GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### GLP10-01-02 : Interi m Repor t 1 9 - Analysi s o fPFBS
. PFHS
. an d PFO S i n Groundwate r Sample s Collecte d a t th e Off-Sit e B P Propert yi n Decatur
. A Li n Jul y201 1 Stud yTitl e Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m 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 St
. Paul , M N 55144 Project Identificatio n GLP10-01-02-1 9 Tota l Numbe ro fPage s

7 0

^•^ 1 ^^ ^

Th e testin g reported herei n mee t th e requirement s o fISO/IE C 17025-200 5 "Genera l Requirement s fo rth e '^^ 1 ^^1^.-
. Competenc e o fTestin g an d Calibratio n Laboratories", i n accordanc e wit h th e A2L ACertificat e #2052.01
. lACCREpiTEP j Testin g tha t 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

Pag e 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



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

Pag e 2 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



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

t 1 9 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a

t th e Off-Site B P Propert

yi n Decatur , A Li n Jul y201 1 Study : Analysi s o fPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Act (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

•Thes e are environmenta l sample s where there i s n o specifi ctest substance , n o specifi ctest syste m an d n o dosin g ofa test system . •Th e reference substance s have 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
.
\ Gar yHoHenstein/Sponso rRepresentative Date

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

Pag e 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## QUALITYASSURANC E STATEMEN T Repor t Title : Interi m Repor

t 1 9 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a

t th e Off-Site B P Propert

yi n Decatur , A Li n Jul y201 1 Study : Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s audite d b yth e 3 M Environmenta l Laborator yQualit yAssurance Uni t (QAU) , as indicate d i n th e followin g table
. Th e finding s were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector
.
Inspectio n Date s 8/12/11,8/15/1 1

L^^viX^. ^ Phas e

Dat a / 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



# . //.r^^C y^^XS' k QA U RepresentdKiv

e Date

Pag e 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



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

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

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

s 1 4 8. 6 La b Contro l Spike s (LCSs ) 1 4 8. 7 Analytica l Metho d Uncertaint y1 7 8. 9 Fiel d Matri xSpike s (FMS ) 1 7

Pag e 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### 9 Data Summar

yan d Discussio n 1 7 1 0 Conclusio n 2 0 1 1 Data/Sampl e Retentio n 2 0 1 2 Attachments 2 0 1 3 Signature s 2 1 

## LIS TO F TABLE S Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Results (B P Groundwater , Jul y2011 ) 9 Tabl e 2
. Sampl e Descriptio n Ke yCod e 1 1 Tabl e 3
. Instmmen t Parameter s 1 2 Tabl e 4
. Liqui d Chromatograph yCondition s 1 2 Tabl e 5
. Mas s Transition s 1 3 Tabl e 6
. Limi t o

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

yContro l Spik

e Recover

y1 5 Tabl e 7 continued
. Laborator yContro l Spik

e Recover

y1 6 Tabl e 8
. Analytica l Uncertaint y1 7 Tabl e 9
. Fiel d Matri xSpik e Level s 1 7 Tabl e 10
. DALGWBPMW4 7 11071 3 1 8 Tabl e 11
. DALGWBPMW12 1 11071 3 1 8 Tabl e 12
. Tri p Blan k

1 9 Tabl e 13
. Rinseat e Blan k 1 9

Pag e 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## \ 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 , (clange(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 StudyInitiation : Marc h 8,201 0 Interi m 1 9 Experimenta l Termination : August 3 , 201 0 Interi m Repor

t Completion : Date ofInteri m Repor t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d a t 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 f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## \ 2 Summary 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-Site B P Propert

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

yfo rperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e groundwate rsample s fro m eac h samplin g location
. Sample s als o include d tw o fiel d matri xspike (FMS ) sample s fo reac h location , on e tri p blan k set containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d on e equipmen t rinseate blank
. Th e equipmen t rinseate blan k di d no t have a FM S sampl e prepare d fo rdeterminatio n ofPFBS , PFHS , an d PFO S recovery . Th e groundwate rsamples , tri p blank s an d equipmen t rinseate blan k associate d wit h GLP10-01-02-1 9 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 rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP-10-01-02-19
. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s are summarize d i n Tabl e 1
. Th e equipmen t rinseate an d th e tri p blan k sampl e were belowth e lowe rlimi t o fquantitatio n (LLOQ) , indicatin g adequat e contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections
. Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S + 10% , PFH S + 11 % an d PFO S + 29%
.

Pag e 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Propert

y- Jul y201 1



### Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Result s (B P Groundwater , Jul y2011)
. Samplin g Locatio n DA LGWBPMW4 7 11071 3 DALGWBPMW12 1 11071 3 Tri p Blank s (Milli-Q TM Water ) GLP10-01-02-1 9 Equipmen t rinseat e blank : DALGWBPMW12 1 PFB S Avg
. Cone
. (ng/mL ) ±RP D 0.18 8 ±2.7 % <0.025 0 <0.025 0 <0.025 0 PFH S

Avg
. Cone
. (ng/mL ) ±RP D 0.13 8 ±2.2 % <0.025 0 <0.025 0 <0.025 0 PFOS

Avg
. Cone
. (ng/mL ) ±RP D 0.21 0 ±3.8 % <0.040 0 <0,040 0 <0.040 0 Th e analytica l method uncertaintie s associate d wit h th e reported result s are : PFBS ±10% , PFH S ±1 1 % , an d PFOS ±29%
.

Thi s analytica l stud ywa s conducte d a s par t o fth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama
. Th e objectiv e o fth e overal l progra m i s t o gai n informatio n regardin g concentration s o fperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediment s tha t ar e associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groundwate rsample s collecte d fro m tw o well s locate d a t th e off-sit e B P propert y i n Decatur , A Lfo rPFBS , PFHS , an d PFO S i n a n effort t o characteriz e regiona l groundwate rconditions
. Th e 3 M Environmenta l Laboratoryprepare d sampl e container s (25 0 m Lhigh-densit ypolyethylen e bottles ) whic h wer e shippe d t o Decatur , A LWesto n personne l prio rt o fiel d sampling
. Sampl e container s fo reac h samplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d tw o fiel d matri xspik e samples
. Eac h empt ycontaine rwa s marke d wit h a "fil l t o here " lin e t o produc e a fina l sampl e volum e o f20 0 mL
. Container s designate d fo rfiel d matri xsample s wer e fortifie d wit h a n appropriat e matri xspik e solutio n containin g PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o bein g sen t t o th e fiel d fo rsampl e collection
. Al l sampl e bottle s include d th e additio n o f^^02-PFBS , ^^Ca-PFHS , an d ^^Ca-PFO S (interna l standard ) at a nomina l concentratio n o f1 ng/mL
. Se e sectio n 8. 8 o fth e report fo rfiel d matri xspik e levels
. Sample s wer e prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laboratorymetho d ETS-8-044. 0 "Determinatio n o fPerfluorinate d Compound s I n Wate rb yHig h Performanc e Liqui d Chromatography/Mas s SpectrometryDirect injectio n Analysis"
. Th e us e o finterna l standard s wa s use d t o ai d i n th e dat a qualityobjectives
. Tabl e 1 summarize s th e averag e PFBS , PFHS , an d PFO S concentration s fo rth e duplicat e sample s collected , th e tri p blank , an d aqueou s equipmen t rinseate blank
. Table s 10-1 3 summariz e th e individua l sampl e result s an d th e associate d fiel d matri xspik e recoveries
. Al l result s fo rth e quality contro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discussed elsewher e i n thi s report fX^ ^ 

## A'MTest&JDontmlSubstance M Ther e wa s no t a tes t substanc e o rcontro l substance s i n th e classi csens e o fa GL P study
. Thi s stud y wa s purel yanalytica l i n nature .
Pag e 9 of70GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## 5 Referenc e Substance s

Referenc e Substanc e 

### Chemica l Nam e Chemica l Fomriul a Identifie r Us e Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFH S (linear ) 

### Perfluorohexan e sulfonat e C6F13SO3" Sodiu m Sal t Target Analyt e Reference Standar d Wellingto n 04/02/201 3 Froze n LPFHXSAM08 TCR08-001 8 Crystallin e 98 % t'CJPFH S (linear ) 

### Sodiu m Perfluorohexanesulfonate '"Cs^'CsFiaSOaNa " CAS#MPFC-C-051 1 Intema l Standar

d Wellingto n 05/25/201 4 Froze n 09231 0 TCR11-001 6 Liqui d 5Mg/mL<^

'
Referenc e Substanc e 

### Chemica l Nam e Chemica l Fonmul a Identifie r Use Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO S (linear ) 

### Perfluorooctan e sulfonate CeFiySO a Potassiu m Sal t CAS #2795-39- 3 Target Analyt e Reference Standar d Wellingto n 10/18/201 3 Froze n LPFOSKBM0 6 TCR08-000 1 Crystallin e 98 % PFO S (linea r+ branclied ) 

### Perfluorooctan e sulfonate C8F17SO3" Potassiu m Sal t CAS #2795-39- 3 LC S Reference Standar

d 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 Whit e Powde r 86.4 % r'C J PFO S (linear ) 

### Sodiu m Perfluorooctanesulfbnate "CsFiySOa-Na * CAS#MPFC-C-051 1 Intema l Standar

d Wellingto n 05/25/201 4 Froze n 09231 0 TCR11-001 6 Liqui d 5|jg/mL<^ ' (1 ) Custo m mixtur

e o fseve n mass-latiele d (^^0 ) periluoroallcylcarboxyll cadds , tw o mass labele d ("C ) perfluoroalkylsulfonate s an d on e mass-labele d ("C ) perfluoro-1-octanesulfonamlde
.

Pag e 1 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1

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 TC R Numbe r Physica l Descriptio n Purit y PFB S (predominantl ylinear ) Perfiuorobutan e sulfonat e C4F9SO3 " Potassiu m Sal t Targe t Analyt e Referenc e Standar d 3 M 01/10/201 7 Froze n 41-2600-8442- 5 TCR-12 1 Whit e Powde r 96.7 % [1802 ] PFB S (linear ) f^OJ-Ammoniu m Perfluorobutanesulfbnat e C4F9S[^^02]0-NH4 '

N A Intema l Standait l RT I Intemationa l 03/09/201 5 Froze n 11546-107- 2 TCR-1009 , TCR-103 1 Liqui d >99 %


### 6 Tes t Syste m Th e test system s fo rthi s stud yare groundwate rsample s collecte d fro m well s locate d i n Decatur , A Lby Westo n Solutions , Inc
. personnel
. Sample s fo rthi s studyare "rea l worid " samples , no t dose d wit h a specifi clot oftest substance
. Tabl e 2
. Sampl e Descriptio n Ke yCode
. strin g Numbe r Exampl e 1 2 3 4 5 Strin g Descripto r Exampl e DA LGWBPMW47011071 3 Samplin g Locatio n Wel l I D Samplin g Poin t Samplin g Dat e Sampl e Typ e DA L= Decatur , Alabam a GW = Groundwate r Example : BPMM/47 110713-Jul y13,201 1 0=primarysampl e DB=duplicat e sampl e L S = lo wspik e M S = midspil( e H S = higlispil( e 

## 7 Metho d Summary 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 "Detemninatio n ofPerfluorinate d Compound s I n Wate rbyHig h Perfomnanc e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
.

Pag e 1 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m LNalgene TM (high-densit ypolyethylene ) bottle s prepare d at th e 3 M Environmenta l Laboratory
. Sampl e bottle s associate d wit h GLP10-01-02-1 9 were retume d t o th e laborator ya t ambien t condition s o n Jul y18 , 2011
. Sample s were store d refrigerate d a t th e laborator

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

an d Tri p Blan k

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

## 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Durin g th e preparatio n ofth 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 of1 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 Lprio rt o bein g sen t t o th e fiel d fo rsampl e collectio n 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h perfomnanc

e 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

wdata har

d copie s place d i n th e fina l data packet , an d are briefl ydescribe d below
. Tabl e 3
. Instrumen t Parameters
. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat a 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 Polarity Softwar e ETSKirl ( ETS-8-044. 0 7/29/11-PFB S an d PFH S Agilen t 120 0 Betasi l 01 8 (4. 6 m m X100 mm) , 5 n Betasi l 01 8 (4. 6 m m X100 mm) , 5 n

2 5 n L Applie d Biosystem s AP I 550 0 Turtx) Spra

y Turtx) Io n electrod e Negativ e Analyst 1.5. 2 EJSK\t k ETS-8-044. 0 8/2/11-PFO S Agilen t 120 0 Betasi l 01 8 (4. 6 m m X100 mm) , 5 n Betasi l 01 8 (4. 6 m m X100 mm) , 5 n

2 5 n L Applie d Biosystem s AP I 550 0 Turtx) Spra

y Turtx j Io n electrod e Negativ e Analyst 1.5. 2 

### Tabl e 4
. Liqui d Chromatograph yConditions
. Ste p Numbe r Tota l Tim e

(min ) Flo wRat e

(ftUmin ) Percen t A

( 2 m M ammoniu m acetate ) Percent S (Metl)ano O ETS-8-044. 0 Analyze d 7/29/1 1 an d 8/2/1 1 0 1 2 3 4 5 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

Pag e 1 2 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### Tabl e 5
. Mas s Transitions
.

Analyt e PFB S PFH S PFO S Mas s Transitio n

Q1/Q 3 299/8 0 299/9 9 399/8 0 399/9 9 499/8 0 499/9 9 499/13 0 Referenc e

Materia l structur e Linea r Unea r Linea r Intema l Standar d

[" O J PFB S t^CJPFH S ["C^PFO S Mas s Transitio n Q1/Q 3 303 m 402/8 0 507/8 0 Dwel l tim e wa s 3 0 mse cfo reac h transition
. Th e individua l transition s were summe d t o produce a "tota l

io n chromatogram " (TIC) , whic h wa s use d fo rquantitation
. 

## \ 8 Analytica l Result s B ACalibratio n Sample s were analyze d usin g a stabl e isotop e interna l standar d calibratio n curve . Calibratio n standard s were prepare d b

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

ycontro l sample s a

t a nomina l concentratio n of1 ng/mL
. Acalibratio n curve rangin g fro m approximatel y0.02 5 ng/m Lt o 10 0 ng/m Lwa s prepared
. Sampl e DA LG WBPMW47 wa s quantitate d usin g extema l calibratio n du e t o inconsisten t intema l standar d are a counts . 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

yofeac 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 f100±25 % (100±30 % fo rth e lowes t curve point) were met fo ral l analytes
. Th e correlatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFBS , PFHS , an d PFOS
. 8. 2 Syste m Suitabilit y Acalibratio n standar

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

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

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

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

Pag e 1 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### Tabl e 6
. Limi t o fQuantitatio n (LOQ)
. Samplin g locatio n DA LGWBPMW4 7 11071 3 DALGWBPMW12 1 11071 3 PFB S LOQ , ng/m L 0.025 0 0.025 0 PFH S

LOQ , ng/m L 0.025 0 0.025 0 PFO S

LOQ , ng/m L 0.10 0 0.040 0 

### 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs) were analyze d t o confir m that th e instmmen 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 o f100 % ±25 % fo rPFBS , PFHS , an d PFOS
. 

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

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

e t o detennin e th e LOQ fo rPFBS , PFHS , an d PFOS
. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience
. Equipmen t rinseate blank s are aqueou s sample s that reflec t th e efficienc

yofequipmen t cleanin g i n th e fiel d betwee n differen t sampl e collection s an d are proofo fn o cros s contaminatio n ofsample s fro m th e equipment
. 

## 8. 6 La b Contro l Spil<e s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set . LCS s were prepare d byspikin g know n amounts o fth e analyt e into Mill i Q wate ro r syntheti cgroundwate rt o produce th e desire d concentration
. Th e spike d wate rsample s were the n prepare d an d analyze d i n th e sam e manne ras th e samples
. Th e metho d acceptance criteria , averag e o fLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <20%
. 7/29/1 1 Analysi s - interna l standar d calibration : Al l LCS s met acceptance criteri a fo rPFB S an d PFHS
. 7/29/1 1 Analysi s - externa l standar d calibration : Al l LCS s met acceptance criteri a fo rPFB S an d PFHS
. 8/2/1 1 Analysi s - intema l standar d calibration : Al l LCS s me t acceptance criteri a fo rPFOS
. 8/2/1 1 Analysi s - extema l standar d calibration : Th e lo

wset ofLC S sample s fo rPFO S had a n averag e recover yof122%
. Th e mi d an d hig h sets o fLC S sample s met acceptance criteri a fo rPFOS
. A s th e reference materia l use d fo rquantitatio n o fPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s are comprise d ofbot h linea ran d branche d isomers , additiona l LC S sample s o f PFO S (linea ran d branched ) were prepare d a t thre e concentration s i n triplicat e t o evaluat e th e potentia l fo ranalytica l bias
. 8/2/1 1 Analysi s - intema l standar d calibration : Th e low , mid , an d hig h linea ran d branche d LCS s had averag e recoverie s of129% , 122% , an d 122%
. 8/2/1 1 Analysi s - extema l standar d calibration : Th e lo

wlinea ran d branche d LC S set had a n averag e recover yof126%
. Th e mi d an d hig h sets ofLC S sample s met acceptance criteri a fo rPFOS
. Th e followin g calculation s were use d t o generat e data i n Tabl e 7 fo rlaborator ycontro l spikes
.

