GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 

# 3 M

GLP10-01-02 : Interi m Repor t 2 3 - Analysi s o

fPFBS . PFHS . an d PFO S i n Groundwate r Sample s Collecte d a

t th e Off-Sit e 61 0 Well s i n Decatur . A L i n Septembe r201 1

Stud y Titl e Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m Data Requiremen t EP ATSC 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 Report Completio n Date

Dat e ofsignin g Performin g Laboratory 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 St
. Paul , M N 55144 Project Identificatio n GLP10-01-02-2 3 Tota l Numbe r o

fPage s 6 0
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 fTestin g an d Calibratio n Laboratories", i n accordanc e wit h th e A2LACertificat e #2052.01 . D j Testin g tha t complie s wit h thi s Internationa l Standar d als o operat e I n accordanc e wit h IS O 9001:2000 . Testin g Cer t #2052.0 1

Pag e 1 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1



### GL P COMPLIANC E STATEMEN T Repor t Title : Interi m Repor

t 2 3 - Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a

t th e Off-Sit e 61 0 Well s i n Decatur , A L i n Septembe r201 1 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s where there i s n o specifi ctest 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 hav

e no t bee n determine d unde rGLPs
.


### 4t ; 

# l( Gar yHoh i instein , Sponso rRepresentative Date

Jaisimh a Kesari , P.ErrDEE , Stud yDirecto r

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### QUALIT YASSURANC E STATEMEN T Repor t Title : Interi m Repor

t 2 3 - Analysi s o

fPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a

t th e Off-Sit e 61 0 Well s i n Decatur , A L i n Septembe r201 1 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) 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 audite d b yth e 3 M Environmenta l Laborator yQualit yAssurance Uni t (QAU) , as indicate d i n th e followin g table
. 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 Phas e Date R e porte d t o Inspectio n Date s Phas e Testin g Facilit y Managemen t Stud yDirecto r 10/6/1 1 In-Phas e Sampl e Preparatio n 10/11/1 1 10/11/1 1 10/17-10/18/1 1 Dat a an d Repor

t 10/31/1 1 10/31/1 1



### QA U Represellativ e Date

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### TABL E O F CONTENT S GL P Compliance Statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e ofContents 5 Lis t ofTable s 6 1 Stud yInfomriatio n 7 2 Summar

y8 3 Introductio n 8 4 Test & Contro l Substance s 9 5 Reference Substance s 9 6 Test Syste m 1 7 Metho d Summar

y1 7. 1 Method s 1 7. 2 Sampl e Collectio n 1 7. 3 Sampl e Preparatio n 1 7. 4 Analysi s 1 8 Analytica l Results 1 2 8. 1 Calibratio n 1 2 8. 2 Syste m Suitabilit y1 3 8. 3 Limi t o

fQuantitatio n (LOQ ) 1 3 8. 4 Continuin g Calibratio n 1 3 8. 5 Blank

s 1 3 8. 6 La b Contro l Spike s (LCSs ) 1 3 8. 7 Analytica l Metho d Uncertaint y'.1 5 8. 9 Fiel d Matri xSpike s (FMS ) 1 5

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9 Data Summar

yan d Discussio n 1 6 1 0 Conclusio n 1 9 1 1 Data/Sampl e Retentio n 1 9 1 2 Attachments 1 9 1 3 Signature s 2 0 

### LIS TO F TABLE S Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Results (Off-Sit e 61 0 Wells ) 8 Tabl e 2 . Sampl e Descriptio n Ke yCod e 1 1 Tabl e 3 . Instrumen t Parameter s 1 2 Tabl e 4 . Liqui d Chromatograph yCondition s 1 2 Tabl e 5 . Mass Transition s 1 2 Tabl e 6 : Limi t ofQuantitatio n (LOQ ) 1 3 Tabl e 7 . Laborator

yContro l Spik

e Recover

y1 4 Tabl e 8 . Analytica l Uncertaint y1 5 Tabl e 9 . Fiel d Matri xSpik e Level s 1 6 Tabl e 10 . DA L G W6 1 O

S 11092 1 1 7 Tabl e 11 . DA L G W61OL 11092 1 1 7 Tabl e 12 . Tri p Blan k

1 8

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### 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 St
. Paul , M N 55144 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 , (clanqe(a>mmm.com) : phon e (65 1 )-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow , Analys t Kevi n Eich , 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 3 Experimenta l Termination : Octobe r8,201 1 Interi m Repor

t Completion : Date o

fInteri m Repor

t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792 . Th e tes t substanc e an d analytica l referenc e 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 7 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

2 Summary Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m two differen t well s identifie d a s th e off-sit e 61 0 Well s i n Decatur , AL
. Atota l ofeleve n sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator

yfo rperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e groundwate rsample s fro m eac h samplin g location
. Sample s als o include d tw o fiel d matri xspike (FMS ) sample s fo reac h locatio n an d on e tri p blan k

set containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes
. Th e groundwate rsample s an d tri p blank s associate d wit h GLP10-01-02-2 3 were receive d fro m Westo n personne l o n Octobe r6,2011 . Al l ofth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r 3 M projec t GLP10-01-02-23
. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s are summarize d i n Tabl e 1 . Th e tri p blan k sampl e wa s belowth e lowe rlimi t ofquantitatio n (LLOQ) , indicatin g adequat e contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections
. Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S + 9.3% , PFH S + 8.4 % an d PFOS + 14% . Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Result s (Off-Sit e 61 0 Wells).
3M LIM S I D Sampl e Descriptio n PFB S Concentratio n (ng/mL) PFH S

Concentratio n (ng/mL) PFO S

Concentratio n (ng/mL) GLP10-01-01-023-00 1 DA L G W61OS-0-11092 1 0.050 9 0.080 9 0.17 7 GLP10-01-01-023-00 2 DALGW610S-DB-11092 1 0.0544 0.085 5 0.12 8 Averag e 0.0527 0.0832 0.153 %RPD Sample/Sample

Dup 6. 6 5. 5 32(1 ) GLP10-01-01-023-00 5 DA L G W61OL-0-11092 1 0.243 0.25 0 1.3 5 GLP10-01-01-023-00 6 DA L G W61OL-DB-11092 1 0.25 2 0.26 0 1.4 7 Average 0.24

8 0.255 1.4 1 VoRPD Sample/Sample

Dup 3. 6 3. 9 8. 5 GLP10-01-01-023-00 9 DAL-GW-TRIP01- 1 <0.025 0 <0.025 0 <0.0232 Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S ±9.3% , PFH S ±8. 4 % , an d PFO S ±14% . (1 ) Th e relative percen t difference (RPD ) di d no t meet metho d acceptance criteri a of<20% .
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 ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groundwate rsample s collecte d fro m th e off-sit e 61 0 Well s locate d i n Decatur , A L fo rPFBS , PFHS , an d PFO S i n a n effor t t o characteriz e regiona l groundwate rconditions
.

Pag e 8 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

Th e 3 M Environmenta l Laborator yprepare d sampl e container s (25 0 m L high-densit

ypolyethylen e bottles ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling
. Sampl e container s fo reac h samplin g locatio n include d a fiel d sample , field sampl e duplicate , an d tw o field matri xspik

e samples
. Eac h empt

ycontaine rwa s marke d wit h a "fil l t o here " lin e t o produce a final sampl e volum e o

f20 0 mL
. Container

s designate d fo rfield matri xsample s were fortifie d wit h a n appropriat e matri xspike solutio n containin g PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o bein g sen t t o th e field fo rsampl e collection
. Al l sampl e bottle s include d th e additio n of^*02-PFBS , "Ca-PFHS , an d "Cs-PFO S (interna l standard ) a t a nomina l concentratio n of1 ng/mL
. Al l sampl e bottle s als o include d th e additio n of^^C4-PF0 S (surrogat e standard ) a t a nomina l concentratio n of0. 1 ng/mL
. Se e sectio n 8. 8 ofth e repor t fo rfield matri xspike levels
. Th e "C4-PFO S surrogat e standar d was inadvertentl yno

t include d i n th e analysi s ofth e samples
. 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 ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s I n Wate rb

yLC/MS/MS ; Direc

t Injectio n Analysis"
. Th e us e o finterna l standard s wa s use d t o ai d i n th e data qualit yobjectives
. Tabl e 1 summarize s th e averag e PFBS , PFHS , an d PFO S concentration s fo rth e duplicat e sample s collecte d an d th e tri p blank
. Table s 10-1 2 summariz e th e individua l sampl e results an d th e associate d field matri xspike 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 repor

t 

### 4 Test & Control Substances There wa s no

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

### 5 Reference

Substances
Referenc e Substanc e PFH S (linear) r'CJPFH S (linear) Chemica l Nam e Perfluorohexan e sulfonat e Sodiu m Perfluorohexanesulfonate Chemica l Formul a CeF-isSOa "Cs^CsFisSOsNa ' Identifie r Sodiu m Sal t CAS#MPFC-C-051 1 Us e Target Analyt e Reference Standar d Intema l Standar d Source Wellingto n Wellingto n Expiratio n Date 03/25/201 8 05/25/201 4 Storag e Condition s Froze n Froze n Chemica l Lo

t Numbe r LPFHxSAMO S 09231 0 TC R Numbe r TCR08-001 8 TCR11-001 6 Physica l Descriptio n Crystallin e Liqui d Purit y 98 % 5 MQ/m L

Pag e 9 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

Referenc e Substanc e PRO S (linear ) PFO S

(linea r+ branched ) ["C J PFOS (linear ) Chemica l Nam e Perfluorooctan e sulfonat e Perfluorooctan e sulfonat e Sodiu m Perfluorooctanesulfonat e Chemica l Formul a CsFiySO a CsFiySO s "CeFiySOjNa " Identifie r Potassiu m Sal t CAS #2795-39- 3 Potassiu m Sal t CAS #2795-39- 3 CAS#MPFC-C-051 1 Us e Fiel d Matri xSpik e Reference Standar

d Target Analyt e Reference

Standar d Intema l Standar d Source Wellingto n Wellingto n Wellingto n Expiratio n Date 10/18/201 8 3/17/201 4 05/25/201 4 Storag e Condition s Froze n Froze n Froze n Chemica l Lo

t Numbe r LPFOSKBM0 6 brPFOSK070 8 09231 0 TC R Numbe r TCR08-000 1 TCR11-001 0 TCR11-001 6 Physica l Descriptio n Crystallin e Liqui d Liqui d Purit y 100 % 99.9 % 5 Mg/m L

Referenc e Substanc e PFB S (predominantl ylinear ) [1802 ] PFB S (linear ) Chemica l Nam e Perfluorobutan e sulfonat e [^®02]-Ammoniu m Perfluorobutanesulfonate Chemica l Formul a C4F9SO3 C4F9S['^02]0-NH4^ Identifie r Potassiu m Sal t NA Us e Target Analyt e Reference Standar d Intema l Standar d Source 3 M RT I Internationa l Expiratio n Date 01/10/201 7 03/09/201 5 Storag e Condition s Froze n Froze n Chemica l Lo

t Numtie r 41-2600-8442- 5 11546-107- 2 TC R Numbe r TCR-12 1 TCR-1009,TCR-103 1 Physica l Descriptio n Whit e Powde r Liqui d Purit y 96.7 % >99 % (1 ) Custo m mixtur

e ofseve n mass-latiele d ("C ) pertluoroail<ylcartx)xyli cacids , two mass labele d ("C ) perfluoroalkylsulfonate s an d on e mass-labele d ('^C ) perfluoro-1-octanesulfonamide
.

