3/8/2005 0 .257 0 .323 Imperial Ave . N . 4/13/2005 ND ND Imperial Ave . N . 4/13/2005 ND ND Imperial Ave . N 3/8/2005 0 .351 ND Imperial Ave . N . 4/13/2005 ND ND Imperial Ave . N . 4/13/2005 ND ND Imperial Ave . N . 4/13/2005 0 .264 ND Imperial Ave, N . 5/16/2005 ND ND Imperial Ave . N . 5/16/2005 0 .2 ND Imperial Ave . N . 5/16/2005 ND ND Imperial Ave . N . 5/16/2005 ND ND Imperial Ave . N . 5/16/2005 ND ND Imperial Ave . N. 5/16/2005 ND ND Imperial Ave . N 3/8/2005 ND ND Imperial Ave . N . 5/16/2005 ND ND 82W01100 8623 28 th St. N . 4/15/2005 ND ND 82W01101 8643 28 th St. N. 5/16/2005 0.2 ND 82W01102 8648 28th St. N. 4/14/2005 ND ND 82W01103 8687 28th St. N . 4/15/2005 ND ND 446288 9043 28th St . N . 5/16/2005 ND ND 82W01125 9049 28 th St . N . 5/16/2005 ND ND 82W01126 9065 28th St . N . 5/16/2005 ND ND 82W01127 9079 28th St . N. 5/16/2005 ND ND 82W01128 9155 28 th St. N . 5/16/2005 ND ND 511739 8244 27th St . N . 4/15/2005 ND ND 457680 8247 27th St . N . 4/15/2005 ND ND 465954 8282 27th St. N. 4/15/2005 ND ND 440589 8301 27 th St. N . 4/15/2005 ND ND 196939 8310 27th St . N . 4/15/2005 0 .733 0 .863 7/13/2005 0.3 0 .2 442140 8341 27th St . N . 4/15/2005 ND ND 82W01104 8352 27 th St. N . 4/15/2005 ND ND 440577 8375 27th St. N . 4/15/2005 ND ND 503288 8478 27th St. N . 4/15/2005 ND ND 453250 8483 27 th St . N . 4/15/2005 ND ND 670740 8555 27th St . N . 4/15/2005 0 .857 1 .23 2 7/13/2005 - GAC ND ND 700594 8570 27th St. N . 4/14/2005 ND ND 670739 8605 27th St . N . 4/14/2005 0 .899 1 .05 2 6/23/2005 ND ND 679966 8623 27th St . N . 4/15/2005 ND ND 82W01106 8639 27th St . N . 4/14/2005 ND ND 82W01107 8644 27th St. N . 4/14/2005 0 .416 0 .686 82W01108 8650 27th St . N . 4/14/2005 0.813 0 .88 4 7/13/2005 0 .9 0 .7 q~l p . 42 82W01109 8655 27th St. N. 82W01110 8656 27th St. N. 82W01111 8685 27th St . N . 82W01112 8709 27th St . N . 82W01113 8715 27th St . N . 415659 8735 27th St . N . 176046 8755 27th St. N . 194159 8785 27th St. N. 176036 8815 27th St. N . 174267 8845 27th St. N . 82W01114 8875 27th St . N . 82W01115 8905 27th St . N . 173927 8925 27th St . N . 4/22/2005 0 .214 ND 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 0 .356 0 .67 5 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 0 .386 ND 4/14/2005 0 .709 0 .70 8 7/13/2005 0 .7 0 .4 4/14/2005 0 .414 0 .582 4/14/2005 0 .488 ND 4/14/2005 0.454 ND 176020 8770 27th St. Ct . N . 82W01117 8780 27th St . Ct . N . 176049 8790 27th St . Ct . N . 182679 8800 27th St . Ct. N . 173925 8810 27th St . Ct . N . 185945 8820 27th St. Ct. N . 162931 8830 27th St. Ct. N . 187000 8840 27th St . Ct . N . 173938 8850 27th St . Ct . N . 182731 8860 27th St. Ct . N . 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 ND ND 4/14/2005 0 .301 ND 4/14/2005 ND ND 4/14/2005 0.357 ND 4/15/2005 0 .727 0 .69 7 7/13/2005 1 .2 0 .5 4/14/2005 0 .608 ND 4/18/2005 0 .711 0.88 7 7/13/2005 0 .5 0 .6 4/14/2005 0.65 ND 577036 616945 554311 598818 590036 577037 588140 569984 582669 587849 8119 8154 8165 8215 8281 8284 8364 8367 8454 8457 26th 26th 26th 26th 26th 26th 26th 26th 26th 26th St . N . St . N . St . N . St . N . St . N. St . N . St . N . St . N . St . N . St . N . 5/16/2005 ND ND 5/16/2005 ND ND 5/16/2005 ND ND 5/16/2005 ND ND 5/23/2005 ND ND 5/16/2005 ND ND 5/16/2005 0 .2 ND 5/16/2005 ND ND 5/16/2005 ND ND 5/16/2005 ND ND 590079 8042 22nd St . Ct . N . 3/7/2005 ND ND 656705 8125 22nd St. N. 3/8/2005 ND ND 597121 8382 22nd St. N 5/16/2005 ND ND 641705 8414 22nd St . N 5/16/2005 ND ND 641458 1873 Ivory Ave . N. 5/16/2005 ND ND 633298 1849 Ivory Ave . N. 5/16/2005 ND ND 637433 1827 Ivo Ave . N . 5/16/2005 ND ND 42 p . 43 633269 1805 633266 1779 628276 1757 622311 1743 623865 1709 633264 1694 645610 1697 628279 1680 633276 1681 637406 1668 615494 1663 658982 1696 82W01147 1683 672580 1665 658960 1634 Ivory Ave . N . 5/16/2005 ND ND Ivory Ave . N . 5/16/2005 ND ND Ivory Ave . N . 5/16/2005 ND ND Ivory Ave. N. 5/16/2005 ND ND Ivory Ave. N. 6/13/2005 0 .2 0 .2 Ivory Ave . N. 6/13/2005 ND ND Ivory Ave . N. 6/13/2005 ND ND Ivory Ave . N . 6/13/2005 ND ND Ivory Ave . N . 6/13/2005 ND ND Ivory Ave . N . 6/13/2005 ND ND Ivory Ave . N . 6/13/2005 ND ND Ivy Ave . N . 51 16/2005 0.2 ND Ivy Ave . N . 6/13/2005 ND ND Ivy Ave . N . 6/13/2005 ND ND Ivy Ave . N . 6/13/2005 ND ND 478956 8281 15th St . N . 3/8/2005 ND ND 512491 8280 15th St . N . 3/8/2005 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 PFOS PFOA Sample ID (ug/L or paornts) p(uagr/tLs poerr per billi billion Bldg 116 Outlet 0 .596 5 .29 Bldg 116 Outlet* 0 .517 5 .5 8 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 43 p . 44 Building 116 Sampling Results for December 7, 2004 Exygen Results PFOS PFOA Sample ID (ug/L or parts (ug/L or per billion) parts pe r billion) Effluent ND ND Effluent* ND ND Effluent Dup ND N D 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 billio n PFOS PFOA Sample ID Field ID Measured Reported Measured Reported Value Level Value Level u/L u/L u/L u L 200502990 05-173 final 0.0 < 0.5 0.0 <1 .0 Note : The reporting level is 0.5 ppb for PFOS and 1 .0 ppb for PFOA . Building 116 Sampling Results for June 6, 2005 Exygen Result s ug/L or parts per billio n Sample ID PFOS PFOA (ug/L) (ug/L) Effluent ND ND Effluent* ND ND Effluent Dup ND N D ND = Not detected = Response between 0 and 0 .025 ug/L NQ = Not quantifiable = Response between 0 .025 ug/L and LOQ (0 .050 uglL) *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 44 p . 45 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 Facilit y 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 200515731 233142 200515732 408198 200515733 406171 200515734 151763 200515735 440575 ID PFO S PFOA Measured VaRleu poerted Value (ppb) Measured Value Reported Valu e (ppb) 0.0000 < 0.5 0.0000 < 1 .0 0.0000 < 0.5 0.0000 < 1.0 0.0000 < 0 .5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1 .0 4 5 p . 46 ~ 200515736 544438 200515737 641472 200515738 TB1SW001 trip blank 200515739 427043 200515740 471471 200515741 460152 200515742 402592 200515743 698214 200515744 109708 200515745 109738 200515746 162915 0.0000 < 0.5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1 .0 0.0000 < 0.5 0.0000 < 1 .0 0.0000 < 0.5 0.0000 < 1 .0 0.0000 < 0.5 0.0000 < 1 .0 0.0000 < 0 .5 0.0000 < 1.0 0.0000 < 0 .5 0.0000 < 1.0 0.0000 < 0.5 0.0000 < 1 .0 0.0000 0.0000 (duplicate) Note : 0.0000 < 0.5 0.0000 < 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 billio n Sample ID PFOS PFOA ( ug/L) (ug/L) H-W6-207643 NQ 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 Duplicat e 6 4 p . 47 0 Hastings February 28, 2005 Sampling Results ug/L or parts per billio n Sample ID PFOS PFOA (ug/L) (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 Duplicat e City of Cottage Grov e 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 billio n Sample ID PFOS PFOA (ug/L) (ug/L) CG-W6-201238 ND ND CG-W6-201238* ND ND CG-W9-165602 ND ND CG-W9-165602* ND ND CG-W5-208806 ND ND CG-W5-208806* ND ND CG-W3-208807 ND ND CG-W3-208807* ND ND CG-W7-201227 ND ND CG-W7-201227* ND ND CG-W8-110464 ND ND CG-W8-110464* ND ND CG-W 11-655944 ND ND CG-WI 1-655944* ND ND CG-W10-191904 ND ND CG-W10-191904* ND ND CG-W2-208809 ND ND ~7 p . 48 CG-W2-208809* ND ND CG-WI-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 Duplicat e 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 Obiections : Sample ID PFOS PFOA (ug/L) (ugn-) 200501452 (Well 3) ND ND 200501453 (Well 4) ND N D ND = < 0 .5 ug/L 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 . L4.S p . 50 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS s1_oi2 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 16-Jun-2005 18 :15 Contract No . : 4191 Lab Sample ID : L7909-1 Y 2 Matrix : N/A Sample Size : 1 .00 mL Sample Receipt date : 22-Jun-2005 Ini tial Calibrati on Date : 13-Sep-2005 Extrac tion Date: 06-Sep-2005 Instrument ID : LC-MS/M S Analysis Date : 13-Sep-2005 Time : 8 :38 :26 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G 168S017 Injec tion Volume (pL): 30.0 Blank Data Filename: FC5G 168S015 Dilution Factor: N/A Concentrati on Units : ng/m L Cal . Ver. Data Filename : FC5G_168S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 0 .410 0 .251 PFOA U 0 .24 7 4 .27 PFNA U 0 .268 PFDA U 0 .259 PFUnA U 0 .257 PFDoA U 0 .255 PFBS PFHxS 0 .291 0 .254 3_7 7 U 0 .255 PFOS U 0 .258 PFOSA U 0 .250 LABELED COMPOUND LAB SPIKE CONC . R(%)2 RETENTIO N FLAG' CONC . FOUND TIME (ng) (n9) 13C2-PFOA 12.0 3.99 33 .2 13C4-PFOS(80) 12.0 6.03 50 .3 13C4-PFOS(99) 12 .0 4 .77 39.7 13C2-PFDA 12.0 10 .7 88.9 4 .70 5 .56 5 .56 5 .41 (1) U =not detecte d (2) R (%) = Percent recovery 16814PFD3_2)ds, S4 Approved b : 11-10-2005 y QA/QC Chemist dd-mm-yyy y 0))((C -,X-YS ANALYTI CAL SER\/1CES LTl] P.O . BOX 2219, 2045 AULLS RD . WEST, SIDNEY, B.C. . CANADA VOL 358 TEL (250) 655-5800 FAX (250) 6%5811 90 p . 51 AXYS METHOD MLA-042 Rev 02 PFOS_s1_D12 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPOR T CUENT iD : Sample Collec tion : 28-Jun-2005 10 :27 Lab Name : AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID : L7932- 1 Matrix : SERUM Sample Size: 1 .00 mL Sample Receipt Date; 29-Jun-2005 Initial Calibrati on Date: 05-Aug-2005 Extracti on Date: 04-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 05-Aug-2005 Time : 21 :17 :29 LC Column ID : C18, Zorbax XDB Extract Volume (mL): 2 Sample data Filename: FCSG_131SO40 Injection Volume (NL) : 30 .0 Blank data Filename : FC5G_131S024 Dilution Factor : N/A Concentration Units : nglm L Cal . Ver. data Filename : FC5G131S03 7 CAL VIER ID : PFC-LIN-03,9CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG FOUND LIMIT TIME PFPeA PFHxA U U 0 .638 0_620 PFHpA U 0 .251 PFOA 30 .9 0 .247 PFNA PFDA PFUnA 2 .60 0 .268 0 .510 0 .259 0 .290 0 .256 PFDoA U 0 .25 5 PFBS U 0 .254 PFHxS 6.03 0.255 PFOS 88.6 0 .258 PFOSA U 0 .250 4 .70 5 .07 5 .38 5 .67 4.90 5.50 LABELED COMPOUND LAB SPIKE CONC . FLAG' CONC. FOUND (ng) (ng) R(y,)2 RETENTION TIME 13C-PFOA 12 .0 7 .69 64 .1 4 .70 13C-PFDA 12 .0 10 .3 85 .8 5 .34 (1) U = not detected (2) R (%) = Percent recovery 16535PFD22.xls, S2 Approved by : ~Rirl~ QAIQC Chemist 11-10d-d2 -m0m-0yy5yy 420 A~CYS AiVALYTICP~L SER-,/ICES LTC~ P.D. BOX 2214, 2045 MILLS RD. WEST, SIOHEY, B.C . WiAOA YSt 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 S' 1 p . 