Pag e 1 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1

LC S Percen t Recover

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

y 

### Tabl e 7
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Intemal standar

d calibration Analyze d 7/29/1 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 PFB S

Calculate d Concentratio n (ng/mL ) 0.21 5 0.21 2 0.22 4 VoRecover

y 10 8 10 7 11 3 109±2.9 % 1.99 1.99 1.99 2.1 4

2.0 2 2.1 3 10 7

10 1 10 7 105 % ±3.3 % 19. 9 19. 9 19. 9 21. 2

21. 6 21. 6 10 6

10 8 10 8 107 % ±1.1 % Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 PFH S

Calculate d Concentratio n (ng/mL ) 0.21 7 0.21 6 0.22 4 VoRecover y 10 9 10 8 11 2 110 % ±1.9 % 1.99 1.99 1.99 2.2 0

2.1 1 2.1 9 11 1

10 6 11 0 109 % ±2.4 % 19. 9 19. 9 19. 9 21. 3

21. 9 21. 8 10 7

11 0 11 0 109 % ±1.6 % ETS-8-044. 0 Extema l standar d calibration Analyze d 7/29/1 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 PFB S

Spike d Concerttratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 Calculate d

Concentratio n (ng/mL ) 0.20 5 0.20 1 0.21 8 VoRecover

y 10 3 10 1 11 0 105 ±4.5 % 1.99 1.99 1.99 2.0 7

1.99 2.1 1 10 4

10 0 10 6 103 % ±3.1 % 19. 9 19. 9 19. 9 19. 8

20. 2 20. 6 99. 7

10 1 104 102 % ±2.2 % PFH S Spike d Concerttratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 Calculate d

Concentratio n (ng/mL ) 0.21 3 0.20 8 0.22 1 VoRecover y 10 7 10 5 11 1 108 % ±2.8 % 1.99 1.99 1.99 2.1 2

2.0 2 2.0 7 10 7

10 1 10 4 104 % ±2.9 % 19. 9 19. 9 19. 9 21. 0

21. 6 21. 8 10 5

10 9 10 9 108 % ±2.1 %

Pag e 1 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Intemal standar

d calibration Analyze d 8/2/1 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 PFO S (linear)

Calculate d Concentratio n (ng/mL ) 0.21 9 0.21 1 0.22 6 VoRecover

y 11 0 10 6 11 4 110 % ±3.6 % 1.99 1.99 1.99 2.1 5

2.0 4 2.1 3 10 8

10 3 10 7 106 % ±2.5 % 19. 9 19. 9 19. 9 21. 1

21. 7 21. 4 10 6

10 9 10 7 107 % ±1.4 % La b I D LCS-110726-1 0 LCS-110726-1 1 LCS-110726-1 2 Averag e ±%RS D LCS-110726-1 3 LCS-110726-1 4 LCS-110726-1 5 Averag e ±%RS D LCS-110726-1 6 LCS-110726-1 7 LCS-110726-1 8 Averag e ±%RS D PFO S (linear+branched )

Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 Calculate d

Concentratio n (ng/mL ) 0.25 2 0.25 4 0.26 4 VoRecover

y 12 7 13 8 133 129 % ±2.5% TM 1.98 1.98 1.98 2.2 9

2.3 9 2.5 3 11 6

12 1 12 8 122 % ±5.0%*^ ' 19. 8 19. 8 19. 8 23. 0

24. 3 25. 3 11 6

12 3 12 8 122 % ±4.9%'^ ' ETS-8-044. 0 Extema l standar d calibration Analyze d 8/2/1 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 PFO S (lineal )

Spike d Concentratio n (ng/mL ) 0.19 9 0.19 9 0.19 9 Calculate d

Concentratio n (ng/mL ) 0.24 3 0.24 1 0.24 5 VoRecover

y 12 2 12 1 12 3 122 % ±0.82% TM 1.9 9 1.99 1.99 1.99

2.0 1 2.0 9 99. 9

10 1 10 5 102 % ±2.6 % 19. 9 19. 9 19. 9 22. 7

21. 8 22. 2 11 4

11 0 11 1 112 % ±1.9 % La b I D LCS-110726-1 0 LCS-110726-1 1 LCS-110726-1 2 Averag e ±%RS D LCS-110726-1 3 LCS-110726-1 4 LCS-110726-1 5 Averag e ±%RS D LCS-110726-1 6 LCS-110726-1 7 LCS-110726-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 Calculate d

Concentratio n (ng/mL ) 0.24 6 0.24 9 0.25 1 VoRecover

y 12 4 12 6 12 7 126 % ±1.2% TM 1.98 1.98 1.98 1.83

1.69 1.95 92. 2

85. 6 98. 4 92.1 % ±7.0 % 19. 8 19. 8 19. 8 17. 8

19. 7 18. 2 90. 0

99. 6 92. 1 93.9 % ±54 % (1 ) Th e averag e recover ydi d no t mee t metho d acceptance criteri a o f100 % ±20%
.

Pag e 1 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I 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 QC dat a that i s contro l charte d an d use d t o evaluat e metho d accurac

yan d precision
. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2
. Th e standar d deviatio n i s calculate d fo rth e set ofaccurac yresults (i n %) obtaine d fo rth e Q C samples
. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h con-espond s t o a confidence leve l of95%
. Th e most recen t 5 0 dat a points were use d t o generat e th e metho d uncertaint

yvalue s liste d i n Tabl e 8
. Th e metho d uncertaint yifo rPFO S b

yETS-12-012- 2 wa s foun d t o b e ±24% , however , since th e highest recover yfo rth e LCSs , th e lo

wset ofbranche d an d linea rLCS , wa s 129% , th e analytica l uncertaint yassigne d t o thi s stud yfo rPFO S wil l b e ±29%
. Tabl e 8
. Analytica l Uncertainty
. Analyt e PFB S PFH S PFO S Standar d Deviatio n

5.1 5 5.3 3 12. 2 lUettio d Uncertaint y

±10 % ±11 % ±29 % 

## 8. 8 Fiel d IVIatri xSpike s (FMS ) Low , mid , an d hig h fiel d matri xspike s (FMS ) were collec:ted a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix
. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offiel d sampl e t o a containe rspike d byth e laborator ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o shippin g sampl e container s fo rsampl e collection
. Fiel d matri xspike recoverie s withi n metho d acceptance criteri a o f100±30 % confin n that "unknown " components i n th e sampl e matri xd o not significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Fiel d matri xspike concentration s mus t b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike
. Fiel d matri xspike s are presente d i n sectio n 9 ofthi s report . Tabl e 9
. Fiel d Matri xSpik e Levels
. Samplin g Locatio n MW47 MW12 1 Tri p Blan k Spik e Leve l Lo w Hig h Lo w Hig h Lo w Mi d Hiq h PFBS , ng/m L

0.25 0 1.0 0 2.0 0 20. 0 0.25 0 1.0 0 20. 0 PFHS , ng/m L

0.25 0 1.0 0 2.0 0 20. 0 0.25 0 1.0 0 20. 0 PFOS , ng/m L

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

- _

(Sample Concentrationo f

FMS - Average Concentration : FieldSampl e & FieldSampl

e Dup. ) ^ Spik e Concentraton


### 9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d fiel d matri xspike recoverie s fo rth e samplin g location s as wel l a s th e Tri p Blan k an d rinseate blank
. Results an d averag e value s ar e rounde d t o thre e significan t figure s 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 xspik

e 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 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### Tabl e 10
. DA LG WBPMW4 7 11071 3 (1 )



### 3MUMSI D GLP1OO1-02-19-005 GLP10-01-02-19-00 6 GLP10-01-02-19-00 7 GLP10-01-02-19-00 8 Descriptio n

DA LG WBPMW47 0 11071 3 DA LG WBPMW47 D B 11071 3 DA LG WBPMW47 LS 11071 3 DA LG WBPMW47 H S 11071 3 Averag e Concentratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 0.19 0 0.18 5 0.43 5 1.1 6 VoRecover

y N A N A 99. 0 97. 3 0.18 8 ng/m L±2.r/ o PFH S Concentratio n (ng/mL ) 0.13 9 0.13 6 0.40 8 1.1 3 VoRecover

y N A N A 10 8 99. 3 0.13 8 ng/mL±2.r/ o PFO S Concentratio n (ng/mL ) 0.20 6 0.21 4 0.50 6 1.36 %Recovery

N A N A 11 8 11 5 0.21 0 ng/m L±3.8 % NA = No t Applicabl e (1 ) Result s generate d usin g extema l standar d calibration
. 

### Tabl e 11
. DA LG WBPMW12 1 11071 3 (1 )



### 3MUMSI D GLP10-01-02-19-01 0 GLP10-01-02-19-01 1 GLP10-01-02-19-01 2 GLP10^1-02-19-01 3 Descriptio n

DALGWBPMW12 1 0 11071 3 DALGWBPMW12 1 D B 11071 3 DALGWBPMW12 1 LS 11071 3 DALGWBPMW12 1 H S 11071 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) <0.025 0 <0.025 0 2.1 1 21. 7 VoRecover

y NA NA 106 109 <0.025 0 PFH S

Concentratio n (ng/mL ) <0.025 0 <0.025 0 2.2 2 21. 6 VoRecover

y N A N A 11 1 108 <0.025 0 PFO S

Concentratio n (ng/mL ) <0.040 0 <0.040 0 2.1 5 21. 7 VoRecover

y N A N A 10 8 10 9 O.040 0 N A= No t Applicabl e (1 ) Result s generate d usin g Intema l standar d calibration
.

Pag e 1 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



### Tabl e 12
. Tri p Blan k (1 )



### 3MUMSI D GLP10-01-02-19-00 1 GLP10-01-O2-19-002 GLP1001-02-19-00 3 GLP1CM)1-02-19-00

4 Descriptio n DALGWTRIP 1 011071 3 DALGWTRIP 1 LS 11071 3 DALGWTRIP 1 M S 11071 3 DALGWTRIP 1 H S 11071 3 PFB S Concentratio n (ng/mL ) <0.025 0 0.26 3 1.0 2 21. 2 %Recover

y NA 105 102 106 PFH S

Concentratio n (ng/mL ) <0.025 0 0.26 8 1.0 4 21. 5 VoRecover

y N A 10 7 10 4 10 8 PFO S Concentratio n (ng/mL ) <0.040 0 0.25 5 1.0 2 20. 9 VoRecover

y N A 102 102 105 N A= No t Applicabl e (1 ) Result s generate d usin g intema l standar d calibration
. 

### Tabl e 13
. Rinseat e Blan k (1 )



### 3MUMSI D GLP1CW)1-02-19-009 Descriptio n

DA LG WBPMW12 1 RS 11071 3 PFB S Concentratio n (ng/mL ) <0.025 0 VoRecover

y NA PFH S Concerrtratio n (ng/mL ) <0.025 0 VoRecover y NA PFO S Concentratio n (ng/mL ) <0.040 0 VoRecover y N A N A= No t Applicabl e (1 ) Result s generate d usin g intema l standar d calibration
.

Pag e 1 9 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## 1 0 Conclusio n Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS
. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein
. 1 1 Data/Sampl e Retentio n Al l remainin g sample s an d associate d projec t data (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 

# 1 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 Attachmen t D : Metho d Deviatio n

Pag e 2 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1



## 1 3 Signature s 

# 1 ^ Date 

# 2£l ) Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r 

# M^^^^^-- ^ Q 'y/fy<!t^^<^oy/ Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yDepartmen t Manage rDate 

# wiiSt M \ 

# 11 Gar yHohenstein , Sponso rRepresentative Date

Jaisimh a Kesari , StudyDirecto r Date

Pag e 2 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1


## ATTACHMEN TA : PROTOCO LAMENDMEN T

Pag e 2 2 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 

### Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 9


## Stud yTitl e Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) I n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
PROTOCO LAMENDMEN 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 2
Samplin g Even t Decatu rPhas e 3 ; Off-Sit e B P Property

Pag e 1 o f7 Pag e 2 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 

### Analytica l Protocol : GLPlb-01-0 2

Amendmen t 1 9 

## Thi s amendmen t modifie s th e followin g portio n o fprotocol : "Analysi s o fPFOS , PFH S an d PFB S I n Groundwater , Soi l an d Sedimen t fo rth e 3 M

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

PROTOCO LREADS : 

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

O READ : 

### N o change s t o th e wordin g o fth e protoco l are required
. Thi s amendmen t onl yaddresse s an d document s th e additio n ofth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s a s par t o fth e 3 M Decatu rPhas e 3 Progra m fo rPFOS , PFH S an d PFB S (GLP10-01-02)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e o fth e wee k o fJul y11 , 2011
. Th e groundwate r sample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s project GLP10-01-02-1 9 an d reporte d a s interi m repor t GLP10-01-02-19 , (reflectin g stud yGLP10-01-0 2 an d amendment-19) ,
Reason ; 

### Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t fo rtw o 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 form
.

Pag e 2 o f7 Pag e 2 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property.-Jul y201 1 

### Analytica l Protocol : GLP1D-01-0 2

Amendmen t 1 9 

## Amendmen t Approva l

Gar yHohenstein , Sponso rRepresentative Dat e 

# ^jlZ.}z4l) Clesto n C
. Lange , Principa l Analytica l Investigato rDate

Willia m Reagen , Ert S Opn s Environmenta l La b Managemen t Dat e

Jaisimh a Kesar i P.E. , DEE , Stud yDirecto r

Pag e 3 o f7 Pag e 2 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 

### Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 9

To : From : 

## cc :
Date : Subject : 

## Environmenta l Healt h & Safet yOperations , Environmenta l Laborator y Genera l Projec t Outlin e Gar yHohenstein , 3 M EHS&Opn s Susa n Wolf , 3 M EHS&Opns ; EnvinDnmenta l La b Willia m Reagen , 3 M EHS&Opns ; Environmenta l La b Clesto n Langey , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Jul y6,201 1 Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas 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 3 M Sponso rRepresentativ e Gar yHotienstei 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 aatiohensteinOmmm.co m 3 M Environmenta l Laborator yManagemen t Willia m K
. Reage n 2 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wkreaaen®mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 ccl^nqetammm.co m Samplin g Coordinato r Timoth yFrtna k Westo n Solution s Jimpthy.frlnaK(aM9tonsolutions,«i m Phone : (334)-332-912 3 GLP10-01^2-1 9 Dep t #530711
. Project #002267444 9 Samplin g schedule d fo rth e wee k o fJul y11 , 201 1 

### Al l verba l an d writte n correspondenc e wil l b e directe d to Gar yHohenstein
.

Pag e 4 o f7 Pag e 2 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 

### Analytica l Protocol : GLP10-01-0 2

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 rPerfiuorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfiuorooctanesulfonat e (PFOS ) 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 fEP ATSC AGoo d Laborator y Practic 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 ensure tha t result s fo r PFBS , PFHS , an d PFO S ar e o fa know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar y Hohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-02-19
. 

## 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 ofquantitatio n wil l b e 0.02 5 ng/m L(ppb ) fo rPFBS , PFHS , an d PFOS
. Two samplin g location s have bee n specified
. Se e attachmen t Afo ra list o fth 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 "fil l t o here " lin e o n eac h 25 0 m LNalgen e tsottl 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 at th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe r bottles
. Al l sampl e bottle s wil l includ e th e additio n o f^^Oa-PFBS , ''^OrPFHS
. an d "Ca-PFO S (intema l standard ) at a nomina l concentratio n of1 ng/mL
. Al l sampl e bottle s wil l als o includ e th e additio n of^^C4-PF0 S (surrogat e spike ) a t a nomina l concentratio n o f0. 1 ng/m LOn e additiona l bottl e wil l b e prepare d t o b e use d fo r th e preparatio n o fth e equipmen t rinseate blank
. ASOOm Lbottl 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 belowlists 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 Hifl h Low Hig h Low Mi d Hig h 

### Spik

e Cone
. (ng/mL) 0.2 5 1. 0 2. 0 2 0 0.25 1.0 2 0

Pag e 5 o f7 Pag e 2 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Slt e B P Property. - Jul y201 1 

### Analytica l Protocol : GLPlb-01-0 2

Amendmen t 1 9 

## Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S fblkjwin g ETS-8-044. 0 "Detemninatio n ofPerfluorinate d Compound s I n Wate rb

yHig h Performance LK|ui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Alternately , sample s ma yb» e analyze d b

yETS 8-154. 3 "Detemninatio n ofPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rBySoli d Phas e Extractio n an d Hig h Perfomnanc e Liqui d Chromatography/Mas s Spectrometry"
. Th e dat a qualit

yobjective s fo rthes e studie s ar e quantitative results fo rth e targe t analyte s wit h a n analytica l accurac yof100±30%
. Fiel d matri xspike s not yieldin g recoverie s vinthi 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 perfluorocarboxyli cacki s an d perfluorosulfoni cacid s at a nomina l concentratio n o f1 ng/mL
. Th e calibratio n curve wil l b e generate d bytakin g th e rati o o fth e standar d pea k are a counts ove rttie intema l standar

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

an d tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an y equipment/rinseat e blank s prepare d i n th e fieM
. Latiorator ycontro l spike s o freagen t wate rprepare d a t th e tim e ofsampl e extractio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d preciston
. Mettio d blank

s o freagen t wate rprepare d at th e tim e o fsampl e extractio n wil l b e use d t o determin e ttie mettio d detectio n limit
. Fo rtiiose samplin g location s where ttie fiel d matri xspike leve l wa s no t appropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspike ma

yb e prepare d an d wil l b e include d i n th e fina l report .

