GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 

# 3 M

GLP10-01-02

. Interi m Repor t 10 : Analysi s o fPFBS

. PFHS

. an d PFO S i n Groundwate r Sample s Collecte d a t Off-Sit e Well s locate d i n Decatur

. A L i n Octobe r201 0
Stud yTitl e Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) I n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
Dat a Requiremen t EP ATSC AGoo d Laborator

yPractic e Standard s 40 CFR Par

t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc

. 140 0 Westo n Wa y Westchester , P A1938 0 Phone : 610-701-376 1 Autho r Susan Wolf 3M Environmenta l Laborator y Interi m Repor t Completio n Dat e

Dat e o fsignin g Performin g Laborator y 3 M Environmental Healt

h and Safet

yOperations Environmental Laborator

y 3 M Center , Bidg 260-05-N-1 7 Maplewood , M N 5514

4 Projec t Identificatio n GLP10-01-02-1 0 Tota l Numbe ro fPage s

5 7

Th e testin g reporte d herei n mee t th e requirement s o fISO/IE C 17025-200 5 "Genera l Requirement s fo rth e Competenc e o fTestin g an d Calibratio n Laboratories", i n accordanc e wit h th e A2L ACertificat e #2052.01

. Testin g tha t complie s wit h thi s Internationa l Standar d als o operat e i n accordanc e wit h IS O 9001:2000

. Certificat e #2052.0 1

Pag e 1 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

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

.

Pag e 2 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Octobe r201 0



## GL P CoiviPLiANC E STATEMEN T Repor t Title : GLP10-01-02 , Interi m Repor t 10

. Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a

t Off-Site Well s locate d i n Decatur , A L i n Octobe r201 0 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 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 ofa test system
. •Th e reference substance s have no t bee n characterize d unde rth e GLP s an d th e stabilit yunde r storag e condition s a

t th e test sit e have no

t bee n detennine d unde rGLPs

.

Gar yHohenstein ; Sponso rRepresentative Date 

# OM^
. ' L Jaisimh a K^ari , P.E. , DEE , StudyDirecto r' Date

Pag e 3 of5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s ofPFBS , PFHS , an d PFO S i n Grundwate rfro m Decatur , A L Octobe r201 0



### QUALIT YASSURANC E STATEMEN T Report Title : GLP10-01-02 , Interi m Report 10

. Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a t th e Off-Sit e Well s locate d i n Decatur , A L i n Octobe r201 0 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 report an d th e accompanyin g dat a wer e audite d b yth e 3 M Environmenta l LaboratoryQualit y Assuranc e Uni t (QAU) , a s indicate d below

. Th e finding s wer e reporte d t o th e principa l investigato r (P.I.) , laboratorymanagemen t an d stud ydirector

.

Inspectio n Date s 12/2/10-12/3/1 0 Phas e Dat a an d Interi m Repor

t Date Reporte d t o Testin g Facilit y Managemen t 12/23/1 0 Stud yDirecto r 12/23/1 0

QA U Represrfitativ e 

# ^

. ^^ej ^

/-^'f l

Dat e

Pag e 4 of5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0



### TABL E O F CONTENT S GL P Compliance statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e ofContents 5 List ofTable s 6 1 Stud yInformatio n 8 2 Summar

y9 3 Introductio n 1 0 4 Test & Contro l Substance s 1 0 5 Reference Substance s 1 1 6 Test Syste m 1 3 7 Metho d Summar

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

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

Pag e 5 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

9 Data Summar

yan d Discussio n 1 7 1 0 Conclusio n 2 6 1 1 Data/Sampl e Retentio n 2 6 1 2 Attachment s 2 6 1 3 Signature s 2 7 

### LIS TO F TABLE S Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Results (Off-Site Groundwater , Decatur , AL ,

Octobe r2010 ) 9 Tabl e 2

. Instalmen t Parameter s 1 4 Tabl e 3

. Liqui d Chromatograph yCondition s 1 4 Tabl e 4

. Mass Transition s 1 4 Tabl e 5

. Limi t ofQuantitatio n (LOQ ) 1 5 Tabl e 6

. Laborator

yContro l Spik

e Recover

y1 6 Tabl e 7

. Analytica l Uncertaint y1 7 Tabl e 8

. Fiel d Matri xSpik e Level s 1 7 Tabl e 9

. DALGW602L10102 9 1 8 Tabl e 10

. DA L GW602 S 10102 9 1 8 Tabl e 11

. DALGW603L10102 9 1 9 Tabl e 12

. DA L GW603 S 10102 8 1 9 Tabl e 13

. DA L GW604 L 10102 9 2 0 Tabl e 14

. DA L GW604 S 10102 9

. > 2 0 Tabl e 15

. DA L GW605 R 10102 9 2 1 Tabl e 16

. DA L GW605L10102 9 2 1 Tabl e 17

. DA L GW607 R 10102 8 2 2 Tabl e 18

. DA L GW607 L 10102 8 2 2 Tabl e 19

. DA L GW609 R 10102 7 2 3 Tabl e 20

. DALGW609L10102 7 2 3

Pag e 6 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Table21

. DALGW6 1 I R 10102 7 2 4 Table22

. DALGW611 L 10102 7 2 4 Tabl e 23

. Tri p Blan k

2 5 Tabl e 24

. DA L G W602 S R B 10102 9 2 5

Pag e 7 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Octobe r201 0



### 1 Study.Informatio n ••#*

. yf-:
- - ' " •• ' ''^'^ Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Stud yDirecto r Jaisimh a Kesari , P.E. , DE E Westo n Solutions , Inc

. Westchester , P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 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(S)mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow ; Analys t Stud yDate s Stud yInitiation : Marc h 8 , 201 0 Interi m Repor

t 1 0 Experimenta l Termination : Novembe r09 , 201 0 Interi m Repor

t Completion : Date o

fInteri m Repor

t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t have 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 f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0



### 2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t Off-Site Well s locate d i n Decatur , AL , representin g fourtee n differen t samplin g locations

. Atota l offorty-five 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 ) analysis , an d include d duplicat e groundwate rsample s fro m eac h samplin g location

. Sample s als o include d on e fiel d matri x spik e (FMS ) sample s fo reac h location , on e tri p blan k containin g Milli-Q TM water , a tri p blan k spike , an d on e equipmen t rinseate sample

. Th e equipmen t rinseate blan k di d no t hav e FM S sample s prepare d fo rdeterminatio n ofPFBS , PFHS , an d PFO S recovery . Th e groundwate rsamples , tri p blan k an d on e equipmen t rinseate blan k were receive d fro m Westo n personne l o n Octobe r29,201 0 an d Novembe r 4 , 2010 : 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 an d conducte d unde r3 M projec t GLP-10-01-02-10

. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s ar e summarize d i n Tabl e 1

. Th e equipmen t rinseate an d th e tri p blan k were belo

wth e lowe rlimi t ofquantitatio n (LLOQ) , indicatin g adequat e contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections

. Th e PFB S concentratio n results fo ral l groun d water s range d fro m 0.061 5 ng/m L t o 0.48 0 ng/mL

. Th e PFH S concentratio n results fo ral l groun d water s range d fro m 0.039 6 ng/m L t o 0.62 2 ng/mL

. Th e PFO S concentratio n results fo ral l groun d water s range d fro m 0.0.0404 ng/m L t o 2.4 1 ng/mL

. Th e metho d uncertaint yfo rPFB S i s 100 % ±16% , PFH S 100 % ±16% , an d PFO S 100 % ±21%

. Tabl e 1

. Summarize d PFOAResult s (Off-Sit e Groundwater , Decatur , AL , Octobe r2010 ) Sampl e I D DA L GW602 L 10102 9 DA L GW602 S 10102 9 DALGW603L10102 9 DA L GW603 S 10102 8 DA L GW604 L 10102 9 DA L GW604 S 10102 9 DA L GW605 R 10102 9 DALGW605L10102 9 DA L GW607 R 10102 8 DA L GW607 L 10102 8 DALGW609L10102 7 DA L GW609 R 10102 7 DA L GW6 1 I R 10102 7 DA L GW6 1 I L 10102 7 Tri p Blan k

(Milli-Q TM Water ) Equipmen t rinseate blank s Avg

. PFB S Concentratio n (nq/mL ) ±RP D 0.081 3 ±0.49 % 0.23 9 ±12 % 0.11 2 ±19 % 0.15 8 ±7.6 % 0.27 9 ±17 % 0.30 3 ±14 % 0.11 9 ±23 % [a ] 0.40 6 ±0.49 % 0.087 0 ±0.12 % 0.061 5 ±2.8 % 0.25 9 ±8.9 % 0.48 0 ±14 % 0.19 1 ±6.3 % 0.31 7 ±1.3 % < 0.025 0 < 0.025 0 Avg

. PFH S

Concentratio n (ng/mL ) ±RP D 0.29 1 ±27 % [a ] 0.12 7 ±6.3 % 0.10 9 ±14 % 0.12 2 ±3.3 % 0.21 5 ±14 % 0.22 4 ±8.5 % 0.066 1 ±3.2 % 0.62 2 ±23 % [a ] 0.070 7 ±13 % 0.082 3 ±38 % [a l 0.47 7 ±1.0 % 0.15 4 ±37 % [a ] 0.039 6 ±32 % [a ] 0.16 7 ±0.60 % < 0.025 0 < 0.025 0 Avg

. PFO S

Concentratio n (ng/mL ) ±RP D 0.74 4 ±8.6 % 0.71 0 ±17 % 0.10 2 ±5.2 % 0.22 0 ±6.8 % 1.4 6 ±3.4 % 0.47 2 ±8.9 % 0.040 3 [b ] 0.52 2 ±2.5 % 0.061 1 ±4.6 % 0.092 0 ±8.2 % 2.4 1 ±5.0 % [c ] 0.16 4 ±39 % [a ] 0.58 0 ±7.2 % 0.93 3 ±5.1 % < 0.040 0 < 0.040 0 N/A ; no t applicabl e [a] Th e sample/sampl e duplicat e RP D was ^0%

. [b ] ARP D coul d no

t b e calculate d as on e ofth e sampl e replicate s wa s <LOQ

. [c] Samplin g locatio n di d not hav e a n appropriate FM S spik e leve l t o sufficientl yevaluat e PFO S recovery .

Pag e 9 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0



### 3 Introductio n Thi s analytica l stud ywa s conducte d a s par t o fth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama

. Th e objectiv e o fth e overal l progra m i s t o gai n informatio n regardin g concentration s o fperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediment s tha t ar e associate d wit h an d nea rth e Decatu rfacility

. Thi s analytica l stud ywa s conducte d t o analyz e ground wate rsample s collecte d fro m off-sit e 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 Laboratoryprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h wer e shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling

. Sampl e bottl e set s fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d a fiel d spik e sample

. Eac h empt ycontaine rfo rgroundwate rsampling s wa s marke d wit h a "fil l t o here " lin e t o produc e a fina l sampl e volum e o f20 0 mL

. Container s designate d fo rfiel d matri xsample s wer e fortifie d wit h a n appropriat e matri xspik e solutio n containin g PFBS , PFHS , an d PFO S prio rt o bein g sen t t o th e fiel d fo r sampl e collection

. Al l sampl e bottle s als o include d th e additio n o finterna l standard s ^^02-PFBS , ^^02 - PFHS , an d ^^C4-PF0 S a t a nomina l concentratio n o f1 ng/mL

. Al l sampl e bottle s als o include d th e additio n o fsurrogat e spik e "C4-PFO S at a nomina l concentratio n o f0. 1 ng/mL

. Se e sectio n 8. 8 o fth e report fo rfiel d matri xspik e levels

. Sample s wer e prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laboratorymetho d ETS-8-044. 0 "Determinatio n o fPerfluorinate d Compound s i n Wate rb yHig h Performanc e Liqui d Chromatography/Mas s SpectrometryDirect Injectio n Analysis"

. Tabl e 1 summarize s th e averag e PFBS , PFHS , an d PFO S concentration s fo rth e duplicat e groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples

. Table s 9-2 4 summariz e th e individua l sampl e result s an d th e associate d FM S recoveries

. Al l result s fo rth e qualit y contro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discussed elsewher e i n thi s report
. 4 Tes t & Contro l Substance s Ther e wa s no t a tes t substanc e o rcontro l substance s i n th e classi csens e o fa GL P study

. Thi s stud y wa s purel yanalytica l i n nature
.