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Off-Sit e 61 0 Wells ; Septembe r201 1

6 Test System Th e test system s fo rthi s stud yare groundwate rsample s collecte d fro m well s locate d i n Decatur , A L b y Westo n Solutions , Inc
. personnel
. Sample s fo rthi s stud yare "rea l world " samples , no t dose d wit h a specifi clo t o ftest substance
. Tabl e 2 . Sampl e Descriptio n Ke yCode
. Strin g Numbe r Strin g Descripto r Exampl e Example DAL-GW- 610S-LS-110921 1 Sample Location DAL= Decatur, Alabama 2 Sample Type GW= Groundwater 3 Well ID Example: DAL610 S = Epilarst L= Limestone

bedrock 4 Sampling Date 110921-September 21, 2011 5 Sample Type 0=primary sample DB = duplicate

sample LS = low spike HS = high spike 7 Method

Summary 7. 1 Metho d Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Metho d ofAnalysi s fo rth e Determinatio n ofPeriluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec 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 associate d wit h GLP10-01-02-2 3 were returne d t o th e laborator ya t ambien t condition s o n Octobe r6 , 2011 . Sample s were store d refrigerate d a t th e laborator

y afte rreceipt
. Aset oflaborator yprepare d Tri p Blan k

an d Tri p Blan k

field matri xspike s were sen t wit h eac h coole rofsampl e collectio n bottles
. 7. 3 Sampl e Preparatio n Sample s were prepare d byremovin g a n aliquot o fth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Durin g th e preparatio n ofth e laborator ycontro l samples , a n aliquot o fa separat e intema l standar d spikin g solutio n was adde d t o th e laborator ycontro l sample s (nomina l concentratio n of1 ng/mL)
. Th e sample s bottle s were spike d wit h a n interna l standar d mi xa t a nomina l concentratio n of1 ng/m L prio rt o bein g sen t t o th e field fo rsampl e collectio n 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h performance liqui d chromatography / tande m mas s spectrometr y(HPLC/MS/MS)
. Detaile d instrumen t

Pag e 1 1 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmas s transition s analyze d ar e describe d i n th e ra

wdat a har

d copie s place d i n th e final dat a packet , an d are briefi ydescribe d below
. Tabl e 3 . Instrumen t Parameters . Instrumen t Nam e ETSKiri < Analytica l Metho d Followe d ETS-8-044. 0 Analysi s Dat e 10/7/1 1 - PFB S PFO S an d PFH S Liqui d Chromatograp h Agilen t 1200 Guar d colum n Betasil 018 (4.6 mm X 100 mm), 5vi Analytica l colum n Betasi l 01 8 (4. 6 m m X 100 mm) , 5 n Injectio n Volum e 2 5 n L Mas s Spectromete r Applie d Biosystem s AP I 550 0 Io n Sourc e Turb o Spra y Electrod e Turb o io n electrod e Polarit y Negativ e Softwar e Analyst 1.5. 2 Tabl e 4 . Liqui d Chromatograph y Conditions . ste p Total

Time Flow

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

acetate) (Methanol) ETS-8-044. 0 Analyze d 10/7/201 1 0 0 75 0 97. 0 3. 0 1 2. 0 75 0 97. 0 3. 0 2 14. 5 75 0 5. 0 95. 0 3 15. 5 75 0 5. 0 95. 0 4 16. 5 75 0 97. 0 3. 0 5 20. 0 75 0 97. 0 3. 0 Tabl e 5 . Mas s Transitions .

Analyte Mass Transition Q1/Q3 Reference

Material Structure Internal Standard Mass

Transition Q1/Q3 PFBS 299/80 Linear ("OJ-PFBS 303/84

299/99 PFHS 399/80 Linear t"CJ-PFHS 402/80

399/99 PFOS 499/80 Linear & Branched t'CJ-PFOS 507/80 PFOS 499/99 Linear & Branched t'CJ-PFOS 507/80 PFOS 499/130 Linear & Branched t'CJ-PFOS 507/80 Dwel l tim e wa s 3 0 mse cfo reac h transition
. Tfi e individua l transition s wer e summe d t o produce a "tota l io n cfiromatogram " (TIC) , wtiicf i was use d fo rquantitation
.

Pag e 1 2 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Weils ; Septembe r201 1



### 8 Analytical

Results 8. 1 Calibratio n Sample s were analyze d usin g a stabl e isotop e intema l standar d calibratio n curve . Calibratio n standard s were prepare d byspikin g know n amounts o fth e stoc k

solutio n containin g th e targe t analyte s into a laboratory-prepare d syntheti cgroundwate rcontainin g calciu m an d magnesium
. Aseparat e intema l standar d spikin g solutio n wa s prepare d an d a n aliquot wa s adde d a t th e sam e leve l t o al l calibratio n standard s an d laborator

ycontro l sample s a

t a nomina l concentratio n o f1 ng/mL
. Acalibratio n curve rangin g fro m approximatel y0.02 5 ng/m L t o 2 5 ng/m L was prepared
. Samplin g locatio n DA L G W6 1 O S was quantitate d usin g externa l calibratio n fo rPFO S du e t o inconsisten t interna l standar d are a counts . Th e reference standar

d use d fo rth e calibratio n standard s fo rPFO S containe d bot h linea ran d branche d isomers
. Aquadratic , 1/

xweighted , calibratio n curve ofth e standar d pea k area/pea k

are a ratio s wa s use d t o fit th e dat a fo reac h analyte
. Th e dat a were no t force d throug h zero durin g th e fitting process . Calculatin g th e standar

d concentration s usin g th e pea k area/pea k

are a ratio s an d th e resultan t calibratio n curve confirme d accurac

yo feac h curve point
. Eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac

yrequirements of100±25 % (100±30 % fo rth e lowest curve point) were met fo ral l analytes
. Th e con-elatio n coefficien t (r) was greate rtha n 0.995 fo rPFBS , PFHS , an d PFOS
. 

### 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
. 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 % RS D was met fo rPFBS , PFHS , an d PFOS
. 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LOQ fo rthi s analysi s i s th e lowest non-zer o calibratio n standar

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

yrequirements an d fo rwhic h th e are a counts o rare a rati o are a t least twic e thos e ofth e appropriat e blanks
. Th e LO Q fo ral l analyte s ca n b e foun d i n Tabl e 6 . Tabl e 6 . Limi t o

fQuantitatio n (LOQ) . Sampling

location PFBS

LOQ, ng/mL PFHS

LOQ, ng/mL PFOS

LOQ, ng/mL DALGW610S-11092 1 0.025 0 0.025 0 0.027 8 DALGW610L-11092 1 0.025 0 0.025 0 0.0232 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibrafio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l CCV s met metho d criteri a of100 % ±25 % fo rPFBS , PFHS , an d PFOS
. 

### 8. 5 Blank s Two type s ofblank

s were prepare d an d analyze d wit h th e samples : procedura l blank s an d tri p blanks
. Procedura l blan k

results were reviewe d an d use d t o evaluat e metho d performance t o detemnin e th e LOQ fo rPFBS , PFHS , an d PFOS
. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience
.
Pag e 1 3 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1



### 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set . LCS s were prepare d byspikin g know n amounts o fth e analyt e into Mill i Q wate ro r syntheti cgroundwate rt o produce th e desire d concentration
. Th e spike d wate rsample s were the n prepare d an d analyze d i n th e sam e manne ras th e samples
. Th e metho d acceptance criteria , averag e ofLC 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 analytes
. 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
. LC S Percen t Recover

y= Calculate d Concentratio n , Spike Concentratio n 100 % LCS % RS D = standar d deviatio n LC S replicate s . ^ ^^y ^ averag e LC S recover

y Tabl e 7 . Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Intema l standar d calibration Analyze d 10/71 1 PFBS PFHS Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) XRecovery Spiked Concentration (ng/mL) Calculated

Concentration (ng/mL) VoRecovery LCS-111006- 1 0.19 8 0.22 9 11 6 0.19 8 0.21 2 10 7 LCS-111006- 2 0.19 8 0.21 3 10 8 0.19 8 0.20 5 10 3 LCS-111006- 3 0.19 8 0.21 8 11 0 0.19 8 0.20 3 10 3 Averag e ±%RS D 111±3.7 % 104 % ±2.2 % LCS-111006- 4 1.9 8 2.2 3 11 3 1.98 2.0 9 10 5 LCS-111006- 5 1.9 8 2.2 1 11 2 1.98 2.0 7 10 5 LCS-111006- 6 1.9 8 2.1 7 11 0 1.98 2.0 6 104 Averag e ±%RS D 112 % ±1.4 % 105 % ±0.55 % LCS-111006- 7 9.9 4 10. 8 10 9 9.9 4 10. 2 102 LCS-111006- 8 9.9 4 10. 5 10 6 9.9 4 9.8 5 99. 1 LCS-111006- 9 9.9 4 10. 8 10 8 9.9 4 10. 1 10 1 Averag e ±%RS D 108 % ±1.4 % 101 % ±1.5 %