Pag e 6 of7 Pag e 2 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-sit e B P Property- Jul y201 1 

### Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 9 Attachmen t A Bottl e reques t - B P Wel l Samplin g Wee k o f1 1 Jul y201 1 Sulfonate s level s Young , Charle s T
. t o cbjacoby2@mmm.com , stwolf@mmm.com , clange@mmm.co m 07/05/201 1 01:43 PM C o „ Frinak , TimothyR. ' Analyse s o f

sulfonate s i

nth e B Pwel l groundwater sample s shoul dals o b e performe dunder GLPlO-01-02 . Previously detennine dlevel s o f th e sulfonate s i

n601 R(clos e t o MW-47 ) and601 L(clos e to MW-121 ) were : Sampl e ID DAL-GW-601R-0
- 06041 3 DAL-GW-601R-0
- 07092 0 DAL-GW-601L-0
- 06041 3 DAL-GW-601L-0
- 07092 0 Sampl e Dat e PFB S PFH S PFO S 13-Apr-0 6 NR0.025 4 N D 20-Sep-0 7 0.033 1 0.058 5 0.064 9 13-Apr-0 6 NR20. 8 2.5 4 20-Sep-0 7 2.9 1 17. 4 2.8 3
Thanks , Charli e Charle s T . Youn g Technical Directo r WestonSolutions , Inc . 1400 Westo nWa

y (5-2 ) Wes t Chester , P

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

Pag e 7 o f7 Pag e 2 9 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I 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 3 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b

Dat a printe d b

yST W Printing Time : 9:39:2 0 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1


### Pag e 3 1 o f 7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b

Dat a printe d b

yST W Printing Time : 9:39:3 5 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1


### Pag e 3 2 o f 7 0GLP10-01-02 ; Interi m Repoi l 1 9 Analysi s o fPFBS
. PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b 

# I Sampl e Name : 1(110729a016 rSsmp h ID:'1 1 003-25-ff ' File : PM k Name:-13C3PFHS0S) - MaM(e«):"402.000J80.00 0 Da Commen t '1. 0 ns/m LF C M d I n Synth
. Wata fAnrwtatlon: " Sampl e Index : 1 6 Sampl e Type : Standar d Concentration : 0.9 4 5 ng/m L Calculate dCone : N/ A Acq . Date : 7/29/201 1 Acq . Time : 7:47:0 1 F M Hodlfied : No Proc . Algorithm : Specif y Par i PerceriCage : 5 0 "k110729a,»« r

eter s - M

O II I Bas t . V)in

< •Split . I Repor t Larges t

Pe « Min , Pea k

Heigtit : Min . Pea k

Hidth : Smoothlr. qHidth : R THindow : Dipecte dRT : : Rela i ! RT : 1 Time : 15- 2 2376 7 3 2 co i 4.076+00 5 15. 6 mi n 3.4« S 3.2e5 ' 3.0e5 ' 2.8* 5 2.6* 5 2.4*5 ' 22* 5 2.0* 5 1.Be5
- 1.6*5
- 1.4*5
- 1.2*5
- 1.0*5
-
6.0* 4 4.0*4 - 2.0* 4 

# I SatTpleName:1c110729aO28 " San^t o ID;'LCS-110726. rRte:Tc110729a.»« r PeakNaine;'13C3PFHS(IS) - Maw(e«):'402.OCXV80.000Da Commen t -0.2pp b LCS " Anrtotatton : ~ Sampl e Index : 2 8 Sampl e Type : Q C Concentration : 0,93 9 ng/m L 

# I Sampl e Name : "k11072ga02 rSampl * ID : 1 1 005« rFie:-k110729a.wtt T Pea k Name : '13C3PFHS(IS) " MiM{et> : '4O2.00CVBao xDa ' Commenl : 'Metho d Blanl TAnnotation : - Sampl e Index : 2 7 Sampl e Typ« : Unknow n Concentration : 0.9 4 5 nq/m L4.2*5
- Calculate dCone : N/ A Acq . Date : 7/29/201 1 4.0*5
- Acq . Time : 11:39:0 0 P M 3.8* 5 3.6*5
- 3.4*5
- 3.2a5
- 3.0a5 - 2.8*5 - 2.6a5 - 2.4eS < 2.2* 5 2.0*5
- 1.6*5 - 1.6*5
- 1.4*5 - 1.2* 5 1.0*5 - 8.0M e.0a4 - 4.0*4 - 2.0*4 - Modified : Proc . Algorithm : Hols e Percentag e Va s Specif y P a SO Base . Sub . Hindov : 1.0 0 Peak-Split . Fac t t : 2 Repor t Larges t

Peak : Ye s Min
- Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : 2 6 Height : Star t Time : En dTime : 0.0 0 0.0 0 0 30. 0 15. 2 H o Valle y IS. 2 534 2 co u .25fc*00 5 15. 1 15. 5

Sampl e Nam*:'k110729a031 " SamptelD:*LCS-11072&4 - Fie:*V110T2a».wlf r Pea k Name : *13C3PFHS(IS) - Ma(a(es) : '402.000)^.00 0 Da ' Comment : '2pp b LCS ' Arvwtatkin: " Sampl i

- - Type : O C ng/m L

Proc . Algorithm : S p Nois e Percentage : Base . Sub . window : Peak-Split . Factor : Repor t Larges t

Pea k Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R THindow : Expecte dRT : Us e Relativ e RT : ecif y P a 5 0 1.0 0 2 : Ye s 0.0 0 0.0 0 0 30. 0 15. 2 r N o Int . Type : Valle y Retentio nTims : Area : 2472 2 Height : 3. E Star t Time : 15. 2 n 0 CO U ;e*oo s 15. 1 n Sampl e Type : Concentr a Calculate c Acq . Dat e Acq . Tim e Modified : Proc . Alg c Hois e Pe r Base . Su b Peak-Spl I Rei>or t L a Min . Pea k Min . Pea k Smoothin g ion :

rithm : Hind o

. Fac t O

C 0.93 8 N/ A 7/30/201 1 1:03:2 9 W l No Specif y P a SO ' : 1.0 0 o r : 2 ges t Peak : Ye s Heigh t Width : rildth : Expecte dRT : Us e Relat I Retentio n Area : Height : Star t Tim e En dTime : v e RT :

Time : 0.0 0

0.0 0 0 30. 0 a 15. 2 n H o Valle y 15. 2 1 245059 6 co u .410*00 5 c 1S, 1 n 15. 5 n

Dat aprinte db y ST

W Printing Time : 9:45:1 9 AM Printin g Date : Thursday , Augus t 25 , Pag e 1 o f 8 201 1 Pag e 3 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS
. PFHS
. an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b

V Sampl B Name:'V11072«s034 " Sampl e ID:-LCS-110726-7 ' Fita : VII0729a
. •Pea k Name : "13C3PFHS(IS) - MaM(Ba):'402.00080.00 0 Da ' I Comment'20ppbLCS ' Annotation: ' Sampl e Type : Concentration : Calculate dCo r Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hois e Percentage : Base . Sub . Mlndo t Peak-Split . Fact e Repor t Larges t

P t Kin . Pea k

Height : Min . Pea k

Width : Smoothin g Width : Q C 0.93 ( N/ A 7/30/201 1 2:06:4 8 A

M Specif yPar
. S O

- : 1.0 0 ng/m L

R TI J RT :

i RT : Int . Type : Valle y Retentio nTime : 15. 2 Area : 225810 9 c t Height ; 3.49e-t00 5 Star t Time : 15. 1 En dTime : 15. 6



# I Sampl e Name : 1(110729a05 rSampl e ID:'OLP1l>O1-02-1&oa rFile : Pea k Name : -13C3PFHS(IS) ' Mm«(e») : '402.00080.00 0 Da Commen t "DALQVWTRIP 1 L S 11071 TAnnotatkm : " Sampl i •- Type : Unknow n ng/m L Sampl * Name : 1(1107288055 - S«n^lD:'OLP1M)1<02-1&O0g rFie : PttakName:'13C3PFHS(IS) rMa*s<««}:-402.00000.00 0 Da ' Comm*nt:-DALGWBPMW121RS1107i rAmotatktn: ' Sampl e lnde:< : 5 5 Sampl e Type : Unknow n Concentration : 0.94 5 iig/m L Calculate dCone : H/ A Acq . Date : 7/30/20 H Acq . Time : 9:30:1 2 A M Modified : Proc . Algorithm : Hois e Percentage : Base . Sub . Mindo w Peak-Split . Fact o Repor t Larges t

P e Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTine : No Specif y P a 5 0 : 1.0 0 r : 2 a k : Ve 5 0.0 0 0.0 0 0 30. 0 15. 2 n No V a1 le y 15. 2 n Area : 234675 4 co u Height : ; Star t Time : En dTime : .96e+00 5 15. 0 n 15. 4 T

l

Sampl e Name : 1(110729306 7 San ^ ID : *OLP1(KlU ^ Pea k Name:-13C3PFHS(tS) " MaM(*«):'402.00O80.000 1 Comment:-DALOWBPMW121D11071 TAnnotation:' " Sampl e Index : 6 9 Sampl e Type : Unknow n Concentration : 0.9 4 5 ng/ml . Calculate dCone : N/ A Acq . Date : 7/30/301 1 Acq . Time : 3:25:5 6 P M Spiecif y Parameter !

Int . Type : Valle y Retentio nTims : 15. 2 Area : 219196 0 co i Height : 3.62e+O0 5 Star t Time : 15. 1 En dTime : 15. 5 Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hois 6 Percentag * Unknow n 0.94 5 r N/ A 7/30/201 1 10:12:2 7 A

M N o Specif y Par a 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s Min . Pe- k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 s e I S . 2 m Valle y 15. 2 a Area : 258937 9 cou n Height : Star t Time : .12et00 5 c f

15. 1 mi Mod i Pro c Sas e Pea k Kin . Min . led : Al g Su b Spl I t L a Pea k Pea k Smoothin g R TWindo w r i t

H i I d

. Fa c qe a He l Widt h Wir t Expecte dRT : Us e Rela t h

v e R T

Dat aprinte db y ST

W Printing Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 2 o f 8 Pag e 3 4 o f7 0GLP10-01-02 : Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b 

# I San*4eName:1(110729aO16 ' Sampt e I0:-1100^-25-ff ' Rte:lc110729a
. P*akNama:'1802PreS(e) " Ma«*<ea):-aos.OOOM.OO O Da ' Commant-1. 0 no/m LFC« U i n Synth
. VVal* rAmotatton: - Sampl e IndeK : 1 6 Sampl e Type : Standar d ncentration : 0.97 5 ng/m L Iculate dCone : N/ A Acq . Dat e Acq . Tim e Modified : Proc . Algorithm : Kois e Pe r Sase . Su b Peak-Spl l entag e

Wlnd o 7/29/2 0 7 : 47:0 1 Ye s Specif y

. Factor : Repor t Larges t

Pea l Mtn . Pea k Min . Pea k Smoothin g R TWindo w Heigh t

Width : Width : Elxpecte dRT : Us e Rela t Int . Typ e Retentio n Area : Height : v e RT :

Time : B a 5 0

1. 1 2 : Y
0 0 30. 0 13. 7 N o s e T o IS.-
- 175229 8 c Star t Time : En dTime r .14e*00 5 13. 6 H . O 1 P M P a

0 0

Ba <



# I Sampl e Name : I d 10729a02ff ' Sampl a ID:-LCS-110726-1 * i PttakName:-1802PFBS(IS) - Ma«»(*«) : *303.000/M.00 0 Da ' Comm*nt : "0.2pp b LCS ' AnfMtatton : ~ Sampl e Inde x 

# I Sampl*Nam* : 1(1107293027 - SamplelD:-1100S«9r - Fl*:1(110729a.wtf r P*a k Nam* : -1802PFBsas rMaaa{8a) : '3O3,00ai«4.00 O Da ' Comnwnt:'liMhodBlani rAnnotatk>n: - Sampl e Index : 2 7 » Type : Unknow n ng/m L Sampl e Type : Concentration : Cal c Acq . late dCon e Date : Time : Modified ! Pro c Nol a &aB P fea k Rep o Min . Mtn . Algorith m Unknow n 0.97 5 H/ A 7/29/201 1 ll:39i0 0 P H o Specif y P a Percentage : 5 0 Sub . Window : 1.0 0 Split . Fa c t Larges t Pea k Heig h Pea k Hidt h hin g Midt h R TWindow : Exp e t a dRT : Us e Relativ e R

T Int . Ret e Are a Type : tlo nTime : o r : 2

eak : Ye s : 0.0 0

0.0 0 0 30. 0 13. 7 H o Bas e T o B a 13. 8 178 4 04 0 co u Height : Sta r Time : En dTime : 2.79e+00 5 13, 6 14. 0



# I Sanq)tekame:ic11072aa03 rSampl a 10 : XCS-110^26-4 ' FI*:'V110729a.wir r Pea k Name:'1802PFBS(ls rMata(e*):-3O3.00ar84.0O 0 Da ' Comnwnt : '2pp b LCS ' Annotatkin: " Sampl e Type : O C Acq . DaC

e : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fac t 7/30/201 1 12:00:0 4 A

M N o Specif y Pa r : 1.0 0 r : 2 Repor t Larges t

Peak : Ye s Hin . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : L's e Relativ e RT : Int . Type : Retentio nTime : Area : l e Height : Star t Time : En dTime : 0.0 0 0.0 0 0 30. 0 s 13. 7 m N o valle y 13.- ' m 784 6 cou n .B3e*00 5 C

f 13. 6 m 13. 9 ml ntr a ion : Calculate dCone : Acq . Acq . Mod i Pro c Hoi s Bas e Pea k fie|» Min . Min . Dat e Tim e led : Algorithm : Percentag e Su b Spl l t L a Pea k Pea k Smoothin g R TW Exp e ndo w 0.96 8 H/A 7/30/201 1 1:03:2 9 A

M Ye s Specif y P a S O Window : 1.0 0

. Factor : 2 ges t Peak : Ye a Heigh t width : Width : t e dRT : Us e Rela t Int . Rete r Are a Heig . Sta r En d1 Typ e tlo n Ti m ime : v e RT : Time : 0.0 0

0.0 0 0 30. 0 13. 7 n No Bas e T o Ba . 13. 7 n 168296 8 cou r .93et00 5 c 13. 6 1 14. 1 n

Dat aprinte db y ST

W Printin g Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , Pag e 3 o f Pag e 3 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 •ETS-Kir k Result s Name : kll0729a.rd b 

# r Sanv h Name:-k11O729a034 ' SMn;4 e ID:'LCS-11072e-7 - FUe : I d 1072Sa.wir r PeakNaiiM:''ie02PFBS<1S) " HaM<0t):-303.QOCU84.00 0 Oa ' ConTMn t 'TOpF^

LCS * Annotation: " Simpl i • Sampl e Type : Concentration : Calculate dCone : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fa d Repor t Urgss t

1 Min . Pea k

Heigh l Min . Pea k

Hidth : Smoothin g Hidth : R TWindow ; Expecte dRT : Us e Relativt , RT : Q C H/ A 7/30/201 1 2:06:4 8 A

M Ye s Specif y P a : 5 0 w : 1.0 0 o r : 2 6ak : Ye s : 0.0 0

0.0 0 0 30. 0 13. 7 n N o Int . Type : Bas e T o Bas i Retentio nTime : 13. 7 m; Area : 156671 7 coun i Height : 2.47etb0 5 c ] Star t Time : 13. 6 m: En dTime : 14. 1 m:



# I Sampl a Name : TrtlOTTSsOS rS«mpl B lD:"GlP1(M)l-02-1W)02'"~Rie : Pea k Hame : 'ie02PFBS((S) " Mata(e«) : -303.OOQflM.00 0 Da ' Conmienl:-DALGWTRIPlLS1107i rAnnotatfen: " Sampl e Index : 5 7 Sampl e Type : Unknow n

L«tlon : 0.97 5 ng/m L :« d Cone : N/

A 

# I Sampl e Name:'It110729a05ff ' SamptelD:'QLP1<M)l-O2-1Ml0 rFle:1c110729«.w r Pea k Name : -1802PFBS(IS) - MaM(e«) : -303.000/84.00 0 Da ' Commw*:"DALGWBPMW12 1 RS1107i rArewtaOon:" " Sampl e Inde.x : 5 5 " Type : Unknow n Sampl e Type : Concentration ; Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Hois e Percentag e Unknow n 0.97 5 N/ A 7/30/201 1 9:30:1 2 A

M N o Specif y P a : 5 0 Base . Sub . Mindow : 1.0 0 Peak-Split . Fa c Min . Pea k

Heig h Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : o r : 2

eak : Te a : 0.0 0

0.0 0 0 30. 0 13. 7 n H o valle y 13. 7 n Area : 162356 4 co u Height : Star t Time : En dTime : 2.eOet00 5 13. 6 n 14- 0 n

13. 5 14. 0 14 5 15. 0 15 5 16. 0 SamplBName:-k110729a06? ' Sampl e ID : ^3lJ>1(H)1•02-1»«1ff ' Fie : PeakName:-1802PFBS(IS rMata(e«):-303.00084.00 0 Da ' Comment : 'DALG WBPMW12 1 0 lions ' Annotation : - Sampl e Index : 6 9 Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fac t 7/30/201 1 10:12:2 7 A

M N o Specif y Param a S O : 1.0 0 m i r : 2 Repor t Larges t

Peak : Ye s Min . Pe» k

Heigh t Min . Pei k

Width : Smoothin g Width : R THindoH : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : 1 7 Height : Star t Time : En dTime : 0.0 0 c 0.0 0 s 30. 0 se c 13. 7 mi n H o Bas e T o Bas e 13. 7 mi n 295 6 count s .BOatOO S op s 13. 6 mi n 14. 1 mi n Sampl e Type : Unknow n Concentration : 0.97 5 Calculate dCone : N/ A Acq . Date : 7/30/201 1 Acq . Time : 2:25:5 6 P M Modified : H o Proc , Algorithm : Specif y Pa r Nois e Percentage : 5 0 Base . Sub . Hindow : 1.0 0 Peak-Split . Factor : 2 ReiMr t Larges t

Peak : Ye s Min . Pea k

Height : 0.0 0 Min . Pea k

Width : 0.0 0 Smoochin g Width : 0 R TWindow : 30. 0 s Expecte dRT : 13. 7 m Us e Relativ e RT : N o ng/m L

amet e

c p s p o L n Int . Type : Bas e T o Bas e Retentio nTime : 13. 7 m Area : 151868 9 cou n Height : 2.49e+00 5 c I n p s Star t Timt : 13. 6 mi n En dTime : 14. 1 m I n