Pag e 1 0 of57GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0



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

.

Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFB S (predominantl ylinear ) Perfluorobutan e sulfonate C4F9S03 ' Potassiu m Sal t 3 M 1/10/201 7 Froze n 41-2600-8442- 5 TCR-12 1 White Powde r 96.7 % PFH S (linear ) Perfluorohexan e sulfonate C6F13SO3" Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHxSAM0 8 TCR08-001 8 Crystallin e 98 %

Referenc e Substanc e Chemica l Nam e Chemica l Fomiul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO S (linear ) Perfluorooctan e sulfonat e CfiFiySO s Potassiu m Sal t CA S #2795-39- 3 Wellingto n 10/18/201 3 Froze n LPFOSKBM0 6 TCR08-000 1 Crystallin e 98 % PFO S (linea r+ branched ) Perfluorooctan e sulfonat e CeFiySOa ' Potassiu m Sal t CAS #2795-39- 3 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 White Powde r 86.4 %

Pag e 1 1 o f5 7GLP10-0 1 -02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "OjrPFB S Labele d - Perfluorobutan e sulfonate C4F9S[''02]0 " Ammoniu m Sal t RT I Internationa l 3/9/201 5 Froze n 11546-107- 2 TCR-1022,TCR-1028an d TCR-103 3 Liqui d 99 % "Oj-PFH S

Labele d - Perfluorohexan e sulfonat e CeFisSrOzj^'Q
Sodiu m Sal t Wellingto n 04/29/201 3 Froze n MPFC-C-041 0 TCR10-003 7 Liqui d NA'^ ' Referenc e Substanc e Chemica l Nam e Chemica l Fomriul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "C,-PFO S Perfluorooctan e sulfonat e CsFi ySO 3 Sodiu m Sal t Wellingto n 04/29/201 3 Froze n MPFC-C-041 0 TCR10-003 7 Liqui d NA<^> (1 ) Compoun d i s par

t ofa custo m mixtur

e ofmass-latiele d perfluorinate d compound s a t a concentratio n of5. 0 pg/mL

.

Pag e 1 2 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

6 Tes t Syste m There wa s no

t a test syste m fo rthi s stud yi n th e classi csens e ofa GL P study

. Thi s stud ywa s conducte d fo ranalysi s ofgroun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b yWesto n Solutions , Inc

. personnel

. Sample s fo rthi s stud yare "rea l worid " environmenta l samples

. Sampl e Descriptio n Ke yCode

. Strin g Numbe r Exampl e 1 2 3 4

5 6 Strin g Descripto r DA L GW602 S 010102 9 Sampl e Locatio n Sampl e Typ e Wel l I D Wel l Leve l
Samplin g Dat e Sampl e Typ e Exampl e DAL = Decatur , Alabam a GW = Groundwate r Example : 602 R = Residu m shallo wwater-bearin g zon e L = Bedroc k

water-bearin g zin e S - Epikars t middl e water-bearin g zon e 101029-Octobe r29,201 0 0=primai ysampl e DB=duplicat e sampl e L S = lo wspik e R B = Rinseat e Blan k

7 Metho d Summar y 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 "Detenninatio n ofPerfluorinate d Compound s I n Wate rb yHig h Perfomnanc

e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

. 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory

. Sampl e bottle s were returne d t o th e laborator ya t ambien t condition s o n Octobe r29 , 201 0 an d Novembe r4 , 2010

. Sample s were store d refrigerate d a t th e laborator

yafte r receipt

. Aset o

flaborator

yprepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspik

e sample 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

. 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 perfonnance liqui d chromatography/tande m mas s spectrometr y(HPLC/MS/MS)

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

wdat a har

d copie s place d i n th e fina l data packet , an d are briefl ydescribe d belo wi n Tabl e 2 , Tabl e 3 an d Tabl e 4

.

Pag e 1 3 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 2

. Instrumen t Parameters

. instrumen t Nam e Analytica l IVIethod Followe d Analysi s Dat e Liqui d Chromatograp h Guard colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETS Ginge r ETS-8-044. 0 11/08/1 0 Agilen t 120 0 Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n Betasi l 01 8 (2. 1 m m X 10 0 mm) , 5 n 2 5 u L Applie d Biosystem s AP I 500 0 Turb o Spra

y Turb o Io n electi-od e Negativ e Analyst 1.4. 2 Tabl e 3

. Liqui d Chromatograph yConditions

. ste p Numbe r 0 1 2 3 4 5 Tota l Tim e

(min ) 0 1. 0 13. 0 15. 0 15. 5 17. 0 Flo wRat e

(fiUmin ) 75 0 75 0 75 0 75 0 75 0 75 0 Percent A

( 2 m M ammoniu m acetate )

97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 Percent S

(Methano O 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 Tabl e 4

. Mas s Transitions

.

Analyt e PFB S PFH S
PFO S fC^PFO S surrogat e Mas s Transitio n Q1/Q3 299/8 0 299/9 9 399/9 9 399/8 0 499/9 9 499/8 0 499/13 0 503/8 0 Intema l Standar d t'OgjPFB S f'OglPFH S
t'CJPFO S ["CslPFO S Mas s Transitio n Q1/Q 3 303/8 4 403/8 4
507/8 0 507/8 0 Dwel l time was 5 0 mse cfo reac h transition

. Th e individua l transition s wer e summe d t o produce a "tota l io n chromatogram " (TIC) , whic h wa s use d fo rquantitation

.
'SK^'Analytica l Result s 8. 1 Calibratio n Sample s were analyze d against a stabl e isotop e matrix-matche d intema 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 laborator yprepare d syntheti cgroundwate rcontainin g calciu m an d magnesium

. A

Pag e 1 4 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

tota l ofeleve n spike d standard s rangin g fro m 0.02 5 ng/m L t o 1 0 ng/m L (nominal ) analyzed

. Th e 0.02 5 ng/m L curve poin t wa s disable d fo rPFO S t o meet accurac ycriteria

. Aquadratic , 1/

xweighted , calibratio n curve ofth e pea k are a counts wa s use d t o fi t th e data fo reac h analyte

. Th e data 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 confinne d accurac

yo feac h curve point

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

yrequirements of100±25 % (100±30 % fo rth e lowest curve point) were me t fo ral l analytes

. Th e con-elatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFBS , PFHS , an d PFOS

. 

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

d wa s analyze d fou rtime s a t th e beginnin g ofth e analytica l sequence t o demonstrat e overal l syste m suitability

. Al l analyte s met th e acceptance criteri a ofless tha n o requa l t o 5 % relative standar

d deviatio n (RSD ) fo rpea k rati o an d retentio n tim e criteri a ofless tha n o requa l t o 2 % RS D wa s met fo rPFB S an d PFOS

. Th e are a rati o fo rPFH S wa s 5.9%

. Ametho d deviatio n i s file d wit h th e ra wdata

. 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LO Q 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 ofth e appropriat e blanks

. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 5

. Tabl e 5

. Limi t o fQuantitatio n (LOQ)

. Analysi s Dat e 11/08/1 0 PFB S

LOQ , ng/m L 0.025 0 PFH S

LOQ , ng/m L 0.025 0 PFO S

LOQ , ng/m L 0.040 0 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 confin n that th e instmmen t respons e an d th e initia l calibratio n curve were stil l i n control

. Al l CCVs met metho d criteri a o f100 % ±25%

. 

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

s were prepare d an d analyze d wit h th e samples : metho d blanks , tri p blank s an d equipmen t rinseate blanks

. Metho d blan k results were reviewe d an d use d t o evaluate metho d perfonnance t o detennin e th e LOQ fo reac h analyte

. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience

. Equipmen t rinseate blank s ar e aqueou s sample s that reflec t th e efficienc

yofequipmen t cleanin g i n th e fiel d betwee n differen t sampl e collection s an d are proofofn o cros s contaminatio n o fsample s fro m th e equipment

. 8. 6 La b Contro l Spike s (LCSs ) La b contro l spike s were prepare d an d analyze d i n triplicat e a t two levels

. LCS s were prepare d b y spikin g know n amounts ofth e targe t analyte s into 1 0 m L oflaborator yprepare d syntheti cgroundwate r t o produce th e desire d concentration

. Th e spike d wate rsample s were the n analyze d i n th e sam e manne ra s th e samples

. Th e metho d acceptance criteria , averag e o fLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <20% , were me t fo rPFBS , PFHS , an d linea rPFOS

. A s th e reference material s use d fo rquantitatio n ofPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s ar

e comprise d oflinea ran d branche d isomers , additiona l LC S sample s o flinea r an d branche d PFO S were prepare d a t two concentration s t o evaluat e th e potentia l fo ranalytica l bias

. Th e linea ran d branche d LC S a t bot h level s di d no

t mee t metho d acceptance criteri a wit h averag e

Pag e 1 5 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

recoverie s of126 % an d 122% , respectively

. Al l LC S results were use d i n th e detenninatio n o fmetho d analytica l uncertaint

yi n sectio n 8.7

. Th e followin g calculation s were use d t o generat e data i n Tabl e 6 fo rlaborator ycontro l spikes :

, „ „ „ . „ Calculate d Concentratio n . , „„. . LC S Percen t Recover

y= * 100 % Spike Concentratio n

LCS % RS D -

• standard deviatio n LC S replicate s . averag e LC S recover

y 100 %

Tabl e 6

. Laborator yContro l Spik e Recovery

. ETS-8-044. 0 Analyze d 11/08/1 0

La b I D LCS-101105- 1 LCS-101105- 2 LCS-101105- 3 Averag e ±%RS D LCS-101105- 4 LCS-101105- 5 LCS-101105- 6 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 Calculate d

Concentratio n (ng/mL ) 0.20 0 0.20 0 0.21 5 VoRecover y

10 1 10 1 10 9 104 % ±4.5 % 1.9 8 1.9 8 .1.9 8 2.0 3

1.8 2 2.0 5 10 3

92. 2 10 4 100 % ±6.6 % PFH S Spike d Concentratio n (ng/mL ) 0A9 8 0.19 8 0.19 8 Calculate d

Concentratio n (ng/mL ) 0.21 2 0.20 7 0.22 0 %Recover y

10 7 10 5 11 1 108 % ±2.8 % 1.9 9 1.9 9 1.9 9 1.9 6

1.9 1 1.9 7 98. 6

95. 9 98. 8 97.8 % ±1.7 %

ETS-8-044. 0 ^alyze d 11/08/1 0

La b I D LCS-101105- 1 LCS-101105- 2 LCS-101105- 3 Averag e ±%RS D LCS-101105- 4 LCS-101105- 5 LCS-101105- 6 Averag e ±%RS D PFO S (linear )

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

Concentratio n (ng/mL ) 0.18 9 0.20 8 0.21 8 YoRecover y

95. 6 10 5 11 0 104 % ±7.1 % 1.9 8 1.9 8 1.9 8 1.9 7

1.8 9 2.0 9 99. 3

95. 4 10 6 100 % ±5.3 % La b I D LCS-101105- 7 LCS-101105- 8 LCS-101105- 9 Averag e ±%RS D LCS-101105-1 0 LCS-101105-1 1 LCS-101105-1 2 Averag e ±%RS D PFO S (linear * branched ) Spike d Concentratio n (ng/mL ) 0.19 6 0.19 6 0.19 6 Calculate d

Concentratio n (ng/mL ) 0.25 6 0.23 4 0.25 0 %Recover y

13 1 11 9 12 8 126 % ±5.0%" ' 1.9 7 1.9 7 1.9 7 2.5 2

2.4 2 2.2 9 12 8

12 3 11 6 122 % ±4.9%'^ ' (1 ) Laborator

ycontro l sampl e averag e recover ydi d no t mee t metho d acceptance criteri a o f100 % ±20%

.