52 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS S1_O12 Form 1A12 ~ PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collec ti on : 28-Jun-2005 10 :30 Lab Name: AXYS ANALYTICAL SERVICES Contract No. : 4191 Lab Sample ID : L7932- 2 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt Date : 29-Jun-2005 Initial Calibration Date : 05-Aug-2005 Extraction Date: 04-Aug-2005 Instrument ID : LC-MSlM S Analysis Date: 05-Aug-2005 Time : 21 :42 :08 LC Column ID: C18, Zorbax XDB Extract Volume (mL) : 2 Sample Datafile : FC5G_131SO42 Injecti on Volume (uL) : 30 .0 Blank Data Fifename : FC5G_131S024 Dilution Factor : NIA Concentration Units : ng/m L Cal . Ver. Data Filename: FCSG_131S037 CAL VIER ID : PFC-LIN-039CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .638 PFHxA U 0 .620 PFHpA U 0 .251 PFOA 24 .2 0 .247 PFNA 148 0 .268 PFDA U 0 .259 PFUnA U 0 .25 6 P FDoA U 0 .255 PFBS U 0 .254 PFHxS 6 .23 0 .255 PFOS 38.0 0 .258 PFOSA U 0 .250 4 .70 5 .07 4 .90 5 .50 LABELED COMPOUND LAB SPIKE CONC. R(%)z RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C-PFOA 13C-PFDA 12.0 8 .09 67.4 410 12.0 11 .2 93.0 5,34 (1) U =not detected (2) R (%) = Percent recovery 16535PF02 2 .xfs. S4 Approved by : QA/QC Chemist 2oo5 dd-mm YYYy A)}((C+ AXYS ANALYI ICAL SERVICES LTU P .O . BOX 2214, 2045 MILLS RD. WEST, SIDNEY, B.C. CANADA VOL 3S8 TFL (250) 655-5800 FAX (250) 655-581 1 S.2 p . 53 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_S1_D12 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collec ti on : 01-Ju1-2005 13 :03 Lab Name : AXYS ANALYTICAL SERVICES Contract No. : 4191 Lab Sample ID : L7932-4 Matrix: SERUM Sample Size: 1 .00 mL Sample Receipt Date: 06-Ju1-2005 Initial Calibration Date: 05-Aug-2005 Extraction Date : 04-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 05-Aug-2005 Time : 21 :54 :26 LC Column ID: C18, Zorbax XDB Extract Volume ( mL) : 2 Sample Datafile : FC5G_131SO43 Injection Volume (pL) : 30 .0 Blank Data Filename : FC5G131S024 Dilu ti on Factor: N/A Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_131S03 7 CAL VIER ID : PFC-LIN-039CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .638 PFHxA U 0 .620 PFHpA U 0.25 1 PFOA PFNA 9 .25 0.247 1 .40 0 .268 PFDA U 0 .259 PFUnA U 0 .256 PFDoA U 0 .255 PFBS U 0 .254 PFHxS 2 .53 0 .255 PFOS 28.4 0 .258 PFOSA U 0 .250 4.66 5 .01 4.90 5 .50 LABELED COMPOUND LAB SPIKE CONC. R(4/,)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng ) 13C-PFOA 12.0 8.14 67.9 4 .66 13C-PFDA 12 .0 10 .7 88.8 5 .34 (1) U =not detecte d (2) R (%) = Percent recove ry 16535PPD22 .x 1s, S5 Approved bY: QA/QC Chemist 11-10-2005 dd-mm-yyyy 40Ce ',X-YS AIVALYriCAL SER\/ICES LTp P.O. BOX 2219, 2045 61t115 RD . WES(, SIDNEY, B.C, CANADA VOL 3S8 TEt (250) 655-5800 FAX (250) 655-581 1 0 p . 54 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 08-Aug-2005 11 :41 Contract No . : 4191 Lab Sample ID : L7932-16 Y2 (A) Matrix : SERUM Sample Size: 1 .00 mL Sample Receipt date : 10-Aug-2005 Initi al Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 12-Sep-2005 Time: 18:50 :23 LC Columri ID: C1 8 Extract Volume (mL) : 2 Sample Datafile: FC5G 167S033 Injection Volume (pL): 30 .0 Blank Data Filename : FC5G 167S031 Dilution Factor: N/A Concentration Units : nglm L Cal . Ver. Data Filename : FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0 .753 0.251 PFOA E PFNA PFDA 0.967 0 .268 0.417 0.259 PFUnA 0.273 0.257 PFDoA U 0.25 5 PFBS U 2 .54 PFHxS 17 .3 2.55 PFOS 85 .9 0.258 PFOSA U 0 .250 4 .22 5.05 5 .41 5 .70 4 .87 5.51 LABELED COMPOUND LAB SPIKE CONC . R(q,)z RETENTIO N FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 12.0 13C4-PFOS(80) 12.0 13C4-PFOS(99) 12 .0 13C2-PFDA 12 .0 11 .3 94 .5 12 .8 107 11 .9 99 .2 12.0 100 4 .70 5.56 5.56 5.36 (1) U = not detected ; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recovery sr55PF_D1_2 .zm. S4 Approved by : 11-10-05 ~ QA/QC Chemis t1 dd-m m -M 1004 -,X-YS AIVALYT It~L SERVICES LT(D P.O . BOX 2219, 2045 AULLS RD. WEST, SIDNEY, B.C., CANADA V81. 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 S# p . 55 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_St D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 09-Aug-2005 11 :41 Contract No. : 4191 Lab Sample ID : WG16755-104 Y2 Matrix: SERUM Sample Size : (DUP L7932-16) 1 .00 mL Sample Receipt date : 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 12-Sep-2005 Time : 19 :04:39 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile: FCSG 167S034 Injection Volume ( pL) : 30 .0 Blank Data Filename : FC5G 167S031 Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0.945 0 .251 PFOA E PFNA PFDA 1 .37 0 .268 0 .439 0 .259 PFUnA PFDoA U U 0.257 0.255 PFBS U 2 .54 PFHxS 14 .5 2.55 PFOS 79 .8 0 .258 PFOSA U 0 .250 4.22 5 .05 5 .36 4.87 5.51 LABELED COMPOUND LAB SPIKE CONC. R (%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 12.0 13C4-PFOS(80) 12.0 13C4-PFOS(99) 12.0 13C2-PFDA 12 .0 11 .7 14 .2 13 .7 14 .3 97 .7 118 114 119 4 .70 5 .56 5 .56 5.36 (1) U = not detected; E= exceeds calibrated linear range, see dilu tion data (2) R (%) = Percent recovery 16755PF_D1 2 .)ds. S5 Approved by: - 11-10-05 QAIQC Chemist dd-mm-yyyy 00(8 AXYS AtVALYTICAL SER\/ICES LTE) P .O. BOX 2219, 2045 MillS RD . WEST. SIDNEY, B .C., CANADA Y8 1. 358 TEl (250) 6S5-5800 FAX (250) 655-581 1 ST~ p . 56 AXYS METHOD MLA-0 42 Rev 02 CLIENT ID : PFOS_Si_012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 08-Aug-2005 11 :41 Con tract No. : 4191 Lab Sample ID : WG16755-104 Y2i Matrix : SERUM Sample Size : (DUP L7932-16 Y2i (A)) 1 .00 mL Sample Receipt date: 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extracti on Date : 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 13-Sep-2005 Time : 1 :43 :59 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample Datafile: FC5G 167S062 Injection Volume (PL) : 10 .0 Blank Data Filename: FC5G 167S031 Dilution Factor: 3 Concentration Units : nghn L Cal. Ver. Data Filename : FC5G_167S059 CAL VER ID : PFC-L(N-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 89.1 0.741 4.70 LABELED COMPOUND LAB SPIKE CONC.- R(0/,)2 RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 9 3C2-PFDA D 12 .0 11 .5 95 .8 4 .70 (1) U = not detected; D = dilution data (2) R (%) = Percent recovery 16755PF_D3_2.xls, S3 Approved by : QA/QC Chemist 11-10-05 dd-mm-yyyy 000 AXYS ANALYi-ICAL SERN/I<=ES LTC> P.O . BOX 2219, 2045 NULLS RD. WEST, SIDNEY, B.C., CANADA VOL 3S8 TEL (250) 6555800 FAX (250) 655-581 1 96 p . 57 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 08-Aug-2005 11 :41 Contract No. : 4191 Lab Sample ID : L7932-16 Y2i (A) Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date: 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction datae: 29-Aug-2005 Analysis datae: 13-Sep-2005 Instrument ID : LC-MS/MS Time: 1 :29 :43 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample data Filename: FC5G 167SO61 Injection Volume (NL) : 10.0 Blank data Filename : FC5G 167S031 Dilution Factor: 3 Con ce ntration Units : ng/m L Cal . Ver. data Filename : FC5G167S059 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB FLAG' CONC FOUND DETECTION RETENTION LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 95 .1 0 .741 4 .70 LABELED COMPOUND LAB SPIKE CONC . R(%)z RETENTIO N FLAG' CONC . FOUND TIME (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D 12 .0 9 .79 81 .6 4 .70 (1) U = not detected ; D = dilution data (2) R (%) = Percent recovery 16T55PF_03_2.xis, S2 Appro ved by: QA/QC Chemist 11-10-05 da-m m-yyyy 00(0 AXYS AIVALYi-ICAL SERVICES LTc) P.O. BOX 2219, 2045 MILLS ND. WEST, SIDNEY, B .C., CANADA Yal 3S8 TEL (250) 655-5800 FAX (250) 655581 1 S1 p . 58 AXYS METHOD MLA-0 42 Rev 02 PFOS S1_012 Form IA/2 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT ID : Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 08-Aug-2005 13 :31 Contract No . : 4191 Lab Sample ID : L7932-17 Y2 Matri x: SERUM Sample Size : 1 .00 mL Sample Receipt date : 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 12-Sep-2005 Time : 19:18:55 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G 167S035 Injection Volume (pL): 30.0 Blank Data Filename : FC5G 167S031 Dilution Factor : N/A Concentration Units : ng/mL Cal . Ver. Data Filename : FC5G_167S027 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 0.367 0.251 PFOA 42.4 0.247 PFNA 1 .07 0.268 PFDA U 0.259 PFUnA U 0 .257 PFDoA U PFBS U 0 .255 2 .54 PFHxS 12.9 2.55 PFOS 51 .1 0.258 PFOSA U 0.250 4 .22 4 .70 5 .05 4.87 5.56 LABELED COMPOUND LAB SPIKE CONC . R(a/,)2 RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12.0 12.0 12.0 12 .0 10 .8 902 11 .5 95.7 12.5 104 12.8 107 4.70 5.56 5 .56 5 .41 (1) U =not detecte d (2) R (%) = Percent recovery 16755PF_Dt 2.zls . S6 Approved by. QA/QC Chemist 11 10-d0 d-mm5 -yyyy 000 AXYS AIVALYTIC'AL SER-,/I(=ES LTE) P.O. BOX 2219, 20t5 MILLS RD . WEST, SIDNEY, B.C., EANdDA VOL 3581E1(250) 655-5800 FAX (250) 655-581 I sr p . 