# Perfluorooctanoic Acid (PFOA) **Site Related Environmental Assessment Program**  **3M and Dyneon LLC** Decatur, Alabama

Quarterly Status Report April 1, 2013 to June 30, 2013

11P-0094-v2-1 

# 3M Company St. Paul, Minnesota

®

# Perfluorooctanoic Acid (PFOA) Site Related Environmental Assessment Program 3M Decatur, Alabama Site

Quarterly Status Report April 1, 2013 to June 30 , 2013

Prepared for: 

## 3M Company

Prepared by: 

## WESTON SOLUTIONS, INC. West Chester , Pennsylvania 19380

W.O. No. 02181.129.138.0001\\ Weston\natacc \ FOLDERS.0 -9\3M
- DECAT \ Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

## i 

# TABLE OF CONTENTS

Section Page 1. BACKGROUND............................................................................................................ 1-1 2. SUMMARY OF ACTIVITIE S ..................................................................................... 2-1



# ATTACHMENTS
Attachment Title 1 GROUNDWATER SAMPLING AND ANALY SIS\\ Weston\natacc \ FOLDERS.0 -9\3M
- DECAT \ Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

## 1-1 

# 1. BACKGROUND
In accordance with the Phase 3 Work Plan for Sampling Environmental Media (WESTON, 2009) and the Memorandum of Understanding (MOU) (3M, 2004) with EPA, 3M is undertaking a Perfluorooctanoic Acid (PFOA) Site

- Related Environmental Monitoring and Assessment Program at their Decatur, Alabama, plant. Per the agreement between EPA and 3M, this report represents the status report of this effort as required by the MOU for the April 1, 2013 through June 30, 2013 time period. For brevity, and following previous convention, this report will be referred to as the June 30, 2013 Quarterly Status Report

.\\ Weston\natacc \ FOLDERS.0 -9\3M
- DECAT \ Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

## 2-1 

# 2. SUMMARY OF ACTIVITIE S
The Phase 2 Work Plan and MOU were finalized on October 25, 2004. Phase 2 of the monitoring program has been completed and Phase 3 commenced on November 19, 2009 with EPA’s acceptance of the Phase 3 Work Plan . This report represents the thirteenth quarterly status report under Phase 3. It covers the April 1, 2013 to June 30, 2013 timeframe and includes a description of activities completed under the Phase 3 Work Plan . In addition to Phase 3 MOU activities, 3M is performing other non

- MOU studies related to PFOA. Where relevant, non

- MOU data may be incorporated in the revised Screening Level Human Exposure Assessment (SLHEA). This non

- MOU information will also be described and provided in these quarterly status reports. Details on activities completed during this reporting period are as follows: On - Site Groundwater Sampling and Analysis As described in the September 30, 2012 Quarterly Status Report, the Phase 3 groundwater characterization program has been completed. The following activities are associated with sampling to obtain additional hydrogeologic and PFOA analytical data for the NPDES Remedial Action Agreement Program being undertaken by 3M under ADEM’s guidance. These are not MOU-related activities.

• On

- site Former Sludge Incorporation Area (FSIA) Groundwater – Groundwater sampling was performed between June 26 and July 3, 2012 at 27 wells in the former sludge incorporation area. Four of the residuum monitoring wells (136R, 137R, 138R and 140R) were dry at the time of sampling and were not sampled. Upon completion of analyses, groundwater PFOA results will be provided in a future quarterly status report.

• 

## Wastewater Treatment Plant Area Groundwater – S ampling was performed on April 29, May 31 and June 27, 2013 at extraction wells WW8R and WW9R in the wastewater treatment plant area. Analysis of the groundwater samples has been completed for the March and April rounds and analytical results are provided in Attachment 1

. In addition, two new extraction wells, WW10R and WW11R , were installed in the wastewater treatment plant area

. After completion of system piping, electrical supply and controls, groundwater pumped from the new extraction wellsJ:\FOLDERS.0-9\3M-DECAT\Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/29/2013 

## 2-2 will be treated by granular activated carbon (GAC) at the existing groundwater treatment system and the wells will be added to the routine monthly sampling of GAC system monitoring points and wellsWW8R and WW9R for PFOA analysis. Screening Level Human Exposure Assessment An Addendum to the Data Assessment Report isbeing prepared and will contain Phase 3 PFOA concentration data in a variety of biotic and abiotic media and describe hydrogeological conditions. The 2008 Phase 2 SLHEA is being updated to incorporate relevant PFOA data collected during Phase 3,an expansion of exposure scenarios under evaluation and the addition of volatilization and aerosolization pathways. Expanded summaries of these activities, where applicable, are included as an attachment to this status report and provi de additional details on the work that has been completed.\\ Weston\natacc \ FOLDERS.0 -9\3M
- DECAT \ Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

# ATTACHMENT 1 ON- SITE GROUNDWATER SAM PLING APRIL 1, 2013 – JUNE 30, 2013\\ Weston\natacc \ FOLDERS.0 -9\3M
- DECAT \ Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

## Att 1-1 ON- SITE GROUNDWATER SAMPLING 3M DECATUR, ALABAMA The following subsections describe non

- MOU on

- site groundwater sampling activities completed during the second quarter of 2013 (April 1 to June 30) in conjunction with the NPDES Remedial Action Agreement Program

. Former Sludge Incorporation Area Groundwater Sampling Groundwater sampling was performed between June 26 and July 3 , 2012 at 27 wells in the former sludge incorporation area. Four of the residuum monitoring wells (136R, 137R, 138R and 140R) were dry at the time of sampling and were not sampled. Upon completion of analyses, groundwater PFOA results will be provided in a future quarterly status report.
Wastewater Treatment Plant Area Groundwater As described in the December 31, 2012 Quarterly Status Report, routine sampling of the two wastewater treatment plant area extraction wells (WW8R and WW9R) and groundwater treatment plant monitoring points is being performed on a monthly basis. Sampling during this reporting period consisted of sample collection on April 29, May 31 and June 27, 2013. Analyses have been completed on the March and April 2013 samples and PFOA results are provided in Table 1 and shown on Figure 1. Following Alabama Department of Environmental Management (ADEM) approval, two new extraction wells, WW10R and WW11R , were installed in the wastewater treatment plant area between June 5 and 6, 2013

. Bedrock was encountered at approximately 31 feet below ground surface (bgs) at WW10R and 24 f eet bgs at WW11R. B oth wells were constructed with 6 inch diameter stainless steel casings and screened in the residuum

. After completion of system piping, electrical supply and controls, groundwater will be pumped from the new extraction wells for granular activated carbon (GAC) treatment at the existing groundwater treatment system. The new wells will be added to the routine monthly sampling of GAC system monitoring points and wells WW8R and WW9R for PFOA analysis.

## Figure 1 Groundwater Average PFOA Concentrations Wastewater Treatment Plant Area Extraction Wells March 2013 - April 2013 

# μ 300 0 150 Feet

File: Y:\3MDec\MXD\WWTP_PFOA_EW_mar_april2013_Results.mxd, 7/19/2013 10:24:19 AM, ricksc Legend



### & < Monitor Well Location

Decatur, AL Imagery: ESRI Bing Mapping Service

Note: PFOA concentrations are the averages of primary and duplicate samples. 

# Well ID Date Average PFOA (ng/mL; ppb) WW8R 3/27/2013 3640 WW8R 4/29/2013 3190 Well ID Date Average PFOA (ng/mL; ppb) WW9R 3/27/2013 3330 WW9R 4/29/2013 2650

## Table 1 On-site Wastewater Treatment Plant Extraction Wells Groundwater Average PFOA Concentrations March 2013 - April 2013

Sample ID Well ID Date PFOA (ng/mL; ppb) DAL-GW-WW8R WW8R 3/27/2013 3640 DAL-GW-WW8R WW8R 4/29/2013 3190 DAL-GW-WW9R WW9R 3/27/2013 3330 DAL-GW-WW9R WW9R 4/29/2013 2650

Notes: PFOA concentration is the average of primary and duplicate sample analytical results.

\\Weston\natacc\FOLDERS.0

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‐ DECAT\Phase_3_Work_Plan\2Q13 Status Report\Attachment 1\Table 1‐ WWTP_Area_Extraction_Wells_GW_PFOA.xls\\ Weston\natacc\ FOLDERS.0 -9\3M- DECAT\Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

# APPEND IX A TO ATTACHMENT 1 WWTP EXTRACTION WELL S - MARCH 2013

ANALYTICAL DATA REPO RTISO13-07 - 033M ENVIROIV'A9ENTAL LABC}RAT~RY R~P~RT A!O_ JS013-07 -03



### '. !! 

# Analysis of PF+aA, PFBS, PFH~, any! PFC)~ in Aquer~us Samples from 3M [~e~atur, Alabama: Grflundwater Treatment Plant GAC Systerr~

— March 2013 Laborats~ry ~~qu~st Dumber: I~C~'13- 07-{~3

Report Date —Date of Last Signature 

# T~:sting Laboratory 3M NHS &S C)per~#ions 3M Environmental Laboratory Building 2~i0-~N -17 Maplewood, Mil ~~'144 -10Qt~ 

# t~equester nary Hohenstein 3M Building 224- 5W -fJ3 Saint Paul, MN ~~144-1007 Phone: {~51) 737-3~7~

The testing repar#ed herean meet the requirearterrts of AMS~I/ISOIIEC 17025:Zt105 "General q) Requirements for the Competent of T+es~ng and Calibratia~ Lat~oratnries ", in accordance with the A2~A,

Testing Certificate # 2052.01. #~C~~~~E~ C3 

## TeStlr~g Cert #2052.01

PAGE 1 tD~ 213tvJ ENV9RC}NMENTAL LA80RAT~RY f?EPt'~RT NO. lS~93-07 -03



### 3 Environmental Laboratory 3M Enviranrn~:ntal Lal~or~tory Technical Glirector: William IC. Reagen, Ph.~. 3M Principal Ana9ytical Investigator: Swan 1Notf Report Author: Chetsie Grochow

3tv1 Decatur Ground+nrater Teeatment Plant System; March 2 13 Sampling

Report C1ate: Date of Last Signat~.~re

•~ ~
the 3Ni Environmental Laboratory analyzed water samples fr+a►n the groundwater treatment plant GAC sys#ert~ at the 3M Decatur, AL facility. Water samples were collected by 1lU'estc~n Sc~lutians personnel on March 27, 2013. Samples were returned to the 3M Environmental Laboratory for analysis of Perfluorooctanoate {PFt3A), Perfluorobutane sulfonate {PFSS), Perf~uorohexane sufifonate (PENS), Perfluorooctan+e sutfona

#e {PFt3S), and the surrogate recovery standards ~3C4-PFOA and ~~C4-PFOS under laboratory project number 8SO13-07-03. Analysis of the samples was completed as specified under 3M Environmental LabQratQry General Project Outtine ~GPaj number GP011 -100. The 3M Environmental Laboratory provided sample eon#ainers for five samp~ir~g lcacations; ACl, ACM2, ACE,1lWV8Ft, and WW9R. The sample set consisted of a feld sample, fiels~ sample duplicate and a field matrix spike. Each ~m{~ty ~antainer was rnariced with a "dill to here" lire that corresponded to a final volurn~ of 2Dfl mL. Gc~nta~ners reserved for field matrix spikes were fortified with an appropriate ma#rix spike solution containing all analytes prior to being sent to #~►e field for sample collection. Sampfe bottles for sampling locations ACM2 and ACE,alor~g with the Trip Blank sample and low spike, were fortfied vrith internal standards and surra~ates pri~sr to being sent to the field foc sample collection. Samples were prepared end analyzed by r~et~od E'f'5-8-044.1 "Method of Analysis for the Determinatic~rs of Per#~~uorinat~ed Compounds in Water by LCIMS /MS; Direct Injection Analysis". Select internal standarr~s were used to aid in the da#a q+uali~r ofaj~ctives. Table 7 sumr~narizes the sarnp9e results using the analytical method identified above. All results for quality+ control samples prepared and analyzed with the samples will be reported and discussed elsewhere in #his report.

