GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### GLP10-01-02 : Interi m Repor t 2 2 - Analysi s o fPFBS . PFHS . an d PFO S i n Groundwate rSample s Collecte d fro m Decatur . AL . 3*^ " Quarte r201 1 Stud yTitl e Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e Sulfonate (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m 

### Data Requiremen t 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 , P

A1938 0 Phone : 610-701-376 1 

### Autho r Susa n Wol f 3 M Environmenta l Laborator y 

### Interi m Report Completio n Date

Dat e ofsignin g 

### Performin g Laboratory 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

y 3 M Center , Bld g 260-05-N-1 7 S t Paul , M N 55144 

### Project Identificatio n GLP10-01-02-2 2 

### Tota l Numbe ro

fPage s 9 9
The testin g reported herei n mee t th e requirement

s o fANSI / ISO/IE C 17025:200

5 "Genera l Requirement

s fo rth e Competenc

e ofTestin g an d Calibratio n laboratories" , i n accordanc e wit h th e A2L

ATestin g Certificate # 2052.01 . Testin g tha t complie s wit h thi s 1 1 Internationa l Standar d als o meet

s principle s ofIS

O 9001:2000 . ACCREDITE D Testin g Cer t #2052.0 1

Page 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



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

t 2 2 - Analysi s o

fPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d fro m Decatur , AL , 3" ^ Quarte r201 1 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonate (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 was conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Good Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

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

fa test system . •Th e reference substance s hav e no t bee n characterize d unde rth e GLP s an d th e stabilit yunde r storag e condition s a

t th e test sit e hav

e no t bee n determine d unde rGLPs
. 

# 3 , Gar yHopenstein,|Sponso rRepresentative Date

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

Pag e 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



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

t 2 2 - Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d fro m Decatur , AL , 3" ^ Quarte r201 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) , a s indicate d i n th e followin g table
. Th e finding s were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector
.
Inspectio n Date s Phas e Dat e R e porte d t o Inspectio n Date s Phas e Testin g Facilit y lUlanagemen t Stud yDirecto r 11/10/11-11/11/1 1 Data / Interi m Repor

t 11/30/1 1 11/30/1 1



### QA U Representative Date

Pag e 4 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### TABL E OF 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 8 2 Summary..
. 9 3 Introductio n 1 1 4 Test & Contro l Substance s 1 1 5 Reference Substance s 1 2 6 Test Syste m 1 3 7 Metho d Summar

y1 4

' 7. 1 Method s 1 4 7. 2 Sampl e Collectio n 1 4 7. 3 Sampl e Preparatio n 1 4 7. 4 Analysi s 1 4 8 Analytica l Results 1 6 8. 1 Calibratio n 1 6 8. 2 Syste m Suitabilit y1 7 8. 3 Limito fQuantitatio n (LOQ ) 1 7 8. 4 Continuin g Calibratio n 1 7 8. 5 Blank

s 1 8 8. 6 La b Contro l Spike s (LCSs ) 1 8 8. 7 Analytica l Metho d Uncertaint y2 1 8. 8 Fiel d Matri xSpike s (FMS ) 2 1

Pag e 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### 9 Data Summar

yan d Discussio n 2 2 1 0 Conclusio n 34 1 1 Data/Sampl e Retentio n 3 4 1 2 Attachment s 34 1 3 Signature s 35 

### LIS TO F TABLE S Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Results (DecaturGroundwater-Q 3 2011)...1 0 Tabl e 2 . Sampl e Descriptio n Ke yCod e 1 3 Tabl e 3 . Instrumen t Parameter s 1 5 Tabl e 4 . Liqui d Chromatograph yCondition s 1 5 Tabl e 5 . Mass Transition s 1 6 Tabl e 6 . Limi t ofQuantitatio n (LOQ ) 1 7 Tabl e 7 . Laborator

yContro l Spik

e Recover

y1 8 Tabl e 8 . Analytica l Uncertaint y2 1 Tabl e 9 . Fiel d Matri xSpike s 2 1 Tabl e 10 . DA L G W203 L 11093 0 2 3 Tabl e 11 . DA L GW220R11093 0 2 3 Tabl e 12 . DA L GW220L11093 0 2 4 Tabl e 13 . DA L GW222 R 11093 0 .....2 4 Tabl e 14 . DA L GW227 R 110922.. . 2 5 Tabl e 1 5 DA L GW227 L 11092 2 2 5 Tabl e 16 . DA L G W3 1 O R 11092 8 2 6 Tabl e 17 . DA L G W312 R 11092 9 2 6 Tabl e 18 . DA L G W317L11092 8 .2 7 Tabl e 19 . DA L G W324 L 11092 3 2 7 Tabl e 20 . DA L G W327 R 11092 8 2 8

Pag e 6 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### Tabl e 21 . DA L G W328 R 11092 7 2 8 Tabl e 22 . DA L G W328L11092 8 2 9 Tabl e 23 . DA L G W330 R 11092 8 2 9 Tabl e 24 . DA L G W330L11092 8 3 0 Tabl e 25 . DA L G W331 S 11092 9 3 0 Tabl e 26 . DA L G W335R11092 7 3 1 Tabl e 27 . DA L G WGRS04 11093 0 3 2 Tabl e 28 . Tri p Blan k

1 :....3 2 Tabl e 29 . Tri p Blan k

2 33 Tabl e 30 . Equipmen t Rinseate Blank s 33

Pag e 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



## 1 Study

Information Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Stud 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 Testing Facility 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 St
. Paul , M N 55144 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator , (clanqe@mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow ; analys t Kell yUkes ; analys t Jonatha n Steege ; analys t Stud yDate s Stud yInitiation : Marc h 8,201 0 Interi m 2 2 Experimenta l Termination : Octobe r25 , 201 1 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 at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792 . Th e tes t substanc e an d analytica l referenc e standard reserv e sample s ar e archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



## 2 Summary Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d i n Decatur , AL , representin g eightee n (18 ) differen t samplin g location s collecte d Septembe r2 2 - 30 , 2011 . Atota l of eighty-two 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)
. Fo reac h samplin g location , fou rsampl e bottle s were collected ; sample , sampl e duplicate , lo wfiel d matri xspike , an d hig h fiel d matri xspike
. Two tri p blank s containin g Milli-Q TM wate ran d appropriat e tri p blan k spike s were analyze d wit h th e groundwate rsamples
. I n addition , two equipmen t rinseate blan k sample s were collected
. Th e equipmen t rinseate blank s di d no t have FM S sample s prepare d fo r determinatio n o

fPFBS , PFHS , o rPFO S recovery . Al l groundwate rsample s fo rthi s projec t were logge d unde rGLP10-01-02-22
. Th e groundwate rsamples , tri p an d equipmen t rinseat e blank s fo rGLP10-01-02-2 2 were receive d fro m Westo n personne l o n Octobe r6 , 2011 . Al l o fth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8-044.0
. Man yofth e groundwate rsample s require d dilutio n t o obtai n PFBS , PFHS , and/o rPFO S concentration s withi n th e rang e o fth e cun/e , i n som e instance s u p t o a 500-fol d dilutio n were required
. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s ar e summarize d i n Tabl e 1 . Equipmen t rinseat e an d th e tri p blank s were belowth e lowe rlimi t ofquantitatio n (LLOQ) , indicatin g adequat e contro l o fsampl e contaminatio n durin g shippin g an d sampl e collections
. Th e PFB S concentratio n results fo ral l groundwate rlocation s range d fro m <0.040 0 ng/m L t o 307 0 ng/mL
. Th e PFH S concentratio n results fo r al l groundwate rlocation s range d fro m 0.0984 ng/m L t o 606 0 ng/mL
. Th e PFO S concentratio n results fo rth e reporte d groundwate rlocation s range d fro m 0.205 ng/m L t o 335 0 ng/mL
. Th e analytica l uncertaintie s associate d wit h th e reporte d results are a s follows : PFB S 100 % ±14% , PFH S 100 % ± 18% , an d PFO S 100 % ±26% .

Pag e 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Result s (Decatu rGroundwate r- 0 3 2011) . PFB S PFH S PFO S Samplin g Locatio n Avg . Cone . (ng/mL) ±%RP D Avg . Cone . (ng/mL) ±%RP D Avg . Cone . (ng/mL ) ±%RP D DA L GW203 L 110930 23. 2 ±9.9 % 14 2 ±9.2 % 47 8 ±3.1 % DALGW220R11093 0 4.7 6 ±2.9 % 17. 9 ±2.2 % 27. 4 ±7.3%'^ ' DALGW220L11093 0 7.87 ±1.0 % 37. 6 ±1.1 % 49. 2 ±10 % DA L GW222 R 11093 0 62. 5 ±0.16 % 42 9 ±0.93 % 51 1 ±0.39 % DA L GW227 R 11092 2 13. 4 ±4.5 % • 61. 7 ±4.5 % 57 8 ±2.1 % DA L GW227 L 11092 2 25 6 ±1.6 % 68. 5 ±0.58 % 47 4 ±3.6 % DA L G W3 1 O

R 11092 8 73 0 ±3.7 % 32 0 ±1.3 % 61 1 ±3.4 % DALGW312 R 11092 9 1140 ±1.8 % 83 1 ±0.48 % 1440 ±8.3 % DA L GW317 L 11092 8 <0.040 0 0.098 4 ±9.3 % 0.20 5 ±8.8 % DALGW324L11092 3 70. 0 ±0.0 % 82. 5 ±0.97 % 21 1 ±0.95 % DA L GW327 R 11092 8 51. 6 ±0.58 % 12 6 ±1.6 % 39 7 ±1.3 % DA L GW328 R 11092 7 27. 9 ±1.4 % 57. 9 ±2.2 % 178 ±0.28 % DA L GW328 L 11092 8 40. 3 ±0.0 % 18. 4 ±1.1 % 1.29 ±3.9 % DA L GW330 R 11092 8 307 0 ±0.48 % 19 6 ±1.5 % 59 3 ±2.4 % DA L GW330 L 11092 8 53 0 ±5.5 % 43 4 ±1.4 % 169 ±1.4 % DA L GW331 S 11092 9 52 5 ±3.8 % 33 1 ±3.0 % 50 6 ±4.5 % DA L GW335 R 11092 7 1080 ±3.7 % 142 0 ±2.1 % 335 0 ±3.3 % DA L GWGRS0 4 110930 1690 ±3.6 % 606 0 ±5.5 % 1330 ±1.5 % Tri p Blan k

(Milli-Q TM Water) - 2 sets <0.040 0 <0.025 0 <0.18 3 Equipmen t Blan k

s - 2 rinseat e blank

s <0.040 0 <0.025 0 <0.232 Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results ar e a s follows : PFB S 100 % ±14% , PFH S 100 % ±18% , an d PFO S 100 % ±26% . (1 ) Th e analytica l uncertaint yhas bee n expande d fo rth e followin g sample s base d o n FM S recovery : DA L G W220 R (PFO S ± 38%) , DA L G W220 L (PFO S ±S8%) , DA L G W222 R (PFO S ±43% ; PFH S ±35%) , DA L G W330 L (PFB S ±34%) , DA L G W 331 S (PFB S ±32%) , DA L G WSS5R (PFB S ±31%) , an d DA L G WGRS04 (PFO S ±S7%)
. (2 ) Samplin g locatio n di d no t contai n a n appropriate spil< e leve l to assess PFO S recovery .

Pag e 1 0 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### 3 Inlj^oduction Thi s analytica l stud ywa s conducte d as par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama
. Th e objective ofth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d i n Decatur , A L fo r PFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on-sit e groundwate rconditions
. Th e 3 M Environmenta l Laborator yprepare d sampl e container s (25 0 m L high-densit

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

ycontaine rwa s marke d wit h a "fil l t o here " lin e t o produce a final sampl e volum e o f20 0 mL
. Container

s designate d fo rfield matri xsample s were fortifie d wit h a n appropriat e matri x spik 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 field fo rsampl e collection
. Se e sectio n 8. 8 ofth e repor t fo rfield matri xspik

e levels
. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "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 Analysis"
. 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 , tri p blank

s an d equipmen t rinseate samples
. Table s 10-3 0 summariz e th e individua l sampl e results an d th e associate d FM S recoveries
. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewher e i n thi s repor

t 4 Test&Control

Substances There was no

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

Pag e 1 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



## 5 Reference

Substances
Referenc e Substanc e PFB S (predominantl y linear ) PFH S (linear ) Chemica l Nam e Perfluorobutan e sulfonat e Perfluorohexan e sulfonat e Chemica l Formul a C4F9SO3 " CgFisSO a Identifie r Potassiu m Sal t Sodiu m Sal t Sourc e 3 M Wellingto n Expiratio n Dat e 1/10/201 7 3/25/201 8 Storag e Condition s Froze n Froze n Chemica l Lo t Numbe r 10 1 LPFHxSAMO S TC R Numbe r TCR-12 1 TCR08-001 8 Physica l Descriptio n Whit e Powde r Crystallin e Purit y 96.7 % 98 % Us e Targe t Analyt e Referenc e Standar d Targe t Analyt e Referenc e Standar d
Referenc e Substanc e PFO S (linear ) PFO S (linea r+ branched ) Chemica l Nam e Perfluorooctan e sulfonat e Perfluorooctan e sulfonat e Chemica l Fomnul a CsF-iySO a CsF-iySO s Identifie r Potassiu m Sal t CA S #2795-39- 3 Potassiu m Sal t CA S #2795-39- 3 Sourc e Wellingto n Wellingto n Expiratio n Dat e 10/18/201 8 03/17/201 4 Storag e Condition s Froze n Froze n Chemica l Lo t Numbe r LPFOSKBM0 6 brPFOSK070 8 TC R Numbe r TCR08-000 1 TCR11-001 0 Physica l Descriptio n Crystallin e Liqui d Purit y 98 % 99.9 % Us e Fiel d Matri xSpik e Referenc e Standar d Targe t Analyt e Referenc e Standar d

Pag e 1 2 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Referenc e Substanc e "Cg-PFO S (linear ) Chemica l Nam e Sodiu m Perfluorooctanesulfonat e Chemica l Formul a "CsFuSOa'Na " Identifie r CAS#MPFC-C-051 1 Sourc e Wellingto n Expiratio n Dat e 05/25/201 4 Storag e Condition s Froze n Chemica l Lo t Numbe r 09231 0 TC R Numbe r TCR11-001 6 Physica l Descriptio n Liqui d Purit y 5|jg/mL<^ > Us e Interna l Standar d (1 ) Custo m mixtur

e ofseve n mass-labele d ( C ) pertluoroalkylcarboxyli cacids , two mass-labele d ("C ) perfluoroalkylsulfbnate s an d on e mass-labele d ("C ) perfluoro- 1 -octanesulfonamide
. 

### 6 Test System Th e tes t syste m fo

rthi s stud yar e groun d watersamples collecte d fro m well s locate

d i n Decatur, A L b

y Westo n Solutions , Inc . personnel . Samples forthi s stud y ar e "real world " samples , no t dose d wit h a specifi c lo t o ftes t substance . Tabl e 2 . Sampl e Descriptio n Ke y Code . Example DALGW

203LDB

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

shallow water-bearing

zone L= Bedrock water-bearing

zone S = Epikarst middle water-bearing

zone 5 Sample Type 0=primary sample DB=duplicate

sample LS = low spike MS = mid spike HS = iiigh spike 6 Sampling Date 110930 = September30,2011

Pag e 1 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



## 7 Method

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 "Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc t Injectio n Analysis"
. 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s were retume d t o th e laborator ya t ambien t condition s o n Octobe r6 , 2011 . Sample s were store d refrigerate d a t th e laborator

yafte rreceipt
. Aset oflaborator y prepare d Tri p Blan k

an d Tri p Blan k

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

## 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Sample s that require d dilutio n were prepare d a s follows : 1:5 dilution s were prepare d b ydilutin g 2m L sampl e wit h 8 m L ofMill i 0 water , 1:1 0 dilution s were prepare d b ydilutin g Im L sampl e wit h 9 m L o fMill i Q water , 1:20 dilution s were prepare d b ydilutin g 0.5m L sampl e wit h 9.5m L ofMill i Q water , 1:5 0 dilution s were prepare d b ydilutin g 0.2m L sampl e wit h 9.8m L ofMill i Q , an d 1:10 0 dilution s were prepare d b ydilufin g O.lm L sampl e wit h 9.9m L ofMill i Q water . Sample s ma

yals o hav

e bee n dilute d furthe rb

yvaryin g th e injectio n volum e durin g analysis
. Samplin g location s DA L G W317 L an d DA L G W328 L were prepare d fo rPFO S b yremovin g a 5 m L aliquot an d addin g a n aliquot ofa separat e intema l standar d spikin g solutio n (nomina l concentratio n of1 ng/mL)
. Thi s sam e procedur e wa s followe d fo rth e laborator ycontro l samples
. 

## 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h performance liqui d chromatography / tande m mas s spectrometr y(HPLC/MS/MS)
. Detaile d instrumen t 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 final dat a packet , an d are briefl ydescribe d below
.