59 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_S1_D12 Form 1A/ 2 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name: AXYS ANALYTICAL SERVICE S Sample Collection : 08-Aug-2005 13 :17 Contract No.: 4191 Lab Sample ID : L7932-19 Y2 Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 12-Sep-2005 Time: 19:47 :27 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile: FC5G 167S037 Injection Volume (pL) : 30-0 Blank Data Filename : FC5G 167S031 Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_167S027 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0 .276 0 .251 PFOA 43 .5 0 .247 PFNA 1 .03 0 .268 PFDA 0.315 0 .259 PFUnA U 0.257 PFDoA U 0.25 5 PFBS U 2.54 PFHxS 10 .6 2 .55 PFOS 51 .4 0.258 PFOSA U 0 .250 4.22 4.70 5.05 5.41 4.87 5.56 LABELED COMPOUND LAB SPIKE CONC . R(0~)2 RETEN11ON FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 12 .0 13C4-PFOS(80) 12 .0 13C4-PFOS(99) 12.0 13C2-PFDA 12.0 10.1 84.1 12.2 102 12.0 99.8 12.3 103 4.70 5.56 5.56 5 .41 (1) U =not detecte d (2) R (%) = Percent recovery 16755PF_D1_2ads, s8 Approved by: i`~~-- QA/QC Chemist 11-1dd0-m-m0-yy5yy 04((0 A?CYS AIVALYTIC'-AL SER\/ICES LTD P.O . BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B .C., CANADA Y8L 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 f9 p . 60 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1_012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 08-Aug-2005 13 :10 Contract No. : 4191 Lab Sample ID : L7932-20 Y2 Matrix: SERUM Sample Size: 1 .00 mL Sample Receipt date : 10-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 12-Sep-2005 Time : 20 :01 :42 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G 167S038 Injection Volume (pL) : 30 .0 Blank Data Filename: FC5G 167S039 Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G167S02 7 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA U 0 .25 1 PFOA 63.3 0 .247 PFNA 1 .55 0.268 PFDA 0.331 0.259 PFUnA U 0 .25 7 PFDoA U 0 .255 PFBS U 2.54 PFHxS 17 .0 2 .55 PFOS 76 .7 0 .258 PFOSA U 0 .250 4.70 5.05 5.36 4 .8 7 5 .51 LABELED COMPOUND LAB SPIKE CONC . R(%)z RETENTION FLAG' CONC. FOUND TIME (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4PFOS(99) 13C2-PFDA 12.0 12 .0 12 .0 12 .0 10.3 10 .8 11 .5 11 .1 85.6 89.8 95 .6 92 .3 4.70 5.56 5.56 5.36 (1) U =not detecte d (2) R (%) = Percent recovery 16755PF 01_2 .xis, S9 Approved by: QA//QC Chemist 11-10-05 dd-m m-yyyy 00)(CO AXYS ANALYI-ICAL SE1 ;ir/ICES LTc> P.O. BOX 2219, 2045 611LLS RD . WEST, SIDNEY, B .C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 60 p . 61 AXYS METHOD MLA-042 Rev 02 CUENT ID : PFOS_S1_012 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 08-Aug-2005 13 :14 Contract No . : 4191 Lab Sample ID : L7932-21 Y2 Matrix: SERUM Sample Size: 1,00 mL Sample Receipt date : 10-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID: LC-MS/MS Analysis Date : 12-Sep-2005 Time : 20:15 :59 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FC5G 167S039 Injection Volume ( NL) : 30 .0 Blank Data Filename : FC5G 167S031 Diluti on Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_167S02 7 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA U U 0.256 0.248 PFHpA PFOA PFNA PFDA PFUnA PFDoA U 0 .251 48 .4 0 .247 0.626 0.268 U 0.259 U 0.257 U 0.255 PFBS U 2 .54 PFHxS 11 .9 2 .55 PFOS 71 .9 0.258 PFOSA U 0.250 4 .70 5 .05 4.87 5.51 LABELED COMPOUND LAB SPIKE CONC. R(y,)z RETENTIO N FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 12_0 10 .9 90 .7 13C4-PFOS(80) 12.0 14.0 117 13C4-PFOS(99) 12 .0 12.9 108 13C2-PFDA 12 .0 14 .6 122 4.70 5.56 5.56 5 .41 (1) U =not detected (2) R (%) = Percent recovery 16755PF D1_2.xls, S10 Approved by : _ - QA/QC Chemistd ~~~ IN((6 AXYS AIVALYTIC'~ L SER-,/ICES LTp P.O. BOX 2214, 2045 MILLS RD . WEST, SIDNEY, B.L, CANADA F813S8 Ill. (250) 655-5800 FAX (250) 655-581 1 61 p . 62 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1_D12 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID: Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 11 -Aug-2005 10:56 Contract No . : 4191 Lab Sample ID: L7932-24 Y 2 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date: 12-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 12-Sep-2005 Time : 20 :44 :30 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : Injection Volume (pL) : 30 .0 Blank Data Filename : Dilution Factor: N/A Concentration Units : ng/mL Cal. Ver. Data Filename : CAL VER ID : FC5G 167SO41 FC5G 167S031 FC5G167S02 7 PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0_256 PFHxA U 0.248 PFHpA PFOA PFNA 0 .321 0.251 10 .7 0.247 0.877 0 .268 PFDA 0.458 0 .259 PFUnA 0 .415 0 .257 PFDoA U PFBS U 0.25 5 2 .54 PFHxS U 2.55 PFOS 23 .1 0 .258 PFOSA U 0 .250 4 .22 4 .70 5 .05 5 .36 5.70 5 .56 LABELED COMPOUND LAB SPIKE CONC . R(o/,)' RETENTIO N FLAG' CONC . FOUND TIM E ing (ng ) 13C2-PFOA 12 .0 10.9 90 .5 13C4-PFOS(80) 12 .0 12.3 103 13C4-PFOS(99) 120 13 .0 108 13C2-PFDA 12 .0 12 .4 103 4 .70 5.56 5.56 5.36 (1) U =not detected (2) R (~) = Percent recovery 16755PF D1 _2 .bs . S12 App roved by: Chemist 11-10-05 OA/QC tld-mm-riYY ~)K(A AXYS AIVALYf lCAL SER\/ICES LTE :), P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, 8 1 , CANADA V8L 3S8 TEL (250) 6555800 FAX (250) 655-581 1 6Z p . 63 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS S1 D12 Fom11A12 PERFLUORENATED ORGANICS ANALYSIS REPOR T Lab Name: AXYS ANALYTICAL SERVICE S Sample Collection : 11 -Aug-2005 10 :59 Contract No . : 4191 Lab Sample ID : L7932-25 Y2 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date: 12-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 12-Sep-2005 Time : 20 :58:46 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_167S042 Injection Volume (pL) : 30 .0 Blank Data Filename : FCSG 167S031 Dilution Factor : N/A Concentration Units : ng/mL Cal. Ver. Data Filename: FC5G_167S02 7 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0 .373 0.251 PFOA 17 .1 0 .247 PFNA 0.848 0 .268 PFDA 0.498 0 .259 PFUnA 0 .398 0.257 PFDoA U 0 .255 PFBS U 2.54 PFHxS 3 .76 2 .55 PFOS 20.1 0 .258 PFOSA U 0.25 0 4.22 4 .70 5.05 5.36 5.70 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC . R (%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (n9) 13C2-PFOA 12.0 13C4-PFOS(80) 12.0 13C4-PFOS(99) 12 .0 13C2-PFDA 12 .0 10.1 84 .2 11 .9 98.9 13.6 114 12.5 104 4.70 5.56 5.51 5 .36 (1) U =not detected (2) R (%) = Percent recovery 16755PF 01_2.xls. S13 Approved by., QA/QC Chemist 11-10-05 dd-mm-yyyl' /AXYS AIVALYTICAL SER\/ICES LT:C) P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B .C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 63 p . 64 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PF. 0 S_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 1 1-Aug-2005 12:31 Contract No . : 4191 Lab Sample ID : L7932-23 Y2 Matri x: SERUM Sample Size : 1 .00 mL Sample Receipt date: 12-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID: LC-MS/M S Analysis Date: 12-Sep-2005 Time: 20 :30:13 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Dataflle : FC5G 167SO40 Injection Volume (NL) : 30 .0 Blank Data Filename : FC5G 167S031 Dilution Factor: N/A Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_167S027 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 0 .711 0 .251 PFOA E PFNA PFDA 1 .46 0.268 0 .376 0.259 PFUnA PFDoA U U 0.257 0 .255 PFBS U 2 .54 PFHxS 20.9 2 .55 PFOS E PFOSA U 0.250 4 .22 5 .05 5.36 4 .8 7 LABELED COMPOUND LAB SPIKE CONC . R(96)z RETENTION FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 12 .0 12 .0 12 .0 12.3 15.5 13.7 15 .2 103 129 114 126 4.70 5.56 5.56 5.36 (1) U = not detected ; E = exceeds calibrated linear range, see dilu tion data (2) R (%) = Percent recove ry 16755PF D1_2j ds, S11 tP" a Approved by: QA/QC Chemist 11-10-05 dd-mm-yyyy ~)~(CC+ AXYS AIVALYTICAL SERVICES LT[> P.O . BOX 2219, 2045 MILLS RD . WEST, SIDNEY, B.C., CANADA VOL 358 TEL (250) 655-5800 FAX (250) 655-581 1 6* p . 65 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection: 11-Aug-2005 12:31 Lab Name: AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID: L7932-23 Y21 Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date: 12-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date: Analysis Date: 29-Aug-2005 Instrument ID : LC-MS/M S 13-Sep-2005 Time: 2:12:31 LC Column ID: C1 8 Extract Volume (mL): 2 Sample Datafile: FCSG 167S064 Injection Volume (NL) : 10 .0 Blank Data Filename: FC5G 167S031 Dilution Factor. 3 Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_167S05 9 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 105 0 .741 4.70 D 113 0 .774 5.56 LABELED COMPOUND LAB SPIKE CONC. R("/o)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng ) 13C2-PFOA D 13C4-PFOS(80) 13C4-PFOS(99) D 13C2-PFDA 12.0 12 .0 13 .3 111 11 .6 96.4 4 .70 5.56 (1) U = not detected ; D = dilution data (2) R (%) = Percent recovery :6755PF_D3 2 .ws, S5 Approved by. QA/QC Chemist ~m~ 0)~({4 AXYS AIVALYTICAL SER"CES LTD P.O. BOX 2219, 2045 MILLS RD . WEST, SIDNEY, B .C., CMNAOA V813S8 TEL (250) 655-5800 fAX (250) 655581 1 6 !~ p . 66 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 11-Aug-2005 12 :33 Contract No . : 4191 Lab Sample ID : L7932-26 Y4 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date: 12-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction datae: 29-Aug-2005 Instrument ID: LC-MS/MS Analysis datae: 12-Sep-2005 Time : 21 :55:49 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample data Filename: FCSG 167SO46 Injection Volume (pL) : 30 .0 Blank data Filename : FC5G 167S031 Dilution Factor : N/A Concentration Units : ng/m L Cal. Ver. data Filename: FC5G_167SO44 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U 0 .256 U 0.248 0 .665 0.251 58 .7 0.247 1 .74 0 .268 0.670 0 .259 U U 0.257 0.255 U 2.54 14 .3 2 .55 73 .4 0 .258 U 0 .250 4.23 4 .70 5 .05 5 .41 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC. R(9~)2 RETENTION FLAG' CONC. FOUND TiME (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12.0 12.0 12.0 12 .0 10 .2 84.9 12 .3 102 10.4 87.0 11 .0 92.0 4.70 5.56 5.56 5.36 (1) U =not detected (2) R (%) = Percent recovery 16755PF_D2_2 .)d5, S2 Approved by: _. . QAlQC Chemist 11-10-05 dd-mm-yyyy -010 AXYS ANALYTICAL SEf2ViCES LTLD P.D . BDX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA Y81358 TEL (250) 655S8o0 FAX (250) 655-581 1 66 p . 