Pag e 1 4 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

Tabl e 7 continued . Laboratory Contro l Spike Recovery . ETS-8-044. 0 Intema l standar

d calibratio n Analyze d 10/7/1 1 PFOS (linear* branched) Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery LCS-111006- 1 0.18 4 0.19 6 10 7 LCS-111006- 2 0.18 4 0.19 1 10 4 LCS-111006- 3 0.18 4 0.19 0 10 3 Averag e ±%RS D 105 % ±2.0 % LCS-111006- 4 1.8 4 1.9 3 10 5 LCS-111006- 5 1.8 4 1.9 0 10 3 LCS-111006- 6 1.8 4 1.9 6 10 6 Averag e ±%RS D 105 % ±1.5 % LCS-111006- 7 9.2 2 9.4 7 10 3 LCS-111006- 8 9.2 2 8.9 9 97. 5 LCS-111006- 9 9.2 2 9.2 6 10 0 Averag e ±%RS D 100 % ±2.7 % ETS-8-044. 0 Externa l standar

d calibratio n Analyze d 10/7/1 1 PFOS (linear + branched) Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) XRecovery LCS-111006- 1 0.18 4 0.17 4 94. 6 LCS-111006- 2 0.18 4 0.17 3 94. 3 LCS-111006- 3 0.18 4 0.17 3 93. 8 Averag e ±%RS D 94.2 % ±0.43 % LCS-111006- 4 1.8 4 1.8 0 97. 6 LCS-111006- 5 1.8 4 1.9 0 10 3 LCS-111006- 6 1.8 4 1.7 4 94. 6 Averag e ±%RS D 98.4 % ±4.3 % LCS-111006- 7 9.2 2 8.6 6 94. 0 LCS-111006- 8 9.2 2 8.9 6 97. 2 LCS-111006- 9 9.2 2 8.8 1 95. 6 Averag e ±%RS D 95.6 % ±1.7 % 

### 8. 7 Analytica l Metho d 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 ofaccurac yresults (i n % ) obtaine d fo rth e Q C samples
. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h

Pag e 1 5 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
con-espond s t o a confidence leve l of95% . Th e most recen t 5 0 dat a points were use d t o generat e th e metho d uncertaint

yvalue s liste d i n Tabl e 8 . Tabl e 8 . Analytica l Uncertainty
. Analyt e Standar d Deviatio n Metho d Uncertaint y PFB S 4.66 ±9.3 % PFH S 4.1 8 ±8.4 % PFO S 6.83 ±14 % 

### 8. 8 Fiel d Matri xSpike s (FMS ) Low , mid , an d hig h field matri xspike s (FMS ) were collecte d a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix
. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offield sampl e t o a containe rspike d b yth e laborator

ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear) prio rt o shippin g sampl e container s fo rsampl e collection
. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of100±30 % confir m that "unknown " components i n th e sampl e matri xd o no

t significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Fiel d matri xspike concentration s must b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e field spike
. Fiel d matri xspike s are presente d i n sectio n 9 ofthi s report . Tabl e 9 . Fiel d Matri xSpik e Levels
. Samplin g Locatio n Spik e Leve l PFBS , ng/m L PFHS , ng/m L PFOS , ng/m L 6 1 OS , 6 1 O

L an d Tri p Blank

s Lo w 0.25 0 0.25 0 0.25 0 6 1 OS , 6 1 O

L an d Tri p Blank

s Hig h 1.0 0 1.0

0 1.0

0

„ (Sample Concentration of FMS - Average Concentration: Field Sample & Field

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

n 

### 9 . Data'Summary

arid Discussion Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank
. Results an d averag e value s are rounde d t o thre e significan t figures accordin g t o EP

Aroundin g rules
. Becaus e ofrounding , value s ma yvar yslightl yfro 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 .

Pag e 1 6 o f6 0Tabl e 10 . DA L G W61 O S 11092 1 GLP10-01-02 ; Interi m Repor t 2 3 Analysi s of PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) %Recovery GLP10-01-01-23-00 1 DA L G W6 1 OS-0-11092 1 0.050 9 N A 0.080 9 N A 0.17 7 N A GLP10-01-01-23-002 DA L G W61OS-DB-11092 1 0.054 4 N A 0.085 5 N A 0.12 8 N A GLP10-01-01-23-00 3 DA L GW610S-LS-11092 1 0.27 9 90. 5 0.30 9 90. 3 0.40 9 10 3 GLP10-01-01-23-004 DA L G W61OS-HS-11092 1 1.1 6 11 1 1.1 6 10 8 0.85 0 69. 8 Average Concentration

(ng/mL) ± %RPD 0.0527 ng/mL±6.6% 0.0832 ng/mL±5.5% 0.153 ng/mL± 32% N A= No t /Applicabl e Result s fo rPFB S an d PFH S wer e generate d usin g intema l standar d calibration
. Results fo rPFO S wer e generate d usin g externa l standar d calibration
. (1 ) Tfi e relative percen t difference (RPD ) di d no t meet metho d acceptance criteri a ofS20%
. Tabl e 11 . DA L G W61 OL 11092 1 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) VoRecovery GLP10-01-01-23-00 5 DA L G W6 1 OL-0-11092 1 0.243 N A 0.25 0 N A 1.35 N A GLP10-01-01-23-00 6 DA L G W6 1 OL-DB-11092 1 0.252 N A 0.26 0 N A 1.47 N A GLP10-01-01-23-00 7 DA L G W61OL-LS-11092 1 0.49 5 99. 0 0.49 3 95. 2 1.54 N C GLP10-01-01-23-00 8 DA L G W61OL-HS-11092 1 1.3 8 11 3 1.3 4 10 9 2.3 2 91. 0 Average Concentration

(ng/mL) ± %RPD 0.248 ng/mL±3.6% 0.255 nfl/mL ±3.9 % 1.41 ng/mL±8.5% NC=No t Calculated
. Th e sampl e concentratio n i s greate rtha n 2xth e spik e leve l NA= No t Applicabl e Results fo rPFBS , PFHS , an d PFO S wer e generate d usin g intema l standar d calibration
.

Pag e 1 7 o f 6 0Tabl e 12 . Tri p Blan k GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Descrrptio n (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-01-23-00 9 DA L GWTRIP01-0-11092 1 <0.025 0 N A <0.025 0 NA <0.0232 NA GLP10-01-01-23-01 0 DA L GWTRIP01 - LS-11092 1 0.254 102 0.24 8 99. 2 0.21 5 86. 0 GLP10-01-01-23-01 1 DA L GWTRIP01-HS-11092 1 1.1 0 11 0 1.0 9 10 9 0.95 3 95. 3 NA = No t Applicabl e Result s fo rPFBS , PFHS , an d PFO S wer e generate d usin g intema l standar d calibration
.

Pag e 1 8 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

10 Conclusion Laborator ycontro l spike s an d field matri xspike s were use d t o detemnin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS
. 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
. 12 Attachments Attachmen t A : Protoco l Amendmen t 2 3 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Method-ETS-8-044. 0 Attachmen t D : Metho d Deviatio n

Pag e 1 9 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1



### 13 Signatures

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

## 4- yL/cy^^// Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yDepartmen t Manage rDate

Gar yHohenstein , Sponso rRepresentative Date

Jaisimh a Kesari , Stud yDirecto r Date

Pag e 2 0 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 2 1 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10-01-02 Amendment

22
Study Title Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

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

PROTOCO L AMENDMEN TNO . 2 3

Amendment

Date: Septembe r14 , 201 1 Performing

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

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

Project Identification GLP10-01-0 2
Sampling

Event Off-Sit e 61 0 Well s

Rag e 1 of6
Pag e 2 2 o f6 0GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s Off-Sit e 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10-01-02 Amendment

23 Thi s amendmen t modifie s th e followin g portio n o fprotocol : "Analysi s o fPFOS , PFH S an d PFB S 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 t o th e wordin g ofth e protoco l ar e required
.

AMEND TO READ: N o change s t o th e wordin g o fth e protoco l ar e required
. Thi s amendmen t onl yaddresse s an d document s th e additio n ofth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s a s par t ofth e 3 M Decatu rPhas e 3 Progra m fo rPFOS , PFH S an d PFB S (GLP10-01-02)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e ofth e wee k ofSeptembe r19 , 2011 . Th e groundwate r sample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S as project GLP1,0-01-02-2 3 an d reporteda s interi m repor t GLP10-01-02-23 , (reflectin g stud yGLP10-01-0 2 an d amendmen t -23). ,
Reason: Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t fo rtw o newwell s locate d a t a n off-sit e location
. Th e GP O i s thre e page s i n lengt h an d include d as attache d t o thi s amendmen t forni
.

Pag e 2 of6 Page 23 o f6 0GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , an d PFO

S i n Groundwate rSample

s Off-Site 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10-01-02 Amendment

23 Amendmen t Approva l

Gar yHoVienstei/i,.Sponso rRepresentative 

# I t Date

' ' 'Dat e Clesto n C : Lange , Principa l Analytica l Investigato r

Willia m Reagen , BH S Opn s Environmenta l La b Managemen t Date

Jaisimh a Kesar i P.E^

DEE , Stud yDirecto r

Pag e 3 of6 Page 2 4 o f6 0GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s Off-Site 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10-01-02 Amendment

23 Environmenta l Healt h & Safet y Operations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gary
. Hohenstein , 3 M EHS&Opn s From : Susa n Wolf , 3 M EHS&Opns ; Environmenta l La b cc : Willia m Reagen , 3 M EHS&Opns ; Environmenta l La b

Clesto n Lange , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Date : Septembe r14 , 201 1 Subject : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d

Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 23 ; Off-Sit e 61 0 Well s 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 Rhone : (651 ) 737-357 0 aahohenstein!a>mmm.co m 3 M Environmenta l Laborator yManagemen t Willia m K.
. Reage n 3 M EH S Opns, Environmenta l Laboratory 260-5N-1 7 Contact s 65 1 733-973 9 wi< reaaen@mmm.co m Principa l Analytica l Investigato r ClestonLang e 3 M EH S Opns, Environmenta l Laboratory 250-5N-1 7 65 1 733-986 0 cdangeOmmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s timothv.frinakOwestonsolutions.co m Phone : (334)-332-S12 3 La b Reques t Numbe r GLP10-01-02-2 3 Si xDigi t Departmen t i^umbe r dep t #530711 , Projec t #002267444 9 Projec t Schedule/Tes t Date s Samplin g schedule d fo rth e wee k o fSeptember-19,.201 1 All verbal and written correspondence

will be directed to Gary Hohenstein.