Pag e 1 6 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Octobe r201 0



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

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

yan d precision

. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2

. Th e standar d deviatio n i s calculate d fo rth e set ofaccurac yresults (i n %) obtaine d fo rth e Q C samples

. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto ro f2 , whic h correspond s t o a confidence leve l of95%

. Tabl e 7

. Analytica l Uncertainty

. Analyt e PFB S PFH S PFO S Standar d Deviatio n

8.0 6 7.9 9 10. 7 Metho d

Uncertaint y 100%±16 % 100%±16 % 100%±21 % 8. 8 Fiel d Matri xSpike s (FMS ) Afiel d matri xspik

e sampl e wa s 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 collec:ted matrix

. Fiel d matri xspike s were generate d b yaddin g a measure d volum e of fiel d sampl e t o a containe rspike d 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 o f100±30 % c^nfimri that "unknown " components i n th e sampl e matri xd o no t significantl yinterfere wit h th e extractio n an d analysi s o fth e analyte s ofinterest

. Fiel d matri xspik e concentration s must b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike

. Fiel d matri xspike s are presente d i n sectio n 9 o fthi s report
. Tabl e 8

. Fiel d IVIatri xSpik e Levels

. Samplin g Locatio n Al l samplin g location s PFBS , ng/m L 0.99 9 PFHS , ng/m L 1.0 0 PFOS , ng/m L

0.99 9 (Sample Concentrationof

FMS - Average Concentration: FieldSampl e & FieldSampl

e Dup. ) .,„„„ , FMS Recover

y = -^ ^ = ^ ^-^ * 100% Spik e Concentraton
9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s as wel l as th e Tri p Blank s an d rinseate blanks

. Results an d averag e value s are rounde d t o thre e significan t figure s accordin g t o EP Aroundin g ailes

. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata

. Fiel d matri xspike recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrate tha t th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges .

Pag e 1 7 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tables

. DA L GW602 L 10102 9

3 M LIM S I D GLP10-01-01-10-02 4 GLP10-01-01-10-02 5 GLP10-01-01-10-02 6 Descriptio n DA L GW602 L 0 10102 9 DA L GW602LD B 10102 9 DA L GW602LL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.081 5 0.081 1 1.0 2 XRecover y

N A N A 94. 0 0.081 3 ng/m L i 0.49 % PFH S Concentratio n (ng/mL ) 0.32 9 0.25 2 1.33 VoRecover y N A N A 104 0.29 1 ng/m L ±17%^^

> PFO S Concentratio n (ng/mL ) 0.71 2 0.77 6 1.8 1 %Recover y N A N A 10 7 0.744 ng/m L ±8.6 % NA= No t /Applicabl e (1 ) Th e sample/sampl e duplicat e RP D was 220%

. Tabl e 10

. DA L G W602 S 10102 9

3MUIVISI D GLP10-01-01-10-02 8 GLP10-01-01-10-02 9 GLP10-01-01-10-03 0 Descriptio n DA L GW602 S 0 10102 9 DA L GW602SD B 10102 9 DA L GW602SL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.22 4 0.25 3 1.4 8 XRecover y

N A N A 12 4 0.23 9 ng/m L ±12 % PFH S Concentratio n (ng/mL ) 0.12 3 0.13 1 0.94 4 %Recover y N A N A 81. 7 0.12 7 ng/m L ±6.3 % PFO S Concentratio n (ng/mL ) 0.64 8 0.77 2 1.49 %Recovery

N A N A 78. 1 0.71 0 ng/m L ±17 % NA= No t /Applicabl e

Pag e 1 8 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 11

. DA L GW603 L 10102 9

3 M LIM S I D GLP10-01-01-10-03 4 GLP10-01-01-10-03 5 GLP10-01-01-10-03 6 Descriptio n DA L GW603 L 0 10102 9 DA L GW603LD B 10102 9 DA L GW603LL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.10 1 0.12 2 1.1 6 %Recover

y N A N A 105 0.11 2 ng/mL±19 % PFH S Concentratio n (ng/mL ) 0.10 1 0.11 6 1.0 4 %Recover

y NA NA 93. 2 0.10 9 ng/m L ±14 % PFO S Concentratio n (ng/mL ) 0.10 5 0.099 7 1.0 2 %Recover

y N A N A 91. 9 0.10 2 ng/m L ±5.2 % \i h = No t Applicabl e Tabl e 12

. DA L G W603 S 10102 8

3I\IIUMSI D GLP10-01-01-10-02 1 GLP10-01-01-10-02 2 GLP10-01-01-10-02 3 Descriptio n DA L GW603 S 0 10102 8 DALGW603SD B 10102 8 DA L GW603SL S 10102 8 Averag e Concentratio n (ng/mL ) ±"ARPD/RS D PFB S Concentratio n (ng/mL ) 0.16 4 0.15 2 1.1 2 %Recover

y N A N A 96. 3 0.15 8 ng/m L ±7.6% PFH S Concentratio n (ng/mL ) 0.12 4 0.12 0 0.95 2 %Recover y NA NA 83. 0 0.12 2 ng/m L ±3.3 % PFO S Concentratio n (ng/mL ) 0.21 2 0.22 7 0.99 7 %Recover y N A N A 77. 8 0.22 0 ng/m L ±6.8 % NA= No t Applicabl e

Pag e 1 9 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 13

. DA L G W604 L 10102 9

3 M LIM S I D GLP10-01-01-10-03 7 GLP10-01-01-10-03 8 GLP10-01-01-10-03 9 Descriptio n DA L GW604 L 0 10102 9 DA L GW604LD B 10102 9 DA L GW604LL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.25 5 0.30 2 1.27 %Recovery

N A N A 99. 2 0.27 9 ng/mL±17 % PFH S Concentratio n (ng/mL ) 0.20 0 0.22 9 1.2 9 %Recover y N A NA 108 0.21 5 ng/m L ±14 % PFO S Concentratio n (ng/mL ) 1.48 1.43 2.3 2 %Recover y N A N A 86. 6 1.4 6 ng/m L ±3.4 % N A= Not Applicabl e Tabl e 14

. DA L G W604 S 10102 9

3 M LIM S I D GLP10-01-01-10-04 0 GLP10-01-01-10-04 1 GLP10-01-01-10-04 2 Descriptio n DA L GW604 S 0 10102 9 DA L GW604SD B 10102 9 DALGW604SL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.32 4 0.28 2 1.3 1 %Recover

y N A N A 10 1 0.30 3 ng/m L ±14 % PFH S Concentratio n (ng/mL ) 0.21 4 0.23 3 1.07 %Recover y N A N A 84. 7 0.22 4 ng/m L ±8.5 % PFO S Concentratio n (ng/mL ) 0.49 3 0.45 1 1.3 3 VoRecover

y N A N A 85. 9 0.47 2 ng/m L ±8.9 % NA= No t Applicabl e

Pag e 2 0 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 15

. DA L G W605 R 10102 9

3MUMSI D GLP10-01-01-10-04 3 GLP10-01-01-10-04 4 GLP10-01-01-10-04 5 Descriptio n DA L GW605 R 0 10102 9 DA L GW605RD B 10102 9 DA L GW605RL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.10 5 0.13 2 1.1 4 %Recover

y N A N A 102 0.11 9 ng/mL±23%'' > PFH S Concentratio n (ng/mL ) 0.067 1 0.065 0 0.93 1 %Recover y N A N A 86. 5 0.066 1 ng/m L ±3.2 % PFO S Concentratio n (ng/mL ) <0.040 0 0.040 3 0.95 2 %Recover y N A N A 91. 3 0.040 3 ng/mL ^ NA= No t Applicabl e (1 ) Tfi e sample/sampl e duplicate RP D wa s 220%

. (2 ) ARP D coul d not b e calculate d a s on e sampl e replicate wa s <LOQ

. Tabl e 16

. DA L GW605 L 10102 9

3 M LIM S I D GLP10-01-01-10-03 1 GLP10-01-01-10-03 2 GLP10-01-01-10-03 3 Descriptio n DA L GW605 L 0 10102 9 DALGW605LD B 10102 9 DA L GW605LL S 10102 9 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.40 7 0.40 5 1.53 %Recover

y N A NA 11 3 0.40 6 ng/m L ±0.49 % PFH S Concentratio n (ng/mL ) 0.69 3 0.55 1 1.89 %Recover y N A N A 12 7 0.62 2 ng/m L ±23 % f^

' PFO S Concentratio n (ng/mL ) 0.52 8 0.51 5 1.4 2 %Recover

y N A N A 89. 9 0.52 2 ng/m L ±2.5 % NA= No t Applicabl e (1 ) Th e sample/sampl e duplicate RP D wa s 220%

.

Pag e 2 1 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 17

. DA L G W607 R 10102 8

3 M LIM S I D GLP10-01-01-10-00 4 GLP10-01-01-10-00 5 GLP10-01-01-10-00 6 Descriptio n DA L GW607 R 0 10102 8 DALGW607RD B 10102 8 DA L GW607RL S 10102 8 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.087 0 0.086 9 1.1 6 %Recover

y N A N A 10 7 0.087 0 ng/m L ±0.12 % PFH S Concentratio n (ng/mL ) 0.066 1 0.075 3 1.1 1 VoRecover y N A NA 10 4 0.070 7 ng/m L ±13 % PFO S Concentratio n (ng/mL ) 0.062 5 0.059 7 1.0 2 VoRecover

y N A N A 96. 0 0.061 1 ng/m L ±4.6 % N A= No t Applicabl e
Tabl e 18

. DA L GW607 L 10102 8

3 M LIM S I D GLP10-01-01-10-00 1 GLP10-01-01-10-00 2 GLP10-01-01-10-00 3 Descriptio n DA L GW607 L 0 10102 8 DA L GW607LD B 10102 8 DA L GW607LL S 10102 8 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.060 6 0.062 3 1.1 2 VoRecover

y N A N A 10 6 0.061 5 ng/m L ±2.8 % PFH S Concentratio n (ng/mL ) 0.066 5 0.098 0 1.0 4 VoRecover

y N A N A 95. 8 0.082 3 ng/mL±38Vo^ ' PFO S Concentratio n (ng/mL ) 0.088 2 0.095 7 1.06 VoRecover y

. N A N A 96. 9 0.092 0 ng/m L ±8.2 % N A= No t Applicabl e (1 ) Th e sample/sampl e duplicate RP D wa s 220%

.

Pag e 2 2 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 19

. DA L GW609 R 10102 7

3 M LIM S I D GLP10-01-01-10-01 0 GLP10-01-01-10-01 1 GLP10-01-01-10-01 2 Descriptio n DA L GW609 R 0 10102 7 DALGW609RD B 10102 7 DA L GW609RL S 10102 7 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.44 6 0.51 3 1.7 1 VoRecover

y N A N A 12 3 0.48 0 ng/m L ±14 % PFH S Concentratio n (ng/mL ) 0.12 5 0.18 2 1.06 VoRecover y N A N A 90. 7 0.154ng/m L ±3r/o^ ^ PFO S Concentratio n (ng/mL ) 0.13 2 0.19 6 1.09 VoRecover y N A N A 92. 7 0.16 4 ng/m L ±39%^^

^ N A= Not Applicabl e (1 ) Th e sample/sampl e duplicate RP D wa s >20%

. Tabl e 20

. DA L GW609L10102 7

3MUMSI D GL P 10-01-01-10-00 7 GLP10-01-01-10-00 8 GL P 10-01-01-10-00 9 Descriptio n DA L GW609 L 0 10102 7 DA L GW609LD B 10102 7 DALGW609LL S 10102 7 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 0.27 0 0.24 7 1.36 %Recover

y NA N A 11 0 0.25 9 ng/m L ±8.9 % PFH S Concentratio n (ng/mL ) 0.47 9 0.47 4 1.56 VoRecover y

. N A N A 10 8 0.47 7 ng/m L ±1.0 % PFO S Concentratio n (ng/mL ) 2.4 7 2.3 5 3.5 5 VoRecover y N A N A N C 2.4 1 ng/m L ±5.0%'^ ' N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Th e samplin g locatio n di d no t hav e a n appropriate FI\/I S t o sufficientl yevaluate PFO S recovery .

