Document 3Ng66p762o4zqMoRBmb1q8L46

Pmwn Resufis. pc p r i v m 0 5 APR 2 - n H I ! : I ! ______________ M J - 7 7 F Analytical Report 3M Company Analysis o f PFOA and PFOS In W ater Samples from H astings M u nicipality EOS-0186 Exygen Report No. L0004709 Testing Laboratory Exygen Research 3058 Research Drive State College PA 16801 Requester Gary A Hohenstein Manager, Environmental Operations EHS Oprations 3M Company Building 42-2E-27 St. Paul, MN 55106 PR C- oDPrOn -0 0 \-- c 0 rP - c O l~'"` cfl cn PAGE 10PS 41 2 ^ 3 0 5 8 RtaeanJ1 Drive f Stale College PA 16801, USA ^ L tT: 80028811J219 m fF:: 8a1144.272.1019 etygen.com 1 Introduction Results are reported for the analysis o f perfluorooctanoate (PFOA) and perfluorooctenesuifonate (PFOS) in water samples received at Exygen as requested by G ary Hohensteln of 3M Company. The Exygen project number assigned to the samples L0004708. Table I lists the target analytes quantitated for the samples. Table I. Target Analytes for Quantitation P aram eter AffPfW m F orm ula Perfluorooctanoate PFOA or C8 acid C7F1sC O O ' Perfluorooctanesulfonate PFOS or C8 sulfonate C gF i?S O j' 2 Sample Receipt Four samples were received at Exygen In 500 mL white plastic rarrow -m outh bottles. At foe 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 Ferftuorooctane sulfonate (PFOS), Perfluorooctane sutfonytamide (PFOSA), and Perfluorooctanoate (POAA) m W ater," modified for isom er separation, was used to prepare and analyze foe samples. A summary o f foe sample preparation can be found In Section 3.1 and foe modified analysis conditions for isom er separation can be found in Section 3.2, 3.1 W ater Sam ple Preparation Solid phase extraction (SPE) was used to prepare the water samples fo r LC/MS/MS analysis. Forty m ililiters of the water sample was transferred to a Cia SPE cartridge. The cartridge was washed with 5 mL of a 40% methanol: 60% water wash. The cartridge was eluted with 5 m l of 100% methanol. A portion of the extract was transferred to autosam pler vials and analyzed using electrospray LC/MS/MS. PAGeiors 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 of the analyte for the stationary phase in the column relative to the liquid mobile 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, fragmented, and detected- The ions characteristic o f the compounds are observed end quantitated against extracted standards. An HP 1100 system interfaced to an Applied Biosystems API 4000 was used to analyze the sample extracts for quantitation. Isomer separation was obtained using a gradient elution through a Thermo Fluophase RP, 50 x 2.1 mm x 5pm column. The sum o f the isomers is reported as a single value fo r each o f the analytes. The following gradient was performed: Mobile Phase (A): Mobile Phase (5): T im e 0.0 1.0 8.0 10.0 11.0 18.0 2mM Ammonium Acetate in W ater Methanol M 2 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 Parameter Ionization Mode Polarity Transitions Monitored Gas Temperature Drying Gas (N2) Setting B e c tro s p ra y Negative 413->38S (PFOA), 499->80 (PFOS). 415->370 (13C-PFOA, surrogate splice) 350C 7,0 Urnin 4 Analysis 4.1 Calibration A 7-point calibration curve was analyzed initia ly and throughout the analytical sequence for PFOA, PFOS and ,3C PFOA. The calibration points were prepared at 0 ,2 5 .5 0 ,1 0 0 ,2 5 0 ,5 0 0 , and 1000 ng/L (ppt) for LC/MS/MS analysis. C albration standards are prepared using the same SPE procedure used for samples. The instrum ent response versus the concentration was plotted for each point. Using linear regression with 1/x weighting, the slope, /-intercept PAGE3 OF5 and coefficient of determination (r2) were determined. A calibration curve is acceptable if r3 > 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 (CeF i5[13C]F2[1"C}OOH) is used as a surrogate for the water samples. n C PFQA was added to the empty sample containers before the bottles were sent to the field for sam p lin g. In the field, all sample and quality control bottles ware fated to a volum etric HI line with the sample. 