Pag e 4 of6 Page 2 5 o f6 0GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s Off-Sit e 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10r01-02 Amendment

23 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m tw o samplin g locatioh s fo rPerfluorobutanesulfonat e (PFBS) , Perfluoi-ohex'anesulfohat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) fro m newwells,locate d off-site
. Analyse s wil l b e conducte d unde rth e GL P requirement s ofEP ATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792 . Groundwate rsample s wil l b e collecte d byWesto n Solution s personne l th e wee k o fSeptembe r19 , 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 rPFBS , PFHS , an d PFO S are ofa know n precisio n an d accui-acy
. 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 GLP10-01-02-23
. 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b y3 M Environmenta l Laborator yfo rsamplin g th e wee k

ofSeptembe r 14 , 2011 . Sampl e bottle s wil l b e shippe d i n cooler s ovemigh t t o 3 M Decatu rfol-arriva l o n Friday , Septembe r ^6,2011 . 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 3 M Deeatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 4 Tes t Parameter s Th e targete d limi t ofquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS , PFHS , an d PFOS
. Tw o samplin g location s have bee n specified
. Se e attacfimen t Afo ra list ofth e samplin g location s that wil l b e collecte d fo rthi s samplin g even t Fo reac h sarhplin g location , a tota l offou rsampl e bottle s wil l b e collecte d (sample , sampl e duplicate , lo wfiel d matri xspike , an d hig h fiel d matri xspike)
. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL
. On e set oftri p blank s consistin g ofreagent-grad e wate ra s wel l tri p blan k spike s wil l be prepare d at th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe r bottles
. Al l sampl e bottle s wil l includ e th e additio n of'^Oj-PFBS , '^Oz-PFHS , an d '^Ca-PFO S (interna l standard ) at a nomina l concentratio n of1 ng/mL
. Al l sampl e bottle s wil l als o includ e th e additio n o fC4-PFOS (surrogat e spike ) at a nomina l concentratio n of0. 1 ng/mL
. Th e tabl e belowlists th e matri xspike level s that wil l b e prepared
. Wel l No . Sampl e Leve l Spik e Cone . (ng/mL) 610 S andeiO R Lo w 0.2 5 610 S andeiO R Hig h 1. 0 Tri p Blan k Lo w 0.2 5 Tri p Blan k Hig h 1. 0

Pag e 5 o f6 Page 26 o

f60GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s Off-Sit e 61 0 Wells ; Septembe r201 1 Analytical

Protocol:

GLP10^01-02 Amendment

23 Tes t Method s Sample s wil l b e prepare d an d arialyze d b yLC/MS/M S followin g ETS-8-044. 0 "Determinatio n ofPerfluorinate d Compound s I n Wate rb

yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Alternately , sample s ma yb e analyze d b

yETS 8-154. 3 "Determinatio n ofPeifluorinate d Adds , 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"
. Th e data qualit

yobjective s fo rthes e studie s ar e quantitative results fo rth e targe t analyte s wit h a n analytica l accurac yofld0±30%
. Fiel d matri xspike s no t 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 accurac

ystatemen t ma

yb e adjuste d accordingly
. Where applicable , sample s wil l be analyze d against a n interna l standard calibratio n curve . Eac h curvi e poin t wil l contai n isotopically-labele d perfluorocarboxyli cacid s an d perfluorosulfoni cacid s a t a nomina l concentratio n of1 ng/mL
. Th e calibratio n curve wil l b e generate d b ytakin g th e rati o ofth e standar d pea k are a count s ove rth e interna l standar

d pea k are a count s t o fi t th e data fo reac h analyte
. 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e result s fo rth e sannple , sahipl e duplicate , an d th e fiel d matri xspikes
. Tri p blan k an d tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an y equipment/rinseat e blank s prepare d i n th e field
. Laborator yconti-o l spike s ofreagen t wate rprepare d at th e tim e ofsampl e extractio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d precision
. Method blank

s ofreagen t wate rprepare d at th e tim e ofsampl e extractio n wil l b e use d t o deterfnin e th e metho d detectio n lihii t Fo rthos e samplin g location s where th e fiel d matri xspike leve l wa s not iappropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspike mayb e prepare d an d wil l b e include d i n th e fina l report .

Pag e 6 o f6 Pag e 27 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1


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

Pag e 2 8 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOTa.rd b

3 1 - 30 - 29 - 28 - 27 - 26 - 25 - 24 - 23 - 22 - 21 - 20 - 19 - C D 18 - < 17 - 16 - ( 0Are 15 - <D %. 14 - ( 0 c < 13 - 12 - 1 1 - 10 - 9 - 8 - 7 - 6 - 5 - 4 - 3 - 2 - 1 - 0 - 9. 0 10. 0 11. 0 12. 0 13. 0 14. 0 15. 0 16. 0 17. 0 18. 0 19. 0 20. 0 21. 0 22. 0 23. 0 24. 0 Analyt e Cone
. /

I S Cone
. Data printed by PrintingTime: t ST W :07:4 1 A

M Pag e 1 o f 1 Pag e 2 9 o f 6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b

Dat a printe d b yST W Printin g Time : 8:07:0 9 A M Pag e 1 o f 1 Pag e 3 0 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 •Kir k BB2150101 0

Printin g Time : 8:01:3 4 A H Pag e 1 o f 1 Pag e 3 1 o f6 0*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klll007a.rd b 

# I SampleNam«:-|(11IO07aO16 - SampteID:'1 1 003-4O4 ' Fl« : Pea k Name : •13C3PFHS<IS) - Mass(es) ; -402.000^0.00 0 Da * Cotnment : '1. 0 nglm L F C ai d k i Synth
. Wate rAnnotatioo; " Sampl e Index : 1 6 Sampl e Type : Standar d Concentiation : 0. 945 ng/ri L Calculate d Cone : H/ A Acq . Date : 10/7/201 1 Acq . Tine : 2:41:0 7 P M

, AlgoElthm : Specif yI • Percentage : S O

. Sub . Window : l.O C -Split . Factor : 2 Sampl e Name : Ti l 11007a023 - Sampl e ID : '1 1 OOS-223" Fie : "k l 11007a.wlf r Pea k Name ; M3C3PFHS(IS) - Massfes) : "402.000/80.00 0 Da Commen t -Metho d Blank ^ AnrK>tation : ~ Sanpl e Index ; 2 3



# I Sampl e Name : -k11100ra024 ' Sampl e ID : -QLP10-01-02-23-001 ' Pea k Name : -13C3PFHS(iS) - Massfes) : "402.000/80.00 0 Da " Commeni:-DAL-GW-eiOS*- ' Annotatkm; - Sampl e Index : 2 4 Sampl e Type : Unknow n Concentration : 0,94 5 ng/mL Calculate d Cone : K/A Acq . Date : 10/7/201 1 Acq . Tine : 5:30:0 4 P H
Hoi : . Algo l ? Perc e : Specif y Paranete i Sampl e ID : "GL P 1 CM ) 1-02-23-005 * File : M3ss(es) : "402.000/80.00 0 Da Annotation : ~

ameCer s - H

Q II ] Nlndo i Poak-Split . Facto r Repor t Larges t

Peal Hin . Pea

k Height : Min . Pea

k Width : Smoothin g Width : R T Window : mpec l

Height : Star t T i En d Tim s

1 RT : ! RT :

2.47«t00 5 cp s

Dat a printe d b yST W Printin g Time : 8:09:1 0 A M Pag e 1 o f 1 2 Pag e 32 o f6 0*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 3 /Vnalysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : kl11007a.rd b

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e Pag e 3 3 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klll007a.rd b 

# I Sampl e Name : -k111007a016 ' Sampl e ID : '1 1 003-40 ^ Fie : "h i 1 lOOTa.wif r Pea k Name : -13C8PFOSJS(iS) - Mass(e3) : "507.000/80.00 0 Da " C<imrnent;'1.0ng/mLFCs[< J I n Synth
. Water " Armotalion : " Sampl e Index : 1 6 Sampl e Type : Standar d Concentration ; 0.96 0 ng/n L Acq . Date : 10/7/201 1 Acq . Tine : 2:41:0 7 P M Modified : Ye s Ptoc . Algorithm ; Specif yPoiameter s - M Q II I Nois e Percentage : 5 0 Baae . Sub . Hindow : 1.0 0 mi n Peak-Split. Factoi; 2

Peak : Ye s .n . Pea k Height :

. Pea k R T HindoH : Expecte d RT :

'idth : 0.0 0



# I Sampl e Narrw : "V111007a024 " Sampl e ID : "GLPItM)1-02-23-001 " File : •kl11007a.wi r Pea k Name : •13C8PFOS-IS<IS) " Ma»5{«) : -507.000/80.00 0 Da Comment : "DAL-GW-6I0S-0- " Annoeatkm : " • Sanpl e Index : 2 4 Sampl e Type : Unknow n Concentration : 0.96 0 ng/mL Calculate d Cone : N/ A Acq . Date : 10/7/201 1 Acq . Time : 5:30:0 1 P M 

# I Sampl e Name : "k l 11007a023 " Sampl e ID : '1 1 005-223 " Fie : "k t 11007a.w<f r Pea k Name : '13CaPFOS4S{tS) - Massfes) : '507.000/80.00 0 Da Comment : "Metho d Blank* Annotatkxi : " *

:a9e : Baac . Sub . Window : Repor t Larges t Pe ; Hin . Pea k Height : Smoothin g Hldth : R T Window :

RT :

ye s : Specif y Paratoete i Base . Sub . Hindow ; Peak-Split . Facto i Repor t Larges t

Fe ; Min . Pea

k Height ; Min . Pea

k Width : Snoothin g Width : R T Window : Expecte dRT : Int . Type : Area : Height : Bas e T o Bas e 4.0e 4 3.ee 4 3.ee 4 3.4e 4 3.2e 4 3.0e 4 2.8e 4 2.6e4 ' 2.4e 4 2.2e 4 2.0e4 '

1.4M ' 1.2e 4 1.0»4 ' eooo.o6000.0
- 4000. 0 2000.0
- 0.0
- 

# I Samfi e Name : "k111007a031 " Sample ID : 'GLP l 001-02-23-005 " File : Pea k Name:-l3CePF0S-lS(IS)
- Mass{es) ; "507.000^0.00 0 Da
Commenl ; -DAL-GW-610L-*. * AnrHrtaBon ; - Sarapl e Index : 3 1 Sampl e Type ; Unknow n Concentration : 0.96 0 ng/n L Calculate dCone : )1/ A Acq . Date : 10/7/201 1 Acq . Time : 7:57:5 9 P M in : Specif y Pai