67 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_Sl D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID : Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 15-Aug-2005 13 :54 Contract No . : 4191 Lab Sample ID : L7932-28 Y2 Matrix: SERUM Sample Size : 1-00 mL Sample Receipt date : 17-Aug-2005 Initial Calibration Date : 12-Seir2005 Extraction Date: 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date: 12-Sep-2005 Time : 22 :10 :04 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafiie: FC5G 167SO47 Injection Volume (NL) : 30.0 Blank Data Filename : FC5G 1675031 Dilution Factor: N/A Concentration Units : ng/mL Cal . Ver. Data Filename : FC5G_167SO44 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA U 0 .25 1 PFOA PFNA PFDA 5.92 0 .247 4 .70 1 .32 0 .268 5 .05 0.486 0.259 5-41 PFUnA PFDoA 0 .272 0.257 U 0.255 5.75 PFBS U 2.54 PFHxS PFOS PFOSA 3 .76 2 .55 4 .87 29 .5 0 .258 5 .56 U 0 .250 LABELED COMPOUND LAB SPIKE CONC. R(a/,)2 RETENTIO N FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 12.0 13C4-PFOS(80) 12.0 13C4-PFOS(99) 12.0 13C2-PFDA 12 .0 10 .5 87 .2 11 .3 94.4 10.4 86.4 13.6 113 4 .70 5.56 5 .56 5 .41 (1) U = not detected (2) R (%) = Percent recovery 16755PF_D2_2 .)ds, Ss Approved by: QA/QC Chemist dd-mm-yyy "-1y 0 -05 AXYS AEVALYTIC'AL SERVICES LTO P.O. BOX 2219, 2045 AHiIS RD. WEST, SIDNEY, B .C., CANADA 48L 358 TEL (250) 655-5800 FAX (250) 655-581 1 67 p . 68 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS S1 D12 Form IA/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 16rAug-2005 09 :43 Contract No .. Matrix : 4191 SERUM Lab Sample ID : L7932-29 Y4 Sample Size: 1 .00 mL Sample Receipt date : 17-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 12-Sep-2005 Time : 22 :24 :21 LC Column ID: C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_167SO48 Injection Volume (NL) : 30.0 Blank Data Filename : FC5G 167S031 Dilution Factor. N/A Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_167SO44 CAL VER ID : PFC-L1N-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA U U 0 .256 0 .248 1 .16 0 .251 30.7 0.247 2 .96 0.268 0 .362 0 .259 U 0 .257 U U 0 .25 5 2.54 7.13 2.55 56 .8 0.258 U 0.250 4 .23 4.70 5.05 5 .36 4.87 5.51 LABELED COMPOUND LAB SPIKE CONC . R(~~o)z RETENTION FLAG' CONC . FOUND TIME (ng) (n9 ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 12.0 12.0 12.0 10 .5 87 .8 11 .9 99 .0 13.7 114 13.4 112 4 .70 5.56 5.56 5.36 (1) U =not detected (2) R (%) = Percent recovery 16755PF_D2 2AS, S4 Approved by. QA/QC Chemist 11-10-os dd-mm-yyyy ~)~(CC AXYS AIV ALYf ICAL SEf2V1CES IL-FE :) P.O. BOX 2219, 2045 AUl1S RD. WEST, SIDNEY, B .C., CANADA VOL 3S8 TEL ( 250) 6555800 FAX (250) 655-581 1 69 p . 69 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1 D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID: Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 16-Aug-2005 09:40 Contract No .: 4191 Lab Sample ID : L7932-30 Y2 Mat rix: SERUM Sample Size: 1 .00 mL Sample Receipt date: 17-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date : 12-Sep-2005 Time : 22 :38:38 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G 167SO49 Injection Volume (NL) : 30.0 Blank Data Filename : FC5G 167S031 Dilu tion Factor: N/A Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_167SO4 4 CAL VER ID : PFC-t1N-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 1 .06 0 .251 PFOA 27.5 0 .247 PFNA 2.60 0 .268 PFDA 0 .430 0.259 PFUnA U 0.257 PFDoA U 0.255 PFBS U 2 .54 PFHxS 5.04 2 .55 PFOS 62.0 0 .258 PFOSA U 0 .250 4.23 4 .70 5 .05 5 .36 4 .87 5.51 LABELED COMPOUND LAB SPIKE CONC . R (%f RETENTION FLAG' CONC. FOUND TIME (n9) (n9) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 12 .0 12.0 12.0 10.3 86.2 13.1 109 12.2 101 13 .7 115 4.70 5.56 5 .56 5 .36 (1) U =not detecte d (2) R (%) = Percent recovery 16755PF_022xk . S5 Approved b Y : 11 -- -1 QA0 IQC Ch- emis0 t dd-m5 m-yyyy 410 AXYS AIVALYTI~~.L SER-,/ICES LTID PO. B0X 2219, 2045 MILLS RD . WEST, SIDNEY, B.C, CANADA VOL 3S8 TEL (250) 6S55800 FAX (250) 655-581 1 67 p . 70 AXYS METHOD MLA-042 Rev 02 PFOS_S1 D12 Form 1A 12 PERFLUORINATED ORGANICS ANALYSIS REPOR T CLIENT ID: Lab Name: AXYS ANALYTICAL SERVICE S Sample Collection : 16-Aug-2005 09:37 Contract No . : 4191 Lab Sample ID : L7932-32 Y2 Matrix : SERUM Sample Size: 1 .00 mL Sample Receipt date : 17-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date: 29-Aug-2005 Instrument ID: LC-MS/MS Analysis Date: 12-Sep-2005 Time: 22 :52:53 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Data file : FC5G 167S050 Injection Volume (pL): 30 .0 Blank Data Filename: FC5G 167S031 Dilution Factor: N/A Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_167SO44 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION FLAG' FOUND LIMIT RETENTION TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0.253 0 .251 PFOA 13.3 0 .247 PFNA 1 .02 0 .268 PFDA 0 .265 0 .259 PFUnA U 0.257 PFDoA U 0.255 PFBS U 2 .54 PFHxS U 2 .55 PFOS 12 .3 0 .258 PFOSA U 0 .250 4 .23 4 .70 5 .05 5 .36 5 .51 LABELED COMPOUND LAB SPIKE CONC. R(%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 13C4 -PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 8 .70 72 .5 12.0 12 .6 105 12.0 13.7 114 12.0 11 .2 93.7 4.70 5.56 5.56 5.36 (1) U =not detected (2) R (%) = Percent recovery 16755PF_D2_2.x 1s, S6 Approved by. QA/QC Chemist dd-mrryyyy ~D))(~' AXYS AfVALYI I~AL SER\/tCES LT[--) P.O. BOX 2219, 2045 MILLS RD . WEST, SIDNEY, B.C., CANADA VOL 3S8 TEL (250) 65S-5800 FAX (250) 655-581 1 -70 p . 71 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Lab Name : AXYS ANALYTICAL SERVICES Sample Collection: 16-Aug-2005 09 :35 Contract No. : 4191 Lab Sample ID: L7932-33 Y2 Matrix: SERUM Sample Size: 1 .00 mL Sample Receipt date : 17-Aug-2005 Initial Calibrati on Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/MS Analysis Date : 12-Sep-2005 Time : 23 :07:08 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample Datafite: FC5G 167S051 Injection Volume (NL): 30 .0 Diluti on Factor : N/A Concentration Units : ng/m L Blank Data Filename: FC5G 167S031 Cal. Ver. Data Filename : FC5G_167SO44 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0.454 0.251 PFOA 15.5 0.247 PFNA 0 .660 0.268 PFDA U 0 .259 PFUnA U 0 .257 PFDoA U 0 .255 PFBS U 2 .54 PFHxS U 2 .55 PFOS 12.7 0.258 PFOSA U 0.250 4.23 4.70 5.05 5.51 LABELED COMPOUND LAB SPIKE CONC . R)2 RETENTIO N FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 12.0 13C4-PFOS(80) 12.0 13C4-P FOS(99) 12.0 13C2-PFDA 12.0 10 .7 89.1 14 .0 116 15 .2 126 14.1 118 4 .70 5 .56 5 .56 5 .36 (1) U =not detected (2) R (h) = Percent recovery 16755PF_D2_2.bs, S7 Approved by: .; ~ QA/QC Chemist 11-10-05 dd-mm-yyyy ~))~(0 AXYS AIVALVTICAL SERVICES LT[] P .O . BOX 2219, 2045 MIt15 RD. WEST, SIDNEY, B .C., (ANADAY81358 TEl (250) 655-5800 FAX (250) 655-581 1 1-7 p . 72 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1 D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 17-Aug-2005 18 :11 Contract No. : 4191 Lab Sample ID : L7932-35 Y 2 Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 19-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 :21 :23 LC Column ED : C1 8 Extract Volume (mL) : 2 Sample Datafile: FCSG 167S052 Injection Volume (NL): 30 .0 Blank Data Filename : FCSG 167S031 Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_167SO44 CAL VER ID : PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0.256 PFHxA U 0.248 PFHpA 0 .352 0.251 PFOA 74 .6 0 .247 PFNA 2 .16 0 .268 PFDA 0.466 0.259 PFUnA 0 .384 0.257 PFDoA U 0.255 PFBS U 2.54 PFHxS 13 .4 2 .55 PFOS 91 .0 0 .258 PFOSA U 0 .25 0 4.23 4.70 5 .05 5 .36 5.70 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC. R(g6)z RETENTION FLAG' CONC . FOUND TIME (n9) (ng) 13C2-PFOA 12.0 9 .13 76 .0 13C4-PFOS(80) 12.0 11 .3 94.3 13C4-PFOS(99) 12 .0 11 .3 94_6 13C2-PFDA 12 .0 11 .6 96 .5 4.70 5.56 5 .56 5 .36 (1) U =not detected (2) R (~o) = Percent recovery 16755PF D2 2_xls, S8 Approved by: c~ T'~ ttao a5 QA/QC Chemist dd-mm-yyy y aJ~ICO AXYS AIVALYTICAL SERVICES LTr-) P.O. BOX 2219, 2045 MILLS U. WEST, S(DNEY, B.C., CANADA VOL 3S8 TEL (250) 6555800 FAX (250) 655-581 1 1A p . 73 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1_D12 Form 1A 12 PERFLUORiNATED ORGANICS ANALYSIS REPORT ID : Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 18-Aug-2005 18 :15 Contract No . : 4191 Lab Sample ID: L7932-39 Y4 Matrix : SERUM Sample Size: 1 .00 mL Sample Receipt date: 23-Aug-2005 Initial Calibration Date : 12-Sep-2005 Extraction Date: Analysis Date: 29-Aug-2005 Instrument ID : LC-MS/MS 13-Sep-2005 Time : 0:18:25 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafie : FC5G_1675056 Injection Volume (pL) : 30.0 Blank Data Filename : FC5G 167S031 Dilution Factor: N/A Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_167SO44 CAL VER ID: PFC-LiN-044CS-F COMPOUND LAB CONC FLAG' FOUND DETECTION RETENTION LIMIT 71ME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA U 0 .25 1 PFOA 9 .66 0.247 PFNA 1 .35 0.268 PFDA 0.375 0.259 PFUnA U 0 .257 PFDoA U 0 .255 PFBS U 2.54 PFHxS 4 .52 2.55 PFOS 26 .6 0_258 PFOSA U 0 .250 4 .70 5 .05 5.36 4 .8 7 5 .51 LABELED COMPOUND LAB SPIKE CONC. FLAG' CONC. FOUND (n9) (ng ) R (a/,)2 RETENTIO N TIME 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99 ) 13C2-PFDA 12.0 9 .15 12.0 13 .8 12.0 12.8 12 .0 12.8 76 .2 115 107 106 4.70 5.56 5 .56 5 .36 (1) U = not detected (2) R (%) = Percent recovery 16755PF_D2_2.,ds, S12 Approved by : QAlQC Chemist 11-10-05 dd-mm-yyyy e0(0 AXYS ANALYTIC`AL SER\/ICES LTC), P.O. BOX 2219, 20t5 AOLIS RD . WEST, SIDNEY, B_C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 73 p . 