Dat aprinte db y ST

W Printin g Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 4 o f 8 Pag e 3 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b

¥^Sanpl8Name:"k110729a0ie r Sampt o ID:'1 1 OOMS ^ Fil8:-k110728a.v.tt r IPea k Name;'PFBS
- M«M{ei):-299.000/80.00 0 Da.299.00a«9.00 0 Da ' IComment'1. 0 nfl/mLFC«t dI nSynth . Wate r

Arvwtatbn: " Sampl . Stan c ir d 1.0 0 Sampl e Type : Concentr atio r Acq . Date : Acq . Time : Modified : Proc . Algorithm : Sp . Hois e Percentage : Base . Sub . Window : Peak-Split , Factor : Repor t Larges t

Pea k Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R TWindow : 30. 0 Expecte dRT : Us e Relativ e RT : H i S O

3, 7

Height : Star t Time : En dTime : 243142 5 count s

4.ne+00 5 cp s 13. 6 mi n 4.0e 5 3.Be 5 3.6e5
- 3.4e 5 3J2e 5 3.0e 5 2.6e 5 2.6e 5 2.4e5
- 2,2e 5 2.0e5
- 1,Sa5
-
1.4e5 - 1.2e5 - 1.0e5 - 8.0e4 - 6.0e4 - 4.0e4- 2.0e4 - 

# I Sanv^Nsme:1c110729a02S r Sanqil e ID : t,CS-110726- r FUe:-V11072d>.wi r Ptta k Name : -PFBS ' MaM<es) : "299.000/80.00 0 Da,299.00Q/!99.DO O Da ' Commen t

-0.2pp b LCS
- Annotation: " Sampl e Index : 

# T Sampt aName:'V110729a02 r Sampl aID:'1 1 00&«S r Fie : 1(110729a.wff

T Pea k Name : "PFBS ' MaM(e«) : "299.000/80^ 0 Da.299.O0Qm.0O 0 Da ' Comment:'Metho dBtardTAnnotation:
- Sampl e Inde!< : 2 7 Sampl e Type : Unknow n Concentration : N/ A1800
- Calculate dCone : < 0 Acq , Date : 7/29/201 1 ^TQQ . Acq . Time : 11:39:0 0 P M fy E Modified : 1 c . Algorithm : Spe i s e Percentage : 9 0 Base . Sub . Window : l. i Peak-Split . Factor : 2 Repor t Larges t

PeaK : Y

< Min . Pea k

Height : 0 Min . Pea k

Width : 0 lOChIn g Width : 0 R TWindow : 30. 0 Expecte dRT : 13. 7 telati i RT : Int . Type : Retentio nTime : Area : Height : Star t Time : En dTime : Bas e T o 13. a 1099 S l.eOe'O O 13. 6 13. 9 160 0 1S0 0 140 0 130 0 120 0 1100
- 100 0



# I Sam|ileN«me:*k110729aO3l
- SaTi«>lelD:1.CS-11072&4
- Fte:1c110729a.wi r Pea k Name : -PFBS ' HaM(e«) : '298.00ai80XXX ) Da,299.000/99.00 0 Da
Commen t

*2pp b LCS
- Annotation : ~

8.0e5 ' 7.5e 5 7.0e 5 6.5e S 6.0e 5 5,5e 5 5.0e5 ' 4.5e 5 4.0e 5 3.Se 5 3.0eS ' 2.5e5
- 2.0tt 5 1.5a 5 1.0e5 ' 5.0e4
- 15 5 16, 0

Sampl e Type ; O C Concentration : 0.19 9 Calculate dCone : 0.21 5 Acq , Date : 7/30/201 1 Acq . Time : 12:00:0 4 A M Modified : N o Proc . Algorithm : Specif y Pa r Nois 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 R TWindow : 30. 0 s Expecte dRT : 13, 7 m Vs c Relativ e RT : K o Int . Type : Bas e T o Ba s Retentio nTime : 13. 8 m Area : 49387 6 cou n Height : 7,99o+00 4 o ng/m L ng/m L

amet e Bi n

n

Star t Time : 13. 6 mi n En dTime : 14. 0 m i n Concentration : Calculate dCone : Acq , Date : Acq . Time : Modified : Proc . Algorithm : Hois e Percentage : Base , Sub . Windo v 1.9 9 2.1 1 7/30/201 1 1:03:2 9 A

M Ve a Specif y Pa r SO 1.0 0 Peak-Split . Factor : 2 Rejior t Larges t

Peak : Ye s Min . Pea k

Height : Min . Pea k

Hidth : Smoothin g Width : R TWindow : Expecte dRT : L's e Relativ e RT : Int . Type : Retentio nTimt : 0.0 0 0.0 0 0 ng/m L ng/m L

amet e mi n

30. 0 se c 13. 7 m No Manua l 13. 7 m Area : 473264 1 cou n Height : fi Star t Time : En dTime : 53et00 5 c 13. 6 ra 14. 0 m L

n
L n : s p s I n i n

0.0 - 15. 5 16. 0 Dat aprinte db y ST

W Printing Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , Pag e 5 o f Pag e 3 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS
. PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b 

# I Sarrpl e Name:'V110729a034 - Sampl e ID : "LCS-110726- rHIa:'Vt10729a.wi( r Pea k Name:-pros ' M«M(e«}:'299.000/BO.OO O Da.299.000im.00 0 Da ' Convnai ±"ZOpp b LCS ' Annotation: " Sampl e Index : 34 Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split . Fac t Repor t Larges t

P Min . Pea k

Heigh l Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Inc . Type : Retentio nTime : Q C 19. 9 ng/m L 21. 2 ng/m L 7/30/201 1 2:06:4 8 A

M Ye s Specif y Parameter s - M Q II I : 5 0 w : 1.0 0 mi n o r : 2 0.0 0 cp s

0.0 0 se c 0 point s 30. 0 se c 13. 7 mi n N o Manua l 13. 7 mi n Area : 4102563 7 count s Height : Star t Time : En dTime : ;.19et00 6 cp s 13. 6 mi n 14. 1 mi n

13 5 14. 0 14 5 1^. 0 1^. 5 16. 0 

# I Sampl e Name : •k110T29»05 rSamft e ID:-GLP1Wl1,02-1frOO r^E 7 Pea k Name:'PFBS ' Maaa(e«):-299.OOCV80.000 Da,299,00(V99.00 a Da ' Cortwnent-DALGWTRIP1LS1107i rAnnotatton:- " Sampl e Index : 5 7 I.IOeS
1.05e 5 1.00e5
- 950e4
- 9X0e4
- 850e4
- 8.0ae4
- 750e4
- 7.00e4
- 6.50e4
- ^ S.00e4
- I55064
- 

### I

- 5.00M 450e4
- 4.00e4
- 350»4
- 3.00e4
- 250e4
- 2.00e4
- 150e4- ' 1.00e4 ' 5000.0 0 0.0 0 

# I Sampl e Name : I d 10729a05? ' SamplelO:-OLP1CKl1-02-1&O09 ' Fle:-k110729a.vi« r Pea k Name : TFB5 - MaM(ee) : "299JXXV8DJOO O D a ,299.000^.00 0 Da ' Coim)ent-DALGWE1PMWI21RS110713 ' Amototkm: - Sampl e Type : Concentration : Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Nois e Percentag . Unknow n H/A < 0 7/30/201 1 9:30:1 2 A

M N o Specif y Pa t : 5 0 Base . Sub . Window : 1.0 0 Peak-Split , Fa c o r : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heig h Min . Pea k

Widt h Smoochin g Widt h R THindow : Expecte dRT : Us e Relativ e R

T Retentio nTime : Area : Height : Star t Time : En dTime : O.O O 0.0 0 0 30. 0 s 13. 7 m N o Ba3 « T o Ba s 13. 7 m 696 9 cou n 1.60et00 3 c 13. 6 m 13. 9 m

11 5 15. 0 1^. 5 16. 0 

# I Sampl e Nan»:Tc110729a069^ Sampl a ID : •OLP1O4J1.02-19O10 ^ F»a:-k110729a.«« r Pea k Name : -PFBS ' Ma(a(ea) : -299.00CV80X)00 Da.299,00ara9,00 0 Da " Comm©rt;"DALGWBPMW12101107i rAnnotation : * Sampl e Index : 6 9 Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hois e Percentag e Unknow n M/ A 0.2S 3 7/30/:01 1 10:12:2 7 A

M N o Specif y Pa n S O Base . Sub . Window : 1.0 0 Peak-Split . Fac t i r : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 0.0 0 0.0 0 0 30. 0 S t 13. 7 m N o Valle y 13. 7 m 1.13e+00 5 cp s 13. 6 mi n 14. 0 mi n S..P1 . Typ.: : Concentr a Calculat e Acq . Dac e Acq . Tim e Modified : Proc , Al g Nois e Pe r Base . Su b Peak-Spl l Con e

rith m Unknow n

M/ A 0.016 4 7/30/201 1 2:25:5 6 P

M H o Specif y P a entage : 5 0 Win d w : 1.0 0

. Factor : 2 Reijor t Larges t

Peak : Ye s Min . Pea k Min . Pea k Smoothin g R TWindo w Height : 0.0 0

Widt h Widt h Expecte dRT : Us e Rela t int . Typ e Retentio n Area : Height : v e R

T Time : Star t Time : En dTime : 0.0 0 0 30. 0 13, 7 H o Bas e T o B a 13. 8 4 557 5 co u 7.67e.00 3 13. 6 13. 9 

# 1 i 750 0 700 0 650 0 600 0 550 0 500 0 450 0 400 0 350 0 300 0 250 0

150 0 100 0 50 0 0 11.4 7



# L 124 9



### 1 

# to"mT .Wwif.K k 19 5 16. 0 Dat aprinte db y ST

W Printin g Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , Pag e 6 o f 8 Pag e 3 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b 

# I SarrvleName:"k11072da016 ' Sampl e ID:'1 1 00»2&« - File:-k11D729a.wti r Pea k Name : 'PFHS ' Masa{ee) : -399.000/99.00 0 Da.399.00(V80.00 0 Da ' Commen t "1. 0 mini
. F C et d I n Synth
. Watei " Amotatton : ~ Sampl e IndeK : 1 6 Sampl e Type : Standar d Concentration : 1.0 0 ng/m L Calculate dCone : 1.0 7 ng/m L Acq . Date : 7/29/201 1 Acq , Time : 7:47:0 1 P M N o Baf e Algorithm ; S j Sub . Window : Fact e Repor t Larges t Pea l Min . Pea k Height : Min . Pea k Hidth : Smoothin g Hidth : RT Window : Expecte d RT : Us e Rela l
Height : Star t Tim e En dTime : : RT : 

# I Sampl e Name:-Ic110729a027 - Sampl e 10:'1 1 OO&e? ' Fle:'K110729a.w» r Pea k Nante : 'PFHS ' Ma««(ea) : -399,000/99.00 0 Da,399.000/80.00 0 Da ' Comment : "Metho d Blanl ^ Annotatkin : - Sampl e Index : 2 7 4^e4 - 4.0e 4 3.Se 4 3.6e4 - 3,4* 4 3.2e4 ' 3,0e 4 2.8e 4 2.6e 4

. 2.4e 4

- 2.2e 4 2.0e 4 1.8e4 1.6e4 1.4e4 1.2e4 1. 0 8000.0 ' 6000. 0 4000.0 ' 2000. 0 Sampl e Type : Concentration : Calculate d Cone : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wlnd o Peak-Split , Fac t Unknow n N/ A < 0 7/29/201 1 11:39:0 0 P M Ye s Specif yPa r 5 0 1.0 0 it : 1 Repor t Larges t Pea>: : Ye s Min . Pea k Heigh t Min . Pea k Width : Smoothin g Width : RT Window : Expecte d RT : Us e Relativ e RT : Int . Tvpe : Retentio n Time : Area : Height : Star t Time : End Time : 0.0 0 0.0 0 a 30. 0 s 15. 2 m N o Manua l 15. 2 m 319 7 cou n .40et00 3 c 15. 2 m 15. t B

13. 0 i^iii.j,icrwh^iVitfl ; tff\ i 

## .juA v JiUfOs^eff^j^iiSti ^ J A SampleNan'«:-k110729a031 " SamplelD:"LCS-11072&J - Fle:1c110729a.iMf r Pea k Nanrte : -PFHS ' MaM<e«) : "399.000/99.00 0 D a ,399.000/80.00 0 Da ' Comment : '2pp b LCS " Annotatton : " " Sampl e Index : 3 1 LOSee
LOOeS
9.50e S 9.00e5 ' 8.50e S 6.00e 5 7.50e5
- 7.00e5
- 6.50e 5 6,0Oe5
- 550eS
5X0eS
450eS
4,00eS
3.50eS
3.00eS
2.50e5
- 2.00eS
1.50e5
- LOOe S 5.00e4 ' 0.00
- 

# I Senil e Name : •k110729a02ff ' Sampl e ID : "LCS-110726-1 - Flle:*k110729a.»« r Pea k Name : 'PFHS ' Maas(e«) : -399.00099.00 0 Da,399.OOa'8aO0 O Da ' Commen t "0:2pp b LCS " Annotatkin : " " Sampl e Index : 2 8 Sampl e Type : Q C Concentration : 0,19 9 ng/m L Calculate dCone : 0.21 7 ng/m L Acq , Date : 7/30/:01 1 Acq . Time : 12:00:0 4 A M Modified : N o Proc , Algorithm Nois e Percentag e Base . Sub . Wind o Peak-Split . Fac t Repor t Larges t 1 Min . Pea k Heig h Min . Pea k Hidt h Smoothin g Hidt h RT Window : Expecte d RT : Us e Relativ e RT . Int . Type : Retentio n Time : Area : i Height : Star t Time : En d Time : Specif yP a

: 5 0 rf: 1.0 0 or : 1 eak : Ye s : 0.0 0 0.0 0 0 30. 0 15. 2 n N o Valle y 15. 2 1569 3 co u 9.70e*00 4 15. 1 n 15. 4 n Sampl e Type : Concentration : Calculate d Cone : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Q C 1,9 9 2.2 0 7/30/201 1 ng/m L 1:03:2 5 A

M N o Specif yParamet e 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Fac t Repor t Larges t P Min . Pea k Heigh t Min . Pea k Width : Smoothin g Width : RT Window : Us e Relativ e RT : Int . Type : Retentio n Time : Area : 6 0 Height : End Time : jr : 1

•ak : ye s

0. 0 0, 0 0 30. 0 15. 2 N o Valle y 15. 2 559 5 C O .OBetOO o 15. 1 15. 6 mi n

p o mi n
mi n cp s mi n mi n



# -^ A Dat aprinte db y ST

W Printin g Time : 9:45:1 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 7 o f 8 Pag e 3 9 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729a.rd b 

# I San ^ Nsmo : 1c11072S*034 ' Swnpl e 10:-LCS.110726- rRto : I d lOTZga.wttT PM k Name:-f>FHS * Mnt<M) : *399.00(y09.00 0 Oa,3a9.0O{V8OJlO O Da ' Comnont'TOppt , LCS ' Sampl e Index : Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e 3 4 O C 19. 9 21, 3 7/30/201 1 2:06:4 8 A

^ H o ng/m L

ng/m L
Specif y Paramet e 5 0 Base . Sub . Window : 1.0 0 Peak-Split , Fac t Repor t Larges t

P Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : 4 9 Height : Star t Time : En dTime : r : 1 a k : Ye s mi n 0.0 0 cp s 0,0 0 se c 0 30. 0 15. 2 N o Valle y 15. 2 4793 7 c .27e+00 6 15. 1 15. 6 p o

s e c mi n
mi n unt s c p s mi n mi n



# I Sampl e Name;'VI10728a05 rSampl e 10:-GLP1IM]1.02-194X12 " FUa: 1 Pea k Name:'PFHS - Uata{e«) : "399.00099.00 0 Oa,399.00(VBaO0 0 Da ' Comment-DALOWTRIP1LS1107i rAmotatkm:" ' Sampl e Index : 5 7 

# I SMi^Name:iniO729a0G5 ' San^l e ID : "OLPI04)1-02- 1 ^009 " Fie:-k110729a.Mf r P*a k Name : -pFHS " Masses) : -399.000^9.00 0 Da,399.00Q«0.00 0 Da ' Commen(:-DALGWBPMW121RS110717 - AmotaUon: - Sampl e Index : S S Sampl e Type : Concentration : Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Unknow n N/ A < 0 7/30/201 1 9:30:1 2 A

M N o Specif y P a Hois e Percentage : S O Base . Sub . Win d Peak-Split . Fa c w : 1.0 0

o r : I Repor t Larges t

Peak : Ye s Min . Pea k

Heig h Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : Us e Relativ e R

T int . Type : Retentio nTime : Area : Height : Star t Time : En dTime : : 0.0 0 0.0 0 0 30. 0 15. 2 n No Valle y 190 9 co u 6.4ee<00 2 15. 2 n 15. 3 n

1.2e 4 1.0e 4 8000.0 - G000.0 ' 4000. 0 2000. 0 0.0 - i.i^'iU'iPuMii^iiiMHiw'i^'wM** * j/\rf^ , 

# _ J

Sampl e Type : ConcentratIon : Calculate dCone : Acq . Time : Modified : Proc . Algorithm : Hois e Percentag e Unknow n H/A 0.26 8 7/30/201 1 10:12:2 7 A

M H o Specif y Par a S O Base . Sub . Window : 1.0 0 Peak-Split . Factor : 1 Repor t Larges t

P Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : a k : Ye s 0.0 0 0.0 0 0 30. 0 S t 15. 2 m N o Valle y 15. 2 m Area : 78696 5 cou n Height : Star t Time : En dTime : .25et00 5 C F 15. 1 m