Hin . Pea

k Wid : Smoothin g Hid ' Expecte dRT : Us e Relativ e I Int . Type : Retentio n Tim i Area ; Height : Star t Time ;

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 3 o f 1 2 Pag e 3 4 of6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

# I Sampl e Name : •k111007a041 - Sampl e ID:-LCS-111006-1 ' File;-K111007a.wf r Pea k Name : "13C8PFOS-«S(IS rMass(e5) ; "507.000/80.00 0 Da ' Commen t "OJfpp b LCS - Annotation: - 

# I Sampl e Nan>e:*k1110073035 ' Sampl e ID:'GLP10-01-02-23409 ' File : Pea k Name : '13C8PFO&^S(iS} ' Mass(es) : '507.000/BO.OO O Da Comment:-DAL-GW-TRIPOl-O - Aimolalion: - Sampl e Index : 3 S Sampl e Type : Unknow n Concentration : 0.96 0 ng/n L Calculate d Cone : Dat e .cq . Tim , 10/7/201 1

9:22:2 9 P

M

Peak-Split . Factor : Repor t Larges t Peak : Min . Pea k Height :

Bas e T o Bas e s Type : 0.95 1

Proc . Algorithm ; Specif yParameter s - K Q ] Nois e Percentage : 5 0 Base . Sub . Window : l.OD mi n Peak-Split . Factor : 2 Repor t Larges t Peak : Ye s Min . Pea k Height : 0.0 0 cp s Hin . Pea k Width : 0.0 0 se c Snoothin g Hldth : 0 point s R T * Expec t 1 RT :

! RT : 16. 2

I I o ) Relati i

. Type : Bas e T o Bas e •ntio n Time : 16. 1 mi n > : 51822 8 count s

8.17e H 15. 9



# I SamplsName:*k111O07aD44 ' Sampl e ID:-LCS-111006^ ' File:-k111 i Pea k Name : 'ISCBPFOS-ISflS) - Mass(as) : -507.000m0.00 0 Da Comment : -2pp b LCS " Annotation: " Sampl e Index : 44 Sampl e Type ; Q C Concentration : 0.95 1 ng/m L Calculate d Cone : N/ A Acq . Date : lO/B/201 1 Acq . Time : 12:32:3 ^ A M ; Specif y Paraneter j :-Spl i Fact e iport Largest

Peak; Yes n. Peak Height: 0.00 ~'sBk Width: 0.00 Snoothing width: 0 RT Window; 30.0 St Expecte d RT ; ! Rela i
Height : Star tT : End Tlm i iRT : N

o 

## ( Sampl e Name:T(111007a04 rSampl e ID : -LCS-111006- rFile : •k111007a
. Pea k Name : -13C8PFOS-IS(iS) - Mass<es) : -507.000/80.00 0 Da " Commen c"1 0 pp b LCS " Annotatkxt : ~ Sampl e Index : 4 7 Sampl e Type : Q C Concentration : 0.95 4 ng/m L Calculate d Cone ; H/A Acq . Date : 10/6/201 1 Acq . Time ; 1:3S:S 4 A M Modified : Ye s Proc . Algorithm ; Specif yParameter s - M Q II I Nois e percentage : 5 0 Base . Sub . window : 1.0 0 mi n

Snoothin g Hldth : R T Window : Expecte d RT :

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 4 o f 1 2 Pag e 3 5 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b Sampl e Name:-k111007a016 - Sampl e ID:-1 1 003-4(K8 - Flle:-k111007a.wtr r Pea k Name : -ie02PFBS(IS) " Mass(es) : "303.000/84.00 0 Da ' CommonI:'1. 0 ng/m L F C std i n Synth
. Water* Annotation:" " Sampl e Index : 1 6 Sampl e Type ; Standar d Concentration : 0.97 5 ng/n L Calculate d Cone : N/ A Acq . Date : 10/7/201 1 Acq . Tine : 2:41:0 7 P M

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 5 o f 1 2 Pag e 3 6 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

# I Sampl e Name : •l(111007a035 " Sampl e ID : "GLP!CM)1.02-23-009 ' File ; Pea k Name : •1802PFBS(IS) " Mass{es) : "303.000/84.00 0 Da Comment:-DAL-GW-TRIPOI-O - Anfwlalton: - Sampl e Index : 3 5 Sampl e Type : Unknow n Concentration : 0.97 5 ng/m L Calculate d Cone : N/ A Acq . Date : 10/7/201 1 Acq . Time : 9:22:2 9 P H :ied: N o Proc . Algorithm : Specif yPai l Hois e Percentage : S O Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t Peak : Ye s Hin . Pea k Height : 0.0 0 Min . Pea k width : 0.0 0 Smoothin g Width : 0 R T Window : 30. 0 B * Expected RT: 13.7 mi Int . Type : Area : Height : Star tTin e Bas e T o Bas e

le : 13. 7 mi n 116516 0 count s Sampl e Name : "k111007a041 " Sampl e ID:'LCS-111006- rFile:-k111007a.wtf r Pea k Name : '1802PFBS(IS} ' Ma3s(es) : '303.000/84.00 0 Da " Commen t '0.2pp b LCS ' Annotation : " Sampl e Index : 4 1 Sarapl e Type : Q C Concentration : 0.96 6 ng/n L Calculate d Cone : ll/ A Acq . Date ; 10/7/201 1 Acq . Time : 11:29:1 5 P M Proc . Algorithm ; Specif yPa n Mois e Percentage : 5 0 Base . Sub . Window ; 1.0 0 Peak-Split . Factor ; 2 Repor t Larges t Peak : Ye s Hin . Pea k Height : 0.0 0 Hin . Pea k Width : 0.0 0 Smoothin g Width : 0 R T Window : 30. 0 s t Expecte d RT : 13. 7 m i

11. 5 

# I Sampl e Name : "k l 11007aD44 ' Sampl e ID : 'LCS-111006-4 - File : -kU1007a
. Pea k Name : '1802PFBS(IS) - Ma»s(es) ; -303.000^84.00 0 Da Commen t *2pp b LCS - Amwtatton : " Sampl e Index : 4 1 Sampl e Type : Q C Concentration ; 0.96 6 ng/n L Calculate d Cone : N/A Acq . Date : 10/8/201 1 Acq . Time : 12:32:3 4 A M Nois e Percentage ; Base . Sub . window : Peak-Split . Facto r Repor tLarges tPe

a Hin . Pea kHeight : Min . Pea kWidth : Snoothin g Width : R T Window : Expecte d RT : Sampl e Name : "k l 11007a04

rSampl e ID : "LCS-111006-

rFile : "kl l 1007a.*« r Pea kName : -18D2PFBS(iS)

- Mass(as) : *303.00Qr84.00

0 DaCommen t'1 0 pp b LCS ' JSjmotalion

: ~ Sampl e Index ; 4

7 Sampl e Type : Q C Concentration : 0.96 9 ng/ra L Calculate d Cone : t(/ A Acq . Date : lO/B/201 1 Acq . Time : 1:35:5 4 A M Proc . Algorithm : Specif y Parameter i Noia e Percentage : 5 0 Base . Sub . window : I.0 0 mi n Peak-Split . Factor : 2

: Rele t I RT :

• Type : Valle y intlo n Time : 13. 7 l : 11S2U 2 C ( Height : Star t T ; En d Tim . Height : Hin . Pea k Width : Smoothin g width : R T Window : Expecte d RT : Us e Relativ e RT : Int . Type : Area ; 117 1 Height : 1 . 0.0 0

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 6 o f 1 2 Pag e 3 7 o f 6 0*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

# I Sampl e Name : "k111007a0l6 - Sampl e ID : "1 1 003-4( WFlo : "kU1007a
. Pea k Name : "PFBS " Mass(B5) : "asg.OOWSO.OO O Da.299.000«9.00 0 Da ' Commen t "1. 0 ng/m L F C St d i n Synth
. Watei * Annotatkx> : ~ Sampl e Index : 1 6

Type : Standar d Calcula t 0.98 2

Proc . Algorithm : Specif y I Nois e Percentage : 5 0 Base . Sub . Window : l.D t Peak-Split . Factor : 1 Repor t Larges t

Peak : Ye : Hin . Pea

k Height ; 0. ( Hin . Pea

k Width : 0. ( Smoothin g Width : 0 R T Window : 30. 0

11. 5 12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 

## ( Sampl e Name : "k l 11007a023 " Sampl e ID : "1 1 005-223 - Fie : "k l 11007a.wti r Pea k Name : "PFBS " Uassfes) : "299.00^80.00 0 Da ,299.000/99.00 0 Da * Commen t "Metho d Blank " Annotation : Sampl e Index : 2 3 Sanpl e Type : Unknow n

l i f ied : iCone : N o Proc . Algoritlun : Specif y i Nois e Percentage : 5 0 Base . Sub . Window : l.O C Peak-Split . Factor : 2 Repor t Larges t

Peak : Yes Htn . Peak

Height : O.C Hin . Peak

width : O.C Smoothin g Width : 0 R T Window : 30. 0 Expecte dRT : ! Roll • RT : N o

12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 

# I Sampl e Name : •kl110073024 - Sampl e ID : *GLP10-01-02-23-001 " File : 1(1110073
. Pea k Name : -PFBS - Mass<es) : "299.000/80.00 0 Da.299.000/99.00 0 Da " Commen t -DAL-GW-610S-0- - Anrwtation : - sampl e Index : 2 4 Sampl e Type : Unknow n Concentration ' Calculate dCo i Acq . Time : N / A

Base . Sub . Window : l. ( Peak-Split , Factor : 2 Report Largest

Peak: Ye Min . Pea

k Height : 0 . Hin . Pea

k Hldth : 0 . Smoothin g Width : 0 R T Window : 30. 0 ) Relatl i detentio n 1 Mea ; ioight : ! RT : N o

