i
. ' " GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

GLP10-01-01 . Interi m Repor t 22 : Analysi s o fPFO A i n Groundwate r Sample s

Collecte d a t Decatur . A L fo r 3' " Quarte r201 1

Stud y Titl e Analysi s of Perfluorooctanoi cAci d (PFOA) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas 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 y Directo r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc
. 140 0 Westo n Wa y Westchester , P

A1938 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 ofsignin g Performin g Laborator y 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

y 3 M Center , BId g 260-05-N-1 7 Maplewdod , M N 55144 Projec t Identificatio n GLP10-01-01-2 2 Tota l Numbe r o fPage s

5 6 Th e testin g reporte d herei n mee t th e requirement s o fISO/IE C 17025-200 5 "Genera l Requirement s fo rth e Competenc e o f Testin g an d Calibratio n Laboratories", i n accordanc e wit h th e A2L ACertificat e #2052.01
. ^ Testin g tha t complie s wit h thi s Internationa l Standar d als o ooerat e i n accordanc e wit h IS O 9001:2000
. IACCREDITID I Testin g Cer t #2052.0 1
Pag e 1 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g


## GL P CoiviPLiANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 22
. Analysi s ofPFO

Ai n Groundwate rSample s Collecte d a t Decatur , A L fo r3"

^ Quarte r201 1 Study : 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
. 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 ar

e environmenta l sample s where there i s n o specifi ctes t substance , n o specifi ctest syste m an d n o dosin g o

fa test 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 determine d unde rGLPs
. 

# '/ I Gar yHohenstein/

Sponso rRepresentative Date

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

Pag e 3 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 22
. Analysi s o

fPFO Ai n Groundwate rSample s Collecte d a t Decatur , A L fo r3"

^ Quarte r201 1 Study : 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
. Thi s repor

t an d th e accompanyin g data were audite d b yth e 3 M Environmenta l Laborator yQualit y Assurance Uni t (QAU) , a s 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 ydirector
.
Inspectio n Date s Plias e Dat e R e porte d t o Inspectio n Date s Plias e Testin g Facilit y n/lanagemen t Stud yDirecto r 10/24-25/1 1 Interi m Repor t 2 2 Dat a an d Repor

t 11/1/1 1 11/1/1 1



### QA U Representative

Pag e 4 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g



### TABL E O F CONTENT S GL P Compliance Statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e of Contents 5 List of Table s 6 1 Stud yInfonnatio n 8 2 Summar

y9 3 Introductio n 1 0 4 Tes t & Contro l Substance s 1 1 5 Reference Substance s 1 1 6 Test Syste m 1 1 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 3 8. 1 Calibratio n 1 3 8. 2 Syste m Suitabilit y1 4 8. 3 Limi t o

f Quantitatio n (LOQ ) 1 4 8. 4 Continuin g Calibratio n 1 4 8. 5 Blank

s 1 4 8. 6 La b Contro l Spike s (LCSs ) 1 4 8. 7 Analytica l Metho d Uncertaint y1 5 8. 8 Fiel d Matri xSpike s (FMS ) 1 5

Pag e 5 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g



### 9 Data Summar

yan d Discussio n 1 6 1 0 Conclusio n 2 3 1 1 Data/Sampl e Retentio n 2 3 1 2 Attachments 2 4 1 3 Signature s 2 5 LIS TO F TABLE S Tabl e 1
. Summarize d PFO AResults (Decatu rGroundwater , 3" ^ Quarte r2011 ) 1 0 Tabl e 2
. Sampl e Descriptio n Ke yCod e 1 2 Tabl e 3
. Instrumen t Parameter s 1 3 Tabl e 4
. Liqui d Chromatograph yCondition s 1 3 Tabl e 5 . Mass Transition s 1 3 Tabl e 6
. Limi t o

fQuantitatio n (LOQ ) 1 4 Tabl e 7 . Laborator

yContro l Spik

e Recover y1 5 Tabl e 8
. Analytica l Metho d Uncertaint y1 5 Tabl e 9
. Fiel d Matri xSpike Concentration s 1 6 Tabl e 10
. DA L G W203 L 11093 0 1 7 Tabl e 11
. DA L GW220R11093 0 1 7 Tabl e 12
. DA L G W220 L 11093 0 1 7 Tabl e 13
. DA L G W222 R 110930 1 8 Tabl e 14
. DA L G W227R11092 2 1 8 Tabl e 15
. DA L G W227L11092 2 1 8 Tabl e 16
. DA L G W3 1 O

R 11092 8 1 9 Tabl e 17
. DA L G W312 R 11092 9 1 9 Tabl e 18
. DALGW317L11092 8 1 9 Tabl e 19
. DA L G W324L11092 3 2 0 Tabl e 20
. DA L G W327 R 11092 8 2 0

Pag e 6 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Tabl e 21
. DA L G W 328 R 11092 7 2 0 Tabl e 22
. DA L G W 328 L 11092 8 2 1 Tabl e 23
. DA L G W 330 R 11092 8 2 1 Tabl e 24
. DA L G W 330 L 11092 8 2 1 Tabl e 25
. DA L G W331 S 11092 9 2 2 Tabl e 26
. DA L G W 335 R 11092 7 2 2 Tabl e 27
. DA L G W GRS04 110930 2 2 Tabl e 28
. Tri p Blan k

1 2 3 Tabl e 29
. Tri p Blan k

2 2 3 Tabl e 30
. Rinseate Blank s 2 3

Pag e 7 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g



### 1 Study

Information 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 y Directo 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 y Locatio n Testing Facility 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud y Personne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator , (clange@mmm.com) : phon e (65 1 )-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow ; Analys t Kell yUkes ; Analys t Jonatha n Steege , Analys t Stud y Date s Stud yInitiation : Marc h 8,201 0 Interi m 2 2 Experimenta l Terminatio n Date : Octobe r12,201 1 Interi m Repor

t Completion : Date o

f Interi m Repor

t Signin g Locatio n o f Archive 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 standard reserv e sample s ar e archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g

2 Summary Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d i n Decatur , AL , representin g eightee n (18 ) differen t samplin g location s collecte d Septembe r2 3 - 30,2011
. Atota l of eighty-two sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo rperfluorooctanoat 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 fiel d matri xspik e (FMS ) sample s fo reac h location , two tri p blank s containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseate blanks
. Th e equipmen t rinseate blank s di d no t have FM S sample s prepare d fo rdetenninatio n o fPFO Arecovery . Al l ofth e sample s were prepare d an d analyze d fo rPFO Afollowin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP10-01-01-22
. Th e groundwate rsamples , tri p blank s an d equipmen t rinseate blank s fo rGLP10-0 1 -0 1 -2 2 were receive d fro m Westo n personne l o n Octobe r6,2011
. Al l o fth e sample s were prepare d an d analyze d fo rPFO Afollowin g 3 M Environmenta l Laborator yMetho d ETS-8-044.0
. Man yo fth e groundwate r sample s require d dilutio n t o attai n PFO Aconcentration s withi n th e rang e o fth 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 Aconcentration s are summarize d i n Tabl e 1
. Th e equipmen t rinseate an d th e tri p blank s associate d wit h GLP10-01-01-2 2 were belowth e lowe rlimi t of quantitatio n (LLOQ ) o f0.024 0 ng/mL
. Concentratio n results fo ral l groundwate rsample s range d fro m 0.32 2 ng/m L t o 358 0 ng/mL
. Th e analytica l uncertaint yfo rPFO Ai s +12%
.

Pag e 9 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Tabl e 1 . Summarize d PFO A Result s (Decatu rGroundwater , 3''' ' Quarte r 2011 ) Sampl e I D Avg
. PFO A Concentratio n (ng/mL ) Relativ e Percen t Differenc e (RPD ) DALGW203L11093 0 139 14 % DA L GW220 R 11093 0 29. 3 3.4 % DALGW220L11093 0 49. 8 0.0 % DA L GW222 R 11093 0 36 6 [a ] 3.8 % DA L GW227 R 11092 2 25 1 3.2 % DA L GW227 L 110922 14 4 0.70 % DA L G W 3 1 O

R 11092 8 96 9 1.9 % DA L GW312 R 11092 9 198 0 2.0 % DA L G W 317 L 11092 8 0.32 2 11 % DALGW324L11092 3 29 2 0.68 % DALGW327 R 11092 8 66 1 4.7 % DALGW328 R 11092 7 36 1 0.55 % DA L GW328 L 11092 8 10 2 3.0 % DALGW330R11092 8 35 8 2.2 % DA L GW330 L 11092 8 37 6 5.1 % DA L G W 331 S 11092 9 73 5 2.4 % DALGW335R11092 7 358 0 [b ] 0.0 % DA L GWGRS0 4 110930 301 0 3.3 % Tri p Blan k

(Mllli-Q TM Water) - 2 sets < 0.024 0 N/ A Equipmen t Blan k

s < 0.024 0 N/ A N/A; no t applicabl e Th e analytica l metho d uncertaint yfo rPFO Ai s +12%
. [a ] Th e FM S recover

ydi d no t meet acceptance criteria
. Metho d uncertaint yi s expande d t o +39 % fo rsamplin g locatio n DA L G W222R110930
. [b ] Samplin g locatio n DA L GW335 R 11092 7 di d no t hav e a n appropriate FM S t o asses s PFO Aaccuracy. ' 

### 3 Introduction Thi s analytica l stud ywa s conducte d a s par t o fth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama
. Th e objective ofth 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 a s 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 i n Decatur , A L fo rPFO

Ai n a n effor

t t o characteriz e on-sit e groundwate rconditions
. 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 sets fo reac h groundwate rsamplin g locatio n include d a fiel d samjjle , fiel d sampl e duplicate , an d fiel d spike samples
. Eac h empt

ycontaine rfo rgroundwate rsampling s wa s marke d wit h a "fil l t o here " lin e t o produce a fina l sampl e volum e of 20 0 mL
. Container s designate d fo rfiel d matri xsample s were fortifie d wit h a n appropriat e matri xspike solutio n containin g PFO Aprio rt o bein g sen t t o th e fiel d fo rsampl e collection
. Se e sectio n 8. 8 of th e repor t fo rfiel d matri xspik

e levels
. Th e aqueou s equipmen t rinseate sampl e wa s collecte d i n a plai n bottl e withou t fortification
. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysis"
.
Pag e 1 0 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Tabl e 1 summarize s th e averag e PFO Aconcentration s fo rth e duplicat e groundwate rsample s collected , an d fo rth e two tri p blank s an d aqueou s rinseate samples
. Table s 10-3 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 ar e reporte d an d discusse d elsewher e i n thi s report . 4 Test & Control Substances There wa s no

t a test substance o rcontro l substance s i n th e classi csens e o fa GL P study
. Thi s stud y was purel yanalytica l i n nature . 5 Reference

Substances Th e analytica l reference substance s use d fo rthi s stud yare liste d below
.