Pag e 1 4 o f9 9

### Tabl e 3 . Instrumen t Parameters . GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Instrumen t Name ET S Buste r ETSKiri < Analytica l Metho

d Followe d ETS-8-044. 0 ETS-8-044. 0 Analysi s Dat

e 10/12/1 1 10/20/11 , 10/24/1 1 Liqui d Chromatograp h Agilen t 110 0 Agilen t 1200 Guard colum n Prism RP (2.1 mm

X 50 mm), 5 n Betasi l 01 8 (4. 6 m m X 100 mm) , 5 u Analytica l colum n Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n Betasi l 01 8 (4. 6 m m X 100 mm) , 5 n Injectio n Volum e 2or10u L 1 0 o r5 0 u L IVIas s Spectromete r Applie d Biosystem s fiP\ 400 0 Applie d Biosystem s AP I 550 0 Io n Sourc e Turb o Spra y Turb o Spra y Electrod e Turb o io n electrod e Turb o io n electrod e Polarit y Negativ e Negativ e Softwar e Analyst 1.4. 2 Analyst 1.5. 2 

### Tabl e 4 . Liqui d Chromatograph y Conditions . ste p 7ota

/ 77in e Flow

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

acetate) (Methanol) ETS-8-044.0

Analysis

10112111 0 0 30 0 97. 0 3. 0 1 2. 0 30 0 97. 0 3. 0 2 14. 5 • 30 0 5. 0 95. 0 3 15. 5 30 0 5. 0 95. 0 4 16. 5 30 0 97. 0 3. 0 5 20. 0 30 0 97. 0 3. 0 ETS-8-044.0

Analysis

10/20111 and

10/2A/11 0 0 75 0 97. 0 3. 0 1 2. 0 75 0 97. 0 S. O 2 14. 5 75 0 5. 0 95. 0 3 15. 5 75 0 5. 0 95. 0 4 16. 5 75 0 97. 0 3. 0 5 20. 0 75 0 97. 0 3. 0

Pag e 1 5 o f99

### Tabl e 5 . IVIass Transitions . , GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Analyte Reference Material Structure Mass Transition Q1IQ3 Intemal Standard Mass

Transition Q1/Q3 PFBS Linear 299/80 NA NA 299199 PFHS Linear 399180 NA NA 399/99 PFOS Linear+Branched 499/80 ["CJPFOS'" 507/80 499/99 499/130 Dwel l tim e was 7 5 mse c(10/12/1 1 analysis ) o r3 0 mse c(10/20/1 1 an d 10/24/1 1 analysis ) fo react i 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
. N A= No t Applicabl e (1 ) Intema l standar

d wa s onl yuse d fo rth e analysi s oflocation s DA L G W317 L an d DA L G WS28 L fo rPFOS
. 

## 8 Analytical

Results 8. 1 Calibratio n 8.1. 1 Extema l Standar d Calibratio n -10/12/1 1 an d 10/20/1 1 analysis : Sample s were analyze d against a n externa l standar d calibratio n curve . Calibratio n standard s were prepare d b

yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s into Mill i Q water . Atota l o ffiftee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L were prepared , however , no

t al l analytica l run s include d al l fiftee n standards
. Lo wcurve points ma

yhave bee n disable d t o meet accurac yo rmetho d blan k

criteria
. Aquadratic , 1/

xweighted , calibratio n curve o fth e pea k are a counts wa s use d t o fit th e dat a fo reac h analyte
. Th e dat a were no t force d throug h zero durin g th e fittin g process . Calculatin g th e standar d concentration s usin g th e pea k are a confirme d accurac yofeac h curve point
. Th e PFO S reference standar d use d fo rth e preparatio n ofth e calibratio n standard s containe d bot h linea r an d branche d isomers
. Th e sample s conaine d bot h linea ran d branche d isomers , man ywit h concentration s >10 0 ng/mL , however , th e field matri xspike s were prepare d usin g predominantl ylinea r PFOS
. T o hel p minimiz e an ypotenfia l analytica l bia s i n th e quantitatio n oflinea risomer s ofPFO S against mixe d linea ran d branche d PFOS , th e linea rPFO S peak s an d th e branche d PFO S peak s were integrate d separately
. Fo rth e linea rcalibration , onl yth e linea rpeak s ofal l sample s were integrated , includin g th e calibratio n curve . Th e branche d calibratio n wa s don e i n th e sam e manner , integratin g onl y th e branche d isomers
. Th e concentration s ofth e calibratio n curve points were base d o n th e percen t linea ran d branche d isomer s i n th e standard , 21.1 % branche d an d 78.8 % linear
. Th e final calculate d concentration s were detemnined usin g th e summe d calculate d concentration s o fth e linea ran d branche d peaks
. 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 lowest curve point) were met fo ral i analytes
. Th e correlatio n coefficien t (r) wa s greate rtha n 0.99 5 fo rPFBS , PFHS , an d PFOS
. 8.1.2 Intema l Standar d Calibratio n -10/24/1 1 analysis : Samplin g location s DA L G W317 L an d DA L G W328 L fo rPFO S were analyze d against a matrixmatche d stabl e isotop e interna l standar d calibratio n curve . Calibratio n standard s were prepare d b y
Pag e 1 6 o f9 9GLP10-01-02 ; Interi m Repor i 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### spikin g know n amounts o fth e stoc k

solutio n containin g th e targe t analyte s into a laboratory-prepare d syntheti cgroundwate rcontainin g calciu m an d magnesium
. Th e calibratio n standard s containe d a n intema l standar

d mi xcontainin g "Cs-PFO S a t a nomina l concentratio n o f1 ng/mL
. Atota l o

fthirtee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 2 5 ng/m L were analyze d fo rPFOS
. Th e PFO S reference standar

d use d fo rth e preparatio n ofth e calibratio n standard s containe d bot h linea ran d branche d isomers
. Aquadratic , 1/ xweighted , calibratio n curve o fth e rati o o

fth e standar

d pea k are a counts ove rth e intema l standar d pea k are a counts wa s use d t o fit th e data fo reac h analyte
. Th e dat a were no t force d throug h zero durin g th e fitting process . Eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac yrequirements o

f 100±25 % (100±30 % fo rth e lowest curve point) were met fo ral l analytes
. Th e correlatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFOS
. Th e PFO S linea ran d branche d isomer s were integrate d togethe ras on e analyt e pea k

an d no t separatel yas don e fo rth e 10/12/1 1 an d 10/20/1 1 analyses
. Thes e sample s di d no t requir e th e linea ran d branche d isomer s t o b e integrate d separatel ysince th e sample s had lo w amounts o

fPFO S an d were aide d wit h th e additio n ofintema l standar d "Cs-PFOS
. 

## 8. 2 Syste m Suitability Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofth e analytica l sequence t o demonstrat e overal l syste m suitability
. Th e acceptance criteri a 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 met fo rPFBS , PFHS , an d PFO S fo reac h analytica l batc h wit h th e exceptio n ofth e 10/12/1 1 an d 10/20/1 1 analyses , i n whic h PFO S (linea ran d branche d summed ) had a n are a coun t RS D of7.5 % i n th e 10/12/1 1 analysi s an d 9.1 % i n th e 10/20/1 1 analysis
. Ametho d deviatio n i s include d i n Attachmen t D
. 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LOQ fo rthi s analysi s i s th e lowes t non-zer o calibratio n standar

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

yrequirements an d fo rwhic h th e are a counts are a t least twic e thos e o

fth e appropriat e blanks
. Th e LOQ s associate d wit h th e sampl e analysi s are liste d i n th e tabl e below
. Tabl e 6 . Limi t o

fQuantitatio n (LOQ) . Analysis Date Dilution PFBS LOQ, nglmL PFHS

LOQ, nglmL PFOS

LOQ, nglmL

10/12/1 1 1 0.040 0 0.025 0 0.232
10/12/1 1 5 0.20 0 0.12 5 1.1 6 10/12/1 1 1 0 0.40 0 0.25 0 2.32 10/12/1 1 2 0 0.80 0 0.50 0 4.6 4 10/12/1 5 0 2.0 0 1.2 5 11. 6 10/12/1 1 100 4.0 0 2.5 0 23. 2 10/12/1 1
50 0 20. 0 12. 5 11 6 10/20/1 1 1 NA 0.025 0 0.0232 10/20/1 50 0 N A 12. 5 11. 6 10/24/1 1 1 N A N A 0.0232 NA= No t Applicable ; analytica l results fo rwer e no t reporte d fro m th e njn
. 

### 8. 4 Continuin g Calibratio n Durin g th e cours e o

feac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l reporte d sample s were brackete d b yCCVs that met metho d criteri a o f100 % ±25 % wit h th e exceptio n o fsevera l CCVs analyze d fo rPFO S o n 10/12/1 1 whic h had recoverie s greate rtha n 125 % (127 % - 135%)
. Sampl e sets brackete d b yth e non-complian t CCVs include : DA L G W317L , DA L G W324L ,
Pag e 1 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### DA L G W327R , DA L G W328R , DA L G W328L , DA L G W330R , DA L G W330L , DA ; G W331S , DA L G W335R , an d DA L G WGRS04
. Ametho d deviatio n i s include d wit h th e ra wdata
. 

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

s were prepare d an d analyze d wit h th e samples : metho d procedura l blanks , field/trip blanks , an d equipmen t blanks
. Metho d procedura l blan k results were reviewe d an d use d t o evaluate metho d performance an d t o determin e th e LOQ fo reac h analyte
. 8. 6 La b Contro l Spike s (LCSs ) Three lab control spike levels were prepared and analyzed in triplicate

with each preparation

set. LCSs were prepared

by spiking known amounts of

the analyte into 10 mLof Milli Q water or synthetic groundwater

to produce the desired concentration. The

spiked water samples were

then analyzed

in the same manner

as the samples. The

method acceptance

criteria, average

of LCS at each level should be within 100%± 20% with an RSD <20%. Fo rth e 10/12/1 1 an d 10/20/1 1 analyses , th e PFO S LC S recover ywa s base d o n th e su m ofth e calculate d concentration s ofth e linea ran d branche d isomer s integrate d separately
. Al l LCS s met acceptance criteri a fo reac h analyt e except fo rth e 0.2pp b an d 2pp b LCS s fo rPFO S i n th e 10/20/1 1 analysis , whic h had averag e recoverie s o f74.1 % an d 78.1 % respectively
. Ametho d deviatio n i s include d wit h th e ra

wdata
. Th e followin g calculation s were use d t o generat e dat a i n Tabl e 7 fo rlaborator ycontro l spikes
. LC S Percen t Recover

y= Calculate d Concentration , Spike Concentratio n 100 % LCS % RS D = standard deviatio n LC S replicate s ,

averag e LC S recover

y 100 %


### Tabl e 7 . Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Analyze d 10/12/1 1 Extema l Calibratio n PFB S PFHS Spiked Concentration Calculated

Concentration Spiked Concentration Calculated

Concentration LabID (nglmL) (nglmL) VoRecovery (nglmL) (nglmL) %Recovery LCS-111007- 1 2.0 0 2.07 10 3 2.0 0 2.1 0 10 5 LCS-111007- 2 2.0 0 2.0 4 102 2.0 0 2.0 3 10 1 LCS-111007- 3 2.0 0 2.1 0 10 5 2.0 0 2.0 9 104 Averag e ±%RS D 103 % ±1.5 % 103% ±2.0 % LCS-111007- 4 20. 0 18. 4 92. 0 20. 0 18. 3 91. 6 LCS-111007- 5 20. 0 19. 0 95. 2 20. 0 19. 1 95. 6 LCS-111007- 6 20. 0 19. 3 96. 5 20. 0 18. 8 93. 9 Averag e ±%RS D 94.6 % ±2.4 % 93.7% ±2.1 % LCS-111007- 7 49. 8 50. 8 102 49. 8 54. 7 11 0 LCS-111007- 8 49. 8 49. 6 99. 6 49. 8 50. 4 10 1 LCS-111007- 9 49. 8 50. 5 10 1 49. 8 51. 0 102 Averag e ±%RS D 101 % ±1.2 % 104 % ±4.7 %

Pag e 1 8 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### Tabl e 7 continued . Laboratory Contro l Spike Recovery . ETS-8-044. 0 Analyze d 10/12/1 1 Extema l Calibratio n PFOS (Linear+Branched

summed) Spiked Calculated Calculated LabID Concentration

(nglmL) Cone

(Linear) (nglmL) Cone

(Branched) (nglmL) %Recovei y LCS-111007- 1 1.8 5 1.4

4 0.382 98. 5 LCS-111007- 2 1.8 5 1.3

2 0.354 90. 5 LCS-111007- 3 1.8 5 1.4

4 0.38 3 98. 5 Averag e ±%RS D 95.8% ±4.8 % LCS-111007- 4 18. 5 14. 4 3.7 6 98. 2 LCS-111007- 5 18. 5 15. 2 3.9 5 10 4 LCS-111007- 6 18. 5 14. 4 3.7 8 98. 3 Averag e ±%RS D 100 % ±3.1 % LCS-111007- 7 46. 2 35. 1 9.70 97. 0 LCS-111007- 8 46. 2 35. 1 9.5 6 96. 7 LCS-111007- 9 46. 2 36. 1 9.6 9 99. 1 Averag e ±%RS D 97.6% ±1.4 % ETS-8-044. 0 Analyze d 10/20/1 1 Extema l Calibratio n PFHS Spiked Concentration Calculated

Concentration LabID (nglmL) (nglmL) VoRecovery LCS-111020- 1 2.0 0 0.17 4 86. 8 LCS-111020- 2 2.0 0 0.17 2 86. 1 LCS-111020- S 2.0 0 0.17 0 85. 1 Averag e ±%RS D 86.0% ±0.99 % LCS-111020- 4 2.0 0 1.76 87. 8 LCS-111020- 5 2.0 0 1.6 5 82. 6 LCS-111020- 6 2.0 0 1.70 84. 8 Averag e ±%RS D 85.1 % ±3.1 % LCS-111020- 7 20. 0 17. 8 89. 0 LCS-111020- 8 20. 0 16. 8 84. 2 LCS-111020- 9 20. 0 17. 4 87. 1 Averag e ±%RS D 86.8% ±2.8 %

Pag e 1 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### Tabl e 7 continued . Laboratory Contro l Spike Recovery . ETS-8-044. 0 Analyze d 10/20/1 1 Extema l Calibratio n PFOS (Linear+Branched

summed) LabID Spiked

Concentration (nglmL) Calculated

Cone (Uneai) (nglmL) Calculated

Cone (Branched) (nglmL) VoRecovery LCS-111020- 1 0.18 5 0.11 3 0.032 0 78. 4 LCS-111020- 2 0.18 5 0.11 2 0.029 9 76. 7 LCS-111020- S 0.18 5 0.098 9 0.025 5 67. 2 Averag e ±%RS D 74.1 % ±8.1% TM LGS-111020- 4 1.8 5 1.1 6 0.31 6 79. 8 LCS-111020- 5 1.8 5 1.0

7 0.305 74. 3 LCS-111020- 6 1.8 5 1.1 7 0.31 2 80. 1 Averag e ±%RS D 78.1 % ±4.2%' " LCS-111020- 7 18. 5 13. 7 3.52 93. 1 LCS-111020- 8 18. 5 13. 0 3.4 0 88. 6 LCS-111020- 9 18. 5 13. 2 3.2 8 89. 1 Averag e ±%RS D 90.3 % ±2.7 % ETS-8-044. 0 Analyze d 10/24/1 1 Intema l Standar

d Calibratio n PFOS (Linear + Branched) Spiked Concentration Calculated

Concentration LabID (nglmL) (nglmL) VoRecovery LCS-111024- 1 0.184 0.16 6 90. 0 LCS-111024- 2 0.184 0.16 6 90. 1 LCS-111024- 3 0.184 0.16 7 90. 9 Averag e ±%RS D 90.3% ±0.55 % LCS-111024 4 1.8 4 1.7

2 93. 7 LCS-111024- 5 1.8 4 1.7

2 93. 5 LCS-111024- 6 1.8 4 1.6

5 89. 7 Averag e ±%RS D 92.3% ±2.4 % LCS-111024- 7 9.2 2 8.8 9 96. 4 LCS-111024- 8 9.2 2 8.0 1 86. 9 LCS-111024- 9 9.2 2 8.9 1 96. 7 Averag e ±%RS D 93.3% ±6.0 % (1 ) LC S averag e di d no t meet acceptance criteri a o f100 ±20% .

Pag e 2 0 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



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

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

yan d precision
. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2
. Th e standar d deviatio n i s calculate d fo rth e set o faccurac yresults (i n % ) obtaine d fo rth e LC S 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 o f95% . Th e most recen t 5 0 dat a points were use d t o generat e th e metho d uncertaint

yvalues
. Th e analytica l metho d uncertaint yfo rPFO S whe n determine d b yETS-12 - 012. 2 wa s ±18% , however , since th e averag e recover yo fth e lo wset ofLC S sample s analyze d o n 10/12/1 1 had a n averag e recover yof74. 1 % , th e analytica l uncertaint yfo rthi s analysi s wil l b e expande d fo rPFO S t o ±26% . Tabl e 8 . Analytica l Uncertainty
. Analyt e Standar d Deviatio n Metho d Uncertaint y PFB S 6.9 3 ±14 % PFH S 9.0 5 ±18 % . PFO S N A ±26 % (1 ) NA = No

t Applicabl e 

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

ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o shippin g sampl e container s fo rsampl e collection
. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of100±30 % confir m tha t "unknown " components i n th e sampl e matri xd o no t significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Fiel d matri xspik e concentration s must b e 50 % o fth e sampl e concentratio n t o b e considere d a n appropriat e field spike
. Fiel d matri xspike s are presente d i n sectio n 9 o fthi s report . Tabl e 9 . Fiel d IVIatri xSpikes
. Samplin g Locatio n Spik e Leve l PFB S (ng/mL ) PFH S

(ng/mL ) PFO S

(ng/mL ) 317 L LowFM S Hig h FM S 1.00

10. 0 1.00

10. 0 1.00

10. 0 220R , 220L , 328 L Lo wFM S Hig h FM S 10. 0

10 0 10. 0

10 0 10. 0

10 0 203L , 222R , 227L , 227R , 3 1 OR , 324L , 327R , 330L , 331S , 335 R LowFM S Hig h FM S 10 0

100 0 10 0

100 0 10 0

100 0 GRS04 , 312R , 330 R LowFM S Hig h FM S 100 0

500 0 100 0

500 0 100 0

500 0 328 R LowFM S Hig h FM S 10 0

50 0 10 0

50 0 10 0

50 0 LowFM S 10. 0 10. 0 10. 0 Tri p Blan k

Set s 1 an d 2 Mi d FM S 10 0 10 0 10 0 Hig h FM S 100 0 100 0 100 0 (Sampl e Concentratio

no f FM S - Averag

e Concentration : FieldSampl e & FieldSampl

e Dup. ) FM S Recover y = * 100 % Spik e Concentrato

n
Pag e 2 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### d Bata Summary

and Discussion Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blank
. Results an d averag e value s are rounde d t o thre e significan t figures accordin g t o EP Aroundin g rules
. Becaus e o frounding , value s ma

yvar yslightl y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspike recoverie s meetin g th e metho d acceptance criteri a o f±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G W220 R (Tabl e 11 ) - Th e recover yofth e H S fo rPFO S wa s 61.9% . Since thi s wa s th e onl y appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFO S t o ±38% . DA L G W220 L (Tabl e 12 ) - Th e recover yofth e H S fo rPFO S wa s 61.9% . Since thi s wa s th e onl y appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFO S t o ±38% . DA L G W222 R (Tabl e 13 ) - Th e recover yo fth e H S fo rPFBS , PFHS , an d PFO S wa s 66.8% , 65. 1 % , an d 56.9% , respectively
. Since th e L S fo rPFB S met acceptance criteria , th e metho d uncertaint ywil l no t b e adjuste d fo rPFBS
. Since th e H S was th e onl yappropriat e spike leve l fo rPFH S an d PFOS , th e analytica l uncertaint

yhas bee n adjuste d fo rPFH S t o ±35 % an d fo rPFO S t o ±43% . DA L G W327 R (Tabl e 20 ) - Th e recover yo fth e H S fo rPFB S an d PFH S wa s 65.4 % an d 69. 1 % , respectively
. Since th e LS fo rPFB S an d PFH S met acceptance criteria , th e metho d uncertaint ywil l not b e adjusted
. DA L G W330 L (Tabl e 24 ) - Th e recover yo fth e H S fo rPFB S wa s 66.1% . Since thi s wa s th e onl y appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±34% . DA L G W331 S (Tabl e 25 ) - Th e recover yofth e H S fo rPFB S wa s 68.5% . Since thi s was th e onl y appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±32% . DA L G W335 R (Tabl e 26 ) - Th e recover yo fth e H S fo rPFB S wa s 69.1% . Since thi s wa s th e onl y appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±3 1 % . DA L G WGRS0 4 (Tabl e 27 ) - Th e recover yo fth e LS fo rPFO S wa s 63.0% . Since thi s wa s th e most appropriat e spike level , th e analytica l uncertaint yhas bee n adjuste d fo rPFO S t o ±37% . Tri p Blan k

1 (Tabl e 28 ) - Th e recover yo fth e M S fo rPFO S wa s 68.0% . Tri p Blan k

2 (Tabl e 29 ) - Th e recover yo fth e M S an d H S fo rPFO S was 65.9 % an d 68.9% , respectively
.

