GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample

s FSIA- Decatur, AL ; Jun e 201 1

GLP10-01-01

. Interi m Repor t 18 : Analysi s o fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur
. A L i n Jun e 201 1
Stud yTitl e Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc
. 140 0 Westo n Wa y Westchester , PA1938 0 Phone:610-701-376 1 Autho r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor t Completio n Dat e

Dat e o fsignin g Performin g Laborator y 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

y 3 M Center , Bld g 260-05-N-1 7 Maplewood , M N 5514 4 Projec t Identificatio n GLP10-01-01-1 8 Tota l Numbe ro fPage s

7 1
Th e testin g reported herei n mee t th e requirement

s ofiSO/iE C 17025-200 5 "Genera l Requirement

s fo rth e Competenc

e ofTestin g an d Calibratio n Laboratories" , I n accordanc e wit h th e A21 ACertificate #2052.01
. Testin g tha t complie s wit h thi s intemationa i Standar d als o operat e i n accordanc

e wit h IS O 9001:2000
. Testin g Cer t #2052.0 1

Page 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Thi s pag e has bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 18
. Analysi s ofPFO

Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n Jun e 201 1 Study : Analysi s ofPerfluorooctanoi cAci d (PFOA) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

•Thes e are environmenta l sample s where there i s n o specifi ctes t substance , n o specifi ctes t syste m an d n o dosin g ofa tes t system
. •Th e reference substance s hav e no t bee n characterize d unde rth e GLP s an d th e stabilit yunde r storag e condition s a

t th e test sit e have no

t bee n detennine d unde rGLPs

.


# 1 ± % 

# ' 2 ^ % Gar yHobiensteiii fSponso rRepresentative Dat e

Jaisimh a Kesari , P.E. , DEE , Stud yDirecto r

Pag e 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 18
. Analysi s ofPFO

Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n Jun e 201 1 Study : Analysi s ofPerfluorooctanoi cAci d (PFOA) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s repor

t an d th e accompanyin g dat a were audite d b yth e 3 M Environmenta l Laborator yQualit y Assuranc e Uni t (QAU) , as indicate d below
. Th e finding s were reporte d t o th e principa l investigato r (P.I.) , laborator

ymanagemen t an d stud ydirecto r

Inspectio n Date s 8/4/11-8/5/1 1 Phas e Data / Interi m Repor

t Dat e Reporte d t o

Testin g Facilit y Managemen t 8/18/1 1 Stud yDirecto r 8/18/1 1



### QA U Representative

Pag e 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### TABL E O F CONTENT S GL P Compliance statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e o fContents 5 List o fTable s 6 1 Stud yInfomnatio n 8 2 Summar

y9 3 Introductio n 1 0 4 Test & Contro l Substance s 1 1 5 Reference Substance s 1 1 6 Tes t Syste m 1 2 7 Metho d Summar

y1 2 7. 1 Method s 1 2 7. 2 Sampl e Collectio n 1 2 7. 3 Sampl e Preparatio n 1 2 7. 4 Analysi s 1 2 8 Analytica l Results 1 4 8. 1 Calibratio n 1 4 8. 2 Syste m Suitabilit y1 4 8. 3 Limi t ofQuantitatio n (LOQ ) 1 4 8. 4 Continuin g Calibratio n 1 4 8. 5 Blank

s 1 5 8. 6 La b Contro l Spike s (LCSs ) 1 5 8. 7 Analytica l Metho d Uncertaint y1 8 8. 8 Fiel d Matri xSpike s (FMS ) 1 8

Pag e 5 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### 9 Data Summar

yan d Discussio n 1 9 1 0 Conclusio n 3 1 1 1 Data/Sampl e Retentio n 3 1 1 2 /\ttachment s 3 1 1 3 Signature s 32 

### LIS TO F TABLE S Tabl e 1
. Summarize d PFO AResults (FSI AGroundwater , Decatur , AL , Jun e 2011 ) 1 0 Tabl e 2
. Instmmen t Parameter s 1 3 Tabl e 3
. Liqui d Chromatograph yCondition s 1 3 Tabl e 4
. Mas s Transition s 1 3 Tabl e 5
. Limi t ofQuantitatio n (LOQ ) 1 4 Tabl e 6
. Laborator

yContro l Spik

e Recover

y1 6 Tabl e 7
. Analytica l Metho d Uncertaint y1 8 Tables
. Fiel d Matri xSpike Level s 1 8 Tabl e 9
. DALGW130R11063 0 2 0 Tabl e 10
. DA L GW130 S 11063 0 2 0 Tabl e 11
. DALGW130L11063 0 2 0 Tabl e 12
. DA L GW131 R 11062 2 2 1 Tabl e 13
. DA L G W131 S 11062 2 2 1 Tabl e 14
. DALGW13 1 L11062 2 2 1 Tabl e 15
. DA L G W133R11063 0 2 2 Tabl e 16
. DA L GW133 S 11063 0 2 2 Tabl e 17
. DALGW133L11063 0 2 2 Tabl e 18
. DA L G W134 R 11062 8 2 3 Tabl e 19
. DA L GW134 S 11062 8 2 3 Tabl e 20
. DALG W134L11062 8 2 3

Pag e 6 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 21
. DALGW135R11062 8 2 4 Tabl e 22
. DA L GW135 S 11062 8 2 4 Tabl e 23
. DALGW135L11062 8 2 4 Tabl e 24
. DA L GW136 S 11063 0 2 5 Table25
. DALG W136L11063 0 2 5 Tabl e 26
. DA L GW137 S 11062 4 2 5 Table27
. DALG W137 L 11062 4 2 6 Table28
. DALG W138 S 11063 0 2 6 Table29
. DALG W138L11063 0 2 6 Table30
. DALG W138R11063 0 2 7 Table31.DALGWCW26C11062 2 2 7 Tabl e 32
. DA L G WCW26L11062 2 2 7 Tabl e 33
. DA L G W140R11062 2 2 8 Table34
. DALG W141R11063 0 2 8 Table35
. DALG W142 R 11062 2 2 8 Table36
. DALG W143 R 11062 2 2 9 Table37
. DALG W144 S 11062 2 2 9 Tabl e 38
. Tri p Blan k

1 2 9 Tabl e 39
. Tri p Blan k

2 3 0 Tabl e 40
. Rinseat e Blank s 3 0

Pag e 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Stud yDirecto r Jaisimh a Kesari , P.E. , DE E Westo n Solutions , Inc
. Westchester, P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigato r(clanqe@mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analys t Chelsi e Grochow , Analys t Kevi n Eich , Analys t Kell yUkes , Analys t Jonatha n Steege , Analys t Stud yDate s Stud yInitiation : Marc h 8 , 201 0 Interi m Repor

t 1 8 Experimenta l Termination : Jul y29 , 201 1 Interi m Repor

t Completion : Dat e ofInteri m Repor t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792
. Th e tes t substanc e an d analytica l referenc e standar d reserv e sample s ar e archive d a t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t th e Fomne r Sludg e Incorporatio n Are a (FSIA) i n Decatur , AL , representin g thirtydifferen t samplin g locations
. A tota l ofon e hundre d fifty-fou rsampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo r perfluorooctanoat e (PFOA ) analysis , an d include d duplicat e groundwate rsample s fro m eac h samplin g location
. Sample s als o include d a t leas t tw o fiel d matri xspik

e (FMS ) sample s fo reac h location , tw o tri p blan k sets containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseates. Th e equipmen t rinseate blank s di d not have FM S sample s prepare d fo rdetenninatio n o fPFO A recovery . Th e groundwate rsamples , tri p blanks , an d two equipmen t rinseate blank s were receive d fro m Westo n personne l o n Jul y8,2011
. Al l ofth e sample s were prepare d an d analyze d fo rPFO A followin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 unde r3 M projec t GLP-10-01-01-18

. Man yofth e groundwate rsample s require d dilutio n t o attai n PFO Aconcentration s withi n th e rang e of th e curve , i n som e instance s u p t o 100-fol d dilutio n were required
. Th e averag e measure d PFO A concentration s are summarize d i n Tabl e 1
. Th e equipmen t rinseates an d th e tri p blank s were below th e lowe rlimi t ofquantitatio n (LLOQ ) of0.025 0 ng/mL , indicatin g adequat e contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections
. Th e PFO Aconcentratio n results fo ral l groundwater

s range d ove rfou rorder

s ofmagnitud e fro m 0.27 7 ng/m L t o 352 0 ng/mL

. Th e analytica l uncertaint ywa s estimate d a

t 100±15%
.

Pag e 9 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 1
. Summarize d PFO AResult s (FSI AGroundwater , Decatur , AL , Jun e 2011 ) Sampl e I D DALGW130R11063 0 DALGW130S11063 0 DALGW130L11063 0 DA L GW131 R 11062 2 DA L GW131 S 11062 2 DA L G W131 L 11062 2 DALGW133R11063 0 DALGW133S11063 0 DALGW133L11063 0 DALGW134R11062 8 DALGW134S11062 8 DALGW134L11062 8 DALGW135R11062 8 DALGW135S11062 8 DALGW135L11062 8 DALGW136S11063 0 DALGW136L11063 0 DALGW137S11062 4 DALGW137L11062 4 DALGW138R11063 0 DALGW138S11063 0 DALGW138L11063 0 DALGWCW26C11062 2 DALGWCW26L11062 2 DA L GW140 R 11062 2 DA L GW141 R 11063 0 DALGW142R11062 2 DA L GW143 R 11062 2 DA L GW144 S 11062 2 Tri p Blank

s (Milli-Q TM Water

) GLP10-01-01-1 8 Equipmen t rinseate blanks : DA L G W130 L an d DA L G W133 S Avg
. PFOA Concentratio n (ng/mL ) 83 0 179 65. 1 243 0 26. 2 95. 1 108 31 3 22 8 180 0 9.8 0 56 0 352 0 21. 0 [a] 27 8 [a] 13 1 79. 0 0.27 7 0.37 7 29 1 154 0.89 3 42 6 64 5 12 9 1.5 8 50. 8 24. 1 50. 6 < 0.025 0 < 0.025 0 Relativ e

Percen t Differenc e 1.7 % 1.1 % 5.4 % 9.9 % 3.8 % 2.4 % 0.0 % 1.0 % 1.8 % 0.56 % 2.6 % 12 % 3.1 % 7.2 % 4.0 % 0.0 % 1.8 % 5.4 % 2.4 % 2.1 % 1.3 % 0.34 % 0.47 % 0.16 % 2.3 % 1.3 % 2.6 % 6.2 % 6.1 % N/ A N/ A N/A : no t applicabl e The analytical uncertaint

yfo rPFO Awa s estimate d a t 100+15%
. [a ] Sampling locatio n di d no

t hav e an appropriat

e FM S spik e leve l t o sufficientl

yevaluat e PFO A recovery.

Thi s analytica l stud ywa s conducte d a s par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilitylocate d i n Decatur , Alabama
. Th e objective o fth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctanoat e (PFOA ) i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d a t th e Fomne rSludg e Incorporatio n Are a (FSIA ) i n Decatur , A L fo rPFO

Ai n a n effor

t t o characteriz e regiona l groundwate rconditions
.

Pag e 1 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Th e 3 M Environmenta l Laborator yprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling
. Sampl e bottl e set s fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d a minimu m oftw o fiel d spike samples
. Eac h empt ycontaine rfo rgroundwate rsampling s wa s mari<e d wit h a "fil l t o here " lin e t o produce a fina l sampl e volum e of20 0 mL
. Container s designate d fo rfiel d matri xsample s were fortifie d wit h a n appropriat e matri xspik e solutio n containin g PFO Aprio rt o bein g sen t t o th e fiel d fo r sampl e collection
. Se e sectio n 8. 8 ofth e repor t fo rfiel d matri xspike levels
. Sample s were prepare d an d analyze d accordin g t o th e procedure define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Determinatio n ofPerfluorinate d Compound s i n Wate rb yHig h Perfomrianc

e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Tabl e 1 summarize s th e averag e PFO Aconcentration s fo rth e duplicat e groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples
. Table s 9-4 0 summariz e th e individua l sampl e results an d th e associate d FM S recoveries
. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s are reporte d an d discusse d elsewhere i n thi s report
.

There wa s no

t a test substance o rcontro l substance s i n th e classi csens e ofa GL P study
. Thi s stud y wa s purel yanalytica l i n nature
.

Th e analytica l reference substance s use d fo rthi s stud yare liste d below
.
Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Us e Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO A(Linear ) Perfluorooctanoate C7F15COO H CAS #335^7- 1 Targe t Analyt e Reference Standar

d Oakwoo d Products 01/17/201 8 Froze n 344 0 TCR07-004 1 Powde r 99.1 % PFO A (Unea r+ Branched ) Perfluorooctanoate C7F15COO H Ammoniu m Sal t CAS #335-67- 1 LC S Reference Standar d 3 M 02/27/201 7 Froze n 33 2 TCR-12 3 Whit e powde r 95 % "Cg-PFOA

Perfluorooctanoate ^'CsHFisOz CAS#MPFC-C-051 1 Intema l Standar

d Wellingto n 05/25/201 4 Froze n 05241 1 TCR11-001 6 Liqui d NA<^ ' "CirPFO A

Perfluorooctanoat e ^^C8HF1502 CAS#MPFC-C-091 0 Intema l Standar

d Wellingto n 09/28/201 3 Froze n 09231 0 TCR11-004 8 Liqui d NA TM (1 ) Compoun d i s par

t o fa custo m mixtur

e ofmass-lat)ele d perfluorinate d compound s a t a concentratio n o f5. 0 pg/mL

.

Pag e 1 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### There wa s no

t a tes t syste m fo rthi s stud yi n th e classi csens e ofa GL P study
. Thi s stud ywa s conducte d fo ranalysi s ofgroun d wate rsample s collecte d fro m well s locate d i n Decatur , A L byWesto n Solutions , Inc
. personnel
. Sample s fo rthi s stud yare "rea l worid " environmenta l samples
. Sampl e Descriptio n Ke yCode

. strin g Humbec Exampl e 1 2 3

4 5 Strin g Descripto r Exampl e DA L GW131 R 011062 2 Sampl e Locatio n Wel l I D Wel l Leve l
Samplin g Dat e Sampl e Typ e DAL = Decatur , Alabam a Example : 13 1 R = Residu m shallo wwater-ljearin g zon e L = Bedroc k

water-bearin g zin e S = Epikars t middl e water-bearin g zon e 110622-Jun e 22,201 1 0=primarysampl e 1=duplicat e sampl e L S = lo wspik e IVI S = mi d spik e H S = hig h spik e



## 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Determinatio n ofPerfluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
.
.,T M , 

## 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene'" " (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s associate d wit h GLP10-01-01-1 8 were returne d t o th e laborator yat ambien t condition s o n Jul y8,2011
. Sample s were store d refrigerate d a t th e laborator

y afte rreceipt
. Aset o flaborator yprepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspike s were sen t wit h eac h coole rofsampl e collectio n bottles
. 

## 7. 3 Sampl e Preparatio n Sample s were prepare d byremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Sample s that require d dilutio n were prepare d bydilution s 1m L sampl e wit h 9 mLs ofMilli- Q wate r (dilutio n 1:10)

. Sample s that require d dilutio n were prepare d b ydilution s ofIm L sampl e wit h 9 mLs o f Mill i Q wate r(dilutio n 1:10)

. Sample s requirin g a 1:100 dilutio n were prepare d b yaddin g 0. 1 m L sampl e t o 9. 9 mLs ofMilli Q wate r 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFO Ausin g hig h performance liqui d chromatography

/ tande m mas s spectrometr y(HPLC/MS/MS)

. Detaile d instrumen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmas s transition s analyze d are describe d i n th e

Pag e 1 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### ra wdat a har

d copie s place d i n th e fina l dat a packet , an d are briefl ydescribe d belowi n Tabl e 2 , Tabl e 3 an d Tabl e 4
. Tabl e 2
. Instrumen t Parameters
. instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n injectio n Volum e IVIas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETSKir H ETS-8-044. 0 7/15/11-7/19/1 1 Agilen t 1200 Pris m R P (2. 1 m m X 5 0 mm) , 5 n Betasi l C1 8 (2. 1 m m X10 0 mm) , 5 n

5or25n L Applie d Biosystem s AP I 550 0 Turb o Spra

y Turb o io n electrod e Negativ e Analyst 1.5. 2 ETSKir k ETS-8-044. 0 7/28/11-7/29/1 1 Agilen t 120 0 Betasi l C I 8 (4. 6 m m X 100 mm) , 5 n Betasi l C I 8 (4. 6 m m X 100 mm) , 5 u

2 5 n L Applie d Biosystem s AP I 550 0 Turb o Spra

y Turb o io n electrod e Negative Analyst 1.5. 2 

### Tabl e 3
. Liqui d Chromatograpfi yConditions

. ste p Number Tota l Tim e

(min ) Flo wRat e

(idJmin ) Percen t A

( 2 m M ammoniu m acetate ) Percen t B (Methano O 7/15/11-7/19/1 1 Analysi s 0 1 2 3 4 5 0. 0

2. 0 14. 5 15. 5 15. 6 20. 0 30 0

30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 7/28/1 1 -7/29/1 1 Analysi s 0 1 2 3 4 5 0. 0

2. 0 14. 5 15. 5 16. 5 20. 0 75 0

75 0 75 0 75 0 75 0 75 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 

### Tabl e 4
. Mas s Transitions
.

Analyt e
PFOA Mas s Transitio n Q1/Q 3 413/36 9 413/21 9 413/16 9 Intema l Standar d ^^ '
t'CJPFO A Mas s Transitio n Q1/Q 3 421/37 6 Dwel l tim e wa s 2 0 o r3 0 mse cfo reac h transition
. Th e individua l transition s were summe d t o produce a 'tota l io n chromatogram " (TIC) , whic h wa s use d fo rquantitation
. (1 ) Intema l standar

d wa s onl yuse d fo ranalysi s performe d o n 7/28/11

.

Pag e 1 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### 8. 1 Calibratio n Al l sample s were initiall yanalyze d against a n externa l standar d calibratio n curve . Calibratio n standard s were prepare d b

yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s into a laboratory-Mill i Q water
. Atota l offifteen spike d standard s rangin g fro m 0.02 5 ng/m L t o 10 0 ng/m L (nominal ) were prepared
. Aquadratic , 1/ xweighted , calibratio n curve ofth e pea k are a counts wa s use d t o fi t th e dat a fo rPFOA

. Th e dat a were no t force d throug h zer

o durin g th e fittin g process . Calculatin g th e standar

d concentration s usin g th e pea k are a confirme d accurac

yofeac h curve point
. Sampl e DA L G W135 S wa s repeate d usin g a stabl e isotop e intema l standar d calibratio n curve . Calibratio n standard s were prepare d b yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s into a laboratory-prepare d syntheti cgroundwate rcontainin g calciu m an d magnesium
. A separat e intema l standar d spikin g solutio n wa s prepare d an d a n aliquot wa s adde d at th e sam e leve l t o al l calibratio n standard s an d laborator ycontro l sample s a

t a nomina l concentratio n of1 ng/mL

. A calibratio n curve rangin g fro m approximatel y0.02 5 ng/m L t o 100 ng/m L wa s prepared
. Aquadratic , 1/ x weighted , calibratio n curve ofth e standar d pea k area / pea k are a ratio s wa s use d t o fit th e dat a fo reac h analyte
. Th e dat a were no t force d throug h zer

o durin g th e fitting process . Calculatin g th e standar d concentration s usin g th e pea k area / pea k are a ratio s an d th e resultan t calibratio n curve confirme d accurac yofeac h curve point
. Fo rbot h analytica l mns , eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac yrequirements of100±25 % (100±30 % fo rth e lowest curve point) were met fo ral l analytes
. Th e con-elatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFOA

. 8. 2 Syste m Suitabilit y Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofth e analytica l sequence t o demonstrat e overal l syste m suitability
. Th e acceptance criteri a o fles s tha n o requa l t o 5 % relative standar d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a ofles s tha n o requa l t o 2 % RS D wa s met fo rPFOA

. 