Referenc e Substanc e PFO A (Linear) PFO A (Linea ran d Branclied ) Chemica l Nam e Perfluorooctanoate Perfluorooctanoate Chemica l Formul a CyFisCOQ - C7F15COO " Identifie r CA S # 335-67- 1 CAS #95328-99- 7 Us e FM S Reference Standar d Target Analyt e an d LC S

Reference Standar

d Source Oakwoo d Products Wellingto n Expiratio n Date 01/17/201 8 03/17/201 4 Storag e Condition s Froze n Froze n Chemica l Lo

t Numbe r 344 0 TPFOA031 1 TC R Numbe r TCR07-004 1 TCR11-000 9 Physica l Descriptio n Powde r Liqui d Purit y 99.1 % 98.3 % 6 Tes* System There was 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 o

f groun 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 yar e "rea l worid " environmenta l samples
.

Pag e 1 1 o f 5 6Tabl e 2 . Sampl e Descriptio n Key Code . GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g

Example DALGW

203LDB

110930 Strin g Numbe r Strin g Descripto r Exampl e 1 Sampling Location DAL= Decatur, Alabama 2 Sample Type GW= Ground water 3 Well Identifier Example: 203L 4 Well Level R = Residuum

shallow water-bearing

zone L= Bedrock water-bearing

zone S = Epikarst middle water-bearing

zone 5 Sample Type 0=primary sample DB=duplicate

sample LS = low spike HS = high spike 6 Sampling Date 110930 = September30,2011 

### 7 Method

Summary 7. 1 Method s Analysi s fo ral l analyte s was complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysis"
. 

### 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s were retume d t o th e laborator ya t ambien t condition s o n Octobe r6 , 201 1 Sample s were store d refrigerate d a t th e laborator

yafte rreceipt
. Two sets oflaborator y prepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspike s were sen t wit h th e sampl e collectio n bottles
. 

### 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin 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 as follows : 1:5 dilution s were prepare d b ydilutin g 2m L sampl e wit h 8 m L o fMill i Q water , 1:1 0 dilution s were prepare d b ydilutin g 1 m L sampl e wit h 9 m L ofMill i Q water , 1:2 0 dilution s were prepare d b ydilutin g 0.5m L sampl e wit h 9.5m L ofMill i Q water , 1:5 0 dilution s were prepare d b ydilutin g 0.2m L sampl e wit h 9.8m L o fMill i Q , an d 1:10 0 dilution s were prepare d bydilutin g 0. 1 m L sampl e wit h 9.9m L ofMill i Q water . 7. 4 Analysi s Al l stud y samples an d qualit

y control samples wer

e analyze d fo r PFO A using hig h performanc e liqui d chromatography

/ tandem mas s spectrometr y (HPLC/MS/MS) . Detaile d instrumen

t parameters , the liqui d chromatograph

y gradien t program , an d the specifi c mas s transitions analyzed ar e describe

d i n the ra wdat a har d copie s place d i n the fina l dat

a packet , and ar

e briefl y describe

d belo wi n Tabl e 3 , Tabl e 4 an d Tabl e 5 .

Pag e 1 2 o f5 6Tabl e 3 . Instrumen t Parameters . GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Instrumen t Nam e ETS Buste r Analytica l Metho d Followe d ETS-8-044. 0 Analysi s Date s 10/7/1 1 Projec t GLP10-01-01-2 2 Liqui d Ciiromatograp h Agilen t 1100 Guar d colum n Pris m R P (2. 1 m m X 5 0 mm) , 5 n Analytica l colum n Betasi l 01 8 (2. 1 m m X 100 mm) , 5| i Injectio n Volum e 1 0 n L IVIas s Spectromete r Applie d Biosystem s AP I 400 0 Io n Sourc e Turb o Spra y Electrod e Turb o io n electrod e Polarit y Negativ e Softwar e Analyst 1.4. 2 Tabl e 4 . Liqui d Chromatograph y Conditions . step Total

Time Flow

Rate Percent A Percent B Number (min) (fiUmin) (2 mM ammonium

acetate) (MethanoO ETS-8-044. 0 0 0 30 0 97. 0 3. 0 1 2. 0 30 0 97. 0 3. 0 2 14. 5 30 0 5. 0 95. 0 3 15. 5 30 0 5. 0 95. 0 4 16. 5 30 0 97. 0 3. 0 5 20. 0 30 0 97. 0 3. 0 Tabl e 5 . Mas s Transitions .

Analyte Mass Transition Q1/Q3 Reference Material Structure PFOA 413/369 Linear* Branched 413/219 413/169 Dwel l tim e wa s 10 0 mse cforeac h transition
. Th e individua l transition s wer e summe d t o produc e a "tota l io n chromatogram " (TIC) , whic h wa s use d forquantitation
. 

### 8 Analytical

Results 8. 1 Calibratio n Sample s were analyze d against a n extema l standar d calibratio n curve . Calibratio n standard s were prepare d byspikin g know n amounts o f th e stoc k

solutio n containin g PFO

A(reference standar

d containin g bot h linea ran d branche d isomers ) into Mill i Q water . Standard s rangin g fro m 0.025 0 ng/m L t o 100 ng/m L (nominal ) were analyzed
. 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 reac h analyte
. Th e dat a were no t force d throug h zero 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 curv

e
Pag e 1 3 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac yrequirements o

f 100±25 % (100±30 % fo rth e lowes t curve point) were met fo ral l analytes
. Th e con-elatio n coefficien t (r ) was greate rtha n 0.99 5 fo rPFOA
. 

### 8. 2 Syste m Suitability Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofeac h analytica l sequence t o demonstrat e overal l syste m suitability
. Analysi s run s met th e acceptance criteri a ofles 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%RSDfo rPFOA
. 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LO Q for thi s analysi s i s the lowes t non-zer o calibratio n standar

d i n the curv

e tha t meet s linearit y an d accurac

y requirement

s an d for which the area count s ar e a t leas t twnc e thos e o fthe appropriat

e blanks . Th e nominal LO Q foral l analyte s ca n b e found i n Tabl e 6 . Tabl e 6 . Limi t o

fQuantitatio n (LOQ) . Analysis

Date PFOA

LOQ, ng/mL 10/7/1 1 0.024 0 (1 ) Analytica l LOQ wittiou t sampl e dilutio n factor s applied
. 8. 4 Continuin g Calibratio n Durin g th e cours e o

f eac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instmmen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l reporte d sample s were brackete d b yCCV s that met metho d criteri a o f100 % ±25%
. 

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

f blank s were prepare d an d analyze d wit h th e samples : metho d procedura l blanks , tri p blank s an d equipmen t rinseate blanks
. Metho d procedura l blan k results were reviewe d an d use d t o evaluat e metho d performance an d t o determin e th e LOQ fo rPFOA
. Tri p blank s reflec t th e shippin g an d sampl e collectio n condition s th e sampl e bottle s an d sample s experience
. Equipmen t rinseate blank s ar e aqueou s sample s tha

t reflec t th e efficienc

yo fequipmen t cleanin g i n th e fiel d betwee n differen t sampl e collection s an d ar e proo f o f n o cros s contaminatio n ofsample s fro m th e equipment
. 8. 6 La b Contro l Spike s (LCSs ) 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 b

yspikin g know n amounts o f th e analyt e into laborator yreagen t water , 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% , wa s met fo ral l LCSs
. Th e followin g calculation s were use d t o generat e dat a i n Tabl e 7 fo rlaborator ycontro l spikes :
1 o . r . Calculate d Concentratio n ,,... , LC S Percen t Recover

y= * 100 % Spike Concentratio n LCS % RS D = standard deviatio n LC S replicate s . ^ ^^^^ ^ averag e LC S recover

y

Pag e 1 4 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Tabl e 7 . Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Analyze d 10/7/1 1 PFOA(Linear + Branched) Spiked Calculated Concentration Concentration Lab ID (ng/mL) (ng/mL) VoRecovery LCS-111007- 1 1.9 1 2.0 4 10 7 LCS-111007- 2 1.9 1 1.9 2 10 0 LCS-111007- 3 1.9 1 2.0 2 10 6 Averag e ±%RS D 104 % ±3.6 % LCS-111007- 4 19. 1 18. 8 98. 6 LCS-111007- 5 19. 1 19. 7 10 3 LCS-111007- 6 19. 1 19. 0 99. 2 Averag e ±%RS D 100% ±2.4 % LCS-111007- 7 47. 7 45. 1 94. 6 LCS-111007- 8 47. 7 45. 2 94. 8 LCS-111007- 9 47. 7 46. 2 96. 9 Averag e ±%RS D 95.4% ±1.3 % 

### 8. 7 Analytica l Method Uncertainty Analytica l uncertaint

yi s base d o n historica l Q C 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 set o faccurac yresults (i n % ) obtaine d fo rmost recen t fift yQ 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 con-espond s t o a confidence leve l of 95%
. Tabl e 8
. Analytica l Metho d Uncertaint y Analyt e PFO A Metho d Standar d Deviatio n Metho d

Uncertaint y Analyt e PFO A ETS-8-044. 0 5.9 9 ±12 % 

### 8. 8 Fiel d Matri xSpike s (FMS ) Fiel d 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 of fiel d sampl e t o a containe rspike d byth e laborator ywit h PFO

A(reference standar

d containin g primaril y linea rPFOA

) 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 o f 100±30 % confin n that "unknown " components i n th e sampl e matri x d o no t significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s of interest
. Fiel d matri xspik e concentration s must b e 50 % of th e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike
. Fiel d matri xspike s are presente d i n sectio n 9 o fthi s report .

