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il RESEARCH Precise Research. Proven Results. RECEIVED r.p P T C " ' C 05APR26 AHIIvll ________________j% r? 7F Analytical Report 3M Company A nalysis o f PFO A and PFO S In W ater Sam ples from H astings M u n icip ality EOS-0186 Exygen Report No. L0Q04709 Testing Laboratory Exygen Research 3058 Research Drive State College, PA 16801 Requester Gary A. Hohenstein Manager, Environmental Operations EHS Operations 3M Company Building 42-2E-27 St. Paul, MN 55106 2005HAY-3 PH 2* 51* PAGE 10 F 5 3 ^ 3 0 5 8 Researdti Drive m ^L S ta ie Cofege PA 16801, USA T: 800.28811.3219 m `FF:: 814.272.1019 exygen.com 1 Introduction Results are reported for the analysis o f perfiuorooctanoate fPFOA) and perfluorooctanesulfonate (PFOS) In water samples received at Exygen as requested by G ary H ohensteh o f 3M Company, The Exygen project num ber assigned to the samples is L0004709. Table I lists the target analytes quantitated for the samples. Table I. Target Analytes for Quantitation P aram eter Perfluorooctenoate Acronym PFOA or C8 acid F orm ula CyFuCOO' Perfluorooctanesulfonate PFOS or C8 sulfonate C5F17S0 1 2 Sample Receipt Four samples were received at Exygen in 500 mL white plastic narrow-m outh bottles. At the request o f 3M, all samples were analyzed. A copy o f a l sample log-in Information is presented in Attachment A. The samples were received on 03/01/05. The samples were shipped am bient via UPS. The samples were stored refrigerated from tim e o f receipt until analysis. 3 Methods - Analytical and Preparatory The Exygen method entitled, "Method o f Analysis for the Determination o f Perfluorooctane sulfonate (PFOS), Perfluorooctane sulfonyfamkte (PFOSA), and Perfiuorooctanoate (POAA) in W ater/' modified fo r isom er separation, was used to prepare and analyze the samples. A summary o f foe sample preparation can be found in Section 3.1 and foe m odified analysis conditions for isomer separation can be found in Section 3.2. 3.1 W ater Sam ple Preparation Solid phase extraction (SPE) was used to prepare the w ater samples fo r LC/MS/MS analysis. Forty m illiliters of the water sample was transferred to a C18 SPE cartridge. The cartridge was washed with 5 mL of a 40% methanol: 60% water wash. The cartridge was eluted with 5 mL of 100% methanol. A portion of the extract was transferred to autosam pler vials and analyzed using electrosprey LC/MS/MS. PAGE 2 OF5 3.2 Sam ple Analysis by LC/MS/MS In High Pressure Liquid Chromatography (HPLC), an aliquot o f extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity o f the analyte for the stationary phase in the column relative to the liquid m oble phase, the analyte Is retained fo r a characteristic amount o f time. Following HPLC separation, m ass spectrom etry provides a rapid and accurate means for analyzing a wide range o f organic compounds. M olecules are ionized, fragm ented, and detected. The ions characteristic o f the compounds are observed and quantitated against extracted standards. An HP 1100 system interfaced to an Applied Biosystems API 4000 was used to analyze the sam ple extracts for quantitation. Isomer separation was obtained using a gradient elution through a Therm o Fiuophase RP, 50 x 2.1 mm x 5pm column. The sum o f the isom ers is reported as a single value for each o f the analytes. The following gradient was performed: Mobile Phase (A): Mobile Phase (B): Time 0.0 1.0 8.0 10,0 11.0 18.0 2mM Ammonium Acetate in W ater M ethanol M 2fc 65 35 65 35 25 75 25 75 65 35 65 35 The following parameters were used for operation o f the mass spectrom eter: Param eter Ionization Mode Polarity Transitions Monitored Gas Temperature Drying Gas <N2) Setting Electrospray Negative 413->369 (PFOA), 499->80 (PFOS). 