~_( The testing reported herein meet the rQquirements of ANSIlISOlIEC 17025:2Q05 "General ~I 

### ~. ` ` Requirements for the Competence of Testing and Galibraation oratories ", in :- ~J acoordan+ce wiNa ~e A2LA Testing Certificate # 20 2.01. =AGC~s~~[ k~~L~

T@St1I1CJ C

@I't #~~rJ~.~'~

PAGE 2t3F 2131lAEAtVIRt7NAAEIVTAL tA8{7RAT~RY J~,EP47RT t1lO_ IS013-D7 -03



### Table 1. Sample Results Surtimary

PFDA ~'FBS PFHS PFOS Concerrtration Concentration Conaen#ration Concentration 3~WI LIMS ID Sample Description {ngtmL) (nghnL) {nglmL) {ngirnL) iS033-0 ?-03-(~31 DAL- ~W -ACI; Sample 2190 106[3 3D80 250 IS413-d ? -03-OD2 DAL-~WACI~ Sam le Du 2250 1D64 1090 252D Average 2220 {'S 1060 {'y 9{190 ~'~ 2490 ~'~ °1a12PD Sett eJSam le Du 2.? 0.0 0.92 2.8 IS093-07 -03-DD4 DAL- GW -A~M2; Sample 52.9 2300 170 +D.{3509 (SQ13-0~ -05 DAL- GW- ~iCM2~ Sam ie Du 50.9 2330 171 O.U526 Average ~1.~ ~~'~ 2320 ~'~ 17'~ ~i'~ 4.051 ~~ °IaRPD S,3m 1~ISam IB Du 3.9 1.$ 4.59 3.3 ISU13-07 -03-107 L7AL-GW -ACE; Sample O.fl362 ~0.02~(i ~D.0433 <0.0232 IS013-fl7-03-8 DAL-GWACE Sam le Du fl.fl398 <0.4250 0.052'l <p_0232 Average 0.0384 ~3~ •c0.0250 ~'} 0.0477 ~~ <U.0232 ~3j %RPD 5~ripleJSample Dup 9.5 NA 18 NA ISrJ13-07-03-01a C3AL- ~W -WW8R; Sample 3660 38Q 1 ?6fl 5170 1St71~ -07.03-411 ~~4L-GW -WW8R~ Sam le Du 3620 389 1760 5070 Average 5640 ~~f 385 ~~) 980 t~} 5120 {~~ %RF'D Spiet5ample Dup 1.1 2.3 0.0 2.0 ISd13-07 -03-013 DAL- GUV-WIN9F2; Sample 326 273 1490 4530 ISCD13-07 -03-fl14 DAL- ~W -WW9R~ Sam le Du 3404 283 947fl 4780 Average 3330 {~~ 278 {~i 34d0 ~~~ d660 ~'~ °loRPD S~npletSample Dup d.2 3.6 4.2 3.4 I~dA = iVot Applicable {1) I~ep~ted resul#s v~ere prepared ~d ar~lyzed by E('S-8-D94.9 using extemai star~ard c~ibraticm_ The ~atytical method ~cer#ainties associated witli the re~+orted results are as follows: PFOA ±18°to, PFBS ± ~1 °lo, PFHS ±95°la, and PFC7S ± 24°fo. ~2) Sampi~ did nok have an ~proExiate FMS #o access r~c~very_ See section 4fic~ rn~ details_ (3) Reported results were pr+e~ared and sraaiyzed by ETS-8-444.1 using inte~na! standard csibration. The an~yfical method certainties associated wifh the r~orf~ed results are ~s fo~lcrrv,+s: PFOA ± 16°fo, PFBS ±22°Jo, PFHS ± 94°l0, ar►d PFOS ± 24°l0_



## 2.9 Methods Analysis was sample

#ed u$ing 3M Envircjnmental Laboratory Method ETA-8- 44.1 "Methc~ of Analysis fc~r the Deteraninatian of Perfluarinated Compounds in 1Nater by LCIMSIMS; direct Injection Analysis". 'able 2 Target Analytes.

Tar et Ana s Acron Reference Material Structure Perfluoraockanoic Acid Cfl Acid PFOA Linear +ranched Perfluarobutar~sulf~nats (C4 Sulfonste) PFBS Line Perfluorohex~esutfor~te Ck'i Suffor~te PFHS L+near Perfluorc~ctan~sulfonate (C8 S~f~ate) PF~S Lir~ar ~- Branched

PAGE 3{3F 213A~1 ENVIRC3NA9ENTAL tABQRATORY REP{~RT N{?. ISCJ93-07 -113



# ~.2 Sample Coll+ectc~n Samples were collected on Maa-~ch 27, 2013 in NalgeneT"1(high-density polyethylene) bc~ri~es prepared at th~ 3M Envir~nmen#a! Laboratory. Prior to sample oollecti~n, bott{es designated for field matrix spikes were spiked in the laboratory with a knows volume of an appropriate matrix spiking solution ~ntaining PFOA, PFBS, PFHS,and PFt}S. Sample battles fc~r sarnpting locations ACM2 and ACE, along with the Trip Blank sample and low spike, were fortified wi#h a mi~ttiare of rr~ass-labeled intemat standards at a nominal concen#ration of 1 ngJmL and a mixture of surrogate recovery standards at a nominal concentration of D.1 ng(mL. Collected sample tx~ttles were received by the Laboratory at ambient condrtians on Aprif 1, 2t193. 

# 2.3 Sample Prep~ra~tit~n Samp[e sets ACI, ACM2, WW8R, W`W9R, and 'the Trip Blank high spike were diluted 3:1~D0 and analyzed for ail analytes. The 1:140 dilutions were prepared by removing a 0.1 mL aliquot of the well mixed sample and adding 9.8 mL of methanol and D.1 mL of ~ surrogate spiking solution. ~'r~paret! samples were analyzed by e~t#emal standard calibration. The ACE and A~M2 sample sets and the Trip Blank sample and low spike were prepares! and analyzed for alf analytes by transferring an aliquot of ~e well mixed sampfe into an autovial. Prepared samples were analyzed by internal standard calibra~on. During the preparation of the tabaratory control samples for internal standard calibration, are aliquot ~of a separate intema! standard spiting sr~lution was added to the laboratory intro! samples {nominal concentration of 1 nglmL). The sample bottles for ACE,ACM2,end Trip Blank were spiked with an internal standard mix at a nominal concentration of 1 nglmL prior to being sent to the field for sample col~ectian. The laboratory conir+ol samples were analyzed in the same manner as the samples. 2.4 ~41'ta~~/SIS All samples and quality contr~i samples wire ana9yzed for #our target analytes using high performance liquid chromatographyltandem mass spectrometry (HPLCJMSlMS}. Pertinent instrument parameters, the liquid chromatography gradient program, ar~d the speafic mass trans ions analyzed are described in the tables below. Due to #tie nature of the sample,the wide range of concentrations found in the sar~pte, and ~e

environmer►tal

occurrence of multiple isomers of the labarator}~s analytes of interest, the software used for processing tf~e analytical results is not able #c~ t~nsis #envy integrate the anatyt~cat peak, manual integration of the analytical peak is necessary. All manual integrations are performed following tl7e procedures outlined in rnetho~3 ETA- 'i2-0~~. The consistency of the laboratory's integration is ensured through the training of laboratory personnel, the peer review prc~oess requited for all r~a~ua! integrations, the review of rnanua( integrations by the QAtl, and where necessary the review of manual integrations by laboratory management.

## ~~r ~n~vr~an~n~~~vrAC caeo~ro~zv REPORT NC7. tS093-d7 -03



### Table 3. Instrument Parame #ers.

Instrumerrt Narr~e ~1'S KiNc ETS tGrk Analysis Dates 413/13 -exte►nai standard calibration 414113

- internal star~dar~i c~ibraticm A»al 'cal Method ETS-F3-444.3 ETS- 8-044.1 Liquid Chromato~raph Agii~t 1260 ,Agile# 1260 ward column Betasil C18 {4.6 mn ~ aDD mm),5 Betasil C18 (4.6 rr~n X 100 rr~n), 5 Maly~icai column Basil G18 {4.~ rr~n X 3{lD rrun }, 5 B~;tasil C18 {4.6 rr~n X 'lU0 rr~n), 5 Injection Volume 2 5 or 20 20 Mass S meter Lied Bins ems Tri IeQuad 550D lied Bios ems Tri IeQuad 5500 lon Source T►~tjo 8 ra T~bo S Pota ' alive Id alive Scrttware Analysk 1.6.1 Analyst 1 _~6.1 

### Table 4. Liquid Chromatography Gradien# Prt~gram.
Step Number Total Time

min Flaw Ra#e

( minj PercerttA

2mN►ammonium

acefate Fer+centB

NJ~`hen 0 O.Ofl ?50 90.E 1 D_D 1 O.fiO ?~0 90.fl '10.0 2 -0.00 750 7fl.0 3p.Q 3 6.00 ?50 70.{3 30_U 4 11.0 75~ 2fl.0 80.0

13.0 ?~0 20.0 8QA 6 1~_5 ?50 10.0 '~0.0 7 16_D 75D 10_D 90.0 8 16.5 750 90.0 10.0 9 19.0 750 9Q_fl 1D_0 

## Table 5. Mass Tr~nsitians

~~~ Mass Transition ~t1/Q3 Irltemai Standard t9~ Mass Transitiarr Q11t~S

PFOA 4131369 [~~]PFt>A 421137E 4131299 4131169 PFBS 299I$D ~~e~PFBS 303184 299199 PFHS 399199 [isCsIPFHS 402/8fl 399!80

PFOS 49~J199 ~13Cg3PFOS 507180 499180 499/130 [13C,~jPF{)A surrogate 41713 2 [~~jPFOA 4211376 ~~C.~ PFOS su ate 50318U 13C8 PFOS 507l8t3 Du~11 tirr~e was 5{l for e~h tr~nsi~an. The individual transi~cu~s were sumrr~ed 4o produce ~ 'Yotat ion chrome #ogr~n° (TIC), which was used fnr quantitation. 1 Internal standards were used for fhe arse! ~s on A14113_

PACE 5 t9F 21

## sr~~nrvi~zc~~vn~~nrT.~~ c~~o~iarorzr f2EPC7RT NO. ISC}93-t17 -03

r 

# 3.~f +Calibratifln In #emal Standard Calibration Analysis: samples were analyzed against ~ matrix-ma #coed stai~l~ isoto~ internal standard ~alibratian curve. Calibration standards were prepared by spiking known amounts of stock soluutions in #o 50 mL raf laboratory prep~r~d reagent water. The calibration standards ~cantained are inte►nal

standard max at a norninai c~ncentra#ion of 1 nglmL. A total of #hirteen calibrati standards ringing from {)A25 nglmL to 25 ng /rnL {nominal) were analyzed with the pr~par~d samples. Of ~ese thirt~eri calibration standards, eleven contained the surrogates at conc~n#rati~ns ranging from 0.025 n~lmL to 1 ~4 ng

/mL nominal. A quadratic,l /x weighted, calibration aurWe of the ratio of the standard peak area counts over tt~e internal standard peak area counts was used to fit the data for each analyte. Tt~e da

#a were nc~t forced through zero during the fitking prflcess. Calculating the s#~nd~rd concentrations using the peak area ra~c~s and the resultant calibration curve confirmed accuracy of ead~ curve poSnt. The reference standards of P~OA and PFtJS used #o prepare the calibrati~ standa~r~ls consisted of both linear and branched isomers. Each curve point was quantitated using the overall calibr-~tion curve and reviewed for accuracy. Method calibrati~r~ accuracy requirements of 100±25% ~1{?0-!-3~ %for the lowest curve poin #) vrere rne# for all analytes. The c~arr~lation coefficient {r) was greater than 0. 95 for al# ana(ykes. F~ttem~ Standard C",alibratian Analysis: Samples were analyzed against an e~err~al standard calibrati~ cxarve. Calibration standarids wire prepared by spiking known amounts of tl~e sf~ock solution containing the #arget analytes into 9fl:1~? methanol: Milli-t~ laboratory water. A to#ai of tin spiked s#~nd~rds ringing fr~n 0.~2 nglrnL to 25 ng /ml. {nominal) were analyzed. The ten standards also contained the surrogates ai concentrations ranging from 0.02 ng1mL to 26 nglmL nominal. A quadratic, the weighted, calibration curve ~f the standard peak area jaunts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. ~C:alculating the standard concentrations using the pear area counts and the resultant calibration curve cx+nfirme~l acr,~.~racy of each curve point. Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method ca~fibration accuracy requirements of 100 ±25% (100±30°lo for the I+~west curve point} were met far all ~nalytes. Tt~e correlation c~efficierrt (r) was greeter than 0.995 for all analykes. 

# 3.2 System Suitability A calibration standard was analyzed four times at the beginning of the analytical sequence to demons#rate overall system suitability_ The acceptance c►iteria for system suitability samples is I?~c than or equa(to ~ °lo rela~ve standard deviation (RSA) fear peak areafratio and re#entiot~ time criteria of less than or equal to 2°lo RSC}. Tt~aese criteria were met far all analykes. 

# 3.3 Limit of Quantitatic►n ~Lt~►Q) Thy L{)Q as defined in methc~ ETS-&Q44.1 is the lowest non-zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twig ti~ose of the appropriate blan~CS. 'fie LOQs associated with the sample analysis are listed in Table 6.

PAGE 6 OF 213Ad ENVtRONflAENTAL tA8{)RATOF2Y REPt)RT NC7. !SO'13-07-113

.. e •

~, Analyte Gatibration ~{7C1, nglmL PFOA ~ntema! standard (l.024Q PFBS ~ntemai standard x_0250 PFHS ~ntema! standard fl.025D PF~S ~ntemal standard D.0232 PF~A Ejdemal standard fl.fl192 ~'~ PFBS Exterr~a9 st~►dard fl.fl2D0 ~1~ PFHS E~dtemai st~dard D.fl200 {'~ PF4S Exketr~l standard {3.{1485 {~} {1 } Tfie dilution facts was r~ applied to the L~Q. 

# 3.4 Continuing Cafibratiar~ During the course of t3~e analytical sequ~n+ae, several ecmtinuing ca(ibra#ion verification samples {CCVs}w~r~ analyzed to confirm that the instrument response .and the ini~a! calibration curare were still in +control. 3'he me~od ac.~ep #ante criteria of 100% ± 2~°!o was met far a!l ana~ykes. 

## 3.~ B11nkS Two types of blanks were pr~par~d and anatyzed with the samples: method blanks/solvent blanks end field/trip blanks. Each blank resin# was reviewed and used to revaluate rnei~od performance to determine the LUQ #or each a~tatyte. 

## 3.f Lab Control Spikes (LCS~~ ~.ow, mid, and high I~b control spikes were prepared #ar the urge# analyt~s and anafyzer~ in triplicate, while only low and high lab control spikes were prepar~c! far the surroga #yes. LCSs were prepared by spiking known amounts of the analytes into either 10 m~ of dal~o~-a #cry-prepared matrix matched water or 1 mL of Milli -Q water to produce the desired c~oncen#ratian. When applicable, the LCSs were then diluted with me#har~ol in the satr€~ manner as the samples. Method ETA-8-044.1 states that the average recovery of LCSs at east spiking leuel be within 8U°10- 92Q°lo witfi~ ~ RSL~ 520%. Ail LCS samples met r~ei~od accuracy criteria except where noted below. Ex#emal standard analysis: Mid level L~Ss did not meet average recovery criteria for PFB~ {121 %) arad PFOS (122°l0}. High level LCSs did not meet average r~cavery cxxi#teria PFG1S (124%). Internal standard analysis: Mid level LCSs did not mgt auerage retx~very cxiteria far PFUS (124°l0). High le~re~ LC~s did not meet a~rerage recovery cxi#eria for PFBS {122%) and PF4S ~~22%). A method deviation is included v,~th the raw data. All LGSs wire us+~d in the determination of the analytical method uncertainty in sec#ian 3.9. The following calc~.~lations w~r~ used to generate data in Table 7.

~C8 Percent Recovery = ~alcufated Concentration x

100°✓n Spike Concentration
~~~p~o ~~~ _standard deviation LCS replicates x ~~~0~4