Pag e 1 5 o f 5 6Tabl e 9 . Fiel d Matri x Spike Concentration s GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Locatio n (Wel l ID

) Spik e Leve l PFO A Spik e Concentratio n (ng/mL) 317 L Lo wSpik e 1 Hig h Spik e 1 0 220R , 220L , an d 328 L Lo wSpik e 1 0 Hig h Spik e 100 203L , 222R , 227L , 227R , 3 1 OR, 324L , 327R , 330L , 331S , an d 335 R Lo wSpik e 100 203L , 222R , 227L , 227R , 3 1 OR, 324L , 327R , 330L , 331S , an d 335 R Hig h Spik e 100 0 GRS04 , 312R , an d 330 R Lo wSpik e 100 0 Hig h Spik e 500 0 328 R Lo wSpik e 100 Hig h Spik e 50 0 Tri p Blank

s Lo wSpike 1 0 Mi d Spik e 100 Tri p Blank

s Hig h Spik e 100 0 (Sampl e Concentratio

n o f FM S - Averag

e Concentration : FieldSampl e & FieldSampl

e Dup. ) ^ , „ , FM S Recover y = -^ ^ — * 100 % Spik e Concentrato

n 

### 9 Data Summary

and Discussion Th e table s belowsummariz e th e sampl e results an d fiel d matri xspik e recoverie s fo rth e samplin g location s a s wel l as th e Tri p Blank s an d rinseate blank
. Results an d averag e value s are rounde d t o thre e significan t figure s accordin g t o EP Aroundin g rules
. Becaus e o frounding , 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 W 222 R (Tabl e 13) - Hig h spike recover ywa s 61.4%
. Metho d uncertaint yi s expande d t o ±39%
. DA L G W335 R (Tabl e 26 ) - Samplin g locatio n di d no t have a n appropriat e fiel d matri xspike leve l t o accuratel yasses s PFO

Arecovery .

Pag e 1 6 o f 5 6Tabl e 10 . DA L GW203 L 11093 0 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

PFOA Concentration 3MUMSID Description (ng/mL) VoRecovery GLP10-01-01-22-00 1 DA L GW203 L 011093 0 14 8 N A GLP10-01-01-22-002 DALGW203 L D B 11093 0 12 9 N A GLP10-01-01-22-00 3 DALGW203LLS11093 0 24 1 10 3 GLP10-01-01-22-004 DALGW203 L H S 110930 101 0 87. 2 Average Concentration

(ng/mL) ± %RPD 139 ng/mL±14% NA= No t Applicabl e Sample s analyze d usin g a 1 ;5

0 dilutio n factor . Tabl e 11 . DA L G W220 R 11093 0 PFOA Concentration 3M LIMS ID Description (ng/mL) %Recovery GLP10-01-01-22-00 5 DA L GW220 R 011093 0 28. 8 N A GLP10-01-01-22-00 6 DALGW220 R D B 110930 29. 8 NA GLP10-01-01-22-00 7 DALGW220RLS11093 0 37. 1 N C GLP10-01-01-22-00 8 DALGW220 R H S 110930 11 3 83. 7 Average Concentration

(ng/mL) ± %RPD 29.3 ng/mL±3.4% N A= No t Applicabl e N C = No t Calculated ; tti e sampl e concentratio n i s greate rttia n 2xtti e spil<e level
. Sample s analyze d usin g a 1:5 dilutio n factor
. Tabl e 12 . DA L G W220 L 11093 0 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-00 9 DA L GW220 L 011093 0 49. 8 NA GLP10-01-01-22-01 0 DALGW220 L D B 110930 49. 8 NA GLP10-01-01-22-01 1 DALGW220LL S 11093 0 57. 6 N C GLP10-01-01-22-01 2 DALGW220 L H S 11093 0 133 83. 2 Average Concentration

(ng/mL) ± %RPD 49.8 ng/mL±0.0% N A= No t /\pplicabl e N C = No t Calculated ; th e sampl e concentratio n i s greate rUia n 2xth e spil< e level
. Sample s analyze d usin g a 1:5 dilutio n factor
.

Pag e 1 7 o f 5 6Tabl e 13 . DA L G W222 R 11093 0 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g

PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-01 3 DA L GW222 R 011093 0 35 9 NA GLP10-01-01-22-01 4 DALGW222 R D B 110930 37 3 NA GLP10-01-01-22-01 5 DALGW222RL S 110930 46 2 N C GLP10-01-01-22-01 6 DALGW222 R H S 11093 0 98 0 61.4<^ > Average Concentration

(ng/mL) ± %RPD 366 ng/mL±3.8%'^ N A= No t /Applicabl e N C = No t Calculated ; th e sample concentration is greate rthan 2 xth e spik e level
. Sample s analyze d using a 1:5

0 dilutio n factor
. (1 ) FM S recover ydi d no t mee t acceptanc

e criteri a o f 10 0 ±30%
. (2 ) Mettio d uncertaint

yha s been expande

d t o ±39%
. Tabl e 14 . DA L G W227 R 11092 2 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-01 7 DA L GW227 R 011092 2 24 7 NA GLP10-01-01-22-01 8 DALGW227 R D B 11092 2 25 5 NA GLP10-01-01-22-01 9 DALGW227 R L S 11092 2 34 5 N C GLP10-01-01-22-02 0 DALGW227 R H S 11092 2 1040 78. 9 Average Concentration

(ng/mL) ± %RPD 251 ng/mL±3.2% N A= No t /Applicable N C = No t Calculated ; th e sample concentiBtion is greate rthan 2 xth e spil^ e level
. Sample s analyze d using a 1:2

0 dilutio n facto r Tabl e 15 . DA L G W227 L 11092 2 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-02 1 DA L GW227 L 011092 2 14 3 NA GLP10-01-01-22-02 2 DALGW227 L D B 110922 14 4 NA GLP10-01-01-22-02 3 DALGW227LLS11092 2 22 4 80. 5 GLP10-01-01-22-02 4 DALGW227LH S 11092 2 91 8 77. 5 Average Concentration

(ng/mL) ± VoRPD 144 ng/mL±0.70% N A= Not/Applicable Sample s analyze d using a 1;2

0 dilutio n factor
.

Page 1 8 o f 5 6Tabl e 16 . DA L G W3 1 OR 11092 8 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g

PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-02 5 DA L GW310 R 011092 8 97 8 NA GLP10-01-01-22-02 6 DALGW3 1 O R D B 11092 8 96 0 NA GLP10-01-01-22-02 7 DALGW3 1 O R LS 11092 8 105 0 N C GLP10-01-01-22-02 8 DALGW3 1 O R H S 11092 8 1770 80. 1 Average Concentration

(ng/mL) ± VoRPD 969 ng/mL±1.9% NA= No t Applicabl e NO = No t Calculated ; Ui e sampl e concent^tio n i s greate rtha n 2xth e spik e level
. Sample s analyze d usin g a 1:10 0 dilutio n factor
. Tabl e 17 . DA L G W312 R 11092 9 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-02 9 DA L GW312 R 011092 9 196 0 NA GLP10-01-01-22-03 0 DALGW312 R D B 11092 9 200 0 NA GLP10-01-01-22-03 1 DALGW312 R LS 11092 9 270 0 72. 0 GLP10-01-01-22-032 DALGW312 R H S 11092 9 656 0 91. 6 Average Concentration

(ng/mL) ± VoRPD 1980 ng/mL±2.0% NA= No t Applicabl e Sample , sampl e duplicate, an d L S vmr e analyze d usin g a 1:10

0 dilutio n fector. Th e H S was analyze d usin g a 1:50

0 dilutio n factor . Tabl e 18 . DA L G W317 L 11092 8 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-03 3 DA L G W 317 L 011092 8 0.34 0 N A GLP10-01-01-22-034 DALGW317 L D B 11092 8 0.304 NA GLP10-01-01-22-03 5 DALG W 317LL S 11092 8 1.1 8 85. 8 GLP10-01-01-22-03 6 DA L GW317LH S 11092 8 9.3 7 90. 5 Average Concentration

(ng/mL) ± VoRPD 0.322 ng/mL±11% N A= No t Applicabl e

Pag e 1 9 o f5 6Tabl e 19 . DA L G W324 L 11092 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g

PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-03 7 DA L GW324 L 011092 3 29 3 N A GLP10-01-01-22-03 8 DALGW324LD B 11092 3 29 1 N A GLP10-01-01-22-03 9 DALGW324 L L S 11092 3 37 8 N C GLP10-01-01-22-04 0 DALGW324 L H S 11092 3 111 0 81. 8 Average Concentration

(ng/mL) ± VoRPD 292 ng/mL±0.68% N A= No t /Applicabl e N C = No t Calculated ; th e sample concenti^ition is greate rthan 2 xttie spik e level
. Sample s analyze d using a 1:5

0 dilutio n factor
. Tabl e 20 . DA L G W327 R 11092 8 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-04 1 DA L GW327 R 011092 8 64 5 N A GLP10-01-01-22-042 DALGW327 R D B 11092 8 67 6 NA GLP10-01-01-22-04 3 DALGW327RLS11092 8 77 1 N C GLP10-01-01-22-044 DALGW327 R H S 11092 8 140 0 74. 0 Average Concentration

(ng/mL) ± VoRPD 661 ng/mL±4.7% N A= No t /Applicabl e N C = No t Calculated ; ttie sample concenti^tio n is greate rttian 2 xttie spik e level
. Sample s analyze d using a 1:5

0 dilutio n facto r Tabl e 21 . DA L G W328 R 11092 7 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-04 5 DA L GW328 R 011092 7 36 2 NA GLP10-01-01-22-04 6 DALGW328 R D B 11092 7 36 0 NA GLP10-01-01-22-04 7 DALGW328RL S 11092 7 42 5 N C GLP10-01-01-22-04 8 DALGW328 R H S 11092 7 71 5 70. 8 Average Concentration

(ng/mL) ± %RPD 361 ng/mL± 0.55% N A= No t Applicabl e N C = No t Calculated ; th e sample concenti^tio n i s greate rttian 2

xth e spik e level
. Sample s analyze d using a 1:2

0 dilutio n factor
.