Pag e 2 3 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 21

. DA L G W6 1 I R 10102 7

3 M LIM S I D GLP10-01-01-10-01 3 GLP10-01-01-10-01 4 GLP10-01-01-10-01 5 Descriptio n DA L GW611 R 0 10102 7 DA L GW611RD B 10102 7 DALGW611 R LS 10102 7 Averag e Concentratio n (ng/mL ) ±VoRPD/RS D PFB S Concentratio n (ng/mL ) 0.18 5 0.19 7 1.2 3 VoRecover

y N A N A 10 4 0.19 1 ng/m L ±6.3 % PFH S Concentratio n (ng/mL ) 0.033 3 0.045 9 1.04 VoRecover y N A N A 10 0 0.039 6 ng/m L ±32 % f^

' PFO S Concentratio n (ng/mL ) 0.55 9 0.60 1 1.60 VoRecover y N A N A 102 0.58 0 ng/m L ±7.2 % NA= No t Applicabl e (1 ) Th e sample/sampl e duplicate RP D wa s 220%

. Tabl e 22

. DA L G W611 L 10102 7

3 M LIM S I D GLP10-01-01-10-01 6 GLP10-01-01-10-01 7 GLP10-01-01-10-01 8 Descriptio n DA L GW611L 0 10102 7 DALGW611LD B 10102 7 DALGW611 L LS 10102 7 Averag e Concentratio n (ng/mL ) ±VoRPD/RS D PFB S Concentratio n (ng/mL ) 0.31 5 0.31 9 1.36 VoRecover

y N A N A 104 0.31 7 ng/m L ±1.3 % PFH S Concentratio n (ng/mL ) 0.16 7 0.16 6 1.06 VoRecover y N A N A 89. 4 0.16 7 ng/m L ±0.60 % PFO S Concentratio n (ng/mL ) 0.95 7 0.90 9 1.85 VoRecover y N A N A 91. 8 0.93 3 ng/m L ±5.1 % NA= Not Applicabl e

Pag e 2 4 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Tabl e 23

. Tri p Blan k

3 M LIM S I D GLP10-01-01-10-01 9 GLP10-01-01-10-02 0 Descriptio n TRI P BLAN KSAMPL E TRI P BLAN KFM S PFB S Concentratio n (ng/mL ) <0.025 0 1.0 5 VoRecover

y N A 10 5 PFH S

Concentratio n (ng/mL ) <0.025 0 0.93 2 %Recover y N A 93. 2 PFO S

Concentratio n (ng/mL ) <0.040 0 0.93 3 %Recover y N A 93. 4 NA= No t Applicabl e Tabl e 24

. DA L G W602 S R B 10102 9

3 M LIM S I D GLP10-01-01-10-02 7 Descriptio n DA L GW602SR B 10102 9 PFB S Concerttratio n (ng/mL ) <0.025 0 PFH S

Concentratio n (ng/mL ) <0.025 0 PFO S

Concentratio n (ng/mL ) <0.040 0 N A= No t Applicabl e

Pag e 2 5 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

10..emtlusio n .{^'MV- : ..^:n?5U. , \^?^^' ^ " ' :1^^^i C Laborator ycontro l spike s an d field matri xspike s were use d t o detennin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS

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

. 1 1 Data/Sampl e Retentio n Al l remainin g sample s an d associate d projec t data (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures

. 

### 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 1 0 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d Attachmen t D : Metho d Deviatio n

Pag e 2 6 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Octobe r201 0



### 1 3 Signature s 

# ^4)21 " I Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date 

## ^^JTT^^O/ / Willia m K

. Reagen , Ph.D. , 3 M Environmenta l Laborator yManage r Date

Gar yHohenitein,/^!^ ! Sponso rRepresentative / / 

# l \ 

# ou ^ Date



# M L I /Dat e Jaisimh a Kes^i^tud yDirecto r

Pag e 2 7 of5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Attachment AOctober201 0 ^ ,...• , r , . . , ^

. n../ , r,. < o o Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 0



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

Decatu rPhas e 3 Site-Relate d Monitorin g Progran n

PROTOCO L AMENDMEN TNO

. 1 0

Amendmen t Date : Octobe r19 , 201 0 Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

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

Laborator yProjec t Identificatio n

GLP10-01-0 2

Samplin g Even t Off-Sit e Phas e 3 NewMonitorin g Well s

Pag e 1 of7 Pag e 2 8 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t AOctobe r201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 0 

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

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

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

.

AMEN D T

O READ : N o change s t o th e wordin g o fth e protoco l are required

. Thi s amendmen t onl yaddresse s an d document s th e additio n o fth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s fro m Decatur , AL , an d conducte d a s par t o fth e 3 M Decatu rPhas e 3 Progra m fo rPFOS , PFH S an d PFB S (GLP10-01-02)

. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e o fOctobe r25 , 2010

. 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 y LIM S a s project GLPlO-01-02-1 0 an d reporte d a s interi m repor t GLPlO-01-02-10 , (reflectin g stud y GLP10-01-0 2 an d amendmen t -10)

.

Reason : Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Projec t Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio 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 as attache d t o thi s amendmen t form

.

Pag e 2 of7 Pag e 2 0 o f5 7Attachmen t A GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 0 

### Amendmen t Approva l



# ifti- u w/m^/jj
. 

# "

A '0 Gar yHohenstein , Sponso rRepresentative Date

^ D3te Clesto n C

. Lange , Principa l Analytica l Investigato r


### / o / ' ^ o yj>c ya Willia m Reagen l EH S Opn s Environmenta l La b Managemen t 

# (M>v/ / Date



# \\kk

_ I Date Jaisimh a Kfesar

i P.E. , DEE , Stud yDirecto r

Pag e 3 of7 Pag e 3 0 o f5 7Attachmen t A GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 0 

### Environmenta l Healt h & Safet yOperations , 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

Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charle s Young , Westo n Solution s Ti m Frinak , Westo n Solution s Date : Ocotbe r19,201 0 Subject : Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d

Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 1 0 - Off-Sit e Phas e 3 Ne w Monitorin g Well s 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r Projec t Schedulerres t Date s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 Qahohenstein(a)mmm.co m 3 M Environmenta l Laborator yManagemen t Willia m K

. Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wkreaaen(S)mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanaeOmmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinakiawestonsolutions.co m Phone : (334)-332-912 3 GLP10-01-02-1 0 Dep t #530711 , Project #002267444 9 Samplin g schedule d fo rth e wee k o fOctobe r25 , 201 0 Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein

. Pag e 4 o f7 Pag e 3 1 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen tAOctobe r201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 0 

### 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 surfac e wate ran d groundwate rsample s collecte d fro m twenty-fiv e samplin g location s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) a s par t o fth e Avenu e A Investigation

. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC AGoo d Laborator y Practic 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 Octobe r25 , 2010

. Th e 3 M Environmenta l Laborator ywil l prepare th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFBS , PFHS , an d PFO S are o fa 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
- 01-02-10

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

o fOctobe r 25,2010

. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l o n Friday , Octobe r22 , 2010

. 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

Pag e 5 o f7 Pag e 3 2 o f5 7GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachment AOctober201 0 , .- , ow, ^ n. . /i n Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 0 

### 4 Tes t Parameter s Th e targete d limi t ofquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS

. PFHS , an d PFOS

. Atota l o fseventee n samplin g location s hav e bee n specified

. Se e attachmen t Afo ra list o fth e samplin g location s that wil l b e collecte d fo rthi s samplin g event
. Fo reac h samplin g location , a tota l o fthre e sampl e bottle s wil l b e collecte d (sample , sampl e duplicate , an d a 1 ng/m L 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

. Tw o sets o ftri p blank

s consistin g ofreagent-grad e wate ran d a 1 ng/m L tri p blan k

spike wil l b e prepare d at th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles

. Al l sampl e bottle s wil l includ e th e additio n o f^^Oz-PFBS , ^^OrPFHS , an d "Ca-PFO S (interna l standard ) at a nomina l concentratio n o f1 ng/mL

. Al l sampl e bottle s wil l als o includ e th e additio n o f ^C4-PF0 S (surrogat e spike ) at a nomina l concentratio n of0. 1 ng/mL

. On e additiona l bottl e wil l b e prepare d t o b e use d fo rth e preparatio n ofth e equipmen t rinseate blank

. A500m L bottl e oflaborator yreagen t wate rwil l b e sen t wit h th e sampl e bottle s t o b e use d t o generat e th e rinseate blan k sample

. Atota l o f5 6 sampl e bottle s wil l b e prepared

. 

### 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 "Detenninatio n o fPerfluorinate d Compound s I n Wate rb

yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

. Altemately , sample s ma yb e analyze d b

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

. Th e data qualit

yobjective s fo rthes e studie s ar e quantitative results fo rth e targe t analyte s wit h a n analytica l accurac yof100+30%

. Fiel d matri xspike s not yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly

. Where applicable , sample s wil l be analyze d against a n interna l standar d calibratio n curve . Eac h curve poin t wil l contai n isotopically-labele d perfluorocarboxyli cacid s an d perfluorosulfoni cacid s a t a nomina l concentratio n o f1 ng/mL

. Th e calibratio n curve wil l b e generate d b ytakin g th e rati o ofth e standar d pea k are a counts ove rth e intema l standar

d pea k are a counts t o fit th e dat a fo reac h analyte

. 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e results fo rth e sample , sampl e duplicate , an d th e fiel d matri xspike

. Tri p blan k

an d tri p blan k

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

. Metho d blank

s o freagen t wate rprepare d at th e tim e o fsampl e extractio n wil l be use d t o determin e th e metho d detectio n limit

. Fo rthos e samplin g location s where th e field matri xspike leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspik

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

Pag e 6 o f7 Pag e 3 3 o f5 7Attachmen t A

Attachmen t A GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 0 

## Bottl e Reques t Phas e 3 Investigatio n Off-site Phas e 3 New Monitorin g Well s

02181.129.108.000 1 

## DAT EREQUESTED : 1 8 October 201 0 October 201 0 DAT EREQUIRED : 2 5
Thi s reques t

addresse s th e bottl e requirement s fo r th e followin g wells : 602 R 602 S 602 L 603 R 603 S 603 L 604 R

604 S 604 L 605 R 605 L 607 S

607 L 609 R 609 L 611 R 611 L

Tota l Wells : 1 7 Sampl e Summar y No
. of Sample s 1 7 1 2 Sampl e Typ e

Groundwater Rinseate Sampl e Tri p Blank s Commen t Will needHPLC water Anticipate 1 pe r

cooler Note : Some o f

th e well s hav e limite dvolume s o th e smaller th e volume requirement s th e better
. 