average LCS recovery

PAGE7~2131v9,ENVtRONAAENT.4t tA8{?RATaRY REPORT Nfl. ISO93-07-Q3



### Table 7. Lab Cfln

#rol Spike Results.

ECS-8- 1044.1 Extemai Standard Calibr~fion Anatyzed 4,'3f 93 PFOA (Linear +Branched) ~'FOS (linear +Branched) Spiked Calt~lafied Spiked Calculated Concsr~lrat~an Cancerihafi+rm Concentration Cflncenfration Lab IQ ~nglmL} (nglmL) °kRecovery {nghttL) (ng1mL~ °Recovery LCS- 1304{3-1 0.191 0292 111 ~.18a 0.198 107 LCS- 9304{x.3-2 ~D.191 02D1 ~~05 0.985 0.1 9 108 LCS-~ 30403-3 x.191 0.2'!1 '] 1D {}.185 0.20{? 1~D8 Avet~gie ~ %RSLY 109° /n ± 3.d°In 1U$ °lo ± 0.5d °10 LCS-X30403-4 1.91 229 920 1.85 224 121 LCS- '~344D3

-5 1.91 2.26 '~ 18 1.85 2.24 121 LCS- 9304{)3-6 1.97 2.33 722 1.85 2.28 123 l4Vef'dge ~ °laRSD 120% t 1.7°la 922 °l4 ± 0.95 °!4 {i? LCS- ~3d403-Z 19.1 22,1 914 18_~ 23A 124 LCS- 130403-8 19.'~ 21.0 X10 18.5 223 921 LCS- '130403-9 '19.1 22.1 116 1$.5 23.5 127 AVet~gE #' °IoRSD 114°1n ± S.0°lo 924°10 # 2.d °Jo ~~~
ETS- 8- 1144.1 Exteanal standard calibration Analyzed 4W3113 PFBS PFNS Spiked Calculated Spiked Caic~ulatec! Concerstr~ation Conceritrati~ ~ancentration Concentration Lab ID (nghr~L) (nghnL) %Recovery {nglmL) (ng/mLj °,~Rt~ very LCS- 930403-1 {1.199 D221 '111 0.'!99 0216 1D8 LCS- 3304(~i-2 0.199 0219 '~10 x_199 0.214 108 LCS- 130403-3 0.199 X223 112 1}_'!99 0223 112 Average t °lof2SD 

## ~ ~ ~ °r~ ± a.~Ar~ 109°!0 ± 21 °~ ACS- 130403-4 1.99 2.39 3~0 1.99 2.32 117 LCS- 3304D3-5 1.99 2.41 'f21 1.99 2.36 119. LCS- 9304113-6 1.99 2.45 923 1.99 2.37 11~ Ave~dge ~ °loFiSD 921 °h ± 1.3° /n'~~ 11$°l0 ± 0.9$% LCS- 130403 -7 20.0 22.9 '114 20.0 22.1 910 LC5- 930403-8 20.fl 22.1 '!10 20.0 21.1 105 ACS- 9304fl3-9 20.7 23.8 X 19 20.0 21.9 909 Avenge t °JaRSD '' 114°k # $.9°!0 10$°Jo # 24 °fo (1) LtSs did not meet soceptarace criteria of 10D ± 2{?°l0_

PAGE 8 OF 21

## sn~Fn►vr~z~nrn~~rvTac usawarc~Rv REPORT NtJ. IS093 -07-03



### 7abfe 7 continued. Lab Control Spike Results.


## ors- ~-oa4.~ External Star~rd Calibra5on Anal ed 4!3/13 PF{)A sau a#e PF0.S su ate Spiked Calculated Spiked Calculated Conaerrtrafion Concentratia~ Concentration Corscentration Lab ID n mL n mL °loRecave n L n rr►L °loRec~vs LCS- 1304{13-1 0.199 02Q2 ifJ1 0. ?9D ~D.196 '1p3 LCS- '!304{}3-2 0.19 0.2{~'i 9(kl ~.3~0 0.197 103 LCS- 1304fl3-3 D.199 02Q8 104 4.'190 0.195 1D3 Average ~ %RSD 108%± 1.7°l0 903°l0 ± 0,0°l0 LCS- '!304(13-4 1.99 x.09 905 1.94 2.06 149 LCS- a3~4403-~ 1.99 2.13 9d7 1.90 2.D5 108 LCS- 1304fl36 1.99 x.12 1~ 1.90 2.05 108 Avera ± ~

/9RSC? '1 d6°~fl ± 0.9d°Jo 1~8°Id ± 0.53°lfl
ETS-8 -044.1 Internal Standard Calibration Anal ed 4l4W43 PFOA (Linear +Branched} PFOS (!_inear +Branched} Spiked +Caicul~ted Spiked Calculated Concentration Ccncer►trati~ Concentration Concentration Lab ID (ngtmL) (n±gtmL] °leRecove►'Y {n9hn~) ~nglmL) °kRec:ov+ery LCS- 930404 -1 0.190 0.2{x.5 '~D8 0.984 0.297 118 LCS- 1304 4-2 x.190 x_242 906 0.984 D.21a 117 LCS- 130404 -3 D.19D D_19? 304 0.184 028 119 Avers t °foFtSD 1D6°Jo ± 1.9°l0 118 °l0 ± 0.8~°!fl ~C~?304{)4 -4 1.90 2.2~ 118 1.84 2.35 12~ LCS- 3304{14 -5 1.90 2.21 916 1.84 2.17 118 LAS- 130404 -6 1.90 223 117 1.84 2.32 126 Average ± °laRSD 917°Ifl ± 0.85% 12d °lfl ± d.3% ~i~ LCS- 130404 -7 9.52 10.E 311 921 10.4 113 LCS- 13d40h-8 9.~2 '11.8 '~24 921 11.4 124 LCS- 93D4tk~-J 9.52 '12.D 126 921 11.9 129 Avers e t %RSD '' 120°l0 ± 6.8°Jo 122°la ± 6.7 °lti {~~ (1) LCSs did riot meef accepfance cri#eria of itl0 ± 2D°lo.

PAGE 9 C7F 213M ENVIRDNA?EIVTAL tABdRATQRY REPORT l4'f1. IS(733 -07-03



### Table 7 continued, Lab Control Spike Results.
ETS,8 -Od4.1 Intemai Standard Calibrstian Anal ed 4!4!13 ~'FB5 PFHS Spiked Calculated Spiked Calculated Concentration Concer~tr~tior~ Concentration Goncentrafiion ~.ab ID n mL n L %R~cove n L n L °kRecave LCS- '~304fl4 -1 0.198 0215 '~t38 0.198 [1.219 111 ACS- 934464-2 fl.198 d_221 '~12 0.198 02'6 109 LCS- 130404 -3 ti.198 0237 910 ~3.~98 023 108 Average ~ °fflRSD 114% ± 1.8°!4 ~ ~ °Jo # 1.4°,~ LGS- 130404 -~ 198 2.34 318 1.98 2.32 117 LCS- 730404 -~ 1.98 2.34 '~ 18 1.98 229 116 LAS- 1304{34 -6 1.98 x.44 123 1.98 2.38 120 AVerd $%RSD 120°!0 ± 2.d°fo 918°!0 ± 1.$°l0 LAS- 130404-7 9.94 19.3 '~ 14 9.911 11.4 111 LCS- 130404 -8 9.94 'i2.5 126 9.94 11.8 119 ACS- 93D404-9 9.94 12.6 927 9.94 12.2 123 AVe~ge ± °loRSD 922 °Jo ± 5.9°k'~~ 11$°l0 ± 5.2%

ETS-8-DA~3.1 In #ernal St~dard Calibration Analyzed4

/4!13 PF~A surrogate PFflS surrogate

Spiked +Calcxlfa~ed Spiked Calculated Concentration Conce»tratic~n Concentration Concentration Lab (D n mL n L °kRecove n L n L %ReooY@ LCS- ?3Ck104 -1 fl.198 0.191 96.4 0.189 0.186 98.4 LCS- 93040A-2 ~D.198 0.189 95.5 0.189 0.186 9&~ LC~730404 -3 ~I.1~8 0.186 9~.9 0.189 0.19D 101 Average ~ °loRSD 95.8°~ ± 7.S°lo 99.3°,~ ± 1.5°~ ~C5- "I30A{{}4-~4 1.98 1.95 98.5 1.89 1.95 103 LCS- 9304[k4 -5 1.98 2.Q1 102 1.89 1.87 98.8 LCS- 73D404 -6 1.98 2.~0 1fl1 1.89 1.92 102 Aver ± °IaRSD 14?9 °~6 ±1.8 °le 101 °14 ±22 °h (1 } LCSs did not meet acceptance criteria of 9 ~ ± 2()°l0.

PAGE 9d t3F 21

## ~n~~rvvr~zarvn~~nrra~. t~aowaro,~v REPORT Nom. ISO93-07 -03



# 3.~ Analytical Metho~f Uncertainty Analytir.~l u~ac~rtainty is based ~n historical QG data thai is control charted and used to evaluate method ~ccxaracy and precision. The method uncertainty is calculated fc~ilawing ETS-1~-012.2. The standard deviation is calculated fior t3~e set of accuracy results din %) obtained ftir the QC samples. The e~anded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence i~v~l of 95°,/0. The rne~od uncertainty was deterrnine+~ to be ±17%for PFBS and ±16°lo for PFOS using internal calibration and ±~ 5%for PFBS and ±20%for PF~S using e~ctemal calibration, but based on the percent bias of the LCSs, the meth!uncertainly has been e~anded for PFBS and PF~S. T~bl~ 8. Analytical Method Uncertainty. Analyke Calibration MetFaod S#andard Deaiatian Method Uncertairrty PFt3A E~demal Standard 8.86 ±18%a PFBS Fasternal S#andard i~tA X1410 PFt-IS ~ctetnal S~atidard 7.71 ±15% PFOS Ex6err~al Starxlard NA ±2410 PFOA Internal St~nd~d $.D2 ±16% PFBS ~nteR13( Standard fdA ±22 °/a P~HS Internal Stand~d 7.02 ±1~°l0 PF4S ~nt~nal Standard NA ±24% NA= Not Applicable 

## 3.8 Field a

#rix Spikes {FMS) Afield matrix spike was collected at each sarnplin~ point to verify that the ana9ytical method is applicable to the collected matrix. Field matrix spikes are generated by adding ~ measured volume of fteld sample to a ct~ntainer spiked by the laboratory with the #arget analytes prior to shipping sample c~n#ainers for sample collec6an. Feld rnatri~c spike recoveries wi#hin method acceptance criteria of 10fl±3~ °lo confirm that "unknown" components in the simple matrix do not sig~ificant~y interfere with the e~raction and analysis of ~e analytes of interest. The standards used for the preparation of t#~e field matrix spiking solutions contained reference materials comprised of bo#h linear and branched isomers #or PF4A and PFOS. Field matrix spikes are presented in section 4 t~f this report.