## 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LO Q fo rthi s analysi s i s th e lowest non-zer o calibratio n standar

d i n th e curve that meets linearit y an d accurac

yrequirements an d fo rwhic h th e are a counts are a t least twic e thos e o fth e appropriat e blanks
. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 5
. Tabl e 5
. Limi t o fQuantitatio n (LOQ)

. Analysi s Date s 7/15/11,7/28/1 1 PFOA

LOQ , ng/m L 0.025 0 

## 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l CCVs met metho d criteri a of100 % ±25 % fo rPFOA

.

Pag e 1 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



## 8. 5 Blank s Thre e type s ofblank

s were prepare d an d analyze d wit h th e samples : solven t blanks , tri p blanks , an d equipmen t rinseate blanks
. Solven t blan k results were reviewe d an d use d t o evaluat e metho d performance t o determin e th e LO Q fo rPFOA

. Tri p blank s refiec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience
. Equipmen t rinseate blank s are aqueou s sample s that refiec

t th e efficienc

yofequipmen t cleanin g i n th e field betwee n differen t sampl e collection s an d are proofofn o cros s contaminatio n ofsample s fro m th e equipment
. 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set
. LCS s were prepare d byspikin g know n amounts ofth e analyt e into 1 0 m L oflaborator y Mill i Q wate ro rsyntheti cgroundwater , t o produce th e desire d concentration
. Th e spike d wate rsample s were the n analyze d i n th e sam e manne ra s th e samples
. Th e metho d acceptance criteria , averag e o f LC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <20% , were met fo rth e linea rPFO ALC S samples
. A s th e reference material s use d fo rquantitatio n ofPFO Ai s predominantl ylinear , an d th e PFO Apresen t i n th e wate rsample s are comprise d oflinea ran d branche d isomers , additiona l LC S sample s o flinea r an d branche d PFO

Awere prepare d a

t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias
. Th e linea ran d branche d LC S met metho d acceptance criteri a a t al l levels
. Al l LC S sample s were use d i n th e detemninatio n ofmetho d uncertaint yi n sectio n 8.7
. Th e followin g calculation s were use d t o generat e dat a i n Tabl e 6 fo rlaborator ycontro l spikes :

, ^or
. . r . Calculate d Concentratio n , . „„„ , LC S Percen t Recover

y= * 100 % Spik e Concentratio n LCS%RS D = Standar

d deviatio n LC S replicate s .^^py ^ averag e LC S recover

y

Pag e 1 5 o f7 1

### Tabl e 6
. Laborator yContro l Spik e Recovery
. GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1

ETS-8-044. 0 Analyze d 7/15/201 1
La b I D LCS-110714- 1 LCS-110714- 2 LCS-110714- 3 Averag e ±%RS D LCS-110714- 4 LCS-110714- 5 LCS-110714- 6 Averag e ±%RS D LCS-110714- 7 LCS-110714- 8 LCS-110714- 9 Averag e ±%RS D Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 LinearPFO A

Calculate d Concentratio n (ng/mL ) 0.51 0 0.50 6 0.54 7 %Recover y

10 2 10 2 11 0 105 % ±4.4 % 4.9 8 4.9 8 4.9 8 5.1 6

5.2 6 5.2 6 10 4

10 6 10 6 105 % ±1.1 % 29. 9 29. 9 29. 9 28. 3

27. 5 28. 4 94. 6

92. 0 94. 9 93.8%±1.r/ o ETS-8-044. 0 Analyze d 7/15/201 1
La b I D LCS-110714-1 0 EC F LCS-110714-1 1 EC F LCS-110714-1 2 EC F Averag e ±%RS D LCS-110714-1 3 EC F LCS-110714-1 4 EC F LCS-110714-1 5 EC F Averag e ±%RS D LCS-110714-1 6 EC F LCS-110714-1 7 EC F LCS-110714-1 8 EC F Averag e ±%RS D Ur n Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 3a r+ Branche d P F

Calculate d Concentratio n (ng/mL ) 0.52 2 0.47 0 0.49 1 •OA

VoRecover y 10 5 94. 4 98. 5 99.3 % ±5.4 % 4.9 9 4.9 9 4.9 9 4.9 6

4.9 9 5.1 8 99. 3

100 104 101 % ±2.5 % 29. 9 29. 9 29. 9 31. 3

30. 3 30. 5 10 5

10 1 10 2 103 % ±2.0 %

Pag e 1 6 o f7 1

### Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1

ETS-8-044. 0 Analyze d 7/28/201 1
La b I D LCS-110726- 1 LCS-110726- 2 LCS-110726- 3 Averag e ±%RS D LCS-110726- 4 LCS-110726- 5 LCS-110726- 6 Averag e ±%RS D LCS-110726- 7 LCS-110726- 8 LCS-110726- 9 Averag e ±%RS D Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 LinearPFO A

Calculate d Concentratio n (ng/mL ) 0.21 0 0.21 1 0.22 1 %Recover y

10 6 10 6 11 1 108%±2.r/ o 1.9 9 1.9 9 1.9 9 2.0 3

1.9 7 2.0 2 10 2

98. 7 10 2 101 % ±1.9 % 19. 9 19. 9 19. 9 19. 1

19. 3 19. 3 96. 0

97. 0 96. 8 96.6 % ±0.55 % ETS-8-044. 0 Analyze d 7/28/201 1
La b I D LCS-110726-1 0 EC F LCS-110726-1 1 EC F LCS-110726-1 2 EC F Averag e ±%RS D LCS-110726-1 3 EC F LCS-110726-1 4 EC F LCS-110726-1 5 EC F Averag e ±%RS D LCS-110726-1 6 EC F LCS-110726-1 7 EC F LCS-110726-1 8 EC F Averag e ±%RS D Li m Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 3ar+BrancfiedP F

Calculate d Concentratio n (ng/mL ) 0.20 6 0.21 5 0.21 7 •OA

%Recover y 104 10 8 10 9 10r/o±2.5 % 1.9 9 1.9 9 1.9 9 1.9 9

2.0 1 2.1 4 99. 8

10 1 10 7 103 % ±3.8 % 19. 9 19. 9 19. 9 20. 2

21. 7 22. 7 10 2

10 9 114 108 % ±5.6 %

Pag e 1 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



## 8. 7 Analytica l Metho d Uncertaint y Analytica l uncertaint

yi s base d o n historica l QC dat a that i s contro l charte d an d use d t o evaluat e metho d accurac

yan d precision
. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2

. Th e standar d deviatio n i s calculate d fo rth e se t o faccurac yresults (i n %) obtaine d fo rth e Q C samples
. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h correspond s t o a confidence leve l of95%
. Tabl e 8
. Analytica l Metho d Uncertainty
. Analyt e PFO A Metho d

ETS-8-044. 0 Standar d [)eviatio n 7.2 8 Metho d

Uncertaint y ±15 % 

## 8. 8 Fiel d Matri xSpike s (FMS ) Aminiu m o

ftw o field matri xspike s were collecte d a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix
. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offield sampl e t o a containe rspike d b yth e laborator

ywit h th e targe t analyte s prio rt o shippin g sampl e container

s fo rsampl e collection
. Fiel d matri xspike recoverie s withi n metho d acceptance criteri a of100±30 % confir m that "unknown " components i n th e sampl e matri xd o no t significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Fiel d matri xspike concentration s must b e 50 % of th e sampl e concentratio n t o b e considere d a n appropriat e field spike
. Fiel d matri xspike s are presente d i n sectio n 9 ofthi s report
. Tabl e 9. Fiel d Matri xSpil< e Levels
. Samplin g Locatio n 134S , 135S , 136R , 137R , 137S , 137L , 138 L 130L , 131S , 131L , 133R , 135L , 136S , 136L , 141R , 142R , 143R , 144 S 130R , 130S , 133S , 133L , 134L , 138R , 138S , CW26C , CW26L , 140 R 131R , 134R , 135 R
Tri p Blan k Spik e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h PFOA , ng/m L

0.098 5 0.98 5 9.8 5 0.98 5 9.85 98. 7 9.85 98. 7 49 4 98. 7 195 6 0.98 5 9.8 5 98. 7 49 4

_(Sample Concentrationof FMS - Averag e Concentration : FieldSampl e & FieldSampl

e Dup. ) ^ Spik e Concentraton 100 %

Pag e 1 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s as wel l as th e Tri p Blank s an d rinseate blanks
. Results an d averag e value s are rounde d t o thre e significan t figures accordin g t o EP Aroundin g rules
. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspike recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G W135S11062 8 - Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no

t have a n appropriat e FM S spike leve l t o sufficientl yevaluat e PFO Arecovery . DA L G W135L11062 8 - Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no

t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery .

Pag e 1 9 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 10
. DA L G W130 R 11063 0

3IVIUMSI D GLP10-01-01-18-00 6 GLP10-01-01-18-00 7 GLP10-01-01-18-00 8 GLP10-01-01-18-00 9 GLP10-01-01-18-01 0 Descriptio n DA L GW130 R 011063 0 DA L GW130RD B 11063 0 DA L GW130RL S 110630 DA L GW130 R M S 11063 0 DALGW130RHS11063 0 Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 83 7 82 3 83 3 92 1 128 0 VoRecovery :

N A NA N C N C 91. 2 83 0 ng/m L ±1.7 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 11
. DA L G W130 S 11063 0

3IVIUMSI D GLP10-01-01-18-01 1 GLP10-01-01-18-01 2 GLP10-01-01-18-01 3 GLP10-01-01-18-01 4 GLP10-01-01-18-01 5

Averag e Con e Descriptio n

DA L GW130 S 011063 0 DA L GW130SD B 11063 0 DA L GW130 S LS11063 0 DALGW130SMS11063 0 DA L GW130SH S 11063 0 entiytio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 18 0 17 8 18 1 26 5 70 8 17 9 ng/m L VoRecover

y N A NA N C 87. 1 107 ±1.1 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. 

### Tabl e 12
. DA L G W130 L 11063 0

3IVIUMSI D GLP10-01-01-18-01 6 GLP10-01-01-18-01 7 GLP10-01-01-18-01 8 GLP10-01-01-18-01 9 GLP10-01-01-18-02 0 Descriptio n DA L GW130 L 011063 0 DA L GW130LD B 110630 DA L GW130LL S 11063 0 DA L GW 1 SO

L M S 11063 0 DALGW130 L H S 110630 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 66. 8 63. 3 68. 7 74. 8 15 8 VoRecovery

^ N A N A N C N C 94. 2 65. 1 ng/m L ±5.4 % NA = Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 13
. DA L G W131 R 11062 2

3IVIUIVISt D GLP10-01-01-18-02 1 GLP10-01-01-18-02 2 GLP10-01-01-18-02 3 GLP10-01-01-18-02 4 Descriptio n DA L GW131 R 011062 2 DA L GW131RD B 110622 DA L GW131RL S 110622 DA L GW131RH S 11062 2 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 231 0 255 0 249 0 406 0 VoRecover

y N A N A N C 83. 3 243 0 ng/m L ±9.9 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 14
. DALG W131 S 11062 2

3 M LIM S I D GLP10-01-01-18-02 5 GLP10-01-01-18-02 6 GLP10-01-01-18-02 7 GLP10-01-01-18-02 8 GLP10-01-01-18-02 9

Averag e Con e Descriptio n

DA L GW131 S 011062 2 DALGW131SD B 110622 DA L GW131SL S 11062 2 DA L GW131 S M S 11062 2 DA L GW131SH S 110622 entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 26. 7 25. 7 26. 6 36. 0 11 5 26.2ng/m l VoRecover

y N A NA N C N C 90. 0 .±3.8 % NA = No t Applicabl e N O = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 15
. DA L G W131 L 11062 2

3 M LIM S I D GLP10-01-01-18-03 0 GLP10-01-01-18-03 1 GLP10-01-01-18-032 GLP10-01-01-18-03 3 GLP10-01-01-18-034 Descriptio n DA L GW131 L 011062 2 DA L GW131LD B 110622 DA L GW131 L LS11062 2 DA L G W131 L M S 11062 2 DALGW131LHS11062 2 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 93. 9 ^ 96. 2 97. 3 107 185 VoRecover

y N A NA N C N C 91. 1 95. 1 ng/m L ±2.4 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 16
. DA L G W133 R 11063 0

3IVILIIVISI D GLP10-01-01-18-04 5 GLP10-01-01-18-04 6 GLP10-01-01-18-04 7 GLP10-01-01-18-04 8 GLP10-01-01-18-04 9 Descriptio n DA L GW133 R 011063 0 DA L GW133RD B 110630 DA L GW133RL S 11063 0 DA L GW133 R M S 11063 0 DALGW133RHS11063 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 108 108 96. 6 11 2 19 0 10 8 ng/m L VoRecover

y N A N A N C N C 83. 1 ±0.0 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. 

### Tabl e 17
. DA L G W133 S 11063 0

SIVILIMSI D GLP10-01-01-18-04 0 GLP10-01-01-18-04 1 GLP10-01-01-18-042 GLP10-01-01-18-04 3 GLP10-01-01-18-044 Descriptio n DA L GW133 S 011063 0 DA L GW133SD B 110630 DA L GW133SL S 11063 0 DALGW133SMS11063 0 DA L GW133SH S 110630 Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 31 1 31 4 31 6 39 7 76 8 VoRecover

y N A N A N C N C 92. 3 31 3 ng/m L ±1.0 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 18
. DA L G W133 L 11063 0

3 M LIM S I D GLP10-01-01-18-03 5 GLP10-01-01-18-03 6 GLP10-01-01-18-03 7 GLP10-01-01-18-03 8 GLP10-01-01-18-03 9

Averag e Con e Descriptio n

DA L GW133 L 011063 0 DA L GW133LD B 11063 0 DA L GW133 L LS11063 0 DA L GW133 L M S 11063 0 DA L GW133LH S 11063 0 entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 23 0 22 6 26 5 41 7 70 8 22 8 ng/m L VoRecover

y NA NA N C N C 97. 3 ±18 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 19
. DA L G W134 R 11062 8

3 M LIM S I D GLP10-01-01-18-05 0 GLP10-01-01-18-05 1 GLP10-01-01-18-05 2 GLP10-01-01-18-05 3 Descriptio n DA L GW134 R 011062 8 DALGW134RDB11062 8 DA L GW134 R LS11062 8 DA L GW134RH S 11062 8 Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 179 0 180 0 187 0 361 0 VoRecover

y N A N A N C 92. 8 180 0 ng/m L ±0.56 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 20
. DA L G W134 S 11062 8

3 M LIM S I D GLP10-01-01-18-05 9 GLP10-01-01-18-06 0 GLP10-01-01-18-06 1 GLP10-01-01-18-06 2 GLP10-01-01-18-06 3

Averag e Con e Descriptio n

DA L GW134 S 011062 8 DA L GW134SD B 11062 8 DA L GW134SL S 11062 8 DA L GW134 S M S 11062 8 DA L GW134SH S 11062 8 entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 9.6 7 9.9 2 9.6 0 10. 7 19. 6 9.8 0 ng/m l VoRecover

y NA NA N C N C 99. 5 .±2.6 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 21
. DALG W134 L 11062 8

3 M LIM S I D GLP10-01-01-18-05 4 GLP10-01-01-18-05 5 GLP10-01-01-18-05 6 GLP10-01-01-18-05 7 GLP10-01-01-18-05 8 Descriptio n DA L GW134 L 011062 8 DA L GW134LD B 11062 8 DA L GW134 L LS11062 8 DA L GW134 L M S 11062 8 DA L GW134LH S 11062 8 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 52 7 59 2 60 2 67 7 101 0 VoRecover

y N A N A N C N C 91. 3 56 0 ng/m L ±12 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
.

Pag e 2 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 22
. DA L G W135 R 11062 8

3 M LIM S I D11119999nil_j_i_j_iCDCDCDCD Descriptio n

DA L GW135 R 011062 8 DALGW135RDB11062 8 DA L GW135RL S 11062 8 DA L GW135RH S 11062 8 Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 357 0 346 0 360 0 525 0 VoRecover y

N A N A N C 88. 7 352 0 ng/m L ±3.1 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 23
. DA L G W135 S 11062 8

3 M LIM S I D GLP1001-01-18-06 9 GLP10-01-01-18-07 0 GLP1001-01-18-07 1 GLP10-01-01-18-07 2 GLP1O01-01-18-07 3 Descriptio n DA L GW135 S 011062 8 DALGW135SDB11062 8 DALGW135SLS11062 8 DA L GW135 S M S 11062 8 DALGW135SHS11062 8 Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 20. 2 21. 7 NA<^ ' NA TM 44. 3 VoRecover y

N A N A NA<^ ' NA'^ ' N C 21. 0 ng/m L ±7.2%' ^ N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. (1 ) Sampl e no

t analyze d du e t o spike concentratio n no t bein g appropriate compare d t o sampl e concentration
. (2 ) Samplin g locatio n di d no t hav e a n appropriate spike leve l t o evaluat e PFO Arecovery . 

### Tabl e 24
. DA L G W135 L 11062 8

3 M LIM S I D GLP10-01-01-18-07 4 GLP1001-01-18-07 5 GLP1001-01-18-07 6 GLP10-01-01-18-07 7 GLP10-01-01-18-07 8 Descriptio n DA L GW135 L 011062 8 DA L GW135LD B 11062 8 DA L GW135LL S 11062 8 DA L GW135 L M S 11062 8 DA L GW135LH S 11062 8 Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 28 3 27 2 27 8 28 9 36 5 VoRecover y

N A N A N C N C N C 27 8 ng/m L ±4.0%' " N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. (1 ) Samplin g locatio n di d no t have a n appropriate spik e leve l t o evaluat e PFO

Arecovery .