415->370 (13C-PFOA, surrogate spike) 350flC 7.0 L/min 4 Analysis 4.1 C alibration A 7-polnt calibration curve was analyzed initially and throughout the analytical sequence for PFOA, PFOS and ,3C PFOA. The calibration points were prepared at 0,25.50,100,250,500, and 1000 ng/L (ppt) for LC/MS/MS analysis. C albration standards are prepared using the same SPE procedure used for samples. The Instrument response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, /-intercept PAGE 3 OF5 and coefficient o f determ ination (r2) were determined. A calibration curve is acceptable if r2 > 0.985. For the results reported here, calibration criteria were m e t The calibration curves are Included in the raw data in Attachm ent C. 4.2 Surrogates 13C PFOA (CqF 15[,3C)F2[1!C]OOH) is used as a surrogate fo r the water samples. 1SC PFOA was added to the empty sample containers before the bottles were sent to the field for sampling. In the field, all sample and quality control battles w e re filled to & volum etric fll line with the sample. 13C PFOA recoveries can be found in Attachm ent B, 4.3 Laboratory C ontrol Spikes Laboratory control spikes in the analytical set were prepared by addng a known concentration o f PFOA, 13C PFOA, and PFOS to laboratory reagents. Laboratory control spikes are used to assess method accuracy. The laboratory control spfces m ust show recoveries between 70* 130% or the data is rejected. For the results reported here, the laboratory control spikes were w ithin the acceptable range. 4 .4 Field M atrix Spikes A low and a high m atrix spike were prepared with toe sam ple and sample duplicate in toe field. Compounds were added to the em pty sample containers before the bottles were sent to the field fo r sampling. Matrix spikes are used to assess method accuracy in the m atrix. The m atrix spikes should show recoveries between 70*130%. For the results reported here, the m atrix spikes were w ithin the acceptable range. 4.5 Sample Related Comments The water samples were collected in duplicate, Duplicate sample results are reported in Attachm ent B. 5 Data Summary Please see Attachment B for a detailed listing o f toe analytical results. The results are reported in parts per bilion (n g /m l) for PFOA and PFOS . PAGE4 OF5 6 Statement of Accuracy Based on results o f laboratory control spikes, field m atrix spikes, and surrogate spices, the analytical accuracy fo r PFOS and PFOA results is 30%. Laboratory control spices, surrogate spikes, and field m atrix spikes showed recoveries within this range. Specific sam ple recoveries are given in Attachm ent B. 7 Data/Sample Retention Samples w ii be returned to 3M 60 days after final reporting. All electronic data is archived on retrievable m edia and hard copy reports are stored in data folders m aintained by E xygen. Hardcopy data is stored for a minimum o f five years. The client w ill be notified 30 days prior to the disposal o f hardcopy data. 8 Attachments 7.1 Attachm ent A: Analytical