: 15. 4 m l 1.25e 5 1.20e 5 1.15e 5 1.10a 5 ^JC6» 5 1.00a 5 9.50e 4 9.00e 4 S.50e 4 8.00e 4 7J0e 4
•7.00e 4 1 e.oo» 4

- 550* 4 5.00* 4 4.50e 4 4.00e 4 3.50e 4 3.00e 4 2.50a 4 2.00e 4 1.50e 4 1.00* 4 5000.0 0 0.0 0 1 5 2 2

V.f ^ 17.5 7



# 1 1 

# 1 Sampl e Name : i(110729a069 ^ Sanv)lelb:S3LP1M)1-03-l&O10 ^ Fie : Pea k Name : TFHS ' MaM(ei):-399.00a«9.000Da,399.00aQO;00 0 Da Comment : -OA LG WBPMW12 1 01107i rAnnotatkin : " • Sampl e Index : 6 9 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.017 9 ng/m L44e4
- Acq . Date : 7/30/201 1 Acq . Time : 3:25:5 6 P M 4.2*4
- 4.0e 4 s - M Q II I 3.8*4
-

3.6*4
- 3.2* 4 3.0e 4 Z8e 4 2.6e 4 2.4* 4 2 A 4 2.0B 4

1.2e4 ' 1.0e4 ' 8000. 0 6000. 0 4000.0 - 2000.0 ' Modified : Proc . Al g Nol» e Pe r Base . Su b Peak-Spl i Ye s

rithm : Specif y Window :
, Facto r Repor t Larges t

Pe a Min . Pea k Min . Pea k Smoothin g R TWindo w Height :

Width : Width : Expecte dRT : Us e Rela t Int . Typ e Rettntlo n Height : v e RT :

Time : 5 0 P a

1.0 0 3 Y 0 0 30. 0 15- 2 No anua l 15. 2 57 7 9 9 7 . letO O 0 0

0 0

0.0 ' 15.2 1 

# 1 .

•jffi>iir*tf;f'rrf*it^r*jt^ , Dat aprinte db y ST

W Printin g Time : 9:45:2 0 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 8 o f 8 Pag e 4 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729 a ext.rd b
k l 10729 a ext.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -1.33e+00 4 x'> 2 • ^ 2.33e•^00 6 x+ 1.52e•^004 ( r= 0.9998 )

2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 

### 6 0 6 5 7 0 7 5 8 5 

### 9 0 9 5 10 0 Dat a printe d b

ySTW Printing Time : 9:41:3 9 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1 Pag e 4 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729 a ext.rdb
k l 10729 a ext.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -2.44e-^00 4 x* 2 + 2.89e•^00 6 x+ 3.35e-^00 3 ( r= 0.9998 )

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

yST W Printing Time : 9:41:5 5 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1


### Pag e 4 2 of 7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729 a ext.rd b 

# r Sanv>leName:-k11O729a0ie rSwnpl e ID : "1 1 003-2&« - FUs:'V110729a.wt r Pea k Name : "PFBS - Mat«(ei) : *299.000i'80.00 0 D a ,299.000/99.00 0 Da ConwtMn t -1. 0 ng/m LF C « d I n Synth
. Wate rAnnotation : ~ Sanp L" • ' a Type : Standar d ng/m L ng/m L4.0e5 .

3.Se5
- amet«r , - M

O i n^.SeS
mi n 3'*** " 3,2e5 - se c 3-0e5
- polnt s e c 2,8e5 li n 2,6eS 2.4e5 ' 25* 5 2.0e5 ' 1.8e 5 1.6e 5 1/»e5
- 1.2e 5 1.0e 5 8.De4 ' 6.0e 4 4J>e4 ' 2.0e4 - Sample Type : Concentration : Calculate dCone : Acq . Time : Hodilled : Proc . Algorithm : Noise Percer.tag e Base . Sub . Windo ' Ptafc-Split . Fact e Repor t Larg-s t P Min . Pea k Heigh t Min . Pea k Hidth : Smoothing Hidth : R THindow : Expecte dRT; Use Relativ e RT : Int . Type : Retentio nTime : Standar d

1.0 0 1.0^ 7/29/201 1 7:*7:0 1 P M Ye a Specif y P a 5 0 r : 2 ak : ye s 0,0 0 0.0 0 0 30. 0 c 13. 7 n N o Manua l 13. 7 1 Area : 2<3101 9 cour Height : Star t Time : En dTime : .ITe-tOOS c

13. 6 R H. O n



# I Sampl e Name : •Ml0729a02 rSampl e ID : *LX»-110726- rFlle:T(1l072e».wt r Pea k Name : "PFBS * MHa{ea) : -29g.00a«ao0 0 Da.299.000/99.00 0 Da * CommenfOJIppbLCS " Annotation; - Sampl e Index : Z S 

# I Sampl e Name : I d 10729a027 " Sampl e ID : 1 1 OOS«s rFie : T d 10729a.*w r Pea k Name : *PFBS ' Maaa{ea) : -209.00(V80i>0 0 Da,299.000/99.00 0 Da ' Comment:-Metho d Btant fAnnotalkin: " ampl e Index : 2 7 Sampl e Type : Unknow n Concentration : N/A Calculate d Cone : < 0 Modified : N o Proc . Algorithm : Specif y Pari s e Percentage : 50

Mtn
. Pea k

Hidth : othin g Width : R TWindow : Expecte d RT :
Height : Star t Tim e En dTime :



# I Sampl e Name : iri10729a031 - Sampl e ID:-LCS-11072fr4 - Ne:Sd1072da.wtt r Pea k Name : -PFBS ' Maas(ee) : "299.00080.00 0 Da.299.00CV99.00 0 Da Comment : ''2pp b LCS - Annotatkin : ~ Sampl e Inde x Sample Type : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e O C 0.19 9 0,20 5 7/30/201 1 ng/m

L ng/m L 12:00:0 * A

M N o Specif y P a 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t P Kin . Pea k Heigh t Min . Pea k Width: Smoothin g Width: R THindow : Expecte dRT: ak : Yes 0.0 0 0.0 0 0 30. 0 13. 7 amet

e

c p s p o nl n Sampl e Type : Q C

Us e Relativ e RT : N o Int
. Type : Bas e T o B i Retentio n Time : 13. 9 Area : 0387 6 co i Height : 1.99e*0Q t Star t Time : 13. 6 En d Time : H. 0 Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Noise Percentag e 1.9 9

2.0 7 7/30/201 1 1:03:2 9 A M Ye s Specif y P a 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Fac t r : Z Repor t Larges t Peak : Yes Min . Pe» k Heigh t Min . Pea k Width: Smoothin g Width: R THindow : Expecte dRT : Use Relativ e RT: Retentio nTimt : 0.0 0 0.0 0 0 30. 0 s ng/m

L ng/m L

amete mlr,

p o 13. 7 mi

n N o Manua l 13. 7 n i n 8.53e.00 5 cp 3

Dat aprinte db y ST

W Printin g Time : 9:43:1 3 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 3 Pag e 4 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729 aext.rd b 

# I Sampl e Name ; 10)107298034 ^ Sampl e 10:-LCS-110726- rFlla : 1(1107293
. Pea k Name:'PFBS - Maa^ee):-299.00080,00 0 Da.299.000iS9.00 O Da ' Comment : "ZOpp b LCS - Annotation: " Sampl e Index : 3 4 Concentration : Calculate dCone : Acq , Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentag e Base . Sub . Wind o 19. 9 19. 8 7/30/201 1 2:06:( 8 A

M Ye s Specif y P a 5 0 : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R TWindow : Us e Relativ e RT : Int . Type : Retentio nTime : 0.0 0 30. 0 13. 7 H o Manua l 13. T Acta : <10301$ 0 c o Height : ng/m L ng/m L

mi n c p 3 p o ni n
nii i .19e*00 6 cp s

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

# I Sampl e Name : 1(1107298061 ' SaR^ID:-GLi>1M)1-02-19O05 - Fle:1c1l0728a.wH r Pea k Name : -pfBS rMa««(ea) : •SasjOOOOOOO O Da.299.OOaiS9.00 0 Da ' Comment : 'DA LG WBPMW4 7 011071 T Sampl e Index : fil Sampl e Typ e ConcentraC I Unknow n

an : N/ A Calculate dCone : 0.19 0 Acq . Date : Acq . Time : Modified : Proc . Algo r Nois e Perc e Base . Sub . Peak-Split . 7/30/20 1 11:36:5 7 No thm : Specif y tage : SO ng/m L

A M Parameter s Window : 1.0 0 mi n Factor : 2 Repor t Larges t

PeaK : V e Min . Pea k

K iqht : 0 . 0 CDS Min . Pea k

Width : 0.0 0 se c Smoothin g Width ! 0 R TWindow : Expecte dR

T Us e Rtlatl v Retentio nT Area : Height : Star t Time : 30. 0

13. 7 RT : H o Valle y me : 13. 7 45905 5 c 7,68e*00 4 13, 5 M Q II I

mi n

unt s c p s mi n



# I Sampl e Name : idlO729a01C rSampl e ID:-1 1 003-2&« ' Flto:1ri10729a,wi r Pea k Name : 'PFHS ' Uaaa{e«) : -399.00(Vd9.00 0 Da.399.00(V80.00 0 Oa ' Commen t '1. 0 ng/m LF C ctd i n Synth
. Wate rAnnotatk>n : " Sampl e Index : 1 6 Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hols e Percentag e 1.0 0 7/:9/201 1 7:47:0 1 P

M N o ng/m L

ng/m L
Specif y Paramet e 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ye s Hin . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R THindow : Expecte dRT : lis c Relativ e RT : Int . Type : Retentio nTime : O.O C O.O C 0 30. 0 15. 2 H o Valle y 15. 2 Area : 282935 3 co u Height : Star t Time : En dTime : .81e>00 5 15. 1 15. 5 mi n

p o mi n

cp s li n Bi n 

# I Sarrfil e Name : 1t110729a02 rSampl e ID : "1 1 OOS- S Pea k Name : TFHS - Mat«{es}:-399,000/9 9 JU O D a ,3 1 Comment:-Metho d BtanK" AnnotaUon:' - Sampl e Index ; 2 7 Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Hois e Percentag e H/ A 0.002 H ng/ m 7/29/201 1 11:39:0 0 P

M H o Specif y Parame t 5 0 Base . Sub . Hindow : 1.0 0 mi n Peak-Split . Fac t s r : 2 Rei>or t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : Height : Star t Time : En dTime : 0.0 0 c p 0.0 0 s e 0 p , 30. 0 se c 15, 2 mi n No Bas e T o Bas e 15. 2 mi n 951 6 count s .lle+00 3 cp s 15. 2 mi n 15. 1 mi n

WJ O 16 3 17. 0 17. 5 Dat aprinte db y ST

W Printin g Time : 9:43:1 3 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 2 o f 3 Pag e 4 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0729 aext.rd b 

# I Sanv>leName:1c110729a02e^ Sampl e ID:-LCS-11072S- rRla:1c110729a.vrtr r Pea k Name : -PFHS - Mae*<e») : -390.00099.00 0 Da,399.00a«0.00 0 Da Commen t -0.2pp b LCS " Annotatkm: " Sampl e Indei; : 2 6 Sampl e Type : O C Concentration : 0.19 9 ng/m L Calculate d Cone : 0.21 3 ng/m L Acq
. Date : 7/30/201 1 Acq
. Time : 1Z:00:0 ( A M Modified : Proc . Algo r Nois e Perce : thm : Base . Sub . Wlnd o Peak-Split . Fac t Ye s Specif y 5 0 P

- ; 1.0 0 3r : 2 Repor t Larges t

Peak : Ye s Min . Pea k

H . Min . Pea k

H Smoothin g H R TWindow : Expecte dR

T Us e Relativ t Int . Type : Retentio nT Area : Height : Star t Time : En dTime : Igh t

dth : dth : HT :
S 0

0 0 30. 0 15. 2 H o Manua l 15. 2 646 2 9,70etO O 15. 1 15. 4 aramet e

0 0 cp s 0 0 se e p o mi n
mi n n t s mi n mi n



# I Sampl e Name : 1(110729a034 - Sampl e ID:-LCS-110726-7 - Rle:1(110729a.wt r Pea k Name : "PFHS " MaM(ea) : -399.00039.00 0 Oa,399.00080.00 0 Da Commen t -20pp b LCS ' Annotatkin : " Sampl e Index : 3 4 

# I SampleName:1(110729a03 rSampl e ID:ICS- l 10726- rFle:1c110729a.wt r Pea k Name : TFHS ' Maea<aa) ; -399.000/98.00 0 Da,399.00O80X0 0 Oa ' Commenl : -2pp b LCS ' Annotatkm ; " Sampl e Index : 3 1 Sampl e Type : Q C Concentration ; 1.9 9 ng/m L Calculate d Cone : 2.1 2 ng/m L1.05e6 ' Acq
. Date : 7/30/201 1 1.00e6 ' g.50e 5 » - M Q 11 1 aooe s

8,S0e 5 8.00eS ' I t s 7.50e 5

7.00e5 ' 6,50e5 j6.00e5 . i 530e 5 I5X0e 5 4,50e 5 4,0OeS ' 3.50e5 ' 3.00e5 - 2.S0e 5 2.00e5
- 150e5
- 1.00e5 - 5.00»4 ' 0.00 - Acq , Time : Modified : Proc . Algorithm : Hois e Percentag e 1:03:2 9 A M Ye s Specif y P a 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

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Area : 6 0 Height ; Stai t Time : En dTiwe : 0.0 0 0.0 0 0 30. 0 15. 2 H o Manua l 15. 2 1 5B3 7 co u .08e+00 6 15, 1 n 15. 5 n



# A

Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Pioc . Algorithm : Nois e Percentag e I S 2 1 7/30 / 2:06 : Y e Spec i Base . Sub . Window : Peak-Split . Fac t r : Repor t Larges t

Peak : Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R THindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 30 . 1 5 N o Manu 1 5 Area : 4974560 1 Height : Star t Time : En dTime : .27e + 1 5 1 5 t> c 9 0 ng/m L ng/m L -Oi l a Y •. 0



### . ? 0 0 0 1 2

a l 7 0 1 6 A M Paramet e

0 0 cp s 0 0 se c s e c mi n
mi n mi n mi n 

# I San^Name:1c110729a061 " Sartvi|elD:-OLPlCK)1-O2-1&O05 ' Fla: ' Pea k Name : TFHS ' Mats{e(} : -399.00ar99.00 0 Da,399.000/80J>0 0 Oa ' Comment:-DALGWBPMVM701107i rAnnotatton: - Sampl e Index : 6 1 5.4e4 - 5.2a4 - 5.0*4 - 4.Se4 - 4.6*4 - 4.4e4 - 4.2e4 - 4.0e4 - 3.8e4 - 3.6e4 - 3.4e4 - 3,2e4 - 3.0e4 - Sampl e Type : Concentration : Calculate dCon e Acq , Date : Acq . Time : Modified : Proc . Algorith m Nois e Percentag e Unknow n H/ A 0.13 9 ng/m L 7/30/201 1 11:36:5 7 A

M Ye s Specif y Paramet e Base . Sub . Window : 1.0 0 mi n Peak-Split . Fa c o r : 2 Reiioc t Larges t

Peak : Ye s Min . Pea k

Heig h Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Area : Height : Star t Time : En dTime : : 0.0 0 cp s 0.0 0 se c 0 p o 30. 0 se c 15, 2 mi n No Manua l 15. 2 roln 0316 1 count s 5.52e*00 4 cp s 15. 0 mi n 15. Jmi n

6000.0
- 6000. 0 4000. 0 2000. 0 0. 0 15. 1 K 

# J L ryf^^-N^^^T*-:^ ^ Dat aprinte db y ST

W Printing Time : 9:43:1 3 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 3 o f 3 Pag e 4 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b



# 1 C O 

# 1
( 0 2 7 J 26 - 25 - 24 - 23 - 22 - 2 1 20 - 19 - 18 - 17 - 1 6 15 - 14 - 13 - 12 - 11 - 10 - 9 - 8 - 7 - 6 - 5 - 4 - 3 - 2 - 1 - 0 - 1 2 1 4 Analyt e Cone
. /

I S Gone
. Dat a printe d b

yST W Printing Time : 9:45:5 2 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1 Pag e 4 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b 

# I San^Name:Tc110802«01 F Simpt o IDi'l l OOMW fFfc : Tel l 0802a
. wt T PwikNanM:'13CBPFOS-IS0S) - MH(m):-507.000v80.00 0 Da ' Coramsn t "I.OnB/m LF= C tt d I n Synth
. VWn rAmotaUon: "
O.Se 4 9.0o 4 8,5e 4 8,06 4 7,5e 4 Calculate dCone : Acq . Date : Acq , Time : Modified : Proc , Algorithm : Min . Pea k

Heigh t Mtn . Pea k

Hidth : Smoothin g Hidth : R TWindow : tlxpecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : N/ A 8/2/201 1 8:38:2 6 P

M N o IntelllOu a 0.0 0 0.0 0 0 p

< 30. 0 16. 2 N o Valle y 16. 2 1 Area : 61390 0 co u Height : Star t Time : En dTime : 9,77e+00 4 15. 1 1 16. 5 r 7.0 g

4.5« 4 4.0e4 ' 3.5»4' 3.0 M 2.Se4 ' 2.0* 4 1.5* 4 1.0»4

16. 0 1& S 

# I Sampl e Name:'k110B02«025 - Sanqd a IO:-LCS-110726>1 - FUe:1(110802a.Mi« r pHkNarM:-13CSPFO&4S0S) ' MaM(M):"507.OOtkfSO.OOODa Comment-0,2pp b LCS * AnnotatlMi: - Sampl e Index : 2 6 I Svnpt e Name : nc l 10802*024 - Sampl e 10 : "1 1 005-129 - FUe:-k110802«
. I Pea k Name:'13CSPFOS4S{IS} - U«u(tta):-507.00080^)0 0 Da ' I Comment:-Metho d Btani rAmotatkm: - Sampl e Type : Concentration : Calculate dCon e Acq . Date : Acq , Time : Modified : Proc , Algorith m Min . Pea k