Pag e 2 2 o f9 9

### Tabl e 10 . DA L G W203 L 11093 0 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) %Recovery GLP1(K)1-02-22-00 1 DA L GW203 L 011093 0 24. 3 N A 148 NA 48 5 NA GLP10-01-02-22-O02 DALGW203 L D B 110930 22. 0 N A 135 NA 47 0 NA GLP10-01-02-22-00 3 DALGW203 L LS 110930 106 82. 9 23 0 88. 5 66 8 N C GLP10-01-02-22-004 DALGW203 L H S 110930 81 9 79. 6 95 2 81. 1 119 0 71. 2 Average Concentralion

(ng/mL) ± %RPD 23.2

ng/mL±9.9% 142 ng/mL±9.2% 478 ng/mL±3.1% N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. Sample s dilute d 50

xan d analyze d 10/12/11
. 

### Tabl e 11 . DA L G W220R11093 0 PPB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-00 5 DA L GW220 R 011093 0 4.6 9 N A 17 7 N A 26. 4 N A GLP10-01-02-22-00 6 DALGW220 R D B 110930 48 3 N A 18. 1 N A 28. 4 N A GLP10-01-02-22-00 7 DALGW220 R LS 110930 12. 7 79. 4 25. 3 74. 0 33. 4 N C GLP10-01-02-22-00 8 DALGW220RH S 110930 84. 4 79. 6 99. 0 81. 1 89. 3 61.9 TM Average Concentration

(ng/mL) ± %RPD 4.76

ng/mL±2.9% 17.9 ng/mL±2.2% 27.4 ng/mL± 7.3%^ N A= No t /\pplicabl e N O = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. Sample s dilute d 5

xan d analyze d 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100% ±30% . (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFO S t o ±38% .

Pag e 2 3 o f9 9

### Tabl e 12 . DA L G W220 L 110930 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-00 9 DA L GW220 L 011093 0 7.9 1 N A 37. 8 NA 46. 6 N A GLP10-01-02-22-01 0 DALGW220LD B 110930 7.8 3 N A 37. 4 N A 51. 7 N A GLP10-01-02-22-01 1 DA L GW220LL S 110930 15 7 78. 3 45. 1 N C 53. 3 N C GLP10-01-O2-22-01 2 DALGW220 L H S 110930 86. 3 78. 4 11 9 81. 4 11 1 .61.9 TM Average Concentration

(ng/mL) ± VoRPD 7.87 ng/mL±1.0% 37.6 ng/mL±1.1% 49.2ng/mL±10%'^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. Sample s dilute d 5

xan d analyze d 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100% ±30% . (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFO S t o ±38% . 

### Tabl e 13 . DA L G W222 R 11093 0 PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-01 3 DA L GW222 R 011093 0 62. 4 NA 42 7 NA 51 0 NA GLP10-01-02-22-01 4 DA L GW222RD B 110930 62. 5 NA 43 1 NA 51 2 NA GLP10-01-02-22-01 5 DALGW222 R LS 110930 149 86. 6 53 2 N C 62 5 N C GLP10-01-02-22-01 6 DALGW222 R H S 110930 73 0 66.8 TM 108 0 65. 1 TM 108 0 56.9 TM Average Concentration

(ng/mL) ± VoRPD 62.5

ng/mL±0.16% 429 ng/mL± 0.93% 511 ng/mL±0.39%'^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 50

xan d analyze d 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100% ±30% . TTi e analytica l uncertaint

ywil l b e adjuste d base d o n th e recover yo fth e mos

t appropriate spikin g level
. (2 ) TTi e analytica l uncertaint

yhas bee n adjuste d fo rPFH S t o ±35 % an d fo rPFO S t o ±43% .

Pag e 2 4 o f9 9

### Tabl e 14 . DA L G W227R11092 2 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) %Recovery GLP10-01-02-22-01 7 DA L GW227 R 011092 2 13. 1 N A 60. 3 N A 58 4 NA GLP10-01-02-22-01 8 DALGW227 R D B 11092 2 13 7 N A 63. 1 N A 57 2 NA GLP10-01-02-22-01 9 DALGW227RL S 110922 . 95. 7 82. 3 147 85. 3 63 7 N C GLP10-01-02-22-02 0 DALGW227 R H S 11092 2 83 2 81. 9 95 5 89. 3 138 0 80. 2 Average Concentration

(ng/mL) ± %RPD 13.4 ng/mL±4.5% 61.7 ng/mL±4.5% 578 ng/mL±2.1% N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 20

xan d analyze d 10/12/11
. 

### Tabl e 15 . DA L G W227 L 11092 2 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) %Recovery (ng/mL) VoRecovery GLP10-01-02-22-02 1 DA L GW227 L 011092 2 25 8 N A 68. 7 N A 48 2 N A GLP10-01-02-22-02 2 DALGW227 L D B 11092 2 25 4 N A 68. 3 N A 46 5 N A GLP10-01-02-22-02 3 DALGW227 L LS 11092 2 32 9 N C 147 78. 5 54 2 N C GLP10-01-02-22-02 4 DALGW227LH S 11092 2 96 6 71. 0 98 9 92. 1 130 0 82. 7 Average Concentration

(ng/mL) ± VoRPD 256

ng/mL±1.6% 68.5 ng/mL±0.58% 474 ng/mL±3.6% N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 20

xan d analyze d 10/12/11
. Fo rPFBS , th e H S wa s furthe rdilute d t o 40x .

Pag e 2 5 o f9 9

### Tabl e 16 . DA L G W3 1 O R 11092 8 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-02 5 DA L GW310R O 11092 8 71 6 N A 31 8 N A 60 0 NA GLP10-01-02-22-02 6 DA L G W3 1 O R D B 11092 8 74 3 N A 32 2 NA 62 1 N A GLP10-01-02-22-02 7 DA L G W3 1 O R L S 11092 8 78 2 N C 39 5 N C 69 2 N C GLP10-01-02-22-02 8 DA L G W3 1 O R H S 11092 8 145 0 72. 1 .108 0 76. 0 136 0 75. 0 Average Concentration

(ng/mL) ± VoRPD 730ng/mL±3.7% 320 ng/mL±1.3% 611 ng/mL±3.4% NA= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d lOO

xan d analyze d o n 10/12/11
. 

### Tabl e 17 . DA L G W312 R 11092 9 PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) %Recovery GLP10-O1-02-22-02 9 DA L GW312 R 011092 9 1130 N A 82 9 NA 138 0 N A GLP10-01-02-22-03 0 DALGW312 R D B 11092 9 115 0 N A 83 3 NA 150 0 N A GLP10-01-02-22-03 1 DALGW312 R LS 11092 9 191 0 77. 0 162 0 78. 9 219 0 75. 0 GLP10-01-02-22-032 DALGW312 R H S 11092 9 526 0 82. 4 515 0 86. 4 599 0 91. 0 Average Concentration

(ng/mL) ± %RPD 1140 ng/mL±1.8% 831 ng/mL±0.48% 1440 ng/mL±8.3% NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. Sample s dilute d 10O

xexcept H S was dilute d 500x . Sample s analyze d 10/12/11
.

Pag e 2 6 o f9 9

### Tabl e 18 . DA L G W317 L 11092 8 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-03 3 DA L G W317 L Oi l 092 8 <0.040 0 N A 010 3 NA 021 4 N A GLP10-01-02-22-034 DALGW317 L D B 11092 8 <0.040 0 N A 0.093 8 NA 019 6 N A GLP10-01-02-22-03 5 DALGW317 L L S 11092 8 081 3 81. 3 0.90 7 80. 9 0.92 3 71. 8 GLP10-01-02-22-03 6 DALGW317 L H S 11092 8 8.3 7 83. 7 8.65 85. 5 NA<^ > NA*^ ' Average Concentration

(ng/mL) ± VoRPD <0.0400 ng/mL 0.0984 ng/mL±9.3% 0.205 ng/mL±8.8% NA = No t Applicabl e Results fo rPFB S an d PFH S reporte d fro m 10/12/1 1 analysis
. Result s fo rPFO S reporte d firo m 10/24/1 1 intema l standar d analysis
. (1 ) Sampl e was no

t analyzed since th e spik

e leve l wa s no

t expecte d t o b e appropriate a s compare d to th e sampl e concentration
. 

### Tabl e 19 . DA L G W324 L 11092 3 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) VoRecovery (rtg/mL) %Recovery GLP10-01-02-22-03 7 DA L GW324 L 011092 3 70. 0 N A 82. 9 NA 21 2 NA GLP10-01-02-22-O38 DALGW324 L D B 11092 3 70. 0 N A 82. 1 NA 21 0 NA GLP10-01-02-22-03 9 DA L GW324 L LS11092 3 146 76. 0 163 80. 5 27 4 N C GLP10-01-02-22-04 0 DALGW324 L H S 11092 3 80 0 73. 0 84 6 76. 4 99 9 78. 9 Average Concentration

(ng/mL) ± VoRPD 70.0

ng/mL±0.0% 82.5 ng/mL±0.97% 211 ng/mL ±0.95% NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 50xan d analyze d 10/12/11
.

Pag e 2 7 o f9 9

### Tabl e 20 . DA L G W327 R 11092 8 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-04 1 DA L GW327 R 011092 8 51. 4 NA 125 N A 39 4 N A GLP10-01-02-22-042 DALGW327 R D B 11092 8 51. 7 NA 127 N A 39 9 N A GLP10-01-02-22-04 3 DA L GW327 R LS11092 8 135 83. 5 21 4 88. 0 48 5 N C GLP10-01-02-22-044 DALGW327 R H S 11092 8 70 6 65.4 TM 81 7 69. 1 TM 1140 74. 4 Average Concentration

(ng/mL) ± VoRPD 51.6

ng/mL±0.58% 126 ng/mL±1.6% 397 ng/mL±1.3% N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. Sample s dilute d 50

xan d analyze d 10/12/11
. (1 ) Fiel d matri

xspik e di d no t mee t metho d acceptanc

e criteri a o

f100 % ±30% . Th e analytica l uncertaint y wil l b e adjuste d base d on the recover

yo fth e mos t appropriat

e spiking level . 

### Tabl e 21 . DA L G W328 R 11092 7 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-O2-22-O4

5 DA L GW328 R 011092 7 27. 7 N A 57. 2 NA 178 N A GLP10-01-02-22-04 6 DALGW328 R D B 11092 7 28. 1 N A 58. 5 N A 178 N A GLP10-01-02-22-04 7 DALGW328RL S 11092 7 10 6 78. 1 13 7 79. 2 24 9 71. 5 GLP10-01-02-22-04 8 DALGW328 R H S 11092 7 38 0 70. 4 42 6 73. 6 54 5 73. 5 Average Concentration

(ng/mL) ± VoRPD 27. 9 ng/m L ±14 % 57.9 ng/mL±2.2% 178 ng/mL±0.28% N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 20

xan d analyze d 10/12/11
.

Pag e 2 8 o f9 9

### Tabl e 22 . DA L G W328 L 11092 8 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-04 9 DA L GW328 L 011092 8 40. 3 N A 18. 3 NA 1.3 1 N A GLP10-01-02-22-05 0 DALGW328 L D B 11092 8 40. 3 N A 18. 5 NA 1.26 N A GLP10-01-02-22-05 1 DA L GW328LL S 11092 8 47. 9 76. 0 26 7 83. 0 8.6 4 73. 6 GLP10-01-02-22-05 2 DALGW328 L H S 11092 8 11 5 74. 7 98. 2 79. 8 NA'^ ' NA'^ ' Average Concentration

(ng/mL) ± VoRPD 40.3

ng/mL±0.0% 18.4ng/mL±1.1Vo 1.29 ng/mL±3.9% NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d lOxan d analyze d fo rPFB S an d PFH S o n 10/12/11
. Result s fo rPFO S reporte d o n undilute d sample s analyze d 10/24/1 1 b yintema l standar

d calibration
. (1 ) Sampl e was no

t analyze d since th e spik

e leve l wa s no

t expecte d t o b e appropriate a s compare d to th e sampl e concentration
. 

### Tabl e 23 . DA L G W330 R 11092 8 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-05 3 DA L GW330 R 011092 8 207 0 N A 197 NA 60 0 NA GLP10-01-02-22-05 4 DALGW330 R D B 11092 8 206 0 N A 194 NA 58 6 N A GLP10-01-02-22-05 5 DALGW330RL S 11092 8 278 0 N C 95 8 76. 3 1430 83. 7 GLP10-01-02-22-05 6 DALGW330 R H S 11092 8 598 0 78. 3 436 0 83. 3 529 0 93. 9 Average Concentration

(ng/mL) ± VoRPD 3070

ng/mL±OMVo 196 ng/mL±1.5% 593 ng/m L ±2.4 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d lOO

xexcept H S was dilute d 500x . Sample s analyze d 10/12/11
.

Pag e 2 9 o f9 9

### Tabl e 24 . DA L G W330 L 11092 8 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-05 7 DA L GW330 L 011092 8 544 N A 43 1 NA 16 8 N A GLP10-01-02-22-05 8 DALGW330 L D B 11092 8 51 5 N A 43 7 NA 17 0 N A GLP10-01-02-22-05 9 DA L GW330 L LS11092 8 50 4 N C 52 6 N C 25 4 85. 0 GLP10-01-02-22-06 0 DALGW330 L H S 11092 8 119 0 66. 1 TM 1280 84. 6 107 0 90 1 Average Concentration

(ng/mL) ± VoRPD 530 ng/m L ±5.5%* ^ 434 ng/mL± 1.4% 169

ng/mL±1.4% NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. Sample s dilute d 50

xan d analyze d 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a o f100% ±30% . (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±34% . 

### Tabl e 25 . DA L G W331 S 11092 9 PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) %Recovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-06 1 DA L GW331S 0 11092 9 535 NA 33 6 N A 51 7 N A GLP10-01-02-22-062 DALGW331SD B 11092 9 51 5 NA 32 6 NA 49 4 N A GLP10-01-02-22-06 3 DALGW331SL S 11092 9 59 6 N C 40 3 N C 59 8 92. 5 GLP10-01-02-22-064 DALGW331SHS11092 9 121 0 68.5 TM 109 0 75. 9 131 0 80. 4 Average Concentration

(ng/mL) ± VoRPD 525

ng/mL±3.8%'^ 331 ng/mL±3.0% 506 ng/mL±4.5% NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level
. Sample s dilute d 50

xan d analyze d o n 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100% ±30% . (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±32% .

Pag e 3 0 o f9 9

### Tabl e 26 . DA L G W335 R 11092 7 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-06 5 DA L GW335 R 011092 7 73 5 NA 143 0 N A - 340 0 NA GLP10-01-02-22-06 6 DALGW335 R D B 11092 7 74 4 NA 140 0 N A 329 0 NA GLP10-01-02-22-06 7 DA L GW335RL S 11092 7 74 8 N C NA<^ ' NA<^

> NA<^' NA(^ ' GLP10-01-02-22-06 8 DALGW335 R H S 11092 7 1430 69. 1 TM 218 0 76. 5 417 0 N C Average Concentration

(ng/mL) ± VoRPD 1080ng/mL±3.7%^ 1420ng/mL±2.1% 335 0 ng/m L ±3.3%*' " N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d 50

xfo rPFB S an d analyze d o n 10/12/11
. Sample s wer e dilute d 500

xfo rPFH S an d PFO S an d analyze d o n 10/20/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100% ±30% . (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFB S t o ±31% . (3 ) Sampl e vra

s no t analyze d since th e spik

e leve l was no

t expecte d t o b e appropriate a s compare d t o th e sampl e concentration
. (4 ) N o appropriate spik

e leve l was availabl e t o asses s sampl e recover yfo rPFOS
.