Page 20 o f 5 6Tabl e 22 . DA L G W328 L 11092 8 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

PFOA Concerttration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-04 9 DA L GW328 L 011092 8 100 NA GLP10-01-01-22-05 0 DALGW328 L D B 11092 8 103 NA GLP10-01-01-22-05 1 DALGW328 L LS 11092 8 10 9 N C GLP10-01-01-22-05 2 DALGW328 L H S 11092 8 179 77. 5 Average Concentration

(ng/mL) ± VoRPD 102 ng/mL±3.0% N A= No t /Applicabl e N O = No t Calculated ; Ui e sampl e concentratio n i s greate rtha n 2xttie spik e level
. Sample s analyze d usin g a 1:1 0 dilutio n factor
. Tabl e 23 . DA L G W330 R 11092 8 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-05 3 DA L GW330 R 011092 8 36 2 NA GLP10-01-01-22-05 4 DALGW330 R D B 11092 8 35 4 NA GLP10-01-01-22-05 5 DALGW330RL S 11092 8 121 0 85. 2 GLP10-01-01-22-05 6 DALGW330 R H S 11092 8 482 0 89. 2 Average Concentration

(ng/mL) ± VoRPD 358 ng/mL±2.2% N A= No t Applicabl e N C = No t Calculated ; th e sampl e concentratio n i s greate rtha n 2xttie spik e level
. Sample , sampl e duplicate, an d L S wer e analyze d usin g a 1:10

0 dilutio n facto r Th e H S was analyze d usin g a 1:50

0 dilutio n factor . Tabl e 24 . DA L G W330 L 11092 8 PFOA Concentration 3M LIMS ID Description (n^mL) VoRecovery GLP10-01-01-22-05 7 DA L GW330 L 011092 8 36 6 NA GLP10-01-01-22-05 8 DALGW330 L D B 11092 8 38 5 NA GLP10-01-01-22-05 9 DALGW330 L LS 11092 8 52 0 N C GLP10-01-01-22-06 0 DALGW330LH S 11092 8 1270 89. 5 Average Concentration

(ng/mL) ± VoRPD 376 ng/mL±5.1% NA= No t /Applicabl e N C = No t Calculated ; th e sampl e concenfatio n i s greate rtha n 2xttie spik e level
. Sample s analyze d usin g a 1:5 0 dilutio n facto r

Pag e 2 1 o f 5 6Tabl e 25 . DA L G W331 S 11092 9 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-06 1 DA L GW331S 0 11092 9 74 4 NA GLP10-01-01-22-06 2 DALGW331SDB11092 9 72 6 NA GLP10-01-01-22-06 3 DALGW331SL S 11092 9 80 8 N C GLP10-01-01-22-06 4 DA L GW331SH S 11092 9 1440 70. 5 Average Concentration

(ng/mL) ± VoRPD 735 ng/mL±2.4% N A= No t /Applicabl e N C = No t Calculated ; th e sampl e concenti'atio n i s greate rtha n 2xttie spik e level
. Sample s analyze d usin g a 1:5 0 dilutio n factor
. Tabl e 26 . DA L G W335 R 11092 7 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-06 5 DA L GW335 R 011092 7 358 0 NA GLP10-01-01-22-06 6 DALGW335 R D B 11092 7 358 0 NA GLP10-01-01-22-06 7 DALGW335 R LS 11092 7 353 0 N C GLP10-01-01-22-06 8 DALGW335 R H S 11092 7 425 0 N C Average Concentration

(ng/mL) ± VoRPD 3580 ng/mL±0.0%'^' N A= No t Applicabl e N C = No t Calculated ; th e sampl e concenti^tio n i s greate rtha n 2xttie spik e level
. Sample s analyze d usin g a 1:5 0 dilutio n factor
. (1 ) Samplin g location doe s no t hav e a n appropriat

e matri xspik e leve l t o asses s accuracy . Tabl e 27 . DA L G WGRS0411093 0 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-06 9 DA L GWGRS0 4 011093 0 306 0 NA GLP10-01-01-22-07 0 DA L G W GRS04 D B 110930 296 0 NA GLP10-01-01-22-07 1 DA L G W GRS04 LS 110930 372 0 N C GLP10-01-01-22-072 DA L G W GRS04 H S 11093 0 699 0 79. 6 Average Concentration

(ng/mL) ± VoRPD 3010 ng/mL±3.3% NA= No t Applicabl e N C = No t Calculated ; th e sampl e concentratio n i s greate rtha n 2xth e spik e level
. Sample , sampl e duplicate , an d LS wer e analyze d usin g a 1:10

0 dilutio n factor
. Th e H S was analyze d usin g a 1:500 dilutio n factor
.

Pag e 2 2 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g

Tabl e 28 . Tri p Blan k

1 PFOA Concentration 3M LIMS ID Description (ng/mL) VoRecovery GLP10-01-01-22-074 DA L G W TRIP0 1 0 <0.024 0 N A GLP10-01-01-22-07 5 DA L G W TRIP0 1 LS 8.5 0 85. 0 GLP10-01-01-22-07 6 DA L G W TRIP0 1 M S 85. 6 85. 6 GLP10-01-01-22-07 7 DA L G W TRIP0 1 H S 91 3 91. 3 N A= No t Applicabl e Tabl e 29 . Tri p Blan k

2 PFOA 3M LIMS ID Descnptfo n Concentration (ng/mL) %Recovery GLP10-01-01-22-07 8 DALGWTRIP0 2 0 <0.024 0 N A GLP10-01-01-22-07 9 DALGWTRIP02L S 8.5 5 85. 5 GLP10-01-01-22-08 0 DALGWTRIP02M S 94. 0 94. 0 GLP10-01-01-22-08 1 DALGWTRIP02H S 100 0 100 N A= No t /Applicable Tabl e 30 . Rinseat e Blank s PFOA 3M LIMS ID Description Concerttration (ng/mL) GLP10-01-01-22-08 2 DALGW203 L R B 11093 0 <0.024 0 GLP10-01-01-22-08 3 DALGW220 L R B 110930 <0.024 0 10 Conclusion Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l metho d 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
. 

### 11 Data/Sample

Retention Al l remainin g sample s an d associate 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
.

Pag e 2 3 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g



### 12 Attachments Attachmen t A : Protoco l Amendmen t 2 2 (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 Attachmen t D : Metho d Deviatio n

Pag e 2 4 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g

13 Signatures

' Date Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r

Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yDepartmen t Manage rDat e



# 1 Gar yHohenstein , Sponso rRepresentative



# z . Date

Jaisimh a Kesari , StudyDirecto r Dat e

Pag e 2 5 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 2 6 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g 

### Analytical

Protocol:

GLP10-01-01 Amendment

22
Study Title Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Gribundwater , 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 . 2 2

Amendmen t Date : Septembe r14 , 201 1 Performing

Laboratory 3 M Environmental , Health , an d Safet yOperation s

3 M Environmenta l Laboratory Buildin g 260-5N-1 7 IVIaplewood , M N 55144-100 0 Laboratory

Project Identification GLP10-01-0 1 Sampling

Event Decatu r3"

^ Quarte rGroundwate rSamplin g

Pag e 1 o f7 Pag e 2 7 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Amendment

22 Thi s amendmen t modifie s th e followin g portio n o fprotocol : "Analysi s o f Perfluorooctanoi 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 "

PROTOCOLREADS: N o change s to th e wordin g o f th e prdtOGpl ar

e required
.

AMEND TO READ: N o change s t o th e wordin g o f th e protoco l ar

e required
. Thi s amendmen t onl yaddresse s an d documents th e additio n of th e Genera l Projec t Outlin e (GPO) fo rth e collectio n an d analysi s ofgroundwate rsample s a t Decatur , AL , an d conducte d a s par t o f th 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 ofth e wee k ofSeptembe r19
. Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d into thi e 3 M Environmenta l Labbrator yLIM S a s projec t GLP10-01-01-2 2 an d reporte d as Interi m repor t GLP10-^01-01-122 , (reflectin g stud yGLPiO-01 - 0 1 an d amendmen t -22)
.
Reason : Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Projec t Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio p even t t o b e conducte d fo rth e 3 M Decatur , A L facility
. Th e GP O i s fou rpages i n lengt h an d included a s attached t o thi s amendment fonn
.

Pag e 2 of7 Pag e 2 8 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Arriendmeht

22 Amendmen t Approva l

Gar yHohen ; tein , Sponso rRepresentativ e Dat e 

# 7}i4jzill Dat e Clesto n C
. Lange , Principa l Analytica l Investgato r

Willia m Reagen , EH C Opn s Environmenta l La b Managemen t Dat e

I Dat ^ Jaisimh a Kes ; E , Stud yDirecto r

Pag e 3 o f 7 Page 29 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Anhendment22 <«J|V I Environmenta l Healt h & Safet yOperations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gar

yHohenstein , 3 M EHS&Qpn s From : Susa n Wolf , 3M EHS&Opns ; Environmenta l Lab cc : Willia m Reagen , 3 M EHS&Opns ; Environmenta l Lab

Clesto n Lange , 3 M EHS&Opns ; Environmenta l Lab Ja i Kesari , Westo n Solution s Charies Young , Westo n Solution s Date : Septembe r14 , 201 1 Subject : Analysi s o

f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Related.Monitorin g Program ; GL P Interi m Repor t 2 2 - Decatu r3" " Quarte r201 1 Groundwate rSamplin g 1 Genera l Projec t Informatio n
3 M 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 aahohenstein®mmrn.co m 3I WEnvironmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S opns , Environmenta l Lalwrator y 250-5N-1 7 65 1 733-973 9 Contact s wkreaaen ® 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 cclanoe®mmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinak®westonsolutions.co m Phone ; (334)-332-912 3 La b Reques t Numbe r GLP10-01-01-2 2 Si xDigi t Departrlien t Numbe r Dep t #530711 , Projec t #002267444 9 Projec t Sctiedule/Tes t Date s Samplin g schedule d fo rth e wee k o fSeptembe r19 , 201 1 Ail verbal and written correspondence will be directed to Gary Hohenstein.
Pag e 4 o f7 Pag e 3 0 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Amendment

22 

### 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laboratory(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundvyate r sample s collecte d ;frori i seventee n groundwate rwell s fo rPerfluorooctanoi cAci d (PFOA)
. Analyse s wil l b e conducte d unde rth e GL P requirerfient s o fEP ATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792
. Groundwater-sample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k o f Septembe r1.9 , 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 f a know n precisib n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-01-22
. 