FMS Recovery - ~~ample Cancentratic~ of FMS

- Average Concentration:FeldSample &Field Sample Dup_} s,~~~~~ Spike ~ncentraton 

### Table 9. Field Matrix Spike Concentrations

Final Concentration (ngh~►~) Location Description ~'FflA PFBS PFiiS PFt3S ACI Field Matrix Spike 211 ~ '1990 197 20~Q RCM2, ASE Field Matrix Spike 10.5 9.96 9.86 1 ~.{~ WW8R, WW9R Field Matrix Spike 4220 3980 394 4DOQ Trip Blanc Low Feld Matrix Spike 10.5 9.96 9.8& 10.{3

Huh Field H+~#nxSpike 4224 3980 394fl 4DOD

PAGE '~1 t}~ 213M ENV {ROlVN1ENTAL iA~30RATORY REPORT IV~7. ISt713-07 -03



### ~'he tables below summarize the sam~te resul#s and field matrix spike reco~✓eries fior the three locations ~s well as the Trip Blank. Each table provides the average concen#ration and the relative pe►-~cent difference ~ °loRPD)of the sample aid sample duplicate. Results ar~r~ av~r-age values are rr~undec! to #hree s6gnificant figures. Percent relative difference {%RPD) values are rounded to two sign cant figures. Secaus~ of rounding, values may vary slightly from #hose listed in ~e raw data. Feld matte spikes meeting tie method acoep #ante criteria at ±30 °l0, demonstrate that the method is appr+~priate for #hie given matrix. All field mafrix spike samples and surrogate recovery standards met me~od ~~ceptance criteria except where noted belovu.

DAL-GW-ACM2; the FMS sample {10 ng /mL) was not ~ppr4~riate for PFflA, PFBS, or PFNS; however, it~e FMS sample for PFQ~ and tie surrogate recovery standards ~~C~ -PFOA and 13C~ -PFOS, met method acceptant~e criteria. Igo additional QC samples were ~repar~d.

PAGE 92 {7~ 213M ElUVJRONJVIEIVTAt tA80RATC~RY REPC)RT tv'O. 1593 -07-03



## Table 1U. DAL GW ACI 13{327 t'}

P~~DA ~FBS Cancerairation Conce~#rakion 3M LIMS ![~ Description (ngrrtaL) °Recovery {ngimL) °laR~ very IS013-07 -03-fl~1 DAL- ~W

-ACf-0-90327 219D t~fA 106 I~lA IS013-07-03-002 QAL-GW- ACI-L3B- '13Q327 22x0 NA 106th NA tSD13-07- CI3--(~3 DAL-GW-ACI-FMS- '~30~27 ~ 421fl 94.3 2930 94.D Average Concentration {n~mL) ± °loRPD ,2220 ng/mL ± 2.7°k 1460 ng/mL ± 0.0°l0

PFHS PFOS Concentration Concen#ration ~+I LIMS ID description (ngtr~~L) ° /QRecovery {ng/mL, %very ISQ13-07-0~fl1 DAt-~W ACt-4930327 1480 NA 245fl NA IS013-07-03-002 ~AL-~W fi,CB-DB- 13Q327 1090 NA 252{3 MA tSIJi3-07-03-003 L7AL-GW~1Ci-f=MS- 13{I3~? 2950 94.7 ~k590 105 Average Concentration {ngrmL) ± %oRPD 1090 nglm~ # 0.92°!0 2d9d Itg/mL ± 2.$ °Jo

13~. -P~~l~ 13~'{-PFOS

3M LIMS ld descri tiara %Recave %aRecove ISfJ13-D7-03-OD1 DAB-GW- AC1-0- 13D327 1{HT 101 IS013- 0 ?-03-0D2 DAL-GW-

ACI -0B- 13fl327 104 1~D2 IS013-0?-03-0D3 DAL-GW-ACI- FMS130327 96.8 1D3 Average Concerrtration jngrmL) ± °iflRSD 1 ~ °~ ± 3.7°6 1Q2°/4 ± 0.93 °,~
NA =Nat Applicable ~1 j Samples were analyzed by +ex#emal standard calibration. The surrogate recovery starxiards i3C~-PFOA and 1304-PFCtS were add~;ci to Use samples during sample preparation.

PAGE 93 C3F 2'I

## sn~Fn~vr~zar~nsENra~ casa~ro~zv REPQRT IVO. lS093- Q7 -~T3



### Table 19. DAL G~t►l

ACM213U327

PFOA ~1~ PFBS tip
Ct>ncer~tration Concentration 3M ~I~+IS ID description {nglmL) °kRecovery (nglmL) °loRec~ very lSC193-07-03-t1~4 DAL-GW- ACM2-0- 13D327 52.9 !'dR 23p0 NA IS013-0~-03-405 DAL-GW- ACM2 -0B- 13D327 5Q:9 t+iAA 2330 NA tSt713-07-+D3-tHl6 DAB- GVJ -A~M2- FMS

- 130327 61.9 NC 2320 d~dC Average Cancer~trat9on (n~tmt)± °I~RPD 51.9 ng/m~ ± 3.9%0 2320 nglmL ± °1.8%
~FHS cif PF{fS ~ Concentration Concxntratian 3M AIMS Id Descri firm n L %Recave n mL °loRec:ove IS013-0 ?-03~ -004 DAL-GUII-ACM2 -{?-130327 17D NA 0.0509 NA ISO93-0 ?-03-fl05 DAL- t~W-

ACM2 -0B- 130327 1~1 NA 0.0526 NA tSlJ13-fl?-03-006 ClAL-GW-ACM2- FMS- 13D327 176 t~lC 1D.1 100 A~erageCcrnceon {nglmL) ± ° /aRPD 371 nglrnL ±0.58°Iti 0.0518ng1roL ±3.3 °,~

isC~d'F~'?A ~~y ~3G4-PFflS ~
mil LIMS id Description %Recovery %Recflvery IS013-07 -03-{}04 DAL-GW-ACM2-0- 130327 1{l3 94.1 IS01~ -07-03-005 DAL- GW- ACM2 -0B- 130327 103 98.5 iS013-[17 -03-{IQC~ DAL-GW-ACM2- Fh~.S- 13D327 1D3 9d.7 Aver e Concentration n mL # %F2SD 303°!0 ± 4.4°~ 95.8 ° /a ± 2.5°l0
PL4 =blot AQplicabte NC = Nc>t Calculated; Spike Bevel was less #han 0.5x the endogenous sample cor ntration. (1) Simples wee analyzed by e~ckemai staruiard calib~atic~n_ The surrogate recovery standards 13C~ -PFOA and t3C4-PFOS were .added to the samples ding sample preparation. {2} Samples wexe analyzed by irk l s#andard calibration.

PACE 14 t3F 213A9 EtVVlRC31'UhAFNTAL L,4BORAT~RY R,EPURT 1V0. /5033-t37 -03



### Table 12. DAL GW ASE 930327 {'~

~'FOA PFBS Cflncentr~tion C+~centration ~iN LIMS iD Descri tion n mL °loRecove n L %Reeve IS013- 0 ?-03-~D7 DRL-GW-

ACE-0- 13t1327 0.0362 t~dA <0.025(1 MA ISd93-07-03-008 DAL -GVv-ACE-L7B- 130327 0.038 tdA <0.025Q NA IS013-fl7-03- C}t~~J DAL -GW- ACE-FNlS- 130327 10.2 96:4 9.85 g8.g Average Concsr~tration {nglmL) # °IaRPD O.Q880 nglmL # 9.5°~6 <OA250 nglmL
PFHS PFOS Concentration Cancer~tration ~I L.IlVlS 1~ ~escnptiori ~ng7mL] 96Recovery ~nglmL) °IaReaovery ISC313-07-03--007 DAL -GW- ACE-U-13{1327 x.0433 NA <D.02~2 NA tSQ13-07-0~UD8 DAL -GW- ACE- [jB- 13D327 O.fl521 f~A ~.fl232 NA IS013-07-03-009 dAL- ~W-RCE-FMS

- 13{1327 9.31 93.9 10.4 104 Aver e Can~centraiion n mL # ° /aRPD O.Od7? L ± 98°10 ~O.d232 n mL

~3Ga-PFOA '~F05
3N( LIMS ID Description °loRecovery °laR~ecovery ISd13- D7 -03-D07 ISf313-D7 -03-008 IS013-07 -03-OD~ DAL-GW-AGE-0- 130327

DAL -GUV- ACE-DB- 130327 DAL -GiN ACE- F14~~- 13{3327 1fl2 1p5 164 112

110 '!07 Av+~rage Ccsncer~tration (ng/mLj± ° /aRSD 104

°l0 ± 1.5°l0 ~I V.'I I4 ~' Z.d~~U NA =Nat Appiic~ble {1) Samples uver~e analyzed by ir~tsmal s#andard calibraticjn.

PAGE 15 C3F 213IVf FtUVlRONA!lEIVTAL GA8C3RAT~t2Y REPORT fVO. !SC}33-t?7 -t13



### Table 13. DAL GW WW8R 930327 ~1~


## ~~aA ~FBs C~nc~ntration Ccmcerrtration 3M LIMS ID L~scription (ng/traL~ °Recovery (nglmL) °kReabvery ISt}13-0? -03-090 DA~~W-

WW8R-0- 130327 366Q NA 380 NA ISQ13-07-03-111 DAL-GW-WW8R-0&130327 362D NA 3$9 NA 15013-07-03-012 DAL-GW- VIAN8R -CMS- 130327 762 9d.3 41DD 93.4 Average Concentration {nglm~) ± °IflRPD 3Sd0 n~'mL ±^i.i °~ .385 ng1mL ±23°k
PFHS PFOS Concentration Concentr~lion 3M LIMS ID Descri tia~ n L %FtecQVe n mL %Reaove lS1~13-0~-03-010 DAB- ~W- WW8R- t}- 13fl32? 1760 NR 5170 NA IS013-0? -03-011 D,AL

-GW WW8R -13B- 130327 176D h!R X070 NA !8013-07 -03-t312 DAL-GW-WW8R-Ftv3S- 130327 x520 95.4 9679 114 AverageConcer~trati4n~nglmL ) ± °l4RPD 976flng~ImL ±O.U°fo 5320nghnL ±2.0°!Q

3NI LIMS Id Description °loRecovery %Recovery IS013-07 -03-D10 13AL

-GW WWSR-0- 13{132 96.0 1~D1 1S013-07 -03D11 DAL-GW-

V~+W8R -D &930327 94.8 107 ISO13-07-03012 DAL-GW- WUV8R -FNSS- 130327 93.4 9~i.0 Avers eConcenb~ation n rr~L ± °IoRSD 94.7°6 ±1.4°h 99.3 °l0 ±29°le
MA =tit Appiic.~ble (1 } Samples were anafiyzed by e3ctemal standard caiibrati~_ The surragatQ recovery standards 13C~-PFOA ~d 1~Ca-PF~S vu~;re added to the samples dt~ing sample ~eparafion.

PAGE 96 C3F 213lU9 ENVlR~NA9ENTAt tABORA7DRY REPORT IVO. ISU93-07 -03



### Table 14. DAL GW iNW9R 13U327 ~'~

PFOA PFBS C+ancentration Concentration 3~N ~.IMS I~ Descri tion n mL °foRecave n mL °.~R~ve IS013-07-03-013 Dl~- ~V+~- 1NU1t9R-0- 13fl327 326Q ~3A 273 NA IS~13-07-03-094 QAL-GW-VNN9R -0B- 130327 340D NA 2$3 NA ISC313-fl7-03-015 DAL-GW- W'W9R-FMS- 13U327 ?5?0 100 426fl 1DD Average Concentration {n~ImL)± °IoRPD 3330 ngtmL ±4.2 °k 278 ngtmL t 3.6°k

PFHS PF05 Concerltr~tion Cc>ncentratitsn ~+f LIMS ID Description (ngim~j ~oRecovery (ngtmLy °loRecovery (S013-D7 -03-013 DAB-GW-

WW9F2- 0- 13tD327 1410 NA X530 NA iSC113-07 -03-(i14 C?,A~

-GV1l W~N9R-l3B- 130327 1470 NA. 4780 N,q IStJ13-07 -03dJ15 DAL-GW-WW9R- FMS

- 13{3327 X70 102 90713 110 Aver e Goncer~tration n m~ ± °IbRPD 1440 r~ mL ± d.2% AS60 n L # 5.4°/a

'~C4-PFOA ~C#

-PFOS

3l~Il AIMS ID Description °loRecovery ~'loReoovery IS013-fl7-03-013 IS013-d7-03-014 ISO43-07-03-415 D;AL-GW- WW9R-0- 13fl327 DAL-GW- W~l9F2-DB- 93D32? L7AL -UWWW9R

-FMS- 130327 102 105 96.3 103

106 301 Average Conceon {ngfnaL)± °IoRSD 901"'!o ± d.5°fo 108°l0 ± 2.2°10
NA =1~1ot A~licabie (1) samples wee analyzed by eactemat standarr3 cali~etia~_ The surrogate recovery standards 13Ca -PFflA ~d 13C4-

-F"Ffl5 were added to the sarraples d~ru,~ sample ~ep~ ration.