13C PFOA recoveries can be found in Attachm ent B. 4.3 Laboratory Control SpIKas Laboratory control spikes in the analytical set were prepared by adding a known concentration o f PFOA, 19C PFOA, and PFO$ to laboratory reagents. Laboratory control spikes are used to assess method accuracy. The laboratory control sp ite s must show recoveries between 70130% or the data is rejected . For the results reported here, the laboratory control spikes were within the acceptable range. 4.4 Field M atrix Spikes A low and a high m atrix spike were prepared with the sample and sample duplicate in the field. Compounds were added to the em pty sam ple 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 within the acceptable range. 4.5 Sam pl R elated C om m enta The water samples were collected in duplicale. Duplicate ampie results ara reported in Attachment B. 5 Data Summary Please see Attachment B for a detailed listing o f the analytical results. The results are reported m parts per bilion (ng/mL) for PFOA and PFOS . PAGE4 OF5 6 Statement of Accuracy Based on results o f laboratory control spites, fo ld m atrix spikes, and surrogate sp ites, the analytical accuracy for P f OS and PFOA results is 30%. Laboratory control spites, surrogate spikes, and Held m atrix spikes showed recoveries within this range. Specific sample recoveries are given in Attachm ent B. 7 Data/Sample Retention Samples w il 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 Exygen. Hardcopy data is stored for a minimum o f five years. The client w ill be notified 30 days prior to the disposal of hardcopy data. $ Attachments 7.1 Attachm ent A: Analytical Results 72 Attachment 8 : Spike Recovery Data 7.3 Attachm ent C: Chain o f Custody Forms 7.4 Attachm ent D: Raw Analytical Data PAGB30F3 SI SECTION A Sum m ary o f PFOA and PFOS In W ater Samples E05-0186 L4709-1 L4709-2 N-W6-207643 H-W6-207643 Dltp Analyte Found (ng/mL) ca Add PFOA C8 Sulfonate PFOS Perfluoroootenoete PwfluorooctanMuMorat Nb NO ND NO _ NO Not detected at or above 0.025 ng/m L NQ * Not quantifiable * Measured concentration between 0.025 rtfl/mL and the Limit of Quantitation (LOQ) which I? 0.050 ng/mL. 0006 53 X p a s Drive f% 16801, USA ^ T J:: 814072.1039 I F F: : 814.231.1580 exygen.tiim SECTION B RESEARCH ^Precise Research. Pmuen Results. F M d Matrix Spike Racovary Summary for PFOA and PFOS fn W atar EOS-0186 Sample Description H-WS-2^7643 Low Spike <1414*3,0.1 ppbSplita) H-W6-207643 High Spike (bU*-4,1ppfeSpBu) CSAchfPFOA_______________ C8 Sulfaiurte PFOS Amount Amt Found Amount Amt Found Amount Spiked In Sample Recovered Recovery in Sample Recovered Recovery (nuftnU ina/mL) in tfm i-l____ (%) (naAny (ng/mL) (%) 0.1 ND 0.128 128 ND 0.117 117 1 ND 1.04 104 ND 1.03 103 NO = Not detected at or above 0.029 ng/mL . NQ Not quanttflebie Measured concertfration between 0.025 nflrtnL and the Limit of Quantitation (LOQ) which It 0,050 ng/mL CTZ =>Z) m# A o / a g. Drive !, PA 16301, USA m TJ:8:08I0X02288113219 m fcF: 814.27:2.1019 exygen.com Surrogat Spike Recovery Summary for 1SC-PFDA in Watar 05-0186 Exygen ID Sampla Description L47-1 L4709-2 L4709-3, L4709-4 \ H-W6-207643 H-W6-207643 Dup H-W8-207843 Low Spk H-W6-207643 High Spk Amount Spiked (ng/mL) n C-PFOA Amount Recovered (no/mL) Recovery _) _ 0.5 0.491 0.5 0.522 0.5 0.546 0.5 0.540 98 104 109 108 0007 S6 ich Drive >, PA 16801, USA 800.2813219 : 814372. exygen.com SECTION C 57 3058 Research Orive State College, PA 16801 Phone: 814-272-1039 Fax: 814-231-1580 Log in #: P ro je c t: 4819 P0001275 Company Name: 3M Subm itted By: KENT LINDSTROM Login Type: Started: Im m ediate R eceipt o f Sam ples True Date Start; 03/01/2005 Due Date: 03/11/2005 Received Date: 03/01/2005 Received By: Am m erm an, M ark Spread Sam ple: Label: Exygen SD /Pl: Rlsha, Karen P roject T itle/Type: C ottage G rove R esidential W ater Sam pling / ROUTINE Login Notes: Conform Notes: Conform COC Sam ple: C onform CO C : Conform Sem ple: Conform Request: Package PK000SSSQ Carton Packaaaa / Container De / Condition SM onar/ IO Login Date: 3/1/2005 11:31:46AM Package 4 Contents Unoompnomtied UPS 125765560142913994 Ttm.flatalfTfflB. None 22.3 C ontainer# C0063087 C006308B PKOOOS0S1 Gross W eiotit gH Container Type 253.90 g 500 ml Clear Plastic Narrow 259,00 g 500 ml Clear Plastic Narrow Login Data; 3/1/2003 11:34:38AM Package & Contenta Uncompromised P re se rva tiva NONE NONE UPS 1Z57965E0140875806 ivifia. Lot None 22.3 ConttiMt Sfitti, W tfflM B CanfolmrTvQo C0063039 252.90 g 300 mi Clear Plastic Narrow C0063090 244.40 g 500 ml Clear PJaatic Narrow P re se rva tive NONE NONE Mfa, Lot P inrtlO T ( H w d tfd B i RECEIVED Ammerman, Mark Mfa. ID RECEIVED Ammerman, Mark Mfa. IP L0004709-0001 L0004709-0002 L0004709-0003 L00047Q9-0004 S a rflilm C0063067 C0063089 C0053085 C0O63090 Matrix LIQUID LIQUID LIQUID LIQUID Sample fragten Semole Water HW6-207643 Water HW8-207643Dup Water KW8-207843LowSpice Water HW8-207643HighSpite Data Samolad Data Loacied In Data Due 02/26/2005 03/01/2005 03/11/2005 02/26/2005 03/01/2005 03/11/2005 02/26/2005 03/01/2005 03/11/2005 02/2&/205 03/01/2005 03/11/2005 3/1/2005 L0flin.rpt 0008 Report Version: Feb 22 2005 9:53AM Page 1 of 2 50 instance: R0149340 illlMII Login Reviewed By; ^ Login D ate/Tlm e; f l 5^5 3/1/2005 Login .rpt 0009 Report Version; Feb 22 2005 9:53AM Page 2 of 2 5? Instance: R0149340 iw n iiiin 3 M E n v iro n m en ta l L a b o ra to ry FomMTTft'FWO SkippingUAwk JMBktoiJC-l S3BOutiiAvan LPMLMNfiBUM TitopikMM: iwiihUwliliia (WH7TMM mrnrnm (H1}TTM?SS FAX;fttl) 77M17 'kcgy*^ ConbctNane SjBtjR"ra^r Company HEfenet'<3Mang Addrew Chain of Custody /Request for Laboratory Analytical 08547 Project KVProied Name U v s 4 f> i^ S Template* ~ PmJwiUad L tW lS^y w - \ Dept*<iMbo C 3 c r 3 . i l U Jkll 1L Fln ReportDue Date HHama) Due Data CUee/JoUPrajBct # O 2 - 2 - 6 1 Piatt AvabMe Date Due * & S ~ - 0 /? < g - i& h i city, stata, zip Jr! e Telephone* FAX* Contract Lab c : >0 V e- K ^ -f^ o -U ^ - : f R ( ^ fc _ ^ -v e o r - a i t y fe v * * * /* * /+ S-- PreearvaMv--: A nalysis Requested: o < JA i-3L = /--J L 4 1 *s*i Hem * Client Sample IdanBBcatlon 1. W u i t n - a o ^ f c v ^ 2. \ ^ x i . - i o f i < 4 3 h o D 3M UMS# m te M S6* Data Time Sampled Sampled M ?V Mttrix/ Madia tx9 zc X ii ii r k*nntaitfe*MnmdNd> 1I 11 ? a r > / 8r< 3 (M rnirtalM tm biliwhNbf T f SM_____ ft. U ( J S f i L -- 4. \ A b J ( t - 7 o ^ t . Q ^ S U . ^ ' y l l C * 5. AT \ i iiz v //W \/ l1 t1 ft 7. ft. ft. 10. .;^U t..7. M -- g r > J - -'am # -: : T, i- ( l * ^i r f c r ____________________ Cojectof* signature: w jg :;; 3S T4 . ! ^sj^9 ^ppedy* /- i W!--y ^ V * # ir $ Z iP - /3 r y fSJ* ` //S Cj f ._ -- A - ---------------- -- / 7 * r* . 5Sb ; i.4&- T k /JZ -> a Se : -* r - /, /V <{ * 4 t Sample Condition Upon Receipt Temperature: ahnA iiotlie CoCr *C yZ^Accaptabie o Other O Received on Ice Cepk kr , CammartK it n> e > ^ 6 t? ts l ~ L <X--L 0 y < -A u>w w il< to n ilw 2/28/2005 Project: E05-8186 3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY SAMPLE Contract Lab(s): EXYGEN Page I of 1 Requester: Hohenstein, G u y A (0042-02E-27) Department 530711 Project Number 0022674449 Date Received: 2/25/2005 Project Description: Hastings Municipal Well PC's U Completion Date: Project Lead: Kent Lindstrom Phone Number 651-778-5352 Email Address: krlindstrom@mmm.com SOhKi.p nDate: __/ _____ f Comments: Pace field sampling. ' Note: Reference trip blank on E05-0184. BGJ 2/28/05 E05-0I86 samples traveled with E05-0184 samples. AC, PLf, 2/28/2005. 3M Sample Number Sampled Date Sample Description E05-0186-79868 PFOA PFOS 2/28/2005 PFOA PFOSbyESMS H-W6-207643 Components PFOA PFOS E05-0186-79869 Analysis Code PFOA PFOS 2/28/2005 H-W6-207643 Duo Analytical Method Comoeecati PFOA PFOA PFOSbyESMS PFOS 3/15/2005 3/15/2005 Analysis Dus Dot 3/15/2005 3/15/2005 0011