Heig h Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : l's e Relativ e R

T Int . Type : Retentio nTime : Unknow n 0.96 0 ng/m L N/ A a/2/201 1 11:27:1 4 P

M r e s IntelllQua n- IQA1 1 : 0.0 0 cp s 0 point s 30. 0 se c 16. 2 mi n No Bas e T o Bas e 16. 2 mi n Area : &5570 9 count s Height : Star t Time : En dTime : ].5<BtO0 5 cp s IS. l mi n 16. 1 mi n 

### i



## f * 1.4* 5

1.2* 5 1.1* 5 1.0e 5

a.0e 4 7.0* 4 6.0* 4

3,0e 4 2.0e 4 

# I Sampl e Name : 1(110802*028 - Sampl e ID:'LCS-11072&4 ' Fle: 1 Pea k Name:-13C8PFOS-IS(IS) - M«««(e*):-507,0Oai'8O.00 O Da Commen t •2pp b LCS - Annotatfan: - Sampl e Index : 2 9 1.15* 5 I.IOe S 1.05e 5 I.OOeS ' S.50e4 9.00* 4 8.50* 4 8,00* 4 7.50* 4 7.00* 4 6.50e4 ' 6.00* 4 S.SO M 5.00* 4 4.50* 4 4.00* 4 3.50* 4 • 3.00*4 ' 2.50*4 - 2.00*4 - 1.S0e4 ' Sampl e Type : Concentration : Acq . Date : Acq . Time : Modided : Proc . Algorith m Min . Fea k

Heig h Min . Pea k

Hidt h R THindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Area : Height : Star t Time : En dTime ; Q C 0.9S 3 ng/m L N/ A e/2/:oi i 11:16:1 8 P

M N o IntelllQua n- ; 0,0 0 cp s 0.0 0 se c 30. 0 se c 16. 2 mi n Valle y 16. 2 mi n 1.15e*00 S cp s 16. 4 mi n IQAI I



## ! 1.15* 5 1.10* 5 1.05* 5 1J»* 5

8.50» t 8.00* 4 7.50* 4
6.50* 4 6.00* 4 5.50 M 5.00* 4 4,50* 4 4,00* 4 3,50* 4 3J»* 4 2.50 M 2.00* 4 IJO M 1.00* 4 5ooao o 0.0 0 J Sampl e Type : Concentration : Calculate dCon e Acq . Time r Modified : Proc , Algorith m Min . Pea k

Helgh i Min . Pea k

Widt h Smoothin g Widt h R TWindow : E:tpecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Q C 0.95 3 N/ A 8/3/201 1 12:51:1 6 H o A

M IntelllQua n- : 0.0 0 0.0 0 0 30. 0 No Valle y 16. 2 cp s poi n

mi n Acea : 71279 2 count s Height : Star t Time : En dTime : i.ieetoo s 16. 1 16. 4 c p s mi n

16. 0 16. 3 1.00*4 - 5000.0 0 0.0 0 16. 0 16. 5 Tim* , mt n Dat aprinte db y ST

W Printing Time : 9:47:2 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 6 Pag e 4 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS
. PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b

I San<)l e Name : 1(110802*031 - S«mplelD:'LCS-110726- rRo : Te l 10802a.w« r I PaakNama:-13C8PFOS-IS0S> - MaM(««) : "507.000/80.00 0 Da ' I Convnen t '20pp b LCS '

ntelllQua . 0.0 0 I 0.0 0 ! Acq , Time :
Mi n Pea k

Heigh t Min , Pea k

Width : Smoothin g Hidth : Expecte d RT : Us e Relativ e RT : Int , Type :

14. 0 14. 5 

# I Sampl e Name : 1(1108028041 - Sampl e ID : •LCS-110726-13 " Rte : I d 10802a.wlf T Pea k Nam* : -13CSPFOS-IS<IS> - Ma**{e*} : -SO7.00a'80.O0O Da ' Conment-2pp b LC S EC P Annotation: " Sampl e Index : 4 2

se : Q

C 1^. 5 16. 0 16 5 Time , mi n 

# I Sampl * Name : 1(110802a03ff ' Sampl * ID : TCS-110726-10 ^ Rto : Ic l 10802*.wM T Pea k Name:'1X:8PFOS-IS(t5> - Ma««{es):-S07.00(V80M) 0 Da Comment:-0.2pp b LC S EC P AnooteUon: - Sampl e Indent : 3 9 Sampl e Type : Q C Concentration : 0.95 3 ng/m L Calculate dCone : H/A Acq . Date : 8/3/201 1 Acq , Time : 4:22:1 9 A M Modified : Proc . Algo r Min . Pea k

H e Min . Pea k

W thm : ight : dth : Smoothin g Width : R TWindow : Expecte dR

T L's e Relativ e Int . Type : Retentio nT Area : Height : Star t Time : En dTime : RT :

6 2 9 Ye s ntelliOua n 0.0 0 c 0.0 0 s 0 p o 30. 0 s 16. 2 m No Valle y 16. 2 m 36 0 cou n 66e*00 4 c 16. 1 m

Swnpl e Name : 1c110802a044 - Sampl e ID : 1.CS-110726-16 " Fle:1<110802a.»« r Pea k Name : '13C8PFOS-IS(IS)' ' Ma*s(e*) : -507.00Q'80.00 0 Da ' Comment : "20pp b LC S EC P Annotation: - Sampl e Index : 4 5 1.10*5
- 1.06*5
- 1.00e5
- 0.50e4
- 9.00e4
- 8,50e4 ' 8.00*4 ' 7.50e 4 7.00e 4 6.50e 4 \6.00* 4 I5.50e4 '

= 5.00*4
- 4.50*4
- 4.00*4
- 3.50*4 ' 3.00* 4 2.50* 4 2.00*4
- 1.50* 4 1.00e 4 5000.00 ' 0.0 0 Sampl e Type : Concentration : Acq . Time : Modified : Proc . Algorith m Min . Pea k

Heig h Min . Pea k

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

T Int . Type : Retentio nTime : Area : s Height : Star t Time : En dTime : Q C 0.95 4 H/A e/3/201 1 5:26:1 1 A

f Ye s IntelliQ u : 0,0 0 0.0 0 0 30. 0 16. 2 N o Valle y 16, 2 3962 8 C

O 1.08e+00 5 15. 1 16. 4 Sampl e Type : Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Min . Pea k

Heigh r Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Q C 0.95 3 n g H/A a/3/201 1 6:29:3 0 A

K Ye s IntelllQua n- : 0.0 0 cp s 0.0 0 se c 0 poi n 30. 0 se c 16. 2 mi n H o Eas e T o Bas e 16. 2 mi n

15. 5 16. 0 16, 5 16, 0 18 5 "nine , mt n Dat aprinte db y ST

W Printin g Time : 9:47:2 9 A M Printin g Date : Thursday , Augus t 25 , Pag e 2 o f 6 Pag e 4 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b 

# 1 Sampl a Name : Ir110802a05 rSampl e ID:-GLP 1 (Ml-02- 1 » • Pea k Name : *13C8PFOS-IS(ls rM*t^**) : *507.00(V80.00 0 Da * Comm*nt:-DALGUVBPUVV121RS110713 - AnnotBtton: - Sampl e Inde>: : 5 3 Sampl e Type : Unknow n ng/m L Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Min . Pea k

Heigh t Min . Pea k

Midth : Smoothin g Hidth : R THindow : Expecte dRT : Us e Relativ e RT : N/ A e/3/20 1 9:18:2 5 A

M Ye s IntelllQua n- 0,0 0 cp s 0 poin t 30. 0 se c 15. 2 mi n H o Int . Type : Bas e T o Retentio nTime : 16. 1 Area : 101736 8 c Height : 1.64e*00 5 Star t Time : 16. 0 En dTime : 13. 4 Bas e mi n ount s cp s mi n mil l IQAI I



### ^ 

## 1 1.6* 5 1.5* 5 1.4* 5 1.3* 5 1.2e 5 1.1* 5 1.0e 5 8.0e 4 8.0 M 7.0* 4 6.0* 4 5.0* 4 4.0 M

14. 0 14. 5 

# I

^?J ^ Sanpl e Name : V t 10802*066: ' Sampl a ID:-OLP1&O1-02-1&«1ff ' Fite:1c110802«.vi4 r Pea k Name:-13C8PFOS-IS(IS) - Ma««(e*):-507.00CV8aoa Q Da ' CoiT¥nefll:'DALOVUBPMVV12101107i rAnnotatkm: - Sampl e Index : 6 7

: lir.know n ng/m L 00 5 

# I Sanv4aName : 1(110802*054 - SamplelD:'OLP1(M>1-02.1&O0 rFle:-V110802a.Mti r Pea k Nam*:-13C8PFOS-IS(tS) " M«**(**):-507.00080.00 0 Da Comment:-DA LGWTRIP I L S 110713 " Annotation; - Sampl e Index : 5 5 Sampl e Type : Unknow n Concentration : 0.96 0 ng/Ri L Calculate d Cone : N/A, Acq - Date : 8/3/201 1 l.'eo- ] Acq
. Time : 10:00:3 9 A M 1.6*5
-

1.5*5 - 1.4*5
- 1.3* 5 1.2*5 - 1.1*5 - 1.0*5 - ao*4
- 8.0*4 - 7,0*4 - 6.0*4 - 5,0*4 - 4.0*4 - 3.0*4 - 2.0* 4 1.0*4 - Kin . Pea k

Height : Min . Pea k

Width : 0 Smoothin g Width : 0 R TWindow : 3 0 Expecte dRT : 1 Us e Relativ e RT : H Int . Type : Va l Retentio nTime : I Area : 114462 2 Height : 1.77 e Star t Time : 16. 0 En dTime : 16, J

UJ O 14, 5

Sampl e Type : Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Min . Pea k

Heigh ' Hin . Pea k

Hidt h Smoochin g Widt h R TWindow ; Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : Ur-know n 0.96 0 H/ A 8/3/201 1 2:14:0 9 P

H Ye s IntelllQu a : 0.0 0 0.0 0 30. 0 lS- 2 n N o Valle y 16. 2 n Area : 45021 5 cou r Height : Star t Time : En dTime : 7,93e't00 4 c la. l 1 16, 4 n 

# I &leName:1[110802aOie rSampl e ID : 1 1 00»-25'« - hle:Sc110802*!«tf r Pea k Name : TFOS - Ma«*(es) : -499.000i«9,00 0 Da,4a9.00aB0.0O O Oa,4S9.00CV130.000 Da ' Comment:-l.OnB/mLFC«tdln5ynth.Water - Annotation: - Sampl e Index : 1 7 1.15e5
- 1.10*5
- 1.05e5
- 1.00e5
- 9.50e4 ' 9.00e 4 8,50*4
- aXKM
7,50*4
- 7.00* 4

^ 6.00*4 - I 5.50*4 - 5.00* 4 4.50*4 - 4.00*4 - 3.50*4 - 3.00*4 - 2.50*4 - 2.00*4 - 1.50*4 - 1.00*4 - 5000.00 - 0.00 - Sampl e Type : Concentration : Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Hois e Percentag e Base . Sub . Hind o Peak-Split , Fa c Reiior t Larges t

1 Kin . Pea k

Heigh ' Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Standar d 1,0 0 r.g/m L 1.0 9 ng/m L 8/2/201 1 8:38:2 6 P

M H o Specif y Paramet e : 5 0 rf: 1.0 0 mi n o t : 2 eak : Ye a : 0.0 0 cp s 0.0 0 se c 0 p o 30. 0 se c 16. 3 mi n N o Valle y 16. 2 Bi n Area : 77976 5 count s Height : Star t Time : En dTim? : l,ne»00 5 cp s 16. 1 mi n 16. ) mi n

Dat aprinte db y ST

W Printin g Time : 9:47:2 9 ftM Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 3 o f 6 Pag e 4 9 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b

I S«m|)l e Nama:-k11D802a024 - Sunpt e ID:-1 1 005-129 - Fie : I d 10902a.wW } PukNanw:-PFOS - MM*<M):-499.00Q/99.000Oa.499.000/8O.00ODa.499.0(NV13O.00OOa I Coimont-MethodBbnK - Annotation: - Sampl e Type : Concentration : Calculate dCone : Acq . Dste : Acq . Time : Mod i Iled : Ptoc , Algorithm : Hois e percentag e Unknow n N/ A 0.0054 0 e/2/201 1 11:27:1 4 Ye s Specif y ng/m L

P M Paramet e Base . Sub . Window : 1.0 0 mi n Peak-Split . Fac t Repor t Larges t

P Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 3 r : 2 a k : Ye 0 . 0 . 0 30. 0 16. 3 H o Manua l 16. 2 Area : 2256 6 c Height : Star t Time : En dTime : .30e*00 ' 15. 0 15. 3 ) 0 cp s > 0 se c mi n

c p s mi n mi n



# I SampleName:1<110802a(n8 " Sampl e ID : "LCS-11072&4 - File : 1(110802*.»* r P«« k Name : -PFOS ' Mas«<e«) : '439.000^.00 0 Da,499.00a/80.00 0 Oa,499,00CV130.00 0 Da Commen t "2pp b LCS " Anrwtatlon : ~ Sampl e Index : 

# I Sampl e Name : 1(110802*025- Sampl e ID:-LCS-110726- rFle:1c1100a2a.wH r Pea k Nam* ; -pFOS - Mat«(e*) : *499.O0Q'g9.O0O D a .499.000/80.00 0 Da .499iXXV130.00 0 Da ' Comment : *0.2pp b LCS - Annotabon : ~ Sampl e Type : Concentration : Calculate dCon e Acq
- Date : Acq . Time : Modified : Pcoc . Algorith m Q C 0.19 9 ng/m L 0.21 9 ng/m L 8/2/201 1 11:18:1 8 P

M No Specif y Parameter s - M Q II I Nola e Percentage : 5 0 Base . Sub . Win d Peak-Split . Fa c w : 1.0 0 mi n

o t : 2 Repor t Larges t

Peak : Ye s Min . Pea k

Heig h Min . Pea k

Widt h Smoothin g Widt h R TWindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Area : Height : : 0.0 0 cp s 0.0 0 se c 0 point s 30. 0 se e 16. 3 iDi n No Valle y 16. 2 mi n 7953 2 count s 2.93e-t00 4 cp s ft P 2.8* 4 2.6* 4

1.8* 4

4000. 0 2000. 0 

# I Sampl e Name : 1(1108O2aO3 rSampl e ID : TCS-110726- rFB«:1c110e02a.wtf r Pea k Name : -PFCS - Ma««(**) : -498.000/98.00 0 08.499.000^0.00 0 Da,499.0oa'130.00 0 Da ' Comment-20pp b LCS ' Annotation :

" e Type : Q C .g/ri L Sampl e Type : Q C Concentration : Calculate dCone : Acq , Date : Acq . Time : Modilled : Proc , Algorithm : Nois o Percentag e 1.9 9 2.1 5 8/3/201 1 12:51:4 5 N o Specif y P 5 0 Base . Sub . Window : l.O C Peak-Split . Fac t r : 2 Repor t Larges t

Peak : Ye a Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R THindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTims : ng/m L ng/m L A M
aramet e mi n 0.0 0 cp s 0.0 0 se c 0 30. 0 16. 3 N o Valle y 16. 2 Area : 176924 7 C O Height : Star t Tine : En dTime : .eOo-fOO S 16, 1 15. 4 mi n

unt s c p s Bi n mi n 2.7* 5 2.Ge 5 23* 5 2.4* 5 2.3«5 - 2J*5 - 2.1*5 - 2.0e5 < 1,9*5 - 1Ae5 - 1.7* 5 1,6*5 - 15*5 - 1.4*5 - 1.3*5 - 1.2*5 - 1.1*5 - 1.0*5 - 9.0M 8.0*4 - 7.0*4 - 6.0e4 - 5.0*4 - 4.0e4 - 3.0*4 - 2.0*4 - 1.0*4 - Sampl e Type : Concentration : Calculate dCone : Acq , Date : Acq , Time : Modified : Ptoc , Algorithm : Nois e Percentag e Q C 19. 9 21. 1 8/3/201 1 1:51:5 8 A

M No Specif y P a 5 0 Base . Sub . window : 1.0 0 Peak-Split . Fac t Rejjor t Larges t

P Min . Pea k

Heigh t Min . Pea k

Width : Smoisthin g Width : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : a r : 2 :ak : Ye s 0.0 0 0.0 0 0 No Valle y 16. 2 1 Area : 2257028 4 c o Height : Star t Tine : En dTime : .I9e-f00 5 c 16. 1 n IS. 5 E - M Q 11 1



### = 

# t 1 3.4* 6 3.2* 6 3.0* 6 2.8* 6 2,6* 6 2.4* 6 2,2* 6 2.0* 6 1.8* 6 1.6* 6 1.4* 6 1.2* 6 1.0* 6 8.0* 5 6.0* 5

15. 5 16. 0 16 5 17. 0 17, 5 16. 0 18 J Dat a printe d b

yST W Printing Time : 9:47:2 9 A M Printin g Date : Thursday , Augus t 25 , Pag e 4 o f 6 Pag e 5 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 *ETS-Kir k Result s Name : kll0802a.rd b

TSampl * Name : 1<110802a038fSampl e ID:-LCS-110726-10 ' Fl* : 1c110802a.v«fl r I Pea k Name:-PFOS - Ma*s(e«):-499.00(V99.000Da.499.00ai'BO.OOODa.499.000/13aooODa I Commen t ^.2pp b LC S EC F AmotaUon : " Sampl e Inde>: : 3 9 Sampl e Type : Q C Concentration : 0.19 8 ng/m L Calculate d Cone : 0,25 2 ng/m L Acq
. Date : 8/3/201 1 Acq
. Tlnre : 1:22:4 9 A M Proc . Algorithm : Specif y Parameter s - M Q II I Hols e Percentage : 5 0 Base , Sub
. Hindow : 1.0 0 mi n Repor t Larges t