Bas e T o Bas e 

# I Sampl e Name : 1(1110073031 " Sampl e ID : "GLPHW)1-02-23-005 ' File:-k111007a.wtf r Pea k Nama : "PFBS " Massfes) : -299.000/80.00 0 Da,299.000/99.00 0 Da Commen t "DAL-GW-610L-ft- ' Annotation : ~ Sampl e Index : 3 1 0.24 3 10/7/201 1 7:57:5 9 I Proc . Algorithm : Specif yi Nois e Percentage : 5 0 Sub . Window : l.OC t-Spl H Fac t Repor t Larges t Peak : Ye i Kin . Pea k Height : O. C Hin . Pea k Width : O. C Snoothin g Hldth : 0 R T Window : 30. 0 Expecte d RT : 13. 7 > Rela t i RT ;

38705 2 count s 5.64e<-00 4 cp s 13. 5 mi n 14. 0 mi n

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e V o f 1 2 Pag e 3 8 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

# I SamploName:"k111007a041 - Samp(olD:'LCS-111 C Pea k Name : "PFBS " Mass(es) : -299.OOIV80.000 Da,2 ' Commen t "0.2pp b LCS " Annotatton : 

# I Sampl e Name : "kllI007a035 ' Sampl e ID : - i Pea k Name : 'PFBS * Mass(es) ; -299.000«0.0 < Comment:-OAL-GW-TRIPOI-O " AnnolaBon: - Sampl e Index : 3 5 Sanpl e Type : Unknow n Calculate d Cone : < 0 Acq . Date : 10/7/201 1 Acq . Time : 9:22:2 9 P M Modit : N o

: Height : R T Hindow : Expecte d RT : Us e Relativ e 1 ) Type : Q C 0.19 8 ng/m L 0.22 9 ng/m L 10/7/201 1 11:29:1 5 P

M lilied : ic . Algorithm : : S B Percentage :

R T Hindow : Expecte d RT : Us e Relativ e I 5.8e 4 5.6e 4 5.4» 4 5.2e 4 5.0e 4 4.8e 4 4.6e4 4/4e4 4.2e 4

3/4e4 - 32e 4 3.0e4 ' 2.&e4 ' 2.6e4 - 2AtA 2.2e4 - 2.0e4 '

12e4 - 1.0*4 ' 8000. 0 6000.0 - 4000.0 - 2000.0 - 13. 0 13 J 14. 0 14. 5 15. 0 15. 5 16. 0 

# I Samp(eN3me:-V111007a044 - Sampts ID : " I Pea k Name : -pFBS " Mai*(es) : •299.000/80.0 < Commen t •2pp b LCS " Annotalioo:" " Sampl e Index : 4 4 Sampl e Type : Q C Concentration : 1.9 8 n < Calculate d Cone : 2.2 3 n t

Base . Sub . window : Peak-Split . Factor : Repor tLarges tPeak : Min . PeakHeight :

Star tTime : 5.5Ba-^00 5 cp s S.4e5 ' 5.2e5 ' 5.0e5 - 4.ee5 - 4.6e5 - 4.4e5 - 4.2e5 - 4.0e5 - 3.8e5 - 3,6e5 - 3,4e5 - 3.2e5 - 3.0e5 - 2.8eS 2.eeS 2.4e5 - 2.2e5 ' 2.0e 5 1.8e5-

8.0e 4 6.0e 4 4.0e 4 2.0» 4 

# I Sampl e Name : "kl l 1007304 rSampl e ID : 'LCS-11 1 Pea k Name : "PFBS - Mass(es) : -299.000/80.00 0 Da.2 i Comment:-1 0 pp b LC^ - Annotation : " " Sampl e Index : 4 7 Sampl e Type : Q C Concentration : 9.9 4 ng/n L Calculate d Cone ; 10. B ng/ra L Acq . Date : 10/8/201 1 Acq . Time : 1:3S:5 4 A H Modified ; N o Proc , Algorithm ; Specif yParameter s - M Q 1 Nois e Percentage : 5 0

Min . Pea k width ; Smoothin g Width : R T Window : Expecte d RT :

En d Time :

Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 8 o f 1 2 Pag e 3 9 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s of PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

## ( Sampl e Name : "k l 11007a016 " Sampl e ID : "1 1 003-W-d ' Flo : "k l 11007a,wi( r Pea k Name : "PFHS - Massfes) : -399.000/99.00 0 Da.399.000^0.00 0 Da * Commenl : '1. 0 ng/m L F C st d i n Synlh.Waler - Annolation ; " * Sampl e Index : 1 6 Sampl e Type : Standar d Concentration : 1.0 0 ng/m L Calculate dCone : 0.99 8 ng/m L Acq . Date : 10/7/201 1 Acq . Tine : 2:41:0 7 P H

Base . Sub . Windo i Peak-Split . Fact i Repor t Larg i Min . Pea

k Heigh i Min . Pea

k widt h Smoothin g Widt h Peat

16. 0 16. 5 17. 0 17. 5 

## [ Sampl e Name : "k l 110073023 " Sampl e ID : "1 1 005-223 - Fie : 'k l 11007a.*« r Pea k N3me : 'PFHS " M3ss{es) : "399.000/99.00 0 Da.399.000/80.00 0 Da Commen t 'Metho d Btsnk - Annotatnn; ~ 2100 - 2000 - 190 0 180 0 170 0 160 0 150 0 1400 ' Nois e Per

< :age : Sub . Windo i Repor t Larg i Min . Pea

k Heigh t Min . Pea

k Width : Smoothin g Width : R T Hindow : Expecte dRT :

Area : Height : Pea l

120 0 110 0 1000 -



## ( Sampl e Name : *k111007a024 ' Sampl e ID : -GLP1041'02- : Pea k Name : -pFHS - Mass(*s) : -399.000/99.00 0 Da,399.0C Comment : "DAL-GW-610S-0- ' Annotation; " Sampl e Index ; 2 4 Sampl e Type : Unknow n

Nois < Base . Sub . Hindo w Peak-Split . Facto : Repor t Larg i Hin . Pea k Heigh ' Hin . Pea k Widt h Snoothin g Widt h R T Window : )e0 9

Peak :

! Rel i ; RT : 

## ( Sampl e Name : 1(1110078031 - Sampl e ID : -GLPKM)1-02-23-005 " File : •k111007a.wif r Pea k Name : "PFHS " Mass(es) ; "399.000/99.00 0 Da,399.000/80.00 0 Da Commen t "OAL-GWAeiOL-O- - Annotation : ~ Sampl e Index ; 3 1 0.25 0 10/7/201 1 7:57:5 9 P

M

Peak-Split . Fact e Repor t Larges t

P e Hin . Pea

k Height : Hin . Pea

k Width ; Smoothin g width : R T Window : Expecte dRT ; Us e Relativ e RT :

13. 0 13, 5 14. 0 14, 5 15, 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 9 o f 1 2 Pag e 4 0 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

# I Sampl e Name:-k111007B03S ' Sampl e ID : "GL P 1041-02-23-009 ' File:-k1110073.wi r Pea k Name : "PFHS ' Massfos) ; '399.000/99.00 0 Da.399.000^0.00 0 Da ' Commenl : 'DAL-GW-TRIPOI-O ' Annolation : - Sampl e Index ; 3 5 Sampl e Type : Unknow n Acq
. Date : Acq
. Time : Modified : ichm ; Specif y I llois e Percentage : 50 Base . Sub . Window : 1 . O f Peak-Split . Factor ; 1 Repor tLarges tPeak : Ye : Min . Pea kHeight : 0. ( Min . Pea kWidth : 0. ( Smoothin g Width : 0 R T Hindow : 30. 0 Expecte d RT : 15. 2 Us e Relativ e RT : N o imetec s - K Q I

Height : Valle y 15. 2 mi n 189 1 count s l,03e+00 2 cp s



# I Sampl B Name : 1(1110073044 ' Sampl e ID : 'LCS-111006-4 ' File:*k11l007a.M r Pea k Name : "PFHS ' Massfes) : -399.000/99,00 0 Da,399.000/80.00 0 Da Comment : -2pp b LCS - Annotation: " Sample Type: QC Concentration : 1.9 8 ng/m L Calculate d Cone : 2.0 9 ng/m L Acq
. Date ; lO/S/201 1 

# I Sampl e Name : ^kl l I007a041 ' Sampl e ID : ' I Pea k Name : "PFHS ' Mass{es) : '399.000/99.0 { Commen t "0.2pp b LCS ' Annotation : " Sampl e Index : 4 1 Sampl e Type : Q C Concentration ; 0.19 8 ng /

Base . Sub . Window : Peafc-SplIt . Factor : Repor tLarges tPeak :

8.40e*0O 4 cp s

. 0 14. 5 15. 0 15. 5 16. 0 18. 5 17. 0 17. 5 

## ( Sampl e Name : -k l 11007304 rS3mpl e ID : - Pea k Nama : 'PFHS ' Mass(es) : "399.000/99
. Commen t '1 0 pp b LCS ' Annotation;" " Sampl e Index ; 4 7

12:3 2 :3 4 Acq . Time ; Modified : N o Proc . Algorithm : Specif y Par i IJois e Percentage : 50 Base . Sub . Window ; 1.0 0 Peak-Split . Factor : 1 Repor tLarges tPeak : Ye s Min . Pea kWidth : 0.0 0 Snoothin g Width : 0 Us e Rel i Int . Ty i Area : Height : iRT :

! RT : 15. 2

H o 7.5e 5 7.0e5 - 6.5e5 6.0e5 5.5e5 - in : Specif y Parameter ; Peak-Split . Facto r Repor tLarges tpea l Kin . Pea kHeight : Kin . Pea kWidth : Smoothin g Itidth : R T Window : Expecte d RT : 3.4e 6 3.2e 6 3.0e6 - 2.6e6 - 2.6e6 - 2.40 6 2.2e 6 2.0e6 - 1.ee6 - 1.6«6 - 1.4e6 - 1.2e 6 1.0e6 - B.0e5 - 6.0e5 - 4.0eS 15. 5 16. 0 Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 1 0 o f 1 2 Pag e 4 1 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s of PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOVa.rd b 

## ( Sampl e Name : -kil l 0078016 - Sampl e ID : '1 1 003-4O-8 - Fie : T d 11007a,¥rt r Pea k Name : -PFOS - Mass{es) : -499.000/99.00 0 D a ,499.000/80.00 0 D3.499,000/130.00 0 03 " Commenl ; "1, 0 ng/m L F C Bt d i n Synth , Watei * Annolation : ~ Sampl e Index : 1 6