74 AXYS METHOD MLA-042 Rev 02 CLIENT PFOS_S1_D12 Form 1AJ2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICES Sample Collection: 18-Aug-2005 18 :17 Contract No. : Matrix: 4191 SERUM Lab Sample ID: WG16755-105 Y2i (DUP L7932-37 Y2i (A)) Sample Size: 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 : 13-Sep-2005 Time: 3 :09:35 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_167S068 Injection Volume (pL) : 10.0 Blank Data Filename : FC5G 167S031 Dilution Factor: 3 Concen tration Units : ng/m L Cal . Ver. Data Filename: CAL VER ID : FC5G_167S059 PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 103 0 .741 4.70 LABELED COMPOUND LAB SPIKE CONC. R(a/a)Z RETENTION FLAG' CONC. FOUND TIME (ng) (ng ) 13C2-PFOA 13C4PFOS(80 ) 7 3C4-PFOS(99) 13C2-PFDA D 12.0 9 .66 80.5 4 .70 (1) U = not detected; D= dilu tion data (2) R (%) = Percent recovery 16755PF_D3_2. )ds. S9 Approved by : CP =wmw,~' QA/QC Chemist 11-10-05 dd-mm-m 4)](0 4AXyS AIVALYT1C'AL SE12VI~CES LTC7 P.O . BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA Y8t 3S81E1 (250) 655-5800 FAX (250) 6 55-581 1 7 f+ p . 75 AXYS METHOD MLA-042 Rev 02 CLIENT ID : PFOS_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collection : 18-Aug-200518 :17 Lab Name : AXYS ANALYTICAL SERVICES Contract No. : Matrix : 4191 SERUM Lab Sample ID : WG16755-105 Y2 (DUP L7932-37 Y2) Sample Size : 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 : C1 8 Extract Volume (mL) : 2 Sample Datafile: Injection Volume (NL) : 30 .0 Blank Data Filename: Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename : CAL VER ID : FCSG_167S054 FC5G_167S031 FC5G_167SO44 PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 2 .62 0 .251 PFOA E PFNA 1 .83 0.268 PFDA 0.894 0.259 PFUnA U 0.257 PFDoA U 0.255 PFBS U 2 .54 PFHxS 14.5 2 .55 PFOS 72.7 0 .258 PFOSA U 0 .250 4 .18 5.05 5.36 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC . R( %)2 RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 12 .0 12.0 12.0 10 .2 85 .0 4.70 14 .5 121 5.51 13.2 110 5.51 15.0 125 5 .36 (1) U = not detected ; E = exceeds calibrated linear range, see dilution data (2) R (%) = Percent recove 16755PF 02_2xls. S10 Appror ved y by : 1 .!~1 -- --- - 1 QAiQ0 C Chemist -05 dd-m m-yyyy ~~(~@ .`XYS AIVALYf'ICAL SERN/1CES LTiD P.O . BOX 2219, 2045 MILLS RD. WEST, SfDNEY, B .t, CANADA V8L 358 TEL (250) 655-5800 FAX (250) 655581 1 1S p . 76 AXYS METHOD MLA-042 Rev 02 PFOS S1 D12 Form I A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T CLIENT ID : Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 18-Aug-2005 18:17 Contract No . : 4191 Lab Sample ID: L7932-37 Y2 Mat rix: SERUM Sample Size: 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 : 23:35:39 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_167S053 Injection Volume (pL): 30 .0 Blank Data Filename : FC5G 167S031 Dilution Factor : NIA Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_167SO44 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 2 .08 0.251 PFOA E PFNA 1 .75 0.268 PFDA 0.910 0 .259 PFUnA U 0 .25 7 PFDoA U 0 .255 PFBS U 2 .54 PFHxS 13.4 2.55 PFOS 70.3 0.258 PFOSA U 0.250 4 .23 5.05 5.36 4.8 7 5.51 LABELED COMPOUND LAB SPIKE CONC . R(o/a)z RETENTION FLAG' CONC. FOUND TIME (n9) (ng) 13C2-PFOA 12 .0 9.98 13C4-PFOS(80) 12 .0 13.5 13C4-PFOS(99) 12 .0 13.0 13C2-PFDA 12 .0 13.7 83.1 112 108 114 4 .70 5.51 5.51 5.36 (1) U = not detected; E = exceeds calibrated linear range, see dilution dat a (2) R (%) = Percent recovery 16755PF_02 2xls, S9 Approved by: QA/~ QC~ Chemist 11-10-05 dd,,,,,,,-m , 4)~((A ~XYS ANALYT B~~L SER- /I (= ES LT 11--) P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY. B.C. CANADA Y8l 358 iEl (250) 6555800 FAX (2S0) 655581 1 76 p . 77 AXYS METHOD MLA-042 Rev 02 PFOS_Sl_D12 Form 1A12 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) Matrix : SERUM Sample Size: 1 .00 mL Sample Receipt date : 23-Aug-2005 Initial Calibration Date: 12-Sep-2005 Extraction Date : 29-Aug-2006 Instrument ID : LC-MS/MS Analysis Date : 13-Sep-2005 Time : 2 :55 :19 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample Datafi le : FC5G_167S067 Injection Volume (NL) : 10.0 Blank Data Filename : FC5G_167S031 Diluti on Factor. 3 Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_167S05 9 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA D 104 0 .741 4 .70 LABELED COMPOUND LAB SPIKE CONC . R(% )z RETENTIO N FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D 12.0 9 .67 80 .6 4 .70 (1) U = not detected; D= dilution data (2) R (k) = Percent recovery 16755PF_03_2.bs, S8 11-10-05 Approved by QA/QC Chemist dd mm yyyy 0))((0 &,X-YS ANALY7 ICAL SERVICES LTC) P.O . BOX 2214, 2045 MILlS RD. WEST, SIDNEY, B.C., CANADA V8l 3S8 TEL (250) 655-5800 FAX (250) 65S581 1 77 p . 78 AXYS METHOD MLA-042 Rev 02 PFOS S1_012 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT CLIENT 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 ml Sampie 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 : C1 8 Extract Volume (mL) : 2 Sample Datafi le : FC5G_167S069 Injection Volume (pL) : 10 .0 Blank Data Filename : FC5G_167S031 Dilution Factor : 3 Concentration Units : ng/m L Cal . Ver. Data Filename : CAL VER ID: FC5G_167S059 PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENT10N FLAG' FOUND LIMIT TIME PFPeA UD 0 .767 PFHxA UD 0 .744 PFHpA UD 0 .753 PFOA D 96.1 0.741 PFNA UD 0 .804 PFDA UD 0.777 PFUnA UD 0.770 PFDoA UD 0.765 PFBS UD 7.62 PFHxS 0 16 .3 7.65 PFOS 0 67 .8 0.774 PFOSA UD 0 .750 4.70 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC . R(%)2 RETENTION FLAG' CONC . FOUND TIME (ng) (ng ) 13C2-PFOA D 12.0 11 .4 94 .7 13C4-PFOS(80) D 12 .0 12.1 101 13C4-PFOS(99) D 12.0 11 .1 92 .7 13C2-PFDA 0 12_0 9 .86 82 .2 4.70 5.56 5.56 5.41 (1) U = not detected; D= diluti on dat a (2) R (%) = Percent recove ry 16755PF_03 2.)ds, S10 Approved by. 1-1 1 QA/QC Chemist dd-mm y~ yyy AXYS ANALYTIC--AL SER-,/I(--ES LTc) P.O . BOX 2219, 2045 AliLlS RD . WEST, SIDNEY, B.C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655581 1 71? p . 79 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID : Sample Collection : 22-Aug-2005 16 :20 Lab Name: AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID: L7932-41 Y4 (A) Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date : 24-Aug-2005 Initial Calibrati on Date: 15-Sep-2005 Extraction datae : 06-Sep-2005 Instrument ID : LC-MS/M S Analysis datae : 16-Sep-2005 Time : 13 :23:23 LC Column ID: C1 8 Extract Volume (mL) : 2 Sample data Filename: FC5G_176S011 Injection Volume (NL) : 10.0 Blank data Filename : FC5G_159S016 Dilu tion Factor : 3 Concentration Units : ng/mL Cal. Ver. data Filename : FC5G_176S008 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB CONC FLAG' DETECTION RETENTION FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0 .638 UD 0 .620 UD 0628 D 19 .6 0 .618 D 1 .78 0 .670 D 0 .952 0 .648 UD 0 .640 UD 0 .638 UD 0 .635 D 5 .56 0 .638 D 8 .91 2 .58 UD 0 .625 4 .70 5 .12 5 .46 4 .93 5 .56 LABELED COMPOUND LAB SPIKE CONC. R (%)2 RETENTIO N FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D D D D 12 .0 12.0 12.0 12.0 11 .1 92 .9 11 .3 94 .3 13 .6 113 11 .7 97 .6 4 .70 5 .56 5 .56 5 .41 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 1681 4PF05_2. )ds . S2 Approved by : QA/QC Chemist 11-10d-d-2mm0-0yy5yy "0)}(C4 A7CVS AIVALYf IC'AL SER-,/ICES LTp P .D . BOX 2214, 2045 MILLS RD. WEST, S14NEY, B.C, CANADA Y8l 358 TEL (250) 655-5800 FAX (250) 655-581 1 71 p . 80 AXYS METHOD MLA -042 Rev 03 CLIENT PFOS_St_o12 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPORT ID : Sample Collection : 22-Aug-2005 16 :20 Lab Name : AXYS ANALYTICAL SERVICE S Con tr act No. : 4191 Lab Sample ID : WG16814-104 Y3 Ma trix- SERUM Sample Size : 1 .00 mL Sample Receipt date : 24-Aug-2005 Initial Calibration Date: 15-Sep-2005 Extraction Date : 06-Sep-2005 Instrument ID : LC-MS/M S Analysis Date : 16-Sep-2005 Time : 0 :08 :02 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_175S013 Injecti on Volume (pL) : 10 .0 Blank Data Filename : FC5G_159S016 Dilution Factor : 3 Concen tration Units : ng/m L Cal. Ver. Data Filename : FC5G_175S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC FLAG' DETECTION RETENTION FOUND LIMIT TIME PFPeA UD 0 .63 8 PFHxA UD 0 .620 PFHpA UD 0 .628 PFOA D 21 .1 0 .618 PFNA D 1 .56 0 .670 PFDA 0 1 .00 0 .648 PFUnA PFDoA UD UD 0 .640 0 .638 PFBS UD 0 .635 PFHxS PFOS D 2 .62 0 .638 D 12.8 2 .58 PFOSA UD 0 .625 4 .70 5 .05 5 .41 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC . FLAG' CONC . FOUND (ng) (ng) R (%)2 RETENTIO N TIME 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D 12.0 0 12.0 D 12.0 0 12.0 13 .4 14 .7 12.2 13 .8 112 122 102 115 4 .70 5 .56 5 .56 5 .41 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16814PFD4_2xls, S3 Approved by : QA/QC Chemist 11-10-2005 dd-mm-yyy y M~)~((0 AXYS AIVALYTICAL SERVICES LTID P .O . BOX 2219, 2045 MILLS RD . WEST, SIDNEY, B.C., CANADA Y8 1 3S81EL (2S0) 6555800 FAX (250) 655-581 1 go p . 81 AXYS METHOD MLA-0 42 Rev 03 CLIENT PFOS_St_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT (D- Sample Collection : 24-Aug-2005 17:18 Lab Name: AXYS ANALYTICAL SERVICES Con tract No. : 4191 Lab Sample ID : L7932-44 Y 3 Ma trix : SERUM Sample Size : 1 .00 mL Sample Receipt date : 26-Aug-2005 Initial Calibrati on Date: 15-Sep -2005 Extracti on Date: 06-Sep-2005 Instrument ID: LC-MS/M S Analysis Date : 16-Sep-2005 Time : 0 :36:32 LC Column ID: C1 8 Extr act Volume (mL) : 2 Sample Datafile : FC5G175S015 Injection Volume (pL) : 100 Blank Data Filename : FC5G_159S016 Diluti on Factor: 3 Concen tr ati on Units : ng/m L Cal. Ver . Data Filename : FC5G_175S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0 .638 UD 0 .620 UD 0 .628 D 32.7 0 .618 D 0 .963 0 .670 UD 0 .648 UD 0 .640 UD 0 .638 UD 0 .635 D 14 .5 0 .638 D 41 .5 2 .58 UD 0 .625 4 .70 5 .05 4 .87 5 .51 LABELED COMPOUND LAB SPIKE CONC . R (%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (n9 ) 13C2-PFOA 13C4-P FOS(80) 13C4-PFOS(99) 13C2-PFDA D 12 .0 0 12 .0 D 12 .0 D 12 .0 15.1 14 .2 14.4 14 .2 126 118 120 118 4 .70 5 .56 5 .56 5 .41 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16814PFD4_2.xls, S5 Approved by: QA/QC Chemist 11-10-2005 dd-mm-yyyy ~))](CC AXYS AfVALYTIC-AL SERVICES LTL7 P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655-5811 91 p . 