Peak : Min . Pea k

Height : Min . Pea k

VJidth : Smoothin g Vlldth : R TWindow : 3 0 Expecte dRT : 1 Vif, Relativ e RT : N Int . Type : Ma n Retentio nTime : 1 Area : 18460 9 Height : l,e6 e Ye s 0,0 0 0,0 0 0 0

, 3

a l

. 2 00 4



# I Sampl e Name : 1(110802aO44 - Sampl e ID:*LCS-110726-16^ Fl*:1(110e02«.vii r P«a k Name : -PFOS ' Mat«(e«) : -4a9.00(V&9.00 0 Da,499.00af80.00 0 Da,499.000/130.00 0 Da Comment-20pp b LC S EC P Annotatkm:' ^ Sampl e Index : 1 5 Sampl e Type : Q C Concentration : 19. 8 ng/m L Calculate dCone : 23. 0 ng/m L Acq . Date : 8/3/201 1 Acq . Time : 6:29:3 0 A M I Sampl e Nam* : VI10802a041 - Sampl e ID : 1.CS-110726- 1 rFie : 1(110802a.MM T Pee k Name : TFOS - MM«(**):-499J10ai99.000Da.499.00aQaOOOD*,499.00a/130.000Da ' I Commw * •2pp b LC S ECF - Annolatkxi: "

1.5* 5 1.4* 5 1.3*5
- 1,2*5
- 1,1* 5 1.0*5
- 9.0*4
- 8.0*4
- 7.0*4
- Sampl e Index : 1 2 Sampl e Type : O C Concentration : 1.9 8 Calculate dCone : 2.2 9 Acq . Date : 8/3/201 1 Acq . Time : 5:26:1 1 A M Modified : Ye s Proc . Algorithm : Specif y Pa r Nois e Percentage : 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak : Ve s Min . Pea k

Height : 0.0 0 Mtn . Pea k

Width : 0.0 0 Smoothin g Width : 0 R TWindow : 30. 0 s Expecte dRT : 16. 3 m Us e Relativ e RT : N o Int . Type : Manua l Retentio nTime : 16. 2 m Area : 162099 5 cou n Height : 1.74e*00 5 c iq/m L ig/m L

mi n c p s s e c p o i n
i n p s

UJ O u s 15. 5 16J ) 16, 5 1^ 0 17 5 18. 0 18. 5

Modified : Ye s Proc , Algorithm : Specif y Par ;

itags : 5 0 Bas t lindo h Peak-Spl i Repor t Larges t

Peak : Min . Pea k

Height : Min . Pea k

Hidth : Smoothin g Hidth : R THindov : 30, 0 Expecte dRT : L's e Relativ e RT : N i Int . Type : Ma m 6. 3

1735557 8 count s 1.70e*0O 6 cp s 15, e mi n 15. 5 mi n 1.7* 6 1.6*6
- 1,Se 6 1,4* 6 1.3*8
- 1.2* 6 1.1*6
- 1.0*6
- 9.0*5
- 8.0*5
- 7.0*5
- 6.0*5
- 5.0*5
- 4J)eS
3.0e5
- 2.0*5
- 

# I SarMiNamaTvTlMC ^ P«a k Nam* : -PFOS ' MMs(es) : -499.000/99.00 0 Da,499.00QnO.OOO O a ,499.000^30.00 0 Da Comment*DALOWBPIyIW12 1 RS1107i rArmotafion: " Sampl e Index : 5 3 Sampl e Type : N/ A Calculate dCone : Acq . Date : Acq . Time: . Modified : Proc , Algorithm : Nois e Percentag e Base . Sub . Wind c Peak-Split . Fac t < - 0 8/3/20 1 9:18:2 5 Ye s Specif y 5 0 A M Parame t i : 1.0 0 mi n o r : 2 Retor t Larges t

Peak : Y Min . Pea k

Heigh t Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Va nRelativ e RT : Retentio nTime : Area : Height : Star t Time : En dTime : 0 D 0 30. 0 16. 3 N o Manua l 16. 0 726 5 l.66e*0 0 15, 9 16. 2 0 0 c p 0 0 s e P " s e c mi n
mi n mi n mi n 280 0

15. 0 15 3 18. 0 16 5 17. 0 17. 5 18. 0 18 5 Dat aprinte db y ST

W Printing Time : 9:47:2 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 5 o f 6 Pag e 5 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802a.rd b

Name:1(110802a054 " Swnpl B ID:"QIP1(W)1-02-1W>02 - File: ! P»a k Nam* : 'PFOS ' hU«»(a«) : '439.00099.00 0 Da,499.000fSO.OO O Da.4S Coimwnt-DALGWTRIPIL S 11071 7 Arvwtalion : " " Sampl e Index : 5 5 5.0*4 - 4.8*4 - 4.0*4 - 4.4*4 - 4.2*4 - 4.0*4 - 3.8*4 - 3.6e4 - 3.4*4 - 3.2*4 - 3.0*4 - 2,8*4 - 2,6*4 - 2,4*4 - 2.2*4 - 2,0*4 - 1J*4 - 1,6*4 1 Sampl e Type : Concentration : Calculate dCon e Acq . Date : Acq . Time : Modified : Proc . Algorith m Hois e Porcentag r Base . Sub . Hind o Peak-Split . Fa c Repor t Larges t

1 Min . Pea k

Heig h Min . Pea k

Hidt h Smoothin g Widt h K TWindow : Expecte dRT : Us e Relativ e R

T Int . Type : Retentio nTime : Unknow n 0.25 5 ng/m L 8/3/201 1 10:00:3 9 A

M N o Specif y Paramet e : 5 0 >< : 1.0 0 mi n o r : 2 eak : Ye s

0.0 0 cp s 0.0 0 fe e 0 p o 30. 0 se c IS. 3 mi n N o Valle y 15. 2 mi n Area : 33915 0 count s Height : Star t Time : En dTime : 5.13e-f00 4 cp s 1&- 1 mi n 15. 3 mi n

4000.0 - 2000.0 - ..-T««ilDM t Sampl e Name : 1(110e02a066 rSampl e ID : ^3LP1OO1-02-1&O10 ' n*:-k1108D2a.wifr r P*a k Name : TFOS ' M«**(**) ; '499.00098.00 0 D«,499.000/BO.OO O D*.499.000/130.00 0 D* - Commeot:*DALGVWBPUWt2 1 0110713 ^ Awiotatton: - Sampl e Index : 6 7 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.023 7 ng/m L Acq . Date : 6/3/201 1 Acq . Time : 2:11:0 9 P M
Percenta l ;ub . Min t 5 0 Nols
. Bas e Peak-Split . Factor : Repor t Larges t

Pea k Min . Pea k

Height : Min . Pea k

Hidth : Smoothin g Width : R TWindow : 30. 0 Expecte dRT : 16. 3 0.0 0 cp s 0.0 0 se e

; Rela l Int . Tvpe : Retentio n1 . RT : No 16. 2 1965 5 . 280 0 260 0 2400
- 220 0 200 0 180 0 I1600
- 

## f I 140 0 1200 '

14. 0 14. 5 15. 0 I I

Dat aprinte db y ST

W Printin g Time : 9:47:2 9 A M Printin g Date : Thursday , Augus t 25 , 201 1 Pag e 6 o f 6 Pag e 5 2 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802 a ext.rd b
k l 10802 a ext.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= 4.17e-H003 x^ a - ^ 9.02e-H00

5 x- K-4.02e-H004 ( r= 0.9972 )



### 9. 0 10. 0 11. 0 12. 0 13. 0 14. 0 15. 0 16. 0 17. 0 18. 0 19. 0 20. 0 21. 0 22. 0 23. 0 24. 0 25. 0

Concentration , ng/m L Dat a printe d b

yST W Printing Time : 9:48:2 3 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 1 o f 1 Pag e 5 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 *ETS-Kir k Result s Name : kll0802 aext.rd b 

# I Singl e Name : 1(110e02aOie rSampl e ID : "1 1 003^5 ^ FUe:*V110802a.<Mr r PM k Name : 'PFOS ' Mna(et) : "499.000/99.00 0 Da,499.00(VSO.OO 0 Da,499.000^30.00 0 Da ' Connen t '1. 0 ng/m LF C tt d I n Synlh
. VMa TAnnotation : ~ Sampl e Index : 1 7 Sampl e Type : Standar d 

## - ^^^ ^ 1.10eS< 1.05* 5 I " 1.00e5 -

9.50 M 9.00 M e.50M ' 8.00* 4 7.50M 7.00*4 - 

### I »^ - ^ 6.00*4 - I 5.50*4 - 5.00* 4 4.50*4 < 4.00* 4 3.5064 - 3.00* 4 2.50 M 2.00 M 1J0* 4 1.00* 4 5000.0 0 0.0 0 Concftntration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc , Algorithm : Kois e Percentag e 1.0 0 0.90 6 8/2/20 1 8:38:2 6 N o Specif y S O ng/m L ng/m L P M Pacamet e Base . Sub . Vllndow : 1.0 0 mi n Pealt~split . Tact- : Repot t Larges t

P « Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R THindow : Expecte dRT : Us e Relativ e RT : int . Type : Retentio nTime : i : 2 a t : Y

e 0 30. 0 16. 3 N o Valle y 16. 2 Area : 77976 5 c Height : Star t Time : En dTime : .176*00 5 16. 1 16. 4 0 0 cp s 3 0 se c s e c mi n
mi n mi n mi n

14. 0 14 5 

# I Sampt e Name : 1(110802*024 ' S«mpt o 10:1 1 005-129 - File : TcllOaoaa.wtf r Pea k H«me : TFOS " Ma*s(a«) : -499.000/99.00 0 Da,499.000^0.00 0 Da,499.000/130.00 0 Da ' Commenl:-Metho d Btam rAnnotation: " Sampl e Index : 2 5 Sampl e Type : Unknow n Concentration : H/ A Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Nois e Percentage : Base
- Sub . Hindo * Peah-Spllt . Fact o 0.068 7 i/2/20 1 11:27: H Ye s Specif y 5 0 P M Pa r 1.0 0 i : 2 Repor t Larges t

Peak : Y

e Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 0 0 0 30. 0 16. 3 No Manua l 16. 2 Area : 2185 1 c Height : 2 Star t Time : En dTime : 286-^00 : 16. 3 J O
• » )
m ig/m L

meter s mlr . e p s poin t n

m n n



# I S«npteName:T(110802B025 " Sampl e ID : •LCS-110726-1 - Ble:*V110802a.w« r Pea k Name : -PFOS * Mns(e*] : '499.000/99.00 0 Da,499.CO0/8O.DO 0 Da,499.000^30.00 0 Da * Commer t T).2pp b LCS " Annotatk>n : ^ Sampl e Index : 2 6 Sampl e Type : Q C Concentration : 0.19 9 ng/m L Calculate dCone : 0.21 3 ng/m L 1/2/201 1 2J*4
- I Sampl e Name:'V110802a028 - Sampl e 10:-LCS-11072&4 - Fle:>1108Caa.wtf r Pea k Name:-PFOS - Ms**(e«):-499JXX)/99.000Da,499.00CV80.000Da,499.00(V130.00 0 0« - I Comment:-2ppbLCS ' Annotation: ' ampl e Index : 2 9
Acq . Tim t ll:4B: U P M Modltled : Pioc . Algorithm : Nol.i « Percentag e Base . Sub . Wind o Peak-Split , Fac t Repor t Larges t

f Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R TWindow : Expecte dRT : l>at > Relativ e RT : Int . Type : Retentio nTime : Are* : 1 Height : Star t Time : N o Specif y P a 5 0 rf: 1.0 0 3 r : 2 a k : Ye s 0.0 0 0 30. 0 15. 3 r H o Valle y 16. 2 n 953 2 co u .93et00 4 16, 1 n 1.2* 4 1.0e4 ' 8000. 0 G000. D 4000.0 - 2000. 0 Sampl e Type : Q C Concentration : 1,9 9 Calculate dCone : 1.9 9 Acq . Date : 8/3/101 1 Acq , Time : 12:51:1 5 A h Modified : N o Ptoc , Algorithm : Specif y Pa r Nola e Percentage : 5 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 2 Min . Pea k

Height : 0.0 0 Min . Pea hWidth : 0.0 0 Smoothin g Width : 0 R TWindow : 30. 0 3 Expecte dRT : 16. 3 n Us e Relativ e RT : No Int . Type : Valle y Retentio nTime : 16. 2 m Area : 17692* 7 cou n Height : 2.e0e'0D 5 e Star t Time : 16. ] D D En dTime : 16. 1 n ng/m L ng/m L

mi n
poin t i n
i n t s p s i n - M

Q II I



### J 2.7* 5

2.ae 5 2,5e5
- 2.4*5
- 2.3*5
- 2.2 e -

1.7»5
- 1.6e5
- 1.5e5
- 1.4e5
- 1,3*5
- 1.2e5
- 1,1*5
- 1,0e5
- 9.0e4
- 8.0*4
- 7.0* 4 • 6.0M
5.0*4
- 4.0*4
- 3.0*4
-

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

W Printing Time : 9:49:5 3 A M Printing Date : Thursday , Augus t 25 , Pag e 1 o f 3 Pag e 5 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS
. PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 *ETS-Kir k Result s Name : kll0802 aext.rd b 

# I S*nTteName:1<110802a031 " Sampl e IO:"LCS-110726-7 - FUe:Tc1108O2*.*t r Pea k Name : -pFOS - Ma««<e«) : -499.000^.00 0 Da,499.000.«0.00 0 Da,499.000/130.00 0 Da ' Commen t -20pp b LCS " Annotation: " Sampl e Inde y: 3 2 Sampl e Typie : Q C Concentration : 19. 9 ng/m L Calculate d Cone : 22. 7 ng/m L Acq
. Date : 8/3/201 1 Acq
. Time : 1:54:5 6 A M

Peak-Split . Factor : Repor t Larges t

Peak ! Min . Pea k

Height : Min . Pea k

tlidth : Smoothin g tlidth : R TWindow : Expecte dRT : Us e Relativ e RT : Valle y

i e : 1J . 2 2257028 ^ c



# I SamplaNama:-k110802aD41 - Sampl e ID:-LCS-110728-13 - F1e:*k110S02a.wt r Pea k Name : 'PFOS ' MaM(e«) : '499.000/99.00 0 Da,4g9.00CVBO.OO O O a .499.000/130.00 0 Da ' Commen t '2pp b LC S ECP * Annotation : Sampl e Ii 

# I Sampl e Name : VI10d02a03ff ' Sampl e 10:-LCS-110726-10^ Fle:1(110802a.wH r P*a k Name : -PfOS - Ma*a(e*) : "499.000/99.00 0 Da,499.000/SO.OO D Oa.499.00Ck'130.00 0 Da ' Comment : -0.2pp b LC S EC p Arvwtatbn : - Sampl e Index : 3 9 Sampl e Type : Q C Concentration : 0.19 8 ng/m L Calculate dCone : 0.2* 6 ng/m L Acq
. Date : 8/3/201 1 '•"* ' Acq . Time : 4:22:4 9 A M 1.7*4 - Modified : Ye s Ptoc . Algorithm : Specif y Para m Nois e Percentage : 5 0 Base . Sub . Window : l.0 0 m Peak-Split , Factor : 2 Repor t Larges t

Peak : Ye s tet a

Min . Pea k

Height : 0.0 0 cp s Min . Pea k

Width : 0.0 0 Smoothin g Vlldth : 0 R TMindow : 30. 0 se e Expecte dRT : 16. 3 mi n Us e Relativ e RT : H e Int . Type : Manua l Retentio nTime : 16. 2 mi n Area : 18163 6 count s Height : l.e5e*00 < ep s Star t Time : IS. 8 mi n En dTime : 16. 3 mi n poin t M Q II I

J 

### f 1 1.8* 4 1.5* 4

1.3* 4 1.2* 4 1.1* 4 1.0* 4 9000J ) 8000, 0 7000. 0 6000. 0 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 

# I Saiiq)leName:'V110802a044 * Sampl e ID : 1.CS-110726-16 rFle:1(110a02a.wi r Pea k Name : -PFOS - li«aM(et) : -49d.000[%.00 0 O a ,499.00080.00 0 D a ,499.000 ^ 30.00 0 Da ' Comment:-20pp b LC S EC P Amotatton: - Sampl e Index : * 5 Sampl e Type : Q C Concentration : 19. 8 ng/m L Calculate dCone : 17. 8 ng/m L Acq . Date : B/3/201 1 Acq . Time : 6:29:3 0 A H Sampl e Type : O C Concentration : Calculate dCone : Acq . Date : Acq . Time : Modified : Proc . Algorithm : Mola e Percentag e 1.9 8 1.8 3 e/3/201 1 ng/m L

ng/m L 5:26:1 1 A

M Ye s Specif y P a 5 0 Base . Sub . Window : 1.0 0 Peak-Split , Factor : 2 Repot t Larges t

Peak : Ye s Min . Pea k

Heigh t Min . Pea k

Hidth : Smoothin g Hidth : R THindow : Expecte dRT : L's e Relativ e RT : Int . Type : Retentio nTime : O.O i O.O i 30. 0 16. 3 H o Manua l 16. 2 Area : 162075 8 co u Height : Star t Time : En dTime : .740*00 5 15, 8 16- 4 mi n

ep s p o mi n
•ni n cp s roln mi n Modified : Ye s Proe . Algorithm : Specif y Param e Nois e Percentage : Base . Sub , Windo w Peak-Split . Fact o Repor t Larges t

