GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample

s Off-Sit e BP Propert

y- July201 1 

# 3 M

GLP10-01-01
. Interi m Repor t 19 : Analysi s o fPFO Ai n Groundwate rSample s Collecte d a t

th e Off-Sit e B P Propert yi n Decatur
. A L i n Jul y201 1 Stud yTitl e Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc
. 140 0 Westo n Way Westchester , PA1938 0 Phone:610-701-376 1 Autho r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor t Completio n Dat e

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

y 3 M Center , BId g 260-05-N-1 7 S t Paul , M N 55144 Projec t Identificatio n GLP10-01-01-1 9 Tota l Numbe ro f Page s

5 2 

# «i ^ lACCREDITED l Tli e testin g reported herei n mee t th e requirement

s ofISO/IE C 17025-200 5 "Genera l Requirement

s fo rth e Competenc

e of Testin g an d Calibratio n Laboratories" , I n accordanc e wit h th e A2L ACertificate #2052.01
. Testin g that complie s wit h thi s Intemationa l Standar d als o operat e i n accordanc

e wit h IS O 9001:2000
. 

### Testin g Cert

#2052.0 1

Page 1 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO AI n Wate rSample s Off-Sit e B P Property- Jul y201 1

Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1



### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 19
. Analysi s ofPFO

Ai n Groundwate rSample s Collecte d a t th e Off-Sit e B P Propert

yi n Decatur , A L i n Jul y201 1 Study : Analysi s of Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

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

t th e test sit e have no

t bee n determine d unde rGLPs
.
%
.



# X ( Gar yHojfiensjein , Sponso rRepresentative Date

^ Jaisimh a Kesari , P.E. , DEE , Stud yDirecto rDat e

Pag e 3 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 19
. Analysi s ofPFO

Ai n Groundwate rSample s Collecte d a t th e Off-Sit e B P Propert

yi n Decatur , A L i n Jul y201 1 Study : Analysi s of Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s repor

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

ymanagemen t an d stud ydirector
.
Inspectio n Date s 8/12/11,8/15/1 1 Phas e Data / Interi m Repor

t Dat e Reporte d t o

Testin g Facilit y Managemen t 8/23/1 1 Stud yDirecto r 8/23/1 1 

# ^^xs~-i { QA U Representative

Pag e 4 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1



### TABL E O F CONTENT S GL P Complianc e Statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e of Contents 5 List of Table s 6 1 Stud yInformatio n 7 2 Summar

y8 3 Introductio n 9 4 Tes t & Contro l Substance s 9 5 Reference Substance s 1 0 6 Test Syste m 1 0 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 2 8. 3 Limi t of Quantitatio 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 y1 6 8. 8 Fiel d Matri xSpike s (FMS ) 1 6

Pag e 5 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

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 Attachment s 1 9 1 3 Signature s 2 0 

### LIS TO F TABLE S Tabl e 1
. Summarize d PFO AResults (B P Groundwater , Decatur , AL , Jul y2011 ) 9 Sampl e Descriptio n Ke

yCod e 1 0 Tabl e 2
. Instrumen t Parameter s 1 1 Tabl e 3
. Liqui d Chromatograph yCondition s 1 2 Tabl e 4
. Mass Transition s 1 2 Tabl e 5 . Limi t of Quantitatio n (LOQ ) 1 3 Tabl e 6
. Laborator

yContro l Spik

e Recover

y1 4 Tabl e 6 continued
. Laborator yContro l Spike Recover

y1 5 Tabl e 7 . Analytica l Metho d Uncertaint y1 6 Tabl e 8
. Fiel d Matri xSpike Level s 1 6 Tabl e 9
. DA L GWBPMW4 7 11071 3 1 7 Tabl e 10
. DALGWBPMW12 1 11071 3 1 7 Tabl e 11
. Tri p Blan k

1 7 Tabl e 12
. Rinseat e Blan k 1 8

Pag e 6 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

j 1 Stud yInformatio n Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Stud yDirecto r Jaisimh a Kesari , P.E. , DE E Westo n Solutions , Inc
. Westchester , P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 St
. Paul , M N 55144 Stud yPersonne 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 (651)-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 yDate s Stud yInitiation : Marc h 8,201 0 Interi m Repor

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

t Completion : Dat e of Interi m Repor t Signin g Locatio n o f Archive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792
. Th e tes t substanc e an d analytica l referenc e standar d 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 f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

1 2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m two differen t well s locate d a t th e Off-Sit e B P Propert

yi n Decatur , AL
. Atota l o fthirtee n sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator

yfo rperfluorooctanoat e (PFOA) analysi s an d include d duplicat e groundwate r sample s fro m eac h samplin g location
. Sample s als o include d tw o fiel d matri xspike (FMS ) sample s fo r eac h location , on e tri p blan k containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d on e equipmen t rinseate. Th e equipmen t rinseate blan k di d no t have a FM S sampl e prepare d fo rth e determinatio n o f PFO

Arecovery . Th e groundwate rsamples , tri p blanks , an d equipmen t rinseate blan k were receive d fro m Westo n personne l o n Jul y18,2011
. Al l ofth e sample s were prepare d an d analyze d fo rPFO

Afollowin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 unde r3 M projec t GLP-10-01-01-19
. Th e averag e measure d PFO Aconcentration s are summarize d i n Tabl e 1
. Th e equipmen t rinseate an d th e tri p blank s were belowth e lowe rlimi t ofquantitatio n (LLOQ ) o f0.025 0 ng/mL , indicatin g adequat e contro l o f sampl e contaminatio n durin g shippin g an d sampl e collections
. Th e analytica l uncertaint

ywa s estimate d a

t 100±14%
.

Pag e 8 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

Tabl e 1
. Summarize d PFO AResult s (B P Groundwater , Decatur , AL , Jul y2011 ) Sampl e I D DA L GWBPMW4 7 11071 3 DALGWBPMW12 1 11071 3 Tri p Blank

s (Milli-Q TM Water) GLP10-01-01-1 9 Equipmen t rinseate blank : DALGWBPMW12 1 Avg
. PFOA Concentratio n (ng/mL ) 0.35 1 0.064 8 < 0.025 0 < 0.025 0 Relativ e

Percen t Differenc e 2.0 % 10 % N/ A N/ A N/A : no t applicabl e Th e analytical uncertaint

yfo rPFO Awa s estimate d a t 100+14%
. [ " 3 Introductio n Thi s analytica l stud ywa s conducte d a s par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama
. Th e objective ofth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctanoat e (PFOA ) i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m tw o well s locate d a t th e off-sit e B P propert

yi n Decatur , A L fo rPFO

Ai n a n effor

t t o characteriz e regiona l groundwate r conditions
. Th e 3 M Environmenta l Laborator yprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling
. Sampl e bottl e set s fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d tw o fiel d spike samples
. Eac h empt

ycontaine rfo rgroundwate rsampling s wa s mari<e d wit h a "fil l t o here " lin e t o produce a final sampl e volum e of 20 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 PFO Aprio 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^^Cs-PFO A(intema l standard ) a

t a nomina l concentratio n of 1 ng/mL
. Se e sectio n 8. 8 ofth e repor t fo rfield matri xspike levels
. 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 "Determinatio n ofPerfluorinate d Compound s i n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Th e us e ofa n intema l standar

d wa s use d t o ai d i n th e dat a qualit yobjectives
. Tabl e 1 summarize s th e averag e PFO Aconcentration s fo rth e duplicat e groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples
. Table s 9-1 2 summariz e th e individua l sampl e results an d th e associate d FM S recoveries
. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s are reporte d an d discusse d elsewhere i n thi s report . 

### 1 4 Tests , Contro l Substance s I There wa s no

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

Pag e 9 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1



### \ 5 Referenc e Substance s Th e analytica l reference substance s use d fo rthi s stud yare liste d below
.

Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Us e Sourc e Expiratio n Dat e Storag e Condition s Chemica l Lo t Numbe r TO R Numbe r Physica l Descriptio n Purit y PFO A(Linear ) Perfluorooctanoat e C7F15COO H CA S #335-67- 1 Targe t Analyt e Referenc e Standar d Oakwoo d Product s 01/17/201 8 Froze n 344 0 TCR07-004 1 Powde r 99.1 % PFO A

(Unea r+ Branched ) Perfluorooctanoat e C7F15COO H /Ammoniu m Sal t GA S #335-67- 1 LC S Referenc e Standar d 3 M 02/27/201 7 Froze n 33 2 TCR-12 3 Whit e powde r 95 % "Cs-PFO A

Perfluorooctanoat e ''C8HF15O 2 CAS#MPFC-C-051 1 Intema l Standar d Wellingto n 05/25/201 4 Froze n IVIPFC-C-051 1 TOR11-001 6 Liqui d NA<^ ' (1 ) Compoun d i s par

t o f a custo m mixtur

e o f mass-lat)ele d periluorinate d compound s at a concentratio n o f5. 0 pg/mL
. 

### 6 Tes t Syste m There wa s no

t a tes t syste m fo rthi s stud yi n th e classi csens e ofa GL P study
. Thi s stud ywa s conducte d fo ranalysi s of groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L byWesto n Solutions , Inc
. personnel
. Sample s fo rthi s stud yare "rea l worid " environmenta l samples
. Sampl e Descriptio n Ke yCode
. strin g Numbe r Exampl e 1 2 3 4 strin g Descripto r Exampl e DA L GWBPMW4 7 011071 3 Sampl e Locatio n Wel l I D Samplin g Dat e Sampl e Typ e DAL = Decatur , Alabam a Example : BPMW4 7 110713-Jul y13,201 1 0=primarysampl e DB=duplicat e sampl e L S = lo wspik e M S = mi d spik e H S = hig h spik e

Pag e 1 0 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

\ 7 Metho d Summar yj 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Determinatio n of Perfluorinate 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 GLP10-01-01-1 9 were returne d t o th e laborator ya t ambien t condition s o n Jul y18 , 2011
. Sample s were store d refrigerate d at th e laborator y afte rreceipt
. Ase t of laborator yprepare d Tri p Blan k

an d Tri p Blan k

field matri xspike s were sen t wit h th e set of sampl e collectio n bottles
. 