Pag e 2 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 /Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 25
. DA L G W136 S 11063 0

3 M LIM S I D GLP10O1-01-18-08 8 GLP10-01-01-18-08 9 GLP10-01-01-18-09 0 GLP10-01-01-18-09 1 GLP10-01-01-18-09 2 Descriptio n DA L GW136 S 011063 0 DALGW136SDB11063 0 DA L GW136SL S 11063 0 DA L GW136 S M S 11063 0 DA L GW136SH S 11063 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 13 1 13 1 132 136 21 7 VoRecover

y N A NA N C N C 87. 1 13 1 ng/m L ±0.0 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 26
. DA L G W136 L 11063 0

3 M LIM S I D GLP1001-01-18-08 4 GLP1001-01-18-08 5 GLP1001-01-18-08 6 GLP10-01-01-18-15 5 GLP10-01-01-18-08 7 Descriptio n DA L GW136 L 011063 0 DALGW136LDB11063 0 DA L GW136LL S 11063 0 DA L GW136 L M S 11063 0 DA L GW136LH S 110630 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 79. 7 78. 3 79. 6 89. 1 17 0 VoRecover

y N A N A N C N C 92. 2 79. 0 ng/m L ±1.8 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 27
. DA L G W137 S 11062 4

3 M LIM S I D GLP10-01-01-18-09 3 GLP10-01-01-18-09 4 GLP10-01-01-18-09 5 GLP10-01-01-18-09 6 GLP1O01-01-18-09 7 Descriptio n DA L GW137 S 011062 4 DALGW137SDB11062 4 DA L GW137SL S 110624 DALGW137SMS11062 4 DALGW137SHS11062 4 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 0.284 0.26 9 0.38 3 1.1 8 9.32 VoRecover

y NA NA N C 91. 7 91. 8 0.27 7 ng/m L ±5AV o NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 5 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 28
. DA L G W137 L 11062 4

3 M LIM S I D GLP10-01-01-18-09 8 GLP10-01-01-18-09 9 GLP10-01-01-18-10 0 GLP10-01-01-18-10 1 GLP10-01-01-18-10 2 Descriptio n DA L GW137 L 011062 4 DA L GW137LD B 110624 DA L GW137LL S 11062 4 DALGW137LMS11062 4 DA L GW137LH S 110624 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 0.372 038 1 0.47 7 1.3 5 9.9 8 VoRecover

y NA NA N C 98. 8 97. 5 0.37 7 ng/m L ±2.4 % N A= Not/Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. 

### Tabl e 29
. DA L G W138 S 11063 0

3 M LIM S I D GLP10-01-01-18-11 3 GLP10-01-01-18-11 4 GLP10-01-01-18-11 5 GLP10-01-01-18-11 6 GLP10-01-01-18-11 7

Averag e Con e Descriptio n

DA L GW138 S 011063 0 DA L GW138SD B 110630 DA L GW138 S LS11063 0 DA L GW138 S M S 11063 0 DA L GW138SH S 110630 entratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 155 153 16 1 23 1 61 0 154 ng/m L VoRecover

y N A N A N C 78. 0 92. 4 ±13 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 29
. DA L G W138 L 11063 0

3 M LIM S I D GLP10-01-01-18-10 8 GLP10-01-01-18-10 9 GLP10-01-01-18-11 0 GLP10-01-01-18-11 1 GLP10-01-01-18-11 2 Descriptio n DA L GW138 L 011063 0 DA L GW138LD B 11063 0 DA L GW138LL S 11063 0 DA L GW138 L M S 11063 0 DA L GW138LH S 11063 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 089 1 0.89 4 0.974 1.69 9.1 4 VoRecover

y NA NA N C 81 0 83. 7 0.89 3 ng/m L ±0.34 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 6 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 30
. DA L G W138 R 11063 0

3 M LIM S I D GLP10-01-01-18-10 3 GLP1OO1-01-18-104 GLP10-01-01-18-10 5 GLP10-01-01-18-10 6 GLP10-01-01-18-10 7 Descriptio n DA L GW138 R 011063 0 DA L GW138RD B 110630 DA L GW138RL S 11063 0 DA L GW138 R M S 11063 0 DA L GW138RH S 11063 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 29 4 28 8 29 2 37 0 70 9 29 1 ng/m L VoRecover

y NA N A N C N C 84. 7 ±2.1 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 31
. DA L G WCW26 C 11062 2

3 M LIM S I D GLP10-01-01-18-11 8 GLP10-01-01-18-11 9 GLP10-01-01-18-12 0 GLP10-01-01-18-12 1 GLP10-01-01-18-12 2

Averag e Con e Descriptio n

DA L GWCW26 C 011062 2 DA L G WCW26 C D B 11062 2 DA L G WCW26 C LS 110622 DA L G WCW26 C M S 11062 2 DA L G WCW26 C H S 11062 2 entratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 42 7 42 5 43 6 50 2 84 1 42 6 ng/m L VoRecover

y NA NA N C N C 84. 1 ±0.47 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 32
. DA L G WCW26 L 11062 2

3 M LIM S I D GLP10-01-01-18-12 3 GLP10-01-01-18-12 4 GLP10-01-01-18-12 5 GLP1OO1-01-18-12 6 GLP10-01-01-18-12 7 Descriptio n DA L GWCW26 L 011062 2 DA L G WCW26 L D B 11062 2 DA L GWCW26 L LS11062 2 DA L G WCW26 L M S 110622 DA L G WCW26 L H S 110622 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentiatio n (ng/mL ) 64 5 64 4 66 7 72 3 106 0 VoRecover

y N A N A N C N C 84. 2 64 5 ng/m L ±0.16 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Tabl e 33
. DA L G W140 R 11062 2

3 M LIM S I D GLP10-01-01-18-12 8 GLP10-01-01-18-12 9 GLP10-01-01-18-13 0 GLP10-01-01-18-13 1 GLP10-01-01-18-132 Descriptio n DA L GW140 R 011062 2 DA L GW140RD B 11062 2 DA L GW140RL S 110622 DA L GW140 R M S 11062 2 DALGW140RHS11062 2 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 12 7 130 14 1 22 3 56 7 VoRecover

y NA N A N C 95. 7 88. 9 12 9 ng/m L ±2.3 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. 

### Tabl e 34
. DA L G W141 R 11063 0

3 M LIM S I D GLP10-01-01-18-13 5 GLP10-01-01-18-13 6 GLP10-01-01-18-13 7 GLP10-01-01-18-13 8 GLP10-01-01-18-13 9 Descriptio n DA L GW141 R 011063 0 DALG W14 1 RD B 110630 DALGW141RL S 11063 0 DA L GW141 R M S 11063 0 DA L GW141RH S 11063 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 1.59 1.5 7 2.5 0 10. 6 91. 6 VoRecover

y NA NA 93. 4 91. 6 91. 2 1.58 ng/m L ±1.3 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. 

### Tabl e 35
. DA L G W142 R 11062 2

3 M LIM S I D GLP10-01-01-18-14 0 GLP10-01-01-18-14 1 GLP10-01-01-18-142 GLP10-01-01-18-14 3 GLP10-01-01-18-144 Descriptio n DA L GW142 R 011062 2 DA L GW142RD B 110622 DA L GW142RL S 110622 DA L GW142 R M S 11062 2 DA L GW142RH S 11062 2 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 50. 1 51. 4 50. 9 57. 5 144 VoRecover

y N A NA N C N C 94. 5 50. 8 ng/m L ±2.6 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
.

Pag e 2 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1

Tabl e 36
. DA L G W 143 R 11062 2

3 M LIM S I D GLP10-01-01-18-14 5 GLP1001-01-18-14 6 GLP10-01-01-18-14 7 GLP10-01-01-18-14 8 GLP10-01-01-18-14 9 Descriptio n DA L GW143 R 011062 2 DA L GW143RD B 11062 2 DALGW143RL S 11062 2 DA L GW143 R M S 11062 2 DA L GW143RH S 11062 2 Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 23. 3 24. 8 25. 5 33. 1 11 7 VoRecover y

N A N A N C N C 94. 2 24. 1 ng/m L ±6.2 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. Tabl e 37
. DA L G W 144 S 11062 2

3 M LIM S I D GLP10-01-01-18-15 0 GLP10-01-01-18-15 1 GLP10-01-01-18-15 2 GLP10-01-01-18-15 3 GLP10-01-01-18-15 4 Descriptio n DA L GW144 S 011062 8 DA L GW144SD B 11062 8 DA L GW144SL S 11062 8 DA L GW144 S M S 11062 8 DA L GW144SH S 11062 8 Averag e Concentratio n (ng/mL ) ±VoRP D PFO A Concentratio n (ng/mL ) 52. 1 49. 0 51. 2 60. 3 13 8 VoRecover y

N A N A N C N C 88. 6 50. 6 ng/m L ±6.1 % N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. Tabl e 38
. Tri p Blan k 1

3 M LIM S I DIlill999 99555 55CDCDCDCDCD Descriptio n

Tri p Blan k

Se t 1 Sampl e Tri p Blan k

Se t 1 L S Tri p Blan k

Se t 1 M S Tri p Blan k

Se t 1 MH S Tri p Blan k

Se t 1 H S PFO A Concentratio n (ng/mL ) <0.025 0 098 1 10 O 95. 5 49 3 VoRecover y

N A 99. 6 10 2 96. 8 99. 9 N A= Not Applicabl e

Pag e 2 9 o f 7 1

### Tabl e 39
. Tri p Blan k 2

N A= Not Applicabl e 

### Tabl e 40
. Rinseat e Blank s GLP10-01-01 ; Interi m Repor t 1 8 /Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1

3 M LIM S I D GLP1001-01-18-00 1 GLP10-01-01-18-00 2 GLP1001-01-18-00 3 GLP10-01-01-18-00 4 GLP10-01-01-18-00 5 Descriptio n Tri p Blan k

Set 2 Sampl e Tri p Blan k

Set 2 LS Tri p Blan k

Set 2 M S Tri p Blan k

Set 2 MH S Tri p Blan k

Set 2 H S PFOA Concentratio n (ng/mL ) <0.025 0 0.95 4 9.2 9 89. 7 44 3 VoRecover

y N A 96. 9 94. 3 90. 9 89. 8

3 M LIM S I D GLP10-01-01-18-13 3 GLP10-01-01-18-134 Descriptio n DA L GW130LR B 110630 DA L GW133 S RB11063 0 PFOA Concentratio n (ng/mL ) <0.025 0 <0.025 0 VoRecover y N A N A NA = Not/Applicabl e

Pag e 3 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 /Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l methcx i accurac yan d precisio n fo rPFOA

. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein
.

Al l remainin g sample s an d asscx:iate d projec t dat a (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures
.

Attachmen t A : Protoco l Amendmen t 1 8 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d - ETS-8-044. 0

Pag e 3 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 

# 'h4 ^ n^£-2^» ) Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date 

# p9Jf^o^sr^oj / Tllia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yManage r Date

Gar yHohenstein , 3 M Sponso rRepresentative Dat e



# M L Jaisimh a Kesari , Stud yDirecto r jat e

Pag e 3 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 3 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s 

### Analytica l Protocol : GLPi^f-W " ''"" ^

Amendment 1 8



## Stud yTitl e Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m

PROTOCO L AMENDMEN TNO

. 1 8

Amendmen t Date : Jun e 15 , 201 1 Perfonnin g Laborator y 3 M Environmental , Health , an d Safet yOperation s

3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 55144-100 0

laborator yProjec t Identificatio n

GLP10-01-0 1 Samplin g Even t Fomne rSludg e Incorporatio n Are a (FSIA ) Groundwate r

Pag e 1 o f8 Pag e 3 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s 

### Analytica l Protocomp^m'-&h - -""" ^ ^o i i Amendment 1 8 

## Thi s amendmen t modifie s th e foilowin g portio n o fprotocol : "Analysi s o

fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhase 3 Site-Relate d Monitorin g Program "

PROTOCO

L READS : 

### N o change s t o th e wordin g o fth e protoco l ar e required
.

AMEN D T

O READ : 

### N o change s t o th e wordin g o fth e protoco l ar e required
. Thi s amendmen t onl yaddresse s an d document s th e additio n o fth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s a t Decatur , AL , an d conducte d a s par t o fth e 3 M Decatu rPhas e 3 Progra m fo rPFO A(GLP10-01-01)

. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e durin g th e wee k o fJun e 20
. 2011
. Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s project GLP10-01-01-1 8 an d reporte d a s interi m report GLP10-01-01-18 , (reflectin g stud yGLP10-01 - 0 1 an d amendment-18)

.

Reason : 

### Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t t o b e conducte d fo rth e 3 M Decatur , A L facility
. Th e GP O i s fiv e page s i n lengt h an d include d a s attache d t o thi s amendmen t fbmi
.

Pag e 2 o f8 Pag e 3 5 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFOAi n wate rsample s 

### Analytica l Protocoimtf^m^ ' '"" ^ '°^ ' Amendment 1 8 Amendmen t Approva l

^ / 

# mi/ j Jp^Am/'ri Gar yHohenstein , Sponso rRepresentative Dat e 

# 0/, d 'zo/ V Clesto n C

. Lange , Principa l Analytica l Investigato r Dat e


# / S " 

# J 

# c/^' ^ 

# ^O/ / Willia m Reagen , EH S Opn s Environmenta l La b Managemen t



# U/Mv/
. Dat e 

# £/^/i l D6t e Jaisimh a KesafrPt. , DEE , Stud yDirecto r

Pag e 3 o f 8 Pag e 3 6 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 

### Analytica l Protocol : GW10-01-0 1

Amendmen t 1 8 

## Environmenta l Healt h & SafetyOperations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gar

yHohenstein , 3 M EHS&Opn s From : Susa n Wolf , 3 M EHS&Opns ; Environmenta l La b cc : V\/illia m Reagen , 3 M EHS&Opns ; Environmenta l La b

Clesto n Lange , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Date : Jun e 15,201 1 Subject : Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 1 8 - Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r- Jun e 201 1 Samplin g 

## 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xOlsl t Departmen t Numbe r 1 Projec t Schedule/Tes t Date s 3 H Sponso rRepresentativ e GaryHohenstei n 3 M EH S Operation s 3IVI Buildin g 224-5W-0 3 Sain t Paul
. M N 55144-100 0 Phone : (651 ) 737-357 0 Qahohenstein@mmm.co m 3 M Environmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S Opns , Environmenta l 1 aborator y 260-5N-1 7 65 1 733-973 9 wkreaqenP!mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanae@mmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinak@westonsolutions.co m Phone : (334}-332-912 3 QLP1(M)1-01-1 8 Dep t #530711
. Project #002267444 9 Samplin g schedule d fb rth e wee k o fJun e 20,201 1 

### Al l verba l an d writte n correspondenc e wil l b e directe d t o GaryHohenstein
.

Pag e 4 o f8 Pag e 3 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL : Jun e 201 1 

### Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 8 2 Backgroun d informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m thirty-on e groundwate rwell s fo rPerfluorooctanoi cAci d (PFOA ) fro m th e Forme r Sludg e Incorporatio n Are a (FSIA)

. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEP ATSC A Goo d Laborator

yPractic e Standard s 4 0 CF R 792. Groundwate rsample s fro m Decatur
. A L wil l b e collecte d byWesto n Solution s personne l th e wee k o fJun e 20 , 2011
. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFO Aar e o fa know n precisio n an d accuracy . Th e fina l report wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m report GLP10-01-01-18

. 

## 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b y3 M Environmenta l Laborator yfo rsamplin g th e wee k

o fJun e 20 , 2011
. Sampl e bottle s wil l b e shippe d i n cooler s to 3 M Decatu rfo raniva l b yFriday , Jun e 17 , 2011
. Sampl e botdes shoul d b e store d refrigerate d on-sit e unti l sampl e collection
. Marti n Smit h \

Westo n Traile r 3 M Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 

## 4 Tes t Parameter s Th e targete d limi t o fquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFOA

. Atota l ofthirty-on e samplin g location s have bee n specified
. Fo reac h samplin g location , a sample , sampl e duplicat e an d a minimu m o ftw o fiel d mabi xspike s wil l b e collected
. Tabl e 1 indicate s tiie wel l I D an d correspondin g fiel d spike levels
. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e botd e wil l b e 20 0 mL
. Tw o set s oftri p blank

s consistin g o freagent-grad e water , a low-leve l ti p blan k spike , micMeve l fiel d spike , mid-hig h fiel d spike , an d a high-leve l tri p blan k spike wil l b e prepare d at th e 3 M Environmenta l Laborator yan d sen t t o tiie samplin g locatio n witi i tiie othe rbottles
. Two additiona l bottle s wil l b e prepare d t o b e use d fo rth e preparatio n ofth e equipmen t rinseat e blanks
. A1- L containe ro flaborator yreagen t wate rwil l b e provide d fo rth e collectio n o ftine equipmen t rinseat e blanks
. Base d o n th e results fro m previousl ycollecte d sample s fro m th e FSI A{GLP10-01-01-0 7 an d GLP10-01-01-11) , most samplin g location s wil l require dilutio n wiU i laborator yreagen t wate rprio rt o sampl e analysis
. However , samplin g location s identifie d i n Se t 1 ofTabl e 1 are expecte d t o contai n PFOAconcentiratio n <1 0 ng/mL

. Fo r sample s collecte d firo m Uies e samplin g locations , th e sample , sampl e duplicat e an d fiel d mabi xspike s wil l contai n ttie additio n ofintema l standar d Ca-PFO

Aa t a nomina l concentratio n o f1 ng/mL , a s wil l th e tiip blank s samples , tri p blan k

lowspikes , an d tw o equipmen t rinseate blanks
. Th e additiona l o fintema l standard wil l b e use d t o ai d i n th e analysi s oftiie samples
. Atota l o f16 9 sampl e bottle s \N\\ \ b e prepared
.

Pag e 5 o f8 Pag e 3 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s 

### Analytica l Protocompmf-4^'''"' ' ^'' '

Amendmen t 1 8 Tabl e 1
. Samplin g Location s an d Fiel d Matri xSplic e levels
. Set # 1
2
3 4

5 Wel l No
. 1348,1358,136R,137R
. 137S , 137Land138 L 130L
. 1318,131L
. 133R , 135L
. 1368,136L , 141R , 142R , 143 R an d 144 R 130R
. 1308,1338,133L
. 134L , 138R , 1388
. CW26C

. CW26 L an d 140 R 131R
. 134Rand135 R
Tri p Blan k

Set s 1 an d 2 Sampl e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h 

### Spike Cone

. (ng/mL ) 0. 1 1. 0 1 0 1 1 0 10 0 1 0 10 0 50 0 10 0 200 0 1 1 0 10 0 50 0 

## 5 Tes t IMethod s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 0 "Determinatio n o fPerfluorinate d Compound s I n Wate rbyHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Th e dat a qualit yobjective s fo rtiiese studie s are quantitative result s forth e targe t analyte s wit h a n analytica l accurac

yo f100±30%
. Fiel d matri xspike s not yieldin g recoverie s wittii n 100t30 % wil l b e addresse d i n tiie repor

t an d tiie fina l accurac

ystatemen t ma

yb e adjuste d accordingly
. Base d o n th e result s fro m previousl ycollecte d sample s firo m th e FSI A(GLP10^1-01-0 7 an d GLP10-01-01-11) , mos t samplin g tocations wil l require dilutio n wit h laborator yreagen t wate rprio rto sampl e analysi s b yETS-8-044.0

. Fo rsample s containin g intema l stendard : sample s wil l b e analyze d agains t a n intema l standard calibratio n curve . Eac h cun/

e poin t wil l contei n isotopically-labele d perfluorocarisoxyli cacid s an d perfluorosutfoni cacid s a t a nomina l concentiatio n o f1 ng/m L Th e calibratio n curv e wil l b e generate d b ytakin g tiie rati o o ftiie standaix l pea k are a count s ove rth e intema l stendard pea k are a count e to fi t th e dat e fo reac h analyte
. Alternately , sample s ma yb e analyze d b

yETS 8-154. 3 "Determinatio n o fPerfluorinate d Adds , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Exbractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometi yo rETS-8-110. 1 "Metho d o fAnalysi s fo rtiie Detemninatio n o f Perfluorinate d Compound s i n Water , Soi l an d Sedimen t byLC/MS/MS"

. 

