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 ACTIVITIES ..................................................................................... 2-1

ATTACHMENTS

Attachment Title

1 GROUNDWATER SAMPLING AND ANALYSIS
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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 ACTIVITIES 

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 – Sampling 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 wells 
J:\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 wells WW8R and WW9R for PFOA analysis. 

Screening Level Human Exposure Assessment 

An Addendum to the Data Assessment Report is being 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 provide 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 SAMPLING

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 feet bgs at WW11R. Both 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 μ March 2013 - April 2013

300 150 Feet 0

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.

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APPENDIX A TO ATTACHMENT 1

WWTP EXTRACTION WELLS - MARCH 2013

ANALYTICAL DATA REPORT ISO13-07-03
3M 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~ 21
3tvJ 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 2 t3F 21
31lAEAtVIRt7NAAEIVTAL 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-~W ACI~ 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-GW ACE 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 4 fic~ 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 21
3A~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

2 mN►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

4131299 [~~]PFt>A 421137E

4131169

PFBS

299I$D

~~e~PFBS 303184

299199

PFHS

399199

[isCsIPFHS 402/8fl

399!80

PFOS

49~J199

499180 ~13Cg3PFOS 507180

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 21
3Ad 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

PAGE7~21
31v9,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 '] 1 D {}.185 0.20{? 1~D8

Avet~gie ~ %RSLY 109°/n ± 3.d°In 1 U$°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 1 D6°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 i tl0 ± 2D°lo.

PAGE 9 C7F 21
3M 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}~ 21
3M 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~ 21
3M 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 1 Q2°/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 21
3A9 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 21
3IVf 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 21
3lU9 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-UW WW9R-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~ 21
3A~ 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 ATTACHMENT 1

WWTP EXTRACTION WELLS - APRIL 2013

ANALYTICAL DATA REPORT ISO13-07-04
3M 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 ~ 21
3M 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 2 C]F 21
3M 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 4 fa 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 ± 9 5°!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 3 OF 21
3~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~E4~21
3M 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

4131219 [~~]PFt~ 421J376

413/1{19

PFSS

23J18d

~y~FBS 3031&t

299199

~~s sssrss

I~~IPFHS 402199

3991'80

PFOS

489199

499180 ['~aIPFOS 5D7J8fl

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 21
3JI+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}~ 21
3M ~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% 1 d5°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 7 V~~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 21
3M 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 ~ 21
3A9 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 11 Q°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}~ 21
3ltA~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~21
3M 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~ 21
3NlEN1tlRONibfENTAt 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 ± i 0%

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 {~ 21
3M 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 ~ 21
3M 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

IS013 U7-04-010 DAL-GI+V W W8R-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-~WW V4'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 (321
3M 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 ~ 21
3M 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 21
3M 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