### 7. 3 Sampl e Preparatio n Sample s were prepare d byremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Durin g th e preparatio n of th e laborator ycontro l samples , a n aliquot ofa separat e intema l standar d spikin g solutio n wa s adde d t o th e laborator ycontro l sample s (nomina l concentratio n o f1 ng/mL)
. Th e sample s bottle s were spike d wit h a n intema 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 collection
. 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFO Ausin g hig h performance liqui d chromatography

/ tande m mas s spectrometr y(HPLC/MS/MS)
. Detaile d instrumen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmas s transition s analyze d are describe d i n th e ra wdat a har

d copie s place d i n th e final dat a packet , an d are briefl ydescribe d belowi n Tabl e 2 , Tabl e 3 an d Tabl e 4
. Tabl e 2
. Instrumen t Parameters
. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETSKIr k ETS-8-044. 0 7/28/11-7/29/1 1 Agilen t 120 0 Betasi l C1 8 (4. 6 m m X 100 mm) , 5 n Betasi l 01 8 (4. 6 m m X 10 0 mm) , 5 u

2 5 n L /Applied Biosystem s AP I 550 0 Tutb o Spra

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

Pag e 1 1 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

Tabl e 3
. Liqui d Chromatograph yConditions
. ste p Number Tota l Tim e

(min ) Flo wRat e

(pUmIn ) Percen t A

( 2 m M ammoniu m acetate ) Percent B (Methano O 7/28/11-7/29/1 1 Analysi s 0 1 2 3 4 5 0. 0

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

75 0 75 0 75 0 75 0 75 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 Tabl e 4
. Mas s Transitions
.

Analyt e PFOA Mas s Transitio n Q1/Q 3 413/36 9 413/21 9 413/16 9 Intema l standar d fCJPFO A Mas s Transitio n Q1/Q 3 421/37 6 Dwel l tim e wa s 3 0 mse cfo reacf i transition
. Tfi e individua l transition s were summe d t o produce a "tota l io n chromatogram " (TIC) , whic h wa s use d fo rquantitation
. 8 Analytica l Result s 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 ofth e stoc k solutio n containin g th e targe t analyte s into a laboratory-prepare d syntheti cgroundw^ate 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 at a nomina l concentratio n of1 ng/mL
. Acalibratio n curve rangin g fro m approximatel y0.02 5 ng/m L t o 10 0 ng/m L wa s prepared
. Sampl e DA L G W BPMW4 7 wa s quantitate d usin g extema l calibratio n du e t o inconsisten t interna l standard
. 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 fi t th e dat a fo reac h analyte
. Th e dat a were no t force d throug h zero durin g th e fittin g process . Calculatin g th e standar

d concentration s usin g th e pea k area / pea k are a ratio s an d th e resultan t calibratio n curve confirme d accurac

yo f eac 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 o

f 10 0 ±25 % (10 0 ±30 % fo rth e lowest curve point) were met fo ral l analytes
. Th e con-elatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFOA
. 

### 8. 2 Syste m Suitabilit y Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g o fth e 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 o fles s tha n o requa l t o 2 % RS D wa s met fo rPFOA
.

Pag e 1 2 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

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

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

yrequirements an d fo rwhic h th e are a counts are a t least twic e thos e ofth e appropriat e blanks
. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 5 . Tabl e 5 . Limi t o f Quantitatio n (LOQ)
. Analysi s Dat e iiim ^ PFOA

LOQ , ng/m L 0.025 0 8. 4 Continuin g Calibratio n Durin g th e cours e of eac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l CCVs met metho d criteri a of 100 % ±25 % fo rPFOA
. 

### 8. 5 Blanl( s Thre e type s of blank

s were prepare d an d analyze d wit h th e samples : solven t blanks , tri p blanks , an d equipmen t rinseate blanks
. Solven t blan k results were reviewe d an d use d t o evaluat e metho d performance t o detemnin e th e LO Q fo rPFOA
. Tri p blank s refiec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience
. Equipmen t rinseate blank s are aqueou s sample s that reflec

t th e efficienc

yof equipmen t cleanin g i n th e field betwee n differen t sampl e collection s an d are proof of n o cros s contaminatio n ofsample s fro m th e equipment
. 

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

Awere prepare d a

t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias
. Th e linea ran d branche d LC S met metho d acceptance criteri a a t al l levels
. Al l LC S sample s were use d i n th e detemninatio n of metho d uncertaint yi n sectio n 8.7
. Th e followin g calculation s were use d t o generat e dat a i n Tabl e 6 fo rlaborator ycontro l spikes : 1 ^ o n . r . Calculate d Concentratio n . , .„. , LC S Percen t Recover

y= * 100 % Spik e Concentratio n LCS % RS D = "'^"^^^' ^

^^'^'^"° " "-^ ^

^^P"^'^ " • 100 % averag e LC S recover

y

Pag e 1 3 o f 5 2Tabl e 6
. Laborator yContro l Spik e Recovery
. GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

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

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

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

1.9 7 2.0 2 10 2

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

19. 3 19. 3 96. 0

97. 0 96. 8 96.6 % ±0.55 % ETS-8-044. 0 Intema l standar d calibratio n Analyze d 7/28/201 1
La b I D LCS-110726-1 0 EC F LCS-110726-1 1 EC F LCS-110726-1 2 EC F Averag e ±%RS D LCS-110726-1 3 EC F LCS-110726-1 4 EC F LCS-110726-1 5 EC F Averag e ±%RS D LCS-110726-1 6 EC F LCS-110726-1 7 EC F LCS-110726-1 8 EC F Averag e ±%RS D LI m Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 ia r* Branche d P F

Calculate d Concentratio n (ng/mL ) 0.20 6 0.21 5 0.21 7 O A

VoRecover y 104 10 8 10 9 107%±Z5 % 1.9 9 1.9 9 1.9 9 1.9 9

2.0 1 2.1 4 10 0

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

21. 7 22. 7 10 2

10 9 11 4 108 % ±5.6 %

Pag e 1 4 o f 5 2Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

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

Calculate d Concentratio n (ng/mL ) 0.23 2 0.23 1 0.23 7 VoRecover y

11 7 11 6 11 9 117 % ±1.3 % 1.9 9 1.9 9 1.9 9 2.2 0

2.1 2 2.1 6 110

10 7 10 9 109 % ±1.4 % 19. 9 19. 9 19. 9 20. 3

20. 4 20. 5 10 2

10 3 10 3 103 % ±0.56 % ETS-8-044. 0 Extema l standar d calibratio n Analyze d 7/28/201 1
La b I D LCS-110726-1 0 EC F LCS-110726-1 1 EC F LCS-110726-1 2 EC F Averag e ±%RS D LCS-110726-1 3 EC F LCS-110726-1 4 EC F LCS-110726-1 5 EC F Averag e ±%RS D LCS-110726-1 6 EC F LCS-110726-1 7 EC F LCS-110726-1 8 EC F Averag e ±%RS D Lin t Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 iar * Branche d P F

Calculate d Concentratio n (ng/mL ) 0.23 2 0.22 7 0.23 3 O A

VoRecover y 11 7 114 11 7 116 % ±1.5 % 1.9 9 1.9 9 1.9 9 2.0 9

2.1 4 2.2 6 10 5

10 8 11 4 109 % ±4.2 % 19. 9 19. 9 19. 9 21. 5

22. 9 23. 8 10 8

11 5 120 114 % ±5.3 %

Pag e 1 5 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1



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

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

yan d precision
. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2
. Th e standar d deviatio n i s calculate d fo rth e set o faccurac yresults (i n % ) obtaine d fo 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 con-espond s t o a confidence leve l of 95%
. Tabl e 8
. Analytica l IVIetho d Uncertainty
. Analyt e PFO A Metho d

ETS-8-044. 0 Standar d Deviatio n 7.0 1 IVIethod

Uncertaint y ±14 % 

### 8. 8 Fiel d Matri xSpike s (FMS ) Two field matri xspike s were collecte d at 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 byaddin g a measure d volum e of field sampl e t o a containe rspike d b yth e laborator

ywit h th e targe t analyte s prio rt o shippin g sampl e container s fo rsampl e collection
. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of 100±30 % confin n 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 o f th e analyte s o finterest
. Fiel d matri xspike concentration s must b e 50 % o fth 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 of thi s report . Tabl e 9
. Fiel d Matri xSpik e Levels
. Samplin g Locatio n MW47 IVIW12 1 Tri p Blan k Spik e Leve l Lo w Hig h Lo w Hig h Lo w Mi d Hig h PFOA , ng/m L

0.25 0 1.0 0 2.0 0 20. 0 0.25 0 1.0 0 20. 0

^ . , „ „ (Sample Concentrationof FMS - Average Concentration : FieldSample & FieldSampl e Dup. ) .„,„„„ , FMS Recover

y = - ^ ^^ * 100 % Spik e Concentraton 

### \ 9 Dat a Summar yan d Discussio n | 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 Blan k an d rinseate 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 y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspike recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges .

Pag e 1 6 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

Tabl e 10
. DA L G W BPMW4 7 11071 3 (1 )

3 M LIM S I D GLP10-01-01-19-00 5 GLP10-01-01-19-00 6 GLP10-01-01-19-00 7 GLP10-01-01-19-00 8 Descriptio n DA L G W BPMW47 0 11071 3 DA L G W BPMW47 D B 11071 3 DA L G W BPMW47 LS 11071 3 DA L G W BPMW47 H S 11071 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 0.34 7 0.35 4 0.63 8 1.4 3 VoRecover

y N A NA 11 5 108 0.35 1 ng/m L ±2.0 % NA = No t Applicabl e (1 ) Results generate d usin g extema l standar d calibration
. Tabl e 11
. DA L G W BPMW12 1 11071 3 (1 )

3 M LIM S I D GLP10-01-01-19-01 0 GLP10-01-01-19-01 1 GLP10-01-01-19-01 2 GLP10-01-01-19-01 3 Descriptio n DALGWBPMW12 1 011071 3 DALGWBPMW12 1 D B 11071 3 DA L G W BPMW12 1 LS 11071 3 DA L G W BPMW12 1 H S 11071 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFOA Concentratio n (ng/mL ) 0.068 2 0.061 4 2.1 0 20. 6 VoRecover

y NA NA 102 10 3 0.064 8 ng/m L 110 % N A= No t /Applicabl e (1 ) Results generate d usin g intema l standar d calibration
. Tabl e 11
. Tri p Blan k (1 )

3 M LIM S I D GLP10-01-01-19-00 1 GLP10-01-01-19-00 2 GLP10-01-01-19-00 3 GLP10-01-01-19-00 4 Descriptio n DA L GWTRIP 1 011071 3 DA L GWTRIP 1 LS11071 3 DA L GWTRIP 1 M S 11071 3 DA L GWTRIP1HS 11071 3 PFOA Concentratio n (ng/mL ) <0.025 0 0.24 9 0.96 1 20. 3 VoRecover

y N A 99. 6 96. 1 102 N A= No t Applicabl e (1 ) Results generate d usin g intema l standar d calibration
.