Results 7 2 Attachm ent B: Spike Recovery Data 7 2 Attachm ent C; Chain of Custody Forms 7.4 Attachm ent D: Raw Analytical Data PAGE 5 OF 5 51 SECTION A 1 __ Ana MU al ^ R e jx ir t 1 Sum m ary o f PFO A and PFOS in W ater Sam ples E 05-0186 L4709-1 L47Q9-2 H-W6-207M3 H-W 6-207643 Pup Analyte Found (ng/mL) CS Acid PFOA C8 Sulfonate PFOS P erfluorooctanoat* P e rfkio ro o cU n M iilfo n a t ND NO ND ND ND = Not detected at or above 0.025 ng/m L NQ * Not quantifiable * Measured concentration between 0.025 ng/mL end the Umit of Quantitation (LOQ) which is 0.050 ng/mL. 0006 53 ^ ^ 3 0 5 8 Researrcdh Drive J vstate CoKege * 16801, USA ^ L Jt:: 814422772X1089 S F F;; 814.23 1.1580 exigen,tum SECTION B EwgenR E S E A R C H Precise Research. Proven Results. Figld Matrix Spike Recovery Summary for PFOA and PFOS In Water E05-0186 Sample, Description H-W6-207B43 Low Spike (14146*3,0.1 ppbSptk*) H-W6-2C7643 High Spike (U u e4,i ppbsport) CB Add PFOA______________ C6 Sutfonate PFOS Amount Amt Found Amount Amt Found Amount Spiked In Semple Recovered Recovery fn Sample Recovered Recovery (ng/mL) (ng/mL) In a im i) (%) (ng/mL) (ng/mL) f%) 0.1 ND 0.128 128 ND 0.117 117 1 ND 1.04 104 ND 1.03 103 ND = Not detected at or above 0.029 ng/m L NO " Not quantifiable Measured concentration between 0.025 ng/mL and fte Lim it o f Quantitation (LOQ) which to 0.050 ng/m L \ 55 J^30Sd Research Drive J f ^SStatie Collegei, PA 16801, USA ^ T T:: 800..2288113219 m FFrr 814.27,2.1019 exygen.com n RESEARCH Precise Research. Proven Results. Surrogate Spike Recovery Summary for u C-PFOA in W ater E05-0186 Exygon ID Sample Description L4709-1 L4709-2 L4709-3L4709-4 , H -W 6-207643 H-W6-207643 Dup H-W6-207643 Low Spk H-W6-207643 High Spk Amount Spiked (ng/m L) 1C-PFOA Amount Recovered (n g/m L) Recovery (*) 0.5 0.491 0.5 0.522 0.5 0.546 0.5 0.540 98 104 109 108 0007 56 J ^ 3 0 5 S Researcchh Drive State College, PA 16801, USA ^ T T:: 800.228811.3219 I fF: 814.272.1019 exygen.com SECTION C Fw pn 3068 Research Drive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 I Loqin Login Group: L0004709 L o g in # ; P ro je c t: 4819 P0001275 Company Name: 3M Subm itted By: KENT LINDSTROM Login Type; Im m ediate R eceipt o f Sam ples S ta rte d ; True Date Start; 0 3 /0 1 /2 0 0 5 Due Date: 0 3 /1 1 /2 0 0 5 Received Date: 03/01/2005 Received By: Am m erm an, M ark Spread Sam ple: Label: Exygen SD/P1: R istia* Karen /P roject T itle/T ype: C ottage G rove R esidential W ater Sam pling ROUTINE Login Notes: Conform N otes: C onform COC S am ple; C onform COC: C onform Sam ple: C onform R equest: T ru e T n je T ru e T ru e | f $ I Packed Carton Package?/ Containers Dato / C ondition Tsfim. Cootrol/TumD. D irection f Handled Bv PK0005WO Login Date: 3/1/2005 11;31;4AM Packeis* & Contents Unoompromised UPS 126795560142913994 None 22.3 RECEIVED Ammerman, Mark C on ta in er# C0063087 C0063088 Gross W ekitit dH Container T v 253.90 g 500 ml Clear Plastic Narrow 258.00 g 500 m l Clear Plastic Narrow P reservative NONE NONE Mffl,,,Lot Mfa. ID ill: PKOOOSsei Login Date: 3/1/2005 11:34:30AM Package & Contents Uncompromised UPS 1Z57955E0140675806 Nona 22.3 RECEIVED Ammerman, Mark container.