### 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contei n th e result s for tiie sample , sampl e duplicate , an d fiel d matiri x spikes
. Tri p blan k

an d tri p blan k

spike s wil l b e reporiie d for tiie samplin g even t a s wil l an yequipment/rinseat e blank s prepare d i n th e field
. Laborator ycontro l spike s o freagen t wate rprepare d a t tiie time o fsampl e preparatio n wil l als o b e reporte d an d use d to evaluat e tiie overal l metiio d accurac yan d precision
. Metiio d blank s o freagen t wate rprepare d at tiie time o fsampl e preparatio n wil l b e use d t o detenriin e tiie metiio d detectio n limi t Fo rthos e samplin g location s where tiie fiek l matri xspik e leve l wa s no t appropriate , du e to highe rtiian expecte d analyt e concentiBtions , a laborator ymatri xspike ma

yb e prepare d an d include d i n tiie fina l report

Pag e 6 o f8 Pag e 3 9 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample

s 

### Analytica l Protocol : GLPi^f-lil " """" ^ Amendment 1 8 

## 7 Emai l Correspondenc e Quarterl yG

Wsamplin g - Decatu rForme rSludg e Incorporatio n Area Well s Young , Charle s T
. to : stwolf@mmm.co m 06/13/201102:1 4 P M Cc : "Frinak , Timoth yR." , "Smith , Martin " Sue : WESTO N wil l b e performin g quarterl ygroundwate rsamplin g o fth e forme rsludg e incorporatio n are a (FSIA ) well s beginnin g o n Jun e 20,2011
. Th e attache d wor d documen t show s th e FSIAwell s (highlighte d i n yellow ) tha t wil l b e sample d fo rfluorochemlca l analyses.unde rGLP 10-01-0 1 an d GLP 10-01-02
. I t als o show s samplin g schedul e fo r othe rquarterl ysamplin g (an d conventiona l parameters ) Ms o attache d i s a spreadshee t summarytabl e fro m th e mos t recen t (Nov-2010 ) roun d a t th e FSIAwells
. I n additio n t o th e primary/dupllcate/spik e bottles , w e wil l nee d bottle s an d Milli- Q wate rfo rth e tw o equipmen t rinseat e blank s tha t wil l b e collected
. Thanks , Charli e Charle s T
. Youn g Technica l Directo r Westo n Solutions , Inc
. 140 0 Westo n Way(5-2 ) Wes t Chester , P

A1938 0 (610 ) 701-378 7 Fa x(610 ) 701-340 1



### Pag e 7 o f8 Page 40 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 

### Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 8 Quarteri yG WMonitorin g Firs t an d Tliir d Quarte rRflonitorin g Progra m 201 L 203L * 204 L 206 L 209 L 211 R 212 R 212 D 213 R 213 S 215 R 215 D

216 R 217 R 217 S 217 D 218 R 218 L 220R * 220L * 221 R 222R * 223 R

225 R 225 L 226 R 226 L 227R * 227L * 228 R 228 L 229 R 229 L 305 R

307 L 308 R 3 1 OR * 311 R 313 R 315 R 317L * 319 L 324L * 325 L 328R *

328L * 330R * 330L * 332 S 335R * 

### 50 1 50 3 50 7 5 1 O R 5 1 O L 511 S 1

512 R 512 L GRS04* ^ RW312R * RW327R * RW331S *

Secon d an d Fourtf i Quarte r(Monitorin g Progra m 201 L 203 L 211 R 212 R 212 D 213 R 213 S 217 R 217 S 217 D

Monitorin g well s u i ( ^ Monitorin g we l (**) Monitorin g w e "On e sampl e Will i analysis
. RWindicat e reoo

\ 

### 218 R 218 L ??2 R 223 R 229 R 229 L 305 R 307 L 313 R 315 R
rillbeanalyredforV swil l b e analyze d f

c U s wil l b e analyze d f 3 e collecte d fro m tin

« 7 well s use d I n a

c 

### 324 L 325 L 332 S 335 R 512 R 512 L 130R* * 130S* * 130L* * 131.R* *

'OC s an d isopropy i ) rPFOA , an d VOC s o rPFOA

. J close d landfiH(SW
:tiva groundwate re

> 

### 131S* * 131L* * 133R* * 1338* * 133L* * 134R* * 134S* * 134L* * 135R* * 135S* * 135L* * ethe rusin g EPAM

e / Isopropy i ethe ru s

MIM ) groundwate r (tractio n systems
. 

### 136R* *

1363* * 136L* * 137R* * 137S* * 137L* * 138R* * 138S* * 138L* * CW26C* * CVV26L* *
»o d ^6 0 unles s o l in g EPAMetiio d 8 2

extractio n syste m f b 

### 140R* * 1

141R* * 142R* * 143R* * 144R* *

[herwiselndk»ted
. SO

.
rVO C an d PFOA



### Pag e 8 o f8 Pag e 4 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


### ATTACHMEN TB : REPRESENTATIV E SAIVIPL E 

### CHROMATOGRAM S AN D CALIBRATIO N CURVE(S )

Pag e 4 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kllOTlSa.rd b
k110715a.rd b (PFOA) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -6.93e+00 3 x* 2 + 1.82e+00 6 x+ 3.65e+00 4 ( r= 0.9998 )

4 5 5 0 5 5 Concentration , ng/m L 10 0 Dat aprinte db y ST

W Printin g Time : 10:17:5 9 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 1 o f 1
Pag e 4 3 o f7 1GLP10-01-01 ; InteriiT i Repoi l 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur
. AL ; Jun e 201 1 Result s Name : kll0715a.rd b

•Sampl e Name:-k110715a020 rSampl e tO;*11003-2&-ia r •PM k Name:'PFOA ' Uaw(e():'413^XXV369.000Da,413.0 ( •Comment-5.0no/mLFCitdkiMaQWWe rAnrtotafcn:' ' Sampl e Index : 3 0 Sampl e Type : Calculate dCone : Acq
. Date : Acq
. Time : Modified : Pcoc
. Algorithm : Hois e Percentag e Standar d 5.0 0 ng/m L 5 . H ng/m L 7/15/201 1 10:28:2 2 P

M Ye s Specif y Paramet e 9 0 Base
. Sub
. Window : 1.0 0 mi n Peak-Split
. Fac t r : 3 Repor t Larges t

Peot : Ye s Min
. Pea k

Heigh t Min
. Pea k

Illdth : Smoothin g Width : R T Hindo« : Us e Relativ e RT : Int
. Type : Retentio nTime : Area : 9 2 Height : Star t Time : En dTime : 0.0 0 cp s 0.0 0 se c 30. 0 se c 15. 4 mi n N o Manua l 15. 4 mi n 715 1 count s .2l6t00 6 cp s 15. 3 mi n 15. 7 mi n 1.20»6 - 1.15*6 - 1.10e6 - 1J)5»6 - IJXM - 9.50e5 - ajXtoS 8.50e5 - SJXJeS 7.50e5 - 7J)0e5 -

' 6.50e5 - exoes 5J0e5 - 5.00e 5 4.50e5 ' 4J00t5 - 3.50*5 - 3.00e5 - 2.50eS ' 2.00a5 - 130e5 - 1.00eS 5.00e4 ' 0.00 - 13 5 14. 5 15. 0 15. 5 16. 0 

# I SHnpteName:-V110715a029 - Sampl a ID : "Solven t Blani rFUe:-k110715a.wi r P«a k Name : TFOA ' MaM(et) : "413.000/369.00 0 D a ,413.000219.00 0 01,413.000/ 1 G9.00 0 Oa " Comment:-MliQWaterTN11-0234 ' Arvtotsfion: ' Sampl e Index : 2 9 Sampl e Type : Unknow n Concentration : N/A Cal c Acq
. Acq
. ulate dCone : Dat e Tim e Modified : Pro c Bas e Pea k Rep o Min
. Min
. Al g rithm : Percentag e Su b -Spl i t La Pea k Pea k Smoothin g R T Windo w Exp e Us e Int
. Ket e < 0 7/16/201 1 1:39:1 3 A

M N o Specif y P a 9 0 Window : 1.0 0

- Factor : 3 qes t Peak : Ye s Heigh t Width : Width : :t6 dRT : lela t Typ e itio n Height : Sta r v e RT :

Time : En dTime : 0.0 0 0.0 0 0 30. 0 15- 7 n N o Bas e T o B a 15. 5 541 5 co' j .536*00 3 15. 5 15. 6 n



# [ Sampl e Name : 1(1107158030 ' Sampl e ID : 'LCS-110714-1 - File : 'V1107lSa.Vi4 r P«« k Name : 'PFOA ' Hau(e«) : -413.00(V3e9.00 0 03,413.000/219.00 0 O a ,413.000^69.00 0 Da Commen t 'D.Spp b LCS " Annotation:" " lampl t Index : 3 0 

# I Sanipl e Name : 1(110715a03 TSampl e ID : "LCS-110714 - Pea k Name : -PFQA " Ma««<e«) : "413.00Cra69.00 0 D8.413. a Comment:-Spp b LCS Concentiati c Calculate dt Acq
. Date : Acq
. Time : Modified : Ptoc
. Algo r Nois e Perce i n : 0.49 8

one ; O.51 0 7/16/201 1 1:59:1 8 A

M Ve s thm : Specif y P a tage : 9 0 Base
. Sub
. Window : 1.0 0 Peak-Split
. Repor t Larg i Min
. Pea k

H e raetor : i S t Peak : Ye s i^ht : 0.0 0 Min
. Pea k

Hidth : 0.0 0 Smoothin g W

; R T Hindow : Expecte dR

T Us e Relativ e !nt
. Type : Retentio nT : Area : Height : Star t Time : dth : 0

30. 0 ng/m L

ng/m L

amet e mi n c p s

15. 5 mi n RT : N o Bas e T o B a e (16 : 15. 5 mi n 96387 9 co u 1.38etO0 5 cp s 15. 3 n i n Concentiati o Calculate dC Acq
. Date : Acq
. Time : Modified : Proc
. Algoc i Nois e Perce r 1.9 6 5.1 6 7/16/201 1 3:02:3 8 A

M N ^ Specif y Pa r 9 0 Base
. Sub
. Window : 1.0 0 Peak-Split
. Repor t Larg e Min
. Pea k

He •ac t r : 3 S t Peak : Ye s qh r Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e Int
. Type : Retentio nT i Height : Star t Time : En dTime : KT : 0.0 0 0.0 0 0 30. 0 ; 15. 7 m N o Valle y 15. 4 n 925207 7 eou n .27e+00 6 c 15- 3 n 15. 7 m ng/m L

ig/m L

c p s p o

. n

. n : s p a i n i n

13 ^ 13. 5 14. 0 125e6 ' 120e6 ' 1.15o 6 1-10e 6 1.05e 6 1.00e 6 9.50e 5 9-0Oe 5 8-50e 5 8.00e 5 7.50e 5

. 7.00B 5 : 6.50e 5 6.00e 5 550e 5 5-00* 5 4.50e 5 4XX)e 5 3.50e 5 3.00a 5 2-50e 5 2.00e 5 1.50e 5 1.000 5 5J)0e 4 0.0 0 •-t^4BMi^>i*NMm>ipl*- ^ 14. 5 15. 0 15 5 16. 0 16. 5 17. 0 17. 5 18. 0 Dat a printe d b

yST W Printing Time : 10:27:3 5 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 1 o f 1 0
Pag e 4 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 *ETS-Kir k Result s Name : kll0715a.rd b

I SatnplaNanw:'V110715a03t rSamft e ID:-LCS-110714- rRle:*V110715a.M« r I PeakNaiTM:-PFOA - Ma««<e«):-413.000/369.000Da,413.00Qr219J]CODa,413.00(V169.000Da I Comment-SOpt ^

LCS ' Sampl e IndcK : 3 6 Sampl e Type : Q C Concentcation : 29. 9 Calculate dCone : 28. 3 Acq
. Date : 7/16/201 1 Acq
. Time : 4:06:0 3 A M Modified : Ye s Pcoc
. Algorithm : Specif y P a Uois e Percentage : 9 0 Base
. Sub
. Window : 1.0 0 Peak-Split
. Factor : 2 Repor t Larges t

Peak : Ye s Min
. Pea k

Height : O.O

C Min
. Pea k

Width : O.O

C Smoothin g Width : 0 R T Window : 30. 0 Expecte dRT : 15. 7 Us 6 Relativ e RT : H o Int
. Type : Manua l Retentio nTime : 15. 5 ng/nl
. ng/m L

lamet e mi n
c p s

al n Area : ^605392 7 count s Height : S.84e*00 6 Star t Time : 15. 3 En dTime : lo. O c p s Di n mi n

13 5 14. 0 15. 0 15. 5 16. 0 16. 5 1 ' l o 17. 5 

# I Sampl e Name : 1(110715a04 r S«mpl B ID : TCS-110714-10 " Fie : 1(110715a.wH T Pea k Hame : TFOA " Haas(M) : "413.000/369.00 0 O a.413.000/219.00 0 D a,413.000/169.00 0 Da ' Comment:-0.5pp b LC S ECF

- Annolatlon:" " Sampl e Index : t 3 Sampl e Type : Q C Concentration : 0. 4 9 8 ng/m L Calculate dCone ; 0.52 2 ng/m L Acq
. Date : 7/16/201 1 Acq
. Time : 6:31:0 1 A M Modified : Perr : :entage :

. Hindow : Ye s

9 0 Peak-Split
. Factor : 3 Repior t Larges t

Peak ; Y

i Min
. Pea k

Height : 0
. Min
. Pea hWidth : 0
. Smoothin g Width : 0 R T Window : 30. 0 Expecte dRT : 15, 7 Us e Relativ e RT : N o Retentio n1 Height : Manu ;



# I Satrtil e Name : "k110715a046 rSampl e IO:-LCS-110714-13 ' Fie : ''I(1107l5a.w4 r Pea k Name : "PFOA " Mattes) : '413.000/369.00 0 Da,413.000/219.00 0 Da,413.000/169.00 0 Da " Comment'5pp b LC S EC rAnnotatton: - Sampl e Index : 4 6 Sampl e Type : O C Concentration : 4.9 9 ng/m Li rawR Calculate dCone : 4.9 6 ng/m L'•'~~ ' 9.50eS

9.00e5

- 5 - M Q II I 8.50e5

-

8.00e5

- 7.50e5

-
^' = 7.00e5

-

6.50e5

- 6.00e5

- I 5.50e5

- f5.00o5 - 4.00e 5 3.50 ^ 3.00e S 2-50* 5 2.00e 5 1.50e 5 1-00* 5 5.00 M 0.0 0 

# I Sampl e Name : "k l 107l5a049 - Samit e ID : "LCS-110714-16 " Fie : -fc110715a.st« r Pea k Name : TR3A " MaM(e«) : '413.000/369.00 0 Da,413.000/319.00 0 Da .413.00^169.00 0 Da ' Comment : '30pp b LC S EC P Amotation : ~ Sampl e Index : 4 9 Sampl e Type : Q C
Acq
. Mod i Pro c Bas e Pea k Min
. Min
. Smo o R T W Dat e Tim e led : Algorith m Su b Wind o 7/16/201 1

7:3 7 Y
Split
. Factor : t Larges t

Peak : Pea k Pea k hin g ndo w Hcigh i Hidt h Widt h Expecte dRT : Us e Rela c Int
. Retentio n Are a Height : v e R

T Tlmt, : 8 ) 2 6 A

M 

### ^ t V P a 9 0 1.0 0 3 Ye s 0.0 0 0.0 0 0
N o Ma n a i 15. 5 9B04 7 1.02 e 00 6 Concentration : Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentage : Base
. Sub

- Hindoi
. Peak-Split
. Fact o Min
. Pea k

Height : Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : L's e Relativ e RT : Int
. Type : Retentio nTime : Area : 50 2 Height : 5 Star t Time : En dTime : 29. 9 ng/m L 31. 3 ng/m L 7/16/201 1 8:40:4 6 A

M Ye s Specif y Paramet e 9 0 1.0 0 mi n a k : Ye s 0.0 0 cp s 0.0 0 se c 0 p o 30. 0 se c 15. 7 mi n N o Manua l 15- 5 rain 1700 5 count s 39e^00 6 cp s IS. O mi n 16. 0 mi n

15. 0 15. 5 16. 0 16. 5 17. 0 17 5 14. 5 15. 0 15. 5 16. 0 16- 5 17. 0 17. 5 18. 0 Dat aprinte db y ST

W Printing Time : 10:27:3 5 A M Printin g Date : Tuesday , Augus t 23 , Pag e 2 o f 1 0

Pag e 4 5 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur
. AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# I Sampt o Name : 1(1107158185 " Sampt o ID:"GLP1CW)1-01-ie-093 " FUB : "k110715a.»« r PaakNaiM:'PFQA ' Mats(M):"413.00(V369.000Da.413.000/219.000Da,413.00(yi69.000Da ' Commen t "DA L G W137 5 0110624 ' Annotation: " Sampl e Index : IBS Sampl e Type : Unknow n Concentration : H/ A Calculate dCone : Acq
. Date : Acq
. Tin* : Modified : Proc
. Algorithm : Nois e Percentag e 0.28 4

7/18/201 1 8:35:0 5 A M Ye s Specif y P a 9 0 Base , Sub , Window : 1.0 0 Peak-Split
. Factor : 3 Repor t Larges t Peak : Y«

9 Min
. Pea k Heigh t Min
. Pea k width : Smoothin g Width: R T Window ; Expecte dRT : Use Relativ e RT: Int
. Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 15. 5 n N o Bas e T o B a IS. ED Area : 55387 6 cou Height : Star t Time : En dTime : .21e«0O4

15- 2 n 15- 6 B 

# I San4)leName:*k110715a194^ SamplalD:"OLP1(>O1-01-1M}98 - Fle:'k1l0715a.wH r Pea k Name : "PFOA ' MaH(ea) : "413.000/369.00 0 D a ,413.000/219.00 0 D a ,413.000/169X0 0 Da " Comment:-DALGUV137L0l10e2 rArwwtatkin; " Sampl e Index : 19 4 Sampl e Type : Unknow n Calculate d Cone : 0.37 2 ng/m L Acq
. Date : 7/18/201 1 Acq
. Time : 11:16:1 4 A M )ifie < Proc
. Algorithm : Hois e Per Baae
. Su b Peak-Spl l entag e

. Fac t Specif

y 9 0 Param e

- : 1.0 0 m St : 4 Report Larges t Peah : Yes Min
. Pea k Hln
. Pea k Smoothin g R T Windo w Heigh t Width : Width : Expecte dRT : Us e Rela t Int
. Typ e Retentio n Area : Height : Star t Tlm i En dTime : v e RT : Time : 0

0 0 30. 0 15. 4 N o Bas e T o 15. 4 396 B 0 0 c 0 0 a mi n Bas e ount s ;.90e-f004 cp s 15. 2 15. 6 mi n tec s -

e c 9.0 M 8.5e4 ' 8.0e4 ' 7.5e4

- 7.0e 4 6.5e 4 e.0» 4 5.5e 4 5.0» 4 4.5e4 ' 4.0e4 ' 3.5e 4 3.0 M 2,5M ' 2.0e4 ' 1.5e 4 1.0e4