Pag e 1 7 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

Tabl e 12
. Rinseat e Blan k (1 )

3 M LIM S I D GLP10-01-01-19-00 9 Descriptio n DA L G W BPMW12 1 R S 11071 3 PFOA Concentratio n (ng/mL ) <0.025 0 VoRecover y NA N A= No t /Applicabl e (1 ) Results generate d usin g intema l standar d calibration
.

Pag e 1 8 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

1 0 Conclusio n 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 rPFOA
. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein
. 

### 1 1 Data/Sampl e Retentio n 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
. \1 2 Attachment s Attachmen t A : Protoco l Amendmen t 1 9 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d - ETS-8-044. 0

Pag e 1 9 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1

1 3 Signature s 

# P-Jzshe^f f Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date



### ^ 'j/^Ct/sr^a/l Willia m k ! Reagen , Ph.D. , 3 M Environmenta l Laborator yManage r Dat e

Gar yHohenstein , 7 M Sponso rRepresentative 

# gAMJ y \ Date

Jaisimh a Kesan , Stud yDirecto r

Pag e 2 0 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 2 1 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9


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

SIV i Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
PROTOCO L AMENDMEN TNO
. 1 9

Amendmen t Date : Julys , 201 1 Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

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

GLP10-01-0 1 Samplin g Even t Decatu rPhas e 3 ; Off-Sit e B P Property

Pag e 1 o f7 Pag e 2 2 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9 

### Thi s amendmen t modifie s th e followin g portio n o f protocol : "Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program "

PROTOCO L READS : N o change s t o th e wordin g o f th e protoco l are required
.

/^ENDTOREAO : N o change s t o th e wordin g o f th e protoco l ar e required
. Thi s amendmen t onl yaddresse s an d document s th e additio n o f th e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o f groundwate rsample s a s par t o f th e 3 M Decatu rPhas e 3 Progra m fo rPFOA(GLP10-01-01)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e o f th e wee k o f Jul y11 , 2011
. Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s project GLP10-01-01-1 9 an d reporte d a s interi m report GLP10-01-01-19 , (reflectin g stud yGLP10-01-0 1 an d amendmen t -19)
.
Reaso n ; 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 existin g well s locate d a t a n off-sit e locatio n o n th e B P Property
. Th e GP O i s fou rpage s i n lengt h an d include d a s attache d t o thi s amendmen t fonm
.

Pag e 2 o f 7 Pag e 2 3 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9



### Amendmen t Approva l 

# ^'H ] fMlh'^'i^i / 

# 2 X 

# I L Gar yHbhenstein , Sponso rRepresentative 

# d c Date



# '^//V^^> ' Clesto n C
. Lange , Principa l Analytica l Investigato r Date 

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

# kml ' Date



# TMi l Jaisimh a Kesari^E^. , DEE , Stud yDirecto r Dat e

Pag e 3 o f7 Pag e 2 4 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9 

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

yHohenstein , 3 M EHS&Opn s From : Susa n Wolf , 3 M EHS&Opns ; Environmenta l La b cc : 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 : Jul y6,201 1 Subject : Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 1 9 - Decatu rPhas e 3 ; Off-Sit e B P Property 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r Projec t Schedule/Tes t Date s 3i M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone : (651 ) 737-357 0 qahoheristein(a^mmm,co m 3 M Environmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S Opns
. Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wkreaqen(S>mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanQeSJmmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s TimothY,ffinak(awestonsQlution5.eo m Phone : (334).332-912 3 GLP10-01-01-1 9 Dep t #530711 , Project #002267444 9 Samplin g schedule d fo rth e wael ^ o fJul y11,201 1 Al l verba l an d writte n correspondenc e wil l t> e directe d t o Gar

yHotienstei n an d Ja i Kesari
.

Pag e 4 o f 7 Pag e 2 5 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample

s Off-Sit e BP Propert

y- July201 1 Analytica l Protocol : GLP10-01-O 1

Amendmen t 1 9 

### 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 location s fo rPerfluorooctanoi cAci d (PFOA ) fro m existin g well s locate d o n th e B P property . Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC 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 fJul y11 , 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 r PFO Aar e o f a know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-01-19
. 

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

o fJul y11 , 2011
. Sampl e bottle s wil l b e shippe d i n cooler s ovemigh t t o 3 M Decatu rfo raniva l o n Friday , Jul y8 , 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 Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 4 Tes t Parameter s Th e targete d limi t o f quantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFOA
. Tw o samplin g location s have bee n specified
. Se e attachmen t Afo ra lis t ofth e samplin g location s that wil l b e collecte d fo rthi s samplin g even t Fo reac h samplin g location , a tota l o ffou rsampl e bottle s wil l b e collecte d (sample , sampl e duplicate , lowfiel d matri xspike , an d hig h fiel d matri xspike)
. Th e iil 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 se t o ftri p blank s consistin g o freagent-grad e wate ra s wel l tri p blan k spike s wil l b e prepare d a t 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 o f^^Cs-PFO A(intema l standard ) at a nomina l concentratio n o f 1 ng/mL
. Al l sampl e bottle s wil l als o includ e th e additio n of"C4-PFO A(sumsgate spike ) at a nomina l concentratio n o f 0. 1 ng/mL
. On e additiona l bottl e wil l b e prepare d t o b e use d fo rth e preparatio n ofth e equipmen t rinseate blank
. A500m L bottl e o flaborator yreagen t wate rwil l b e sen t wit h th e sampl e bottle s t o b e use d t o generat e th e rinseate blan k sample
. Th e tabl e beb wlist s th e matri xspike level s that wil l b e prepared
. Wel l No
. MW.4 7 MW-12 1 Tri p Blan k Sampl e Leve l Low Hig h Low Hig h Low Mi d Hig h Spik e Cone
. (ng/mL ) 0.2 5 1. 0 2. 0 2 0 0.2 5 1. 0 2 0 

### 5 Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S follovirtn g ETS-8-044. 0 "Determinatio n ofPerfluorinate d Confipound s i n Wate rb yHig h Perfbnmanc

e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Pag e 5 o f 7 Page 2 6 o

f 5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9 /^alysis"
. Alternately , sample s ma yb e analyze d b

yETS 8-154. 3 "Determinatio n o fPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rBySoli d Phas e Extractto n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
. Th e data qualit

yobjective s fo rthes e studie s are quantitative result s fo rth e targe t analyte s wit h a n analytica l accurac yo f 100±30%
. Fiel d matri xspike s not yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly
. Where applicable , sample s wil l b e analyze d against a n intema l standar d calibratio n curve . Eac h curve poin t wil l contai n isotopically-labele d perfluorocartxjxyli cackJ s an d perfluorosulfbni cacid s at a nomina l concentieitio n o f1 ng/mL
. Th e calibratio n curve wil l b e generate d b ytakin g th e rati o o fth e standar d pea k are a counts ove rth e intema l standar

d pea k are a count s t o fi t th e dat a 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 results fo rth e sample , sampl e duplicate , an d th e fiel d matri xspikes
. Tri p blan k an d tiip 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 tiie fleld. Laborator ycontro l spike s ofreagen t wate rprepare d at th e time o f sampl 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
. Metho d blank

s o f reagen t wate rprepare d a t th e time ofsampl e extractio n wil l b e use d t o detennin e th e mettio d detectio n limit
. Fo rthos e samplin g location s where th e field matii xspike leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concenti^tions , a laborator ymatri xspik

e ma yb e prepare d an d wil l b e include d i n tiie final report .

Pag e 6 o f 7 Pag e 2 7 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 /Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 9 Attachmen t A Bottl e reques t - B P Wei l Samplin g Wee k o f1 1 Jul y201 1 Young , Charle s T
. cbjacoby2@mmm.com , stwolf@mmm.com , clange@mmm.co m 07/05/201 1 01:5 1 PM

^ ^ "Frinak , TimothyR. " Th e acces s agreement

fo r samplin g tw o existin g well s o nth e B Ppropert

y i s i nplac e andit

i s anticipate dtha

t samplin g will occur

nex t week a s apar t o f th e Phas e 3 effort . Analyse s shoul db e performe dunder GLPlO-01-01 . Th e forme r (abandoned ) well s 60I Rand601 Lonth e B Ppropert y wer e clos e t o th e new location s an dwoul dbes t serv e a s a nestimate o f

th e appropriate spikin g levels . PFO Alevel s were 0.10 7 ng/m L(5/2006 ) and0.17 9 ng/m L (9/2007 ) i nth e residuu mwel l 601 Rand19. 8 ng/m L(5/2006 ) and1 1 ng/m

L(9/2007 ) i

nth e bedroc k

well 601L . Th e existin g B Pwell MW-4 7 i s th e residuu mwel l andMW-12 1 i s th e bedroc k well . I nadditio nt o sample s fi-omthes e tw o wells , arinseate blank wil l b e collected . Ca nyou prepare abottl e set

fo r shipment to Marti nSmit

hat th e Decatur

facilit y wit harrival o nMonday , July 11 , 2011 ? Thanks , Charli e Charle s T . Youn g Technica l Directo r Westo nSolutions , Inc . 1400 WestonWa

y (5-2 ) Wes t Chester , P

A 1938 0 (610)701-378 7 Fa x (610 ) 701-340 1

Pag e 7 o f 7 Pag e 2 8 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


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

Pag e 2 9 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFOAi n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

Dat a printe d b

yST W Printin g Time : 9:23:5 7 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1
Pag e 3 0 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

Sampl e Type : 

# I San^Name:-k110728a016 ' Sanvt o ID : "1 1 0O»M rFte:'V110728a.wti r PMkNBme:"13C8PR3A-IS{ls rM»M««) : "421.000376.00 0 Da " Comntn t "1. 0 ngAn L F C «t d I n Synlh
. Wate rAnnotttkin : * Sampl e Index : 1 6 idar d .0 0 ng/m L2^5
- 2.4e5 - 23«5 - M O II I "e5
.