Pag e 3 1 o f9 9

### Tabl e 27 . DA L G WGRS0 4 11093 0 GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-06 9 DA L GWGRS0 4 011093 0 172 0 N A 622 0 N A 132 0 N A GLP10-01-02-22-07 0 DA L G WGRS04 D B 110930 166 0 N A 589 0 N A 134 0 N A GLP10-01-02-22-07 1 DA L GWGRS0 4 LS11093 0 246 0 77. 0 NA<^ ' NA'^ ' 196 0 63. 0 GLP10-01-02-22-072 DA L G WGRS04 H S 110930 553 0 76. 8 1180 0 11 5 533 0 80. 0 Average Concentration

(ng/mL) ± VoRPD 1690

ng/mL±3.6% 6060 ng/m L ±5.5 % 1330 ng/mL±1.5%'^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. Sample s dilute d lOO

xfo rPFB S an d PFOS , except H S was dilute d 500x , an d analyze d o n 10/12/11
. Sample s dilute d 500 xfo rPFH S an d analyze d o n 10/20/11
. (1 ) Sampl e vra

s no t analyze d since th e spike leve l wa s no t expecte d t o b e appropriate a s compare d t o th e sampl e concentration
. (2 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100 % ±30% . TTi e analytica l uncertaint

ywil l b e adjuste d base d o n th e recover yofth e mos

t appropriate spikin g level
. (3 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFO S to ±37% . 

### Tabl e 28 . Tri p Blan k

1 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Descrfpt/o n (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-074 DALGWTRIP0 1 0 <0.040 0 N A <0.025 0 NA <0.18 3 N A GLP10-01-02-22-07 5 DALGWTRIP0 1 LS 8.1 8 81. 8 8.35 83. 5 7.9 8 79. 8 GLP10-01-02-22-07 6 DALGWTRIP0 1 M S 81. 1 81. 1 82. 3 82. 3 68. 0 68. 0 GLP10-01-02-22-07 7 DALGWTRIP0 1 H S 86 7 86. 7 86 9 86. 9 72 7 72. 7 NA = No t Applicabl e FM S Mi d dilute d 10x , FM S Hig h dilute d lOOx, an d analyze d o n 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet method acceptance criteri a of100 % ±30% .

Pag e 32 o f9 9

### Tabl e 29 . Tri p Blan k 2 GLP10-01-02 ; Interi m Repor t 2 2 /^alysi s ofPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3MUMSID Description (ng/mL) VoRecovery (ng/mL) VoRecovery (ng/mL) VoRecovery GLP10-01-02-22-07 8 DALGWTRIP0 2 0 <0.040 0 N A <0.025 0 NA <018 3 NA GLP10-01-02-22-07 9 DALGWTRIP02L S 8.0 9 80. 9 8.2 7 82. 7 7.94 79. 4 GLP10-01-02-22-08 0 DALGWTRIP02M S 79. 1 79. 1 80. 1 80. 1 65. 9 65.9 TM GLP10-01-02-22-08 1 DALGWTRIP02H S 83 8 83. 8 84 2 84. 2 68 9 68. 9 N A= Not/Vpplicabl e FM S Mi d dilute d lOx , FM S Hig h dilute d lOOx, an d analyze d o n 10/12/11
. (1 ) Fiel d matri xspik

e di d no t meet metho d acceptance criteri a o f100 % ±30% . 

### Tabl e 30 . Equipmen t Rinseat e Blank s PFB S PFHS PFO S 3M LIMS ID Description Concentration (ng/mL) Concentration

(ng/mL) Concentration

(ng/mL) GLP10-01-02-22-08 2 GLP10-01-02-22-08 3 DALGW203 L R B 11093 0 DALGW220 L R B 11093 0 <0.040 0 <0.040 0 <0.025 0

<0.025 0 <0.232

<0.232 Sampl e was analyze d o n 10/12/11
.

Pag e 3 3 of9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### 10 Conclusion Laborator ycontro l spike s an d field 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
. 11 '^niafa/Sample

Retention 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
. 

## 12 Attachments Attachmen t A : Protoco l Amendmen t 2 2 (Genera l Projec t Outiine ) 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 3 4 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



## 13 Signatures 

## / 2

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

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

# 'A Gar yHohenstein/Sponso rRepresentative Date

/ / Date Jaisimh a Kesari , Stud yDirecto r

Pag e 3 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 3 6 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater Srd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-01 Amendment

22
Study Title Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

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

PROTOCO L AMENDMEN TNO . 2 2

Amendment

Date: Septembe r14 , 201 1 Performing

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

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

Project

Identification GLP10-01-0 1
Sampling

Event Decatu r3'^

^ Quarte rGroundwate rSamplin g

Page 1 o f7 Pag e 3 7 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater 3rd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-01 Amendment

22 

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

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

PROTOCOLREADS: 

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

AMEND TO READ: 

### N o change s t o th e wordin g ofth 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 at Decatur , AL , an d conducte d a s par t ofth e 3 M Decatu rPhas e 3 Progra m fo rPFO A(GLP10-01-01)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e o fth e wee k o fSeptembe r19 . Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s projec t GLP10-01-01-2 2 an d reporte d a s interi m repor t GLP10-01-01-122 , (reflectin g stud yGLP10-01 - 0 1 an d amendmen t -22)
.
Reason: 

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

Pag e 2 o f7 Pag e 3 8 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater Srd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-01 Amendment

22 

## Amendmen t Approva l 

# Vy Gar yHohen s tein
. Sponso rRepresentative Date



# ikJi Date Clesto n C
. Lange , Principa l Analytica l Investigato r

Willia m Reagen , EH 6 Opn s Environmenta l La b Managemen t Date

Jaisimh a Kes : Stud yDirecto r

Pag e 3 o f7 Pag e 3 9 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater Srd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-0f Amendment

22 

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

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

Clesto n Lange , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charie s Young , Westo n Solution s Date : Septembe r14 , 201 1 Subject : Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 2 2 - Decatu r3' " Quarte r201 1 Groundwate rSamplin g 

## 1 Genera l Projec t Informatio n
3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , IVI N 55144-100 0 Phone:(651)737-357 0 Qahohenstein(@mmm.co m 3N I Environmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 Contact s wkreaQen©mmm.co m Principa l Analytica l Investigato r Clesto n Lang e SW l EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cci a naetffimm m .co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinak(a>westonsolutions.co m Phone : (334)-332-912 3 La b Reques t Numbe r GLP10-01-01-2 2 •Si xDigi t Departmen t Numbe r Dept #530711 , Project #002267444 9 Projec t Schedule/Tes t Date s Samplin g schedule d fo rth e wee k o fSeptembe r19 , 201 1 

### All verbal and written correspondence

will be directed to Gary Hohenstein.
Pag e 4 o f7 Pag e 4 0 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater Srd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-01 Amendment

22 

## 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m seventee n groundwate rwell s fo rPerfluorooctanoi cAci d (PFOA)
. Analyse s wil l b e conducte d unde rth e GL P requirement s ofEP ATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792 . Groundwate rsample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k o f Septembe r19 , 2011 . Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d
. spike s t o ensur e tha t result s fo rPFOAar e ofa know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar

yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-01-22
. 3 Projec t Schedul e Sampl e collectio n bottle s wil l be prepare d b yth e 3 M Environmenta l Laboratory
. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t to 3 M Decatu rfo rarriva l b yFriday , Septembe r16 , 2011 . Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection
. Marti n Smit h \

Westo n Traile r 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 rPFOA
. Atota l o feightee n samplin g location s hav e bee n specified
. Fo reac h samplin g location , fou rsampl e bottle s wil l b e collecte d (sample , sampl e duplicate , lo wfiel d matri xspike , an d hig h field matri xspike)
. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL
. Two sets o ftri p blan k

spike s consistin g ofreagent-grad e water , a s wel l a s WJ

O additiona l bottle s t o b e use d fo rth e preparatio n o fequipmen t rinseate blanks , wil l b e prepare d a t th e 3 M Environmenta l Laborator yan d sen t to th e samplin g locatio n wiU i th e othe rbottles
. Results fro m GLP10-01-01-02 , GLP10-01-01-09 , an d GLP10-01-01-1 7 were use d to detennin e th e field matri xspik e level s fo rGLP10-01-01-2 2 liste d i n Tabl e 1 . Tabl e 1 . Samplin g Location s an d Fiel d Matri xSpike levels . Wel l No . Sampl e Leve l Spike Cone . (ng/mL ) 317 L Low 1 Hig h 1 0 220R , 220L , 328 L Lo w 1 0 Hig h 10 0 203L , 222R , 227R , 227L , 310R , 324L , 327R , 330L , an d 331 S Low 10 0 203L , 222R , 227R , 227L , 310R , 324L , 327R , 330L , an d 331 S Hig h 100 0 GRS04 , 312R
. 330R , an d 335 S Low 100 0 Hig h 500 0 328 R Lo w 10 0 Hig h 50 0 Tri p Blan k

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

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

Set s 1 an d 2 Hig h 100 0

Pag e 5 o f7 Pag e 4 1 o f9 9GLP10-01-02; Interim Report 22 Analysis of PFBS, PFHS, and

PFOS in Groundwater Srd Quarter Sampling

- 2011 

### Analytical

Protocol:

GLP10-01-01 Amendment

22 

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

yHig h Perfomnanc

e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Du e t o previou s data fo rthes e samplin g location s (GLP10-01-01-02 , GLP10-01-01-09 , an d GLP10 - 01-01-17) , sample s GLP10-01-01-2 2 wil l most likel yrequir e dilution
. Sample s requirin g dilutio n wil l b e prepare d i n Milli- Q wate rprio rto analysi s b yETS-8-044.0
. Th e data qualit yobjective s fo rthes e studie s ar e quantitative results fo rtiie targe t analyte s wit h a n analytica l accurac yo f100+30% . Fiel d matri xspike s no t yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor t an d th e filia l accurac

ystatemen t ma

yb e adjuste d accordingly
. Alternately , sample s ma

yb e analyze d b

yETS 8-110. 1 "Analysi s o fFluorochemical s i n Exti-act s Usin g HPLC Electrospray-Mas s Spectrometry-Mas s Spectrometr ya s a n analytica l reference fo rth e sampl e location s analyze d b

ydirec t on-colum n injectio n analysi s ofsample s dilute d wit h methano l a s oppose d t o Milli- Q water . Calibratio n curve s use d fo rbot h ETS-8-044. 0 an d ETS-8-110. 1 wil l b e constructe d usin g a referenc e materia l containin g bot h linea ran d branche d isomer s ofPFOA
. Fiel d matii xspike s wil l b e prepare d wit h a solutio n prepare d wit h a reference materia l containin g predominantl ylinea rPFOA
. Laborator ycontro l sample s (LCS ) o f linea ran d branche d PFO Awil l b e prepare d a

t thre e concentratio n levels
. 

## 6 Reportin g Requirement s . Fo reac h samplin g location , th e repor t wil l contai n th e results fo rUi e sample , sampl e duplicate , an d th e field mati-ixspikes
. Tri p blan k

sets wil l b e reporte d fo rth e samplin g even t a s wil l an yequipmen t blank s prepare d i n th e field
. Laborator

ycontro l spike s o

freagen t wate rprepare d a t th e time o fsampl e extractio n wil l als o b e reporte d an d use d t o evaluat e Ui e overal l metho d accurac yan d precision
. Metho d blank s ofreagen t vrate r prepare d a

t th e tim e ofsampl e exti-actio n wil l be use d t o determin e th e metho d detectio n limit
. An ylaborator y mati-ixspike s that ma

yb e prepare d wil l als o b e include d i n th e final report . 7 Emai l Correspondenc e • Attachmen t A : Samplin g Bottl e Request

Pag e 6 o f7 Pag e 4 2 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 Analytical

Protocol:

GLP10-01-01 Amendment

22 From : Frinak , Timoth yR
. . Sent : Monday , Septembe r12 , 201 1 10:4 8 A M To : Young , Charle s T
. Cc : Smith , Mart:in ; Johnson , Kevi n A. ; Missildine , Bre t C
. Subject : Bottle s - G Wsamplin g Decatur , A L Charlie , Th e 3" * quarte rG Wsamplin g wil l begi n nex t Monda ya t Decatur
. Th e samplin g fo rFC s wil l b e insid e thi s tim e an d includ e th e following : 203 L 220 R ' 220 L 

### 222 R 227 R 227 L 

### 310 R 317 L 324 L 328 R 328 L ,330 R 330 L 335 R GRS0 4 RW312 R RW327 R RW331 S W e wil l als o nee d Milli- Q wate ran d bottle s fo rtw o (2 ) rinseat e blan k samples
.

Pag e 7 o f7 Pag e 4 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


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

Pag e 4 4 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b b l 11012 a linear.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -1.81e+00 3 x'^ 2 + S.55e+005 x+ 1.68e+004 ( r= 0.9997 ) 1.7e 7 1.6e7
- 1.5e7
- 1.4e7
-

3 0 3 5 4 0 Concentration , ng/m L Dat a printe d b yST W Printin g Time : 11:10:2 9 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 o £1
Pag e 4 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

• bl l 1012 a branched.rd b (PFOS) : "Quadratic " Regressio n (" 1 /x " weighting) : y=-2.44e+00 3 x'^ 2 + 4.45e+00 5 x+ 1.66e+00 S ( r= 0.9999 ) 8.0e 6 . 7.5e6 ; 7.0e6^ 6.5e6^ 6.0e6^ 5.5e6^ 5.0e6^ 4.5e6^ c 8 4.0e6 ^ ro" < 3.5e6 ^ 3.0e6 ^ 2.5e6
- 2.0e 6 1.5e6 1.0e6
- 5.0e5 9 1 0 1 1 Concentration , ng/m L 1 2 1 3 1 4 1 5 1 6 1 7 1 8 1 9 Dat a printe d b yST W Printin g Time : 11:05:2 8 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 1
Pag e 4 6 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

** * Buste r J293020 3 Batc hName : blll012a.da b b l 11012a.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -5.75e+00 3 x'^ 2 + 6.98e+00 5 x+ 9.76e+00 3 ( r= 0.9998 ) S.1e7 S.0e7

4 5 5 0 5 5 Concentration , ng/m L 60 6 5 7 0 7 5 8 0 85 90 9 5 10 0 Dat a printe d byST

W Printin g Time : 10:54:5 0 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 o £1
Pag e 4 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

** • Buste r J293020 3 Batc hName : blll012a.da b b l 11012a.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -7.04e+00 S x'^ 2 + 8.84e+00 5 x+ 2.05e+00 4 ( r= 0.9999 )

4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 90 9 5 100
Dat a printe d b yST W Printin g Time : 10:53:4 4 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 1
Pag e 4 8 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b 

# I Sampt o Nome : til11012a017 ' Sarript e ID : •10007.27-8 - Rte : •b111012B
. PeaKNamo : 'PFOS - Mass{M) : '499.0/99. 0 armJ,499.0/B0. 0 amu,499.0/130. 0 Commani : '1. 0 ng'm L F C st d I n MiD I Q Watw * Annoialion: ' Sampl e Index : 1 7 Sampl aType ; Standar d Concentration : 0.73 2 ng/m L Calculate dCone : 0.76 7 ng/m L Acq . Date : 10/12/2 0 Modified : Proc . Algorilli i Nois e Percenta l Base . Sub . Win

< Peak-Split . Fa

i Repor t Larges t Min . Pea

k Height : Smoothin g Width ; R T Window :

Height : Star t Ti n ':4 9 P M

Peat 

# r SarapteName:-b111012B02e - Sampt e ID:-Solven t BJank' FOe: •bl11012a.wtf r Pea k Name : "PFOS * Mass{es) : •499.IV99. 0 am u .499.0/80. 0 am u ,499.0/130. 0 amu " Commen t "Mi i O Wat« rTN11-0334 " Annolatkm : ~ Sampl e irapl e Type : .ration :

Pea k Height :

! Relativ e RT ; Height ; Star t Tim e En dTime ;

13. 0 

# I SampleName:-b111012a030 - SamptelD:-LCS-111007- r Pea k Name : "PFOS " Mas»{es) : -499.0«9. 0 amu,499.0/80. 0 Comment : "2pp* ) LCS " Annotation : ~ Sanpl e Index ; 3 0 Sarapl e Type : O C Calc i Acq . Time ; Modified ; Proc . AJgorittio : Nois e Percentag e Base . Sub . Hindo : Peak-Split . Fact i 0/12 ,

Min . Min . Pea k W : Smoothin g M : R T Window : Expecte d R

T Us e Belativ t Pea) 1.25e5 - 1.20e5 - 1.15e5 - LlOe S I.OSeS I.OOeS9,S0e4 - 9.00e4 - 8.50e4 - S.00e4 - 7.50* 4 • 7.00e4• S.S0e4- S.00e4 ' 5.S0ft4 ' 5.00e4 ' 4.50e4 ' 4.00e4 ' 3.50e4 ' 3.00»4 ' 2.50»4 ' 2.00e 4 1.50e4 1.0064 5000.0 0 0.0 0 

# I Sampl e Name : *b111012a033 " Sampl e ID : •LCS-111M7-4 - File : 1)1110123, ' Pea k Name : "PFOS " Mass{es) : "499.0/99. 0 amu,499.0/80. 0 antu,499.0'130. 0 amu " Comment ; *20pp b LCS " Annoiatkxi : ~ Sampl e Index ; 3 3 Sampl e Type : Q C Concentration : 18. 5 ng/m L Calculate dCone : 14. 4 ng/n L Acq . Date : 10/12/201 1 Acq , Tine ; 8:«5:0 5 P M

1.0 0 0

Type ; Valle i

15. < r4291 5

16.9517.37-J7.4 6 Dat a printe d b yST W Printin g Time : 11:12:5 2 A M Printin g Date : Wednesday , Decembe r 07 , Pag e 1 o f 5
Pag e 4 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

** * Buste r J293020 3 Batc hName : blll012a.da b 

# I Sampl e Name : tlllOIZaOSe " Sampl e ID : 1.CS-111007-7 " Pea k Name : "PFOS " Ma»s{es) : "499.0/99. 0 amu,499.0/80. 0 a i Comment : "SOppb LCS " Annotatton;" " Sampl e Index : 3 6 Sampl e Type : O C Concentration : 16. 2 r Calculate d Cone : 35. 1 r Acq . Date : 10/12/201 1 Acq , Tine ; 9:4B:2 2 P M Modlfi i