## SHIPPIN GINFORMATIO N Pleas e ship to th e followin g address : Marti nSmith\Westo nFiel dOffic e 3 M Decatu r

Plan t 140 0 Stat e Dock s Roa d Decatur , A L3560 1 256-552-618 9

Pag e 7 of7 Pag e 3 4 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg^

% j?|y^^ ^

P^pgjij^roy^wate rfro m Decatur , A L Octobe r201 0 g101108a.rd b (PFBS) : "Quadratic " Regressio n (" 1 /x " weighting) : y= -0.083 6 x'' 2 + 3.5 8 x+ 0.0079 2 ( r= 0.9996 )

0 ) 

### < W
< u <
ra 28 - 27 - 26 - 25 - 24 - 23 - 22 - 2 1 - 20 - 19 - 18 - 17 - 16 - 15 - 14 - 13 - 12 - 1 1 - 10 - 9 - 8 - 7 - 6 - 5 - 4 - 3 - 2 - 1 - 0 - 

# y

* ^ 

### / / 

# y y y 

# y 

# . y y 

# X

y ^ . - ^ 

### ^ / " 

### ,-^' '

^.-- ^ ^



### ^/-" ^ • ^ -- •
-.--•^^'' ^

0. 0 0. 5 1. 0 1. 5 2. 0 2. 5 3. 0 3. 5 4. 0 4. 5 5. 0 5. 5 6. 0 Analyt e Cone

. /

I S Cone

. 6. 5 7. 0 7. 5 8. 0 8. 5 9. 0 9. 5 10. 0
Dat a worke d u

p b yST W Printin g Time : 1:35:4 5 PM Printin g Date : Monday , Januar y03 , 201 1 Pag e 1 o f 1 Pag e 3 5 o f 5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFJ^,%J?|y^^ ^ P|p § irj^rojjj^wate rfro m Decatur , A L Octobe r 201 0

Dat a worke d u

p b yST W Printin g Time : 1:36:0 3 PM Printin g Date : Monday , Januar y03 , 201 1 Pag e 1 o f 1 Pag e 3 6 of 5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFj^^S^J^^yq,^

. Pffi g jij^roy^wate rfro m Decatur , A L Octobe r201 0 g101108a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -0.031 3 x* 2 -H. 6 x- H 0.0088 5 ( r= 0.9996 )

1 4 1 3 1 3 1 2 12- : ti

ll : 1 0 1 0 9 9 8 ^ 8 : 7 7

- 6- i 6 : 5 5 4 4 3 3 ^ , / 2 2 I r I T 0 : . /

, /

o! 5 l.' o l! 5 2! o 2^ 5 3! o 0. 0 3. 5 4. 0 4. 5 5. 0 5. 5 6. 0 Analyt e Cone

. /

I S Cone

. 6. 5 7. 0 7. 5 8. 0 8. 5 9. 0 9. 5 10. 0
Dat a worke d up b

yST W Printin g Time : 1:36:2 1 PM Printin g Date : Monday , Januar y03 , 201 1 Pag e 1 o f 1 Pag e 3 7 o f 5 7Ginge rAG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg^%J?|yq,^,Pfpgirj^royj^waterfro m Decatur , A L Octobe r201 0

I Sampl e N»m«:-g101108a0i rSampt o ID:-08008-191- rFito ; "glOIIOSa.wifl " I P«a k Nama : *MePFOS{IS) ' Mass<aB} : -507.0/80. 0 ami T I Commant'1. 0 ng/m L FCst d i n Synth

. VAbtar * Anrtotation : Sampl e Type : Standar d Concentration : 0.96 0 ng/m L Calculaca d Cone : N/A2.8« 5 Acq

. Date : ll/S/ZOl O Acq

. Time : 1:0S:3 7 P H 2.6» 5 HDJitiad : Froc

. ;,lgorUhm : Min

. Paa KHeigh t Min

. Pea k

Vlidth : 5inootliin< 3 Vlidrh : R TVindav : EKpei:te d RT : Us e Relativ e RT : Inc

. Type : Retentio n Time ; Area : 3 Height ; Star t Tima : En d Timi : Ve- 1 IntelliQ L 0.0 0 0.0 0 0 30. 0 H . 5 N o Valle y lA. i '•171 9 c c 2.866+00 5 14. 3 14. e cp s poi n nil

.

mi n unt s cp s mi n m m lO A

1 2.4» 5

2.2e 5
2.0o 5
1.Be 5
1.6e 5
1.4« S

e.00 4
6.0« 4

13. 6 13. 8 14. 2 14. 4 14. 6 14. 8 15. 0 15. 2 1S. 4 •Sampl«Natna:-g101108aO30
- Sampi e ID : •PaakNamo:-M8PFOS(IS) ' Mass(0s ) Sampl e Indet : Sampl e Type : Concentration : Calculata d Cone : Acq

. L'aca : Acq

. Tine : HodiCisd : Proc

. Algorithm : Mill

. Paa k

Heigh t Mir,

. Pea k

Width : Sraoothin yWidth : R TWindow : Expecte d BT : Us e Relativ e RT : Int

. Type : Retentio n Time ; Haiglit ; Star t Time : En d Timu : 3 0 O C LCS-101105
-

•507.W80. I

0.95 3 nq/m L N/ A 11/8/201 0 1:2^XA AP M Ya ? Int^lliQua n - 0.0 0 se c 0 pci n 30. 0 sa c IJ. S mi n N o Valle v H . 5 mi n 8693 0 count s 3.12e+00 5 cp s 14. 4 mi n 14. 7 mi n lO A

3

1 ' Fila:'fl101108a.Mf r

amu '

3.0e 5
2.8e 5 2.6* 5
2.4« 5
2.2« 5 2.0* 5
1.8a 5
1.6« 5
1.4r t
1.2e 5 l.Oo S a.Oir f
6.0» 4

14. 4 14. 6 14. 8 15. 0 15. 2 15. 4 

# I Sampl a Name : -glOllOSaOSS " Sampt o ID : 'LCS-101105-10 ' Fila ; 'glO l lOSa.wif r Paa k Namo : 'MSPFOSftS rMass(es) : '507.080. 0 amu ' Comman t "Tpp b LC S EC P Anrwtstion: " Sampl e Irjctex : 3 ? Sampl e Typo : O C Concentration : 0.S5 5 nq/m L Calculacar t Cone : N/ A*-*5 ' Acq

. DaCH : 11/8/201 0 Acq

. Time ; 10:09:1 0 P M 3.Be 5 HC'Jifi

. Hin

. pea k

Width : .'Smoothin g Hidth : R TWindow : Expactai J RT : .telllgua n- 0 . 0 0 cp ! 0.0 0 se <

OTe+OO S cp s 3.6e 5 3.4« 5 3.2e 5 3.0e 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0* 5 1.8* 5 1.6*5

- 1.4*5

- 1.2* 5 1.0* 5 8.0* 4 6.0* 4 4.0* 4 2.0* 4 0. O 

# I Sampl a Nam* : 'glO l 108a063 * SampI * ID : 'GLP1CM)l-02
- Paa k Nam* : -M8PF0S(tS rMass{*s) : '507.0/80. 0 amu * Comman t 'DA L GW611L 0 101027 ' Arwotation : " Sampl e Index ; 6 3 Sampl e Type : Unknow n Concentration : 0.96 0 nq/m L Calculate d Cone : N/ A Acq

. Date : 11/9/201 0 Acq

. Time ; 5:25:1 4 A M Hodififad : Ve s Proc
- Algorithm : IntelliQua n - IQJ Win

. Pea k

Height : 0,0 0 cp s Min

. Pea k

Width : 0.0 0 ae c Snioothinc i Width : 0 point s R TKindov : 30, 0 se c E.-pacte d RT : It

. 5 mi n L's e e l a ! RT :

14. 2 14. 4 14. 6 14. 8 15. 0 15. 2 15. 4 Dat aworke du p b y ST W Printin g Time : 1:35:2 0 P M Printin g Date : Monday , Januar y 03 , Pag e 1 o f Pag e 3 8 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg,%Ji^y^M':PfP§i'J&?yfi^wate rfro m Decatur , A L Octobe r201 0

Sampl e Tvpe : Concentration : Calculate dCone : Acq
. Dace : Acq
. Time : Modified : Proc
. Algorithm ; Min
. Pea k

Height : Min
. Pea k

Hidth : Smoothin g Vlidth : R T Window : Expecte dRT : Us e Relativ e RT : Int
. Type : Retentio nTime : Area : 13 ! Height : 4 .' nknow n 0.36 0 N/ A 11/9/201 0 7:32:3 4 A

l Ye s IntelliC u 0.0 0 0.0 0 0 30. 0 IA. 5 N o Valle y 14. 4 163 6 C

O .97«+00 5 

# I Sampl * Nam* : 'gl01108a07o rSan^ * ID : -M*tho d Blant TFda : 'g101108a.M r Paa k Nam* : 'MSPFOStlS) ' Mass(8s) : -507.0/80. 0 amu ' Comman t '1 0 005-181 ' Annotation : ~

4.8* 5 4.6*5
- 4.4*5
- 4.2*5
- 4.0* 5 3.8*5
- 3.6* 5 3,4* 5 3.2a 5 3.0*5
- 2.8* 5 2.6* 5 2.4* 5 2.2*5
- 2.0* 5 1.8* 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0* 4 4.0* 4 2.0* 4
0. 0 13. 6 13. 8 14. 2 14. 4 14. 6 14. 8 15. 0 15. 2 15. 4 

# I Sampl a Nam« : "glO l lOSaOlS
- Sarrvil * ID : -08008-191-8 " Paa k Nama : -MPFBSOS rMass(M) : "303.0/84. 0 amu ' Comman t '1. 0 ngAn L F C st d i n Synlh

. WMer * Annotation : Sampii i Index : 1 9 Sampl e Type : Standar d Concentration : 0.91 5 nq/m L Calculate dCone : N/ A Acq
. Data : ll/'!/201 0 Acq
. Time : <:05:3 7 P M M-Jxiitiod : Vfl S Proc , Algcriclim ; IntelliQua n- IQ A Min
. Pnal c Height ; 0.0 0 ep s Min , Pea k

Width : 0,0 0 sa c Smijothinr j Width ; 0 pcint s R T Window : 30. 0 se c Expecte dRT : 12. 1 mi n Us e Relativ e RT : N o Int
. Type : Valle y Retentio nTime : 12. 1 mi n Area : 25144 7 count s Height : ' .T'^-OO Acp s Star t Time : 12. 0 mi n Enr t Time ; 12. 3 mi n

11. 2 11. 4 11. 6 11. 8 12. 0 12. 2 1Z 4 

# I San^ * Nam* : "glO t 108*030
- SampI * ID : 'LCS-IO l 105-4 - Fil* : 'glO l lOSa.Mf T Paa k NMtm : -MPFBS(tS rMassfss) : "303.0/84. 0 amu " Comman t '2pp b LCS ' Annotation : " Sampl e Index : 3 0 Sampl e Type : y C Concentration : 0. 9 6 3 nq/m L Calculate dCone : N/ A Acq
. Date : 11/8/201 0 Acq
. Time : 1:35:4 4 P M MoJifisd : Min
. Pea k Heig ! Hin
. Pea k Widt l Smoothin g Hidt l R T Window : Expecte d RT : Intel:iQ i : 0.0 0 0.0 0

Height : Star t Ti r En dTime ; 24796 1 C i 9
. 12 e + 00 4 8.0* 4
7.5* 4 7,0* 4
6.5*4

- 6.0* 4
5.5* 4
5.0* 4
4.5* 4 f- • I .0* 4
3.5* 4
3.0* 4
2.5* 4 2,0* 4
1.5* 4
1.0* 4
5000. 0 

# I SampI * Nam* : "glO l 108a039 - SampI * ID : "LCS-lO l 105-10 - Fil* : 'glOllOSa.vw T P*a k Nam* : -MPFBS(IS)
- Mass(*a) : "303.0/84. 0 amu ' Comm*n t "2pp b LC S ECF " Annotation : ~ Sampl e Index : 3 9 Sampl e Type : Q C Concentration : 0.97 0 ng/m L Calculate dCone : N/ A, Acq
. Date ; n/?/201 0 7.0*4