2.1e5 - 2JO»5 - laeS 1^5 - 1.7»5 - 1.6e5 - 1^5 - 5 '*= • I 128 5

* ,.,.5 ^ 1.0e 5 9.0e 4 8.0a4 ' 7J)ft 4 6.0»4 ' 5.0» 4 4.0»4 ' 3J>e4 ' 2.0e4 ' 1.0a 4 Calculate dCone : Acq . Date : Acq , Time : Modified : Proc . Mgoclthm : Hols e Percentag e N/ A 7/28/201 1 3:16:3 2 P

M Ye s Specif y Para m 5 0 Base . Sub . Window : 1.0 0 n > Peak-Split , Fac t t : 2 Repor t Larges t

Peak : Ye s Min
- Pea k

Heigfi t Min . Pea k

Hidth : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio n Time : 0.0 0 0.0 0 30. 0 se c 15. 8 mi n N o Valle y 15. 7 Bi n Area : 150581 7 count s Height : Star t Time : En dTime : .52«*00 S cp s 15. 6 mi n 16. 0 mi n

0.0 - 13. 5 

# I I S«mpteName:'VI10728aO2a rSanvtelD:-LCS-110726-1 - Rto : 1(110728a.»i r P«akNaine:-13CSPPCWrlS(IS} * Uats(e«>:-421.00(V376.000Da ' Ccntntn t 'D.2pp b LCS * Annotation : ~ e Type : Q C 

# I S«mptoN»ma:T(110728aO2 rSampt e ID : "1 1 00&« rFile : 1(1107288
. PM k NanM:-13C6F^^A4S<IS) - MaM(M) : -421.00CV376.00 0 Da * Commwui-MrthodHart TAnnotation: " Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Noia e Percentag e Base . Sub . Wlnd o PeaK-SplIt . Fac t Unknow n 1.0 0 K/A 7/2B/201 1 7:08:2 8 P

M Ye s Specif y P a 5 0 • : 1.0 0 t : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea K

Midth : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio n Time : Area : 1 7 Height : Star t Time : En dTime : 0.0 0 0.0 0 0 30. 0 15. a N o Valle y 15. 7 n Saa 2 cou r .016*00 5 15. 6 R 16. 0 n



# I SwnpieN«me:-k110728a03 rSarr«>lelD:-LCS-110726-4 - Fl« : I d 10728a
. PeakHame:-13C8Pf=OA4S(IS) - Uatt{M) : "421.000076.00 0 Oa " Commw * *2pp b LCS " Annotaflon : ~ Sampl e Index : 3 1 Sampl e Type : Q C 0.99 3 ng/m L Samp l Conc e Calc u Acq . Modi l Proc . Base . Peak
Re po i Min . Min . Smoo l R T w : Expe c Us e R Int . Rete n Area : Heig h e Type : ntration : late dCon e )ace : Time : led : Algorith m O C 0.99 3 N/ A 7/28/2 0 7:29:3 2 Ye s Percentage : 5 0 1 P M P a Sub . Window : 1.0 0 Split . Fa c t Larges t ?ea k Heig h Pea k Hidt h lin g Widt h re dRT : elativ e R

T Type : :lo n Time : o r : 3

eak : Y : 0

0 0 30. 0 15. 8 N o Bas e T o 15. 8 166627 7 2.93e*00 . U

U

B a Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fac t N/ A 7/28/201 1 a : 3?:5 4 P

M N o Specif y P a 5 0

- : 1.0 0 3r : 2 Rejior t Larges t

Peak : Ye s Min . Pea K

Heigh t Min . Pea hWidth : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio n Time : 0.0 0 0.0 0 0 30. 0 15. a N o Valle y 15. 8 Area : 166509 8 co u Height : Star t Time : En dTime : .706.00 5 15. 6 p 16. 0 E

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 : 9:35:1 2 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 6 Pag e 3 1 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 •ETS-Kir k Result s Name : kll0728a.rd b 

# I Sampl e Name : "kHOTZSaOs rSamr^a ID:'LCS-11072e- rnia:-k110728a.wlt r PaakNinM:-13C8PFOA«0S> ' Maaa{aa) : "421.000/376.00 0 Da ' Commart : '20pp b LCS " Ajvwtatton : - Sampl e Index : 34 Sampl e Type : Concentrati < Calculate dCone : Acq . TICM : Modified : Proc . Algor : Nois e Perce n :hm : Base . Sub . Wlnd o Peak-Split . Repor t Larg e -ac t

S t P Min . Pea K

Heigh t Min . Pea k

H : Smoothin g U : R T Window : Expecte dRT : Us e Relativ e Int . Type : dth :

RT : Retentio n Time : Area : Height : Star t Time : En dTime : Q C 0.99 3 N/ A 7/28/2 0 9:36:1 4 N o Specif y S O

- : 1. 1 3r : 2 ak : Y

e 0 0 30. 0 15. 8 N o Bas e T o lE. e 159390 4 c .51e*0O 5 15. 6 15. 9 1 P M P a 1 > O O n n

B a

15. 0 15. 5 16. 0 16. 5 Sampi e Name : 1(110728*044 " Sampl a ID : 'LCS-110726-1 TRIe : V t 10728a.vi« r PeakNanM:-13C8Pr=OA-IS{!S) - hlaM(M):'421.000/376.00 0 Da ' Commen t "2pp b LC S ECF " Annotation : " * Samp l I SampleNama:'V11072e»O41 - Sampl e ID:'LCS-110726-10 - Fie:"k110728a.wH T Pea k Name : *13C8PFOA-IS(IS} - MaM(ee) : '421.0001376.00 0 Oa* ^ Comment : •0.2pp b LC S EC P Annotation : - Sampl e Sampl e Type : Concentration : Calculate dCon e Acq . Time : Modified : Proc . Algorithm : ; Hols e Percentage : Base . Sub . Mindow : Peak-Split . FactO J Repor t Larges t Min
- Pea k

Height ; Min . Pea k

Width : Smoothin g Midth : R T Window : Expecte dRT : Us e Relativ e RT : 0.99 3 n c K/ A 7/29/201 1 12:04:0 8 A

M

Int . Type : Retentio n 1 Height : V a1 le y »e : 15. 7 167905 2 c ( 2.62et00 5

13. 5 Sampl e tJame : '1c11072eaO4 rSampl e ID : TCS-110726-18 - Fie : 1c110728a.wtt r Pea k Name : -13C8PFOMS{IS) - Matc<et) : "42 1 .OOCVST&OO O Da * Comment : "20pp b LC S EC rAnnotation : " " Sampl e Index : 4 7 Sampl e Type : Q C Concentration : 0.99 3 ng/m L Calculate dCone : N/ A

rithm : Specif y Parameter s - M Q II I Sampl e Type : Q C 0,99 4 ng/m L 2.6e5
- Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hois e Percentag e 7/:9/:oi i 1:07:3 2 A

M Ye s Specif y Pa r 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Hidth : Smoochin g Width ; R T Window : Expecte dRT : Us e Relativ e RT : int . Type : Retentio n Time : 0.0 0 0.0 0 0 30. 0 s 15. 6 n

i N o Valle y 15. 7 m Area : 162702 S cou n Height : Star t Time : En dTime : .Ble*00 S c 15. 6 H

I 15. 9 n ameter s - M Q II I

point s e c i n

L s i n I n Sub . Window :
Min . Pea k

Width : Smoothin g Width : R T Window : Expecte dRT :

159720 2 c t 2.53e-f00 5 15. 6 15. 9

13 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 Tlnw.mi n Dat aprinte db y ST

W Printin g Time : 9:35:1 2 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 2 o f 6 Pag e 3 2 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFOAi n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

• San«>leName:-k110728a055 - Sampl e ID:-OLP1CM}1-01-1»-009 ^ Rla:'V110728a.w( r I Pea k Name:-13C8PFOJM3(IS> * Mate(M} : "421.000376.00 0 Da ' I Commenl:"DALGWBPMVV12 1 RS1107i rAnnotatton: " Sampl ' Sampl e Type : Unk t Concentration : 1 0 0 Calculate dCone : H/ A Acq . Date : 7/29/201 1 Acq . Time : 4:5 9 Modified : Y Proc . Algorithm : Spe c Nois e Percentage : Base . Sub . Window : Peak-Split . Factor : Repor t Larges t

Peak : Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R T Window : 3 0 4 9 A M
, f y P a 5 0 1.0 0 2 Ye s 0.0 0 0.0 0 0 0 Expecte dRT : IS. an Int . Type : Valle y Retentio nTime : 15. 8 Area : 156242 0 c t Height : 3,01e+00 S



# I Sampl a Name:'V110728a0e9 rSampl e ID : "OLP1CM}1<01 ' PeakName:*13C8PFOA-IS<tS) ' Man{e«>:-421.00aa7e. < Commei<;-DALGWBPMW12101107i rAnnotation: ' Sampl e Index : 6 9 Sampl e Type : Unknow n Concentration : 1.0 0 ng/m L Calculate d Cone : H/ A 

# I Sampl e Name:-k110728a06 rSampl e ID:'OLP1(M]1-O1-I»00 rFle:*k110728a
. P«ikName:'13C8PFOA4S{(S) * Mate{e«):-421.00CV376.C0ODa ' Comment:-DALGWTRIP 1 LS1107 1 rAnnotaBon: - Sampl e Inde?< : 5 7 Sampl e Type : Unknow n Calculate dCone : Acq . Time : 1.0 0 I H/ A 7/29/201 1 5:42:0 1 A M Modified : H o Proc . Algorithm : Specif yPar i Nois e Percentage : S O Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Rept>r t Larges t Peah : Ye s Min . Pea k Height : 0.0 0 Mi n : Wid i 0.0 0 Smoothin g Width ; R T Window : Expecte dRT :
Height : Star t Tin « En dTime : N o Valle y le : 15. 8 183414 7 co i 3.00e'OD 5 15. 6 16. 0



# I Sampl e Name : 1i11072BaO16 ' Sampl e ID : 1 1 003-2&6 ' FUe:'k110728a.wt r Pea) ( Name : TFQA ' M«M{es) : -413.000OGS.00 0 Da.413.000m9.00 0 Da ,413.000/169.00 0 Da Cwnment : "1. 0 no/m L F C tt d I n Synth
. VMrter " Annotation:" " Sampl e Index : 1 6 Acq . Dat e Acq . Tim e Modified : Proc . Algorithm : Nois e Pe r Base . Su b Peak-Spl i Min . Pea k Min . Pea k Smoothin g R T Windo w 1 1

9 : 29/2 0 55:4 5 Ye s Specif y Window :

. Fac t rges t P Heigh t Width : Width : Expecte dRT : Us e Rela c Int . Typ e Retentio n Area : Height : v e RT :

Time : ea k

B a 1560 8 Star t Time : En dTime : 2 . 6 S O 1 A M

1.0 0 2 Ye s 0 0 0 0 . 0 IS. a H o s e T o IS. a s Oil 0 0

Ba , et00 5 c 15. 7 15. 0 Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hols e Percentag e Base . Sub . Wind c Peak-Split . Fa d Standar d 1.0 0 ng/m L 0.99 8 ng/m L 7/28/201 1 3:16:3 2 P

M Ye s Specif y Paramet e : S O * : 1.0 0 mli i o r : 2 Re!»r t Larges t

Peak : Ye s Min . Pea k

Helgh l Min . Peal ^ Width : Smoothin g width : R T Window : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : 1 6 Height : Star t Time : En dTlm-f : : 0.0 0 cp s 0.0 0 se c 0 p o 30. 0 se c 15. aBi n H o Manua l !I7 H count s 2.6Set00 5 cp s 15. 6 mi n 15. 9 mi n