Base , Sub . Hindow : Peak-Split . Facto i Repor tLarges tPe * Min . Pea kHeight ; Min . Pea kWidth ; Smoothin g width ; R T Window : : Specif y Pataneter i

RT ;

15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 

## ( Sampl e Name : *k l 11007a023 " Sampl e ID : *1 1 005-223 " Fie : 'k l 11007a,wtf r Pea k Name : "PFOS " Mass(es) : "499.000«9.00 0 Da.499.000/80,00 0 Da.499,000/130,00 0 Oa " Commen t "Metho d Blank* Annotation : Sampl e Index ; 23 Sampl e Type : Unknow n Concentration : ll/ A 10/7/201 1 5:08:5 5 P

M

Manua l 16. 1 mi n 1813 1 count s !.05e*00 3 cp s

14. 0 14. 5 15. 0 

# I Sampl e Name : -k l 11007a024 - Sampl e ID : "GL P 10-01-02- 2 Pea k Name : -f>FOS - Mass(es) : "499.000/99.00 0 Da,499.00 i Comment : "DAL-GW-eiOSO- ' Annotatton : " • sampl e Index : 2 4 Sanpl e Type : Unknow n 

# I Sam^J e Name : "k l 11007a03 rSampl e ID : 'GL P 1 (Kll-02-23005 " File : "k l 11007a,wi r Pea k Name : "PFOS " Mass{es) : -499.000^9.00 0 Da.499.000^1.00 0 Da,499.000/130.00 0 Da Commen t "DAL-GW-610L-(X. * Annotation:" * Sampl e Index : 31

: Specif y Paramete i Sub
. I Indow :

. Fac i Repor t Larges t f i Min . Pea k Height : Min . Pea k Width : Smoothin g width : R T Window : Expecte d RT : : Rela t 1 RT : Calculate d Co i Acq . Date : Acq . T i ne :

Smoothin g Wid t R T Window ;

Area : 113138 7 count s Height : 1.0Ee-^00 5 cp s Star t Time : 15. 6 mi n En d Time ; 16. 3 mi n I.OSeS 1.00e5
- 9.50e4
- 9.00e4 ' B.50e4
- 8.00e4
- 7.50*4
- 7.00e4
- 6.50*4
- 6,00e4
-

14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17 . Dat a printe d b yST W Printin g Time : 8:09:1 1 A M Pag e 1 1 o f 1 2 Pag e 4 2 o f 6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klll007a.rd b 

# I SampleN3me:T(111007a035 " Sampl e ID:-GLP10-01-02-23«l9 " File:'kni0073.wif r Pea k Name : -PFOS - Mass(es) : -499.000/99.00 0 Da,499.000/80.00 0 D3,499.000/130.00 0 D3 - Comment:-DAL-GW-TRIPOl-0 - Annolation; -

llfl i algorithm : Specif y Paramet t rcentage ; Base . Sub . Window : Peak-Split . Facto r Repor tLarges tPe

a Hin . Pea kHeight : Min . Pea kWidth : R T Window ; Expecte d RT ; Us e Relativ e RT :

Star tTime : ..55e+00 3 cp s

14. 5 15, 0 17. 5 18. 0 

# I SampteName:1il11007a041 " SampteID : "LCS-I I 1006- rFile:-k111007a
. Pea k Name : TFOS - Ma$s(e$} : '499.000/99.00 0 Da.499.000/80.00 0 Da,499.000/130.00 0 Da * Commen t -0.2pp b LCS - Annotatkin ; ~ Sanpl e Index : 41 Sampl e Type : O C Concentration ; 0 . 1B 4 ng/m L Calculate d Cone : 0.19 6 ng/m L Acq . Date ; 10/7/201 1 Acq . Time ; 11:29:1 5 P M Modified : fe s Proc . Algorithm : Specif y Parameter s - M Q II I Wois e Percentage : 50 t-Spli t ;epor Fact i

Peak : Min. Peak Height: O.l Min . Pea kWidth : O.C Smoothin g Width : 3 R T Window ; 30. 0 Expecte d RT : 16. 2

Height : Star tT i

14, 0 14. 5 15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 18, 5 

# I Sampl e Name : "k l 11007a044 " Sampl e ID : "LCS-11100fr4 " File : "kl l 1007a.w« r Pea k Name : 'PFDS ' Mass(as} : "499.000/99.00 0 Da,499.000/80.00 0 Da.499.000/130.00 0 Da Commenl : '2pp b LCS ' Annotation : " Sampl e Index : 4 4 Sampl e Type ; Q C Concentration : 1.8 4 ng/ra L Calculate d Cone ; 1.9 3 ng/n L Acq . Date : Acq . Tine : 1.7B 5 12:32:3 4 J

• . Sub
. 1 L-Spl H Fac i Repor tLacg ' Min . PeakHeigh t Min . Pea kWidth : Smoothin g width ; R T Windo w Pea l

pee l 1 RT : • Relati '

Star tTine ; 

# I Sampl e Name : 1(111007304 rSampl e ID : "LCS-111006- rFile : "k l 11O07a.wt r Pea k Name ; -PFOS " Mass(es) : -499,000/99.00 0 Da,499.000/80.00 0 Da,499.000/130.00 0 Da Commen t '1 0 pp b LCS - Annotatiofi : ~ Sampl e Index ; 4 7 Sampl e Type : Q C Concentration : 5.2 2 ng/m L Calculate d Cone : 9.4 7 ng/n L Acq . Date : 10/8/201 1 Acq . Tine : 1:35:5 4 A M thn ; Specif y Pat Repor tLarges tPe

f Min . Pea kHeight ; Min . Pea kWidth : Smoothin g width ; R T Window : Expecte d RT :
Height : Star tTime : En d Time :

17. 5 18. 0 15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 18. 5 Dat a printe d b yST W Printin g Time : 8:09 : Pag e 1 2 o f 1 2 Pag e 4 3 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : kl11007a-ext.rd b k l 11007a-ext.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -15 1 9.03e-f00 5 x+ 4.85e-t-003 ( r= 0.9997 )

10. 0 11. 0 12. 0 13. 0 14. 0 15. 0 Concentration , ng/m L 17. 0 18. 0 20. 0 21. 0 22. 0 23. 0
Dat a printe d b y Printin g Time : Pag e 1 o f 1

8:11:4 8 A

M Pag e 4 4 o f 6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : kll1007a-ext.rd b 

# I SampteName:-V1110078016 * Sampl e 10:"1 1 OOi^M * Fla:Te l 11007a.wif r P«a k Name : "PFOS - Masstas) : '499.000/99.00 0 D a ,499.000/80.00 0 Da,499.000/130.00 0 Da ' Comment : -1. 0 ngtm L F C st d I n Synth
. Water " Annolation : -

A l l gor i ttolsi Base . Sub . Window : Repor t Larges t

Pe ; Min . Peal t

Height : Min . Peal^ Wid i : Specif y Pataneter :

.dth : R T Window : Expecte dRT : Us e Relativ e 1 Int . Type : Height : e.98e»00 4 cp s

1S. 0 15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 

# I Sampl e Name : "Kl l 1007aD23 - Sampl e ID : -1 1 005-223 ' Fle:-k111007a.wa r Pea k Name : *PFOS ' Masafas) : '499.000/99.00 0 Da,499.000W).00 0 Da.499.000/130.00 0 Da * Commen t -Metho d Blank - Annolation : ~

Smootliln g width ; R T Window : Use Relativ e RT ;



# I Sampl e Name : *k111007a024 ' Sampl e ID : -GLP10-01-02-23-00 rFile: ' Pea k Name : -PFOS ' lulaas(as) : '499.000/99.00 0 Da.499.000;80.00 0 Da,4 < Comment:-DAL-GW-eiOS-O- - AnnotaUon: " Sampl e Index : 2 4 Sampl e Type : Unknow n 

# I Sampl e Name : "k l 11007aD4 rSampl e ID : -LCS-1 1 lOO& V File : -k l 11007a.wt r Pea k Name : -PFOS ' MaS3(as) : -499.000/99.00 0 Da,499.000/80.00 0 Da.499.000/130.00 0 Da ' Commen L -0.2pp b LCS - Annotation:" "
N / A Calculate dCone : Acq . Tine : 17 7

Proc . Algorithm : Specif y Pararaet c tloia e Percentage : 9 0 Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor : 3 Repor t Larges t

Peak ; Ye a Kin . Pea

k Height : 0.0 0 cp s Hin . Pea

k Width : 0.0 0 se c Snoothin g Width : 0 p c R T Window : 30. 0 se c Expecte d RT ; IS. 9 mi n Calculate d Cone ; 0.17 4 n t Acq . Date : 10/7/201 1 Acq . Tine : 11:29:1 5 P M Modified : M o Proc . Algorithm : Specif yPara o Nois e Percentage : 9 0 Base . Sub . Window : 1.0 0 n

Expecte d RT : 15. 9 ml i Us e Belatlv e RT : M o Int . Type : Bas e T o Bas e Reten t " " ' " Area ; Height : 1.ee4 1.7& 4 1.6e4 ' 1.504 1.4e4 1.3e4 1.2e4

^ 9000. 0 8000. 0

13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 Dat a printe d b yST

W Printin g Time : 8:13:0 8 A M Pag e 1 o f 2 Pag e 4 5 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 Result s Name : klllOOTa-ext.rd b

Dat a printe d b

yST W Printin g Time : 8:13:0 9 A M Pag e 2 o f 2 Pag e 46 o f 60GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1


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

Pag e 4 7 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 

# 3IV I Environmenta l Labomtor 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 Effective Date: Q y- j Approve d By :

Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 Metho d ofAnalysi 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 f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