. Algo l ntage : fiaae. Sub . Window : Peak-Split . Factor ; Repor tLarges tPea k Min . Pea kHeight : Pea kWidth : Smo c ) Wid t 2.1fl6 Z0e 6 1.9o6 - 1.SeE ' 1.7e 6 1.e«B ' 1.5ft6 - 1.4e6 ' 1.3e 6 1.2eel.leS 1.0e6- 9.0e S 8.0* 5 7.0e5 - 6.0e5 5.0e5 4.0e5 3.0e5 2.0e5 I SamriBName:T>in012a057 " Sampl e ID ; "GLP10^H-02-22-001 * File : "b111012a.wi r Pea k Name : 'PFOS ' M3ss(es) : "439.0/99. 0 a i • Commen t "DA L GW203L0 " Annoialioo: - Sampl e Index : 5 7 Sanpl e Type ; Unknow n Calculate d Cone : Acq . Date : lO i Acq . Time : 5: ! Modified : Proc . Algorithm : In l Nois e Percentage : Base . Sub . Uindow : u,499.a>'130. 0 amu "

liQua n - MQI I 5,0e5 ' 4.ae5 4.6e5 ' 4.4e5 ' 426 5 4.0e5 ' 3.8e5 ' 3.6eS ' 3,4e5 - 3.Ze 5 3.0e5 ' 2.8e5 ' 2.6a5 ' 2.4e5 - 2.2e5 ' 2.0e5 ' 1.ee 5 1.6e5 - 1.4e5 '


### Jl 

# I Sampl e Namo : "b111012a061 ' Sampl e ID : "GLPHW)1-02-22-005 " File : "b111012a.wr r Pea k Name : "PFOS " Ma*»(es) : "499.0/99. 0 amu.499.0/80, 0 amu,499.0/130. 0 Comment:-DA L G W220f t 0 " Annotatksn: -

Modified : Proc . Algorithm : Nois e Percentage :

Hin . Pea kHeight : Min . Pea kHidth : Smoothin g Width : :elliQua n - MQ I

Valle y l e : 15. 3 104726 0 c < Height ; Star tTi r E n d Tim e I SainpleName:"b111012aD69 " Sampl e ID : •GLP10-01-02-22-009 " File : •b11l012a.wi( r Pea k Name : "PFOS " M3ss(es): ' • Comment'DA L G W220 L 0 " Annotation: ' Sampl e Index : 6 9 sarapl e Type : Unknow n

Modified ; Y t Proc . Algorithm ; Inte l Base . Sub . window : Peak-Split . Factor :

Larges tPe a e a kHeight : e a kWidth : i n g Width ;

15. 3

64772 5 CO I 3.76et00 5

Dat a printe d b yST W Printin g Time : 11:12:5 2 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 2 o f 5
Pag e 5 0 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

I Sam;i«Nam»:-b111012a073 - Sampl e ID : ^3LP1CKI1^^2.22-013• Flo : •bl110l2a.wii r PM k Nam* : "PFOS - Mass<M]:'499.0/99. 0 anx],499.(VBD. O amu.499.0/130. 0 I Comn»nt:-DALGW222R0 - Annotalkm: -

Dat a printe d b yST W Printin g Time : 11:12:5 2 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 3 o f 5
Pag e 5 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

• * Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:12:5 2 AH Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 4 o f 5
Pag e 5 2 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

** * Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:12:5 2 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e Pag e 5 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS
. an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

I SamFteN3n«:'b1110l2aOi rSampl e ID:'10007-27-8 " FUe:"b111012a.wlf r • Pea k Name : 'PFOS * Ma»<es) : "499.0/99. 0 Bmu,499.0m0. 0 amu.499.<V130 Aam i • Commen t *1. 0 ng'm L F C st d m MP KQ Water

* Annotation : ~ Sampl e Index : 1 7 Sampl e Type ; Standar d Concentration ; 0.19 6 ng ' Calculate d Cone ; 0.19 7 n g Acq . Dato : 10/12/201 1 Acq . Time ; 3;07;4 9 P M 7.0e 4

e.5a4 G,0e 4 5.S»4 5,0e 4

3.Cle 4 25» 4 

# I Sampt o Name : "b111012a028 " Sampl e ID : "Solven t Blanit " Fi% : 'b111012a.wi r Pea k Name : 'PFOS ' Mass(es) : "499.0/99. 0 8mu.499.0/8a o amu,499.(V130^ amu " Comment : 'Mfl i 0 Wate rTN11-0334 * Annotation : Sampl e Index ; 2 B Sanpl e Type ; Unknow n Concentration : H/A Calculate dCone ; < 0 Acq . Date ; 10/12/201 1 Acq . Time : 6:59:3 7 P M Modified : Ye s B T Window : 30. 0 se c Expecte d RT : 15. 3 mi n Use Relative RT : tia

Area : Height ; Star t Ti n En d Time : 3.59e+00 2 cp s

Modified ; B T Window : Expecte d RT : 

# I Sampl e Name : *b111012aO3O " Sampl e ID : ^CS-111007-1 ' Pea k Name : "PFOS " Massfes) : "499.0/99. 0 amu.499.0/80. 0 Comment:"2ppbLCS " Annotation:' " Sampl e Index : 3 0 Sampl e Type : O C Concentration : 1.8 5 ng/n L,^5,5 . Calculate dCone : 0.3S 2 ng/n L Acq . Date : 10/12/201 1 1.20e5
- Acq . Time : 7:41:4 6 P M 1.15«5 - D* 0 se cl.lOeS 15. 3 mi n 1.05e5 - 1.00e5 11^ 2 mi n9.50e4

- ^ 9.00e4 - e400 4 cp s 15. 0 mi n8.50e 4 15, 3 mi n 8.00e4 ' 7.50e 4 g 7.00e4
- ^ 6.50e4 i6.00e4 .

- 5.50B 4 5.00O4
- 4.5004 4.00o4 3.50o4 3.00e 4 2.50» 4 2.00O 4 1.S0» 4 1.00o 4 5000.0 0 0.0 0 I SamploNamo:"b111012a033 " Sampl e ID : TCS-111007-4 ' File:"b1110l2a.wi( r Pea k Nan^ : 'PFOS * Mau{es) : "499.0/99. 0 a r • Commen t '20pp b LCS " Anrwtatlon: ' Sanpl e Index : 33 ig.O/BO. 0 amu,499.0/130. 0 a t

Height ; En dTiro
1S. « 17.3707-4 6 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16 ^ i.iOee 1.05e 6 1.00e 6 9.50eS ' 9.00e5 - 8.S0e5 8.00e 5 7.50e5 - 7.00e 5 6.50B 5 § • 6.00e 5 I " 5.50e 5 £ 5.00e 5 4.5ae 5 4.00e 5 3.50e 5 3.00e 5 230e 5 2.00e 5 1.50e5 1.00e5 5.00e 4 0.0 0 Dat a printe d b yST W Printin g Time : 11:08:4 7 A M Printin g Date ; Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 5
Pag e 5 4 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:08:4 7 A M Printin g Date : Wednesday , Decembe r 0 7 

### Pag e 55 o f 99GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

• Sampl e Name;'b111012a073 ' SamplelD: ' I PeaKNarrte : "PFOS " MaM<es):'499.0/99. 0 1 Comment : "DA L G W 222 R 0 " Anrwtatlon : " " Sanpl e Index ; 73 •GLPIOKH-02-22-013 " Fie : "b111012a.wi r ainu.499.a/80. 0 em u ,499.0/130. 0 amu '

5.4e 5 52e 5 5.0e5 ' 43e5 ' 4.6e 5 AAe5
- 4.2e 5 4.0e 5 3.8e 5 3.6e 5 3,4e 5 3.2e 5 3,0B 5 2^e 5 2.6e 5 2.4e 5 22e 5 2.0e S

12e 5 1.0eS e,0e 4 6.0e 4 4X)e 4 2J)e 4 4, 5 15. 0 1 5 J 16. 0 16. 5 17, 0 17. 5 I SanipleNflme:"bl110128081 " Sampl e ID : •6LP10^1-02-22-Oi rFile : "b111012a.wi r Pea k Name : "PFOS " M8ss{es) : •499.(V99. 0 amu,499.0/BO. O amu,499.0/130. 0 am f I CoowenfOALGW227R0 * Annotation: -

1.2e6 • 1.2e6 ' 1.1e6 ' 1.1e 6 1.0e6
- 9,5o 5 9.ae5 ' 8.5e5
- 8.0e5 ' 7.5e5
- 7.ae5
- 6.S«5 ' 6.0e5 ' 5.5e5 5.0e5
- 4.5e 5 4.0e5
- 3.5e 5 3.065
- 2.5e5
- 2.0o5
-

14. 5 15. 0 17. 0 17. 5 

# I Sampl e Name:'b111012aOSS " Sampl e ID:" ' Pea k Name : "PFOS " Maasfes) : '499,0/99. 0 a t Comment : DA L G W 227 L 0 ' Annolation : ~ Sampl e Index : a s 1.20e6 - 1.15e6 - I.IOee 1.05e6 - 1.00ee 9.50e5 - 9.00e5 - 8.50e5 - 8.00e5 - 7.S0a5 - 7.0085 - § • 6.50e5 - i 6.00*5 - s t 5.50e5
- 5.00e5
- 4.50e5
- 4.00e5 ' 3.50«5 ' 3.00e5
- 2.50e5
- 2.00e5 ' 1.50o5 LOOeS
-
' 5.00e4 ' 0.00
- 

# I SanipleName;"b111012a093 " Sampl e ID : •GLP1fr01-02-22-02S " File:"b111012a.WT r Pea k Name : "PFOS " Mass{es) : "499.0/99. 0 amu.499.0/80. 0 amu,499.0/130. 0 amu " Comment : 'DA L G W 310 R 0 " Annotation : ~
2.ee 5 2.5c 5 2.4e 5 2.3eS 2.2e 5 2.1e 5 2.0eS EKpecte dRT : Us e Relativ e RT ;
Height : Star t Ti l En dTin e

1.0o5 - g.0e4 - e.0e4 - 7.0O4- 6.0e4 - 5.0O4
- 4.0e4 - 3.0o4 - 2.0e4 - 14, 5 15. 0 15. 5 16, 0 16. 5 17. 0 17. 5 13. 5 14. 0 Dat aprinte db y ST W Printin g Time : 11:08:4 7 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 3 o f - 5 15. 5 16. 0 16. 5 17. 0 Time , mir

t
Pag e 5 6 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1
Buste r J293020 3 Batc hName : blll012a.da b 

# I Sampl e Name : •blll012a097 " Sampt o ID : 'GLPKW1-02-22-029 " Fie : "b111012a.wif r Pea k Name : 'PFOS " Mas5(es) : "499,0/99. 0 Bmu.499.0/B0. 0 amu,499.0/130, 0 " Comn>ent:-DALGW312R0 - Annolation: - 

## I Pea k Name : "PFOS " Mass{e») : "499.0/99, 0 Commen t "DA L GW324 L 0 " Annotation: ' ! Index : 10 9

14. 5 15. 0 15. 5 16. 0 16. 5 I Sampl e Name : "b111012a109 " Sampl e ID : "GLP10"01-02-22-03 rFde : "b111012a.wi i iu,499.0/80, 0 amu,499.0/130. 0 amu "

9.De4 ' S.0e4 ' 7.064
- 6,0»4 ' 5.0e4
- 4.0e4 ' 3.0e4 ' 2.0e4 ' 1.0e4 '
Sampl e Nanw : •b111012a117 * Sampl e ID : "GLP1&^1-02-22-041 ' Fie : •l>111012a.wif r 

# I Pea k Name : "PFOS " Mass(e»} ; "499.0/99. 0 Comment:"DALGW327R0 " Annotation: " Sampl e Index : 11 7 Sanpl e Type ; Unknow n Concentration : H/A iu,499.0/80. 0 amu,499.0/130. 0 amu " I SampleName:T>111012a121 " Sampi o ID;"GLP1O-O1-02-22-045 " Flle:-b11101Za,w« r

Height ; Star t Tit u EndTime : 22e5 - 2.0* 5

i.4e5
- 12e5
- 1.0e5
- e.0e4 ' e.0e4 ' 4.0e4 ' 2.0e 4 

# 1 Pea k Name ; "PFOS " Mass(e9) : "499,0/99. 0 a r • Commen t "DA L GW328 R 0 " Annotation: ' Sarnpl e Index : 12 1 Sampl e Type : Unknow n

Modified ;

Height ; Star t T : En d Tin . 2,64e40D5 cpa j,4S9.0/80.0amu,499,0/130. 0 amu '

3.4eS ' 3.265 - 3.0e5 - 2.86 5 2.ee5 - 2.4e5 ' 2.2e5 - 2.06 5
1.eeS 1.4e5 -

13. 0 13. 5 Dat a printe d b

yST W Printin g Time : 11:08:4 7 A M Printin g Date : Wednesday , Decembe r 07 , Pag e 4 o f 5
Pag e 5 7 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

I SamplaNam6:"b111012al33 ' Sampl e ID;"GLPIO-01-02-22-053 " Fle:"b111012a.w1f r

Modified ; R T Hindo i Expecte d 

### • Pea k Name : TFOS " Massfes) : "499.0«9. 0 am u ,499,0/80, 0 a r Comment ; "DA L GWSSOR C Annotation: - Sample Index; 133 Sanple Type: Unknown Concentration; H/A Calculated

Cone: 225. ng/mL Acq- Date; 10/14/2011 ^'^^ Acq . Time : 7:56:1 5 A M 2.8e5 Ye s 30. 0 se c 15. 3 mi n 2.665 Manua l 2.4e5 15. 2 mi n 5261 6 count s l.Sle-tOO S cp s "6 5 H . 9 mi n ^^• ^ 2.0e5

1.2e5 1,0eS 8.0e 4 8.06 4 4.0e 4 2.06 4 J,499.0/130.0amu *

4. 5 15. 0 1S. 5 16. 0 16. 5 17. 0 17. 5 I SampleN8ine:'bl1101Za141 " SampfeID:"GLP10-01-02-22-057 " F4e:"bl110128. w Pea k Name : "PFOS " Mass(es) ; '499.0/99. 0 aniu,499,0 / • Commen t "DA L GW330LO " Annolation: - Sanpl e Index : 14 1 Sampl e Type : Unknow n Calculate d Cone : 88. 5 ng/ra L 1,3e5
- Acq . Date : 10/14/201 1 Acq. Time; 10;45;10 AM ^-^^

1.2e5 Kodiried ; Ye a R TWindow : 30. 0 se c1.2e5 - Expecte d RT ; 15. 3 «i n Us e Relativ e RT : U o • " 1.1e 5 Int
. Type ; Manua l Retentio n Time : 15. 2 rain 1-0e 5 Area ; 78237 8 count s gj^
. Height : 1.14e-tO0 5 cp s Star tTime : 14. 9 ni n 9.0a4- En d Time ; 15. 3 mi n , e.5e4 B.De4 ' £ 7.5e4 . 7.0e4 •£ « 6.5e4 M 6.0e4 5.564 5.064 4.5e4 4.0e4 3.564 3.064 2.5e4 2.0* 4 1.Se 4 iu,499.CV130. 0 amu "

'.O KH 

# i

15. 0 15. 5 16, 0 16. 5 17. 0 17, 5 

# I Sampl e Name : "b111012al45 " Sampl e ID:'GLP10-01-02-22-O6 rFile : "b11l012a.wif r Pea k Name ; "PFOS " Mass(es) : "499.0/99. 0 amu,499.0/80. 0 amu,499.0/130. 0 Comment:-DALGW331S0 " Annotation : " Sampl e Index : 14 5 Saopl e Type ; Unknow n Concentration : H/ A Calculate d Cone : 267 . ng/n L
Modified ; R T Window : Expecte d RT :

3.36e+O0 5 I Sampl e Name : "b111012a157 ' Sampl e ID;'GLP10-01-02-22-069 " File : "blUOIZa.wi T
Sampl e Type ; Calculate d Cone : 75S . r 10/14/201 1 4:23:1 5 P

M

Betenti i Height : Manual

le : 15. 2 322668 6 c i iu,499.0/80. 0 amu,499.0/130. 0 amu "

4.4e5 - 4.2e5 - 4.065 - 3.Be5 - 3.6e5 - 3.4B5 - 3JB5 - 3.0e5 - 2.Be5 - 2.6e5 - 2.4eS 2.2e5 - 2,0e5 -

1J!95 - 1.0e5 - e.0e4 - 6.0e4 -

14 5 15. 0 15. 5 16. 0 16, 5 17. 0 17. 5 5. 0 15. 5 16. 0 16. 5 ^^J 3 17, 5 Dat a printe d b yST W Printin g Time : 11:08:4 7 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 5 o f 5
Pag e 5 8 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

• SampleNBine;'b111012a017 * Sampl e ID : "10007-27-6 " I Pea k Name:'PFBS ' Mass(«s}:'299.0/99. 0 amu,299.a/80
. I Commenti'l.Ong'mLFCGtdlnMliQWatei ' Annotation : Sanpl e Type ; Standar d Concentration ; 1.0 0 ng/m L Calculate dCone ; 0.99 9 ng/n L Acq . Date ; 10/12/201 1 Acq . Time : 3:07:4 9 P M i l f led ; Smoothin g Hidth ; R T Window : Expecte dRT : N o

• : 12. 5 89620 5 CO L 1.ese+oo s 

# I SampleName:"b111012B02B " Sample©:"SolventBlank " File:*b111012a.wH r Pea k Name : "PFBS " Mas5(es):"299.CV99.0amo,299.0/BO , Commen t "M B Q Wate rTN11-0334 " Amolatioo: " Sampl e Index : 2 8 Sanpl e Type : Unknow n Concentration ; H/ A Calculate d Cone : < 0 Acq . Date : 10/12/201 1 Acq . Time ; 6;59;3 7 P M Modif J °d ; itelliQu . 0.0 0 0.0 0