### 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b yth e 3 M Environmenta l Laboratory
. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l byFriday , Septembe r16 , 2011
. Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection
. Marti n Smit h \

Westo n Traile r 3M ! Decatu rPlan t 140 0 Stat e Dock s 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 o f eightee n samplin g location s have bee n specified : Fo reac h samplin g location , fou rsampl e bottle s wil l b e collecte d (sample , sampl e duplicate , lo wfiel d matri xspike , an d hig h field matri xspike)
. The"fiirt o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 2.0 0 mL
. Tw o set e o f tri p blan k spike s consistin g o f reagent-grad e water , a s wel l a s tw o additiona l bottle s t o b e use d fo rth e preparatio n o fequipmen t rinseate blanks , wil l b e prepare d a t th e 3 M Environmerita l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles
. Result s fro m GLP10-01-01-02 , GLP10-O1-O1-O9 , an d GL P 10-01-01-1 7 wer e use d t o determin e th e fiel d matri xspik e level s forGLP10-01-01-2 2 liste d i n Tabl e 1
. Tabid . Samplin g Location s an d Fiel d Matri x Spik e levels . Wel l No . Sampl e Leve l Spik e Cone . (ng/mL ) 317 L Lo w 1 Hig h 1 0 220R , 220L , 328 L Lo w 1 0 Hig h TO O 203L , 222R , 227R , 227L , 3 1 OR , 324L , 327R , 330L , an d 331 S Lo w 10 0 203L , 222R , 227R , 227L , 3 1 OR , 324L , 327R , 330L , an d 331 S Hig h 100 0 GRS04 , 312R , 330R , an d 335 S Lo w 100 0 Hig h 500 0 328 R Lo w 10 0 Hig h 50 0 Tri p Blan k

Set s 1 an d 2 Lo w 1 0 Tri p Blan k

Set s 1 an d 2 Mi d 10 0 Tri p Blan k

Set s 1 an d 2 Hig h 100 0

Pag e 5 o f 7 Page 3 1 o

f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Amendment

22 

### 5 Tes t Method s Sample s wil l b e prepare d an d analyze d byLC/MS/M S followin g ETS-8-044. 0 "Detenninatio n o f Perfluorinate d Compound s I n Wate rb yHig h Performanc e Liqui d Chromatography/Mas s Spectrometr yDirect Injectio n Analysis"
. Duet o previou s dat a fo rthes e samplin g location s (GLP10-01-01-02 , GLP10r01-01-09 , an d GLPlO 01-01-17) , sample s GLP10-01-01-2 2 wil l mos t likel yrequir e dilution
. Sample s requirin g dilutio n wil l be " prepare d i n Milli- Q wate rprio rt o analysi s byETS-8-044.0
. Th e dat a qualit yobjective s fo rthes e studie s ar e quantitativ e result s fo rth e targe t analyte s wit h a n analytica l accuracyo f 100±30%
. Fiel d matri xspike s not yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor t an d th e fina l accuracystatemen t mayb e adjuste d accordingly
. Alternately , sample s mayb e analyze d b yET S 8-110. 1 "Analysi s o f Fluorochemical s i n Extract s Usin g HPLC Electrospray-Mas s Spectrometry-Mas s Spectrometry " a s a n analytica l referenc e fo rth e sampl e tocations analyze d b ydirect onTcolum n injectio n analysi s o fsample s dilute d wit h methano l a s oppose d t o Milli- Q water . Calibratio n curve s use d fo rbot h ETS-8^044. 0 an d ETS-8r110. 1 vvil l b e cohstmcte d usin g a referenc e materia l containin g bot h linea ran d branche d isomers o fPFOA
. Fiel d matri xspike s wil l b e prepai-e d wit h a solutio n prepare d wit h a referenc e materia l containin g predominantl ylinea rPFO ALaborator ycontro l sahnple s (LCS ) o f linea ran d branche d PFO Awil l b e prepare d a t thre e concentratio n levels
. 

### 6 Reportin g Requirement s . Fo reac h samplin g location , th e report ; wil l contai n th e result s fo rth e sample, , sampl e duplicate , an d th e fiel d matri xspikes
. Tri p blarikset s wil l b e reporte d fo rth e samplin g event.a s wil l an yequipmen t blank s prepare d i n th e field
. Laborator

ycontro l spike s o freagen t wate rprepare d at th e time o f sampl e extractio n willials o b e reporte d an d use d t o evaluat e th e overal l metho d accuracyan d precision
. Metho d blank s o f reagen t wate r prepare d at th e tim e o f sampl e extractio n wil l b e use d t o determin e th e metho d detectio n limit
. An ylaborator y matri xspike s tha t mayb e prepare d wil l als o b e include d I n th e fina l report . 7 Emai l Correspondenc e Attachmen t A : Samplin g Bottl e Reques t

Pag e 6 o f 7 Page 3 2 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample

s 3r d Quarte r201 1 Samplin g Analytical

Protocol:

GLP10-01-01 Amendment

22 From : Frinak , Timoth yR
. Sent : Monday , Septembe r12,.201 1 10:4 8 A M To : Young , Charle s T
. Cc : Smith , Martin ; Johnson , Kevi n A. ; Missildine , BretC
. Subject : Bottle s - G

W samplin g Decatur , A L Charlie , Th e S" ' quarte rG W samplin g wil l begi n nex t Monda ya t Decatijr
. Th e samplin g fo rPC s wil l b e insid e thi s tim e an d includ e th e following : 203 L 220 R 220 L .222 R 227 R 227 L 31Q R 317 L 324 L 328 R 328 L 330 R 330 L 335 R GRS0 4 RW312 R RW327 R RW331 S W e wil l als o nee d Milli- Q wate ran d bottle s fo rtw o (2 ) rinseat e blan k samples
.

Pag e 7 o f7 Page 3 3 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g


### ATTACHMEN TB : REPRESENTATIV E SAMPL E CHROMATOGRAM S AN D CALIBRATIO N CURVE(S )

Pag e 3 4 o f 5 6»* * Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g Batc hName : blllOOTa.da b
b111007a.rd b (PFOA) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -2.44e+00 3 x" ! + 6.94e+00 5 x+ 2.25e+00 4 ( r= 0.9995 )

4 0 4 5 5 0 5 5 Concentration , ng/m L Dat a printe d b yST W Printin g Time : 10:12:4 1 A M Printin g Date : Thursday , Novembe r 03 , 201 1 Pag e 1 o f 1 Pag e 3 5 o f 5 6Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g Batc hName : blll007a.da b 

# I SampI o Name : "b l 11007b018 ' Sampl a ID r"10007-27-9 " Fila : "b l 11007b, w Pea k Name : 'PFOA ' Mass(es) : MlS.O/SeS. O aimj.413.0/219. 0 amu.413.(V16 ! Commen t -2. 5 ng/m L F C st d I n M D Q Water " Annolatior : ~ Sanpl a Index : 1 8

Modified : Ye a Proc . Algocithm : IntelliQ i Mill . Peak

Height : 0.0 0 Min . Pea) : Width : 0.0 0 Smoochin g Width : 0 R T Window : 30. 0 Expecte dRT : I • Sa r I Pe a • Co r

! Rel a • RT :

14. 8 15. 0 2819 ^ 285 7 Sampl e Name : "b l 11007a029 ' Sampl e ID : 'Solven t Blank ' File : "b l 11007a.wif r Pea k Name : TFOA ' Mass{es):'413.0/369. 0 amu,413.0/219.0amu,413.Cl/169. 0 Commen t 'MID I Q Wate rTN1 1 -0333 * Annotation : -

Modified : Proc . Algorithm : I n Min . Pea k

Width : Smoothin g Width : 0 R T Window : Expecte dRT : ! Rela l Retentio n ' Area : Height : ! RT :

I Sampl e Name : •b111007a030 ' Sampl e ID:'LCS-111007- rFOe : "bl l 1007a.wtf r Pea k Name : 'PFOA ' Mass{ett) : '413.0/369. 0 a) • Commen t '2pp b LCS " Annotatwn : ~ Sanpl a Index : 3 0 SADpl e Type : O C Concentration : 1.9 1 ng/m L Calculate d Cone : 2.8 0 ng/m L Acq . Date : 10/8/201 1 Acq . Time : 2:27:2 5 A M ^.413.0/169. 0 amu ' 

# I Sampl e Name : •b111007a033 ' Sampl e ID : 'LCS-111007-4 ' File : "b l 11007a.wi r Pea k Name : 'PFOA * Mas5(es) : '413.0/369. 0 amu,413.0«19. 0 amu,413.0/169, 0 am u Commen t '20pp b LCS * Annotation ; ~

i l f ie . Ye a Peoc . Algorithm : InColliQua n Min . Pea k Height : 0.0 0 Min . Pea k Width : 0.0 0 Smoothin g Width : 0 R T Window : 30. 0 Expecte d BT : 14. 9 cp s

! Rel i
Height : Star t T i En dTiro < IRT : H o

4 .00e*00 5 cp 9 14. 7 mi n 15. 0 mi n 3.6e 5 3.4e 5 3.2e S 3.0e S 2.ee 6 2.6e 5 2.4e 5 2.2e 5 2.0e 5

6.0e4 4.0e 4 2.0e 4 ^4.0 7 14.24 ^ 14.3 0 14.55^4.5 6

. 0 14. 2 14. 4 i 6 270 4 274 2 R Twindo t

Height : Star t T J En dTira « 1.6e 6 1.4e 6 1.2e 6

. 15.7 3 15.90^.^ 15. 0 281 9 285 7 Time , mi n Dat a printe d b yST W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , Novembe r 03 , 201 1 Pag e 1 o f 7 Pag e 3 6 o f 5 6Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g Batc hName : blll007a.da b 

# I Samp*eName:T)111007a036 ' Sampl e ID : •LCS-111007-7 ' File : 1>111007a.wi r Pea k Name : *PFOA * Mas9(es) : '413.0/369. 0 8mu.413.0/2ig. O amu.413.0/169. 0 a n Commen t 'SOpp b LCS * Anrwtation : " " Sampl e Index : 3 6 Sampl e Type : O C Concentration : 47. 7 ng/m L Calculate dCone : 62. 0 ng/m L Acq . Date : lO/B/201 1 Acq . Time : 4:34:0 2 A H 5.0e

6 Modified : Ye a Proc . Algorithm : IntelliQua n - IQ J Min . Pea k Height : 0.0 0 cp s Min . Pea k Width : 0.0 0 se c Smoothin g Width : 0 point s R T Window : 30. 0 se c Expecte d RT : Rela l [ RT : Retentio i Height : Star t Ti r En d Tim e 14. 9

370120 4 1 5.44eiO0 6 Sampl e Name : "b l 11O07aO43 ' Sampl e ID : 'GLP10-01-01-22-082 - Fie : 'b111007a.wiff ' 

# I Pea k Name:'PFOA - Mass{esJ:*413
. Commen t 'DA L G W 203 L RB * Annotation : Sampl e Index : 4 3 Sampl e Type ; iu.413.0/219. 0 amu.413.0/169. 0 a i Unknow n N/ A

Modified : Proc . Algorithm i Min . Pea k

Heigh t Mi n. Pea k

Width i i g Width i R T Wl i 1 RT :

Height : Star t Ti n

14. 8 15. 0 281 9 265 7 I SampleName:-b111OO7a059 ' Sampl e ID : •GLP1^01-01-22.00 rFle:'b111007a.wtf r Pea k Name : 'PFOA ' Mass(es} : '413.0/369. 0 a i • Conunen C 'DA L G W 203 L 0 ' Annotation : * Sampl e Index : 6 1 Sampl e Type : Unknow n

itelliQua i 0.0 0 1 0.0 0 ! j,413.0/219. 0 amu.413.0/169. 0 amu '