PACE 17 t3~ 213A~ EtVVlRONMENTAL iA80RATORY REPORT MCI. lSC713-07 -~?3



## Table 1~. Trip Blank Results

PF4A t~FBS Concentration ~Cance~ation

~►+I AIMS ID Descri tic>r~ n mL °kRecove n L °.SRecove IS013-fl?-03-016 DAL- G1Al-TF~IPfl1-0 .D.0240 {~~ NA <0.0250 ~~~ NA tS013-07-03-017 DRS-GW-TRIPti1 -LS 102 {'~ ~.4 9.60 ~~} 96.4 IS013-07-03-018 C1f~-GW-Tf21P01 -HS 4360 ~ X03 4D7D ~ 102

PFHS PFOS Concentration Cartcentratian 3M LIM3 ID Description {nglmL) ° /gRecovery (ngfmL} °IoRe~overy IS013-~7-03-16 DAL- ~W-lRIP01-0 t~.fl?50 t~~ PtF, <0_~D232 ~9; h1A ISfJ1307-03-017 DAB- t~W- 1RIPtl1 -~S 9.14 {~~ 923 9.44 {~~ 94.4 ISfJ13-07 -03-fl18 DAL-GW-TF21P01 -1-IS 4020 ~ 102 AB60 ~ 116

13~-PFOA ~3~.q~~{~S

3M LIMS IQ Description ° /aRecovery °loFiecovery IS013-Q7-03-016 DAL-GW-li21P01-0 94.9 ~'j 98 5 {'~ (S013- 47 -03-D17 DAL- GW-TWPD1 -LS 91.0 ~1~ 9~.0 {~} IS413- ~7 -03-{}1$ t3AL-LiW-1F21P01 -l-IS 102 ~ 105 ~ tVA =Not ApEiiicable {1) Samples were analyzed by internal standard calibration. {2) Samples were analyzed by e~ctema( starxiard calibratic3n.

PAGE 98 t"~F 21

### 3M EAtYti:ONM~NTAL LAB{3f~ATORY R~J'OF?T AJ4. lS093-07-33



# 5 ConclUSic~n Laboratory control spikes were used to determine the analy#ical me #hid accuracy and precision for III analytes. The accuracy an~i precision were then used to estimate the method uncertainty forthe results. Field matrix spike recoveries demonstrated that the analytical methtjd was appropriate fir the given sarr~ple matrix. Ana#ysis was compfe#ed rasing 3M Envir~r~mental Laboratory Method ~TS-$- 044,1 "`Method c,f Analysis for the Determination ~f Perfluorinated Campc~ur~ds in Water by LCJMS /MS, ~ire~t Injection Analysis". Analytical results are reported in Fable ~ and 10-15 of this repack.



# ~ ~a~a 1 Sample R~e#enti~n
All remaining sampte ar~d associated project data {hardcc3py and electronic) will be archived ~ccordir~g t~ 3M Environm~nta# Laboratory standard operating procedures.

~ ~1~ C h ~T1 ~ ~t~S
Attachrr~ent A: Analyte Trend Data for select sampling poir►ts a# the dec~tur Ground Water Trsa#ment 3'lant {GwrP)

GAC system.

8 ~lf~t1c~~l.il'~S 

# /~~..
Susan T. Wo(f, ~M ' cipal Analytical Investigator Date

William K, Re~gen, Ph.C~,, 3M Envir~~ men#al L.aboratary Technics( Director Date

The 3M Environmental i.aboraton/'s C2uality Assurance Unit has ~udit~d the da#a and repvrk for this projec #.

0 Quality 2 ,5' 1 C1ate

This fes #report shalt not ~e reproduced excepf in ~u1/, wi #host wri#ten approval of the 3M Environmen#al Laboratory.

PAGE 99 C?F 2i\\ Weston\natacc\ FOLDERS.0 -9\3M- DECAT\Phase_3_Work_Plan\2Q13 Status Report\2Q13_Status_Report.doc 7/25/2013 

# APPENDIX B TO ATTACH MENT 1 WWTP EXTRACTION WELL S - APRIL 2013 ANALYTICAL DATA REPO RT ISO13 -07- 043M ENV1R0lU'M~NTAL LABORATORY REPt3RT NO. ISf)33

-07 04



# Analysis of PFC3A, PFBS, PFHS, and PFOS in Aqueous Samples from 3M Decatur, Alabama: +Groundwater Treatment Plan# GAC System

— Aprii 2013
laboratory Ret~uest Number: fSC~13 -07-04 Method Requirement: 3M Method ETS-8-044.'1 Report Date —Date of 1.aast Signature 

## Testing Laboratory

•~- • a - .s• • t s •1 ~' _• - sus •• /ii

R @CCU@St

@C 

# Gary Hohenstein 3M Building 224-~W-03 Saint Pau1,1t~N 55'144-1D00 Phone: X851 j 737

-3570

The testing neporked herein meet 1t~ requirenterN~ of AN5IJISOAEC 17025:2005 "Ge~►eral Requir~mer~ts for the Canpe~enae of Testing and {:alibration Labora~#ories ",in accordance with the A2LA Testing Certificate # 2052.Q1. _}

PAGE 1 ~213M ElUVlROIVIv9ENTAt LABORATORY l4EPt3RT lV~. IS{?93-0~ -04

..e • 

### 3M Environmental Laboratc~y Technics! Director. William K. Reagan, Ph.D. 3M Prinapal Analytical Investigator: Susan Wotf Report Author: Cherie Grochow

3M D+ecatur Groundwater Treatmen# Plant System;ApriC 2013 Sampling

Report Date: Date of Last Signa#ure

~ •' !
~'he 3M Environrnerrtal Laboratory analyzed wa #er samples from the groundwatier treatment plant GAC system at the 3M Decatur, AL facility. Water samples were collected by Wes#on ~otutions personnel on April 2J, 2013. Sara~pies were returned to the 3M Envirrmmerrtal Laboratory for analysis of Perfluorooctanoat~ {PF{3A), Perfluorobutane sulfanate {PFBS), Peri7uorohexane ~ulfiflnate (PFHS}, Perfluorooctane sutfonate (PFC3S }, and the surrogate recovery standards 13C~ -PF~A and'3C~-PFt~S under laboratory project number ISC)13-07-04. Analysis of the samples was comple#ed as specified under 3M Environmental Laboratory General Project t~u~ine {GPt))number GPOi'1 -1D06. The 3M Environmental Laboratory provided sampte containers for five sampling locations; ACI, AGM2, ACE, WW8R, and WV'~'9R. The sample set consisted of a field sampte, field sample duplicate and a field matrix spike. Each empty pan#ainer was ra~ariceci wgth a "III to tire" tine that corresponded to a final volume of 2(}tI mL. Containers nesaerved f~ field matrix spikes were fortified with an apprc~iate matrix spike solution caMaining all analytes prig to being sent to the field for sample collection. Sample battles for sampling locations ACM2 and ACE,along with the Trip Blank sample and low spike, were fortified w§th internal standards and surrogates prior to being sent to the field for sample c~iectic~n. Samp{es were prepared and analyzed by method ETS-8-044.1 Method of Analysis for ~e Datermina6 of Perr~uaina #ed Compounds in Water by LCIMSIMS; Direct Injec6an Analysis". Sel~+c# interns! standards were used to aid in the data quality ~jectives. Table 1 summarizes the sample results using the analytical method identified above. RII results for quality corms( samples prepared and analyzed with the samples wil( be reported and discussed elsewhere in this report.

~ The #esting reported heron meet the requirements of AN51/t5011EC 17025:2005 "Genera! ~ Require►nents for the Campetenoe of Testing and Cali3~ratian ~aborataies ", in acaxxdance Frith the A2La Testing Certificate # 2052.Q1. G9~ ~ ~I fc: ~~ f'P" t: f? 

## Testing Cart #2052.01

PACE 2C]F 213M EIVVlRt)NhAENTAL Lt#80RATORY REPORT NO_ lS093

-07 -04



### Table 1. Sample Results Summary

PFOA PF85 PFH3 PFOS Concentration Concentration GonceMration Concentration ~VI LIMS ID Sample Descriprion {n9~~) t~~ 4~~~1 {n9~~-) IS013-07-04-001 DAL-6VIf-ACI; Sampje 1454 1340 767 162D fSO13- 07-04-{l02 DAL-

GW-ACi- Sam 9e Du i~04 138fl 78+6 9720

Average 1480 i~3 1360 ~? 777 ~'3 96i0 ~'~ °JaRPD Sin elS~n le Uu 3.4 ~.9 2.d 6;D IS013- fl7-Q4-+Q~ DAL-GW-,ACM2; Sample 298 1530 fi83 X3.400 ISO13-07-04-{)05 DAL- GW-~ACtvl2- Sam le Du 293 1490 659 0.354

Avera~ 296 ~i'~ °1510 ~~~~ 671 t',~ x.377 ~3f %RPD San 1~5~n le Du 1.7 2.6 3.6 12 t8O13-07-04-DD? DAL- GW~10E, 5aro~~e fl_{1420 ~D.393 DA~51 <0.0232 ISQ13-07-D4-008 DAL-GW' -d4CE~ Serra 1e D 0.0424 0.391 0.058$ <p.fl232

Average 0.042 ~3 0.392 ~3~ 0.0574 ~} <0.0232 #~~ %RPD S~nplei5~rtple Dup 0.95 0..51 6.5 NA IS1~13-07 -04-010 L3A,L-GW-

WW812; Sample 3180 364 160~D 4844 ISO13-07-04-011 DAL-GW-WW8R~ Sam le [lu 3200 364 162 4820 Avera~ 3'190 t'3 36A {~~ 'f 610 ~i~ 483D ~'3 °f~2PD ~n~efS~nple Llup 4.63 O.d 1.2 0.41 IS013-07-04-013 [?AL-GW-WW9R; Sample 2600 240 118fl 426 IS013 -07-04-014 L1AL-GW-

WtiM9R~ Sem le Du 2690 247 121Q 4410

Average 266 {'~ 244 t~~ 9200 ~~~ d340 {~} %12PD S~nplel'S~nple Dup 3.4 2.9 2.6 3.5
NA =Not Applicahte {1) Reputed resulL~s uvere prepared ~d analyzed by ETS-~8 -044.1 using external standard c~itxaUi~. The ar►alyhica! method ~ac:ertainties associated with the resorted results are as fol~uvs= PFOA +_15' 0, PFBS ± 14 %, PFtiS ±14

°Jo, ~d PFOS ± 149"0. (~} Sample did rat have an appropriate CMS to amass recovery_ See section 4fa more details. {3} Reported results were pr~epar~d ~►d analyzed by EfS,B

-044.1 using intt~nal stand~d calibration. Tie ar~ykical metF~d ~aertainties associated with the r~orkeci results are as ft~iows: PFOA ± 159'0, PFBS ± 95 °!0, PFHS ± 949'0, ~d PF05 ± ~39'n_



## 2.1 MQthods Analysis was comple

#ed using 3M Environrnec~tal Laboratory Method E~"5-8 -044.1 "Ntethod of Analysis for the Determina#ion of Perfluorinated Compounds in V4'ater by LCIMSJMS; Direct Injection Analysis ". Table 2 Target Analytes

Ta et ~ s Acron Reterence Material Structure Perfluorooctar~oic Acid C8 Aad PFOA Lir~ar +Branched PerfluoroYxrtar~sutfc~ate (G~ Sulfbe } PFBS Une~ Perfluorohe esulfcu~te Cfi Sulforrate PFFtS Line Per~uoroc~ctanesuffc~ate (C8 Su~f~ate) PFOS Unear+ Branct~d

PACE 3OF 213~M,EN'VlRONME/UTA~L LABORATC7RY R,EPQ/?TN'O. !SO)3-t17 -D4



# 2.2 Sample Collection Samples wrere c:ollectte+d on April 29, 20'13 in Nalgene~f ( high

-density polyethylene)bottt~s prepared at the 3M Environmer~tat Laboratory. Prior to sample collection, bones designated for field matrix spikes waste spiked in the lab~-atory with a known vaume of an appropriate ma#rix spiking solution con#aining PFC}A, PFBS,PFHS,and PFflS_ Sample bottles for sampling locations AClvt2 and ACE,along with the Trip Blank sample and law spike, were fortified with a mixture ofmass- labeled internal standards at a nominal canc~ntcation of 7 ng/mL and a mi~cture of surrogate revery standards at a nominal concentration of ~.1 nglm~. Gol4ected sample bottles were received by the laboratory at ambient conditions an May 3, 21333. 