# I 5ampl6Name;"b111012a030 " SamplelD:"LCS-111007- ' Pea k Name : "PFBS " Massfes) ; "299.0/99. 0 amu,299.Q/B0
. Commeni ; '2pp b LCS ' Anrwtatlon ; * * Sanpl e Index : 3 0
Acq . Tim e ; 7 : 4 1 : -l e P H Modified ; N o Pcoc . Algorithm ; IntelliCua n- IQA Min . Pea

k Height : 0.0 0 cp s Min . Pea

k width ; 0.0 0 se c Smoothin g Hidth : 0 point s R T WindoH : 30. 0 se c Expecte dRT ; Us e Bel i Height : Star t Ti l En dTim e i RT : • Sampl e Name : "bl11012a033 ' Sample ID:'LCS-IIIOO/M " IPea k Name ; "PFB S Massfes) : "299.0/99. 0 a inu,299.0m0. 0 • Comment ; '20pp b LCS " A/inotation : * " Sampl e Index : 3 3 Sampl e Type ; Q C Concentration : 20. 0 ng/m L Calculate dCone : IB. 4 ng/m L 2.6eB
10/12/201 1 Acq . Time : 8:45:0 5 P M 2.5e6
- 2.4D6
- Modified : Y e s 2.4D6
- Proc , Algorithm ; mtelllQua n- MOI I 2.3e6
- Nois e Percentag e S O Base . Sub . Wlnd o I.O O min ' 2.2e6
- Pea)i-Split . Fac t r ; 2 2.1e6
- a k : tl o Min . Peal t

Heigh t 2.0e6
- Min . Pea k

Hidth : 0.0 0 se c 1.9e6
- Smoothin g Hidth ; 1.9e6
- R T Window : 30. 0 se c l.ee6
- 12. 6 mi n Us e Relativ e RT ; 1 1 o 1.7e6
- 1.6e6
- Int . Type ; Valle y 1.6e6
- 12. e mi n 1.5e 6 Area : 1 3 9766 9 count s Height : .egefOo e cp s 1.4«6
- Star t Time : 12. t mi n 1.3e6
- E n dTime : 13. 2 ni n 1 1.2ee
1.1e6
- 1.0e6
- 9.065
- 8.0e5 ' 7.0e5
- 6.0e5
- 5.0o5
- 4.0o5
- 3.0e5
- 2.0e5
- 1.0e5
- 0.0
- File : "bil l 012a, w

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 1 3
Pag e 5 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b 

# I Sampl e Name ; •b111012a036 " Sampl e ID ; "LCS-II1007-7 ' Pea k Name : "PFBS ' Massfes) : '299.0/99. 0 amu,299,0/80, 0 Comment ; "SOppb LCS ' Annotation : " Sampl e Index ; 3 6 Sampl e Type : Q C Commen t 'DA L G W203 L 0 " Annotation; ' Sampl e Index : 5 7 Sampl e Type ; Unknow n

Modified : R T Windov ; Expecte d RT : Us o Relativ e

1.70e-(00 5 cp s 

# I SampteNamo:-b111012a069 " Sampl e ID : "GLP1(M)1-02-22-009 " File : "b111012a.wi r Pea k Name : "PFBS " Mass{es) : -299.0^9. 0 amu.299.oraO. O Commen t "DA L G W220 L 0 " Annotation : "

Height : Star t Tine :

11. 5 12. 0 12, 5 13. 0 13. 5 14, 0 Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 2 o f 1 3
Pag e 6 0 o f9 9GLP10-01-02 ; Interi m Repor i 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

•* * Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST

W Printin g Time : 11:02:0 9 A M "Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e Pag e 6 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 

### Pag e 6 2 o f 99GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS
. an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b 

# I Sampl e Name : "t)lll012a12 rSampl e ID:" i Pea k Name ; 'PFBS ' Mass(es) : '299.0/99. 0 a i Comment : "DA L G W32B R 0 " Annolation : ~ Sampl e Type ; Concentratio n Calculate d Co i Acq . Date ; 27. 7 ng/rs L 10/14/201 1 3:12:5 1 A

M Modified : R T Window : Expecte d BT ; 24e 5 2Je 5 2.2B 5 2,1e 5 2.0e 5 1.9e 5 1.Se 5 1.7e 5 l£e 5 1.5e 5 1,4o5 1.3e 5 U e 5 l.le S 1.0e 5 9,0e 4 6.0* 4 • 7.0«» 4 e.0e 4 5.0e 4 4.0e 4 3.0» 4
1.0e 4 

## ( Sampl e Nanw : "blllOUalZg " Sampl e ID ; "GLP10-01-02-22-049 ' File : "blllOIZa.wi r Pea k Name : "PFBS " Massfes) : "299.0/99, 0 Commen t "DA L G W328 L 0 " Anrwtation : " Sampl e Index : 12 9

Expecte dRT ; Us e Relativ e RT ; K o

Star t T i EndTim e Hanua l ie : 12. 5 ni n 3t6B4t O count s e.69e'O0 S cp s 12. 2 oi n 12. S ni n



# I Sampl e Name : "b l 11012a133 " Sampl e ID : ' < Pea k Name : "PFBS " Mass(es) : "299.0/99. 0 a i Comment : "DA L GW330R0 " AnnotaSon: - Sampl e Index ; 13 3 Saopl e Type : Unknow n

Modified ; R T Window : Expecte d RT : 

# I Sampl e Name : "b111012a14 rSampl e ID : "GL P 10^1-02-22-057 " File : •b111012a,w« r Pea k Naff« ; "PFBS " Mass(es) : "299.0/99. 0 amu,299.a'80. 0 Commen t "DA L GW330 L 0 " Annotation:" "

Height ; Star t Ti l En dTim e 2.75e'00 6 cp s 2.7e 6 2.6e 6 2.5e 6 2.4e 6 2.3e 6 22e e 2,1e 6 2,0e 6 1.9e 6

1.6e 6 1.5e 6 1.4o6

9.0e 5 e.0e 5 7.0e 5 e.0e 5 5,0* 5 4.0e 5 3,0e 5 2,0e 5
12. 0 12, 5 13. 0 Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : WednesdayDecembe r 07 , Pag e 5 o f 1 3
Pag e 6 3 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1
Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b

yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 6 o f 1 3
Pag e 6 4 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3r d Quarte rSamplin g - 201 1
Buste r J293020 3 Batc hName : blll012a.da b 

# T Sampl e Name : 'b111012a043 " Sampl e ID ; "GL P 1CW)1-02-22-082 " Fie : •b111012a.wi r Pea k Name : 'PFBS ' Mass(es} : "299.0/99. 0 amu,299.0/80, 0 amu " Commeni : •DA L GW203 L F?B " Annotattoo: - Sanpl o Index : A 3 Saopl e Type : Unknow n Concentration ; M/ A Calculate dCcnc : 0.0016 5 ng/n LG Acq . Date ; 10/13/201 1 Acq . Tine : 12:16:0 0 A M lllied ; H o tthn : IntelliCua n- 1 sight ; 0.0 0 cp s tdth ; 0.0 0 se c

6.07e<00 3

-.10.1 5 -.10.5 3 11.1 8 10. 5 11. 0 

# I Sampte Name ; 'b111012aOi rSampl e ID : "10007-27-8 " File : •b111012a.wtf r Pea k Name : 'PFHS ' Mass(es) : "399.0/99. 0 amu.399.0/80. 0 amu " Commen t "1. 0 ng'm L F

C sb l i n Ml i Q Watei * Annotation;" " Sarapl e Index ; 1 7 Sarapl e Type ; Standar d Concentration ; 1.0 0 ng/m L Calculate dCone : 1.0 4 ng/n L Acq . Date : 10/12/201 1 Acq . TlQe : 3:07:1 9 P M Modified : H o Proc . Algorithm : IntelliQua r Kin , Pea

k Height ; 0.0 0 : Hin . Pea

k Width ; 0.0 0 £ Smoothing Width: 0p< R T Window : 30. 0 ; Expecte dRT : 14. 2 n Us e Relativ e BT ; N o Typo ; Heigtit : Star t TiEie : En dTirae : Valle y 14. 3 mi n 1735 5 count s l.69e+0D 5 cp s 1.6« 5 1,Se 5 1.4e 5 1.3« 5 1.2o 5 1,1e 5 1.0e 5 9.0e4 8.0e 4 7.0e4 6.0e4 5.0e 4 4.0e4 3.0e4 2.0e4 1.0e 4
12. 0 12. 5 14. 5 15. 0 15. 5 16. 0 16. 5 

# I Sampl e Name : "bll1012a028 " Sampl e ID : 'Solen t Slank " Fie : •b111012a.wi r Pea k Nanw : "PFHS " Mass(es) : "399.0/99. 0 amu,399.0/80. 0 amu " Comment : "Ml i 0 Wate rTN11-0334 ' Annotation : ~ Sampl e Index : 2 3 Sampl e Typ i Conc t lalcu l le dCO I

Proc . Alg i N/f t

H o ithn ; InteliiQua i Min . Pea

k Height : 0.0 0 ( Kin . Pea

k Hidth : 0.0 0 : SDOothin g Width : 0 p < R T Window : 30. 0 :

1 RT : Us e Relati v Int . Type ; Retentio n 1 Height : ! RT : N o

79et00 2 cp s 

# I SampteName:"bll1012a030 ' Sampl e ID : "LCS-IIIOO?-! " File : •bll1012a,wif r Pea k Name : "PFHS " Mass(es) : "399.0/99. 0 amu,399.0/80. 0 Comment : "2pp b LCS " Annotation : " Sampl e Index : 3 0 Sampl e Type ; Q C Calculate dCone : 2.1 0 Acq . Date : 10/12/20 1 Acq . Time : 7:11:1 6 1 HodiCled ; tl o Proc . Algorithm ; IntelliC i Kin . Pea

k Height : 0.0 0 Min . Pea

k Width : 0.0 0 ng/m l

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , December
- 07 , Pag e 7 o f 1 3
Pag e 6 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

** * Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 8 o f 1 3
Pag e 6 6 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

12, 0 

# I SampteName:-b111012a073 " Sampl e ID : "GLP1041-02 - Pea k Name : "PFHS " Mau(es) : "399.0/99. 0 amu,399,0/80
. Commen t "DA L G W222 R 0 " Annolation: " Sampl e Index ; 73 Sampl e Type : Unknow n Calculate d Cone ; 127 . ng/ra L

Proc . Algorithro : Hin . Pea kHeight : Hin . Pea kwidth ; Smoothin g Midth : Expecte d RT : Us e Relativ e Int . Type : 11. 2 tl o Valle y ! ; 11. 3 ssieie i c

c 1.00e<006 13. 9 11, 9



# I Sampl e Name : "b111012a081 " Sampi o ID : •GLP1CW)1-02-22-0i rFlle:"t)111012a
. Pea k Nam* : "PFHS " Mass(Bs) : "399.0/99. 0 a n Comment ; "DA L G W227 R 0 " Annotatkxi: " Sampl e Index : B l Sanpl e Type ; Unknow n Concentration : H/ A Calculate d Cone ; €0. 3 ng/n L Acq . Date : 10/13/201 1 Acq . Tine : 1:37:1 9 P M idl f i c
Expecte d R

l Us e Relati v Int . Type ; H o 

# I SampleName:"b111012B085" SamplelD: Peak Name: "PFHS" MaM(es}:

-399.0/99.0 Comment

"DALGW

227L0" Anrvrtatton:

" Sample Index: 85 Saraple Type; Unknown Concent tat ion: 11/A Calculate d Cone : 68. 7 ng/m L Acq . Date ; 10/13/201 1 Acq . Tine : 3:02:1 2 P M Modified : tl o Proc . Algorithm ; IntelliCua n - IQA Hin , Pea klieight : 0.0 0 cp s Hin . Pea kWidth : 0.0 0 se c Smoothin g width ; 0 point s

, lee'OO S cp s

13.5 14.0 14.5 15.0 Dat a printec i b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 9 o f 1 3
Pag e 6 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1
Buste r J293020 3 Batc hName : blll012a.da b

14. 0 14.5 15. 0 

# I Sampl e Name : l)111012a097 " Sampl e ID : 'GLP10-01-02 - Paa k Name : •PFHS ' Mass(es) : "399.0/99. 0 Commen t "DA L GW312R0 - Annotatton: - Sampl e Index ; 97 Sampl e Type ; Unknow n Concentration : ll/ A Calculate d Cone ; 629 . ng/n L Acq , Date ; 10/13/201 1 Acq . line ; 7 Proc . Algorithm ; 1 Min . Pea kHeight ; Hin . Pea kWidth : Smoothin g width ; R T Hindow ; Expecte d RI ; Us e Relativ e RT :

13. 5 14. 0 14. 5 15. 0 15. 5
Comment : "DA L G W317 L 0 " Sampl e Typ e 

# I Sampl e Name ; •b11101Za109 " Sampl e ID : •GLP10-01-02-22-037 " File : "bl l 1012a.»fi r Pea k Name : "PFHS " Ma£s(es) ; "399.0/99. 0 amu.399.0/80. 0 amu " Commen t "DA L G W324 L 0 " Annotation : ~ Sampl e Index ; 10 9 Sarapl e Type : Unknow n Concentration ; (I/ A

Cone ; 82. 9 ng / Acq
. Ti n Hodlfie c Proc . Algor i 10 . L;29:08 I 2.1e5 - 2.0O5 - 1.9eS cHeight ; >ea kWidth :

9.0e 4 fl.0o4 7.0e 4 6.0e 4 5.0« 4 4.0e 4 3.0» 4 2.0» 4

13. 5 14, 0 14. 5 15. 0 15. 5 Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 1 0 o f 1 3
Pag e 6 8 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1
Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d byST

W Printin g Time : 11:02:0 9 A H Printin g Date : Wednesday , Decembe r 07 , 201 1 Pag e 1 1 o f 1 3
Pag e 6 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

• * Buste r J293020 3 Batc hName : blll012a.da b

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , Pag e 1 2 o f 1 3


### Pag e 70 o f 99GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1

Buste r J293020 3 Batc hName : blll012a.da b

I Sa r • Pa t • Co i Sampl e Name : •b111012aO45 " Sampl e ID : •GLP10-01-02-22-074 " Fie : "b111012a.w f Poa k Name : "PFHS " Ma»»(Bs) : "399.0/99. 0 amu,399.0/80. 0 amu " Comment : "DA L G WTRIP0 1 0 " Annotation : " " Sampl e Index : 4 5 Sanpl e Type ; Unknow n Concentration ; N/A Calculate d Cone : < 0 Acq . Date ; 10/13/2 ( Acq . Tirae ; 12:58;l f Modified : >a k Height ; ^a k Hidtti ; telliQ i

0.0 0 0.0 0

Heigtit ; Star t T i En dTim t 1900 ISO O

- IQ l 1700 cp s 1600 p^int a 15O 0 1400 '"t n 1300 ount E 1200 mi n mi n 1100

1000 

### 1 900
700
500 40 0 300 20 0 10 0 

# I Sampl e Name : 1)1110123043 " Sampl e ID ; "GLP10-01-02-22-082 ' File : "bl l 1012a . Pea k Name : "PFHS " Ma£s(es) : "399.0/99. 0 amu,399.0/SO. O Conwnent : "DA L G W203 L FW " Annotation : ~ Sampl e Index ; 4 3 Sanpl e Type ; Unknow n Concentration : It/ A Calculate dCone ; < 0 •13/2 (

Proc . Algorithn : ; Hin . Pea k Height : 12:1€:0 0 A M itelliQua n - IQA 0.0 0 cps ' O.O O 30. 0

2. 5 13. 0 13 5 14. 0 14,5 . 15. 0 15. 5 16. 0 16. 5

Dat a printe d b yST W Printin g Time : 11:02:0 9 A M Printin g Date : Wednesday , Decembe r 07 , 2 01 1 Pag e 1 3 o f 1 3
Pag e 7 1 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll020 a linear.rd b

1 6 1 8 20 Concentration , ng/m L Dat a printe d b yST

W Printin g Time : 11:21:3 0 A M Pag e 1 o f 1 Pag e 7 2 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i h Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll020 a branched.rd b k l 11020 a branctied.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weigtiting) : y= -1.54e+00 4 + 2.02e+00 6 x+ 20. 3 ( r= 0.9999) ,

4. 0 4. 5 5. 0 5. 5 Concentration , ng/m L Dat a printe d b yST W Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 1 Pag e 7 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 *ETS-Kir k Result s Name : klll020a.rd b k l 11020a.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weigtiting) : y= -7.53e+00 4 x'' 2 + 5.2e+00 6 x+ 4.48e+00 3 ( r= 1.0000 )

1 0 1 2 1 4 1

6 1 8 2 0 2 2 2 4 2 6 2 8

Concentration , ng/m L 3 0 32 3 4 3 6 3 8 4 0
Dat a printe d b yST W Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 1 Pag e 7 4 o f 9 9*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3r d Quarte rSamplin g - 201 1 Result s Name : klll020 a linear.rd b 

# I Sampl e Namo : "k l 11020a0ie " Sampl e ID : "10007-37-0 ' File : "K l 11020a , Pea k Name : "PFOS " Mass(es) : "499.000/99.00 0 D a ,499.000/80.00 0 Da,499.000/130.00 D Da Comment ; "2. 5 ng/m L F C st d t n Mi H Q water " Annotation : ~ Sampl e Inden ; 1 8 Sampl e Type ; Standai d Concentration ; 1.B 3 ng/m L Calculate dCone : 1.6 8 ng/m L Acq . Date ; 10/20/201 1 Acq . Tine : 7:55:5 3 P H Modified: Ha Pioc . Algo i 1 tho : Specif yPacaiieter s - M O 11 1 Mois e Petcencage ; S O Baae . Sub . Hindow : 1.0 0 ni n Peak-Split . Factor ; 2 Repor t Larges t Pealt : te a Kin . Pea k Heigtit : 0.0 0 cp s Min . Pea k Hidth : 0.0 0 se c Smoothin g Width ; 0 point s R T Window : 30. 0 se c Expecte dRT ; 16. 0 mi n : Rel i 1 RT : N o Heigh ' T yp e ; Va11 e y itio nTime ; 16. 0

342072 6 C l

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

# I Sampl e Name : "k l 11020a025 - Sampl e ID : TN11-0356 " Fie : "k l 11020a.w)r r Pea k Name : "PFOS " Mass(e3) : '499.000/99.00 0 Da,499.000/80.00 0 Da.499.000/130.00 0 Da " Comment : 'Metho d Blank ' Annotation: " Sarspl e Index ; 2 5 Sampl e Type ; Unknow n Calculate dCone ; 0.0010 5 Acq . Date ; 10/20/20 1 Acq . Time ; • 10:25:2 1 Modified : Ye s Proc . Algorithm : Specif y I Mois e Percentage ; 5 0 Baae . Sub' . Hindow ; l.O C Peak-Split . Factor : 2 •meter s - H Q I 750 -