3.8e5
- 3.6e5
- 3.4e5
- 3.2e5
- 3.0e5
- 23e5
- 2.6e5
- 2.4e 5 2.2e 5 2.0e5
- 1.8e5
- 1.6e5 1.4e5
- 1.2e5
- 1.0e5
- 

## ( Sampl e Name : •b111007a063 * Sampt e ID : 'GLP10-01-01-22-005 ' Flle:'b111007a.wi r Pea k Name : TFOA ' Mass{es) : '413.0/369. 0 amu,413.0/219. 0 amu,413.0/169. 0 amu ' Commen t 'DA L G W220 R 0 " Anwtation : - Sampl e Index : 6 5 Sampl e Type : Unknow n

8.0e4 6.0e 4 4.0e 4 2.0e 4 14.06^14.17.. , 14.2 3 Calculate d Cone : 28. 8 ng/m L Acq . Date : 10/9/201 1 Acq . Time : 12:44:2 9 P M Modified : Ye s Proc . Algorithm : IntelliQua n - IQ A Min , Pea k Height : 0.0 0 cp s Min . Pea k Width : 0.0 0 se c Smoothin g Width : 0 point s R T Window : 30. 0 se c Expecte d RT : Rela l ! RT : N o

Area : 394053 7 count s Height : 7.22e*00 5 cp s Star t Time : 14. 4 rain 7.0e 5 6.5e 5 6.0e 5 5.5e 5 5.0e 5 4.5e 5 4.0e 5 3.5e 5 3.0e 5 2.5e 5 2.0e S 1.5e S 1.0e S

15.4 6 ^15.5 6 15.7 6 14. 8 15. 0 281 9 285 7 Time , mi n 14. 8 281 9 285 7 Time , mi n Dat aprinte db y ST

W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , November 03 , Pag e 2 o f 7 Pag e 3 7 o f5 6** * Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3r d Quarte r201 1 Samplin g Batc hName : blllOOVa.da b

Fie : •b111007a.wtf r

IntelliOua r : 0.0 0 1 0.0 0 i I SampleName:"bll1DO7a071 ' Sampl e ID:'GLP1CM)1-01-22-009 - Pea k Name:'PFOA ' Mass[es):'413.0/369. 0 amu.413.0/219. 0 amu,413.0/169. 0 amu ' I Comment-DA L G W 220 L 0 ' Annotation : "
1.20e6
- 1.15e6
- 1.10e6
- 1.05e6
- 1.00e 6 9.50e 5 9.0Oe5
- 8.50e5
- e.00eS
7.50e5
- 7.00e5
- g - 6.50eS
- ^ 6.00e5
- I5.50e 5 5.00e 5 4.50e5
- 4.00e5
- 3.50e 5 3.00e 5 2.50e 5 2.00e 5 1.50e5
- 1.00e5 5.006 4 0.0 0 

# I Sampt e Name : t i 11007a075 ' Sampl e ID ; 'GLPKM ) 1-01- 2 Pea k Name : TFOA ' Mawfes) : '413.0/369. 0 amu,413.0/21 9 Commen t 'DA L G W222 R 0 ' /^nfwtatwn : ~ Sampl e Index : ^ ^ Sampl e Type : Unknow n Calculate dCone : 359 . ng/m L Acq . Date : 10/9/201 1 Acq . Time : 4:57:3 4 P M Modified : Ye s Proc . Algorithm : IntolliQua n - IQ A Min . Pea k Height : 0.0 0 cp s Hln . Pea k width ; Smoothin g Width : R T Window : 0 . 0 0 0 30. 0 14. 9

Height : En dTi n

15. 0 281 9 285 7 Time , mi n 

# I Sampl e Name : •b111007a083 ' Sarr^ e ID : •GLPl(W)1-01-22-017 ' Fie : •b111007a.wtt r Pea k Name : 'PFOA ' MassfesJ : '413.0/369. 0 amu,413.0/219. 0 amu.413.0/169. 0 amu ' Commen t *DA L G W227 R 0 ' Annolatkw: "
Calculate dCone : 247 . Acq . Date : 10/9/201 1 Acq . Time : 7:46:1 4 1 Modified : Ye s Proc . Algorithm : IntelliQ i Min . Pea k Height : 0.0 0 Min . Pea k Width : 0.0 0 Smoothin g Width : 0 R T Window : 30. 0 Expecte d RT : • Rela i • RT :
Height ; Star t En dTi t 1.3e 6 1.2e6

9.0e 5 8.0e S

3.06 5 2.0e 5 

# I Sampl e Name : •b111007a087 ' Sampt e ID : •GLP10^1-01-22-02 rFile : •b11l007a.w« r Pea k Name : "PFOA ' Mass(8s) : '413.0/369. 0 amu,413.0/219. 0 amu,413.0/169. 0 amu ' Commen t "DA L G W227 L 0 ' Annotation : "

Modified : Mi n R T Window : Expecte dRT : Us e Relativ e Retentio n T i Area : Height : star t Time : IntelJiCJu ; LHeight : 0.0 0 : Width : 0.0 0 IWidth : 0 f • : 30. 0 RT :

9.10o*00 5 cp s

15. 0 281 9 285 7 Time , mi n Dat a printe d b yST W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , Novembe r 03 , 201 1 Pag e 3 o f 7 Pag e 3 8 o f 5 6Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g Batc hName : blll007a.da b 

# 1 

# " ^ . Pea k Name:'PFOA * Ma3s(es):'413.0/369. 0 a i Commen t

"DA LG W310 R0 ' Annotatkjn: ' Sampl e I Sampl e Name : ti l 1007a095 ' Sampt e ID : •GLP1O^1-01-22-025 ' Fle:-b111007a.wit r ' - • • 119.0amu,413.0/169.0amu ' Type : Calculate d Cone : Acq . Date ; Acq . Time : Modified : Proc . Algorithm : Min . Pea k Height : Min . Pea k Width : Smoothin g Width : R T Window : Expecte d RT : Unkn i N/ A

! Rela l • RT : 1.15e 6 1.10e 6 1.0Se6 1.00e 6 9.50e 5 9.00e 5 8.50e 5 6.00e 5 7.506 5 7.00e 5 § • 6.50e 5 ^ 6.00e 5 I5.50e 5 5.000 5 4.50e 5 4.00e 5 3.50e 5 3.00e 5 2.50e 5 2.00e 5 1.50e 5 1.00e 5 5.00e4 0.0 0 14. 6 15. 0 261 9 285 7 Time , n Sampl e Name : "b l 11007a099 ' Sampt e ID : "GLP10-01-01-22-029 * File : "b l 11007a.wi r



# I Pea k Name : 'PFOA ' Mass(es) : '413.0/369. 0 Commen t

'DA LGW312 R0 " Annotation: ~ Sampl e Index : 10 1 Sampl e Type : Calculate dCo r Acq . Date : Acq . Time : Modified : Unknow n H/ A 1 9 60 . I 10/10/201 1 1:24:0 5 A

M IntelliQ i 0 .0 0 0 . 0 0 Expecte d RT : Us e Relativ e Int . Type :



# I Sampl e Name : ti l 1007a10 r Sampte ID : •GLP10-01-01-22-033 ' Fie : •b111007a.wif r Pea k Name : 'PFOA ' Mass(e5l : *413.0/369. 0 amu.413.0/219. 0 amu,413.0/169. 0 amu " Commen t

*DA LG W317 L0 ' Annotation ; ~ Sampl e Index : 10 9 Sampl e Type ; Unknow n Concentration ; (J/A Calculate dCone : 0.34 0 ng/ro L Acq . Date : 10/10/201 1 Acq . Time : 4;13;1 7 A M itelliOua i 0.0 0 1 0.0 0 : Snoothin c I SampleName:"bll1007a1i rSampt e ID:'GLP10-01-01-22-03 rFilo:t111007a.wi r Sampl e Type : Concentratio n Calculate dCo i

Smoothin g Wi

c R T Window : Expecte dRT :

Height : Star t Tl r En dTime :

14. 6 15. 0 281 9 285 7 Time.,mi n, 7.5eS
7.0e5
- 6.5e5
- 6.0e5
- 5.5e 5 5.0e5
- 4.5e5
- 4.0e 5 3.5e 5 3.0e 5 2.5e 5 2.0o 5 1.5e5
- 1.0e5
- 5.0e 4 0.0
- 15.5 0 ^15.5 9 15.7 9 15. 0 281 9 285 7 TImg . mi n Dat a printe d b yST W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , Novembe r 03 , 201 1 Pag e 4 o f 7 Pag e 3 9 o f 5 6Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s of PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g Batc hName : blll007a.da b

I SampteName:t111007a119 ' Sampt e ID:'GLP1tM)1-01-22-041 * Fie : t111007a.w« r Pea k Name:*PFOA * Mass(es):'413.0/369.0a i • Comment-DA L G W327 R 0 ' Annotatton: ' Sampl e Index ; 12 1 Sampl e Type : Unknow n Concentration : M/A Calculate dCone : 645 . ng/m L Acq . Date : 10/10/201 1 Acq . Time : 8:26;5 5 A M Modified : Ve s Proc . Algorithm : IntelliOua n- IQ A Min . Peak

Height : 0.0 0 cp s Min . Peak

Width ; 0.0 0 se c Smoothin g Width : 0 point s iu,413.0/169.0emu '

R T [indo i 1.2e6 ' 1.1» 6
Height : Star t Time : En dTime ;

14. 8 15. 0 281 9 285 7 Time , mi n 

# I Sampl e Name : t i 11O07a123 ' Sampt e ID : ' i Pea k Name:'PFOA * MaM(es):'413.0/369. 0 Commen t 'DA L G W 32e R 0 ' Annotatwn : Sampl e Index ; 12 5 Sampl e Type : Unknow n

Modified ; Proc . Algorithm : I i Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width ; ( R T Window : Expecte dRT ; 2.1e 6 2.0e 6
1.8e 6 1.7e 6

7.0e 5 6.0e 5 5.0e 5 4.0e 5 3.0e 5 2.0e 5

15. 0 261 9 285 7 

# I Sampt e Name : t111007a131 ' Sampt e ID:' ( Pea k Nanw:'PFOA ' Mass(esJ:'413.0/369. 0 Commen t 'DA L G W328 L 0 ' Annotation : ~ Sampl e Index : 13 3 Sampl e Type ; Unknow n Concentration : N/A Calculate d Cone : 100
. ng/m L Acq
. Date : 10/10/201 1 Acq
. Time : 12:40:2 2 P M Modified :
, Algorithm : Peak Height ; Peak Width : ihln g Width : itelliQu )