## 2.3 Sample Preparation Sample sits ACt, ACM2, WWBR, WW9R, and the Trip Blank high spike were diluted 1:100 and ar~aly~ze~! fot- all analytes. The 1 100 dif~rtions were prepared by removing a 0.1 m~ aliquot of the w,~ell mixed sample and adding 9.8 mL of me#hanol and ~.1 mL of a surrogate spiking solution. Prepared samples were analyzed by external standard calibration. The ACE and ACM2 sample sets and the Trip Slank sample and tow spike were prepared and analyzed for al€ analytes by #ransferring an aliquot of the well mixed sample into an autovial. Prepared samples were analyzed by internal standard calibration. During the preparation of the laboratory c~trol samples far internal si~ndard calibration, an aliquot of a separate irttemal standard spiking solution was added to the laboratory ~on6-ol samples {nominal concentration of 1 nglmL}. The sample bottles for ACE,ACM2,and Trip Blank were spiked wi#h an intema! standard mac at a nominal oonoentration of 9 nglmL prior to being sent to the ~re1~1 for sample collection. The la tort' control samples were analyzed in the same manner as the samples. 2.4 A111E~ISES All sarnp9es and quality+ control samples were analyzed for #ter target analytes using high performance liquid chromatc>graphyltandem mass spectrometry {HPLCJM~/MS). Pertinent instrument parameters, the liquid chromatography gradient program, and the speaf►c mass transi~ons analyzed are described in the tables below.
Due to the nature of the sample,the wide range of concentrations found in the sample, and the environmental occumenae cif multiple isomers of the laborats~ry's analy#es of interest, the software used for processing the analytical results is not able fo consisterrtly integrate the analy6Yca} peak, manual integration of the analytical peak is necessary. All manual irrt~grations are performed following the procedures outlined in method Ei'S- 12 -01D_ The cx~nsistency of the laboratory's integration is ensured through the training of laboratory persor►nel, the peer review process required for all manual integrations, the review of manual integrations by the QAU,and where necessary the review of manual integrations by laboratory management.

PA~E4~213M EN1liRflNMENT}►L LABORATORY ~?EPORT Nt?. IS013

-0? -04



## Table ~, Instrument Parameters.
lnstrumerrt Name ETS tGric ETS Buster Analysis Dates 517113 -e~d~nai starxiard calibra6ora 518113- ir~temal star~darad c~i6~aaccxi 14na1 'cal Method ETS -~E3-044.9 ETS-8-044.1 Liquid ~Chra~r►atograpd~ Agft+ec~t 128 Agiient 1'1DCI Guard colinnn Betasi! C18(d_£ rr~ry X 10D rr~n), 5 Blasi! C18 {4.6 rrr~n X i{~ warn), ~ Analy+ticat column Betasit C18 {4.6 rr~n X 1{30 rr }, 5 Betasil C18 {4.6 rr~n X 9~0 rr~nn}, 5 Injection Vol~ne 2 5 cx 2D 25 Mass S meter lied Bias ems Tri let.~uad 550D lied Rios ems ~4F'I 4000 Ion Source Ttxbo S Tt~o S Pula ' alive alive S+attware ,An t 1.6.1 Maaly~st 1.6.1 

### Table 4. Liquid Chrorr~atography Gra~iieni Prt~gram.
Step 

### Number Totsl Tme



### mrn Flow Rafe



### ( 'n) P to



### mM ammo~rrn» saetate Percent$ 

### Metha D 0_tlD 75D ~t3_D 10.0 1 0.50 750 9Q.0 10.0 2 4.00 750 7fl.0 3D_0 3 6.00 75D 7D.D 3d.~ 4 11.0 750 20.0 80.0 5 13.0 75D 20.D gp_p 6 13.5 75D 1fl.0 90.0 7 16.0 750 10.0 9d_0 8 16.5 750 9d_D 1D_0 9 19.0 760 9d.i~ 10.0 