Dat aprinte db y ST

W Printin g Time : 9:35:1 3 A M Printin g Date : Thursday , Augus t 25 , Pag e 3 o f 6 Pag e 3 3 o f5 2GLP10-01-01 ; Interi mRepor

t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

|l|s.r.vleName:'V110728.02 r Sampl e ID : "1 1 OOE ^ Fte:'V110728a.^ r 1 Pea k Name:'PFOA
- MaM<e«):"413.O0ara69.O00D*,413.O0anig.0OODa,413.00Qn69.000Da
- • Coirment-MettiodBbni r Annotation:' ' Sampl e Index : 2 7 Sampl e Type : Unknow n 1 4 5 4 n Concentration : H/ A Calculate dCone : 0.0035 9 ng/m L Acq . Date : 7/28/201 1 i-'" * 1 Acq . Time : 7:08:2 8 P M i l-B ^ Modified : Ye s Proc . Algorithm : Specif y Parameter s - M Q II I Nois e Percentage : 5 0 •"•** * Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor : 2 1,4e 4 Repor t Larges t

Peak : Ye s Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 fiec ^•^* * Smoothin g Hidth : 0 point s R T Window : 30. 0 se c Ue 4 Expecte dRT : 15. 8 mi n Us e Relativ e RT : N o , , ^ Int . Type : Manua l Retentio n Time : 15. 8 mi n , 1.0* 4 Area : 367B 9 count s g " Height : 5.10 e + 00 3 cp s ^ BOQO O Star t Time : 15. 7 mi n | En dTime : 15. 0 mi n « 1 8000. 0 7000. 0 6000. 0 sooa o 40oa o 3000. 0 2000. 0 1000. 0 1432 1 1I IiiiU^lilHitlilWtt

f 13. 5 14. 0 14 ? iSanvleName:-kn072a.03 r Sam;4elD:-LCS-1107264
- Rle:-k110728a.vi*f r 1 Pea k Name:-PFOA
- hla«a(e«):-413.00aO6a.00DDa,413.0Q0i^ig.00ODa,413.00(yi6d.000Da
- • Conmen t

-2pp b LCS ' Annotation: " 1 Sampl e Index : 3 1 Sampl e Type : Q C Concentration : 1,9 9 ng/m L Calculate dCone : 2.0 3 ng/m L Acq . Date : 7/:a/:01 1 Acq . Tine : 8:32:5 4 P M 5.5e 5 Moditied : H o Proc . Algorithm : Specif y Parameter s - K O II I Nois e Percentage : 5 0 5.0e 5 Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s AfinH Min . Pea k

Height : 0.0 0 cp s ^"^ ^ Min . Pea k

Width : 0.0 0 se c Smoothin g Width : 0 point s R T Window : 30. 0 se c 4,0e 5 Expecte dRT : 15. 8 mi n Us e Relativ e RT : N o Int . Type : Valle y 3-5B 5 Retentio n Tims : 15. 8 mi n - Area : 372759 8 count s g Height : 5.93e+00 5 cp s ^ ao- S Star t Time : 15. 7 mi n 1 " En dTime : 16. 0 mi n | 23e 5
2.0e 5
1.5e 5
1.0e 5
5.0e4 ' j 16.1 6



## 1 "' " 15.7 8 I L 1 

## 1 I I "•«"-"lll i I I I 17.26

^ J 1 II I • l J k '°' ^ 1 UlLl7.5 4 llf^

W 

### I i l i II I i l JliL?TJ 1 ...isa^Hi i Will i UMLuHMIbLdl l M n 14.S 9 '"-"h1 i|BU f

ililiiUMyMPIill P i i

5 1^. 0 15. 5 16. 0 16. 5 17. 0 17. 5 18. 0 Time . m(n

1 5 7 6

A • ° ° 13. 5 14. 0 14 . 1 L-" ^ 1 , 15. 0 15 3 16. 0 18. 5 17. 0 17. 5 16. 0 • Sampl e Name:'k110728a02 r Samp hID:-LCS-110726-1
- Fle:'V11072ea.vrtr r I Pea k Name:-PFOA " Ma««(ei) : "413.000069.00 0 D*.413.000/219.000Da.413.00Qf169.000Da
- • Comment : "0.2pp b LCS " Annotation : ~ Sampl e Index : 2 8 Sampl e Type : Q C Concentration : 0.19 9 ng/m L70* 4 Calculate dCone : 0.21 0 ng/m L Acq . Date : 7/28/201 1 Acq . Time : 7:29:3 2 P M g^g ^ Modified : Ye s Proc . Algorithm : Specif y Parameter s - M Q II I gn ^ Hois e Percentage : 5 0 Base . Sub . Window : 1.0 0 mlr , Peak-Split . Factor : 3 5- . Repor t Larges t

Peak : Ye s Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 se c Smoothin g Width : 0 point s °-°* * R T Window : 30. 0 se c Expecte dRT : 15. 8 mi n Us e Relativ e RT : N o *-° ^ Int . Type : Manua l Retentio n Time : 15. 8 mi n , *0 ^ Area : 41243 0 count s & Heigtit : 6.9eet00 4 cp s ^ Star t Time : 15. 7 mi n | 3.5e 4 En dTime : 16. 0 mi n « 3.0* 4 2.Se 4 2.0e 4 1.Se 4 1.0e 4 5000. 0 14.5 4



### I 1 1 i l 

## i l
13. 5 14. 0 14. 5

• Sampl e Name : •kl10728a034
- Sampl e ID : TCS-110726. r Fle:-V110728».*t r 1 Pea k Name : TFOA
- M«M(et) : "413.000069.00 0 Da,413.00CV21S.OO0Da,413JXXVie9.000Da
1 Comment ; •20pp b ICS " Annotatton: * Sampl e Index : 3 4 Sampl e Type : Q C Concentration : 19. 9 ng/m L Calculate dCone : 19. 1 ng/m L4.Be 6 Acq . Date : 7/28/201 1 Acq . Time : 9:36:1 4 P M *•" « Modified : N o *'^ ^ Proc . Algorithm : Specif y Parameter s - M Q II I 4Je 6 Hois e Percentage : 5 0 Base . Sub . Window : 1.0 0 mi n 4.0e 6 Peak-Split . Factor : 2 Rei>or C Larges t

Peak : Ye s J.ee o Min . Pea k

Height : 0.0 0 cp s -- - Min . Pea k

Width : 0.0 0 se c •*'" " Smoothin g Width : 0 point s 34e 6 R T Window : 30. 0 Se c Expecte dRT : 15. B mi n 3.2e 6 " • • "•'•" " " ' " ' 3.< « Int . Type : Valle y Retentio n Time : 15. 8 mi n , 2.8e 6 Area : 3170723 5 courit s g - 2.6e 6 Height : ).92B+0O i cp s ^ Star t Time : 15. 7 mi n % 2.4e 6 En dTime : 16. 0 mi n e 1 2.2ee 2.0e 6 1.8e 6 1.6e 6 1.4e 6 1.2. 6 1.0e 6 B.0e 5 6.0e 5 4.0« 5 2.0e 5 13. 5 14. 0 14 5 15.7 6

L15.8 I



## 1 H 16.1 2 • L L 18.1 4 

# _AX^SI..;»M> '
i f o 15. 5 16. 0 16. 5 17. 0 it s 18. 0

15.7 6



## 1

- m 15. 0 15 5 16. 0 16. 5 17i ) 17. 5 18. 0 | | I I Dat aprinte db y ST W Printing Time : 9:35:1 3 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 4 o f 6
Pag e 3 4 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

|||San^Name:1c110726a041 " Sampl e ID:"LCS-110726.10
- Fle:"lc110728a.«« r I Pea k Name : "PFOA
- M«aa<ee):"413.00(V369.000D»,413.00Cy219.000Da.413.000/169.000D» ' • Commen t

tl.2pp b LC S EC PAnnotation ; ~ Sampl e Index : 4 1 Sampl e Type : Q C Concentration : 0.19 9 ng/m L Calculate dCone : 0.20 6 ng/m L Acq . Date : 7/29/201 1 55e 4 y Acq . Time : 12:04:0 8 A M Modified : Ye s Proc . Algorithm : Specif y Parameter s - M Q II I =•* * Nois e Percentage : 5 0 Base . Sub . Window : 1-0 0 mi n Peak-Split , Factor : 2 45e 4 Repor t Larges t

Peak : Ye s Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 se c Smoothin g Hidth : 0 point s 4 0e 4 R T Window : 30. 0 se c Expecte dRT : IS. 8 mi n Us e Relativ e RT : N o 3.5e 4 Int . Type : Manua l Retentio nTime : 15. B mi n - Area : 40871 5 count s 8 Height : 5.57et00 4 cp s ^ 3-0 ^ Star t Time : 15. 5 mi n 1 En dTime : 15. 9 mi n •

~ 25e 4
3X>e 4
1 5 M
1J>e 4 5on. o 14.5 6 

## • 1 15.7 6


# 1
i5.6aj H 

### • 'V ^ mk 174

. '"" ^ ^ 1 ,|/ \'^f^r'"* , jJi i "-^liil L
13. 5 UJ O 14. 5 15. 0 15 5 16. 0 16. 5 17. 0 1^ 5 18. 0 1 Sampl e Name:ini0h8aO4 r Samp*BtD:"LCS-110726-1ff ' t*:-k110728a.»4 r • Pea k Name : "PFOA
- Mata(et):"413.00(V36d.OOODa,413.00ai'2l9AX>Da,413.00CV169.000Da " • C««nent-20pp b LC S EC FAnnotatlon:
- Sampl e Indsx : 4 7 Sampl e Type : Q C Concentration : 19. 9 ng/m L Calculate dCone : 20. 2 ng/m L4.2e 6 Acq . Date : 7/29/201 1 Acq . Time : 2:10:5 0 A M 4.0e 6 Modified : Ye s 3 8e 6 Proc . Algorithm : Specif y Parameter s - M Q II I Nois e Percentage : 5 0 3 6e 6 Base . Sub . Window : 1.0 0 mi n Peak-Split , Factor : 2 3.4e 6 Repor t Larges t

Peal: : Ye s Min . Pea k

Height : 0.0 0 cp s 3Je 6 Min . Pea k

Width : 0.0 0 se c Smoochlh g Width : 0 point s 3J>e 6 R T Window : 30. 0 se c Expecte dRT : 15. 8 mi n 2_8 ^ I's e Relativ e RT : N o 2.6e 6 Int . Type : Manua l Retentio nTime : 15. 6 mi n , 24« 6 Area : 3346741 1 count s fr Height : 4.336+00 6 cp s < . 2^ $ Star t Time : 15. 4 mi n 1 En dTime : 16. 1 mi n | j_oe 6 1.8e 6 1.6e 6 1.4e B 1.20 6 1.0e6 ' 6.0e5 ' 6.0e5 ' 4.0e5 ' 2.0e5 ' 0,0- J 15T S