- 5000.0

- o.oV>*4(«f«««! ^ 13. 0 13 5 

# I Sampt o Namo : 'kl1071Sa20 rSampl e ID : "OLP1001-01-18-108^ FUe : 'V1107l5a.wH r Pea k Name:"PFOA - Mata<e«):"413.00(y369.000Da,413.00Q/219JX»Da,413.00(Vl69.000Da Comment-DA L GW138 L 0110630 " Amotatfan:" " Satnpl e Index : 20 8 Sampl e Type : Unknow n Concentration : N/ A Calculate d Cone : 0.89 1 ng/m L Acq
. Date : 7/ie/;01 ] Acq
. Mod i Pto c Hol s Bas e Pea k Tim e led : Algorithm : Pe r Su b Spl l Wind

o

. Fac t 4:4 3

Y « Spe c Repor t Larges t Peak : Pea k Pea k Smoothin g R T Hindo w Exp e Us e Int
. Ret e Area Heigh t

Width: Width: ,te dRT: -.ela t Type tlo n Height : Sta t v e RT:

Time : 1 4 4

f Y 9 0 P M
P a 1.0 0 3 Y 

### < ' f > f >

. 4 N o Bas e 1 165S909 Time : En dTime : .04e ^ 1 T o

. 4 s D O 0 0

B a 00 5

. 6 

# I Sampt o Name:'k110715al99 " Sampl e ID:N3LP1OO1-01-18-103 ' Fle:-k1107lSa.wt r Pea k Name : TFOA " MaM(ea) : '413.OOCV369.000 Da.4 l 3.000319.00 0 Da.413.000/169.00 0 Da Commen t "DA L OWISS R 011063 0 (d l 1:10) " AnnotBtkin : " ^ Sample Index : 19 9 Sample Type : Unknow n Concentration : H/ A Calculate dCone : 294
. ng/m L Acq
. Date : 7/19/201 1 Acq
. Time : 1:32:3 0 P M Proc

- Al g Noise Per Base
. Su b Peak-Spl l Report L a Min
. Pea k Min
. Pea k Smoothin g R T Windo w rith m entag ' Wind c Spe c

. Factor : ges t Heigh Widt h Widt h Expecte dRT : Use Rela t Int
. Type Retentio n Area : Height : v e R

T Time : eak :

3 0 1 f Y 9 0 P a 1.0 0 4 0 0 0 0

. 4 N o Bas e 1 475836 9 Star t Time : En dTime : 5.33e * 1 T o

. 4 0 0

. 0 0 0 o n

B a

13. 0 13 J 19. 0 10. 5 17. 0 17. 5 Dat aprinte db y ST

W Printin g Time : 10:27:3 5 fiM Printin g Date ; Tuesday , Augus t 23 , Pag e 3 o f 1 0
Pag e 4 6 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# TM Sampl e Name:'V110715a139 ' San^t o ID:'OLP10«1-O1<l8.05g " File:VI107l5a.vri r Pea k Name : "PFOA " Ma«a{e«) : '413.000369.00 0 Da,413.000/219.00 0 Da,413.000/169.00 0 Da ' Comment:"OALGW134S011062G rAnnotation: ' Sampl e !nde>r : 13 9 Sampl e Type : Unknow n Concentration : N/ A 4Je5

- Calculate dCone : 9.o 7 ng/m L Acq
. Date : 7/17/;01 1 4.0o5

- Acq
. Time : 4:ZZ:1 6 P M 3.8e5 - 3.605

- 3.4*5

- 3.205

- 3.0e5

- 2.8e5

- 2.6e5

- 2.4e5

- I 2.0e5

- I 1Ae5 - 1.6«5

- 1.4e5

- 1.2e 5 1-0e 5 8.0e4 ' e.0e4 ' 4.0e4 ' Z0e 4 

# I T

Modl f Ptoc
. (Jols e Bare
. Peak R e po r Min
. Min
. led :

A l g P e r <;pl i

- U =pa k Smoothin g R TW l E xpe c Y

srlthm : Spe c entage : Window :

. Facto r ges t Pe a Height : Width : Width : ;e d RT : Us e Rela t Int
. Rete i Area : Heig h Sta n En d T Typ e Lio n v e RT : B Time : 353 5 4
. Time : ine : 

### :

1 0 1 q I V 9 0 Parameter s - 1.0 0 n Y e s 0 0 0

. 4 H o
s e T o 15. 4 9 3 0 0

0 0

m i n Bas e m i n 6e-t00 S cp s 1 1 - 1

. 6 m i n m i n n
p s point s

0. 0 13. 0 13. 5 14. 5 15. 0 15 5 lOiM,

. 

# I SaiTpleName:"k1l0715a08S rSampl e ID:"GLI»HM1-01-1W12S " Flte:"k110715».w W Pea k Name : 'PFOA " MaM(M) : "413.000/369.00 0 Da.413.000/219.00 0 Da.413.000^69.00 0 Da " Conment*DAL0W131 S 011062 2 (dl t 1:10) - 5ampleName:lc1107l5a076 " Sampt o ID:-OLP1OO1-D1-18-0l6 rne:'kll0715a.Mi r Pea k Name : TFOA ' MaM(o«} : "413-000/369.00 0 D a .413.000^19.00 0 Da.413.000/16S.00 0 Da " Comment:'DALGWl30L0110S30(dil1:10 rAmwtatkin:" " Sampl e Index : 7 6 Sampl e Type : Unknow n Concentcation : N/ A Calculate dCone : 66. 8 ng/m L Acq
. Date : 7/16/201 1 Acq

- Time : 6:1 1 :2 6 P M
Percentage : Sub

. Wind ! Nols i Bas e Peak-Split
. Facto i Repor t Larges t

Pe : Min
. Pea k

Height : Min
. Pea k

width : Smoothin g width : R TWindow : Expecte dRT : Us e Relativ e RT : Int
. Type : E

: Specif yParamet E

. .39e+00 6 cp s 15. B mi n 1.4e6 ' 1.3e6 ' 1.3e6 ' 1.2e6

- 1-2e6

- 1.1e6

- 1.1e6

- 1.0»6

- 9.5e5

- 9.0e5

- e.5e5

- 6.0e 5 7.5e5

- 7.0e5

- 6.5e5

- 6.0e5

- S.5e5

- 5.0e5

- 4.5e5

- 4.0e5

- 3.5e5

- 3.0B5

- 2.505

- 2.0e5

- 1.5e5

- I.OeS

13. 0 13. 5 

# I SanvleHame:"k1107lSa098 rSampt o ID:-OLPlOO1-01-1&«30 ^ Fle:'kl10715a.wif r PM k N<me : 'PFOA " MaM(et) ; "413.000^69.00 0 Da.413.000/219.00 0 Da,413.000/169.00 0 Da " Commert:"DALGW131L0110622{dai:10 r" - Sampl e Index : 9 8 Sampl e Type : H/ A Ai:q
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentag e Base
. Sub
. Wind o Peak-Split
. Fac t 7/16/;01 1 10:4S:2 7 P

M Ye s Specif y Pa r 9 0 : 1.0 0 t : 3 Repor t Larges t

Peak : Ye s Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Hindow : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 s 15. 7 m N o Manua l 15. 4 m Area : 100642 9 cou n Height : Star t Time : En dTime : -21e-f00 5 C F 15. 1 m 15. 6 m 120e 5 1.15e 5 1.10e 5 1.05e 5 1.00e5

- 9.50ft4 9.00e4 ' 850e4 ' a00e 4 7-50*4

- 7JX>e4

- 6.50e4

- 6.00e4

- 5.50*4

- 5.00*4

- 450*4

- 4.00e 4 3.50* 4 3.00* 4 2.50* 4 2.00e 4 1.50 M Sampl e Type : Concentl a Ion : Calculate dCone : Acq
. Oat e Acq
. Tim e Modified : Proc
. Algorithm : Nois e Pe r Base
. Su b Peak-Spl l Re|)or t La Min
. Pea k Min
. Pea k Smoothin g R T Windo w entag e Unknow n H/A S3. 9 7/17/2 0 1:55:5 6 Ye s Specif y 9 0 A M
P a Window : 1.0 0

. Fac t 3 t : 4 ges t Peak : Y Heigh t Width : Width : Expecte dRT : l's e Rela t Int
. Typ e Retentio n Area : Height : Star t Ti m En dTime : v e RT :

Time : 0

0 0 30. 0 15. 4 N o Bas e T o 15. 4 1654B64 3 .87e*0 0 15. 1 15. 9 0 0 0 0

Ba s 1.1*6

- 1.0e6

-

7.0* 5 6.0e 5 5.0* 5 4.0* 5 3.0B 5 Z0* S 1.0* 5
15. 0 15 5 16. 0 16- 5 17. 0 17 5 Dat a printe d b

yST W Printing Time : 10:27:3 5 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 4 o f 1 0
Pag e 4 7 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# I San^Nam:-k110715a1i rSampl e IO:-GLP1(M)1-01-1MH5 - FilB:"1c110715a
. PM k NanM : -PFOA - MaM(«a) : '413.000/369.00 0 Da.413.OaQr219.0OO Oa.413.00Wie9.00 0 Da ' Cotim«*-nALGW133R0110630(dfl1:10) " - Sampl e Index : Sampl e Type : Calculate dCone : Acq
. Date : Acq

- Tin« : Modified : Proc
. Algorithm : Nois e Percentag e Base
. Sub
. Wind c Peak-Split
. Fac t Repor t Larges t

P Min
. Pea k

Heigh t Mlh
. Pea k

Width : Smoothin g Width : R T Window : Elxpecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 11 7 Unknow n N/ A loe
. 7/17/201 1 8:36:5 5 A

M Ye s Specif y P a 9 0 i : 1.0 0 o r : 3 ,ak : Ye s : 0.0 0

0.0 0 30. 0 15. 4 n N o Bas e T o B a 15. 4 1 Area : 1B89092 5 c o Height : Star t Time : En dTime : 2.10et00 6 15. 1 J 15. 8 a

13. 0 13- 5 14. 5 15- 0 15. 5 KJ O IB S 17. 0 17. 5 

# I Sampl e Name : •V110715a112 ' Sampl e ID:'0LP1OO1-01-1ftO4Q ^ Fae:-k110715a.wt r Pea k Name : "PFOA - Mae«(es):-413XXXV369.00 0 O a ,413.000219.00 0 Da,413.00CV1Ga.0O O Da " Comment:"DALGW133S0110630(dil1:10) " Amotatton: - Sampl e Index : 11 2 Sampl e Typ e Cal c Acq
. Acq

l ate dCon e Date : Time : Modlfled : Pro c Noi s Bas e Pea k Rep o Min
. Algor
. Perce n th m tag e Unknow n 7 b N/ A 311
. 17/2 0 51:4 9 Ye s Specif y Sub
. Window : Split
. t Larg i Pea k H I Pea k H Smoothin g H R T Window : Expecte dR

T Fac i 3 t Pe a Igh ' d t h d t h 9 0 1

A M
P a 1.0 0 3 : Ye s 0 0 0 30. 0 15. 4 0 0 0 0

13. 0 13- 5 14. 5 15. 0 15- 5 16- 0 16 5 17. 0 ^^ S 

# I Sanv)le^ame:'Vl10715a13O ' Sampl e ID:'OLP10«1.«1-1»4)54

- Fae:-k110715a.viir r Pea k Name : "PFOA

- liAaM(e() : -413-000^369.00 0 Da,413.000219.00 0 D a,413.000/169.00 0 Da ' Comment:-DALQW134L0110628(diI1:10}

- Amotatkm:* " Sampl e Index : 13 0 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 527
. ng/m L Acq
. Date : 7/17/201 1 Acq
. Time : 1:12:2 7 P M 

# I SanpleName:i(1107lSal03 rSampl e ID:-GL P 1001-01-18-035 " FUe:-k1l0715a.wH r Pea k Name:'PFOA ' MaM(e*):'413.0DtV369.000Oa,413.000/219.0O 0 Da,413.00CV169.00 0 Da Commen t "DALGWl33L0110630{d l 1:10) " - Sainpl e Index : 10 3 Sampl e Type : N/ A Calculate dCone : A^q
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentage : Base
. Sub
. Wlndo i Peak-Split
. Fact o Repor t Larges t

P ( Min
. Pea k

Height : Min
. Pea k

Width : Smoothin g Width : R T window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 230
. 7/17/201 1 :':42:0 1 A

M Ye s Specif y P a 9 0 : 1.0 0 r : 4 a k : Ye s 0 30. 0 15. 4 n N o Manua l 15. 4 1 Area : 826047 3 co u Height : £ Star t Time : En dTime : . 4 9e-f00 5 15. 0 n 15. 7 n ng/m L 9.0*5

- 8.5*5

- 8.0eS ' 7.5*5

- 7.0*5

- 6.5*5

- 6.0*5

- 53*5

- 5.0e5

- 4.5e5

- 4.0e5

- 3.5*5

- 3.0*5

- 2.5*5

- 2.0e5

- 1-5e 5 1.0e5 ' 5.0e4

- 0.0

- Modified : Proc
. Algorithm : Nois e Pe r Base
. Su b Peak-Spl l Reiior t La Min
. Pea k Min
. Pea k Smoothin g . Wind c Ye s Specif y P a

: . Facto r rgas t Pe a Heigh t Width : Width : iT : Us e Relativ e RT : Int
. Typ e Retentio n Area : Height : Star t Ti m En dTime : Time :

I B 9 0

1.0 0 4 : Ye s 0.0 0 0.0 0 0 30. 0 15. 1 n N o Bas e T o B a 7



### - 15. 4 4 2 2 C

O 6e-^00 6 15. 0 D 15. 9 n

fcjl'l ',1, 1 iii|i|i|,il|IMiHlli(i|i | HH , , 14 5 15. 0 15. 5 la O 16. 5 17. 0 17. 5 Dat aprinte db y ST

W Printing Time : 10:27:3 5 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 5 o f 1 0
Pag e 4 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# ( Sampl e Name : 'Vt10715a18ff ' Sampl e ID : "GLPl&01-01-18-08tf - File : -k1l0715a.viilr r Pea k Nam* : "PFOA " Ma*a<as) : "413.000/369.00 0 Oa.413.000/219-00 0 Da,413.000/169.00 0 Da " CorTnMnt-DALGW136S011063D<<ai1:10) " Annotation: ' Sampl

. " Sampl e Type : Ur,kn <

im : Specif y Paramet *
Repor t Larges t

Peak : Ye : Min
. Pea k

Height : O. t Min
. Pea k

Width : O. C Smoothin g Width : 0 R T Window : 30. 0 Expecte dRT : 15, 4 Us e Relativ e RT : N o Retentio nTime : 15. 4 Area : 2265304 7 ; Height : 2,o2o-t00 6 Star t Time : 15. 0 En dTime : 15. 0 

# I Sampl e Name:'Tc110715a171 " Sampl e ID:-GLP1WI1*1.1W)84 " Fle:-k110715a.wM r Pea k Name : "PFOA " M&*s(e*) : "413.000/369.00 0 D a ,413.000/219.00 0 D a .413.000/169.00 0 Da " Commert:"DALGW136L0110630{dai:10) - AnnotaOon: "

3.4*5 - 3.2*5 - 3.0*5 - 2.8*5 - 2.GeS ' 2.4* 5 2.2e 5 2.0eS 1.ee5 - 1.6*5 - 1.4*5 - 1.2*5 - 1.0*5 - 8.0*4 - 6-0e4 - 4.0*4 - 2.0*4 - Sampl e Type : Concentration : Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e fercentag e Unknow n N/ A 79. 7 7/ia/201 1 3:39:4 7 A

H Ye s Specif y P a 9 0 Base
. Sub
. Window : 1.0 0 Peak-Split

- Factor : 3 Repor t Larges t

PeaK : Ye s Hin
. P«al c Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 lS- 7 i ; N o Manua l 15. 4 1 Area : Z92501 S co u Height : Star t Time : En dTime : .4ee-tOO S 15. 1 n 15. 6 D 

# i

13. 5 ^.,t,m,0mtmiimmmf m ^^MMIMV^ ^ 

# I Sampl e Name : •V1107l5a2l3 fSampl e ID ; "QIP1&01-01-18-113 - Rle:1(110715a.wt r Pea k Name : "PFOA " Mat«(e«) : '413.000/369.00 0 Da.413.000/219JX) 0 Da.413-00(V169.00 0 Da ' Commert"DALGW138S0110630(dil1:lO) " Annotatton: - Sampl e Index : 21 3 

# I SanvleName:"k110715a22 rSamplBlD:-GlPl(W)l-01-l8-1i rFl*:"k1l0715a.vi*f r Pea k Name : TFOA ' hlaM(e() : "413-000/369.00 0 Da.4l3.00(V219.00 0 Da,413.000/169.000D« " Camnient"OALGWCW26C0110622{dai:l0) " Amotatkm: - Sampl e Index : 22 2 Sampl e Type : Concentration : Calculate dCone : Acq
. Time : Kodllled : Proc
. Algorithm : Nois e Percentag e H/ A 155
. 7/18/201 1 6:30:0 4 P

M Ye « Specif y P a : 9 0 Base
. Sub
. Window : 1.0 0 Peak-Split
. Fac l Repor t Larges t

1 Hln
. Pea k

Heigh t Min
. Pea k

Hidth : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : o r : 3

lak : Ye s : 0.0 0

0.0 0 0 30. 0 15. 4 N o Bas e T o B a 15. 4 D Area : 560 4 33 7 co u Height : Star t Time : En dTime : 7.07e*OO 5 15. 1 n 15. 7 r

. N/A Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc

- Algorithm : Hois e Percentag e 4 27
. 7/18/201 1 &:40:1 9 P Ye s ng/m L

Specif y Paramet e 9 0 Base

- Sub
. Window : 1.0 0 Peak-Split
. Fac t r : 4 ReiMc t Larges t

Peak : Ye s Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : L's e Relativ e RT : Int
. Type : Retentio nTime : mi n 0.0 0 cp s 0.0 0 se c 0 30. 0 15- 4 N o Manua l 15. 4 Area : 1508764 1 c Height : Star t Time : En dTime : .89e*00 6 15. 0 IS. a cp s

mi n 1.8* 6 1.7* 6 1.6*6

- 1.5*6

- 1.4*6

- 1.3ee < 1.2e 6 1.1e6

- 1.0e6

- 9.0*5

- 8.0*5

- 7.0*5

- 6-0*5

- 5.De5

- 4.0*5

- 3.0*5

- 2.0*5

- 1.0*5

- 0. 0 14 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b

yST W Printing Time : 10:27:3 6 A M Printin g Date : Tuesday , Augus t 23 , Pag e 6 o f 1 0

Pag e 4 9 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# TSarTpleNBme:'k110715a22 r Sampl e ID : "OLP1O4)1-01-18-123 * FUe:-k110715a.wtf r Pea k Name : 'PFOA " Ma*a<ae) : '413.000/369.00 0 Da,413.000/219.00 0 Da,413.00(V169.00 0 Da " Co(Tvnent"DALGWCVV26L0110622(<lM:10) " AnwtalNn : ~ Sampl e Indei-. : 22 7 Sampl e Type : Unknow n N/ A Calculate dL Acq
. Time :

Peak-Split
. Facto i Repor t Larges t

Pe ; Min
. Pea k

Height : Min
. Pea k

Width : Smoothin g Width : R T Window : Elxpecte dRT ; Vst , Relativ e RT : Int
. Type : Retentio nTime : Area : 223 ! Height : 2
. leter s - M Q II I



# I S«[TpleN«m*:Tcl107l5b24 r Sampl e ID : "GLPIOOWI-IS-ISS " Hle:'V110715a.wii« r Pea k Name : "PFOA " MaM(e«) : "413.000/369.00 0 Da.413.000/219-00 0 Da,41S-OOIVI69.00 0 Da ' CornnenfOALOWUIROlloeao r Aimotatton:" " Sampl e Index : 25 1 

# I Sampl e Name:'V110715a23ff

- SamplalD:"GLJ>l(M)1-01-18-128

- Fle:"k110715a.w4 r Pea k Nam* : TFOA " Maea(e«) : "413.000/369.00 0 D a,413.000/219.00 0 D a,413.000/169.00 0 Da ' Comment:"DALGWl40R0110622(dl1:10 r Annotatk>n: ~ Sampl e Inde.-i : 23 6 Sampl e Typ e Cone
. ratlo i N/ A Cal c Acq
. Acq
. lat e Oat e Tim e Modified : Pto c Nol s Bas e Pea k Rep o Min
. Min
. i Con e
Algorith m Pe r Su b Spl i enta g Win e

- Fa c t Larges t Pea k Pea k Smoothin g R T W Exp e ndo w Heig h

Widt h Widt h t e dRT : Us e Rela t Int
. Ret e Are a Tvp e Height : Sta r v e R

T Time : : 127
.