- Acq
. Time ; 10:09:1 0 P H 6.5* 4

6.0 M
5.5* 4
5.0*4

- 4.5* 4 I4.0* 4 Modified : Proc

. Algorith m Min

. Pea k

Heig h Hin

. Pea k

Widt h 5»oothin q Widt h R TKindo-.* : E-pecta d BT : Us e Relativ e R

T Int

. Type : R-atentio n Time ; Ye a IntelliQ

. : 0.0 0 0.0 0 0 30. 0 12. 1 N o 7a 1 le i 12. 1 Area : 2507^ 3 e c Height : 3tjr t Time : 7.30e-00 4 12. 0 a n -

cp s se c poin t

mi n unr s cp s mi n

11. 8 1Z 0 12. 2 12. 4 12. 6 12. 8 13. 0 Dat aworke du p b y ST W Printin g Time : 1:35:2 1 P M Printin g Date : Monday , Januar y 03 , 201 1 Pag e 2 o f Pag e 3 9 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg^S^J=i|y^^,Pfp§i.jgroy^waterfro m Decatur

. A L Octobe r201 0 

# I SampI * Name : 'g101108a063 " Sampl e ID : "GLP1(M)l-02- 1 P*a k Namo : "MPFBS(IS) " Ma«»(ea) : "303.0/84. 0 ami / Conim8nt"DALGW611L010102 rAnnotation:
- Sampl e Tvpe : Calculate d Cone : Acq

. Dace : Acq

. Time : McdiEied : Proc

. Algorithm : Miri

. Pea k

Heigh t Min

. Pea KHiJth : Srocothin g Hidth : B TWindow : Expecte d RT : Us e Relativ e RT : Int

. Type : Vnknow n 0.97 5 N/A 11/9/201 0 5:25:1 4 AM N o IntellUju a 0.0 0 0.0 0 0 • p 30. 0 12. 1 N o Valle y

En dTime :



# I SampI * Name : -gl01108a0l9 ' Sampl e ID:-08008-191-6
- Fil« ; "glOHOSa.wif r Pea k Nam* : -MPFHS(IS)
- Man{*a) : '403.0/84. 0 ami T Comm*n t -1. 0 ng/m L F C st d i n Synth

. Water ' Annotation : Sampl e Index : 1 9 Sampl e Type : Standar d Concenrrari'jn : 0.9-J 5 ng/m L Calculate d Cone : N/A Acq

. Date : lI/a/201 0 Acq

. Time : J:05:3 7 P H 

# I SampI * Nam* : •g101108a070 " SampI * ID : "Metho d Blank
- File : -glO l 108a.wif r Paa k Nam* : -MPFBS(IS)
- Ma$s(*s) : "303.0/84. 0 amu " Comm«n t "1 0 005-181 " Annotation:" " Sampl e Inde.'t : 7 0 > Type Unknow n Sampl * : Concentration : CaleulatB dC Acq , Date : Acq
. Time : H.3diried : Ptoc
. Alrjcr i Min
. Peak

H e hm : qh l Min
. Pea k

Widt h .•Jmoothin qWidt h R T Window : Expecte dRT : Ua e Relativ e Int
. Type : Retentio n T i Area ; H•^ight : Star t Tin,e ! En dTime : R

T U nknow n 0.97 5 N/ A 11/9/201 0 7:32:3 4 A

N Ye s InteliiQu a ! 0.0 0 0.0 0 0 p 30. 0 12. 1 ri o Valle y 12. 1 2363C 2 CO

M B.27atO0 4 12. 0 12. 4

11. 6 12. 0 12 2 12. 4 12. 6 1Z 8 13. 0

Modified : Min
. Peak

Height : Min
. Peak

VFldrh ; R TWindow ; E.tpects d RT : Us e Relativ e RT : Int
. T\pe : N o SampI * Nam* : "g10l108a030 ' SampI * ID : "LCS-101105-4
- FUe : "g101108a.wi r Pea k Nam* : 'MPFHSOS fMas»(es) : "403.0/84. 0 amu Comm*n t '2pp b LCS ' Annotation: "

2.5* 5 2.4* 5 2.3* 5 2.2* 5 2.1* 5 2.0* 5

Height : Stsr t Ti r EndTime : 59905 0 C ( I.B9e*00 5 1 3
. . 5 Calculate dCon e Acq
. Oaf. : Acq
. Time : Modified : proc - Algerich m Min
. Peak

Heig h Min

- Peak

Widt h Smoothin g Widt h R T Windo-j : E:^peeta dRT : va aRelativ e R

T Int
. Type : Retentio n Time : N/f t 11/9/201 0 7:25:4 4 P N o IntelliQ u : 0.0 0 0.0 0 0 30. 0 13. 6 N o Valle y 13. 6 Area : 69264 6 c o Haiqhr : oCArt Time : En dTime : 2.59e-'00 5 13. 4 13. 8 1.8* 5 1.7*5
-

1.4* 5 1.3* 5 1.2*5
- 1.1* 5 1.0* 5 9.0* 4 6,0* 4 7.0* 4 6.0* 4 5.0* 4 4,0* 4 3.0* 4 2.0e 4 1.0* 4 0. 0 13. 2 13. 4 13. 6 13. 6 14. 0 14. 2 14. 4 Dat aworke du p b y ST W Printin g Time : 1:35:2 1 P M Printin g Date : Monday , Januar y 03 , 201 1 Pag e 3 o f Pag e 4 0 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg^%Ji|y^^,P^pgitjgrop^waterfro m Decatur , A L Octobe r201 0

1 Sampl e Nam*:"gl01108a039
- Sampt o ID:'LCS-10 1 lOS-lff " File : "gl01108a.v« r I Pea k Nam*:'MPFHSOS rMa««(*a):-4O3.Q«4, 0 amu " I Comm*nt-2pp b LC S ECF
- Ajmotation:
- Sampl e Indax : 3 9 Sampl e Type : Q C ,35 g Concentration : 0.94 0 ng/m L 2.2* 5 Calculate d Cone : N/ A Acq

. Data : 11/^/201 0 2.1* 5 Acq

. Time : 10:09:1 0 P H 2,0* 5 MOslifled : Ve s Proc

. Algorithm : IncelliOua n - lO A1.9* 5 Hin

. Pea k

Height : 0.0 0 cp s Min

. Pea k

Vfidth : 0.0 0 se c1.8* 5 Smoothin g Width : 0 point s R TWindow : 30. 0 set - 1.7* 5 Expecte d RT ; 13. S mi n Us e Relativ e RT : N o 1-6* 5 Int

. Type : Valle y1-5* 5 Retentio n Time : 13. S n.i n Area : 657BS 3 count s 1.4« 5 Height : 2.21e-f00 5 cp s Star t Time : 13. 5 mi n 1-3« 5 En d Time : 13. 8 rain ^ ^^^ ^ § •1.1* 5 1 1,0* 5 9,0* 4 8.0 - 7.0* 4 6,0* 4 5,0 M 4,0* 4 3.0* 4 2,0* 4 1,0* 4 

# J
12. 6 12, 6 13. 0 13. 2 13. 4 ^ 13. 6 13. 8 14. 0 14J Z 14. 4 1 Time , mi n I SampI * Name : "g101108a070
- SampI * ID:-M.tho d Blank
- Fil*:"a101108a.Mf r I P*a k Name:-UPFHS(1S} " IUUs$(es):-403,0/84. 0 amu "
•Comm*nt-1 0 005-181 - Annotafion: " Sampl e Index : 7 0 [ Sampl e Type : Unknow n lis: i Concentration : 0.94 5 ng/m L Calculate d Cone : N/ A Acq

. Date : 11/9/201 0 3^« 5 Acq

. Tliae : 7:32:3 4 AM Modified ; N o ^,0* 5 Proc

. Algorithm ; IntelliQua n - IQ A Min

. pea k

Height : 0.0 0 cp s 2 8* 5 Hin

. Pea k

width : 0.0 0 se e Smoochin g Width : 0 point s R TWindow : 30. 0 se c2.6* 5 Expecte d RT : 13. 5 mi n Us e Relativ e RT : N o j 4e 5 Ir,t

. Type : Valle y Retentio n Time : 13, 5 mi n 2.2* 5 Area : 682B0 5 count s Height : 3.37e»00 5 cp s _„ , Star t Time : 13. 4 mi n 2.0* 5 En d Time : 13. 8 mi n . 1 1.8* 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0* 4 4.0* 4 2.0* 4
l i 6 li e 13. 0 13. 2 13. 4 1—_

_ n 

### 1



# I

13. 6 13. 8 14. 0 14. 2 14. 4 1 1 sampt o Nam*:-gl01l08a063
- Sampl e ID:"GLPltM)l-02-10^16 " File : "glOllOBa.wi r I Pea k Name : -MPrHS<ls rMa«c<es) : "403.0^. 0 amu " Sampi e Inde.t : 5 3 Sarnpi e Type : Unknow n Concentration s 0.94 5 ng/m L Calculate d Cone : H/ A25e 5 Acq

. Date : 11/9/201 0 Acq

. Time t 5:25:1 4 A M 2.4* 5 Modified : Ye.
- 2-3» 5 Proc

. Algerithm : Inte l llO'ia n - lU A, JB S Min

. P«a k

Height ; 0.0 0 cp s Hin

. Pea k

Width : 0.0 0 se c2.1* 5 Smoothin g Width : 0 pc.lnt s R TWindow : 30. 0 se c2.0* 5 Expecte d RT : 13. 6 mi n ,- 5 Us e Relativ e RT : tl o 1.6* 5 Int

. Type : Valle y Retentio n Tin.e : 13. 5 mi n 1.'" 5 Area : 66291 2 count s H-iight : 2.59et00 5 cp s ^'^ ^ Star t Time ; 13. 4 mi n i.5» 5 En d Time : 13. 9 mi n , & 1.4. 5 t 1-3* 5Interit 1.0* 5 9.0e 4 8.0* 4 7.0* 4 6-0* 4 5.0* 4 4.0* 4 3.0* 4 2.0* 4 1.0* 4 1Z 6 12. 8 13. 0 13. : 1 SamptoNam*:-g101108a019
- Sampt o ID : "08008-191-8
- Fito : "gl01108a.M r I Pea k Nam*:-PFBS " Maas(*s):-299.W99. 0 amu,299.0/80. 0 amu "
•Commen t "I.Oi^j/mLF C st d i n Synth

. Wate rAnnotation : " " Sampl e Index : l< i Sampl e Type ; Standar d Concentration : 0.96 9 ng/m L 2.5* 5 Calculate d Cone ; 0.94 4 t.q/m i Acq

. Date : 11/5/201 0 ^,4* 5 Acq

. Time : 4:05:3 7 P M 2,3* 5 Modified ; Ye s 22*5
- R TKindo--J ; 30. 0 se c Expecte d RT : 12. 1 mi n 2.1* 5 Us e Relativ e RT : N o „ , 2.0* 5 Int

. Type : Manua l ASm S Retentio n Time : 12, 1 mi n ^'^ ^ Area : 35420 6 count s 1.8* 5 Height : 2.51e-'00 5 cp s Star t Time : 11. 9 mi n 1-7* 5 En d Time : 12. 4 mi n ^ ^ ^ 1.5* 5
» 1.4* 5 3 - ^ 1.3* 5 1 1.2* 5

- 1.1* 5 1.0* 5 9.0* 4 8-0* 4 7.0* 4 6.0* 4 5.0* 4 4,0* 4 3.0* 4 i0* 4 1.0* 4 11. 2 11. 4 11. 6 13.5 4



# I • m 13- 4 13. 6 13. 8 14. C

121 0



# • 

# 1 A s 1. 8 1Z 0 12. 2 12. 4

Time , mi n 14. 2 14. 4

1Z 6 1Z 8 13- 0 Dat aworke du p b y ST W Printin g Time : 1:35:2 2 P M Printin g Date ; Monday , Januar y 03 , 201 1 Pag e 4 o f Pag e 4 1 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFj^^^J^^y^^ ^ PfPSl-J^ro^i^wate rfro m Decatur , A L Octobe r 201 0

Sampt o Nama:-g101108a030 ' Sampt o 10 : "LCS'101105-4 " Fito:'gl01108a.M r Pea k Nam* : "PFBS " Masses) : "299.0/99. 0 amu,299.0/80, 0 amu * Commen t "2pp b LCS " Annotation: " .<!ampl e Index : 3 0 e Type : Q C ng/m