1 Scop e an d Applicatio n Thi s metho d i s t o b e use d t o quantif yPerfluorobutanoi cAci d (PFBA) , Perfluoropentanoi cAci d (PFPeA) , PerfluorohexanoicAci 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 Performance 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 alternat e metho d suc h a s ETS-8-15 4 "Detenninatio n o f Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
. Thi s metho d i s considere d a performance-base d method
. Data i s considere d acceptabl e a s lon g 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 ti 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 at 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 verit 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 predetermine d amoun t ofAST M Typ e 1 , 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 rLa b Dup ) Alaborator

yduplicat e sampl e i s a separat e aliquot ofa sampl e take n i n th e analytica l laborator ythat i s analyze d separatel ywit h identica l procedures
. Analysi s ofLDS s compare d t o that ofth e firs t aliquot give a measur e ofth 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 detemnin e i ftes t substance s o r othe rinterference s are presen t i n th e fiel d environment
. Thi s sampl e i s als o refen-ed t o a s a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 9 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
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 ofth e FD S compare d t o that ofth 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 o f sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

ymakin g a "fil l t o thi s level " lin e o n th e outsid e ofth e sampl e container
. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample
. I fth e expecte d rang e ofanalyt 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 f an 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 ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t o fth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p detemriin 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 mus t 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 of contro l matri xt o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yat th e tim e o

fsampl e extraction
. At least two level s are included , on e generall yat 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 xspike i s a n aliquot ofa sampl e t o whic h know n quantitie s oftarge t analyte s are adde d i n th e laboratory
. Th e LM S i s analyze d exactl ylik e a laborator

ysampl e t o detemnin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results
. Th e endogenou s concentration s o fth e analyte s i n th e sampl e matri xmust b e detemnined i n a separat e aliquot an d th e measure d value s i n th e LM S con-ected fo rthes e concentrations
. LMS s are optiona l fo ranalysi s ofaqueou 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 ofquantitatio n (LLOQ ) fo ra dataset i s th e lowes t 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
. To simplif ydat a reporting , th e LLO Q i s generall yselecte d a s th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria
. Sampl e LLOQ s are matrix-dependent
. Th e uppe rlimi t 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 of 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 as th e ULOQ
. ETS-8-044. 0 Pag e 3 o f 1 1 Metho d of 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 5 0 o f 6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 

### 3.1 1 Method Blan k A n aliquot ofcontro l matri xthat i s treate d exactl ylik e a laborator

ysampl e includin g exposur e 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 detemnin e i ftest 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 ofa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound
. 

### 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t nomnally foun d i n th e sample(s)
. Asurrogat 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 , surrogate(s ) ar e adde d t o al l sample s an d qualit y contro l samples
. Surrogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedure includin g sampl e collection , preparation , an d analysis
. Inclusio n ofa sun^ogat e 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 ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o prepare calibratio n standard s an d othe rrequire d analyt e solutions
. 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yofth e standard s fo rthi s metho d have no t bee n precisel 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 cenvironmen t an d a cun-ent awarenes s ofloca l regulation s regardin g th e handlin g ofth e chemical s use d i n thi s method
. Areference fil e ofmateria l safet y dat a sheet s (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 ofsolvents , pressurize d ga s an d solven t lines , hig h voltage , an d vacuu m systems . Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l 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 interf'erence s unde r condition s ofanalysi s b

yrunnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 1 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination
. Thes e ma yinclude , bu t are no

t limite d to : was h bottles , Teflon ® line d caps , autovia l caps , HPLC parts , etc . Th e us e o

fdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 

### 6 instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e ofpumpin g u p t o tw o solvents an d equippe d wit h a variabl e volum e injecto rcapabl e ofinjectin g 5-10 0 p L connecte d t o a tande m Mas s Spectromete r (LC/MS/MS)
. I Analytica l balance capabl e ofreadin g t o 0.000 1 g 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 ofspinnin 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 C I 8,4. 6 m m x10 0 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 :

Tim e (min ) % A % B FlowRat e (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 ma yb e use d provide d tha t dat a qualityobjective s are met . ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 2 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 

### 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 PFD A 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 mayprovid e quantitatio n o fisomers tha t more closel ymatche s NM R dat a an d ma yhave th e adde d benefi t o f increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a ar e me t t o assur e adequat e specificity
. Th e previou s infomnatio

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- C 4 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 PerfluorohexanoicAci d (PFH A- 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- CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDo A- 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 ofAnalysi 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 3 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s ma yb 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 : Alternativ e volume s ma yb e prepare d a s lon g a s 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 ofa 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 o

fstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. A n exampl e o fpurit yan d sal t correctio n i s give n belowfo rPFOS
. ^ . , ^ molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t o fsal t 4Q Q 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 CsFiySOs " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 |jg/m L (500 0 ng/mL ) mixe d workin g standard—^Ad d 0.5m L eac h o fth e lOOpg/m L SSS s t o a lOm 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 o f6 month s fro m th e dat e o fpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 4 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1

7. 5 Calibratio n Standard s Usin g th e workin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e a s a guideline
. Note : Volume s o fwate ran d worthin 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 of WS, ng/mL Volume of WS, fiL Final

Volume of Calibration

Standard

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

Concentration

of Calibration

Standard, ng/mL (ppb) in ASTM 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 ofglas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass
. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water . Prepar e metho d Q C sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials
. 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 rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-determine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are no t a t least twic e that ofth e metho d and/o rsolven t blanks
. Th e coefficien t ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.990 . Eac h poin t i n th e curve must b e withi n ±25 % 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 ofAnalysi 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 5 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
b e withi n ±30% . Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata
. Aminimu m of6 points wil l b e use d t o construc t th e calibratio n curve . I fth e calibratio n curve doe s no t meet acceptance criteria , perfor m routin e maintenance o rprepare a ne wstandar d curve (i fnecessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yofth e calibratio n curve . Analyz e a mid-rang e calibratio n standard , on e o fth e sam e standard s use d t o 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 last passin g CCV wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that ar e quantitate d above th e concentratio n ofth 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 f0.02 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 final report . 10. 2 Metho d Blank s Metho d blank

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

s ma yb e injecte d multipl e times , bu t n o 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 instmmen t calibration , prio rt o th e analysi s of CCV samples , an d a

t th e en d o

fth 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 % o fth e are a coun t ofth e LOQ standard
. Th e standar

d deviatio n ofth 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 ofth e metho d blank s excee d 50 % o

fth e LOQ standard , the n th e LO Q must b e raise d t o th e first standar

d leve l i n th e curve that meets criteria , o ralternatively , th e metho d blank s mus t b e evaluate d statisticall yt o detemnin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made
. 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l not b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s field 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 offive t o te n time s highe rtha n th e targete d LO Q an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t o fth e curve . Th e relative standar

d deviatio n ofth e contro l spike s evaluate d independentl ya t eac h concentratio n leve l 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 ofsample 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 o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 6 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s offield matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagged as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targete d fortificatio n level s shoul d b e a t leas t 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 determin e th e statemen t ofaccurac yfo ranalytica l results
. Th e averag e ofth e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 

### 1 1 Data 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 : A
. X r/

, . . (Pea k

Are a - Intercept )
__ Analyt e foun d (ng/mL ) = -^ ^ —xD F Slop e D F = facto rb

ywhic h th e final volum e wa s diluted , i fnecessary . Fo rsample s fortifie d wit h know n amounts ofanalyt e prio rt o extraction , us e th e followin g equatio n t o calculat e th e percen t recovery . Recover y- ^"^^'y*

® ^^^"^ ^ (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) ^ Analyt e adde d (ng/mL ) 

### 1 2 Method Performanc e An ymetho d performance parameter s that are no

t achieve d mus

t b e considere d i n th e evaluatio n o fth e data
. Nonconformance t o an yspecifie d parameter s must b e describe d an d discusse d i fth e Technica l Manage r(non GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data
. I fcriteri a liste d i n thi s metho d perfonnanc e sectio n are no t met , maintenance ma

yb e perfomned o n th e syste m an d sample s reanalyzed , o rothe raction s take n as appropriate
. Documen t al l action s i n th e ra wdata
. I fdat a are t o b e reporte d whe n 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 o fth 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 ofthre e syste m suitabilit ysample s are injecte d a

t th e beginnin g ofeac h analytica l m n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l ofth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial
. Th e syste m suitabilit yinjection s mus

t hav e are a count s wit h a n RS D ofS5% an d a retentio n tim e RS D ofS2 % t o b e compliant
. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t ofdeterminatio 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 mus t 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 must b e withi n 25 % ofth e theoretica l valu e (withi n 30 % fo rlowes t curve point)
. Sample s that are brackete d b

yCCVs no

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

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d ofAnalysi 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 7 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1
Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

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

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 , field matri x spike s an d laborator

ymatri xspikes
. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks
. Sectio n 1 0 contain s additiona l informatio n regardin g th e require d precisio n oflaborator ycontro l spikes
. 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n performin g thi s metho d wil l b e dispose d ofappropriately
. 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 infomnatio n fo rreconstructio n ofth e data
. Informatio 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 (instalmen 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 fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 8 o f6 0GLP10-01-02 ; Interi m Repor t 2 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Off-Sit e 61 0 Wells ; Septembe r201 1 

### ATTACHMEN TD : DEVIATION(S )

Pag e 5 9 o f6 0GLP10-01-02 ; Interi m Repor t 23 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s Off-Site 61 0 Wells ; Septembe r201 1 

### RECOR D O F DEVIATION/NONCONFORMANC E

/. Identification stud y/ Projec t No
. GLP10-01-02-2 3 Date(s ) o fOccurrence : 11/7/2011-k111007a-ex t Documen t Number : ETS-8-044. 0 Deviatio n typ e • SO P • Equipmen t Procedur e 0 Metho d (Ctieci < one ) • Protoco l • GP O • Other : / /
. Description

(attacli

extra pages as needed) 

### Metho d Requirements : 1 . RP D withi n ±20 % (sectio n 10.3)
. 

### Actua l procedure/process : 1 . Samplin g locatio n DAL-GW-6 1 O S ha d a n RP D of32 % fo rPFOS
. 

### ///. Actions

Taken (such as amendment

issued, SOP

revision, etc.) 

### Correctiv e Actio n ( • Ye s 0 No ) Reference : Acceptabilit yo fth e nonconformin g work : 1 . Th e PFO S RP D fo rsamplin g locatio n DAL-GW-6 1 O S wil l b e flagge d i n th e final report . Actions : • Haltin g o fWor k • Clien t Notificatio n • Wor k Recal l • Withholdin g o fRepor t IZ i Other : Deviation s wil l b e note d i n final report . Projec t Lead/PA I Approval : Stud yDirecto r(i fGLP) : Sponso rApprova l (fo rGL P protoco l deviations) : N A Date : Date : Dat e Technica l Reviewe r(optional) : N A Dat e Laborator y^epartnnen 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)

ETS-4-008. 7 Pag e 1 o f1 Documentation

of Deviations

and Control of Nonconforming

Testing

°