: Height ; Hin . I Kin . 1 Smoothin g Hidth : BT Window ; Expecte dRT : Use Relativ e RT : Height : Star t T : En dTi m 6.60e+00 2



# I Sampl e Name : "k l 11D20a027* Sampl e ID : "LCS-111020-1 " File : "k l 11020a.wir r Pea k Name : "PFOS " Mass(e$) : "499.000/99.00 0 D a ,499.000/80.00 0 Da,499.00a n 30.00 0 Da ' Comment ; "0.2pp b LCS " Annotatton:" "

Modified : Ye s Proc . Algorithm ; Specif y Par . Mois e Percentage : 5 0 Base . Sub . Hindow : 1.0 0 Peak-Split . Factor ; 2 Repor t Larges t

Peak ; Ye s Hin . Pea

k Height ; O.D

O Hin . Pea

k Hidth ; 0.0 0 Smoothin g ( R T Window ; 30. 0 

## ( Sampl e Name : "kl l 1020a030 " Sampl e ID : "LCS-111020-4 " Fie : "klllOZOa.wif r Pea k Name : "PFOS " Mas£(e£) : "499.000/99.00 0 Da.499.000/80.00 0 03,499.000/130.00 0 Da Commen t "2pp b LCS " Anriolalion : ~ Sampl e Index ; 3 0 Sampl e Type : O C Concentration ; 1.8 5 ng/raL Calculate dCone ; 1.1 6 ng/m L Acq . Date : 10/21/201 1 Acq . Time : 12;12:1 0 A M Proc . Algorithm : Specif y Par i Base . Sub . window ; 1.0 0 Peak-Spilt . Factor ; 2 Repor t Larges t

Poak : Ye s Hin . Pea

k Height : 0.0 0 Min . Pea

k Hidth : 0.0 0 Smoothin g Width : 0 K THindow ; 30. 0 s f Expecte dRT ; 16. 0 m i ! Rela l • RT ; tl o Int . Type ; Valle y Retentio nTime : 16. 0 mi n Area ; 238249 5 count s Heigtit : 3.42et00 5 cp s 3.4e 5 3.2e 5 3.0e 5 2.8e 5 2.6e 5 2.4e 5 2.2e 5 2.0e 5 1.8e5
- 1.6a 5 1,4e 5 12e 5 1.0e 5 S.0» 4 6.0e 4 4.0e4 2.0e 4
15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Printin g Time : 11:23:2 5 A M Pag e 1 o f 2 Pag e 7 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 Result s Name : klll020 a linear.rd b

Dat a printe d byST

W Printin g Time : 11:23:2 5 A M Pag e 2 o f 2 Pag e 7 6 o f 9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 Result s Name : klll020 a branched.rd b 

# I SampleNaffle:*klll020a018 " Sampl e ID : "10007-37-9 " I Pea k Name : "PFOS * Mau(es) : "499.000/99.00 0 Da,499.0(] Convnen t "2. 5 ng/m L F

C st d i n M H O water* AnrK>Ulk)n: " Sampl e Index ; I B Sampl e Type : Standar d Concentration : 0.49 0 ng/n L Calculate d Cone ; 0.46 9 ng/ra L Acg
. Date ; 10/20/201 1 Modified : Peak-Split . Factor : Repor t Larges t Peak ; Min . Pea k Height : Hin . Pea k Hidth ; SiBOOthin g width : R T Hindow : ] Expecte d RT ; Us e Relativ e R

T :

Star t Tin < En d Time : 16. 0 ni n 4.4e 5 4.2e 5 4.0e 5 3.ee 5 3.ee 5 3.4e 5 3.2e 5 3.0e 5 2.ee 5 2.6e 5 2.4e 5 2.2e 5 2.0e 5

1.4e 5 1.2e 5 1.0e 5

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

# I SampteName:-k111020a025 " SamplelD:*TN1l-0356 " Fle:>111020a.wii r Poa k Name : TFOS " Ma»(es) : "499.000^9.00 0 Da,499.000«0.00 0 D a ,499.000/130.00 0 Da Commen t "Metho d Blank " Annotation: " Sampl e Index : 2 5

ICone ; 0.00013 7 ng/m L

10/20/201 1 I0;25;2 1 P

K

l b . Windoi. L-Spli t Repor t Larges t Peak : Hin . Pea k Height : Min . Pea k Hidth : Smoothin g Hidth ; R T Window : I S Expecte d RT : : Rel i ; RT ;

13. 5 14. 0 14. 5 15. 0 

# I Sampl e Name : "k111020a027 " San«)l e ID:'LCS-111020-1 " Pea k Name : "PFOS " Mass<es) : "499.000/99.00 0 Da,49g.00 0 Commeni : *0.2pp b LCS " Annotation : ~ Sampl e Index ; 2 7 Sampl e Type :

:e d Cone; ' 0.032 0

Base . Sub . -window ; Peak-Split . Factor ; Repor t Larges t

Peak ; ig/ra L

ig/m L

Smoothin g Hidt t R T Hindow : Expecte dRT : Us e Relativ e R I 3.4» 4 3.2e 4 3.0e4
- 2.3e 4 2.6e 4 2.4e 4 2.2e4 2.0O4
-

1.0e 4 8000.0
- 6000. 0 40O0.0
- 2000.0
- 0.0
- 

# I Sampl e Name : 1(111020a030 " Sampl e ID : "LCS-111020-4 " File : "kl11020a.»i r Pea k Name : TFOS " Massfes) : "499.000/99.00 0 Da,499.000/e0.00 0 Da.499.000/130.00 0 Da " Commen t •2pp b LCS " Annotathyi : - Sampl e Index : Sample'Type ; Calculate d Cone ;

Dat a printe d b yST W Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 2 Pag e 7 7 o f 9 9*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll020 a branched.rd b 

# I SamplaName:-k111020a033 ' Sampi o ID : "LCS-111020- rFite:•k11l020a.svf r Pea k Name : "PFOS " Massfes) : "499.000/99.00 0 Da.499.000ffl0.00 0 Da,499.000/130.00 0 Da * Common! : •20pp b LCS " Annolation: " Sampl e Index ; 3 3 Sampl e Type ; O C Concentration : 18. 5 ng/ra L Calculate d Cone ; 3.5 2 ng/mL Acq . Date : 10/21/201 1 Xcq . Time : 1:16; H A H Modified : Proc . Algo . tlois e Percentage ; Base . Sub . Hindox : Peak-Split . Factor : Repor t Larges t Pea k Min . pea k Height ; Min . Pea k Hidth ; Smoothin g Width : R T Window ; Expecte d RT ; Us e Relativ e RT : Specif yParameter s

Valle y i e : 15. » 693193 B c t Height ; Star t Time : En d Time :

Dat a printe d b yST W Wednesday , Decembe r 07 , Sub . Mindo k
Min . Peak

Width ; Smoothin g Width : R T Window : Expecte dRT : Sampl e Name : "k111020a050 " Sampl e ID ; "GLP l 0-01-02-22-065 * File : •kl11020a
. Pea k Name : "PFOS " Mass(Bs) : "499.000/99.00 0 Da,499.000/80.00 0 Da,499.000/130.00 0 Da ' Commen t "DA L G W335 R 0 " Annotation : ~ Sampl e Index ; 5 0 Sampl e Type : Unknow n

on ; Il/ A Cone ; 2080 . ng/n L

-ttun ; Specif yPoramote i :age ; 5 0

9.73e+00 5 cp s

Pag e 2 o f 2 Pag e 7 8 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3r d Quarte rSamplin g - 201 1 Result s Name : klll020a.rd b
I Sampl e Name : •k111O20aO18* Sampl e ID : "10007-37-9 " File : "kill020a
. Pea k Name : "PFHS " Massfes) : '399.000/99.00 0 Da.399.00D/80.00 0 Da ' I Commeni : *2. 5 ng/m L F C atd I n M D Q water* Annotation : - ampl e Index : I S ampl e Type ; Standar d oncentcation : 2.5 0 ng/n L alculate d Cone : 2.5 1 ng/m L e q . Date : 10/20/201 1 7:55:5 3 P M Acq . Ti n Modified : Proc . Algorithm : £ Ilois e Percentage ; Peak-Split . Facto i Repor tLarges tPe

e Min . Pea kHeight : Min . Pea kHidth ; Smoothin g Hidth : R T Window : Expecte d RT : Us e Relativ e RT : H o 

# I Sampl e Name : "k l 11020a025 " Sampl e ID ; TN11-0356 " F»« : "k l 11020a, w Pea k Narrw : "PFHS " Mass(ea) : "399.000/99.00 0 Da.399.000/80.00 0 Da ' Commen t "MettKx

J Blank " Annotatkin : ~ Sampl e Index : 2 5 Sarapl e Type ;

Min . Pea k Height : Min , Pea k Hidth ; Smoothin g Hidth ;

Bas e T o Bas e Height ; Star t Ti t En d Time :

17. 0 17. 5 

# I Sampt e Name : T(111020a027 ' Sampl e ID : "LCS-111020-1 ' File : "kll H Pea k Name : "PFHS " Mass(es) : "399.000/99.00 0 Da,399.000/30.00 0 Da " Commen L "0.2pp b LCS ' Annotation : ~ Sampl e Index : 2 7 Sampl e Type : Q C Concentration ; 0.20 0 ng/rs L Calculate d Cone : 0.17 4 ng/m L
lifl i ttoii Algo r Specif y Parame t Sub . HindOH : Peak-Split . Factor : Repor tLarges tPeak ; Min . Pea kwidth ;

1 RT ; 

# I Samid e Name : "k111020a030 " Sampl e ID : "LCS-111020-4 " File : 'kllio : Pea k Name ; "PFHS "
. Mass(as) : -399.000^9.00 0 Da.399.000re0.00 0 Da " Commen t "2pp b LCS " Annotation: " Sanpl e Index : 3 0 Sampl e Type : Q C Concentration : 2.0 0 ng/n L Calculate d Cone : 1.7 6 ng/m L Acq . Date : 10/21/201 1 Acq . Time : 12:12:1 0 A M Proc . Algor J Base . Sub . window : Peak-Split . Factor ; Repor t Larges t Peak : Min . Pea k Hidth : Smoothin g Hidth : R T Hindow : 3 0 Expecte d RT : 1 1

190605 5 C 1.26e+00 6 15. 0 1.25e6 - 1.20e6 - 1.15e6 - I.IOee 1.05*6 - i.oooe9.50e5 - 9.00o5 - 8.5005 - 8.00«5 - 7.50e5 - 7.00e5 -

, 6.50e5 - S.00e5 - 5.50e5 - 5.00e5 - 4.50e 5 4.00e 5 3.50e5 ' 3.00e 5 2.50eS 2.00e 5 1.50e5 1.00e5 5.00e 4 0.0 0 13. 0 13. 5 14. 0 17. 0 17. S Dat a printe d b yST W Printin g Time : 11:19:2 0 A M .Pag e 1 o f 2 Pag e 7 9 o f9 9*ETS-Kir k GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 Result s Name : kH1020a.rd b

Dat a printe d b yST

W Printin g Time : 11:19:2 0 A M Pag e 2 o f 2 Pag e 8 0 o f 9 9GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3r d Quarte rSamplin g - 201 1 Result s Name : klll024a.rd b

Dat a printe d b yST W Wednesday , Decembe r 07 > 201 1 Pag e 1 o f 1 Pag e 8 1 o f9 9*ETS-Kir k GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll024a.rd b 

# ( Sampl e Name : "kl l 1024a017 ' Sampl e ID : "1 1 003-40- rFie : "k l 11024a.w« r Pea k Name : "13C6PFOS-IS(IS rMaM(es) : "507.000/80.00 0 Da " Commen t "1. 0 n^ftn L F C st d I n Synth
. Watof " Annotation ; - Sanpl e Index : 1 7 Sampl e Type : Standar d Concentration ; 0.96 0 ng/o L Calculate d Cone ; H/A Acq . Date : 10/21/201 1 Acq . Time : 7:42;4 1 P M Modified ; Ve s Proc . Algorithm : Specif yParameter s - H Q II I tlois e Percentage : 5 0 Base . Sub . Hindow ; 1.0 0 mi n Peak-Split . Factor ; 2 Repor t Larges t Peak : ^e a Min . Pea k Height ; O.O O cp s Min . Pea k Hidth : O.O O se c (idth ; R T Window :

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

# I SamiJ e Name : "kl l 1024aO25 " Sampl e ID: * Pea k Name : "13CePFOS^S(IS rMass(BS) : * ! Commen t "Metho d Blank " Annotation; " Sampl e Index ; 2 5

. Algorithm ; Specif y Pa n

Pea k Height ;

iight : ;ac t Time : i dTime ;



# I Sampl e Name : 1(1110243027 " Sampi o ID : "LCS-111024-1 " File : "kl11024a.iM r Pea k Name : "13CBPFOS4S(iS) " M8»s(e») : "507,000/80.00 0 Da " Commen t "0.2pp b LCS " Annotation:" " Sanpl e Index : 2 7 Sampl e Type ; Q C Concentration ; 0.95 3 ng/n L Calculate d Cone : M/ A Acq . Date ; 10/24/201 1 Acq . Tine : 11:16:2 3 P M

. Sub . Kindox : -Split . Facto i :: t Larges t Pe i Sisoothin g Wid I R T Window ; Expecte d RT ;

Height ; Star t Ti r En d Time : Valle ;

(1945 6 

# I Sampl e Name : •k111024a030 " Sampte ID : " I PeakName:"13C8PFOS-IS(IS) " Masa{es);" l Comment•2ppbLCS " Annotation:" " Sanpl e Index : 3 0 Sampl e Type ; O C Concentration ; 0.95 3 n . •25/20 1 12;20;3 0 Specif y Paramet i

Expecte dRT :

15. 0 15. 5 16. 0 16. 5 15. 0 15 ^ 16. 0 16. 5 17. 0 17. 5 18. 0 18. 5 Dat a printe d b yST W Wednesday , Decembe r 07 , 201 1 Pag e 1 o f 4 Pag e 82 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll024a.rd b 

# I SamploName:"k111024a033 * Sampl e ID : "LCS-111024- rFite:"k111024a.wtf P Pea k Name : "13C8PFO&^S(IS) • Ma»s{es) : "507.000«0.00 0 Da " Commen t "10pp b LCS " AnnolaOon : * * Sampl e Index ; 33

Modified ;

R T Window ; Expecte d R

T Us e Relativ i Int . Type : Height ; Endrime ;

15. 5 16. 0 16. 5 

# I Sampte Name : "k111024a040 " Sampl e ID ; "GLP l 0^1-02-22-033 " File : Pea k Name : "ISCSPFOS-ISllS rMa3»(e9) : "507.000/80.00 0 Da Commen t "DA L GW317L0 " Annotation: - Sampl e Index ; 4 0 Sanpl e Type ; Unknow n Concentration ; 0.95 5 ng/m L Calculate dCone : H/A Acq . Date ; 10/25/201 1 Acq . Tirae : 3;51:1 2 A M liti i

Area : Height ; in ; Specif y Paran

,ge : 5 0 idow ; 1.0 0 r

77393 1 c

c l.lSetOO S 16. 0

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

# I SamploName:"k111024aO44 * Sampl e ID : "GLPl0-01-02-22-049 ' Fite:"k111024a.w( r Pea k Name : "13C6PFOS4S(ISJ " Mas4(es) : "507.000/30.00 0 Da " Commeni : "DA L GW328L0 * Annotation:" " Sampl e Index ; 1 1 Sampl e Type : Unknow n Concentration ; 0.95 5 ng/m L^ Calculate dCone : N/ A

ic
. Algor i .s e Perce r le
. Sub
. V ik-SpliC , Hin . Poa

k Hidth ; Smoothin g Hidth ; R T Hindow : : Specif y Parame t

Height : Star t Ti l EndTim e 

# I Sampl e Name ; "k l 11024a0i rSampt e ID : "1 1 003-40^ " Pea k Name ; TFOS - Mass(es) ; "499.000^9.00 0 Da.499.0 1 Cofranen t "1. 0 ng/m L F

C std I n Synth
. Wate rAnnolation; " Sampl e Index ; 1 7

Proc . Algor i Base . Sub . ( :-Spli < Fac t Repor t Larges t

Peak ; Min . Peak

Hidth : Smoothin g Width : R T Window ; 3 ( Expec ; Rela l IRT : ; RT ; Retentio nTi i Area : Height : 1.00e5 - 9.50e4 ' 9.0ae4 ' 8.50e4 ' 8.00e4 ' 7.50e4 - 7.00©4 - 6.50e4 ' S.00e 4 g 5.50e4 - j 5.00e4 -

- 4.50 M 4.00e4 ' 3.50e 4 3.00*4 - 2.S0» 4 2.00e 4 1.50e4 1.00e4 - 5000.0 0 0.0 0 15. 0 15. 5 16. 0 16, 5 17. 0 17. 5 Dat aprinte db y ST W Wednesday , Decembe r 07 , Pag e 2 o f 4 Pag e 8 3 o f9 9*ETS-Kir k GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 Result s Name : klll024a.rd b

Dat aprinte db y ST W Wednesday , Decembe r 07 , 201 1 Pag e 3 o f Pag e 8 4 o f9 9GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 Result s Name : klll024a.rd b 

# ( Sampl e Name ; >111024aO40 " Sampl e ID ; "GLP l 0-01-02-22-033 " File : Pea k Name : "PFOS " Mass(es) : "499.000/99.00 0 Da,499.000/80.00 0 Da. - Comment:"DALGW317L0 ' AnnotatJon; - Sampl e Index ; 4 0 Sampl e Type ; Unknow n Concentration : N/ A Calculate d Cone : 0.21 1 ng/n L Acq . Date ; 10/25/201 1 ) . Acq . Tine : 3:54;1 2 A M Hodifi f 1.7e 4

; Specif y Paranete i Base . Sub . Window ; l.D O Peak-Split. Factor: t Repor t Larges t Peak : Ye s Hin . Pea k Height ; 0.0 0

Us e Relativ i Retentio n T : Height : § " 1.0e4 - I 9000.0 - 8000.0 - 7000.0 - 6000.0 - 5000. 0 4000.0 - 3000.0 - 2000.0 - 10D0. 0 0.0 - 17. 0 17. 5 18. 0 18. 5 

# I Sampt e Name : "k111024aO44 " Sampt e ID : "GLP l Wll-02-22-049 " File;"k111024a.w« r Pea k Name : "PFOS " M3*s(es) ; "499.OO(V99.O0 O O a ,499.000/80.00 0 Da,499.000/130.00 0 Da - Commen t "DA L G W328 L 0 " Annolation : " Sanpl e Index : 4 4 Sanpl e Type ; Unknow n

Peak-Split . Facto i Repor tLarges tPe l Hin . Pea kHeight : Min . Pea kWidth : Smoothin g width ; R T Window : Expecte d RT ; 0,0 0 cp s 7.0e 4

! Rela l
Height : Star tTi n En d Time ; ; RT ;

Dat a printe d b yST W Wednesday , Decembe r 07 , 201 1 Pag e 4 o f 4 Pag e 8 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 

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

Pag e 8 6 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 

# 3IV I Eiwironmenta l Laborator y

Method Method of Analysis

for the Determination

of Perfluorinated

Compounds

in Water by LC/MS/MS;

Direct Injection

Analysis Method Number:

ETS-8-044.0 Adoption

Date: Upon Signing Effectiv e Date : Q 1^y'o' 7 Approve d By :

Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 8 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



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

yrequir e preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Determinatio n of Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
. Thi s metho d i s considere d a performance-base d method
. Data i s considere d acceptabl e a s lon g a s th e define d Q C elements are satisfied
. Sampl e collectio n i s no

t covere d underthi s analytica l procedure . 2 Metho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS
. Sample s containin g heav y particulat e ma

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

t multipl e concentrations
. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g field 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 flagged a s suc h (wit h expande d accurac

ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Fortificatio n level s fo rfield matri xspike s an d fo rlaborator ymatri xspike s shoul d b e at least 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o determin e th e statemen t o f accurac yfo ranalytica l results
. 3 Definition s 3. 1 Calibratio n Standar d Asolutio n prepare d b

yspikin g a know n volum e ofth e Workin g Standar d (WS ) into a predeteirnine 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 y Duplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

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

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

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d a s a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures
. Th e purpos e ofth e F B i s t o determin e i ftes t substance s o r othe rinteri'erence s ar

e presen t i n th e field environment
. Thi s sampl e i s als o refen-ed t o a s a Tri p Blank
.

ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 8 8 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### 3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n 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 befor e th e bottle s are sen t t o th e field fo rcollectio n o faqueou 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 ofth e sampl e analysis
. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s ofanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are no t know n o rma

yvary . At least on e separate , un-spike d sampl e mus t b e take n a

t th e sam e tim e an d place as eac h FMS
. 3. 7 Laborator y Contro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s ofth e targe t analyte s ar e adde d i n th e laborator

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

ysampl e t o determin e whethe rth e metho d i s i n control
. LCS s shoul d b e prepare d eac h da ysample s are extracted
. 3. 8 Laborator y Matri xSpik e (LMS ) Alaborator

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

ysampl e t o determin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results
. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e determine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations
. LMS s are optiona l fo ranalysi s ofaqueou s samples
. 

## 3. 9 Laboratory Sampl e Aportio n o raliquot ofa sampl e receive d fro m th e field fo rtesting
. 

## 3.1 0 Limi t o

fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e 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 roufin e operatin g conditions
. T o simplif ydat a reporting , th e LLO Q i s generall yselecte d a s th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria
. Sampl e LLOQs 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 ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 8 9 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 

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

ysampl e includin g 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 ftest substance s o rothe rinterference s are presen t i n th e laborator y environment , th e reagents , o rth e apparatus . 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yofmateria l intende d t o represen t th e origina l source material
. 3.1 3 Stoc k

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

## 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s not normall y foun d i n th e sample(s)
. Asun^ogat e compoun d i s typicall ya targe t analyt e wit h a t least on e ato m containin g a n isotopically-labele d substitution
. I fused , sun-ogate(s) are adde d t o al l sample s an d qualit y contro l samples
. Surrogate(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 ofa surrogat e analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired
. 3.1 5 Workin g Standar d (WS ) Asolutio n ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o prepare calibratio n standard s an d othe rrequire d analyt e solutions
. 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yofth e standard s fo rthi s metho d have no t bee n precisel ydetemnined ; however , eac h shoul d b e treate d a s a potentia l healt h hazard
. Th e analyst shoul d wea rgloves , a la b coat , an d safet

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

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a curren t awarenes s ofloca 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 sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t 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 informatio n an d cautions
. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware
. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s ofanalysi s b

yrunnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 0 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


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

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

fdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e o fpumpin g u p t o tw o solvents an d equippe d wit h a variabl e volum e injecto rcapabl e ofinjectin g 5-10 0 p L connecte d t o a tande m Mass Spectromete r (LC/MS/MS)
. I Analytica l balance capabl e ofreadin g t o 0.000 1 g Adevice t o collec

t ra wdat a fo rpea k

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

### 50pL , lOOpL , 250pL , 500ML , 

### lOOOpL
. 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e ofspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi c Syste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C18,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program : FlowRat e

Tim e (min ) % A % B (mL/min ) 0. 0 9 7 3 1. 0 0. 5 9 7 3 1. 0 11. 0 5 9 5 1. 0 13. 5 5 9 5 1. 0 13. 6 9 7 3 1. 0 17. 0 9 7 3 1. 0 Injectio n Volume : 10 0 pL
. 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 ofAnalysi 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 9 1 o f9 9GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1 

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

16 9 an d 36 3 - » 11 9 PFOA 41 3 ^

369 , 41 3 - » 21 9 an d 41 3 16 9 PFN A 46 3 419 , 46 3 ^ 16 9 an d 46 3 ^21 9 PFD A 51 3 ^

469 , 51 3 - > 21 9 an d 51 3 ^ 26 9 PFUn A 56 3 ^ 519 , 56 3 26 9 an d 56 3 - » 21 9 PFDoA 61 3 ^ 569 , 61 3 ^

16 9 an d 61 3 31 9 PFB S 29 9 8 0 an d 29 9 ^ 9 9 PFH S 39 9 8 0 an d 39 9 9 9 PFO S 49 9 ^ 80 , 49 9 9 9 an d 49 9 ^ 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s 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 a s a guide , altemat

e instnjment

s an d equipmen

t ma y b e used . 7 Reagent s an d Standard s 7. 1 Chemical s Wate r- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A.C.S
. Reagen t Grad e 7. 2 Standard s Perfiuorobutanoi cAci d (PFBA- C4 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 Perfluorohexanoi cAci d (PFH A- C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PF0A-C 8 acid) ; 3 M Perfluorononanoi cAci d (PFN A- C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA-CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA- C l 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C 4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 9 2 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s ma yb e used
. 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—^Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L ofreagen t water . Note : Alternativ e volume s ma yb e prepare d a s lon g as th e ratio s ofth e solven t t o solut e ratio s are maintained
. 

## 7. 4 Stoc k

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

d preparatio n procedur

e serve s a s a n example
. Weighe d amounts an d final volume s ma yb e change d t o sui t th e need s ofa particula rstudy
. Fo rexample , p L volume s ma yb e spike d into volumetri cflasks whe n dilutin g stoc k

solution s t o appropriat e levels
. 100 pg/m L targe t analyt e SSSs—^Weig h ou t 1 0 m g o fanalytica l standar

d (correcte d fo rpercen t sal t an d purity ) an d dilut e t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container
. Prepar e a separat e solutio n fo reac h analyte
. Expiratio n date s an d storag e condition s ofstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. A n exampl e ofpurit yan d sal t con-ectio n i s give n belowfo rPFOS
. X - rX molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t o fsal t 49 9 PFO S (K" " )sal t correctio n facto r= —= 0.927 5 53 8 1 0 m g CsFiySOa'K

* wit h purit

y90 % = 8.35m g CsF^SOs " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 pg/m L (500 0 ng/mL ) mixe d workin g standard—Ad d 0.5m L eac h ofth e lOOpg/m L SSS s t o a lOm L volumetri c flask an d brin g u p t o volum e wit h solvent
. 25 0 ng/m L mixe d worl<in g standard—Ad d 1.25m L o fth e 5 pg/m L -mixe d workin 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 L mixe d standard—Ad d 625p L o fth e 5 pg/mL-mixe d workin g standar d solutio n t o a 25m L volumetri c flask an d brin g u p t o volum e wit h solvent
. Storag e Conditions—Stor e al l SSS s an d workin g standard s i n accordance wit h laborator ystandar d operatin g procedur e o ri n a refrigerato ra

t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 3 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1



### 7. 5 Calibratio n Standard s Usin g th e workin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e a s a guideline
. Note : Volume s o fwate ran d worthin g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline
. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d a s needed
. Concentration of WS, ng/mL Volume of WS, pL Final

Volume of Calibration

Standard

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

Concentration

of Calibration

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

## 8 Sampl e Handlin g 8. 1 Wate 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 ofglas s autovials , t o preven t th e possibl yoffluorochemical 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 QC 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 fro m th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-detennine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are no t a t least twic e that ofth e metho d and/o rsolven t blanks
. Th e coefficien t ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o requa l t o 0.990 . Eac h poin t i n th e curve must b e withi n ±25 % o fth e theoretica l concentratio n wit h th e exceptio n o fth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 4 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### b e withi n ±30% . Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata
. Aminimu m o f6 points wil l b e use d t o constmc t th e calibratio n curve . I fth e calibratio n curve doe s no t meet acceptance criteria , perfomri routin e maintenance o rprepare a ne wstandar

d curve (i fnecessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yo fth 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 construc t th e calibratio n curve , a

t a minimu m afte rever ytent h sample , no

t includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set . Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable
. Th e calibratio n curve an d th e last passin g CCV wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that are quantitate d above th e concentratio n o fth e highest standar

d i n th e curve shoul d b e furthe rdilute d an d reanalyzed
. 1 0 Qualit y Contro l 10. 1 Dat a Qualit y Objective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LOQ 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 wdata an d footnote d i n th e final report . 10. 2 Metho d Blank s Metho d blank

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

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

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

d deviatio n ofth e are a counts ofthes e metho d blank s shoul d b e calculate d an d reported
. I f th e mea n are a counts 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 ralternatively , th e metho d blank s mus t b e evaluate d statisticall yt o determin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made
. 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s fleld blanks
. 10. 4 Surrogat e Spike s Surrogat e spike s are no

t require d bu t ma

yb e use d o n projec

t specifi crequirements
. 10. 5 La b Contro l Sampl e Triplicat e la b contro l spike s a t a minimu m o

ftwo differen t concentration s are t o b e prepare d wit h eac h preparatio n batch
. Lo wla b contro l spike s shoul d b e prepare d at concentration s i n th e rang e offive t o te n time s highe rtha n th e targete d LO Q an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t o fth e curve . Th e relative standar

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

ETS-8-044. 0 Pag e 9 o f1 1 Metho d ofAnalysi s fo rth e Detemninatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 5 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 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 o f70 % t o 130% , ma

yb e flagged as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targete d fortificatio n level s shoul d b e a t 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 determin e th e statemen t ofaccurac yfo ranalytica l results
. Th e averag e ofth e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 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 : A1 fJ /

; 1 X (Pea k

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

ywhic h th e final volum e wa s diluted , i fnecessary . Fo rsample s fortifie d wit h know n amounts ofanalyt e prio rt o extraction , us e th e followin g equatio n t o calculat e th e percen t recovery . Recov e - '^'^'^^^^'^^^'^'^^'^^'^^'^'S^^'^^'^'^^^^'^^^'^^ ^ xlO O Analyt e adde d (ng/mL ) 1 2 Metho d Performanc e An ymetho d performance parameter s that are no

t achieve d must b e considere d i n th e evaluatio n ofth 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 performance sectio n are no t met , maintenance ma

yb e performe d o n th e syste m an d sample s reanalyzed , o rothe raction s take n a s appropriate
. Documen t al l action s i n th e ra wdata
. I fdat a are t o b e reporte d whe n performance criteri a have no t bee n met , th e dat a must b e footnote d o n table s an d discusse d i n th e tex

t 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 ofeac h analytica l ai n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l o fth e calitiratio n curve an d are repeate d injection s fro m on e autosample rvial
. Th e syste m suitabilit yinjection s must have are a counts wit h a n RS D 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 ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.990 . Eac h poin t i n th e curve must b e withi n +25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

yb e withi n ±30% . CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac yof eac h curve poin t mus

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

yCCVs no

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

ETS-8-044. 0 Pag e 1 0 of1 1 Metho d ofAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 6 o f9 9GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


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

ychromatographi cretentio n tim e (withi n 4 % of standard ) an d th e mas s spectra l respons e 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 LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n ofappropriat e blank s an d th e accurac

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 ar

e designe d t o generat e dat a that are accurat e t o +/-30%
. Sectio n 1 0 contain s additiona l infomiatio 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 no t b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks
. Sectio n 1 0 contain s additiona l informatio n regardin g th e require d precisio n o flaborator ycontro l spikes
. 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfonnin g thi s metho d wil l b e dispose d ofappropriately
. Th e origina l sample s wil l b e archive d a

t th e 3 M Environmenta l Laborator yi n accordance wit h interna l procedures
. 

## 1 4 Record s Eac h data packag e generate d fo ra stud ymust includ e al l supportin g informatio n fo rreconstmctio n ofth e data
. Informatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

ypages) , instalmen 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 of1 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 9 7 o f9 9GLP10-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sr d Quarte rSamplin g - 201 1


### ATTACHIVIEN TD : DEVIATION(S )

Pag e 9 8 o f9 9GLP l 0-01-02 ; Interi m Repor t 2 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r 3rd Quarte rSamplin g - 201 1 

## RECOR D O F DEVIATION/NONCONFORMANC E

/. Identification Stud y/ Projec t No
. GLP10-01-02-2 2 Date(s ) o fOccurrence : b l l 1012a , kin020 a Documen t Number : ETS-8-044. 0 Deviatio n typ e • SO P • Equipmen t Procedur e 0 Metho d (Chec k one ) • Protoco l • GP O • Other : / /
. Description

(attach

extra pages as needed) 

### Metho d Requirements : 1 . Syste m Suitabilit yare a count s wit h RS D <5 % (sectio n 12.1)
. 2 . FM S recover ywithi n ±30 % (sectio n 10.6)
. 3 . LC S recover ywithi n ±20 % (sectio n 10.5)
. 4 . CC V recover ywithi n ±25 % (sectio n 12.2)
. 

### Actua l procedure/process : 1 . Th e syste m suitabilit yare a coun t RS D fo rPFO S wa s 7.5 % fo r'b111012 a PFO S sum ' an d 9.1 % fo r 'kl l 1020 a PFO S sum'
. 2 . Th e followin g samplin g location s ha d FM S sample s outsid e metho d acceptanc e criteri a fo rru n b l 11012a : DA L G W220 R fo rPFO S H S (61.9%) , DA L G W220 L fo rPFO S M S (61.9%) , DA L G W222 R fo rPFB S M S (66.8%) , PFH S H S (65.1%) , an d PFO S H S (56.9%) , DA L G W327 R fo rPFB S H S (65.4% ) an d PFH S H S (69.1%) , DA L G W330 L fo rPFB S (66.1%) , DA L G W331 8 fo rPFB S (68.5%) , DA L G W335 R fo rPFB S (69.1%) , DA L G WGRS0 4 fo rPFO S L S (63.0%) , TRIP0 1 fo rPFO S M S (68.0%) , an d TRIP0 2 fo rPFO S M S (65.9% ) an d H S (68.9%)
. 3 . Th e 0.2pp b LCS s ha d a n averag e recover yo f74. 1 % an d th e 2pp b LCS s ha d a n averag e recover yo f 78.1 % fo rPFO S i n ru n bl l 1020 a (summed)
. 4 . Fiv e CCV s fo rPFO S (summed ) i n ru n b111012 a ha d recoverie s greate rtha n 125 % (127 % -135%)
. 

### ///. Actions

Taken) (such as amendment

issued, SOP

revision, etc.) 

### Correctiv e Actio n ( • Ye s 0 No ) Reference : Acceptabilityo fth e nonconformin g work :

Th e syste m suitabilit yresult s fo rPFO S wil l b e note d i n th e fina l report . Samplin g location s wit h FM S recoverie s outsid e metho d acceptanc e criteri a wil l b e flagge d i n th e repor t an d th e analytica l uncertaint yadjuste d fo rth e sample s wher e th e non-complian t FM S wa s th e mos t appropriat e spikin g concentration
. Th e tri p blank s wer e als o relativel ylow , especiall yfo rPFOS , whic h ma yexplai n wh ysevera l sampl e FMS s ar e low
. Th e non-complian t LCS s wil l b e flagge d i n th e fina l report . Th e accurac yo fth e CCV s fo rPFO S increase d throughou t th e run , whic h suggest s instrumen t drift
. However , sinc e th e sampl e concentration s ar e simila rt o tha t o fpreviou s studie s performe d i n th e pas t fo r thi s sampl e set , sample s wer e no t re-analyzed
. Actions : • Haltin g o fWor k • Clien t Notificatio n • Wor k Recal l • Withholdin g o fRepor t 0 Other : Deviation s wil l b e note d i n fina l report . 

### Projec t Lead/PA I Approval : StudyDirecto r(i fGLP) : Sponso rApprova l (fo rGLI vprotoco l deviations) : N A Date : Date : Date : Technica l Reviewe r(optional) : N A Date : N A Laborator yDepartmen t Manage rApproval : Date :

IV. Authorization

to Resume

Work Where halting of work occurred, resumption

of work must first be approved

by Laboratory

Management 

### Laborator yDepartment Manage rApproval : N ADate : N A Deviation

No. (assigned

by Study Director or Team Leader at the end of study or project) ETS-4-008. 7 Pag e 1 o f1 Documentatio n o fDeviation s an d Contro l o fNonconformin g Testin g Pag e 9 9 o f9 9