82 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collection : 25-Aug-2005 10 :45 Lab Name : AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID : L7932-43 Y 3 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date : 26-Aug-2005 Initial Calibrati on Date : 15-Sep-2005 Extraction Date : 06-Sep-2005 Instrument ID: LC-MS/M S Analysis Date : 16-Sep-2005 Time : 0 :22:18 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Datafite : FC5G_175S014 Injection Volume (NL) : 10 .0 Blank Data Filename : FC5G_159S016 Dilution Factor : 3 Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_175S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PF$S PFHxS PFOS PFOSA UD 0 .638 UD 0 .620 UD 0 .628 D 10 .2 0 .618 UD 0 .670 UD 0 .648 UD 0 .640 UD 0 .638 UD 0 .635 D 0 .905 0 .638 0 24 .2 2 .58 UD 0 .625 4 .70 4 .87 5 .56 LABELED COMPOUND LAB SPIKE CONC. R(y,)2 RETENTIO N FLAG' CONC . FOUND TIME (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D D D D 12.0 12.0 12.0 12 .0 12 .7 106 11 .2 92.9 14 .5 121 14 .2 118 4 .70 5 .56 5 .56 5 .41 (1) U = not detected ; D = dilution data (2) R (%) = Percent recovery 16814PFD4_2.xls, S4 Approved by : U/f QA/QC Chemist 11-10d-d2-m0m0-yy5yy i~]((8 AXYS AIVALYf ICAL SERVICES LT[D P .O . BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B .C., CANADA VOL 3S8 TEL ( 250) 655-5800 FAX (250) 655-581 1 9z p . 83 AXYS METHOD MLA -042 Rev 03 CLIENT PFOS_S1_012 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Sample Collection : 25-Aug-2005 10 :48 Lab Name: AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID : L7932-45 Y2 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date : 26-Aug-2005 Initial Calibra ti on Date : 13-Sep-2005 Extraction Date : 06-Sep-2005 Instrument ED : LC-MS/M S Analysis Date : 13-Sep-2005 Time : 10 :03 :59 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafi le : FC5G_168S023 Injection Volume (pL) : 30 .0 Blank Data Filename : FC5G_168S015 Dilu tion Factor: N/A Concentra ti on Units : ng/m L Cal. Ver. Data Filename : FCSG_168S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA 0 .401 0 .251 PFOA 80 .5 0 .247 PFNA 1 .77 0 .268 PFDA PFUnA 0 .841 0 .259 0 .343 0 .257 PFDoA U 0.255 PFBS U 0 .254 PFHxS 49 .4 0 .255 PFOS E PFOSA U 0250 4 .18 4 .70 5 .05 5 .36 5 .70 4 .87 LABELED COMPOUND LAB SPIKE CONC . R(y,)z RETENTION FLAG' CONC . FOUND TIM E (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 12 .0 12 .0 12 .0 11 .5 95 .9 4 .70 10.3 86.0 5 .56 12.7 106 5 .56 12.6 105 5 .36 (1) U = not detected ; E = exceeds calibrated linear range, see diluti on data (2) R (%) = Percent recovery 16814PFD3_2x1s, S10 Approved by: 1~ " 11-to-2o0s QA/QC Chemist dd-mm-yyy y 010 AXYS ANALYTK`AL SERVICES LTI ::> P.O. BOX 2219, 2055 NULLS RD. WEST, SIDNEY, B.C., CANADA VOL 3S8 TEL (250) 6555800 FAX (250) 655-581 1 83 p . 84 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_S1_012 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name: AXYS ANALYTICAL SERVICES Sample Collection : 25-Aug-2005 10 :48 Contract No . : 4191 Lab Sample ID : L7932-45 Y2i Matrix : SERUM Sample Size : 1 .00 mL 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 : 11 :29 :32 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_168S029 Injec tion Volume (pL): 10 .0 Blank Data Filename : FC5G_168S015 Dilution Factor: 3 Concentration Units : ng/mL Cal . Ver. Data Filename : FC5G_168S01 0 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB CONC FLAG' FOUND DETECTION RETENTION LIMIT TIME PFPeA X PFHxA X PFHpA X PFOA X PFNA X PFDA X PFUnA X PFDoA X PFBS X PFHxS X PFOS PFOSA 0 163 X 0 .645 5 .51 LABELED COMPOUND LAB SPIKE CONC . R(%)z RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA X 13C4-PFOS(80) X 13C4-PFOS(99) D 13C2-PFDA X 12 .0 10 .7 89 .0 5 .56 (1) D= dilution data ; X = results reported separately (2) R (%) = Percent recovery 16614PF03_2 xls, S15 Approved by : is~i~ - QA/QC Chemist 11-10-2005 dd-mm-yyyy )))((C' AXYS ANALVTICAL SERVICES LT[D P.O . BOX 2219, 2045 MILLS RD . WEST, SIDNEY, l.C., CANADA VOL 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 g~' p . 85 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_Si_D12 Form 1Al2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Sample Collection : 25-Aug-2005 18 :35 Lab Name : AXYS ANALYTICAL SERVICE S Contr act No. : 4191 Lab Sample ID : L7932-47 Y2i Ma trix : SERUM Sample Size: 1 .00 ml Sample Receipt date: 31-Aug-2005 Initial Calibration Date: 13-Sep-2005 Extraction Date : 06-Sep-2005 Instrument ID : LC-MS/MS Analysis Date : 13-Sep-2005 Time : 11 :43:48 LC Column ID: C1 8 Ex tract Volume (mL): 2 Sample Datafile : FC5G_168S030 Injection Volume (NL) : 10 .0 Blank Data Filename : FC5G_168S015 Dilution Factor : 3 Concen tration Units : ng/m L Cal . Ver. Data Filename : FC5G_168S01 0 CAL VER ID: PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0 .638 UD 0 .620 UD 0 .62 7 0 63 .3 0 .617 4 .70 D 1 .03 0 .670 505 D 0 .775 0 .647 5.36 UD 0_64 1 UD 0 .637 UD 0 .635 D 11 .9 0 .637 4 .8 7 D 73 .1 0 .645 5 .56 UD 0 .625 LABELED COMPOUND LAB FLAG' SPIKE CONC. R (%)2 RETENTIO N CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS(80) 13C4.PFOS(99) 13C2-PFDA 0 12.0 D 12 .0 D 12.0 D 12 .0 13 .4 112 13 .4 111 12 .1 101 11 .4 95 .2 4 .70 5 .56 5 .56 5 .41 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16814PFD3_2. xAs, 816 Approved by: QA/QC Chemist t~-1a2odd0 -mm5 -yyyy 080 AXYS AIVALYTICAL SERVICES LT [D P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B .C., CANADA V81 35B TEL ( 250) 655-5800 FAX (250) 655-581 1 g ~, p . 86 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_s1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 25-Aug-2005 18:39 Contract No. : 4191 Lab Sample ID: L7932-48 Y 1 Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date : 31-Aug-2005 Initial Calibration Date : 13-Sep-2005 Extraction Date : 06-Sep-2005 Instrument ID : LC-MSIM S Analysis Date : 13-Sep-2005 Time : 10 :32 :29 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FC5G 168S025 Injection Volume (NL) : 30 .0 Blank Data Filename : FC5G 168S015 Dilution Factor : N/A Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_168S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION FLAG' FOUND LIMIT RETENTION TIME PFPeA U 0 .256 PFHxA U 0 .248 PFHpA U 0 .25 1 PFOA 14 .6 0 .247 PFNA 1 .49 0 .268 PFDA 0 .312 0 .259 PFUnA U 0 .25 7 PFDoA U 0 .255 PFBS U 0 .254 PFHxS 2 .29 0.255 PFOS 30 .8 0 .258 PFOSA U 0,250 4 .70 5.05 5.36 4 .8 7 5 .51 LABELED COMPOUND LAB SPIKE CONC . R(y,)z RETENTION FLAG' CONC . FOUND TIME (ng) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12.0 12.0 12 .0 12 .0 12.0 99.8 15.7 131 15.9 133 16.2 135 4 .70 5 .51 5 .51 5.36 (1) U = not detecte d (2) R (%) = Percent recovery 16814PFD3_2.xls, S12 Approved by: QA ~ /Q ~ .eC ;is'` Chemist 11-10-2005 dd-mm-yyyy 6))((0 AXYS ANALYTICAL SER\/ICES LTID P.O . BOX 2219, 2045 MILIS RD . WEST, SIDNEY, B .C., CANADA V81 3S8 TEL (250) 6555800 FAX (250) 655-581 1 gb p . 87 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_SI_Dt2 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID: Sample Collection : 29-Aug-2005 09 :59 Lab Name : AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID: L7932-49 Y 3 Matrix : SERUM Sample Size: 1 .00 mL 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 : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FC5G 175S016 Injection Volume (ML) : 10 .0 Blank Data Filename : FC5G_159S016 Dilution Factor : 3 Concentration Units : ng/m L Cal. Ver. Data Filename : CAL VER ID : FC5G175S01 0 PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND UMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0 .638 UD 0 .620 UD 0 .628 D 7.21 0 .618 1) 1 .30 0.670 D 0 .650 0 .648 UD 0 .640 UD 0 .638 UD 0 .635 D 9 .50 0 .638 D 38.9 2 .58 UD 0 .625 4 .70 5 .05 5 .41 4 .87 5 .56 LABELED COMPOUND LAB SPIKE CONC. FLAG' CONC . FOUND (ng) (ng) R(% )z RETENTION TIME 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA D 12.0 D 12.0 0 12.0 D 12 .0 10 .9 11 .9 10 .7 10 .8 91 .0 99 .4 89 .2 89.7 4 .70 5.56 5.56 5.41 (1) U= not detected ; D = dilution data (2) R (%) = Percent recovery 16814PFD4_2.x1s, ss Approved by : ~s~inl'f~ QA/QC Chemist 11- 1 0-2005 dd-mm-yyy y 01(0 AXYS AIVALYI-It~L SERVI1CES LT(::) P.O . BOX 2219,204S IAIUS RD_ WEST, SIDNEY, 81, CANADA Y8 1. 3S8 IEL (250) 655-5800 FAX (250) 655-581 1 97 p . 88 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID : Sample Collection : 31-Aug-2005 09 :56 Lab Name: AXYS ANALYTICAL SERVICE S Contract No. : 4191 Lab Sample ID: WG16982-104 i Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 01-Sep-2005 Initial Calibration Date : 22-Sep-2005 Extraction Date : 21-Sep-2005 Instrument ID : LC-MS/M S Analysis Date: 23-Sep-2005 Time: 0 :41 :20 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile: FCSG_181S054 Injection Volume (pL) : 10 .0 Blank Data Filename : FC5G_181S070 Dilu tion Factor: 3 Concentration Units : ng/m L Cal. Ver. Data Filename: FC5G_181SO4 8 CAL VER ID : PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0 .639 PFHxA UD 0 .620 PFHpA UD 0 .628 PFOA D 26.7 0 .618 PFNA D 1 .00 0 .670 PFDA UD 0 .648 PFUnA UD 0.641 PFDoA UD 0.638 PFBS UD 0.635 PFHxS D 5.34 0 .638 PFOS D 32.7 0 .645 PFOSA UD 0 .625 4 .65 5 .05 4 .80 5 .46 LABELED COMPOUND LAB SPIKE CONC. R(a/o)z RETENTION FLAG' CONC. FOUND TIME (n9) (n9) 13C2-PFOA 13C4-P FOS (80) 13C4-PFOS (99) 13C24PFDA D D D 12.0 12.0 12 .0 D 12 .0 12.3 103 12 .4 103 11 .6 97 .0 10.5 87.3 4.65 5.46 5.46 5 .36 (1) U = not detected; D= dilution data (2) R (%) = Percent recover y 16982PFD1_2 .4s, S4 Approved by: QA/QC Chemist 0-0 dd-,,m yy~y ONO AXYS AIVALYfI~AL SER\/ICES LTiD P.O . BOX 2219, 2045 MILLS RD . WEST, SIDNEY, 8.