15.S3 ^ 

# n • • 

# •
1 3 5 14. 0 14. 5 15. 0 15. 5 16. 0 16 5 17. 0 17. 5 la O
= T^"* ' - . ! I Pea k

Name : "PFOA * Maw(ea) : -413.OOCV369.000 Da.413^)00219.00 0 Da.413.000/169.00 0 Da " I Comment : "2pp b LC S EC PAnnolatton : - Sampl e Index : 4 1 Sampl e Type : Q C ,s „ ConcentcaCIon : 1-9 9 iig/m L5.0e 5 Calculate dCone : 1.9 9 ng/m L Acq . Date : 7/29/201 1 4.8e 5 Acq . Time : 1:07:3 2 A M ^^ ^ Modified : Ye s 44^ 5 Proc . Algorithm : Specif y Parameter s - M Q II I Nois e Percentage : S O 4.2* 5 Base . Sub . Window : 1.0 0 mtr , Peak-Split . Factor : 2 ^•"• S Repor t Larges t

Peak : Ye s 1 »«• ; Min . Pea k

Height : 0.0 0 cp s " Min . Pea k

Width : 0.0 0 se e 3.6e 5 Smoothin g Width : 0 point s R T Window : 30. 0 se c 3.4e 5 Expecte dRT : 15. 8 mi n ,.>_ « Us e Relativ e RT : N o 3.2e 5 30e 5 Int . Type : Manua l '" ^ Retentio nTime : 15. 7 mi n , 2.8e 5 Area : 355880 3 count s g Height : 5.01e»00 5 cp s » : 2,6* 5 Star t Time : IS. 4 mi n 1 En dTime : 16. 0 mi n | •''^ ^

- 2.2e 5 2.0e 5 1.6e S 1.6e 5 1.4e 5 1.2* 5 1.0* 5 8.0e 4 6.0* 4 4.0* 4 2.0* 4 15.62.. . ^ 1 

## I I 

# • A M^ . 13. 5 14. 0 14 5 1^. 0 15 5 16. 0 16. 5 Tim e mi n • Sampl e Name : 1(110728*055 " Sampl e ID : ^3LP1W)1-O1-1&O09
- Fle:-Ml0728a.v ^ I Pea k Name : "PFOA
- Ma*a(e>):"413.00Q'369M0Da.413.OO(V319.000Da,413.0O0/169.0OODa
- • Commert:-DALGWBPUW121RS1107i r Annotation:
- Sampl e Index : 5 5 Sampl e Type : Unknow n,4 ^ ConcenCiation : N/ A Calculate dCone : ' ' 0 2 0* 4 Acq . Date : 7/29/201 1 Acq . Time : 4:59:4 9 A M ,_g„4 . Modified : Ye s . g^ . Proc . Algorithm : Specif y Parameter s - M Q II I Nois e Percentage : 5 0 - ^ Base . Sub . Window : 1.0 0 mi n '•'• * Peak-Split . Factor : 2 Reixjr t Larges t

Peak : Ye s '-^ ^ Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 se c ^•^• 4 Smoothin g Midth : 0 point s R T Window : 30. 0 se c 1.4* 4 Expecte dRT : 15. B mi n Us e Relativ e RT : H o 1.3* 4 Int . Type : Manua l 1.2* 4 Retentio nTime : 15. 6 mi n , Area : 2S22 0 count s § 1.1*4
- Helght : 1.01e->00 3 cp s ^ Star t Time : 15. 7 mi n 1 , (w . En dTime : IS. 9 mi n |

—9000, 0 6000. 0
6000. 0 5000. 0 4ooa o 3000. 0 2000. 0 1000. 0 0. 0 16.1 6



# 1
n 15.7 5 fl ' S Lt I l 1 • ill , 17. 0 1:^. 5 18. 0

18.1 3 1 i l "•so , U 173 5 \m\ i6.a o . I iH I L J Uv°,^i>i'iiit^'^ iiwuir aI I 15.3 4 H J WLUl . u. mJ..,,.H M WUt

t ,,,:;: ^ '"^^ ^ l i s 14. 0 14. 5 15. 0 15 5 16. 0 16 5 U^iUinMlulM w 1 lUH^fliffi F •^TT l Ifl " 17. 0 17. 5 18. 0 Dat aprinte db y ST W Printing Time : 9:35:1 3 A M Printin g Date : Thursday , Augus t 25 , Pag e 5 o f 6 Pag e 3 5 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728a.rd b

• San^lBMamBrTtilO ^ I Pea k Name : "PFOA " Hata<*e):"413.00a'369.000Da.413.00(V219.000Da.413.000n69.000Da ' • ConwnonfDALGWTRIP I LS110713 " Annotatton:" " Sampl e Index : 5 7 Sampl e Typ e N/ A Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fac t 0.24 3 7/29/201 1 S:4Z:0 t

A M N o Specif y P a

• : 1.0 0 3r : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R T Window : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 16. 8 n N o Valle y Area : 52650 2 cou r Height : Star t Time : En dTime : .tle'-OO i c IS. 7 n 15. 9 I > ng/m L

ameter s - M

Q II I 

# r Sampl e Name:-k110728a06g ^ S«mpte|D:"GLPiaO1-O1.19O10 ^ Fle:-k110728a.vi4 r Pea k Name : TFOA " Masses):'413.000069.00 0 Da.413.000/219.00 0 D a .413.000/168.00 0 Da " Commeot:"DALGWBPMW1210110713 - - Sampl e Index : 6 9 Sampl e Type : Concentration : K/A Calculate dCone : 0.068 2 Acq . Date : 7/29/201 1 Acq . Time : 9:55:1 5 A M Modified : Ye s Proc . Algorithm : Specif y Pa r Hois e Percentage : 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

PeaK : Ye s Min . Pea k

Height : 0.0 0 Min . Pea k

Width : 0.0 0 Smoothin g Width : 0 ng/m L

ktneter s - M

O II I mi n

s e c point s R T Window : 30. 0 se c Expecte dRT : 15- B n Us e Relativ e RT : N o Int . Type : Manua l Retentio nTime : 15. 8 m In
i n Height : 2.01et00 4 cp s Star t Time : 15. 5 m i n ^ ^ 2.1* 4 2.0* 4 1.9* 4 1.8* 4 1.7* 4
1.5* 4 1.4* 4 1.3* 4 1.2* 4

Dat a printe d b yST W Printin g Time : 9:35:1 3 A M Printin g Date : Thursday , Augus t 25 , Pag e 6 o f 6 Pag e 3 6 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728 a ext.rdb k110728 a ext.rd b (PFOA) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -7.06e+00 3 x* 2 + 1.7 1 e+00 6 x+ 1.66e+00 4 ( r= 0.9994 ) 1.03e 8 1.00e 8

4 5 5 0 5 5 Concentration , ng/m L Dat a printe d b

yST W Printing Time : 9:35:5 1 AM Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1
Pag e 3 7 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728 a ext.rdb

• SanipleMame:-k110728a0i rSampl e ID:*11003-25-8 " Rto:l(11O720a.wt r I Pea k Name:'PFOA - MaM{**):-413.000r3e9.000Da.413.00(V219.0000a,413.00CV169.0000a * • Comment-1.DnaftnLF C tt d I n Synth
. Wal*r - Annotation: - Sampl e Indey : 1 6 • B TyF>e : Standar d ng/m L ng/m L Sampl e Type : Standar d Concentration : Calculate dCone : 0 . Acq . Date : l/2 i Acq . Time : 3:1 6 Modified : Y Proc . Algorithm : Spe c Kois e Percentage : Base . Sub . Window : Peak-Split . Factor : Repor t Larges t

Peak : Min . Pea k

Height : Min . Pea k

Hidth : Smoothin g Width : .0 0 96 7 /201 1 :3 2 P M e s i l y P a 5 0 1.0 0 2 0.0 0 0.0 0 0

Int . Typ e Retentio n Area : Height : Tim e Ma n 1 GS901 1 2.S5 e a l

. 7 ml 00 5 c p 15. 9 mi n 2.6a 5 3.Se 5 2.4* 5 2J3e5 2.2e 5 2.1* 5 2J>* 5 1.9* 5 1.8* 5 1.7e 5 1.6* 5 1.5* 5 1.4* 5 1.3* 5 1J* S 1.1* 5 1.0* 5 9.0* 4 8.0* 4 7.0* 4 6.0* 4 5.0 M 4.0* 4 3.0» 4 2.0 M 1.0* 4 0_ 0 14.5 5

i 

# K 1 5 7 5

B i , rNmwr ' tfi»,'<. iviii,":"-;ii , •T-rrW ^ 

# I sampl e Name : •1<1l0728a02E rSampl e ID : "LCS-110726.1 ' FUe:"k110728a.wW r Pea k Name : 'PFOA ' MaM(**) : '413.000/369.00 0 Da,413.00CV219.00 0 Da.413JXXV169.00 0 Oa " Comment-0.2pp b LCS * Annatatk>n: ~ Sampl e Index : 2 8 

# I Sampl e Name : lc11072BaO2 rSampl e ID : M l 00S«9 ' Fie : 1(110728a.wt T Pea k Nam* : TFOA * Masa(*a) : '413.OO0ir369.OD0 D a ,413.000/219.00 0 Da ,413.000/169.00 0 Da ' Comm»nt:"M*t>>o d Blank - Annotation: - Sampl e Index : 2 7 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.0060 6 ng/m L Acq . Date : 7/2B/201 1 Acq . Time : Modified : Proc . Algorith m Hois e Percentag i Base . Sub . Wind i Peak-Split . Fa d 7:0B:2 8 P M Ye s Specif y P a : 5 0 J : 1.0 0 o i : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh l Min . Pea k

Widt h Smoothin g Midt h R T Window : Us e Relativ e R

T int . Type : Retentio nTime : Area : Height : Star t Time : En dTime : 0.0 0 0 30. 0 15. 7 D N * Manua l 15. 8 2696 3 co u <.92e-00 3 15. 9 n 1.7e 4 1.6* 4 1.5e 4 1.4« 4 1.3* 4 1.2* 4 1.1* 4 1.0e4 90oa o 8000. 0 7000. 0 6000. 0 5000:0 - 4000. 0 3000. 0 2000. 0 1000. 0 143 4