L

Manua l te : 12. : mj2T 7

12. 0 12. 2 12. 4 12. 6 12. 8 13. 0 

# I San»pto Nam* : "g101108a039 " Sampt o ID ; "LCS-IO l 105-10 " Fito : "glO l lOea.wi T Paa k Name : "PFBS " Mass<*s) ; •299.0ra9. 0 amu,299.0/80. 0 amu " Commen t "2pp b LC S EC P Annotation : " Sampl e Type : Q C Concentrati o Calculate dC Acq
. Date : Acq
. Time : Modified : R T h-indow : Expecte dRT ; Us e Relativ e Int
. Type : Retentio nT i Area : Height ; Star t Time ; EndTime : : 0.0 0

nc : 0.024 1 11/9/2D1 0 10:09:1 0 Ve s 30. 0 12. 1 RT : N

o Manual ne : 12- 1 2427 6 c c 6.55e*00 3 12. 0 12. 2 ng / ng / P H
mi n

cp s mi n mL mL

1 6500

6000 5500 5000 4500 4000 3500 3000 2500 2000 1500 

# I Sampl e Nam* : •g10110ea063 " Sampt o ID:"GLPlCK>1-02-ltM)16 " FiJ« : 'g101108a.w r Paa k Nam* : "PFBS ' Mass(as} : "299.0/99. 0 amu,299-0/80. 0 amu " Comment-DALGW611L0101027 " Annotaton: " lampl e Ir,
. 6 3 Sampl e Type ; Unknow n Concentration : N/ A Calculate dCone : 0.31 5 ng/m L Acq , Date : 11/9/301 0 Acq
. Time : 5:25:1 4 A M Mcdifiad : Proc
. Algori t Nais e Percen t Ba?e , Sub
. W

i Peak-Split
. F Min
. Paa

k Hel Min
. Pea k Wl d Pmoorhin g Wi

d R T Window : Expecte dRT :

Heiijht : .•^tart Tim
. En dTim-? : N o 8.5* 4 8.0* 4 7.5* 4 7.0* 4 6.5*4

- 6.0* 4 5.5* 4 5.0* 4 4.5*4

- 4-0* 4 3.5* 4 3.0* 4 2.5*4

- Z0ft 4 1.5* 4 1.0* 4 5000. 0
0. 0 

# I Sampt o Nam* : "glO l 108a070 ' Sampt o ID : "Matho d Btonk " Fito : "g10l108a.wi r Paa k Nam* : "PFBS " Ma«8(*s) : "299.0/99. 0 CortOTwn t "1 0 005-181 " Annotation : " Sampl e Index : 7 0 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.0020 2 Acq
. Date : 11/9/201 0

7:32:3 4 A

M Ac q Time : Modified : R T Window : Ex p Us e In t Re t Hel c St a End cte dR Relat l Type : ntio n ht : t Tim e Time :

12. 0 12. 2 1Z 4 12. 6 12. 8 13. 0 Tim* , mi n Dat a worke d u

p byST W Printin g Time : 1:35:2 2 P M Printin g Date : Monday , Januar y03 , Pag e 5 o f 201 1 Pag e 4 2 o f5 7Ginge rAG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFg^%J?|y^^ ^ P ffig jijgroy^wate rfro m Decatur

. A L Octobe r201 0 

# I SampI * Name : "glOIIOSaOl? ' Sampt o ID : "OeOOS-igi-a " Pea k Name : "PFHS " Mass{es} : "399.0/99. 0 amu,399.0/80. 0 Comman t "1. 0 nglm l F C st d i n Synth

. Water " Annotation : " " Sampl e Tvpe : Concentration : Calculate d Con e Ac!! . Date ; Acq . Time : MoJifled : Proc . Algorith m Min
. Pea k Heig h Min
. Pea k Widt h Smoochin g Hidt h R T Window : Expecte d RT : Us e Relativ e R T int
. Type : Retentio n Time ; Standar d 1.0 0 1.0 3 ll/e/201 0 J:05;3 7 p N o Intellit' u : 0.0 0 0.0 0 0 30. 0 13. 3 N o Valle y 13. S Area ; 144)53 5 c o Height : Star t Tine : En d Time ; 5.03e-'00 5 13. 4 13. e 5,0* 5 4.8* 5 4,6* 5 4,4*5
- 4.2* 5 4.0* 5 3.8* 5 3.6* 5 3.4* 5 3.2* 5 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0e 5 1.8* 5 1.6e S 1.4* 5 1.2e 5 1.0e 5 8.0* 4 6.0* 4 4.0» 4 2.0* 4 0. 0 1Z 6 iz a _J4^0 3 14. 0 

# I Sampt o Nam* ; "glO l 108*030 ^ Sampt o ID : "LCS-10110&4 " Fio : "glOllOSa.M r Pea k Nam* : "PFHS " Mass<*a} : "399,0/99. 0 amu,399.0/80. 0 amu " Commen t "2pp b LCS " Annotation : " Sarapl e Index : 3 0 sampl e Type : Q C Concentration ; 1.9 9 nq/m L Calculate d Cone : 1.5 6 ng/m L Ac:^

. Datu : 11/^/201 0 Acq

. Time : 7:25:4 4 P M

Proc . Algerithm : Min
. P.*a

k H-iigh t Min
. Pea k Width : Sraccthln g Width : R T Window : Expecte d RT : Us e Relativ e RT : Int . Type : Retentio n Time : Intelll O 0.0 0 0.0 0 0 •0. 0 n. e N o Valle y 13. C Area : 313760 1 =



# I SampI * Nam* : "g101108a039 ' Sampt o ID : "LCS-IOI105-10 * FHe : *gl0110ea.wi r Pea k Name : "PFHS " Mass(es) : "399.0/99. 0 amu,399.0/80. 0 amu Commen t "2pp b LC S ECF " Annotation : " Sampl e Index : 3 5 Sampl e Type : u C Concentration : 0. 0 0 ng/m L Calculate d Cone : 0-13 5 ng/m L Acq
. Modified ; R Twindow : EKpeete d RT : Us e Relativ e 11/8/201 0 10:09:1 0 p r Modified : Ye a B TKindov : 30. 0 Expecte d RT : 13

. 6 Us e Relativ e RT : N o Int

. Type : Manua l Retentio n Time : 13. 5 Area : 2T5a4 4 z i Height ; S.36e'0'} 4 Star t Time : 13. 3 En d Time : 13. 7 

# I Sampt o Name:-gl01108a063
- Sampt o ID : "GLP10-01-02-l(H}i rFito:-g10ll08a.wi r Pea k Name : "PFHS " Mass{ea) : -399.0/99. 0 amu,399.0/80. 0 anu T Commen t "OALGW611L0101027 * • -

8.0* 4
7.5* 4
7.0e 4
6.5* 4
6.0* 4
5.5* 4
5.0* 4
8
. 4.5* 4 2 ^ I 4.0* 4 3.5* 4 3.0* 4 2.5* 4 2.0* 4 1.5* 4
1.0* 4
5000. 0 0. 0 Dat a worke d u p byST W Printin g Time : 1:35:2 4 PM Printin g Date : Monday , Januar y03 , 201 1 Pag e 6 o f Pag e 4 3 o f5 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFl?e%ii?y^M^:Pfft§i'J&?y<5^w3*^' ' ^^ ^ ^^^^ur

. A L Octobe r201 0

•SampI * Nam*:'g101108a07O
- Sampt o ID : "Matho d Blank
- Fito : -g101108a.wi r I Paa k Nam* : "PFHS " Mas«(es} : "399.0/99. 0 Bmu,399.0/80. 0 amu " m Comman t •10005-181 - Annotation:" " Sampl e Type : Unknow n Concentration : N/ A Calculate d Cone : 0.00059 5 Acq

. Data : 11/9/201 0 Acq
- Time : 7:32:3 4 AM 

# I Sampl a Name : 'glO l 108aOig
- Sampt o ID : -08008-191-6 - Fito : 'g101106a.\Mf r Pea k Narrw : "PFOS " MaM<es} : "499.0/99. 0 amu,499,0/80, 0 amu.499.0/130. 0 amu " Commen t '1. 0 ng/m L F C st d I n Synth

. V^tater ' Annotation : " " Sampl e Index : 1 9 Sampl e Type : Standar d Concentration : 0.9 9 3 ng/m L Calculate dCone : 1.0 3 ng/m L Acq
. Date : 11/8/201 0 .cq . Ti : 1:05:3 7 P H 5.0* 5

4.8* 5 4.6* 5 4.4* 5 4.2* 5 4.0* 5 3.6* 5 3.6*5

- 3-4* 5 3.2* 5 3.0* 5 28* 5 I Z6* 5 I 2.4*5 22* 5 Z0e 5 1-8* 5 1.6* 5 1.4* 5 1,2* 5 1.0* 5 8.0* 4 6,0* 4 4.0* 4 20* 4 0. 0 13. 6 13. 6 14. 0 14. 2 14. 4 14. 6 14. 6 I Sampt o Nama : -g101108a030 ' Sampt o ID : "LCS-101105-4 ' Fito : "glOIIOea.wi T I Paa k Nama:
- PFOS " Uass(*a) : "499.0/99. 0 1 Commen t "2pp b LCS
- Annotation : " " Sampl e Inde x Sampl e Tvpe : Concentratl o Calculate d C Acq

. Date : Acq

. Time ;
h i Window : Expecte d RT : Us 6 Relativ e int

. Type : Ratantio n T i Height. : Star t Time ; En d Tim^• : 3 0 y c

: 1.9 B ng/m L 3nc : 1.9 7 ng/m L 11/9/201 0 7:25:4 4 P H
30. 0 se c 14. 5 mi n RT : N o Manua l ae : 14. 5 mi n 313956 8 count s l-lletOO e ep s 14. 4 mi n 14. S mi n arr u

1 J.499.CV80. 0 a r

1.05* 6 1.00* 6 9.50* 5 9.00* 5 6.50* 5 8.00e S 7.50e 5 7-00e 5 6.50e 5 6.00e 5 5.S0e 5 5.00e 5 4.50* 5 4.00* 5 3.50* 5 3.00* 5 250* 5 Z00* 5 1.50* 5 1.00* 5 5.00* 4 1 nu,499.0/130. 0 amu " 

# I Sampt o Nam* : "glO l lD8a039
- Sampt o tD : "LCS-10 1 lOS-lQ
- Fito : "glO l 106a.Mf r Paa k Name : "PFOS " Mass(*s) : "499.0/99. 0 amu.499.0/80. 0 amu.499.0/130. 0 amu " Convnan t "2pp b LC S ECF " Annobtion : "

2.5 2 n c 11/9/201 0 10!09;1 0 P

H 9.5* 5

9.0*5

- 8.5* 5 aOe 5 7.5* 5 7-0* 5 6.5* 5 6.0* 5

^ 5,0* 5 I 4.5*5
-

13- 6 14. 0 14. 2 14. 4 14. 6 14. 8 13. 6 13. 8 14. 0 14. 2 14. 4 14. 6 Dat a worke d up b

yST W Printin g Time : 1:35:2 4 PM Printin g Date : Monday , Januar y03 , Pag e 7 o f 201 1 Pag e 4 4 o f5 7*•* * Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFge%Ji^y^M^:P^ft8i'J&?!J<5^wate rfro m Decatur

. A L Octobe r201 0 

# 1 Sampl e Nam* : "gl0110aa063 " Sampt o ID : "GLP1CM)1-02-10-016 " Fito:-gl011O8a. w Paa k Nama : "PFOS " Ma«s(es) : "499.0/99. 0 amu.499.ora0. 0 amu,499.0/130. 0 amu " Comment " DALGW611L010102 rAnnotation:
- Sampl e Index : 6 3 j Sampt o Name : "glQ l 108a070 - Sampt o ID : -Metho d Stanl TFito : " g 101108a.wif r
Sampl e Tvpe : Concentration ; Calculate d Cone ; Acq