(., CANADA V81 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 8g p . 89 AXYS METHOD MLA-042 Rev 03 PFOS_Si_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T CLIENT ID : Sample Collection : 31-Aug-2005 09 :56 Lab Name: AXYS ANALYTICAL SERVICES Contract No . : 4191 Lab Sample ID : L7932-51 i(A) Matrix : SERUM Sample Size : 1 .00 mL 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 : C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_181S053 Injection Volume (pL): 10 .0 Blank Data Filename : FC5G_181S070 Dilution Factor : 3 Concentration Units : ng/m L Cal. Ver. Data Filename : FC5G_181SO48 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0 .639 PFHxA UD 0 .620 PFHpA UD 0 .628 PFOA D 27.0 0.618 PFNA D 1 .55 0.670 PFDA UD 0.648 PFUnA UD 0.641 PFDoA UD 0 .638 PFBS UD 0 .635 PFHxS D 5 .27 0 .638 PFOS D 28.5 0 .645 PFOSA UD 0.625 4.65 4.99 4 .80 5.46 LABELED COMPOUND LAB FLAG' SPIKE CONC. R(o,)2 RETENTION CONC. FOUND TIME (ng) (ng ) 13C2-PFOA D 12 .0 13C4-PFOS (80) D 12 .0 13C4-PFOS (99) D 12.0 13C2-PFDA D 12 .0 11 .4 94 .9 14.6 122 13.5 113 10.1 83 .8 4 .65 5 .46 5.46 5 .36 (1) U = not detected; D= dilution data (2) R (4/6) = Percent recovery 16982PF07 2.xls, S3 Approved by: QA/QC Chemist 19-10-05 dd. mm-yyyy d)~({C~ AXYS AIVALYTICAL SER-s/1CES LTE :) P.O. BOX 2214, 2045 AUL15 RD. WEST SIDNEY, B .C., CANADA Y8L 3S8 TEL (250) 655-5800 FAX (250) 655-5811 9`1 P . 90 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_SI_0I2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 31-Aug-2005 10 :03 Contract No . : 4191 Lab Sample ID : L7932-52 i Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 01-Sep-2005 Extraction Date : 21-Sep-2005 Analysis Date : 23-Sep-2005 Time: 0 :55:34 Initial Calibration Date : 22-Sep-2005 Instrument ID: LC-MS/MS LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_181S055 Injection Volume (L) : 10.0 Blank Data Filename : FC5G 181S070 Dilution Factor: 3 Concentration Units : ng/mL Cal . Ver. Data Filename: FC5G_181SO48 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0.63 9 PFHxA UD 0.620 PFHpA UD 0.628 PFOA D 72 .9 0 .618 PFNA D 1 .51 0 .670 PFDA D 0.739 0 .648 PFUnA UD 0 .641 PFDoA UD 0 .638 PFBS UD 0 .635 PFHxS D 12.5 0.638 PFOS D 87.6 0.645 PFOSA UD 0.625 4 .65 4 .99 5.36 4 .80 5 .46 LABELED COMPOUND LAB FLAG' SPIKE CONC. R ( o/,)z RETENTION CONC . FOUND TIME (n9) (n9 ) 13C2-PFOA 13C4-PFOS 13C4-PFOS (99) 13C2-PFDA D 12.0 (80) D 12.0 D 12.0 d 12.0 12 .2 102 4.65 12 .9 108 5.46 13 .2 110 5 .46 10 .3 85.6 5 .36 (1) U= not detected; D = dilution data (2) R (%) = Percent recovery 1 6982 PF01_2.ds, S5 Approved by : ~-~ QAlQC Chemist 11-10-05 dd-mm-yysy ~)~((@ AXYS AIVALYi-ICAL SEIZVICES LTID P .O. BOX 2219, 20451dIUS RD. WEST, SIDNEY, B .C., CANADA Y8l 3S8 TEL (250) 655-5800 FAX (250) 655-58] 1 q6 P . 91 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS St D72 Form 1AJ2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collection: 31-Aug-2005 10 :32 Lab Name : AXYS ANALYTICAL SERVICE S Contract No . : 4191 Lab Sample ID : L7932-53 1 Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 01-Sep-2005 Initial Calibration Date : 22-S ep-2005 Extraction Date : 21-Sep-2005 Instrument ID : LC-MS/MS Analysis Date: 23-Sep-2005 Time : 1 :09 :49 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FC5G_181S056 Injection Volume (pL) : 10.0 Blank Data Filename: FC5G_181S070 Dilution Factor : 3 Concentration Units : ng/mL Cal . Ver. Data Filename : CAL VER ID : FC5G_181SO48 PFC-LIN-0 55CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0.639 PFHxA UD 0.620 PFHpA D 1 .95 0.628 PFOA D 110 0.618 PFNA D 2 .92 0.670 PFDA D 1 .32 0 .648 PFUnA UD 0 .64 1 PFDoA UD 0 .638 PFBS UD 0 .635 PFHxS D 20 .0 0 .638 PFOS D 111 0 .645 PFOSA UD 0.625 4 .18 4 .65 5.05 5.36 4 .80 5 .46 LABELED COMPOUND LAB SPIKE CONC . R(~/,)2 RETENTION FLAG' CONC. FOUND TIME (n9) (n9) 13C2-PFOA D 12.0 13C4-PFOS (80) D 12.0 13C4-PFOS (99) D 12.0 13C2-PFDA D 12.0 12 .1 101 4 .65 12 .0 99.6 5 .46 12 .7 1 p6 5 .46 10 .8 90 .0 5.36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recover y 16982PF DI _2-4s. S6 App roved by : ~ QA/QC Chemist 11 -10- 05 cd-mm-yyyy 400 AXYS AIVALYi-ICAL SER\/ICES LT[D P.O . BOX 2219, 2015 MILLS M. WEST, SIDNEY, B .C., CANADA V81 3S$ TEI. (250) 655-5800 FAX (250) 655-581 1 q1 p . 92 AXYS METHOD MLA-0 42 Rev 03 CLIENT PFOS S1 D72 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID: Sample Collection : 31-Aug-2005 10 :30 Lab Name: AXYS ANALYTICAL SERVICE S Con tr act No . : 4191 Lab Sample ID : Matrix : SERUM Sample Size : L7932-54 i 1 .00 mL Sample Receipt date : 01-Sep-2005 Initial Calibration Date: 22-Sep-2005 Extraction Date : 21-Sep-2005 Instrument ID : LC-MS/M S Analysis Date : 23-Sep-2005 Time : 1 :24 :02 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Data fi ie: FC5G_181S057 Injection Volume (NL) : 10 .0 Blank Data Filename : FC5G 181S070 Dilution Factor : 3 Concentration Units : ng/m L Cal. Ver . Data Filename : FC5G_181SO48 CAL VER ID : PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0_63 9 PFHxA UD 0 .620 PFHpA UD 0.628 PFOA D 55.4 0.618 PFNA D 2 .36 0.670 PFDA UD 0.648 PFUnA UD 0.641 PFDoA UD 0.638 PFBS UD 0 .635 PFHxS D 6.59 0 .638 PFOS D 60 .0 0 .645 PFOSA UD 0.625 4.65 5.05 4 .80 5 .46 LABELED COMPOUND LAB SPIKE CONC . R (%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS ( 80) 13C4-PFOS 13C2-PFDA D 12.0 D 12 .0 (99) D 12 .0 D 12 .0 11 .8 98.2 15.0 125 13.4 112 10.1 84 .4 4 .65 5.51 5 .46 5 .36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16982PFD7 2_x1s, s7 Approved by : QA/QC Chemist 11 - 10-05 darnm-yyyy 4)~((0 AXYS AIVALYTICAL SERN/ICES LT(D P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B .C., CANADA VOL 3S8 TEL (250) 6S5-5800 FAX (250) 855581 1 1 ;L p . 93 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_S1_D12 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPORT Lab Name : AXYS ANALYTICAL SERVICES Sample Collection : 08-Sep-2005 11 :48 Con tract No . : 4191 Lab Sample ID : L7932-56 i Matrix : SERUM Sample Size : 1 .00 ml Sample Receipt date : 09-Sep-2005 Extraction Date : 21-Sep-2005 Analysis Date: 23-Sep-2005 Time : 1 :38 :15 Initial Calibration Date: 22-Sep-2005 Instrument ID-. LC-MS/M S LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FC5G 181S058 Injection Volume (NL) : 10 .0 Blank Data Filename : FC5G 1815070 Dilution Factor: 3 Concen tration Units : ng/m L Cal . Ver. Data Filename : FC5G_181S048 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC FLAG' FOUND DETECTION LIMIT RETENTION TIME PFPeA UD 0.639 PFHxA UD 0 .620 PFHpA UD 0 .628 PFOA D 2 .63 0 .618 PFNA D 0.866 0.670 PFDA UD 0.648 PFUnA UD 0.641 PFDoA UD 0.638 PFBS UD 0 .635 PFHxS D 5.19 0 .638 PFOS D 17 .4 0 .645 PFOSA UD 0 .625 4 .65 4 .99 4 .80 5.46 LABELED COMPOUND LAB SPIKE CONC . R(o/,) 2 RETENTIO N FLAG' CONC . FOUND TIME (n9) (n9 ) 13C2-PFOA D 12.0 13C4-PFOS (80) D 12.0 13C4-PFOS (99) D 12.0 13C2-PFDA D 12 .0 12 .9 17 .0 14 .1 11 .5 107 4 .65 142 5 .46 117 5.46 96 .1 5.36 ( 1) U = not detected ; D = dilution data (2) R (%) = Percent recover y 18982PFD 1 2 .xas. S8 Approved by. QAJQC Chemist >>_~0-0e dd-mm-yyyy 0)~[(A AXYS AfVALITICAL SERVICES LTE) P.O. BOX 2219, 2045 MILLS R0 . WEST, SIDNEY. B .C., CANADA VOL 3S8 TEL (250) 6555800 FAX (250) 655581 1 !~ p . 94 AXYS METHOD MLA-042 Rev 03 CLIENT ID: PFOSS1 012 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection : 12-Sep-2005 17 :42 Lab Name : AXYS ANALYTICAL SERVICES Contract No.: 4191 Lab Sample ID : L7932-58 i Matrix : SERUM Sample Size : 1 .00 mL Sample Receipt date: 14-Sep-2005 Initi al Calibration Date : 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID : LC-MS/MS Analysis Date : 23-Sep-2005 Time: 1 :52:30 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_181S059 Injection Volume (pL): 10 .0 Blank Data Filename : FC5G_181S070 Dilution Factor: 3 Concentration Units : ng/m L Cal. Ver. Data Fllename : FC5G_181SO48 CAL VER ID : PFC-LIN-055CS-F COMPOUND LAB CONC FLAG' DETECTION FOUND 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 LAB SPIKE CONC. R(y,)2 RETENTION FLAG' CONC. FOUND T1ME (ng) (ng) 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS (99) 13C2-PFDA D D D 12 .0 12 .0 12 .0 D 12.0 11 .7 97 .8 4.65 15.1 126 5_46 15.2 127 5.46 10 .6 88.0 5.36 (1) U = not detected ; D = dilution data (2) R (%) = Percent recovery 96982PF012xis, S9 Approved by : QA/QC Chemist 11-10-05 dd-mm-yyyy +~)~((C+ AXYS AtV ALYf IC.~iL SER-%/ICES LTL7 P.O. BOX 2219, 2045 MILLS R0. WEST, SIDNEY, B .C., CANADA Y8L 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 61 Joh p . 95 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_Si_o12 Form 1Ai2 PERFLUORINATED ORGANICS ANALYSIS REPORT Sample Collection : 12-Sep-2005 17:46 Lab Name : AXYS ANALYTICAL SERVICES Contract No. : 4191 Lab Sample ID : L7932-59 i Matrix : SERUM Sample Size : 1 .00 mL 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 : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_181S060 Injection Volume ({jL) : 10 .0 Blank Data Filename : FC5G_181S070 Dilution Factor: 3 Concentra tion Units : nglm L Cal . Ver. Data Filename : FC5G_181SO48 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0.639 UD 0.620 D 0.962 0 .628 D 68.3 0 .618 D 0.957 0 .670 UD 0 .648 UD 0_641 UD 0 .638 UD 0.635 D 13 .8 0.638 D 50 .1 0.545 UD 0.625 4 .14 4 .65 4 .99 4 .80 5 .46 LABELED COMPOUND LAB SPIKE CONC. R ( o/,)z RETENTION FLAG' CONC . FOUND TIME (ng) (ng) 13C2-PFOA 13C4-PFOS (80) 13C4-PFOS 13C2-PFDA D 12.0 D 12.0 (99) D 12 .0 D 12 .0 11 .8 98.4 4.65 15 .0 125 5.46 14 .1 117 5.46 12 .7 106 5 .36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 11-10-05 1 6982PFO 1 _2 .)as, sic Approved by: ~~~~----~ QA/QC Chemist dd-mm-yyyy ~~(CD AXYS AfVALYi ICAL SERViCES LT~ P.O. BOX 2219, 2045 MILLS RD_ WEST, SIDNEY, B.C., CANADA V8L 3S8 TEl (250) 655-5800 FAX (250) 655-5811 5 ~, p . 