7/19/201 1 3:16:5 1 A

M Ye s Specif y P a r : 9 0 ow : 1.0 0 'eak : Ye s

0.0 0 0 30. 0 15. 1 n N o Valle y 15. 4 n 46044B 7 cou r Time : En dTime : 5.e6e-t00 5 15. 1 1 15. 6 n

1^. 0 15. 5 16. 0 16 5 ^^s i 17 5 Sampl e Name : 'Vl10715b2S r Sampl e ID : "OL P10^1-01-18-140 " Pie : 'k110715a.Jr r Pea k Nam* : TFOA ' lite«s(ea) : "413.000/369.00 0 Oa.413.00CU219.00 0 Da,413.000/169.00 0 Da

Commen t

"DALG W142R 0 11062 2 (d l 1:10) ' Amotatkin:- " Sampl e '

. Sampl e Type : Calculate dCone
. Acq
. Time : Modified : Proc
. Algorithm

Nois e Percentag
. Unknow n H/A 1.5 9 ng / 7/19/:01 1 10:07:2 7 A

M Ye s Specif y Param e : 9 0 Base
. Sub
. Window : 1.0 0 m i Peak-Split

- Fac l Repor t Larges t

1 Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : o r : 3

eak : Ye s : 0.0 0 c

0.0 0 s 0 30. 0 se c 15. 4 mi n N o Manua l 15. 4 mi n Sampl e Type : Unkf Concentration : Calculate dCone : N/ A 50. 1 n Acq
. Date : 7/19/201 1 Acq
. Time : 1 Modified : ;53:1 7 A M Ye s Proc

- Algcrithro : Specif y Par a Nois e Percentage : Base
. Sub
. Window : Peak-Split
. Facto r Repor t Larges t

Pe a Min
. Peaf
. Height : Min
. Pea k

Width : Smoothin g Width : R T Window ; Expecte dRT : Us e Relativ e RT : int
. Type : B Retentio nTime : Area : 185 7 Height : 2
. Star t Time : En dTime : 9 0 1.0 0 4 : Ye s 0.0 0 0 30. 0 s e 15- 4 in l N o s e T o Bas e 15- 4 m l 7 8 coun t le-tOO S c p 15- 1 m l 15. 6 m l 2.4* 5 2.3*5

- 2.2e5

- 2.1e S 2.0e5

- 1.9*5

- 1.8*5

- 1.7*5

- 1.6*5

- 1.5*5

- 1.4*5

- 1.3e5

- 1.2e5

- l.leS

1.0*5

- 9.0*4

- 8.0*4

- 7.0*4

- 6.0*4

- 5.0*4

- 4.0*4

- 3.0*4

- 2.0*4

- 1.0*4

- m^t^mlttfi^Sia^af i 'e;7 3 17.0 6 17.39.^175 1

Dat aprinte db y ST

W Printin g Time : 10:27:3 6 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 7 o f 1 0
Pag e 5 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# n SanvI a Name : "^107151)261 - Sanqil e ID:-GLP1(V01-O1-18-14 rFUe : "k110715a.vri r Pea k Name : "PFOA " Ma**<**) : "413.000i369.00 0 Da.413.0O0i/219.0OODa.413.O0CV169.00O Da ' ConvtMrt:"OALGW143ROll0622<dil1:10 rAnnotatkm ; Sampl e Type : Concentration : Calculate dCo m Acq
. Time : 23. 3 r 7/19/201 1 3:03:0 2 P

M Modified : Ye s Proc
. Algorithm : Specif y Parameter s - K Q II I Nois e Percentage : 9 0 Bafe
. Sub
. Window : 1.0 0 mi n Peak-Split
. Factoc : 5 Repor t Larges t

Peak : Ye s Min
. Pea k

Height : 0.0 0 cp s Min
. Pea k

V?idth ; O.O O se c Smoothin g Width : 0 point s R T Window ; 30. 0 se c Expecte dRT : 15. 4 mi n Vs b Relativ e RT : N o Int
. Type : Bas e T o Bas e Retentio nTime : 15. 4 mi n Acea : 425276 5 count s Height : 5.S3e»O0 5 cp s Star t Time : 15. 1 mi n En dTime : 15. 7 mi n



# I S«n¥l*Name:"k110715a06 rSaF(^>leP:-GIJ>1(«1-01-1W)06 - Flle:1c11071^.«i r Pea k Name : "PFOA " Maca<ea) : "413.00(V369JM O D«.413.00CV219.000Da,413.00(V169-00 0 Da * Comnent-DALCW130R0110630<dai:100) - Arawtatkm: - Sanpl e Index : 6 2 Sampl e Type : •Sampl e Name:-kl10715b266 ^ Sampl e ID:"VLPIOOI-Ol-IS-ISO " Ple:-k110715a.wH r I Pea k Name : "PFOA * MaM<aa) : "413.000ir3e9.00 0 Da,413.00(V219.00 0 Oa.413.000/169.00 0 Da " •Comment:*DALGW144S0110828Mai;10 rAnnotatton:" " Sampl e Index : 27 0 Sampl e Type : Unknow n N/ A Calculate dC Acq
. Date : Acq
. Time : Modified : Proc
. Algot I Nois e Perce r one : 52. 1 ng/m L 7/19/201 1 4:49:1 2 P

H Ye s :hm : Specif y Paramet e :age : 9 0 Base
. Sub
. Window : 1.0 0 mi n Peak-Split
. Repor t Larg e Min
. Pea k

He Min
. Pea k

W l factor : 4 S t Peak : Ye s ght : 0.0 0 cp s 1th : 0.0 0 se e Smoothin g Width : 0 p o R T Window : Expecte dRT : Us e Relativ e Int
. Type : Retentio nT l Area : Height : Star t Time : En dTime : 30. 0 se c 15. 4 mi n RT : N o Bas e T o Bas e lae : 15. 4 mi n 192731 8 count s 2.3Se*00 5 cp s 15. 1 mi n 15. 6 mi n 2.3* 5 2.2e 5 2.1e5

- 2.0* 5 1.9e 5 1.8e 5 1.7* 5 1.6*5 ' 1.5*5

- 1.4* 5 1.3* 5 1.2* 5 1.1* 5 1.0e5 ' g.0e4 ' 8.0* 4 7.004

- 6.0*4

- 5.0* 4 4.0*4

- 3.0*4

- 2-0*4

- 1.0e4

- 0. 0 13. 0 ;wt i

:entratl i N/ A 

# I Sampl*N*me:1c110715a071 " Samp|e|D:-GLJ>1OO1-01-1fr011 " Fi*:"k110715a.wtt r Pea k Name : "PFOA " Maa»(es) : '413.000/369.00 0 Da.413.000/219.00 0 D a ,413.000/169.00 0 Da ' C(Knmen(:*DALGW130S0110630(dHl:10) " Anrwtatkin: ~ Sampl e Index : 7 1 Sampl e Type : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentag e 7/16/201 1 1:15:1 8 P

M Ye s Specif y Para m 9 0 Base
. Sub
. Window : 1.0 0 ra Peak-Split
. Fac t r : 3 Repor t Larges t

Peak : Ye s

R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime ; 0.0 0 0.0 0 0 30. 0 se c 15. 7 mi n N o Manua l 15. 5 mi n Area : 1480299 0 coun t Height : Star t Time : En dTine : .72e*00 6 cp s 15. 1 mi n 15. 7 mi n 

### 1 1.7* 6 1.6* 6 15* 6 1.4* 6 1-3* 6 1J2e6 1-1* 6 1 ^ 9J)e 5 8.0e 5 7-Oe S e^ 5 5.0e 5 4-0e 5 3.0e 5 2.0e 5 1.0e 5 15
.

J M/ A ng/m L Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentag e 7/16/201 1 4:25:4 3 P

M Ye s Specif y Param e 9 0 Base
. Sub
. Window : 1.0 0 m l Peak-Split
. Fac t r : 3 Repor t Larges t

Peak : Ye a Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 0.0 0 c 0.0 0 s 0 30. 0 se c 15. 1 mi n N o Valle y 15. 4 mi n Area : 3052407 3 count * Height : Star t Time : En dTime : .46e-i-00 o cp s 15. 1 mi n 15. 6 mi n

13. 5 14. 0 U S 15. 0 15. 5 10. 0 15. 0 15 5 16. 0 16. 5 17. 0 17 5 Dat aprinte db y ST

W Printing Time : 10:27:3 6 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 8 o f 1 0
Pag e 5 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAI n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0715a.rd b 

# I Sampl e Name : 'k1107l5a085 ' Sampi s ID : -GLP1CM)1-01-1&«21 " FUe : "kl10715a.wi r Pea k Name : "PFOA " Mat*<e«) : "413.000069-00 0 D«.413.00ar219-00 0 Da.413-00CV169.00 0 Da " Coirm*rt:"DAL<5W131R0110622<(iai:100 rAmotaton: - Sampl e Index : 6 5 Sampl e Type : Unknow n Concentration ; N/ A Calculate dCone : 2310
. ng/m L4.2*6

- Acq
. Date : 7/16/201 1 Acq
. Time : 9:21:4 4 P M 4.0*6

- Mod i fi t Ptoc
. I Ye s

Ithm : Specif y Parame t

Peak
. Base
. Sub
. Hlndo ' Peak-Split
. Fact i Repor t La
. Min
. Pea k

Height : Min
. Pea k

Width ; Smoothin g Width ; R T I • • i RT ; : Relat H

, Type : R e tent ] Area : Height ; le : 15. 4 mi n

3839077 5 count s 4.34e400 e cp s 15. 0 mi n 3.Be 6 3.eee 3.4*6

- 3.2*6

- 3.0*6 ' 2-8* 6 2.6e 6 2.4e6 ' 2.2e6

- 2.0* 6 1.6e6 ' 1.6e6 ' 1.4e6 < 12*6

- 1-0e6

- 8.0e5

- 6.0*5 < 4.0*5

- 2.0*5

- 0.0 - 13- 0 13. 5 14. 0 14 5 15. 0 15 5 16. 0 16 5 17- 0 17 5 

# I Sampl e Hame:-kll07lSal6 rSampl e ID : "GLP1001-01-18-079 " FUe:"k1107lSa.v)i4 r Pea k Name : "PFOA " Ma«*(*s) : *413.000069.00 0 D a ,413.000219.00 0 D a ,413.000^69.00 0 Da " Commen t "DALG W1% R 0 11062 8 <<i a 1:100) " Annotatbn: - Sampl e Index ; 16 7 Sampl e Type : Sub

. Wln i :age : Specif y Param i

9 0 1.0 0 ra: 

# I Sampl e Name:'k110715a12C rSaiT^ID:^LP1&01-01-18-050 - Fle:"k110715a.M« r Pea k Nam* : TFOA ' Ma*s(**) : "413.000069.00 0 D*,413J»0>'219-00 0 Da.413.00(V1GS.OO O Oa " Comment:"DALGW134R0110628(dl1:100 rArmotabon: - Satnpl e Inde.-t : 12 6 Sampl e Type : Unknow n Concentiation : N/ A Calculate dCone : 1790
. ng/m L3 2«f i Acq
. Date : 7/17/201 1 " Acq
. Time : 11:17:1 3 A M 3.0*6

-

M Q II I 2.8*6 '

Z6e6

- Z4e6

- 2.2e6

- 2.006

- & 1.6*6

- 1 1.6*6

- I 1.4e6 < 1.2* 6 1.0* 6 Nols t Base
. Peak-Split , Facto r Repor t Larges t

Pea l Min
. Pea k

Height : Kin
. Pea k

Hidth : Smoothin g Width : R TWindow : 30. 0 Expecte d RT : Us e Relativ e RT : Int
. Type : Bas e T o Bas ' Retentio nTime : 15. 5 m: Area : 3042043 0 cou i Height : 3.32e-f00 dcj 5. 5

14. 5 15. 0 15. 5 16- 0 16 5 17. 0 17 5 I SanvleName:'V110715a158 ' Sampl e ID:'OLP1(M>1-01-18-074 " Fie : *1c1107 1 Sa.wHT Pea k Nam* : TFOA ' M«ta(*«):'413.00Q069.000Da,413.00Q/219.000Da,4l3.000/l6aj>DODa ' I CoinnenL'DALGWl^LOll0628(dOl:10) " Annotatkm: '

5.0*6

- 4.8*6

- 4.6*6

- 4.4*6

- 4.2*6

- 4.0*6

- 3.8e6 < 3.6e6 < 3.4*6

- 3.2*6

- 3.0*6

- 2.8*6

- 2.6*6

- 2.4*6

- 2.2*6

- 2.0*6

- 1.8*6

- 1.6*6

- 1.4*6

- 1.2* 6 1.0* 6 6.0* 5 6.0*5

- 4.0*5

- Z0*5 ' 0.0

- N/ A Calculate d Acq
. Date : Acq
. Time : Modified : Proc
. Algo r Hois e Perc e Base
. Sub
. Peak-Split
. on e

th m 3570
. 7/18/201 1 2:13:5 0 A

M Ye s Specif y P a tage : 9 0 Indow : 1.0 0 Repor t Larges t

Peak : Ye s Min
. Pea k

H ig h Min
. Pea k

Hidt h Smoothit, g Hidt h R T Hindow : Expecte dR

T Us e Relati v Retentio nT Area : Height : Star t Time : En dTine : R

T 0.0 0

0.0 0 0 30. 0 s 15. 7 n N o Manua l 15. 5 n 5622297 4 CO

u 5.BOe-.00 6 c 15. 1 r

r IS. O r

r Sampl e Index ; Sampl e Type : Concentration : Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Percentag e 15 8 Unknow n H/ A 283
. 7/17/2 0 11:03: 0 Ye s Specif y 9 0 P
P a Base
. Sub
. Hindow : 1.0 0 Peak-Split
. Fac t ^r : 3 Rei>or t Larges t

Peak : Y Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Vs o Relativ e RT : Int
. Type : Retentio nTime : Area : 4 6 Height : Star t Time : En dTime : 0 0 0 30. 0 15. 7 N o Manua l 15. 5 2215 6 .ISe.O O 15. 0 16- 0 0 0 0 0

14 5 15. 0 15. 5 16J ) 16 5 17X ) 17 5 la O 15. 0 15 5 16. 0 16 5 17X ) 17. 5 18. 0 Dat aprinte db y ST

W Printin g Time : 10:27:3 6 AM Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 9 o f 1 0
Pag e 5 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur
. AL ; Jun e 201 1 Result s Name : kll0715a.rd b

•Sarn)leNam*:"K110715a144 ' Sampl e ID : "GLP1tMH-01-18-064 " Rle:"»t110715a-»« r •Pea k Name:-PFOA " Ma*«<e«):-413.00QQ69.000Da,413.00Q'2ig.00ODa,413.00(V169.00OOa ' I Commen t Tri p Blan k S« l 1 Sample " Anrwtatkm : ~ Sampl e Index : 14

4 Sample Type :

•atio i N / A Calculate dCone : Acq
. Time : Modified : Proc
. Algorithm : Base
. Sub
. Wind

o Peak-Split
. Fac t Repor t Larges t P Min
. Pea k Heigh t Min
. Pea k Width: Smoothin g Width: R T Window : Expecte dRT : Use Relativ e RT: Int
. Type : Retentio nTime : Acea : Height : Star t Time : En dTime : < 0

7/17/201 1 6:07:2 2 P M Ye s Specif y P a 9 0 ^ : 1.0 0 sr : 3 ..ak : Ye s 0.0 0 0 30. 0 15. 4 n N o Bas e T o Ba
. 15. 4 1 955 2 cou : 5.21e+00 3 15. 4 1 15. 5 n 

# I SampteN*m*:"k110715a23€ rSainpl e ID : "GLPI001-01-18-133 " Fte:"kl10715a.wi r Pea k Name : "PFOA " MB«*(e*) : "413.000/369.00 0 D a ,413.000/219.00 0 D a ,413.000/169JX WDa " Coffiment:-DALGW130LRB110630 rAnnotatton: " Sample lnde:< : 23 6 Sample Type : ratio ; N/A Calculate dCone : Acq
. Date : Acq

- Time : Modified : Proc
. Algorithm : Hoise Percentage : Base
. Sub
. Windo

w Peak-Split
. Fact o < 0

7/19/201 1 2:36:2 0 A M Ye s Specif y P a 9 0 1.0 0 r : 4 Repor t Larges t Peak : Yes Min
. Pea k Height : Min
. Pea k Width : Smoothin g Width : R T Window : Expecte dRT : Use Relativ e RT: Int
. Type : Retentio nTime : Area : 1 Height : 6 Star t Time : En dTime : 0.0 0 0.0 0 0 30. 0 = 15. 5 r . H o Manua l 15. 5 n = 41 8 cour 30et00 3 c 15. 4 n 15. 5 n

Dat aprinte db y ST

W Printin g Time : 10:27:3 6 A M Printin g Date : Tuesday , Augus t 23 , Pag e 1 0 o f 1 0
Pag e 5 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0728a.rd b
k l 10728a.rd b (PFOA) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -0.0030 7 x* 2 + 1.09 x+ 0.016 6 ( r= 0.9998 ) 80 , 75 -

6 5 7 0 7 5 8 0 8 5 9 0 9 5 100 4 0 4 5 5 0 5 5 Analyt e Cone

. /

I S Cone

. Dat a printe d b

yST W Printing Time : 10:26:1 1 A M Printing Date : Tuesday , Augus t 23 , Pag e 1 o f 1 201 1 Pag e 5 4 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFOAi n wate rsample s FSI A- Decatur
. AL ; Jun e 201 1 *ETS-Kir k Result s Name : kll0728a.rd b 

# I Sampl e Name : •V110728a01S - Sampt o ID : "1100M5« " Pea k Name : "13CaPfOA-IS(IS} * Maaa<»c} : -421.000/376. C Commen t "1. 0 ng/m L F C it d I n Synth