Pe . Min . Pea k

Height : Min . Pea k

Width : Smoothin g Width : R TWindow : Expecte dRT : Us e Relativ e RT : Int . Type : Retentio nTime : 5 0 1.0 0 m i : 2 k : Ye s 0.0 0 c 0.0 0 s 0 30. 0 se c 16, 3 roln N o Manua l 16. 2 mi n Area : 1734507 0 count s Height : 1 Star t Time : En dTime : 70e-.00 6 ep s IS. 9 mi n 16. 1 roln

15. 5 16. 0 16. 5 17. 0 17. 5 1SJ ) 1S. 5 15. 0 15. 5 16. 0 18 5 17. 0 17. 5 18. 0 18 5 Dat aprinte db y ST

W Printing Time : 9:49:5 3 A M Printin g Date : Thursday , Augus t 25 , Pag e 2 o f 3 Pag e 5 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS
. an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1 Result s Name : kll0802 a ext.-rd b

•S«nvlaNeme:-lc110802aOSff ' San^l e ID:-QLP1001-02-19-005 - File : I Pea k Name:-PFOS - Ua«s(e*):-499.000i'99.00 0 Oa,499.00a«),O0 0 Da , •Cofwn*nt-DALGWBPMW470110713 - Annolatton: ~ Sample Index : 5 9

Unknow n Sample Type : alc i mtrati c H/

A 0,20 6 ng/m

L B/3/201 1 11:25:1 0 A

M
Nol ! Percentag e uase . Sub . Hindow : Peak-Split . Facto i Report Larges t Pe a Min . Pea k Height : Min . Pea k Width: Smoothing Width: R THindow : Expecte dRT: Vs^ Relativ e RT : Specif y Parameter : 50 1.0 0 mi

n 1.3* 4 13* 4 1.2* 4 1,2* 4 1.1* 4 1.1* 4 1.0* 4 9500. 0 9000. 0 8500. 0 8000. 0 7500. 0 7000. 0 6500. 0 6000. 0 5600. 0 5000. 0 4500. 0 3500. 0 3000. 0 2S0O. O 2O0O.O 1500. 0 1000. 0 500. 1 'WM * 1 6

16.0 K 1 5



# I I

-.- •1M

7 

# 1 i i H J l ^•Jll6i » 15.7 ^ ^^m p ^

•fTY ^ JM^ ^

m, . lu 

## P"!^ TM ,^V m 17.4 1

ILJ M 

### w f P ^17.7 7 il k '" » 

### n, i ^in u '.WwW w

Dat a printe d b

yST W Printing Time : 9:49:5 3 A M Printing Date : Thursday , Augus t 25 , 201 1 Pag e 3 o f 3 Pag e 5 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1


## ATTACHMEN TC : ANALYTICA LMETHO D

Pag e 5 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Sit e B P Property- Jul y201 1


# Environmenta l Laboiafioff y

Metho d Metho d o fAnalysi 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 <//( ^ / o " 7
Approve d By : 

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

ETS-8-044. 0 Pag e 1 of1 1 Metho d ofAnalysi s fo rtli e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i 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) , Perfluorododecanoi cAci d (PFDoA) , Perfiuorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfiuorooctanesulfonat e (PFOS ) b yHig h Perfomnanc

e Liqui d Chromatograph ycouple d t o a tande m Mas s Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples
. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Determinatio n o f Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
. Thi s metho d i s considere d a performance-base d method
. Data i s considere d acceptabl e a s lon g as th e define d Q C elements are satisfied
. Sampl e collectio n i s not covere d unde rthi s analytica l procedure
. 2 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS
. Sample s containin g heav y particulat e ma

yno t b e suitabl e fo ranalysi s b ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thi s i s a performance-base d method
. Metho d accurac yi s determine d fo reac h sampl e se t usin g multipl e laborator ycontro l spike s at multipl e concentrations
. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o 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 as suc h (wit h expande d accurac

ystatements) , o rwil l no

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

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

yspikin g a know n volum e ofth e Workin g Standar d (WS ) into a predetermine d amoun t o fAST M Typ e i , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method
. Calibratio n standard s are use d t o calibrat e th e instrumen 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 ofth e precisio n associate d wit h laborator yprocedures , bu t no

t wit h sampl e collection , preservation , o rstorag e procedures
. 

## 3. 3 Fiel d Blan k

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d as 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 o fth e F B i s t o determin e i ftes t substance s o r othe rinterference s are presen t i n th e field environment
. Thi s sampl e i s als o refen-ed t o as a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 9 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i 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 as th e sample
. Th e FD S i s handle d unde ridentica l circumstance s an d treate d exactl yth e sam e throughou t field an d laborator y procedures
. Analysi s ofth e FD S compare d t o that ofth e first 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 before th e bottle s are sen t t o th e field fo rcollectio n ofaqueou s samples
. Aknown , specifi cvolum e of sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

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

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

t a n appropriat e leve l i s made
. Th e FM S i s analyze d t o ascertai n i 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 ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s o fth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylike a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s o fanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are 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 as eac h FMS
. 

## 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator ya t th e tim e ofsampl e extraction
. At least tw o level s are included , on e generall ya t th e lo wen d ofth e calibratio n curve an d on e nea rth e mi d t o uppe rrang e 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 o fa sampl e t o whic h know n quantitie s oftarge t analyte s are adde d i n th e laboratory
. Th e LM S i s analyze d exactl ylike a laborator ysampl e t o determin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results
. Th e endogenou s concentration s o fth e analyte s i n th e sampl e matri xmust b e detemnined i n a separat e aliquot an d th e measure d value s i n th e LM S con'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 ofa sampl e receive d fi-om th e field fo rtesting
. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t o fquantitatio 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 ofquantitatio 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 as th e ULOQ
. ETS-8-044. 0 Pag e 3 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 0 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Slt e B P Property- Jul y201 1


## 3.1 1 Metho d Blan k A n aliquot ofcontro l matri xthat i s treate d exactl ylike a laborator ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that are use d wit h othe rlaborator ysamples
. Th e metho d blan k i s use d t o determin e i ftes t substance s o rothe rinterference s are presen t i n th e laborator y environment , th e reagents , o rth e apparatus . 3.1 2 Sampl e Asampl e i s a n aliquot remove d fi-om a large rquantit yo fmateria 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 o fa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound
. 

## 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t normall y foun d i n th e sample(s)
. Asun-ogat e compoun d i s typicall ya targe t analyt e wit h at least on e ato m containin g a n isotopically-labele d substitution
. I fused , surrogate(s ) ar e adde d t o al l sample s an d qualit y contro l samples
. Sun-ogate(s) are adde d t o quantitativel yevaluat e th e entire analytica l procedur e includin g sampl e collection , preparation , an d analysis
. Inclusio n o fa sun-ogat e analyt e i s a n optiona l qualit ycontro l measur

e an d i s NOTrequired
. 

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

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

yglasse s t o preven t 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 curren t awarenes s o floca l regulation s regardin g th e handlin g ofth e chemical s use d i n thi s method
. Areference file ofmateria l safet y dat a sheet s (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems . Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l infomnatio n an d cautions
. 

## 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware
. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s ofanalysi s b

ymnnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 1 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Slt e B P Property- Jul y201 1


### Parts an d supplie s that contai n Tefion® 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 ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 

## 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h perfomnanc

e liqui d chromatograp h capabl e ofpumpin g u p t o two solvents an d equippe d wit h a variabl e volum e injecto rcapabl e o finjectin g 5-10 0 |J Lconnecte d t o a tande m Mass Spectromete r (LC/MS/MS)
. I Analytica l balance capabl e o freadin g t o 0.000 1 g Adevice t o collec

t ra wdata fo rpea k

integratio n an d quantitatio n 15-m Lan d 50-m Ldisposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25IJL , 50|JL , IOOJJL , 250|JL , 

### SOOpL , 1000|JL
. 

### 1 m Lplasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s as appropriat e Centrifug e capabl e ofspinnin g 15-m Lan d 50-m Lpolypropylen 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 C I 8,4. 6 m m x100 mm , 5 |j m Temperature : lO' 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 |J L Quantitation : Pea k

Are a - quadrati ccurve fit, 1/ xweighted
. Ru n Time : ~ 1 7 minutes
. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met . ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 2 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i 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 PFBA PFPe A PFH A PFHpA PFOA PFN A PFDA PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 31 3 ^26 9 an d 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 fisomers tha t more closel ymatche s NM R dat a an d ma yhav e th e adde d benefi t o f increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a ar e me t t o assur e adequat e specificity
. Th e previou s informatio n i s intende d as a guide , alternat e instruments 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 as 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 (PF0A-C 8 acid) ; 3 M PerfluorononanoicAci d (PFNA-C 9 acid) ; Oakwoo d Products , in c Perfluorodecanoi cAci d (PFDA-CI O acid) ; Oakwoo d Products , In c PerfluoroundecanoicAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c PerfluorododecanoicAci d (PFDoA-CI 2 acid) ; Oakwoo d Products , In c Perfiuorobutanesulfonat e (PFB S - C 4 sulfonate) ; 3 M Perfiuorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfiuorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 3 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Slt 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 Lofreagen t water . Note : Altemative volume s ma yb e prepare d a s lon g as 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 procedure serve s a s a n example
. Weighe d amounts an d final volume s ma yb e change d t o sui t th e need s o fa particula rstudy
. Fo rexample , IJ Lvolume s ma yb e spike d into volumetri cflasks whe n dilutin g stoc k

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

, ^ XX Xmolecula 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 CsFiySOs'K

" wit h purit

y90 % = 8.35m g C8F17SO3 " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 (jg/m L(500 0 ng/mL ) mixe d workin g standard-^d d 0.5m L eac h ofth e 100|jg/m LSSS s t o a 10m Lvolumetri c fiask an d brin g u p t o volum e wit h solvent
. 25 0 ng/m Lmixe d worthin g standard—Ad d 1.25m L ofth e 5 iig/m L-mixe d wori<in g standar d solutio n t o a 25m L volumetri cflask

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m Lmixe d standard—Ad d 625|J Lo fth e 5 |jg/mL-mixe d woricin g standar d solutio n t o a 25m Lvolumetri c flask an d brin g u p t o volum e wit h solvent
. Storag e Conditions—Stor e al l SSS s an d workin g standard s i n accordance wit h laborator ystandar d operatin g procedure o ri n a refrigerato ra t 4''±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 4 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s

Off-Slt e B P Property- Jul y201 1


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

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

Calibratio n Standar d (m L o fAST M Typ e 1 Water , o r 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 AS77M Typ e 1 Water , o rotiie rsuitabl e wate r 0.02 5 0.037 5 0.05 0 0.07 5 0.10 0 0.25 0 0.50 0 1.00 2.5 0 5.0 0 10. 0 

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

ynot b e suitabl e fo r analysi s b

ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial
. Plasti ci s prefen-ed ove rth e us e o fglas s autovials , t o preven t th e possibl yo ffluorochemical stickin g t o th e glass
. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water . Prepar e metho d Q C sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials
. Prepar e a t least five metho d blanks
. 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

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

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

xo runweighted , o rb

yquadrati cfil (y= ax

^ + bx+ c) , weighte d 1/

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

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

wpoints ma

yb e exclude d fi-om th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-determine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are not at least twic e that o fth e metho d and/o rsolven t blanks
. Th e coefficien t ofdetemninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 5 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1


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

yofth e calibratio n curve . Analyz e a mid-rang e calibratio n standard , on e 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 , not includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set . Calibratio n verificatio n injection s must b e withi n +25 % t o b e considere d acceptable
. Th e calibratio n curve an d th e last passin g CCV wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that are quantitate d above th e concentratio n ofth e highest standar d i n th e 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 targete d LOQ of0.02 5 ng/mL
. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e final report . 

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

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

s ma yb e injecte d multipl e times , bu t n o more tha n 3 injection s shoul d b e remove d 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 o f CCV samples , an d at th e en d ofth e analytica l mn . Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % ofth e are a coun t ofth e LOQ standard
. Th e standar

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

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

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

## 10. 4 Surrogat e Spike s Sun-ogat e spike s are not 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 oftw o differen t concentration s are t o b e prepare d wit h eac h preparatio n batch
. Lowla b contro l spike s shoul d b e prepare d at concentration s i n th e rang e o ffive 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 fth e curve . Th e relative standar

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

ETS-8-044. 0 Pag e 9 o f1 1 Metho d o fAnalysi s fo rth e Detemninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 6 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i 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 offield matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e fiagged as suc h (wit h expande d accurac ystatements) , o rwil l no

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

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

^ ^ Slop e D F = facto rb

ywhic h th e final volum e wa s diluted , i fnecessary . Fo rsample s fortifie d wit h know n amounts o fanalyt e prio rt o extraction , us e th e followin g equatio n t o calculat e th e percen t recovery . P
_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 not 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 fcriteri 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 fdat a are t o b e reporte d whe n perfomnanc e criteri a have no

t bee n met , th e data must b e footnote d o n table s an d discusse d i n th e tex

t ofth e report . 

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

ystandard s are no

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

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

t th e beginnin g o feac h analytica l m n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l ofth e calibratio n cun/

e an d are repeate d injection s fro m on e autosample rvial
. Th e syste m suitabilit yinjection s must have are a counts wit h a n RS D ofS5% an d a retentio n tim e RS D ofS2 % t o b e compliant
. 

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

yb e withi n ±30%
. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence are evaluate d as 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 mus

t b e withi n 25 % o fth e theoretica l valu e (withi n 30 % fo rlowest curve point)
. Sample s that are brackete d b

yCCVs no

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

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o fAnalysi s fo rth e Detemninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 7 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Sit e B P Property- Jul y201 1


### Demonstratio n o fSpecificity : Specificit yi s demonstrate d bychromatographi cretentio n time (withi n 4 % o f standard ) an d th e mas s spectra l respons e ofuniqu e ions
. 12. 3 Sensitivit y Th e targete d limi t o fquantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n ofappropriat e blank s an d th e accurac

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

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

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

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

## 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n 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 a

t th e 3 M Environmenta l Laborator yi n accordance wit h intema l procedures
. 1 4 Record s Eac h data packag e generate d fo ra stud ymust includ e al l supportin g infomnatio n fo rreconstmctio n o fth e data
. Infomnatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

d pre p sheets/records , instmmen t m n lo g (instmmen t batc h records , instmmen 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 fChange s 

# }

ETS-8-044. 0 Pag e 1 1 o f1 1 Metho d o fAnalysi s fo rth e Detemninatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 8 o f7 0GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s

Off-Slt e B P Property- Jul y201 1


## ATTACHMEN TD : DEVIATION(S )

Pag e 6 9 o f7 0

### GLP10-01-02 ; Interi m Repor t 1 9 Analysi s o fPFBS , PFHS , an d PFO

S I n Wate rSample

s Off-Sit e BP Propert

y- July201 1 

# RECOR D O F DEVIATION/NONCONFORMANC E

/
. Identificatio n stud y/ Projec t No
. GLP10-01-02-1 9 Deviatio n typ e (Chec k one ) D

D SO P Protoco l Date(s ) o fOccurrence :

j<110802 a an d k l 10802 a ex t D Equipmen t Procedur e D GP O Documen t Number : ETS-8-044. 0 0 D Metho d Other : //
. Descriptio n (attac h extr a page s a s needed ) 

## Metho d Requirements : 1
. LC S averag e recoverie s withi n ±20 % (sectio n 10.5)
. 

## Actua l procedure/process : 1
. k l 10802a ; interna l standar d calibration : Th e low , mid , an d hig h PFO S EC F LC S sample s ha d averag e recoverie s of129% , 122% , an d 122%
. k110802 a ext ; externa l standard calibration : Th e lowPFO S (linear) LC S ha d a n averag e recover yo f122%
. Th e lowPFO S (linea ran d branched ) LC S ha d a n averag e recover yo f126%
. 

## ///
. Action s Take n

(suc h a s amendmen t issued , SO P revision , etc. ) 

## Correctiv e Actio n ( D Ye s IZ fNo ) Reference : Acceptabilit yo fth e nonconformin g work : 1
. Th e recoverie s fo rth e LCS s (linea r+ branched ) outsid e metho d acceptanc e criteri a wil l b e flagge d i n th e fina l report . Al l o fth e LCS s prepare d wit h thi s stud ywer e evaluate d b yETS-12-01 2 t o determin e th e metho d analytica l uncertainty
. Th e analytica l uncertaintywhe n evaluate d byETS-12-01 2 wa s detennine d t o b e ±24 % fo rPFOS
. However , th e analytica l uncertaintyfo rthi s stud ywil l b e se t at ±29% , base d o n th e recover yo fth e lowse t o flinea r+ branche d LC S fro m ru n k l 10802a
. Actions : D Haltin g o fWori < D Clien t Notificatio n D Wor k Recal l D Withholdin g o fRepor t 1 3 Other : Deviation s wil l b e note d i n fina l report . 

## Project Lead/PA I Approval : ( 1 stud yDirecto r(i fGLP) : Sponso rApprova l (fo rGL P protoco l deviations) : N A Date : 

# KJ M Date> Dat e 

# L L 

# Wl L Technica l Reviewe r(optional) : N A Date : NA Laborator yDepartrpen t Man s 

# rgd ^ Approval : Date :

IV
. Authorizatio n t o Resum e Wor k Where haltin g o fwor k

occurred , resumptio n o fwor k mus t firs t b e approve d b yLaborator yManagemen t 

## Laborator yDepartmen t Manage rApproval : NADate : NA Deviatio n No
. (assigned b

yStudyDirecto ro rTea

m Leade ra

t th e en d ofstudyo rproject ) ETS-4-008. 7 Pag e 1 o f1 Documentatio n o fDeviation s an d Contro l o fNonconformin g Testin g ^^ ®