0.0 0 0.0 0

Star t Time : 1.10e6 - 1.05e 6 1.00e 6 9.50e 5 9.00e 5 8.S0e 5 8.00e 5 7.50e 5 7.00e 5 6.S0e 5 6.00e 5 5.50e 5 5.00e 5 4.50e 5 4.00e 5 3.50e 5 3.00e 5 2.50e 5 2.00e 5 1.50e 5 1.00e 5 5.00e 4 0.0 0 

# I Sampt e Name : t i 11007a135 ' Sampt e ID : ' < Pea k Nanw:-PFOA ' Mass(e9):'413.0/369. 0 Commen t 'DA L G W330 R 0 ' Annotetten : - Sampl e Index ; 13 7
Acq . Time : Modified ; Proc . Algorith m Min . Pea k Heigh ( Min . Pea k Widt h Smoothin g Widt h itelliQua n • 0.0 0 cp [ 0.0 0 se t
I RT : 4.8e 5 4.6e 5 4.4e 5 4.2& 5 4.0e 5 3.8e 5 3.6e 5 3.4e 5 3.2e 5 3.0e 5 2.8e 5 2.6e 5 2.4e 5 2.2e 5 2.0e 5 1.8e 5 1.6e 5 1.4o 5 1.2e 5 1.0e 5 8.0e 4 6.0e 4 4.0» 4 2.0e 4 14. 6 15. 0 261 9 285 7 Time , mi n 15. 0 281 9 285 7 Time , mi n Dat aprinte db y ST

W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , November 03 , Pag e 5 o f 7 201 1 Pag e 4 0 o f 5 6Buste r J293020 3 GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g Batc hName : blll007a.da b

I SampteName:t111007a143 ' Sampt e ID:'GLP1{M)1-01-22-O5 rFie : t111007a.wit r Pea k Name : "PFOA * Mass(es) : '413.0/369. 0 a • Comnrten t

"DA LGW330 L0 ' Annotafion : " " Sampl e Index : 14 5 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 366 . ng/m L Acq . Date : 10/10/201 1 Acq . Time : 4:S3;3 2 P M Modified : Ve s
Smoothin g width : R T Window : Expecte dRT : Us e Relativ e RT :
Height ; En dTime : iu,413.0/219. 0 amu,413.0/169. 0 a i

6.5o 5 6.0e 5 7.5e 5 7.0c5 6.5e 5 6.0e 5 5.5e 5 5.0e 5 4.5e 5 4.0e 5 3.5e 5 3.0e 5 2.5e 5 2.0e 5 1.5e5 1.095
- 5.0e4
14. 8 15. 0 281 9 285 7 Time , mi n Sampt e Name : t111007a14 rSampt e ID : •GLP10-01-01-22-061 ' FJe:t111007a.wif r



# I Pea k Name : 'PFOA ' Massfes) : *413. i Commen t 'DA L G W331 S 0 " Annolatton : Sampl e Index ; 14 9 Sampl e Type : Unknow n Concentration : K/ A Calculate dCone : 744 . ng/ra L Acq . Date : 10/10/201 1 Acq . Time : 6:18:1 6 P M Modified : Ye s Proc . Algorithm : IntelliQua n- IQ J Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 se c Smoothin g Width : 0 point s R T Window ; 30. 0 se c Expecte dRT : 14. 9 mi n Us e Relativ e RT : N o
Height : iu,413.0/219. 0 amu,413.0/169. 0 amu '

I.7e 6 1.6e 6 1.5e 6 1.4e 6 13e 6 1.20 6 1.1e 6 1.0e 6 9.0e 5 8.0e 5 7.0e 5 6.0e 5 5.0e S 4.0e 5 3.0e S 2.0e 5 1.0e5
- 0.0 - 14. 8 15. 0 281 9 285 7 Time , mi n 

# I SampteName:t1l1007al55 ' Sampl e ID : •GLP10«1-01-22-065 ' Flo:t111007a.w« r Pea k Name : "PFOA ' Mass(es) : "413.0/369. 0 amu,413.0/219. 0 amu.413.0/169. 0 amu ' Commen t 'DA L G W335 R 0 ' Annotation: " Sampl e Index : 15 7 Sampl e Type ; Unltnow n
9:07:1 9 P

M 

## ( Sampl e Name : t111007a159 ' Sampt e ID : *GLP10-01-01-22-069 ' FIte : t111007a.wi r Pea k Name : -PFOA ' Mass{es) : -413.0/359. 0 amu,413.0/219. 0 amu.413.0/169. 0 amu " Comment'DA L G W GRS0 4 0 * Amolatian: -

Smoothln g Width : IntelliQua n- IQ A Min . Pea k

Width ; Expecte dBT :
Retentio n Ti n
En dTime : 2.91e+00 6 cp s

Dat a printe d b yST W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , Novembe r 03 , 201 1 Pag e 6 o f 7 Pag e 4 1 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3r d Quarte r201 1 Samplin g Buste r J293020 3 Batc hName : blll007a.da b 

# f Sampl e Name : t111007t>00 rSampl e ID:'LCS-111010-01 ' Fite:-b111007b
. Pea k Name : *PF0A ' Mass(«a) : '413.0/369. 0 amu,413.0/219. 0 amu.413.0/169. 0 amu ' Comment : 'SOOpp b LCS ' Annotation : " Sampl e Index ; 2 Sampl e Type : Q C Concentration ; 500 . ng/m L Calculate dCone : 478 . ng/m L Acq . Date ; 10/11/201 1 Acq . Time : 1:41:4 9 A M
Peak Height : Smoothin g 1 R T Window ; Expecte dR :

Height : Star t Ti l En d Tim e 7.69e»00 5

14. 8 15. 0 281 9 285 7 Time , mi n

Dat a printe d b yST W Printin g Time : 10:11:0 9 A M Printin g Date : Thursday , Novembe r 03 , Pag e 7 o f 7 Pag e 4 2 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g


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

Pag e 4 3 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO AI n Groundwate rSample s

3rd Quarte r201 1 Samplin g 

# 3IV I Environmenta l Laborator y

Method Method of Analysis

for the Determination

of Perfluorinated

Compounds

in Water by LC/MS/MS;

Direct Injection

Analysis Method Number:

ETS-8-044.0 Adoption

Date: Upon Signing Effectiv e Date : Q ^^r g y/< 3 7
Approve d By :

Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 IVlethod of Analysi 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 4 4 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g


### 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 Perfluorooctanesulfonat e (PFOS ) b yHig h Perfonnance Liqui d Chromatograph ycouple d t o a tande m Mass Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples
. Wate rsample s containin g heav y particulat e ma

yrequir e preparatio n b

ya n altemat e metho d suc h a s ETS-8-15 4 "Determinatio n of 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 a s th e define d Q C elements are satisfied
. Sampl e collectio n i s no

t covere d unde rthi s analytica l procedure . 2 Metho 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

yno t 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 determine 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 % ofth 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 of 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 ofth e Workin g Standar d (WS ) into a predeteimine d amoun t of AST 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 instrumen t respons e wit h respec t t o analyt e concentration
. 3. 2 Laborator y Duplicat e Sampl e (LDS , o r La b Dup ) Alaborator

yduplicat e sampl e i s a separat e aliquot o fa 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 f th 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 Blan k

(FB)/Tri p Blan k 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 referre d t o a s a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o f Analysi 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 4 5 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g
3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n a s 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 o

f th e FD S compare d t o that o fth e firs t sampl e give s a measur e ofth 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 ofth e targe t analyte s are adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n of aqueou s samples
. Aknown , specifi cvolum e of 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 of th 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 of analyt e concentration s i s unknown , multipl e spike s a t 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 of AST 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 ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e 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 of analyt 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 no t 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 place a s eac h FMS
. 3. 7 Laborator y Contro l Sampl e (LCS ) A n aliquot o

f contro l matri xt o whic h know n quantitie s o fth e targe t analyte s ar e adde d i n th e laborator

yat th e tim e o

f sampl e extraction
. A

t leas t tw o level s are included , on e generall ya t th e lo wen d o fth e calibratio n curve an d on e nea rth e mi d t o uppe rrang e ofth e curve . Th e LCS s are extracte d an d analyze d exactl ylik e a laborator

ysampl e t o determin 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 y Matri xSpik e (LMS ) Alaborator

ymatri xspik

e i s a n aliquot of a 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 ylike a laborator ysampl e t o determin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results
. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmus

t b e determine 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 of aqueou s samples
. 3. 9 Laborator y Sampl e Aportio n o raliquot of a 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 of quantitatio n (LLOQ ) fo ra dataset i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits of precisio n an d accurac ydurin g routin e operatin g conditions
. T o simplif ydat a reporting , th e LLOQ 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 of quantitatio n (ULOQ ) fo ra dataset i s th e highest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o f precisio 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 a s th e ULOQ
. ETS-8-044. 0 Pag e 3 o f 1 1 Metho d o f Analysi s fo rth e Determinatio n o f Perfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 6 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g 

### 3.1 1 Method Blan k A n aliquot of contro l matri xthat i s treate d exactl ylik e 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 determin e i f tes 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 yofmateria l intende d t o represen t th e origina l source material
. 3.1 3 Stoc k

Standar d Solutio n (SSS ) Aconcentrate d solutio n of a 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 no t nomnally foun d i n th e sample(s)
. Asun"ogat 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
. Sun'ogate(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 o fa sun'ogate analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired
. 