## Table 5. Mass Transitions

~~~ Mass Transition Cl1 /Q3 Ir~temal Standar8 ~~ ~~ Transitia~ Q1/Q8

PFOP~ 4131369 [~~]PFt~ 421J376 4131219 413/1{19 PFSS 23J18d ~y~FBS 3031&t 299199 

## ~~s sssrss I~~IPFHS 402199 3991'80

PFOS 489199 ['~aIPFOS 5D7J8fl 499180 499/13fl [~~jPFOA surragate 4171372 ['3C8]PFC7A 4211376 ,3C.~ PFOS su aie 503/8D 13C~ PFQS 507f80 CAvel( time was 50 msec fcx each transition. The individual trar~sirti~►s wire summed #a proclucE a "`total ion chromatogram° {T!C), which was used for c~anti~a6ora. 1 Internal standards were used for #~e argil ~s on 518113_3M E1V1/iRONh~IE/UTAL tABt~RRTt3RY REPORT NO. iSt?93-t3? -U4



# 3.'1 ~Calibratio~ Intema! Standard Calibration .Analysis: Samples were analyzed against amatrix- matched sfiable isotope interr►al

standard calibration curve. Calibration standards were prepared by spiking known amounts of stock soluti~s into 50 mL of laboratory+ prepared reagent water. The calibra~on standards c~tained an internal standard mac at a nominal c~oncentra~ ion of 1 ng/mL. A total of thirteen calibratic~ standards ranging from 0.025 nglmL fio 25 nglrr~L {nominal)were analysed with the prepared samples. C7F these thirteen calibration standards, eleven contained ~e surrogates at concentrations ranging from 0.02 ngJmL to 1 t} nglra~L n~aminal_ A quadratic,1 /x weighted, calibration cx~nre of the ratio of ~e standard peak area counis ~v+er the internal standard peak area counis was used to fit the data for ead~ anat~~te. The data were not forced thr~gh zero during the fitting process.. Calculating the standard c~c~er~trati~ns using the peak area ratios and the resultant calibration cx~~rve confirmed accuracy of ead~ curve parrt. The reference si~ndards of P~OA anal PFt3S used to prepare the calibrati standards consisted of bot~~ linear and branched isomers. Each curve point was quantitated ~~ing the overall calibration curve and reviewed for at:curacy. ~riethod calibration accuracy requirements of 100±25°!0 {1 0±30% for tt~e lowest curve {mint)were r~et far ail analytes. The ca~re~ation cc~efficien# {r} was greater than 0.995 far all anatytes. External Standard Calibration Analysis: Samples were analyzed against an external standard calibrati~ curve. Calibrataon standards were prepared by spiking known amounts of the stock solution c~orttaining the target analytes into ~:1Q methanol. Milli-Q laboratory water. A to#al of ten spiked standards ranging frarn {3.02 nglmL to 25 ng/m~ (nominal) were analyzed. The tern standards also eontain+ed the surrogates at concentrations ranging from t}.02 nglra~L to 25 nglmL nominal. A quadratic, 1Ix weighted, calibration curve of the standard peak area counts was used to fit the data for each art~yte. The data were not forced ~rflugh zero during the filing process. Calculating the standard concentrations using the peak area counts and the resutfiarat calibration curve confirmed accuracy of each curve mint. Ead~ curve point was quantitated using the overall calibration rx~rve and reviewed for accuracy. Method ~albratian acr~racy requirements of 140±25% {100±30°lo for the lowest curve poirrt) were met for all analytes. The con-elatian coef~icier~t (r)was greater than 0.99 #ar a8 analytes. 3.2 S~S~~t11 SU11~b111'~j/ A calibration standard was analyzed #'our times a# the beginning of the analytical sequence to demonstrate overall system suitability. The ~cceptanae criteria for system suitability samples is less than or equal to 5% reta~ve standard deviation (RSD) for peak area/ra~tio and retention time criteria of less than or equal tc~ 2% RSD. These criteria were met for al! analykes. 

# 3.3 Limit of Quantitation (LC3Q) ~'he Lt>Q as defined in meths ETS-B -044.1 is ~e lowest non-zero calibr~tic~ standard in the curve that meets linearity and accuracy requiremerr#s and for wfiich the area a~rrts are at least iwic~ those of the appropriate blanks. The LOQs assoaated with the sample analysis ar+e listed in Table 6_

PACE 6 C3F 213JI+t ENVif20NMEJUTAL CABaRATdRY REPORT NO. 1S013

-0~ -04

.•' t ♦e, Anaiyte Calitxation ~~, n~'inL PFOA lrrtemal star~ciard 0.0240 PFBS ~rdema( standard t1.~250 PFHS ~t~Yemal standard 0.025t} PF~S drrtema[ star~ard x.0232 PFOA E~demal stdard {}.0192 t'~ ~'FB~ E~derr~al sfdarr~ +D.{3200 ~ "~ PFHS Exkemal st~dard fl_{12~70 tag PFOS External shard fl.{?185 c+s (1) The dilu6cm fad was nab applied to tt~ LQCt. 

# 3.4 Continuing Calibration During the curse of the analytical sequence, several continuing calibration verifification samples {CCVs) were analyzed to car~firm that the instrument response and the fini al calibration curve vr~re still in control. ~'he method acceptance aiteria flf 9~°l0 ± 2~% vra~ m+~t for a!1 analytes. 

## 3.5 Blanks Two tykes of blanks were prepared and analyzed with the samples: rne~ad blanks/solvent blanks and fiefd/trip banks. Each blank resuPt was r+eview~ed and used to evaluate method ~erFormance to determine the LC~Q far each analyte. 

## 3.6 Lab Control Spikes {LCSs) ~.ow, mid, and high lab control spikes were prepared for the target analytes and analyzed in triplicate, while only low and high lab contra! spikes were prepared for the surrogates. LC~s were prepared by s~king known amourrts flf the analykes iota eith~-10 mL of laboratory-prepared matrix matched water or 1 mL of Mi11i-Q water to produce the desired ~ncenfration. When applicable, the LCSs were then diluted with me#han~ in the same manner as the camp{es. Meth! EfS-8-044.1 states that the average raeecovery of LCSs at each spiking level be v~ithin 80 %- 120°lo with a RSC} <_2U%. All LCS samples met method accuracy criteria. All L{;Ss were used in the determination o'f the analytical method uncertainty in section 3.9. ~'he following calculatic~ts were used to generate data in Table ~. Calculated {;oncentration ACS Percent Recovery = * 140 6 Spike ~oncentrati~

LCS °/a RSD _ standard devi~lic~► LCS replicates ~ 10096 average LCS rrecovery

PACE 7 t}~ 213M ~N1/lRONMEJUTAt LABORATORY REPORT NO. 1SC193

-07-04



### Table 7. Lab Contra) Spike Results.


## ors-~ -o~4.~ E~defr,ai Staru~ard Calibration Analyzed5r7J33 PFOA(Ling +Branched) PFOS Linear +~~nched) Spiked Calcx~lat~ Spiked Calculated Con~r~ation Concerrtration Cancentra#ion Concentration Lab 1D inglmLl (nglm~} °1oRecuverY {n9lmL) (n9~`mL) °kReaovery LCS-"~30~7

-1 {1.191 0.172 89.9 {~_'~85 0.196 103 ACS

- X30507-2 x.191 0.1$3 95.8 D.385 0.192 id4 LCS-'13D5Q7

-3 0.191 0.7t3fi 97.4 fl.185 0.191 1D7 Rvera~ t °IQRSD 94.3°,6 ± ~.2% 1d5 °10 ± 2d°k LCS-X30507

-4 1.99 1.96 963 1.85 2.09 113 LCS-330507-~ 1.99 1.93 901 1.85 2.07 112 LCS- 7305t}

?-6 1.91 1.96 9~~ 1.85 2D~ 111 Ave~d~ ~ %RSD 102% ± 0.98 °1a 112% ± 0.89% LCS-'33115D7

-7 19.1 18.7 97.8 18.5 X0.1 '109 LCS- 93D5~~-8 19.9 172 9D.3 1$_~ 19.5 105 LCS-13d5D]

-9 19.1 18.4 96.2 18.5 20.2 109 AVera~~ °JoRSD 94.8% ±4.2°!0 108°M' #21 °l0
E7~-8-04d_1 External Starxiard Calibration Matyzed 5(7/43 PFBS PFH~ spiked Caitxidated spiked Calt~latsd Concentration Conrer~h~atia► GoncentraEion Cancentration Lab ID {nglmL} (ng~mL} °JoRecovery (ng/m~) (nghnL.) °loRec:overy+ LCS-'130517 -T D.199 0.27 '~04 0.199 0.198 99.7 LCS-130~D7-~ x.199 0.293 107 ~Q.199 0.203 102 LAS-134507-3 0.199 0.297 1~9 0.199 0214 107 Average t aIaRSD 7V~~Id ± LsY~ID 103% ± 3.6 °fa LCS-"i30507

-1! 1.99 2.36 119 1.99 2.2D 111 LCS-330 7

-5 t99 2.32 1'16 1.99 x.16 108 LCS-130507

-6 1.99 2.31 "~ 16 1.99 2.19 110 Avera~f %RSD 117°Jo # 7.5 °h 11U'Ya± 7.4 °ta ACS- 9305D

?-7 20.x6 20.9 945 20.D 19.6 ~2 LCS-130507

-8 2Q.~ 19.9 X9.4 20.0 18.9 94.6 lCS- '!30507

-9 2D_0 21.2 '106 20.0 19.4 97.Q AVBI~~ f °~aRSD 108°l0 ± 3.d% 96.6% ~!' 1.9°fn

PRE 8 CjF 213M EN'ViRONlIA1ENTAL tABORATCJRY REPORT IUO. 15093

-t~7 -04



### Table 7 continued. Lab Con #rol Spike Results.

ETS-8-Od4.1 Extema! Starx#ard Caiibratior: t~ ed 517/13 PFOA su ate PFOS su at+e Spiked Gatculaked Spiked Caltx~tate~i Cancerrhation Concentrati+or► Concentration G~oncentration Lab Id n mL L °JoRecave n L L °loRecov+e LCS- 93(17

-1 0.199 0.186 93.2 {~_99D 0207 109 LGS- 93D5Q7

-2 0.199 x_185 92.7 +D.'~90 D_2~ 1D8 ACS- 930507

-3 0.199 0.191 X5.9 ~.99D 0.2fl9 110 AVeta~ :t °foRSD 93.9°l0 ± 1.8°!0 109°!0 ± 0.92°10 LCS- 330507.4 1.99 1.9D 95.4 1.9~ x.05 108 LCS-"#30x07

-5 9.99 1.95 97.8 1.90 2A8 109 L~CS-3305D7~ 1.93 1.~ 99.5 1.90 2.1D 110 A1tei'a t °l4RSD 9i.6 °la ± 2.2°!0 109°l0 # 0.92°!0

ETS-~-D44.1 ~nt~nai St~xiarzi ~B~Uff3$O(i Anal ed5t8/~3 PFOA(l:inear +Branched) PFOSp..irtear +granched) Spiked Caicx~fated Spiked Galcx~lated Concentration ~oncer►tration C~ncentrration Concentration 

### Lab 10 (ngtmL) tng/m~)
4~oRecave►Y 

### tngtm~) tng~m~) °,Recovery LCS- 9305Q8

-1 0.190 D.193 X01 t}.984 0.184 tJ+3.8 LCS-'#30548-2 0.990 0.1~ +34.6 0.184 D_178 96.9 LCS-'130508

-3 0.19 x_189 99.4 ~3.98A ~D_178 97.0. Avery t °loRSD 98.8% ± 8:d°lo 97.9°!0 ± 13 °le LCS-'130508-4 1.94 2.t}5 90$ 1.84 2A1 109 LCS- 73D5D8

-b 1.9D 2.02 ~~ 1.84 1.92 101 LCS- 33051)8-a6 1.90 2.05 108 1.84 1.97 1D7 Avera~ t%flRSD 107 °k ± 1.9 °JO 1 V( ~ ± Z4~~D LCS- 930508-7 9.52 9.01 94.6 9.21 9.65 1D5 LCS- 93D508

-8 9.52 8.80 92.4 921 9.15 99.4 LCS-'~3t1508-9 9_~2 8.93 93.8 9.21 8.6C} 93.3 Avery t~IoRSD 93.6 °!0 ± 3.2% J9.2°10 ± 5.9°to

PAGE 9~ 213A9 ENV(RONAAEAITAL LABORATORY REPC3RT NO. 1SU93

-07 -~4

.• - • -a ~ a r r ~.


### ETS-8-04~1.~1 lrii~nal S`t~darri Calibration ed ~J8(13 PFBS PFHS

Spiked Calculated Spiked Calculated Cancerr on C~nccrrtration Concentration Concentration Lab ID n mL n L °kRecove n L L °loi2ecove LCS-X30508-1 0.198 ~~ 0.197 99.5 x.198 02' 1 106 LCS- 'I3t1508-2 0.'198 ~ 0.197 99.7 0.~~ D_195 98.4 LAS- 930508-3 0.19$ 0.196 99.0 0.95$ 0.2 9 '106 Average #%RSD 99.d%± 0.36°Jo 103°k ± d.2 °lo LCS- 1305Q8~1 L98 2.27 915 1.98 2.22 '112 LCS- ~3D5fl8-5 1.9& ~.1~ 311 1.98 2.16 1~9 LCS- '30508 -6 1.98 2.09 105 1.98 2.14 108 Aue $°l4RSD 110°la # 4.6°h 110°lO ± 1.9°!n ACS- 93D508-7 9.94 9.48 9~.3 9.94 9.96 10Q LGS- '13D508-8 9.94 9.37 94.2 9.94 9.48 95.4 LCS- 13D~8-9 9.94 9.62 96.8 9.94 9.68 37.4 AveTa~ ~ ~IOR~ .TJ~~I6 ± ~ ~~IO $7.6°/a # 2.s!°lo

ETS- 8-044.'1 ~ntemal Stt~dard Catibr~tion Analyzed 518113 PFt)A surrogate PF{3S surragabe Spiked Calculabad Spiked Calculated Conc:er~trafiion Concentrati~ Concentration Concentration ~.ab ID n mL n L °kRecc~o~ve n L L °JoReoov LCS- 13D5Q8-1 Q.1S8 D297 3~9 O.i89 (3.198 1D5 LCS- 1305t~8-2 0.198 D_217 110 x.189 0.207 1D9 LCS- 9305D8-3 D.198 0218 'd10 x.159 0.223 118 AVetage #°1nR5D 11Q°1a ± 0.53°l0 111$/0 # 6.0°l0 LCS- 1~5D8~t 1.98 2.13 907 1.89 2.D4 108 LCS- 'l305D8-5 1.98 2.13 ){}8 1.89 2.06 1d9 LCS- 9305Q8-6 1.98 2.1? 110 1.89 2.21 117 Avers ~ °IoRSD 1~8°k ±1.4% 111 % ±d.4 °!4

PACE 70 t}~ 213ltA~IVVIRQNMElVTAL LABt~RATORY REPt3RT NO. 1S~fJ13

-07 -04



# 3.7 Analy#icat Methad Uncertainty Analytical unaer#ainty is based on histao~-iECal QC data tha# is control charted and used to evaluate method accuracy and preasion. The method uncertainty is calculated following ETS-12- D12.2. The standard deviation is calcula #e~ for ~e set cif accuracy results {in %) stained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor cif 2,which con-esponds to a confidence level of 95°fo. Table 8. Analytical Method Uncertainty.
Analyte Cal ration Method Standard Deviation Method Uncertair►ty PFOR E~emal Standard 7.56 +15~1a PFBS E~d~nal Starx~rd 6.$6 ±14%a PFHS External Standard 6.92 ±14 °Ja PFOS E~erttal Standard 7.21 ±14 °Jo PF{~A ~~t#ertt~9 Sfiandartl 7.51 ±15°la PFBS ~~emal Stand~d 7.53 ±13 °l0 PFNS 1tlternat Standard &.91 ±14% PFfJS ~t7temal St~nd~d 6.51 ±13°!0 NA= No# Applicable 