96 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collection : 13-Sep-2005 18 :33 Lab Name : AXYS ANALYTICAL SERVICES Contract No . : 4191 Lab Sample ID: L7932-61 i Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date: 15-Sep-2005 Initial Calibration Date : 22-Sep-2005 Extraction Date: 21-Sep-2005 Instrument ID: LC-MS/M S Analysis Date: 23-Sep-2005 Time: 2 :20:55 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FCSG_181S061 Injection Volume (NL): 10 .0 Blank Data Filename: FC5G_181 S070 Diluti on Factor: 3 Concentration Units : ng/m L Cal . Ver. Data Filename: FC5G_181SO48 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0.639 UD 0.620 UD 0.62 8 D 69-0 0.618 D 1 .05 0.670 D 0 .835 0.648 UD UD 0.64 1 0.638 UD 0.635 D 15 .7 0.638 D 77 .2 0.645 UD 0.625 4 .65 4.99 5 .36 4 .87 5 .46 LABELED COMPOUND LAB SPIKE CONC. R(ya)Z RETENTIO N FLAG' CONC. FOUND TIME (n9) (n9) 13C2-PFOA D 12 .0 12 .1 101 4.65 13C4-PFOS (80) D 12-0 14 .3 119 5.46 13C4-PFOS (99) D 12 .0 14 .6 122 5 .46 13C2-PFDA D 12 .0 11 .0 91 .6 5.36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16982PFD 1_2.x 1s.511 Approved by: ,IX QA/QC Chemist 11-1dd0-m-m0-yy5yy 0010 AXYS AIVALYf ICAL SEIIZVICES LT[D P.O . BOX 2214, 2045 MILLS U . WEST, SIDNEY, B .C, CANADA V8L 3S8 TEL (250) 655-5800 FAX (250) 655-5811 910 p . 97 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_St oi2 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPORT ID: Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : 15-Sep-2005 11 :03 Contract No . : 4191 Lab Sample ID : L7932-63 i Matrix : SERUM 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: 2:35:09 LC Column ID : C1 8 Extract Volume (mL): 2 Sample Datafile : FC5G_181S062 Injection Volume (NL) : 10 .0 Blank Data Filename : FC5G 181S070 Dilution Factor : 3 Concentration Units : nglmL Cal . Ver. Data Filename : FC5G_181SO48 CAL VER ID: PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD 0.63 9 PFHxA UD 0.620 PFHpA D 2 .16 0.628 PFOA D 100 0 .618 PFNA D 1 .32 0 .670 PFDA PFUnA UD 0 .64 8 UD 0 .641 PFDoA UD 0 .638 PFBS UD 0.635 PFHxS D 58 .6 0.638 PFOS D 131 0 .645 PFOSA UD 0 .625 4.18 4.65 4 .99 4.80 5.46 LABELED COMPOUND LAB SPIKE CONC. R (%)2 RETENTION FLAG' CONC. FOUND TIME (n9) (n9) 13C2-PFOA 13C4-PFOS 13C4-PFOS 13C2-PFDA D (80) D (99) D D 12 .0 12 .0 12 .0 12 .0 9 .60 80 .0 9.83 81 .9 9.52 79 .3 8 .67 72 .2 4.65 5.46 5.46 5.36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16982PFD1 2As, 972 Approved by : QA/QC Chemist 11-10-05 dd-mm-yyyy 41I0 AXYS ANALYTIC-AL SER-,/ECES LTiD P.O. BOX 2219, 2045 MILLS RD. WEST, SIDNEY, B.C., CANADA VOL 358 TEL ( 250) 655-5800 FAX (2501655-5811 17 p . 98 AXYS METHOD MLA-042 Rev 03 CLIENT PFOS_S1 oi2 Form 1A/2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID: Sample Collection : 15-Sep-2005 11 :05 Lab Name: AXYS ANALYTICAL SERVICE S Contract No .: 4191 Lab Sample ID: L7932-64 i Matrix: SERUM Sample Size : 1 .00 mL Sample Receipt date : 16-Sep-2005 Initial Calibration Date: 22-Sep-2005 Ex traction Date : 21-Sep-2005 Instrument ID : LC-MS/M S Analysis Date : 23-Sep-2005 Time : 2:49 :23 LC Column ID : C1 8 Extract Volume ( mL): 2 Injection Volume (pL) : 10 .0 Sample Datafile : Blank Data Filename: FC5G_181S063 FC5G 181S070 Dilution Factor: 3 Concentration Units : ng/m L Cal . Ver. Data Filename : CAL VER ID: FC5G_181SO48 PFC-LIN-055CS-F COMPOUND LAB FLAG' CONIC FOUND DETECTION RETENTION LIMIT TIME PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS PFOSA UD 0 .639 UD 0 .620 UD 0 .628 D 86.8 0 .618 D 1 .71 0_670 UD 0.648 UD 0.641 UD 0 .638 UD 0 .635 D 34 .5 0 .638 D 125 0 .645 UD 0 .625 4 .65 4.99 4 .80 5.46 LABELED COMPOUND LAB SPIKE CONC . R (%)z RETENTIO N FLAG' CONC. FOUND TIME (ng) (ng ) 13C2-PFOA 13C4-PFOS 13C4-PFOS 13C2-PFDA D 12.0 (80) D 12.0 (99) D 12.0 D 12.0 12 .7 16 .2 14 .0 13 .6 106 4.65 135 5.46 116 5.46 113 5.36 (1) U = not detected ; D= dilution data (2) R (%) = Percent recovery 16982PFD7 2jds, S13 Approved by. ~ 1 i-i0-o5 G1A/QC Chemist dd-mm-yyy y 0))((C AXYS ANALYTIC'AL SF-R\/ICES LTC7 P.O. BOX 2219, 2D45 MN1S RD . WEST, SIDNEY, 8.(., CANADA V8[ 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 qe P . 99 AXYS METHOD MLA-0 42 Rev 02 CLIENT PFOS_s1_o12 Form 1A1 2 PERFLUORINATED ORGANICS ANALYSIS REPOR T ID : Lab Name : AXYS ANALYTICAL SERVICE S Sample Collection : N/A Contract No . : 4191 Lab Sample ID: L7932-1 2 Matrix : Sample Size : 1 .00 mL Sample Receipt Date: 19-Ju1-2005 Initial Calibration Date : 05-Aug-2005 Extraction Date : Analysis Date: 04-Aug-2005 05-Aug-2005 Time : 22:43:43 Instrument ID: LC-MS/MS LC Column ID : C18, Zorbax XDB Extract Volume (mL): 2 Sample Datafile : FC5G 131S047 Injection Volume (pL) : 30 .0 Blank Data Filename : FC5G_131S024 Dilution Factor: N/A Concentration Units : ng/m L Cal . Ver. Data Filename : FCSG131S03 7 CAL VER ID: PFC-LIN-039CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG FOUND LIMIT TIME PFPeA U PFHxA U PFHpA U PFOA U PFNA U P FDA U PFUnA U PFDoA U PFBS U PFHxS U PFOS U PFOSA 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 LABELED COMPOUND LAB SPIKE CONC . R(%)2 RETENTION FLAG' CONC. FOUND TIME (ng) (ng) 13C-PFOA 120 9 .16 13C-PFDA 12 .0 9.10 76 .3 4 .70 75 .8 5.34 (1) U =not detected (2) R (%) = Percent recovery 16535PF02_2 .xls, S9 Approved by : QA/QC Chemist 11-10-2005 dd-mm-yyyy 14~XVS A(VALVTICAL SER'\/ICES LTp P.O. BOX 2219, 2045 MIiLS RD. WEST, SIDNEY, B .C., CANADA Y8L 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 11 p . 100 AXYS METHOD MLA-042 Rev 02 PFOS_St 0I2 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T CLIENT ID : Sample Collection : N/A Lab Name : AXYS ANALYTICAL SERVICE S Contract No. : 4191 Lab Sample ID : L7932-18 Y4 Matrix: N/A Sample Size : 1 .00 mL Sample Receipt date : 10-Aug-2005 Initi al Calibra ti on Date : 12-Sep-2005 Extraction Date : 29-Aug-2005 Instrument ID : LC-MS/M S Analysis Date: 12-Sep-2005 Time : 19:33:09 LC Column ID : C1 8 Extract Volume ( mL) : 2 Sample Datafile : FCSG 167S036 Injection Volume (NL) : 30.0 Blank Data Filename : FC5G 167S031 Dilution Factor : N/A Concentration Units : ng/mL Cal . Ver. Data Filename: FC5G167S027 CAL VER ID: PFC-LIN-044CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U PFHxA U PFHpA U PFOA U PFNA U PFDA U PFUnA U PFDoA U PFBS U PFHxS U PFOS U PFOSA 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 LABELED COMPOUND LAB SPIKE CONC . R(%)z RETENTION FLAG CONC . FOUND TIME (n g) (ng ) 13C2-PFOA 13C4-PFOS(80) 13C4-PFOS(99) 13C2-PFDA 12 .0 8 .36 69 .7 12.0 8 .61 71 .8 12.0 9 .47 79.0 12.0 10 .2 85.0 4.70 5.56 5.56 5.36 (1) U =not detected (2) R (%) = Percent recovery - 16755PF_01_2 .)ds, S7 Approved by : QA/QC Chemist 11-10-05 dd-mm-yyyy 0))((0 AXYS AIVALYT 1~'~L SERVICES LTJD P .O . BOX 2219, 2045 AlliS RD. WEST, SIDNEY, 81, CANADA V8 1. 3581EL (250) 655-5800 FAX (250) 655-581 1 rob p . 101 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_S1_D12 Form 1A12 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collection : N/A Lab Name : AXYS ANALYTICAL SERVICE S Contract No. : 4191 Lab Sample ID : L7932-50 Y2 Matrix : N/A Sample Size : 1 .00 mL Sample Receipt date: 31-Aug-2005 Initial Calibration Date : 13-Sep-2005 Extraction Date: 06-Sep-2005 Ins trument ID: LC-MS/M S Analysis Date: 13-Sep-2005 Time : 11 :01 :03 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_168S027 Injec ti on Volume (NL) : 30 .0 Blank Data Filename : FC5G_168S015 Dilu ti on Factor: N/A Concentrati on Units : ng/m L Cal. Ver. Data Filename: FC5G_168S01 0 CAL VER ID : PFC-LIN-048CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA U PFHxA U PFHpA U PFOA U PFNA U PFDA U PFUnA U PFDoA U PFBS U PFHxS U PFOS U PFOSA U 0 .256 0 .248 0.25 1 0 .247 0 .268 0 .259 0 .257 0 .255 0 .254 0 .255 0 .258 0 .250 LABELED COMPOUND LAB SPIKE CONC . R (%)2 RETENTIO N FLAG' CONC. FOUND TIME (ng) (ng) 13C2-PFOA 12 .0 4 .15 34.6 13C4-PFOS(80) 12 .0 5 .94 49 .5 13C4-PFOS(99) 12 .0 4 .52 37.6 13C2-PFDA 12 .0 10 .7 89.0 4 .65 5 .51 5 .51 5 .36 (1) U = not detecte d (2) R (%) = Percent recovery 16614PFD3_2 .xls, S14 Approved by : ~~970~ QA/QC Chemist 11-10d-d-2m0 m-0yy5 yy ~))((C AXYS ANALVTIC-AL SERVICES LT[] P.O . BOX 2219, 2045 MILIS RD. WEST, SIDNEY, B.C., CANADA Y8L 3S8 TEL (250) 655-5800 FAX (250) 655-581 1 lol p . 102 AXYS METHOD MLA-042 Rev 03 CLIENT ID : PFOS_St_D12 Form I A(2 PERFLUORINATED ORGANICS ANALYSIS REPOR T Sample Collecti on: N/A Lab Name: AXYS ANALYTICAL SERVICES Contract No . : 4191 Lab Sample ID : L7932-65 1 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/M S Analysis Date: 23-Sep-2005 Time : 3 :03 :37 LC Column ID : C1 8 Extract Volume (mL) : 2 Sample Datafile : FC5G_181S064 Injection Volume (}j L) : 10.0 Blank Data Filename : FC5G_181S070 Dilution Factor: 3 Concentration Units : ng/m L Cal . Ver. Data Filename : FC5G_181SO48 CAL VER ID : PFC-LIN-055CS-F COMPOUND LAB CONC DETECTION RETENTION FLAG' FOUND LIMIT TIME PFPeA UD PFHxA UD PFHpA UD PFOA UD PFNA UD PFDA UD PFUnA UD PFDoA UD PFBS UD PFHxS UD PFOS UD PFOSA 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 LABELED COMPOUND LAB SPIKE CONC. R (%)2 RETENTION FLAG' CONC . FOUND TIME (n9) (n9 ) 13C2-PFOA D 12 .0 13C4-PFOS ( 80) D 12 .0 13C4-PFOS (99) D 12 .0 13C2-PFDA D 12 .0 12.8 13.6 14.5 15.2 107 114 121 127 4.65 5.46 5.46 5.36 (1) U = not detected ; D= dilution dat a (2) R (%) = Percent recovery 16982PFD1_2.x1s, $14 Approved by: ~ QA/QC Chemist 11-10-05 ad-mm.yy AXYS AIVALYrBCAL SERVICES LTF-) P .O . BOX 2219,204S IM11S RD. WEST, SIDNEY, 8.[ ., CANADA VOL 35B TEL (250) 65S-5800 FAX (2S0) 655-S81 1 roz