### 3.1 5 Workin g Standar d (WS ) Asolutio n of severa l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o prepar e 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 yo f th e standard s fo rthi s metho d have no t bee n precisel ydetermined ; 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 exposur e 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 curren t awarenes s o floca l regulation s regardin g th e handlin g of th e chemical s use d i n thi s method
. Areference fil e ofmateria 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 mus

t b e familia 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 of solvents , pressurize d gas 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 infomnatio 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 of analysi s b

yrunnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d of Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 7 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g
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 o

f disposabl 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 two solvents an d equippe d wit h a variabl e volum e injecto rcapabl e of injectin g 5-10 0 p L connecte d t o a tande m Mass Spectromete r (LC/MS/MS)
. 1 Analytica l balance capabl e o f readin g t o 0.000 1 g Adevice 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 , 25pL , 50pL , lOOpL , 250pL , 500pL , lOOOpL
. 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e of spinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi c Syste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C18,4. 6 m m x100 mm , 5 p m 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 : FlowRat e

Tim e (min ) % A % B (mL/min ) 0. 0 9 7 3 1. 0 0. 5 9 7 3 1. 0 11. 0 5 9 5 1. 0 13. 5 5 9 5 1. 0 13. 6 9 7 3 1. 0 17. 0 9 7 3 1. 0 Injectio n Volume : 100 pL
. Quantitation : Pea k

Are a - quadrati ccurve fit , 1/ xweighted
. RunTime : ~ 17minutes
. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t mayb 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 f Analysi 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 4 8 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO AI n Groundwate rSample s

3rd Quarte r201 1 Samplin g 

### 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e Transitio n Monitore d PFBA 213^16 9 PFPeA 263^21 9 PFH A 313^26 9 an d 31 3 ^11 9 PFHpA 36 3 ^ 319 , 36 3 ^

16 9 an d 36 3 ^

11 9 PFOA 41 3 369 , 41 3 - » 21 9 an d 41 3 - > 16 9 PFN A 46 3 ^

419 , 46 3 ^

16 9 an d 46 3 - > 21 9 PFDA 51 3 ^

469 , 51 3 ^21 9 an d 51 3 - > 26 9 PFUn A 56 3 ^ 519 , 56 3 ^

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

16 9 an d 61 3 - > 31 9 PFB S 29 9 ^ 8 0 an d 29 9 ^

9 9 PFH S 39 9 8 0 an d 39 9 - » 9 9 PFO S 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 ma yprovid e quantitatio n o f isomers tha t more closel ymatche s NM R dat a an d ma yhav e th e adde d benefi t o f increase d sensitivity
. Th e us e o f on 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 previous informatio

n i s intende

d a s a guide , alternat

e instrument

s an d equipmen

t ma y b 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- C4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n a s 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 (PFO A- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFNA-C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- C I 0 acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C1 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 9 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g
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 ofAmmoniu m acetat e an d dissolve i n 2. 0 L ofreagen t water . Note : Alternative volume s ma yb e prepare d a s 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 procedur

e serve s a s 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 of a particula rstudy
. Fo rexample , p L volume 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 Mg/m L targe t analyt e SSSs—^Weig h ou t 1 0 m g ofanalytica 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 of stoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. A n exampl e of purit yan d sal t connectio n i s give n belowfo rPFOS
. ^ . , ^ molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t ofsal t 49 9 PFO S (K"')sal t correctio n facto r= —= 0.927 5 53 8 1 0 m g CSFITSO/K " wit h purit y90 % = 8.35m g CSFITSOS " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 pg/m L (500 0 ng/mL ) mixe d workin g standard—^Ad d 0.5m L eac h ofth e lOOpg/m L SSS s t o a 10m L volumetri c flas k 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 pg/m L -mixe d wori<in 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 ofth e 5 pg/mL-mixe d wori<in g standar d solutio n t o a 25m L volumetri c flas k 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 procedur e 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 f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 0 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g
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 1 water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e a s a guideline
. Note : Volume s o fwate ran d woricin 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
. Concentration ofWS, ng/mL Volume of WS, fd. Final

Volume of Calibration

Standard

(mL of ASTM Type 1 Water, or other suitable water) Final

Concentration

of Calibration

Standard, ng/mL (ppb) in ASTIVI Type 1 Water, or other suitable water 12 5 1 0 5 0 0.02 5 12 5 1 5 5 0 0.037 5 12 5 2 0 5 0 0.05 0 12 5 3 0 5 0 0.07 5 25 0 2 0 5 0 0.10 0 25 0 5 0 5 0 0.25 0 25 0 10 0 5 0 0.50 0 25 0 20 0 5 0 1.00 500 0 2 5 5 0 2.5 0 500 0 5 0 5 0 5.0 0 500 0 10 0 5 0 10. 0 8 Sampl e Handlin g 8. 1 Wate r Sampl 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

yno t 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 preferre d ove rth e us e of glas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass
. Dilut e sample , i f necessary , wit h AST M Typ e 1 , 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
. Prepar e a t least fiv e metho d blanks
. 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

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

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

xo runweighted , o rb

yquadrati cfi l (

y= ax ^ + b x+ 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 fro m th e calibratio n curve s t o provid e a bette rfi t ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi 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 f thei rare a counts are no t at least twic e that ofth e metho d and/o rsolven t blanks
. Th e coefficien t of determinatio n (r^ ) valu e fo rth e calibratio n curve mus t 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 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o f Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 1 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g
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 construc t th e calibratio n curve . I f th e calibratio n curve doe s no t meet acceptance criteria , perfon n routin e maintenance o rprepar e a ne wstandar d curve (i f necessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yo fth e calibratio n curve . Analyz e a mid-rang e calibratio n standard , on e of th e sam e standard s use d t o constmc t th e calibratio n curve , a

t a minimu m afte rever ytent h sample , no

t 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 las t 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 ar e quantitate d above th e concentratio n o fth e highest standar

d i n th e curve shoul d b e furthe rdilute d an d reanalyzed
. 1 0 Qualit y Contro l 10. 1 Dat a Qualit y Objective 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 LOQ o f 0.02 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 wdata an d footnote d i n th e fina l 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 fiv e metho d blank s must b e prepared
. Metho d blank

s ma yb e injecte d multipl e times , bu t n o mor e tha n 3 injection s shoul d b e remove d fro m 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 o f th e analytica l run . 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 LOQ standard
. Th e standar

d deviatio n of th 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 of th e metho d blank s excee d 50 % o

fth e LOQ standard , the n th e LOQ must b e raise d t o th e firs t standar

d leve l i n th e curve that meets criteria , o ralternatively , 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 flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s fiel d blanks
. 10. 4 Surrogat e Spike s Sun-ogat e 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 o

ftwo 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 offiv e t o te n time s highe rtha n th e targete d LOQ an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t ofth e curve . Th e relative standar

d deviatio n of th e contro l spike s evaluate d independentl ya t eac h concentratio n leve l mus t 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 set of sample s shoul d b e re-injecte d o rre-prepare d a s appropriate
.

ETS-8-044. 0 Pag e 9 o f1 1 Metho d of Analysi 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 5 2 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFOAi n Groundwate rSample s

3rd Quarte r201 1 Samplin g
10. 6 Fiel d Matri x Spike s / La b Matri x Spike s Recoverie s of fiel d 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 o f70 % 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
. Th e targete d fortificatio n level s shoul d b e a t least 50 % ofth 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 detennin e th e statemen t ofaccurac yfo ranalytica l results
. Th e averag e of th e sampl e an d th e fiel d 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 curve (linea rregressio n parameters ) generate d b ya n appropriat e software program : Analyt e foun d (ng/mL ) = (Pea k Area-Intercept ) ^ Slop e D F = facto rb

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

- ^"^'y*®

found (ng/mL) - Average analyte found in sample (ng/mL)

^^QQ Analyt e adde d (ng/mL ) 1 2 Metho d Performanc e An ymetho d performance parameter s that are no

t achieve d must b e considere d i n th e evaluatio n o fth 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 f criteri 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 a s appropriate
. Documen t al l action s i n th e ra wdata
. I f dat a ar e t o b e reporte d whe n perfonnanc e criteri a hav e no t 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 of th e report . 

### 12. 1 Syste m Suitability Syste m Suitabilit

ystandard s are no

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

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

t th e beginnin g ofeac h analytica l nj 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 o fth 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 of^2 % t o b e compliant
. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t of detenninatio 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 sequence 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 yof eac h curve poin t mus

t b e withi n 25 % ofth 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 of1 1 Metho d of Analysi 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 5 3 o f5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g
Demonstratio n o f Specificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % o f standard ) an d th e mas s spectra l respons e ofuniqu e ions
. 12. 3 Sensitivit y Th e targete d limi t of quantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n of appropriat e blank s an d th e accurac

yofth 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 data that ar e accurat e t o +/-30%
. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d accurac yo flaborator

ycontro l spikes , fiel d 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 flagge d 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 fiel d blank s o rrinse blanks
. Sectio n 1 0 contain s additional infomnatio n regardin g the require

d precisio n o

flaborator

y control 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 o fappropriately
. Th e origina l sample s wil l b e archive d a

t th e 3 M Environmenta l Laborator yi n accordance wit h intema l procedures
. 1 4 Record s Eac h data packag e generate d fo ra stud ymust includ e al l supportin g infonnatio n fo rreconstructio n ofth e data
. Infonnatio n fo rth e dat a packag e must include , bu t i s no t 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 ru n lo g (instmmen t batc h records , instrumen 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 o f Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 4 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o fPFO Ai n Groundwate rSample s

3r d Quarte r201 1 Samplin g 

### ATTACHMEN TD : DEVIATION(S )

Pag e 5 5 o f 5 6GLP10-01-01 ; Interi m Repor t 2 2 Analysi s o f PFO Ai n Groundwate rSample s

3rd Quarte r201 1 Samplin g 

## RECOR D O F DEVIATION/NONCONFORMANC E

/. Identification stud y/ Project No
. GLP10-01-01-22 Date(s ) o f Occurrence : b111007 a Documen t Number : ETS-8-044. 0 Deviatio n typ e • SO P (Chec k one ) • Protoco l • Equipmen t Procedure 0 Metho d • GP O • Other : //. Description

(attach

extra pages as needed) Metho d Requirements : 1
. FM S (ETS-8-044. 0 sectio n 10.6) : recoverie s withi n 100 % ±30%
. Actua l procedure/process : 1
. Samplin g locatio n DA L G W 222 R H

S recover yfo rPFO Awa s 61.4%
. ///
. Actions

Taken

(such as amendment

issued, SOP

revision, etc.) Correctiv e Actio n ( • Ye s 0 No

) Reference : Acceptabilit yo f th e nonconformin g work : 1
. The non-complian

t DA L G W 222 R H

S wil l b e flagged i n th e final report . The metho d uncertaint

ywil l b e expande d fo rPFO At o ±39%
. Actions : • Haltin g of Wor k • Clien t Notificatio n • Wor k Recal l • Withholdin g o f Repor t 0 Other : Deviation s wil l b e note d i n fina l report . Projec t Lead/PA I Approval : Susa n Stud yDirecto r(i f GLP) : Sponso rApprova l (fo rGL P proTOCordeviations) : N A Date:/ , Date : N Technica l Reviewe r(optional) : N A Date : N A Laborator yDepartmen t Manage rApproval : Date : IV. Authorization

to Resume

Work Where halting of work occurred, resumption

of work must first

be approved

by Laboratory

Management Laborator

yDepartmen t Manage rApproval : N ADate : N A Deviation

No. (assigned

by Study Director or Team Leader at the end of study or project)

Attachmen t AETS-4-008. 7 Pag e l^o fJ

Documentatio n of Deviation s an d Contro l o f Nonconformin g Testin g Pag e 5 6 o f 5 6