# C0063089 C0063090 G rots Weight d d O o ntalntt.T vpe 292.90 g 500 ml Clear Plastic Narrow 244.40 g 500 ml Clear Plastic Narrow Preservative NONE NONE Mfa, -Lot Mfa. ID Samal* ID L004709-0001 L0004709-0002 L0004709-0003 LQ004709-004 Container C0063067 CO063089 C0063068 C0063090 Matrix LIQUID LIQUID LIQUID LIQUID Fraction Water Samples Sample HW6-2D7643 W ater HW8-207643 Dup W ater HW6-20743 Low Spice W ater HW6-207643 Hlgti Spike 0008 3/1/2005 Report Version; Feb 22 2005 0:53AM Login,rpt Page 1 o f2 52 Puts.Sampled Pale.kwgeti In 02/28/2005 03/01/2005 03/11/2005 j' 02/28/2005 02/28/2005 02/28/2005 03/01/2005 03/01/2005 03/01/2005 03/11/2005 1 i. 03/11/2005 lf|: 03/11/2005 i Instance : RO140340 m V iH lllIR H I Sr B ! Login Reviewed By: Datafflme: U L1 3/1/2005 Logln.rpt 000 Report Version: Feb 22 2005 8:53AM Page 2 of 2 Instance: R0149340 niBDiiiin Form3877 -PWO aoippang w m SMBfcte ?-S-09 6 Burt A w St Paul. MN 106 iw piionK Sm i***m N<hg;fW )7TM S aartrt: <M1>77W51 FAX:(H I) T7S#t7B C ortactN ane Company ^W V PrwectICVPnjiedName U v s 4 fV i v $ Tem plate# Project Lead D ept (m ein) < T 3 0 " 3 - U UAl 1 1L FInal Report Due Date Hrie m tf PueDate WC.iaesOofa/Pmject # CSO Z 2 - ( # 3 ___1 & n 3 * ______________________________ O ateAvalable * M aiing Address PJp-; g IP vny, state, iiip Telephone# SpscfafiMfeudlivw wNof (meant >nl ofOMeeeon. feponmourwt. elco Av^dlviiiMntec FAX# ...... -- -- I 'V ' I f ? ( * v fc _ ^ * - v G O S ~ ~ < 2 1 $ * / -- Date Due HContract Lab P roe erva tfvee : fc f X iI i _________________________________________________________________________________________________ item # Client Sample Menlgfcaiion 3M Date Time M atrix/ UMS# Sampled Sampled Media Erter*wnuntaiofoonWwn ofnee 1. W v J ( '- Z o > f c V 7 2. iiD 3. khpV~ LouJ SpI lO-- 4. 'J m b t ' / fw I ii2.y LI C M2 i lm A/ \ _L \ t 1 5- VOCs Total Num ber o f C ontainers c:-<--*------V-------5ra-?--L--h-------`-e--~------K------------------------------------ A n a ly e Is Requested: t*iO.M--pMlM*j#- d#nh4rhI m #ny^Mh I^bb < M-M. * 4 r " ^ L i J L* 41 *4 >/ a r -- t 8 r< 3 (G M rm X toatlm bitw tolndfci --a 1 ___ |1 1 6. ___ 7. ' 8. 9. H j u10. / V l.i t____ ___ - Item # ^ : v i - - ;; f- * i-j ^ * ] y j- /p m ^ c je /d ^ S 4 u ^ < ^ r f ZT Sample Condition Upon Receipt: Temperature. OVwAnocMed CoCr `C V ^A ooeptabie o O ther 0 Received on lee Coffee tCE tp * * /. ^iSIte' I$*>pedVie: < K i# V *F 4 r S t / - fir s 2 /3 0 5 ` t//s A 7 ; /. y t-- ------- '------- ------- / X y - i w 7 * (* Gwwiflribc ik TO e n 1 rr i f e /jz ^ > th tr - jL Oriyml - Acoompewhu 8R|*e S M ftm n a SUt tor MakMCfcn* 2/28/2005 Project: E05-0186 3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY SAMPLE Contract Lab(s): EXYGEN Page I o f I Requester: Hohenstein, Gary A (0042-Q2E-27) Department 530711 Project Number: 0022674449 Date Received: 2/25/2005 Project Description: Hastings Municipal Well PC's 11 Completion Date: Project Lead: Kent Lindstrom Phone Number: 651-778-5352 Email Address: krlindstrom@mmm.com Comments: Pace field sampling. Note: Reference trip blank on E05-0184. BGJ 2/28/05 05-0186 samples traveled withE05-0184 samples. AC, PLf, 2/28/2005. 3M Sample Number Sampled Date Sample Description E05-0186-79868 Ana^ia Code PFA PFOS 2/28/2005 H-W6-207643 i CffmBapcaft PFOA PFOA PFOSbyESMS PFOS E05-0186-79869 Analysis Code PFOA PFOS 2/28/2005 H-W6-207643 Duo Analytical Method1 Cftmoonciits PFOA PFOA PFOSbyESMS PFOS AmlYgii P i t Pute 3/15/2605 3/15/2005 Anilvijj put Date 3/15/2005 3/15/2005 oon C/
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