## 3.8 Field Matrix Spikes (FMS) Afield matrix spike was collected at each sampling poirrt #o verify that the snafyticat method is applicable to the collected matri~c. Field matrix spikes are genera #ed by adding a measured volume of field sample to a container spiked by the laboratory with the target analytes prior to shipping simple containers for sample callectiQn. Feld matri~c spike recoveries within method acxeptanoe criteria of 10~±3t7°fo confirm that "unknown" components in the sample matrix ~i+a not significanNy interfere with the ex'~~aetion and analysis of ~e analytes of interest. The standards used for ~e preparation of the field rrtatrix spiking solutions stained r~f~rence materials txsmprised of both linear and branched isomers #or PF~A and PFOS. Field matrix spikes are presented in sec~on 4 cif this re~rt.

FMS Recovery = Sample Concentraticxr of FMS— Average Concentratit►n :Feld Sample &Field Sample Dup_~ ~ ~~~~,Q Spike Concerstraton 

### Table 9. Field Matrix Spike Concentrations

Find Goncer~tratia► {rtglmL) Location Descriptiae PFOA PFB s PF1~lS PFOS ACI Field Matrix S{~ike 2000 20 ~ 0 2~Ot? 19~Q AGM2 Field Niahix Sake 1{}D 100 99.8 99.4 ACE Fes!Matrix Spike 10A 10.0 9.99 14.0 W1N8R,WW9R F~e4d Matrix Sake ~ 4DOd 402D 3990 3980
Trip Blar~t Lc~w Faek! Matri~t Spike 10.0 iD.O 9.99 10_D Huh Field ft~katrix Spike 40~D A020 3990 3980

PAGE 91 t~213M EIVUlf2f~NMENTAt LABTJRAT012Y REPORT NO. 15013-{37 -04



# 4 Data Summary and Discussion
~"he tables belflw summarize the sample results and field matrix spike recoveries for th~ five la~tions as well as the Trip Blank. Each table provides the average c~ncen#ration and the relative percent difference {°IoRPD} of th+e sample and sample duplicate. Results and average values are r~nded to three signficarrt figures. Percent relative differenc7e {°IoRPD)values are r~aunded to two signfican# figures. Because of rounding, values may vary slightly from those I'ssted in the raw data. Feld rnatri~c sakes meeting the method at:~eptance aiteria of ±30°l0, demonstrate that the rrrethod is appropriate for the given matrix. All Feld matrix spike samples and surrogate reoavery standards met mettaa! acceptance criteria except where noted below.

DAL

-GIN-ACM2; the FMS sample (1 t? ng/mL)was not app~-~opriate far P~OA, PFBS, PFHS, or PFOS; however, the surrogate recovery standards 13C4-PFOR and ~~Cd-P~O~, met method ac~epfiance criteria. No additional QG sam~ies were prepared.

PACE 92 C~ 213NlEN1tlRONibfENTAt tABOR~ITdRY REPORT Nf3. 1St773

-07 -D4



### Table '10. DAL GW ACI 130429 ~~~ 

## ~Faa PFBS ConcerYtraSon Ca~cerrtration 3M LIMS 1~ C3escriptian (ng/mL) %Recovery {nglmL) °~R~overy IS013-07-D4~}01 DAL-GWy4~Ci-Q-130429 1450 P3A 1340 Nf~ 18093-07-04

-i1t12 DAL~IN

ACI- [~B-13D429 150D NA 1380 NA ISQ13- 07-04 -t~D3 ~A~-GW

ACI-FMS

-330429 3270 89.8 3430 1D3 Average Cflnaery6~tion {nglrnL)± °I~RPD 1480 nglm~ ± 3.d°k 1360 ng/mL± 2.95'0

PFHS PFOS

Concer►tratiUn Concentration 3(VI LIMS ID Description (nglmL) °~Reoaaery (nglmL) °loRec~overy ISt~13-07-09-t~1 DAL -GW AC(-4- 93D429 767 N+A 162Q NA 1~1~13 -07-DA-{102 E}A~-GW- ACI-0B-13d429 786 N{t 1720 NA IS013-07 -04-003 DAL~W

ACI- FMS

- 930429 2fi5D 93.7 3770 106 Average Conc~rrtration {ng/mLj± °~RPD 777 ngtmL ±24 °/a 1670 ngfmL# 6.0°!0
13C~-PFOA 73C~-PFOS

~1 LIMS ID Descri lion °l~Reco " /,oRet~ve 1SCl13-07-04-001 DAL-U'VV- ACI-0-134429 89.7 1D5 IS013- 07-04-OD2 DAL~W

-A~1-D &13429 8$.8 110 tSO13- 07-tlA-flD3 DAL-GVY -ACI-FMS

- 130429 87.6 104 ~4verageConcentr~ation {ng+mL) ± %RSD 88.7°10 ±1.2°k 106 % ±8.1 °l0 !+lFlA = tVot Applicable {1) Samptes were anaty2ed by ~xterr~l skandard calit~a6c~. The surrogate recovery sfarxiardst3C =rPFOA ~d'~

-PFQS were added to the sam~~s d[~r~ sample preparation.

PAGE 93 C}F 21

## ~rt~r ~n~v~~on~~r~nrr~►c. ca~o~ roRY REPDRT Nfl. !St?93-07 -~4



### Table 17. DAL GW ACM2 930429

PFOA {" PUBS ~~f Concen#ratian Canoenh~tian 3M uMS ID Description {ngtmL) %Recovery fnglmL) °,bRecovery ISt}'13- {D7-04-DQ4 DAL~W'- ACM2-0- 13D429 298 NA 1x30 NA ISO13- fl ?-09-005 DAL-GW-

ACM2- dB-13D429 293 NA 14~J0 NA !St}13-07-04{3D6 DAL-GW ACM2-F~t1S-930429 394 MC 163 tVC 

### Average Ca~cerrtration {ngtmL~ ± °IaRPD X96 ngtmL ± 1.T° /a 1310 nghn~± 2.6%

PFHS t~} PF{)S'~ Concerrt~~atian Concen~tratian ~VI LIlt9S ID [3escri i~ n L °r6R+e~ve n °loRecove [SO13- 0~-0A -Q(}4 DAL-GW-

ACM2 -~-130429 fi83 NA 440D NA lS093-0~-09-Q0~ DRL-GW ACM2- dB-130429 6~9 t~lA 4.354 NA IS1~13-07-04-006 DAL-GW-ACM3-F~+/15-130429 792 t~ N,q ~) NA ~) ,Average C~ceon {nglmL) ± °l~RP`D 6?~! nglmL ± 3.6 °10 4.377 ngdmL ± 92 °~

y~ -PFflA t~~ "C4

-PFOS ~
3Nl LIMS ID DESCripti4tt °I~ReCOVery °IaReCOVery IS013-07-D-0-fl09 dAL-GW- f1CM2 -0-134429 95.5 'ID3 ISCt13- 07 -04flD5 DAL-GW-

ACM2 -ClB-134429 X9.4 93.0 fSt)13- fl7-04-Ot16 DAL-GW -ACM2-FMS

-130429 93.9 tVA ~ Ave e Corta~Mration n mL ± °1oRPDJRSD 93.6°fo ± 22~a 98.1 °!o ± i0%
NA =Nat Ap~dicaf~ NC =IVY C~Iculated; Spike Level was less than 0.5x khe endogenot~ sample cor~;entration. {1) Sarc~ples were analy2ed by extemel staruiard cali~ation_ The surrogate recovery staru~ards 13C~s -PFOA ~d'~C4

-PFOS were ceded to the sam~es d~ir~g simple preparation. {2) Samples wire analyzed by internal sta►x3ard calbra6on. {3) Sampk~ was r~o# analyzed usir~ irrtemat calibrati~ due to tF~ high FMS c~ncerrtratic3n.

PAGE 14 {~ 213M EN'VIRONfv1EIVTAt tA80RATORY REPt?RT NO. lS093-07 -Q4



### Table 12. DAB. GW ACE l30~29 {'~

PFOA PFBS Concerrtr~tion Concentration 3M LIN9S ID Descri '~ n mL °kRe~ve n L °laRecave tS413 -07 -04-007 DAL

-G1N`- ACE-t}-13U429 U.D42~ NA 4.393 NR ISCl'13-07 -D4-008 DAL

-GW- ASE- ~&13D42~ O.ikt24 ►JA 0.39'1 NA IS013-07-

04-{}~9 DAL-GW

ACE-FA~t5-

13D429 7.94 79.0 9.61 922 AverageConcentraiian {ngimL) ± ° /nRPD O.d422n~ImL ±fl_95 °lo Q.392ngtmL ±Q.51 °1~

PFHS PFOS Concer~tratia~ Ccxicerrtratior~ 3tV1 LIMS ID Description (ngtmL) °,6Reravery {ngtm~) °1oR+~overy ISC113-07-04-I~7 dAL-GW- ACE-0

-13429 Q.{}551 tJia <0.4~32 NA IS013 -07-04008 DAL

-GW- ACE-DB- 130429 {?_0588 NA x.0232 NA IS013 -07-04-009 DAL

-GW- ACE

-FMS

-130429 8.26 82.1 9.63 96.3 Aver e C~tcerttration n mL ± °IoRPD 0.0570 L # 6.5°la ~c0.0232 n L

13~-PF~Q 73~{ -~~~5

~I LIMS 1@ [?ascription °lai2ecover~r °kRecavery IS013-07 -04-7 ISO'13- fl7 -04fl08 fS013 -D7 -04-9 DAL-GW-

A~E-D-13{}429 DAL -GW- ACE-0&13U429 DAL-GW- RCE-FftAS-13D429 92.9 93.4 100 105

99.1 103 Average C~c~ratr~rlaon {ngtrr~L)± °IaRSD 95.2°1a ± 4.6°ta 102°l0 ± 28°14
1VA = Plot Applicab~ {1) Samples were analyzed by int~nai standard calibration.

PANE 15 ~213M EA11/JRONMENTAL LRSORATC3RY REPOF2T tVO. 1SO13

-0 ?-U4



### Table 13. DAL GW WW8R 130429 ~'~
~FQA PFBS Concer~a~on Gonc~er►tration 3M LIMS D Description (ngtmL) °loRecwvery ~ng/rnL) °1oRecav+~ry IS013U7-04-010 DAL -GI+VWW8R-0- 13d4~9 3180 t~A 3S4 NA I~O13-07-09-11 DAL -~WW WW8R-D &13D429 3206 NA 364 NA tS~13-07-09-012 D,4L -~WWV4'WSR-FN15- 13D429 696D 94.3 4170 94.7 Average Conceon {ngtmL)*_ ° /aRPD 3990 ngtrr~~ # 0.63°h 364 ngtmL± O.Q°Jo
PFHS PFCkS

Goncer►tratian Conafion 3M LIMS Id I~escri mL °loRecove n L °l~RRecc~v~ tSa13-D7 -0~3-(}1D DAL

-GIN WW8R -0- 13x429 1f04 NA 4840 NA lS013-07-0d-011 DAL -GV1t WW8R -D&130429 1620 NA 4820 NA ISC}13-D7-tl~l-0'12 DAL-GW- 1Nl+U8R -FFviS -1429 539D 94.7 8230 85.4 AverageC~ceon~nglmL) ± °l4RPD 1610ngImL ±1.2°l0 483Qng►mL ±0.41°la

13 .~FQQ 13~{-Q~~cJ
3N[ AIMS ID C~scriptiaort °1aRecovery °1oRecavery ISC113-0~-D4-010 DAL -GW U'~~W8R -0-130429 89_~ 103 tS013-07-04011 DAt.-GW WW8R-0&130429 88.8 9U4 IS1713-07-04~012 DAL-GW- VWN8R-Ffl+►S- 13D429 ~d.3 94.9 Aver e Cs~ncerrtr~ation n mL {'° /aRSD $7.3°/a ± 3A°la 100% ±4.8°l0 Ni4 = I~t Applicable (1) Samples were analyzed by extemsl s arci cali[~aticx~_ The surrogate rec~ovvery standards 13Cd -PFOR pct 13C,,-PF{~S werde added to the samples d~iru~ sample preparation.

PAGE 96 (3213M ElVVlROfUMENTAL LABORATORY REPORT Nd. !S{)93-07 -04



### Table 14. DAB GW WW9R 43g429 ~'~

PFOA PFBS Concerrtr~tion CanoeMration 3M LIMS ID Descri n mL °~Rec:ove n mL °kRecove ISfl13-07-04013 DAI_ -GW WW9R -0-130 29 2640 NA 240 NA IS013-07-04014 DAL-GW` -WW9R-0 &930429 269t} Itit~i ~ 247 NA IS013-07-04015 DAL -+GW WW9R-F(v1,S-13D429 5~4fl 79.9 353i} 81.8 Average Concean {nglmL) #°l -0RPD 2650 ngtmL ± 3.d% ~ 2A4 ng/mL ± 29°!a r PFHS PFOS Concentration Conoentratian 3N1 AIMS td description (ngimL) °kRec~ very (nglmL) °foRecovery tS013-07-04 -1113 DAL -GW WW9R -0-13fl429 1'!80 i~f# 4260 NA IS013-07-04 -D14 DAL -GW VVIN9R- [3&13D429 1214 RIA 4490 NA IS413-07-04015 DAL -GW WW9R- FR~i-13~429 4480 823 8870 114 Aver e C~ceon n mL # °IoRPD 9200 n mL ±2.5°l4 434a n L ±3.5°fo
~sC,~-I,FOA 13~ -PFOS

~1 LINlS ID Description %Recovery °loReaovery IS~13-07- 04-013 DAL- t~W-VWV9R-0- 13D429 88.8 104 t5t313-07-04014 DRL-GW-WW9R-DB- 13129 9tt.9 105 15013

-07-04-0'15 DAL -GW WW9R -~R~S- 130429 86.7 93.7 Average Conceon {ngfmL) ± °laRSD 89.8°lm ± 4.S°k 101 °l0 ± 6.6°10 (dA =Not Appiicab~ {1) Samples uu~e anatyced by external standard cali~atian_ 'iY~e surrogate recovery staridards'~Ca -PFOA ~d 13G,-PFOS were ceded to the sam~es d ry sample ~eparatian_

PAC~EE 17 ~ 213M ENU/iROtVMElVTAL LA8{1RATORY REPORT Nfl. lS073-0~ D4



## Table 15. Trip Blank Results

PFOA PFBS

GUnaer►tration Condon 3IV1 LIMS ID Descri i~ n mL °lsRec~ve n L °~Recove IS013- Q7-(kt-016 DAL- GU4+- TR1P{)1-0 <D.(1240 ~~ NA <0.0250 ~i~ NA IS013-07-D4-017 DAL-GW-TRIP01 -LS 8.12 ~') 81.2 S_78 {~~ 87.8

ISC►13- 07-0MD18 DAL-GiM-TF21P~1 -1iS 3570 ~ 89.3 3880 ~ ~.5
PFHS PFOS Goncer~h~tion +Concen#ration 3N1 LIMS iD Description (ng/mL) °laRec:ave►Y {n~tm~1 'YaRecavery ISfJ13-07- 04-016 DRL- LUW- TRIRtD1 -0 «_~25D ~~> NA <0.0232 t'~ NA ISC?13-07-04-fl17 DAL-GW-7RIF'01 -L5 x:32 t~~ 93.3 8.88 {1, 88.8 tS013-07-04-018 Df~I-GW-TRIP~1 -H5 3 ?3Q ~ 93.5 4030 ~ 109

93~-PF{7A 13~,~~~`

3M ~.IMS IQ Description °1~Recovery °IoRecovery IS013-07-04-016 DAL-GW-TRIP~1-0 97.1 ~'~ 90.6 ~~~

!S~►~3-07-D~-fl17 DAL-GW-TF21Pt)1 -~S J9.9 ~~~ E~.8 ~~~ ISt}13-07- D4-018 DAL-GW-TRIP~1 -IiS 89.6 ~ 162
NA =Pmt Applicable {1) Samp{es vvere anal~rzed by internal standard calibration. {2) Samples vine analyzed by e~ckemsi standard calit~aiicm_

PAGE 98 QF 213M EIVVIROIUM~IVTAL LABORATORY REPORT NO. i50t3-07 -04



# ~ c~n~r~~;on Laboratory control spikes were used to determine the analytical method accuracy and precision far ali analytes. The accuracy and precisian were then used to es #imate the method uncertainty for the results. Field matrix spike recoveries ~iemonsUated that the analytical method was appropriate for tine given sample matrix. Analysis was completed using 3N1 Environmental Laboratory Method ETS-B044.1 "Method ~f Analysis f4~ the [determination of Perfluorinat~d Compounds in Water by LC /MSIMS, Direct Injection Analysis". Analytical results are reported i~ Table 1 and ~ 0 -15 of #his report.

~ • ~


## All remaining sample and associated project data {hardcopy and eleciro~ic) will be archived according to 3M Environmental laboratory standard operating prc dures.

~ A'~~~CI7t'ri @~I~S Attachmen# A: Anaiyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTPy GAC System.


# 8 Signatures

Analyiicai Investiga#or

William K. Reagan, Ph.Q, 3(UI Environmental Laboratory Technical Director „~ ~rs~Gl Date

The 3M Environmental Lat~,ratory's C2uality Assurance Unit has audited the data and repork for this project. ,,,,

lilrilfi►I~~iII~I~ifiiJ Quality AsSUrance Date

This test repcarf ~haJ!

not be ,r+eproduced except in full, withoc+t written approval of the 3M Enviraonmen#a!

Ga,baratary.

PAGE 19 OF 2t