14.3 2 ini
. .iiiii.iiiJUiiuyfii u 15.7 6 1 

# i
14.8 S '=-'^ , i°^|H | 

# Midi P ^iwff*!** , ..'T.'-. r.'•;';.•..
. 16.1 6 ,8.,2
. 

## Il 

# i 

# n"r£ l iu|U|||P ^ 'rrPl ' TM 

## [ Sampl e Name : "V l 10728*031 ' Sampl e ID : t.CS-110726-4 " F»e : 'V11072Sa.wl ^ Pea k Name : 'PFOA ' Mau(es) : -413.000i'369.00 0 Da,413.000/219.00 0 Da,4 1 S.OOVI69.00 0 Da Comment : '2pp b LCS ' Sampl e Type : Concentration : Calculate dCon e Acq . Time : Modified : Proc . Algorithi r O C 0.19 9 ng/m L : 0.23 2 ng/m L 7/28/201 1 7:29:3 2 P

M Ye s : Specif y Paramet e Base . Sub . Window : Peak-Split . Factor : Repor t Larges t

Peek : Smoothin g llidt h R THindow : Elxpecce d RT : L's e Relativ e R

T Retentio n Tine : Area : Height : Star t Time : 15. 8

I1Z15 9 c

< 7.00e+00 4 Sampl e Index : 3 1 Sampl e Type : O C Concentration : 1.9 9 Calculate dCone : 2.2 0 Acq . Date : 7/28/201 1 Acq . Time : 8:33:5 1 P M Modified : N o Proc . Algorithm : Specif y P a Nois e Percentage : 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Rei>or t Larges t

Peak : Ye a Min . Pea hHeight : O.O C Min . Pea k

Width : O.OC Smoothin g Width : 0 R T Window : 30. 0 Expecte dRT : 15. 7 Us e Relativ e RT : H o Inc . Type : Valle y Retentio nTime : 15. 8 Area : 372759 8 co u Height : S.93e+00 5 ng/m L ng/m L

ramet e mi n

n i s cp s

Dat aprinte db y ST

W Printing Time : 9:37:0 4 A M Printin g Date : Thursday , Augus t 25 , Pag e 1 o f 3 Pag e 3 8 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFOAi n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728 a ext.rdb 

# I Sampl e Name : ini0728a041 - Sampl a ID : TCS-110726-10 - Fie : M10728a.wtt r Pea k Name : TFOA ' Maas(e«) : "413.OOCV369.00 0 Da.413.000/219.00 0 Da,413.000/169.00 0 Da * Comment : *0.2pp b LC S ECF " Annotation ; ~ Sampl e Inde:( : 1 1 Sampl e Type : Q C Concentration : 0.19 9 ng/m L Calculate dCone : 0.23 2 ng/m L Acq . Date : 7/29/201 1 Acq . Time : 12:01:0 8 A M 

# I San«)leNam*:-V110728a034 - Sampl e ID:'LCS-110726- rFUe : •V110728a.vi4f r Pea k Name : 'PFOA ' Ma«*(*«) : '413.000/369.00 0 Da,413.000/219.00 0 Da,413.00(V169.00 0 Da ' Comnwn t '20pp b LCS " Annotation: " Concentr a ion : Calculate dCone : Acq . Dat e Acq . Ti M Modified : Proc . Al g Nois e Pe r Base . Su b Peak-Spl I rithm :

entag e Wlndo i

. Fact o 19. 9

20. 3 7/28/2 0 9:36:1 1 H o Specif y 1

P M P a : 1.0 0 c : 2 Repor t Larges t

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

Hidth : Hidth : Expecte dRT : Us e Rela t Int . Typ e Retentio n Area : Height : v e RT :

Time : 0

0 0 30. 0 15. 7 H o Valle y 15. 8 3170723 5 Star t Time : En dTime : .92etO O 15. 7 15. 0 0 0 01 ) ng/m L

cameter s - M

Q mi n
? e c point s mi n

c p s nl n

15. 0 15. 5 16. 0 1& 5 17. 0 

# I SanvlaName:'VI10728aO4 rSampl a ID:'LCS-1l072S>i rFle:-kll0728a.wt r Pea k Nam* ; 'PFOA ' Mac*(es) : '413.000/369.00 0 Oa,413.00(V219.00 0 Da,413JX)IV169.00 D Da " Commen t '2pp b LC S EC P AnnotaOon : ~ 5.5* 4 Modified : Proc . Algorith m Hols e Percenta g y e s Specif y P a : 5 0 Base . Sub . Hindow : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s Kin . Pea k

Heig h Min . Pea k

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

T Int . Type : Retentio nTime : Area : : 0.0 0 0.0 0 0 30. 0 15. 7 D H o Manua l 15. B D 1250 1 co u

13. 5 14. 0 

# I Sampl*Name:•k110728a04 rSamplelD:-LCS-110726-16 " Fl* ; 1(110728a.wi r Pea k Name : TFOA " Mass(e«) : '413.00CV369.00 0 Da.413.000/219.00 0 Da,413.000/169.00 0 Da ' Commant : "ZCfip b LC S EC P Annotatnn : ~ Sampl e Sampl e Index : Sampl e Type : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hols e Percentag e H Q C 1.9 9 2.0 9 7/29/201 1 1:07:3 2 A

M Ve s Specif y Pa r 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Fac t Repor t Larges t

P Min . Pe= k

Heigh t Min . Pea k

Width : Smoothin g Width : R T Hindow : Expecte dRT : l's e Relativ e RT : Int . Type : Retentio nTime : r : 2 a k : Ye s 0.0 0 0.0 0 30. 0 s 15. 7 m N o Manua l 15. 7 n Area : 355653 8 cou n Height : Star t Time : En dTime : .01e*00 5 e 15. 4 n 15. 9 m ig/m L

ig/m L

mi n

s e e

. n

. n p s

. n i n irrpl e Type ; Concentration : Calculate dCon e Acq . Date : Acq . Time : Mod i lied : Proc . Algorith m Hois e Percentag e Base . Sub . Hlnd c Peak-Split
- Fac i 19. 9 7/29/201 1 3:10:5 0 A

M Ye s Specif y P a : S O w : t.O O o r : 2 Re|>or t Larges t

Peak : Ye s Min . Pea k

Helgh i Min . Pea k

Widt h Smoothin g Widt h R T Window : Expecte dRT : irs e Relativ e R

T Int . Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 ng/m L

ng/m L

amet e

c p s
e e 15. 7 mi n H o Manua l 15. 6 mi n 4.2* 6 4.0* 6 3.8* 6 3.6*6
- 3.4*6
- 3.2* 6 3.0*6
- 2.6*6
- 2.6* 6 2.4*6
- 2.2* 6 2.0* 6 1.6* 6 1.6*6
- 1.4*6
- 1.2*6
- 1.0*6
- 8.0*5
- ao* 5 4.0*5 - 2.0*5 - 0.0 - 17. 0 17. 5 Dat aprinte db y ST

W Printin g Time : 9:37:0 4 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 2 o f 3 Pag e 3 9 o f5 2GLP10-01-01 ; Interi mRepor

t 1 9 Analysi s o f PFO AI n Wate rSample s Off-Sit e B P Property- Jul y201 1 Result s Name : kll0728 a ext.rdb

• SarnJl e Name : T d 10728*061 ' Sampl e ID : "OLP1(«1-01-1W)06 " Fll*;Tc110728a.yi« r • P*akNBnM:-PFOA ' Ma%«<e*):'413.000/369.00 0 Oa,413.000/219.000Da,413.00Q/169.000Da - • Comm«nt-DALGWBPMW4701107i rAnnotatten; - Sampl e Inde*-. : 6 1 Sampl e Type : Uriknow n 0-31 7 7/29/201 1 7:06;3 5 A

M ng/m L
Algorithm : Specif y Para i Sub . Windo w p u t Peak
- Repor t Larg i Min . Pea k

Height : Min . Pea k

Width : • thin g Width : R T Min i Us e Rela '

Dat a printe d b

yST W Printing Time : 9:37:0 4 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 3 o f 3
Pag e 4 0 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


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

Pag e 4 1 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


# 3 M Environmenta l Laborator y

Metho d Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate r

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q U I n fc>~ )
Approve d By : 

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

ETS-8-044. 0 Pag e 1 o f1 1 Metho d of Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 2 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


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

yrequire preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Detemninatio 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 not covere d unde rthi s analytica l procedure
. 2 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS
. Sample s containin g heav y particulat e ma

ynot b e suitabl e fo ranalysi s b ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thi s i s a performance-base d method
. Metho d accurac yi s 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 detennine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l not 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 at 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 o fth e Wori<in g Standar d (WS ) int o a predetermine d amoun t o f AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method
. Calibratio n standard s are use d t o calibrat e th e instmmen t respons e wit h respec t t o analyt e concentration
. 

### 3. 2 Laborator yDuplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

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

t wit h sampl e collection , preservation , o rstorag e procedures
. 3. 3 Fiel d Blan k

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d a s a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures
. Th e purpos e ofth e F B i s t o determin e i ftest substance s o r othe rinterference s are presen t i n th e fiel d environment
. Thi s sampl e i s als o referre d t o a s a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 3 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 

### 3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e at th e sam e tim e fro m th e sam e locatio n 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 of th 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 ofaqueou s samples
. Aknown , specifi cvolum e o f sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

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

yb e prepare d t o increas e th e likelihoo d that a spike a

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

ycomplicat e th e interpretatio n o fth e sampl e analysis
. 

### 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot of AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s 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 ylike a stud ysampl e t o hel p detennin e i f th e metho d i s i n contro l an d whethe ra los s of analyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are no t know n o rma

yvary . At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d place a s eac h FMS
. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot of contro l matri xt o whic h know n quantitie s o fth e targe t analyte s are adde d i n th e laborator ya t th e tim e of sampl e extraction
. At least tw o level s are included , on e generall yat th e lowen d ofth 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 yMatri xSpik e (LMS ) Alaborator

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

ysampl e t o determin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results
. Th e endogenou s concentration s ofth 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'ecte d fo rthes e concentrations
. LMS s are optiona l fo ranalysi s ofaqueou s samples
. 

### 3. 9 Laborator ySampl e Aportio n o raliquot o f a sampl e receive d fro m th e fiel d fo rtesting
. 3.1 0 Limi t o f Quantitatio n (LOQ ) Th e lowe rlimi t of quantitatio n (LLOQ ) fo ra dataset i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits ofprecisio 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 ofprecisio n an d accurac ydurin g routin e operatin g conditions
. Th e highest standar

d i n th e calibratio n curve that meets metho d criteri a i s define d a s th e ULOQ
. ETS-8-044. 0 Pag e 3 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 4 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 

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

### 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yofmateria l intende d t o represen t th e origina l source material
. 