. VVat*i - Annotatton : Sample Inde>; : 1 6 Sample Typie : Standar d Concentration : 1.0 0 ng/m L Calculate dCone : N/ A Acq
. Date : 7/28/201 1 Acq
. Time : 3:16:3 2 P M Proc
. Algorithm : S Noise Percentage : Base
. Sub
. Windo

w Peak-Split
. Facto r Report Larges t Pe i Min
. Pea k Height : Min
. Pea k Width : Smoothin g Hidth : R T Window : Expecte dRT : Use Relativ e RT : int
. Type : Retentio nTime : Area : 150 S Height ; 2 Star t Time : En dTime : pec :

t :

1. S H o Vai l I S * 1 / b2e * l b l b f y P a 5 0 ..0 0 2 Ye s 0.0 0

e y

. 7 10 5

. 6

. 0 n



# I S»iTpleN»m*:-k110728a028 " Sampl e |D:"LCS-I10y26-1 " FUe:n(110728*.wt r Pea k Name : "13C8PRDA-IS0S) - Ma*i(e*) : "421.000/376.00 0 Da ' Comm*n t "0.2pp b LCS * Annotatton : ~ 

# I Sanv(eName:-V110728a02 rSan ^ ID ; "1 1 005*9 " Rle:-k 1 PeakNama:*13C8PFOA-l3(l5 rMaaa(e*):"421.000376.000Da * Comment : "Pitotho d Blani rAnnotatton : " Sampl e Index : 2 7 Sampl e Type ; Unknow n Concentration : 1.0 0 ng/m L Calculate d Cone : N/ A

Noi ; ;aqe :

. 14 1 nd c Peak-Split
. Facto r Report Larges t Pea l Min
. Pea k Height ; Min

- Pea k Width: Smoothin g Width: R T Vlindow : Expec t 1 RT : Int
. Type : Retentio nTime : Area : !7 i Height : Star t Time : Valle y

15. 7 588 2 c .016*00 5 15. 6

Sample Type : Q C Concentration : 0.99 3 Calculate dCone : N/ A Acq
. Date : 7/28/201 1 Acq
. Time : 7:29:3 2 P M Modified : Yes Proc
. Algorithm : Specif y Pa r Hois e Percentage : 50 Base
. Sub
. Hindow : 1.0 0 Peak-Split
. Factor : 3 Repor t Larges t Peak : Yes Min
. Pea k Height : 0.0 0 Min
. Pea k Width: 0.0 0 Smoothin g Width: 0 R T Hlndo« : 30. 0 s Expecte dRT : 15. 9 i n Us e Relativ e RT : N o ig/m

L

imeter s - M

O II I mi n
cp s s e c point s
Int
. Type : Bas e T o Bas e Retentio nTims : 15. 8 i t Area : 166627 7 coun Height : 2.93e+00 5 cp s Star t Time : 15. 6 m En dTime : 16. 1 m n n 

# I Sampl e Name : 1(110726*031 " Sampl e ID : "LCS-110726-4 " Fle:1(11073aa.wif r Pea k Name : "13C8R=OA^S{(S) " MaH(e*) : *421.000076.00 0 Da ' Comment : '2pp b LCS * Annotatton: " Sample Index : 3 1 Sample Type : Concentrati c Q C i : 0.99 3 ng/m
. Calculate dCone : H/ A Acq
. Date : Acq
. Time : Modified : 7/28/201 1

8:32:5 1 P M N o Proc
. Algorithm : Specif y Parame t Hois e Perce n age : 5 0 Base
. Sub
. tJindow : l
. 0 0 min Peak-Split
. Repor t Larg e Min
. Pea k H e •actor : 2 S t Peak : Yes ght : O.O

O c p Min
. Pea K Width: 0.0 0 s e Smoothin g w

l R T Window : Expecte dRT : Us e Relativ e Int
. Type : Retentio nT l Area : Height : Star t Time : En dTime : :th : 0 p .

30. 0 se c 15. 8 mi

n RT : H o Valle y le : 15. 8 mi

n 166509 8 count s 2.70e+00 5 cp s 15. 6 mi n 16. 0 mi n

Dat aprinte db y ST W Printin g Time : 10:30:0 2 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 1 o f 5

Pag e 5 5 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 *ETS-Kir k Result s Name : kll0728a.rd b 

# I S«ni|)l e Name:-k110728a03 rSampl e ID:'LCS-110726-7 ' File:-k l 10728«.vii r Pea k Name:-laCUPFCWWSflS) " Haaa(ea):"421.00Q'376.0CODa Cetnnert : "ZOpp b LCS ' Annotation: "

Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm ; Nois e Percentag e Base
. Sub
. Wind o Peak-Split
. Fac t N/ A 7/28/201 1 9:36:1 4 P

M N o Specif y P a 5 0 •i : 1.0 0 a r : 2 Repor t Larges t

Peak : Ye s Min
. Pea k

Heigh t Min
. Pea k

Vlidth : Smoothin g Hidth : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 15. 8 n H o Bas e T o B a 15. 8 B Acea : 159390 4 cou r Height : Star t Time : En dTime : .516*00 5 c 15. 6 n 15. 9 n



# I SanpleName:1(110728a044 - San^l e ID : "LCS-110726-13 * Rle:1(110728a.w( r PeakNam*:*13CePFQA4S(lS) " MaM(e«J ; "421.000076.000Da " Comment'2pp b LC S EC rAnnotatton: ' Sampl e Index : 4 4 Sampl e Type : Q C Concentration : 0.99 4 ng/m L2.8*5 i Calculate dCone : H/ A 

# I Sampl e Nam* : "k1l0726sO41 " Sampl e ID : TCS-110726-10 - Fle:*k110728a.<M r Pea k Name : "13C6PFCA-I3{IS) " Maaa{e*) : "421.000/376.00 0 Oa " Cemm*nt:*0.2ppbLCSEC P Annotatton:" " Sampl e Type : Concentration : Calculate dCone : Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Kois e Percentag e Base
. Sub
. Wind o Peak-Split
. Fac t Repor t Larges t

P Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : Q C 0.99 3 N/ A 7/29/201 1 12:04:0 8 A

M Ye s Specif y Pa r

' : 1.0 0 o r : 2 .ak : Ye s : 0.0 0

0.0 0 0 30. 0 s 15. 8 m H o Valle y 15. 7 m Area : 167905 2 cou n Height : Star t Time : En dTime : 2.62et00 5 c 15. 6 m 16. 0 m



# I Sampt*Name:'V11072BaO4 rSampl e ID : "LCS-110726-16 - Fie : 1(110728a.wt r Pea k Name : "13C8PFOA4S{IS) * Man{*«):'421.00CV376.000Da " Comnwnt : "20pp b LC S ECF " Amotatton : ~ Sampl e Index : 4 7 Z5* 5 2.4* 5 2.3* 5 2.2* 5 2.1* 5 • 2.0* 5 1.Se5 1.8* 5 1.7* 5 1.6*5 - 1.5*5 - 1.4*5 - 1.3*5 - 1.2*5 - 1.1*5 - 1.0*5 - g.0e4 - 8.0*4 - 7.0* 4 6.0* 4 5.0* 4 4.0e 4 3.0* 4 Z0e4 ' Acq
. Date : Acq
. Time : Modified : Proc
. Algorithm : Nois e Feccecitag e Base
. Sub
. Hlnd o Peak-Split
. Fac t Repor t Larges t

P Min
. Pea k

Heigh t Min
. Pea k

Vlidth : Smoothin g Width : R T Hindow : Expecte dRT ; Us e Relativ e RT : Int
. Type : Retentio nTime : 7/29/201 1 1:07:3 2 A

M Ye s Specif y P a S O / : 1.0 0 r : 2 a k : Ye s 0.0 0 0 30. 0 s 15. 8 n N o Valle y 15. 7 1 Area : 162702 5 cou r Height : Star t Time : En dTime : .Ble-f00 5 c 15. 6 a 15. 9 B Sampl e Type : Ion : Calculate dCone : Acq
. Dat e Acq
. Tim e Modified : Proc
. Algorithm : Hois e Pe r Base
. Su b Peak-Spl l entag e Q C 0.99 3 N/ A 7/29/2 0 2:10:5 0 Ye s specif y 5 0 1 A M •ig/tti

Parame t Window : 1.0 0

. Fac t Re|»r t Larges t

P Min
. Pea k Min
. Pea k Smoothin g R T Windo w Heigh t

width : width : Expecte dRT : Us e Relativ e RT : Int
. Typ e Retentio n Area : Height ; Star t Ti m En dTime : Time : a r : 2

tak : Ye s

0 0 30. 0 15. 8 H o Valle y 15. 7 0 0 0 0 m1 n

c p P <

159720 2 cou n .53et00 5 cp s 15. 6 15. 9 m n

n

1 M «.o Dat aprinte db y ST

W Printing Time : 10:30:0 3 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 2 o f 5

Pag e 5 6 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0728a.rd b 

# I Sampl e Name : •V110728a07? ' Sampl e ID : "GLP1&«1-01-1W)69 ' Rto:*kll072ea.wt r Pea k Name : "13C8PFOA4S(IS} " Ma*a{ea) : "421.00Ck'376.00 0 Da " Coirmenk"DALG W135 3 0110628 - Anrntstton: ' Sampl e Index : 7 5 Sampl e Type : Unknow n Concentration ; 1.0 0 ng/m L Calculate d Cone : H/ An Acq
. Date : 7/29/201 1 Acq
. Time : 12:02:3 6 P M Modified : Ye s Peak-Split
. Fa c o r : 2 Repor t Larges t

Peak : Ye s Min
. Pea k

Heig h Min
. Pea k

Hidt h Smoothin g Hidt h R T Window : Expecte dRT : Us e Relativ e R

T Int
. Type : Retentio nTime : : 0.0 0 0.0 0 0 15. 8 mi n H o Bas e T o Bas e 15. 8 mi n Area : 172593 7 count s Height ; Star t Time : En dTime : 2.90e-fO0 5 ep s 15. 6 mi n 15. 0 mi n

13 5 

# I SsnplaName:~k110728a02 rSampl e ID : "1100&«9 ^ Fle:'V110728a.w4 r Pea k Name : "PFOA " Ma*a(e*) : "413.OOCV369.00 0 Da ,413.000/219.00 0 Da,413.00(V169.DOO Da Commen t "Metho d Blank " Arvwtatran : ~ Sampl e Index : 2 7 Sampl e Type : Unknow n Concentration : N/ A 

# T Sampl e Name : "kl10728aO16 rS8n^lD:-1 1 00»^&« " FUe:"lc1107a8a.wtf r Pea k Nam* : "PFOA * MaM<*s) : "413.OOCV369.00 0 D a .413.00(V219.00 0 Da,413.00(Vt68JX n Da ' Comnent:"1.0ng/mLFCetdkfSyntti.Wat*; ' Annotaflon:" " Sampl e Inde^ : 1 6 Sampl e Type : Standar d Concentration : 1.0 0 ng/m L Calculate d Cone : 0.99 9 ng/m L Acq
. Date : 7/28/201 1 Acq , Time : 3:16:3 2 P M Modified : Proc
. Algorithm : Hois e Percentage : Base
. Sub
. Windo w Peak-Split
. Fact o Repor t Larges t

P e Min
. Pea k

Height : Min
. Pea k

Width : Smoothin g width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : Ye s Specif y P a 5 0 1.0 0 r ; 2 k : Ye s 0.0 0 0.0 0 0 30. 0 15. 8 N o Manua l 15. 7 Area : 166171 4 co u Height : 2 Star t Time : En dTime : 65e+00 5 15. 6 15. 9



# ( Sampl e Name : "k110726a028 " Sampt o ID : TC&-110726- rFle:1(1l0728a.wtf r Pea k Name : "PFOA " Ma*a(ea) : -413.00(V369.00 0 Da,413.O0a'219.O0 O Da,413.000/169.00 0 Da * ConuTMnt : *0.2pp b LCS * Annotatton : * "

Calculate dCone : Acq
. Date ; Acq
. Time : Modified : Proc
. Algorithm : Hois e Percentag e Base
. Sub
. Wind o Peak-Split
. Fac t 0.0035 9 7/28/20 1 7:08:2 8 Ye s Specif y 5 0 w : 1. 0 o r : 2 Repor t Larges t

Peak : Y

e Min
. Pea k

Heigh t Min
. Pea k

Width : Smoothin g width : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : Area : Height : Star t Time : En dTime : 0
. 0
. 0 30. 0 15. 8 H o Manua l 15. 8 '678 9 c 5.10e-tOO 3 15. 7 15. 0 1.7e 4 1.6e 4 1.5* 4 1.4* 4 1Je 4 1.2e 4 1.1* 4 1.0e 4 9000. 0 8000. 0 70oa o 6000. 0 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 14. 2 TIW.'T'.".'T ? 14.5 4



# ; i U.S 9 ' " 

### WLuk i 15.7 8 

# 1 t^ TM 

# i P 16.1 6 

# 1 f 

# k \ 

### 1 } 17J 6 IN III L 

# UikiU i PiiP f 18.1 2

I I 

# iii" A ||I||]|| M I f 

## " l| f Sampl e Type : O C Concentr e ion : Calculate dCone : Acq

- Dat e Acq
. Tim e Modified : Proc
. Algorithm : Base
. Su b Peak-Spl l 0
. 9 9 1 0 7/28/201 1 7:2 9 3 2 P

M Ye s Spe c Window :

. Factor : ReiJor t Larges t

Peak : Min
. Pea k Min
. Pea k Smoothin g R T Windo w Heigh t

Width : Width : Expecte dRT : Us e Rela t Int
. Typ e Retentio n Area : Height : Star t Ti m En dTime : v e RT :

Time : 3 0 t y P a

S O 1.0 0 3 Ye s 0.0 0 0.0 0 0 0 15. 8 n N o Ma n 243 0 .98 e a l

. 8 : 00 4 c 15. 7 n 1
. 0 n 7.0e4 '

leter s - M

C II I

f3.5* 4 I 3.0a 4

Dat aprinte db y ST

W Printing Time : 10:30:0 3 A M Printin g Date : Tuesday , Augus t 23 , Pag e 3 o f 5 201 1 Pag e 5 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o f PFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 *ETS-Kir k Result s Name : kll0728a.rd b

I San¥leNam*:"W10728a031 * San^)l e ID : "LCS-110726-4 " FUe:1c110728a
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I Sanvi e Nam* : "k l 10728*041 " Sampl e ID:-LCS-110726-ia ' Fle:1c110728a!w( F Pea k Name:-PFOA " Mau(*t):*413.00a/369.000Da,413.000ir219.0DODa.413.00Qn69.000Da I Comnwn t •X).2pp b LC S EC P Amotatton: " 

# I Sampt o Name:'V11072Sa034 ' Sampl e ID:-LCS-110726- rFle:"k110728a.wfr r Pea k Name : "PFOA " Ma*a(at) : -413.000/369.00 0 Da,413.00a'219.00 0 D a ,413.000/169.00 0 D* " Commant : -20pp b LCS ' Annotation : ~
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- 4.2*6

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- 2.8*6

- 2.6*6

- 2.4*6

- 2.2*6

- 2.0*6

- 1.6*6

- 1.6*6

- Sampl e Type : Concentratio n Calculate dC o Acq
. Date : Acq
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# I
( Sampl e Name : -k11072Sa04< ' Sampl e ID : -LCS-110726-13 " Fie : "k1l0728a.wi r Pea k Name : "PFOA " Ma««(e*) : '413.000/369.00 0 Da,413.00(V2ig.OO O D a ,413.000/169.00 0 Da ' Commant : "2pp b LC S ECF " /Annotatton : Sampl e Index : Concentration : Calculate dCone : Acq , Date : Acq

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. Date : Acq
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15. 0 15 5 16. 0 16. 5 17. 0 17. 5 18. 0 Dat aprinte db y ST W Printing Time : 10:30:0 3 A M Printin g Date : Tuesday , Augus t 23 , 201 1 Pag e 4 o f 5

Pag e 5 8 o f 7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1 Result s Name : kll0728a.rd b

I San«)t e Name : 1(1107283047 - S«mF4 e ID:-108-110726-16 ^

FI«:*k110728a.wH r I Pea k Name:-PFOA - MaM<ea):*413.00IV369.0000a^13.0aQr219.000Da,413.00tf1€9.000Da ' I Comment-20pp b LO S EC P Annotation:- - Sampl e Inde>

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p s Sampl e Name : "k110728aO75 " SampI * ID:"OLP1&01-01-1&06g ^ Fle:"k110728a.w<r r Pea k Name : "PFOA " Maw(*a} : "413.000/369.00 0 Da.413.000^19.00 0 Da.413.000/169J}0 0 Da " CommMil:"DALGW135S0110B2 rAnnotation: " Sampl e Index : 7 5 Sampl e Type : Concentration : Calculate dCone : Acq
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Dat aprinte db y ST

W Printin g Time : 10:30:0 3 A M Printin g Date : Tuesday , Augus t 23 , Pag e 5 o f 5
Pag e 5 9 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


### ATTACHMEN TC : ANALYTICA L METHOD(S )

Pag e 6 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


# 3 M Environmenta l Laborator y

Metiio d Mett)o d o fAnalysi s fo rtti e Determinatio n o fPerfluorinate d Compound s i n Wate r

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q <//( ^ / o " l
Approve d By : 

# ^/>^/ o y Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 Metho d o fAnalysi s fo rtti e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 1 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



## 1 Scop e an d Applicatio n Thi s metho d i s t o b e use d t o quantif yPerfluorobutanoi cAci d (PFBA) , Perfluoropentanoi cAci d (PFPeA) , PerfiuorohexanoicAci d (PFHA) , Perfluoroheptanoi cAci d (PFHpA) , Perfluorooctanoi cAci d (PFOA) , Perfluorononanoi cAci d (PFNA) , Perfluorodecanoi cAci d (PFDA) , Perfluoroundecanoi cAci d (PFUnA) , Perfluorododecanoi cAci d (PFDoA) , Perfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfiuorooctanesulfonat e (PFOS ) b yHig h Performance Liqui d Chromatograph ycouple d t o a tande m Mas s Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples
. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Determinatio n o f Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"

. Thi s metho d i s considere d a performance-base d method
. Data i s considere d acceptabl e a s lon g as th e define d Q C elements are satisfied
. Sampl e collectio n i s not covere d unde rthi s analytica l procedure
. 2 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS

. Sample s containin g heav y particulat e ma

ynot b e suitabl e fo ranalysi s b ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thi s i s a performance-base d method
. Metho d accurac yi s detennine d fo reac h sampl e set usin g multipl e laborator ycontro l spike s a

t multipl e concentrations
. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t least 50 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o determin e th e statemen t o f accurac yfo ranalytica l results
. 