### 3.1 3 Stoc k

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

### 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s not 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 , sun'ogate(s ) are adde d t o al l sample s an d qualit y contro l samples
. Sun'ogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedure includin g sampl e collection , preparation , an d analysis
. Inclusio n 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 o f severa l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o prepar e calibratio n standard s an d othe rrequire d analyt e solutions
. 

### 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yof th e standard s fo rthi s metho d have not bee n precisel ydetennined ; however , eac h shoul d b e treate d a s a potentia l healt h hazard
. Th e analyst shoul d wea rgloves , a la b coat , an d safet

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

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a cun^en t awarenes s ofloca l regulation s regardin g th e handlin g of th e chemical s use d i n thi s method
. Areference fil e ofmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t not limite d to , th e us e o f solvents , 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 intert'erence s unde r condition s of analysi s b

ynjnnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 5 o f5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 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 yo f 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 of disposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 

### 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e ofpumpin g u p t o tw o solvents an d equippe d wit h a variabl e volum e injecto rcapabl e of injectin g 5-10 0 ^l L connecte d t o a tande m Mass Spectromete r (LC/MS/MS)
. I Analytica l balance capabl e o f readin g t o 0.000 1 g Adevic e t o collec

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25ijL , SOpL, lOOpL , 250|JL , 500|JL , 1000|JL
. 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e of spinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 

### 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 |j m Analytica l Column : Betasi l CI8,4. 6 m m x10 0 mm , 5 |jn n Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

Are a - quadrati ccurve fit , 1/ xweighted
. Ru n Time : ~ 1 7 minutes
. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met . ETS-8-044. 0 Pag e 5 o f1 1 Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 6 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 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 PFB A PFPe A PFH A PFHp A PFOA PFN A PFD A PFUn A PFDo A PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 31 3 ^26 9 an d 31 3 ^11 9 36 3 - ^ 319 , 36 3 - ^

16 9 an d 36 3 -^11 9 41 3 ^ 369 , 41 3 ^ . 21 9 an d 41 3 - ^ 16 9 46 3 - ^ 419 , 46 3 - ^

16 9 an d 46 3 ^21 9 51 3 - » 469 , 51 3 ^

21 9 an d 51 3 ^

26 9 56 3 - » 519 , 56 3 ^

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

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

9 9 39 9 - * 8 0 an d 39 9 - > 9 9 49 9 ^ 80 , 49 9 ^

9 9 an d 49 9 - > 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n o f isomers tha t mor e closel ymatche s NM R dat a an d mayhav e th e adde d benefi t o f increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a ar e me t t o assur e adequat e specificity
. Th e previou s infomnatio n i s intende d a s a guide , alternat e instalment s an d equipmen t ma yb e used
. 7 Reagent s an d Standard s 7. 1 Chemical s Wate r- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e - A.C.S
. Reagen t Grad e 

### 7. 2 Standard s Perfiuorobutanoi 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 Perfiuorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M PerfluorononanoicAci d (PFNA-C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA-C1 0 acid) ; Oakwoo d Products , In c PerfluoroundecanoicAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c PerfluorododecanoicAci d (PFDoA-C1 2 acid) ; Oakwoo d Products , In c Perfiuorobutanesulfonat e (PFB S - C 4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfiuorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 7 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1
Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s mayb e used
. 

### 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—^Weig h 0. 3 g 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 o fth 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 o f a particula rstudy
. Fo rexample , |J Lvolume s ma yb e spike d int o volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels
. 10 0 (jg/m L targe t analyt e SSSs—^Weig h ou t 1 0 m g o fanalytica l standar d (correcte d fo rpercen t sal t an d purit yan 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
. Prepare a separat e solutio n fo reac h analyte
. Expiratio n date s an d storag e condition s of stoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. A n exampl e o f purit yan d sal t connectio n i s give n belowfo rPFOS
.

, . X - r1 molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t o fsal t 49 9 PFO S (K^ ^ )sal t correctio n facto r= -^ ^ = 0.927 5 53 8 1 0 m g C8F17SO3K

* wit h purit

y90 % = 8.35m g CsFiySOs"(1 0 mg*0.90*0.9275=8.3 5 mg ) 5 Mg/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 10m L volumetri c flas k an d brin g u p t o volum e wit h solvent
. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L ofth e 5 [jg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflas k

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m L mixe d standard—Ad d 625|J Lofth e 5 |jg/mL-mixe d worthin 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 procedure o ri n a refrigerato ra t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 8 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1


### 7. 5 Calibratio n Standard s Usin g th e wori<in g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e a s a guideline
. Note : Volume s ofwate 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
. Concentratio n o f WS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o f WS,M L

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

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

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

Calibratio n Standard , ng/m L (ppb ) i n AST M Typ e 1 Water , o rothe rsuitabl e wate r 0.02 5 0.037 5 0.05 0 0.07 5 0.10 0 0.25 0 0.50 0 1.00 2.5 0 5.0 0 10. 0 8 Sampl e Handlin g 8. 1 Wate rSampl e Preparatio n Thi s metho d i s applicabl e t o clea n wate rsamples
. Sample s containin g heav yparticulat e ma

ynot b e suitabl e fo r analysi s b

ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thoroughl ymi xsampl e before removin g a n aliquot an d placin g i n a labele d plasti cautovial
. Plasti ci s prefen-ed ove rth e us e o f glas s autovials , t o preven t th e possibl yo ffluorochemica l stickin g t o th e glass
. Dilut e sample , i f necessary , 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 int o labele d plasti cautovials
. Prepare at 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 se t 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 ^ + bx+ c) , weighte d 1/

xo runweighted , usin g suitabl e software
. Th e calibratio n curve s ma yinclud e bu t shoul d not b e force d throug h zero . Th e mathematica l metho d use d t o calculat e th e calibratio n curve shoul d b e applie d consistentl ythroughou t a study
. An ychang e shoul d b e thoroughl ydocumente d i n th e ra wdata
. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfi t ove rth e rang e appropriat e t o th e dat a o rbecaus e the ydi d no t meet th e pre-detemnine d acceptance criteria
. Low-leve l curv e points shoul d als o b e exclude d i f thei rare a counts are no t a t least twic e that o fth e metho d and/o rsolven t blanks
. Th e coefficien t of determinatio 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 % o fth e theoretica l concentratio n wit h th e exceptio n o fth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 9 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o fPFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 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 f th e calibratio n curve doe s not meet acceptance criteria , perfom n routin e maintenance o rprepare a newstandar d curve (i f necessary) 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 ofth e sam e standard s use d t o constmc t th e calibratio n curve , at 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 CC V wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that are quantitate d above th e concentratio n ofth e highest standar d i n th e curve shoul d b e furthe rdilute d an d reanalyzed
. 

### 1 0 Qualit yContro l 10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targeted LOQ of 0.02 5 ng/mL
. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e fina l report . 

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

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

s ma yb e injecte d multipl e times , bu t n o mor e tha n 3 injection s shoul d b e remove d fro m a singl e metho d blank
. At a minimum , metho d blank s are analyze d prio rt o instmmen t calibration , prio rt o th e analysi s of CCV samples , an d a

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

d deviatio n o f th e are a count s ofthes e metho d blank s shoul d b e calculate d an d reported
. I f th e mea n are a count s o f th e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ must b e raise d t o th e firs t standar

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

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field
. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l not b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s fiel d blanks
. 

### 10. 4 Surrogat e Spike s Surrogat 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 at a minimu m oftwo 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 at concentration s i n th e rang e o ffiv e t o te n time s highe rtha n th e targete d LOQ an d hig h la b contro l spike s shoul d b e prepare d at concentration s nea rth e mid-poin t o f th e curve . Th e relative standar

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

ETS-8-044. 0 Pag e 9 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 0 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1 

### 10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s o f fiel d matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d as suc h (wit h expande d accurac ystatements) , o rwil l not b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targeted fortificatio n level s shoul d b e a t least 50 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o determin e th e statemen t ofaccurac yfo ranalytica l results
. Th e averag e of th e sampl e an d th e fiel d duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t o fanalyt e foun d (i n ng/mL , base d o n pea k area ) usin g th e standar d curve (linea rregressio n parameters ) generate d b ya n appropriat e software program : Analyt e foun d (ng/mL ) = (Pea k Are a - Intercept ) ^

^ ^ Slop e D F = facto rb

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

_Tota l analyt e foun d (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) Analyt e adde d (ng/mL ) 1 2 Metho d Performanc e An ymetho d performance parameter s that are no

t achieve d must b e considere d i n th e evaluatio n o fth e data
. Nonconfomnanc

e t o an yspecifie d parameter s must b e describe d an d discusse d i fth e Technica l Manage r(non GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data
. I f criteri a liste d i n thi s metho d perfomnanc 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 a s appropriate
. Documen t al l action s i n th e ra wdata
. I f dat a are t o b e reporte d whe n perfomnanc e criteri a have 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 f th e report . 

### 12. 1 Syste m Suitabilit y 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 o f thre e syste m suitabilit ysample s are injecte d a

t th e beginnin g ofeac h analytica l ru n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l o fth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial
. Th e syste m suitabilit yinjection s must have are a count s wit h a n RS D o f <5 % an d a retentio n tim e RS D o f<2 % t o b e compliant
. 

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

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

yCCVs no

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

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o f Analysi s fo rth e Detemninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 1 o f 5 2GLP10-01-01 ; Interi m Repor t 1 9 Analysi s o f PFO Ai n Wate rSample s Off-Sit e B P Property- Jul y201 1
Demonstratio n o f Specificity : Specificit yi s demonstrate d b

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

### 12. 3 Sensitivit y Th e targeted limi t of quantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n of appropriat e blank s an d th e accurac

yofth e low-leve l calibratio n curve points
. Refe r t o Sectio n 1 0 fo radditiona l details
. 

### 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s are designe d t o generat e dat a that are accurat e t o +/-30%
. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d accurac yof laborator

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

ymatri xspikes
. 

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

### 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfomnin g thi s metho d wil l b e dispose d ofappropriately
. Th e origina l sample s wil l b e archive d at th e 3 M Environmenta l Laborator yi n accordance wit h intema l procedures
. 1 4 Record s Eac h dat a packag e generate d fo ra stud ymust includ e al l supportin g infomnatio n fo rreconstructio n ofth e data
. Infomnatio n fo rth e dat a packag e must include , bu t i s not limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

ypages) , instmmen 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 f Change s

ETS-8-044. 0 Pag e 1 1 o f 1 1 Metho d o f Analysi s fo rth e Determinatio n o f Perfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 2 o f 5 2