## 3 Definition s 3. 1 Calibratio n Standar d Asolutio n prepare d b

yspikin g a know n volum e o fth e Worthin g Standar d (WS ) into a predetermine d amoun t o fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method
. Calibratio n standard s are use d t o calibrat e th e instmmen t respons e wit h respec t t o analyt e concentration
. 3. 2 Laborator yDuplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

yduplicat e sampl e i s a separat e aliquot ofa sampl e take n i n th e analytica l laborator ythat i s analyze d separatel ywit h identica l procedures
. Analysi s ofLDS s compare d t o that ofth e firs t aliquot give a measur e o fth e precisio n associate d wit h laborator yprocedures , bu t no

t wit h sampl e collection , preservation , o rstorag e procedures
. 3. 3 Fiel d Blani t (FB)/Tri p Blanl ( AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d a s a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures
. Th e purpos e ofth e F B i s t o determin e i ftes t substance s o r othe rinterference s are presen t i n th e fiel d environment
. Thi s sampl e i s als o refen'e d t o as a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 2 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### 3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e at th e sam e tim e fro m th e sam e locatio n as th e sample
. Th e FD S i s handle d unde ridentica l circumstance s an d treate d exactl yth e sam e throughou t fiel d an d laborator y procedures
. Analysi s ofth e FD S compare d t o that o fth e firs t sampl e give s a measur e o fth e precisio n associate d wit h sampl e collection , preservatio n an d storage , a s wel l a s wit h laborator yprocedures
. 

## 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s o fth e targe t analyte s are adde d t o th e sampl e bottl e i n th e laborator y before th e bottle s are sen t t o th e fiel d fo rcollectio n ofaqueou s samples
. Aknown , specifi cvolum e o f sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

ymakin g a "fil l t o thi s level " lin e o n th e outsid e ofth e sampl e container
. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample
. I fth e expecte d rang e o fanalyt e concentration s i s unknown , multipl e spike s at varyin g level s ma yb e prepare d t o increas e th e likelihoo d that a spike a

t a n appropriat e leve l i s made
. Th e FM S i s analyze d t o ascertai n i fan ymatri x effects , interferences , o rstabilit yissue s ma

ycomplicat e th e interpretatio n ofth e sampl e analysis
. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot o fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s o fth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t o fth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylike a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s o fanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are not know n o rma yvary . At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d plac e a s eac h FMS

. 

## 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator ya t th e tim e ofsampl e extraction
. At least two level s are included , on e generall ya t th e lo wen d ofth e calibratio n curve an d on e nea rth e mi d t o uppe rrang e o fth e curve . Th e LCS s are extracte d an d analyze d exactl ylik e a laborator

ysampl e t o detennin e whethe rth e metho d i s i n control
. LCS s shoul d b e prepare d eac h da ysample s are extracted
. 

## 3. 8 Laborator yMatri xSpik e (LMS ) Alaborator

ymatri xspike i s a n aliquot ofa sampl e t o whic h know n quantitie s oftarge t analyte s are adde d i n th e laboratory
. Th e LM S i s analyze d exactl ylik e a laborator

ysampl e t o detennin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results
. Th e endogenou s concentration s o fth e analyte s i n th e sampl e matri xmust b e detennine d i n a separat e aliquot an d th e measure d value s i n th e LM S con'ecte d fo rthes e concentrations
. LMS s are optiona l fo ranalysi s o faqueou s samples
. 

## 3. 9 Laborator ySampl e Aportio n o raliquot o fa sampl e receive d fro m th e fiel d fo rtesting
. 

## 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t o fquantitatio n (LLOQ ) fo ra datase t i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac ydurin g routin e operatin g conditions
. T o simplif ydat a reporting , th e LLO Q i s generall yselecte d a s th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria
. Sampl e LLOQ s are matrix-dependent
. Th e uppe rlimi t ofquantitatio n (ULOQ ) fo ra datase t i s th e highest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac ydurin g routin e operatin g conditions
. Th e highest standar

d i n th e calibratio n curve that meets metho d criteri a i s define d as th e ULOQ

.
ETS-8-044. 0 Pag e 3 o f1 1 Metho d o fAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 3 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


## 3.1 1 Metho d Blan k A n aliquot ofcontro l matri xthat i s treate d exactl ylike a laborator ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that are use d wit h othe rlaborator ysamples
. Th e metho d blan k i s use d t o detennin e i ftes t substance s o rothe rinterference s are presen t i n th e laborator y environment , th e reagents , o rth e apparatus
. 

## 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yo fmateria l intende d t o represen t th e origina l sourc e material
. 3.1 3 Stoc k

Standar d Solutio n (SSS ) Aconcentrate d solutio n ofa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound
. 

## 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s not normall y foun d i n th e sample(s)

. Asunogat e compoun d i s typicall ya targe t analyt e wit h a t least on e ato m containin g a n isotopically-labele d substitution
. I fused , sun-ogate(s) are adde d t o al l sample s an d qualit y contro l samples
. Surrogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedure includin g sampl e collection , preparation , an d analysis
. Inclusio n ofa sun'ogate analyt e i s a n optiona l qualit ycontro l measure an d i s NO Trequired
. 

## 3.1 5 Workin g Standar d (WS ) Asolutio n ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d as neede d t o prepare calibratio n standard s an d othe rrequire d analyt e solutions
. 

## 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yofth e standard s fo rthi s metho d have no t bee n precisel ydetemnined ; however , eac h shoul d b e treate d a s a potentia l healt h hazard
. Th e analyst shoul d wea rgloves , a la b coat , an d safet

yglasse s t o preven t exposure t o chemical s that migh t b e present
. Th e laborator

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a cun-ent awarenes s o floca l regulation s regardin g th e handlin g o fth e chemical s use d i n thi s method
. Areference fil e o fmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 

## 4. 2 Caution s Th e analyst must b e ^milia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d ga s an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l informatio n an d cautions
. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware
. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s o fanalysi s b

yrunnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 4 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination
. Thes e ma yinclude , bu t are no

t limite d to : was h bottles , Teflon ® line d caps , autovia l caps , HPLC parts , etc
. Th e us e ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 

## 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e ofpumpin g u p t o tw o solvents an d equippe d wit h a variabl e volum e injecto rcapabl e ofinjectin g 5-10 0 |J Lconnecte d t o a tande m Mas s Spectromete r (LC/MS/MS)

. I Analytica l balance capabl e ofreadin g t o 0.000 1 g Adevic e t o collec

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25|JL , SOJJL , 100|JL , 250|JL , 500|JL , 1000|JL

. 

### 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e o fspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 |j m Analytica l Column : Betasi l C18,4. 6 m m x10 0 mm , 5 |jnri Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

Tim e (min ) 0. 0 0. 5 11. 0 13. 5 13. 6 17. 0 % A

9 7 9 7 5 5 9 7 9 7 % B

3 3 9 5 9 5 3 3 FlowRat e

(mL/min ) 1. 0 1. 0 1. 0 1. 0 1. 0 1. 0 Injectio n Volume : 10 0 JJ L Quantitation : Pea k

Are a - quadrati ccurve fit , 1/ xweighted
. Ru n Time : ~ 1 7 minutes
. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met
.
ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 5 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


## 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e following transitions : Analyt e PFBA PFPe A PFH A PFHp A PFOA PFN A PFD A PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263-^21 9 31 3 ^26 9 an d 313-^11 9 36 3 - ^ 319 , 36 3 - ^

16 9 an d 36 3 - ^

11 9 41 3 ^ 369 , 41 3 - » 21 9 an d 41 3 ^ 16 9 46 3 - ^ 419 , 46 3 - ^

16 9 an d 46 3 - ^

21 9 51 3 ^ 469 , 51 3 ^

21 9 an d 51 3 ^

26 9 56 3 - ^ 519 , 56 3 ^

26 9 an d 56 3 ^21 9 61 3 ^ 569 , 61 3 - ^

16 9 an d 61 3 ^

31 9 29 9 - ^ 8 0 an d 29 9 - ^

9 9 39 9 - ^ 8 0 an d 39 9 - ^

9 9 49 9 - ^ 80 , 49 9 - ^

9 9 an d 49 9 - ^

13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s mayprovid e quantitatio n o fisomers tha t more closel ymatche s NM R dat a an d mayhav e th e adde d benefi t o f increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a ar e me t t o assur e adequat e specificity
. Th e previou s informatio n i s intende d as a guide , alternat e instmments an d equipmen t ma yb e used
. 

## 7 Reagent s an d Standard s 7. 1 Chemical s Wate r- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A.C.S

. Reagen t Grad e 7. 2 Standard s Perfluorobutanoi cAci d (PFBA- C 4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r PerfiuorohexanoicAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFNA-C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA-C1 0 acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C I 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C 4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfiuorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Pag e 6 6 o f7 1 

### Analysi sGLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s mayb e used
. 

## 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—Weig h 0. 3 g o fAmmoniu m acetat e an d dissolve i n 2. 0 L ofreagen t water
. Note : Altemativ e volume s ma yb e prepare d as lon g as th e ratio s ofth e solven t t o solut e ratio s are maintained
. 

## 7. 4 Stoc k

Standar d Solutio n (SSS ) an d Workin g Standar d Solutio n Preparatio n Th e followin g standar

d preparatio n procedure serve s as a n example
. Weighe d amounts an d fina l volume s ma yb e change d t o sui t th e need s o fa particula rstudy
. Fo rexample , |J Lvolume s ma yb e spike d into volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels
. 10 0 |jg/m L targe t analyt e SSSs—Weig h ou t 1 0 m g o fanalytica l standar d (correcte d fo rpercen t sal t an d purity ) an d dilut e t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask
. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container
. Prepar e a separat e solutio n fo reac h analyte
. Expiratio n date s an d storag e condition s ofstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandard operatin g procedure
. A n exampl e ofpurit yan d sal t con-ectio n i s give n belowfo rPFOS

.

, . , , molecula rweigh t o fanio n sal t correctio n facto r= = moclecula rweigh t o fsal t

49 9 PFO S (K^

)sal t correctio n facto r= ^^ ^ = 0.927 5 53 8 1 0 m g CsFiySOsK" wit h purit y90 % = 8.35m g CsFiySOs"(1 0 mg*0.90*0.9275=8.3 5 mg ) 5 (jg/m L (500 0 ng/mL ) mixe d workin g standard—^d d 0.5m L eac h ofth e 100|jg/m L SSS s t o a lOm L volumetri c flask an d brin g u p t o volum e wit h solvent
. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L o fth e 5 |jg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflas k

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m L mixe d standard^Ad d 625p L o fth e 5 jjg/mL-mixe d wori<in g standar d solutio n t o a 25m L volumetri c flask an d brin g u p t o volum e wit h solvent
. Storag e Conditions—Stor e al l SSS s an d workin g standard s i n accordance wit h laborator ystandar d operatin g procedure o ri n a refrigerato ra t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 7 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


## 7. 5 Calibratio n Standard s Usin g th e wori<in g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline
. Note : Volume s o fwate ran d wori^in g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline
. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d a s needed
.
Concentratio n o fWS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS.fi L

1 0 1 5 2 0 3 0 2 0 5 0 10 0 20 0 2 5 5 0 10 0 Fina l Volum e o f

Calibratio n Standar d (m L O fAST M Typ e 1 Water , o r ottie rsuitabl e water )

5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 5 0 Fina l Concentratio n o f

Calibratio n Standard , ng/m L (ppb ) I n AST M Typ e 1 Water , o rothe rsuitabl e wate r 0.02 5 0.037 5 0.05 0 0.07 5 0.10 0 0.25 0 0.50 0 1.00 2.5 0 5.0 0 10. 0 

## 8 Sampl e Handlin g 8. 1 Wate rSampl e Preparatio n Thi s metho d i s applicabl e t o clea n wate rsamples
. Sample s containin g heav yparticulat e ma

ynot b e suitabl e fo r analysi s b

ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial
. Plasti ci s prefen'e d ove rth e us e ofglas s autovials , t o preven t th e possibl yo ffluorochemlcal stickin g t o th e glass
. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water
. Prepar e metho d Q C sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials
. Prepare a t least five metho d blanks
. 

## 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

d curv e prio rt o eac h set o fsamples
. Th e standar d curve ma

yb e plotte d usin g a linea rfit, weighte d 1/

xo runweighted , o rb

yquadrati cfil (

y= ax ^ + bx+ c) , weighte d 1/

xo runweighted , usin g suitabl e software
. Th e calibratio n curve s ma yinclud e bu t shoul d no

t b e force d throug h zero . Th e mathematica l metho d use d t o calculat e th e calibratio n curve shoul d b e applie d consistentl ythroughou t a study
. An ychang e shoul d b e thoroughl ydocumente d i n th e ra wdata
. Hig h and/o rlo

wpoints ma

yb e exclude d firom th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e the ydi d no t meet th e pre-detennine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are no t a t least twic e that ofth e metho d and/o rsolven t blanks
. Th e coefficien t o fdeterminatio n (r^ ) valu e fo rth e calibratio n curv e must b e greate rtha n o requa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % o fth e theoretica l concentratio n wit h th e exceptio n o fth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 8 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFO Ai n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### b e withi n ±30%
. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata
. Aminimu m of6 points wil l b e use d t o constmc t th e calibratio n curve . I fth e calibratio n curve doe s not meet acceptance criteria , perfor m routin e maintenance o rprepare a newstandar d curve (i fnecessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yofth e calibratio n curve . Analyz e a mid-rang e calibratio n standard , on e o fth e sam e standard s use d t o construc t th e calibratio n curve , at a minimu m afte rever ytent h sample , not includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set
. Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable
. Th e calibratio n curve an d th e last passin g CCV wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that are quantitate d above th e concentratio n ofth e highest standar d i n th e curv e shoul d b e furthe rdilute d an d reanalyzed
. 

## 1 0 Qualit yContro l 10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LO Q of0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e final report
. 

## 10. 2 Metho d Blank s Metho d blank

s must b e prepare d wit h eac h analysi s batch
. At least five metho d blank s must b e prepared
. Metho d blank

s ma yb e injecte d multipl e times , bu t n o more tha n 3 injection s shoul d b e remove d fi'om a singl e metho d blank
. At a minimum , metho d blank s are analyze d prio rt o instrumen t calibration , prio rt o th e analysi s of CCV samples , an d a

t th e en d ofth e analytica l mn . Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % ofth e are a coun t ofth e LO Q standard
. Th e standar

d deviatio n o fth e are a counts ofthes e metho d blank s shoul d b e calculate d an d reported
. I f th e mea n are a counts o fth e metho d blank s excee d 50 % o fth e LO Q standard , the n th e LO Q must b e raise d t o th e first standar

d leve l i n th e curve that meets criteria , o raltematively , th e metho d blank s must b e evaluate d statisticall yt o determin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made
. 

## 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l not b e exclude d firom reporting
. Th e requiremen t fo r replicate s exclude s field blanks
. 10. 4 Surrogat e Spike s Sun'ogate spike s are no

t require d bu t ma

yb e use d o n projec

t specifi crequirements
. 

## 10. 5 La b Contro l Sampl e Triplicat e la b contro l spike s a t a minimu m oftw o differen t concentration s are t o b e prepare d wit h eac h preparatio n batch
. Lo wla b contro l spike s shoul d b e prepare d a t concentration s i n th e rang e o ffive t o te n time s highe rtha n th e targete d LO Q an d hig h la b contro l spike s shoul d b e prepare d at concentration s nea rth e mid-poin t ofth e curve . Th e relative standar

d deviatio n ofth e contro l spike s evaluate d independentl ya t eac h concentratio n leve l must b e les s tha n o requa l t o 20 % an d th e averag e recover ymust b e 80-120%
. I fth e above criteri a are no t met , th e entire se t o fsample s shoul d b e re-injecte d o rre-prepare d as appropriate
.

ETS-8-044. 0 Pag e 9 o f1 1 Metho d o fAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 9 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1


## 10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s o ffield matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagged as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targete d fortiflcatio n level s shoul d b e a t least 50 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o detemnin e th e statemen t o faccurac yfo ranalytica l results
. Th e averag e ofth e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 

## 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t ofanalyt e foun d (i n ng/mL , base d o n pea k area ) usin g th e standar d curv e (linea rregressio n parameters ) generate d b ya n appropriat e software program : Analyt e foun d (ng/mL ) = (Pea k Are a - Intercept ) ^

^ ^ Slop e D F = facto rb

ywhic h th e final volum e wa s diluted , i fnecessary . Fo rsample s fortifie d wit h know n amounts o fanalyt e prio rt o extraction , us e th e followin g equatio n t o calculat e th e percen t recovery .

_Tota l analyt e foun d (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) Analyt e adde d (ng/mL ) 1 2 Metho d Performanc e An ymetho d perfomnanc

e parameter

s that are not achieve d must b e considere d i n th e evaluatio n ofth e data
. Nonconfonnance t o an yspecifie d parameter s must b e describe d an d discusse d i fth e Technica l Manage r(non GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data
. I fcriteri a liste d i n thi s metho d performance sectio n are no t met , maintenance ma

yb e performe d o n th e syste m an d sample s reanalyzed , o rothe raction s take n as appropriate
. Documen t al l action s i n th e ra wdata
. I fdat a are t o b e reporte d whe n pert'omrianc e criteri a have not bee n met , th e dat a must b e footnote d o n table s an d discusse d i n th e tex

t ofth e report
. 

## 12. 1 Syste m Suitabilit y Syste m Suitabilit

ystandard s are no

t a require d componen t o fthi s method
. I frequire d b yprotoco l o rb

yth e technica l manager , a minimu m o fthre e syste m suitabilit ysample s are injecte d a

t th e beginnin g o feac h analytica l ru n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l ofth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial
. Th e syste m suitabilit yinjection s must have are a counts wit h a n RS D o f^5 % an d a retentio n tim e RS D o fS2 % t o b e compliant
. 

## 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t o fdetenninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

yb e withi n ±30%
. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequenc e are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac yo f eac h curve poin t must b e withi n 25 % o fth e theoretica l valu e (withi n 30 % fo rlowest curve point)

. Sample s that are brackete d b

yCCVs no

t meetin g thes e criteri a must b e reanalyzed
.

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 7 0 o f7 1GLP10-01-01 ; Interi m Repor t 1 8 Analysi s o fPFOAi n wate rsample s FSI A- Decatur , AL ; Jun e 201 1



### Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % of standard ) an d th e mas s spectra l respons e o funiqu e ions
. 

## 12. 3 Sensitivit y Th e targete d limi t ofquantitatio n fo ral l analyte s i s 0.02 5 ng/mL

. Th e LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n ofappropriat e blank s an d th e accurac

yo fth e low-leve l calibratio n curve points
. Refe r t o Sectio n 1 0 fo radditiona l details
. 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s are designe d t o generat e dat a that are accurat e t o +/-30%

. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d accurac yoflaborator

ycontro l spikes , field matri x spike s an d laborator

ymatri xspikes
. 

## 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l not b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks
. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d precisio n o flaborator ycontro l spikes
. 

## 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfonnin g thi s metho d wil l b e dispose d ofappropriately
. Th e origina l sample s wil l b e archive d at th e 3 M Environmenta l Laborator yi n accordance wit h intema l procedures
. 

## 1 4 Record s Eac h dat a packag e generate d fo ra stud ymust includ e al l supportin g infomnatio n fo rreconstmctio n o fth e data
. Infomnatio n fo rth e dat a packag e must include , bu t i s not limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

d pre p sheets/records , instrumen t m n lo g (instalmen t batc h records , instmmen t acquisitio n method , summar

ypages) , instrumen t results files, chromatograms , calibratio n curves , an d dat a calculations
. 

## 1 5 Affecte d Document s None
. 

## 1 6 Revision s Revisio n Numbe rSummar yo fChange s

ETS-8-044. 0 Pag e 1 1 o f1 1 Metho d ofAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 7 1 o f7 1