. Date : Acq

. Time : Modified ; R TWindow : Expecte d RT : Unknow n N/ A 0.95 7 11/9/201 0 5:25:1 4 At Ye s 30. 0 14. 5

Height : Stac t Tlm i En dTlme i I Peak Name : "PFOS " Mass(et) : "499^0/99. 0 I Comment

"1 0 005-181 * Annotation : Sampl e Index : 7 0 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.0051 7 n i Acq
. Date : 11/9/201 0 Acq

- Time : 7;i2:3 4 A H

Height : Star t 1 En dTi r

Dat a worke d u

p byST W Printin g Time : 1:35:2 4 P M Printin g Date : Monday / Januar y03 , Pag e 201 1 Pag e 4 5 o f5 7DocuKgwmdi-efin-a^ib&iWRgiL^rtifocurrent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0



# 3 M Environmenta l Laiioratoi y

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

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q^/f^/o ^

Approve d By : 

# ^/>j/ o - y Willia m K

. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 of1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 6 o f5 7DocuBw?iirt-(ni-02fifesririj88f)^3rtifocurrent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0



### 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) , Perfiuorononanoi cAci d (PFNA) , Perfluorodecanoi cAci d (PFDA) , Perfluoroundecanoi cAci d (PFUnA) , Perfluorododecanoi cAci d (PFDoA) , Perfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) b yHig h Performance Liqui d Chromatograph ycouple d t o a tande m Mass Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples

. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n alternat e metho d suc h as ETS-8-15 4 "Determinatio n o f Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"

. Thi s metho d i s considere d a performance-base d method

. Data i s considere d acceptabl e as lon g as th e define d Q C elements are satisfied

. Sampl e collectio n i s no

t covere d unde rthi s analytica l procedure

. 2 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS

. Sample s containin g heav y particulat e ma

yno t b e suitabl e fo ranalysi s b ythi s method

. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered

. Thi s i s a performance-base d method

. Metho d accurac yi s determine d fo reac h sampl e 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 detemnined usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix

. Sampl e results fo rspike s outsid e o f70 % t o 130% , ma

yb e flagge d as suc h (wit h expande d accurac

ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples

. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t leas t 50 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o detennin e th e statemen t of accurac yfo ranalytica l results

. 

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

yspikin g a know n volum e ofth e Workin g Standar d (WS ) into a predetermine d amoun t ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method

. Calibratio n standard s are use d t o calibrat e th e instmmen t respons e wit h respec t t o analyt e concentration

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

yduplicat e sampl e i s a separat e aliquot ofa sampl e take n i n th e analytica l laborator ythat i s analyze d separatel ywit h identica l procedures

. Analysi s ofLDS s compare d t o that ofth e firs t aliquot give a measur e ofth e precisio n associate d wit h laborator yprocedures , bu t no

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

. 3. 3 Fiel d Blan k

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d as a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures

. Th e purpos e ofth e F B i s t o determin e i ftest substance s o r othe rinterference s ar

e presen t i n th e fiel d environment

. Thi s sampl e i s als o referre d t o as a Tri p Blank

.

ETS-8-044. 0 Pag e 2 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 4 7 o f5 7DocusGupii'd-omS'zrite-iftisefirtifocurrent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0


### 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 fiel d an d laborator y procedures

. Analysi s o

fth e FD S compare d t o that ofth e firs t sampl e give s a measur e o fth e precisio n associate d wit h sampl e collection , preservatio n an d storage , as wel l as wit h laborator yprocedures

. 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s ofth e targe t analyte s are adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n ofaqueou s samples

. Aknown , specifi cvolum e of sampl e mus

t 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 o fanalyt e concentration s i s unknown , multipl e spike s at 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 o fth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles

. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p detennin e i fth e metho d i s i n contro l an d whethe ra los s o fanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues

. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s ar e no t know n o rma

yvary . At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d place as eac h FMS

. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s o fth e targe t analyte s ar

e adde d i n th e laborator

ya t th e tim e ofsampl e extraction

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

ysampl e t o detennin e whethe rth e metho d i s i n control

. LCS s shoul d b e prepare d eac h da ysample s are extracted

. 3. 8 Laborator yMatri xSpik e (LMS ) Alaborator

ymatri xspike i s a n aliquot ofa sampl e t o whic h know n quantitie s oftarge t analyte s are adde d i n th e laboratory

. Th e LM S i s analyze d exactl ylik e a laborator

ysampl e t o determin e whethe rth e sampl e matri xcontribute s 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 detennine d i n a separat e aliquot an d th e measure d value s i n th e LM S con-ected fo rthes e concentrations

. LMS s are optiona l fo ranalysi s ofaqueou s samples

. 3. 9 Laborator ySampl e Aportio n o raliquot o fa sampl e receive d fro m th e fiel d fo rtesting

. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e lowes t concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits ofprecisio n an d accurac ydurin g routin e operatin g conditions

. To simplif ydat a reporting , th e LLO Q i s generall yselecte d as 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 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 4 8 o f5 7Docus(Siwrt-(ma2/iteffirM8«f8i)rtifocurrent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0

3.1 1 Metho d 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 ar e use d wit h othe rlaborator ysamples

. Th e metho d blan k i s use d t o detennin 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 o fa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound

. 

### 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s not nonnall y foun d i n th e sample(s)

. Asurrogat e compoun d i s typicall ya targe t analyt e wit h a t least on e ato m containin g a n isotopically-labele d substitution

. I fused , surrogate(s ) ar e adde d t o al l sample s an d qualit y contro l samples

. Sun-ogate(s) are adde d t o quantitativel yevaluat e th e entire analytica l procedur e includin g sampl e collection , preparation , an d analysis

. Inclusio n ofa sun-ogat e analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired

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

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

. Th e analyst shoul d wea rgloves , a la b coat , an d safet

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

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a cun-ent awarenes s ofloca l regulation s regardin g th e handlin g o fth e chemical s use d i n thi s method

. Areference fil e o fmateria 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 ga s an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l 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

ymnnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 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 4 9 o f5 7Attachmen t C DocuBtiie'iirt-OT>s2ritesri«8eiii)rtifocurrent , fo r1 4 day s fro m 01/03/20 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination

. Thes e ma yinclude , bu t are no

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

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

. 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h performance liqui d chromatograp h capabl e ofpumpin g u p t o two solvents an d equippe d wit h a variabl e volum e injecto rcapabl e ofinjectin g 5-10 0 [J Lconnecte d t o a tande m Mass Spectromete r (LC/MS/MS)

. I Analytica l balance capabl e o freadin g t o 0.000 1 g Adevice t o collec

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes

. Gas tigh t syringes , 25pL , 50[JL , lOOpL , 250|JL , 500pL , 1000|JL

. 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 cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 ij m Analytica l Column : Betasi l C I 8,4. 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 :

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

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

3 3 9 5 9 5 3 3 FlowRat e

(mL/min ) 1. 0 1. 0 1. 0 1. 0 1. 0 1. 0 Injectio n Volume : 100 p L Quantitation : Pea k

Are a - quadrati ccurve fit , 1/ xweighted

. Ru n Time : ~ 1 7 minutes

. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s are met
.
ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 0 o f5 7Attachmen t C Docui(iniE'irt-OT>e2iite8'i«gs#,rtffocurrent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0

6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e PFB A PFPe A PFH A PFHpA PFOA PFN A PFD A PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 31 3 ^26 9 an d 31 3 ^11 9 36 3 - ^ 319 , 36 3 - > 16 9 an d 36 3 - > 11 9 41 3 ^ 369 , 41 3 - > 21 9 an d 41 3 - > 16 9 46 3 - ^ 419 , 46 3 ^

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

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

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

16 9 an d 61 3 ^

31 9 29 9 - ^ 8 0 an d 29 9 - ^

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

9 9 an d 49 9 - > 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , as 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 yhave th e adde d benefi t o f increase d sensitivity

. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a are met t o assur e adequat e specificity

. Th e previou s infonnatio n i s intende d as a guide , alternat e instruments an d equipmen t ma yb e used

. 7 Reagent s an d Standard s 7. 1 Chemical s Water
- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A.C.S

. Reagen t Grad e 7. 2 Standard s Perfluorobutanoi cAci d (PFBA-C 4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPe A- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M Perfiuorononanoi cAci d (PFNA
- C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C1 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 1 o f5 7Docui(iiia?iiKl-0m82/itea-i«K^rtif6current , fo r1 4 day s fro m 01703/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0

Th e previou s informatio n i s intende d as 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 o freagen t water
. Note : Alternative volume s ma yb e prepare d as lon g as th e ratio s o fth e solven t t o solut e ratio s are maintained

. 7. 4 Stoc k

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

d preparatio n procedur

e serve s as a n example

. Weighe d amounts an d fina l volume s ma yb e change d t o sui t th e need s ofa particula rstudy

. Fo rexample , p L volume s ma yb e spike d into volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels

. 10 0 Mg/m L targe t analyt e SSSs—Weig h ou t 1 0 m g o fanalytica l standar

d (correcte d fo rpercen t sal t an d purity ^ an d dilut e t o lOOm L wit h methano l o rothe rsuitabl e solvent , i n a lOOm L volumetri cflask

. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container

. Prepar e a separat e solutio n fo reac h analyte

. Expiratio n date s an d storag e condition s o

fstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure

. A n exampl e ofpurit yan d sal t correctio n i s give n belo wfo rPFOS

. ^

. , ^ molecula rweigh t o fanio n sal t correctio n facto r= = moclecula rweigh t ofsal t

49 9 PFO S (K"
- )sal t correctio n facto r= -i ^ = 0.927 5 53 8 1 0 m g CaFiySOa'l C wit h purit y90 % = 8.35m g C8F17SO3 ' (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 (jg/m L (500 0 ng/mL ) mixe d workin g standard—^Ad d 0.5m L eac h ofth e lOOpg/m L SSS s t o a lOm L volumetri c flas k an d brin g u p t o volum e wit h solvent

. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L o fth e 5 pg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflas k

an d brin g u p t o volum e wit h solvent

. 12 5 ng/m L mixe d standard^Ad d 625p L ofth e 5 pg/mL-mixe d worthin g standar d solutio n t o a 25m L volumetri c flas k an d brin g u p t o volum e wit h solvent

. Storag e Conditions—Stor e al l SSS s an d wori<in g standard s i n accordance wit h laborator ystandar d operatin g procedure o ri n a refrigerato ra t 4°±2° C fo ra maximu m perio d of6 month s fro m th e date o fpreparation

.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 2 o f5 7Attachmen t C Docu;Giii!?iiid(-0ii-e2nk»i«8aiil)rtifocurrent , fo r1 4 day s fro m 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 1/03/201 1

7. 5 Calibratio n Standard s Usin g th e worthin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline

. Note : Volume s ofwate ran d wori<in g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline

. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d as needed

.
Concentratio n o fWS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS.fi L

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

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

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

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

. Sample s containin g heav yparticulat e ma

yno t b e suitabl e fo r analysi s b

ythi s method

. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered

. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial

. Plasti ci s preferre d ove rth e us e ofglas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass

. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water
. Prepar e metho d QC sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials

. Prepar e a t least fiv e metho d blanks

. 

### 9 Sampi e Analysis-LC/MS/M S Analyz e th e standar

d curve prio rt o eac h set ofsamples

. Th e standar d curve ma

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

xo runweighted , o rb

yquadrati cfi l (

y= ax ^ + b x+ c) , weighte d 1/

xo runweighted , usin g suitabl e software

. Th e calibratio n curve s ma yinclud e bu t shoul d no

t b e force d throug h zero . Th e mathematica l metho d use d t o calculat e th e calibratio n curve shoul d b e applie d consistentl ythroughou t a study

. An ychang e shoul d b e thoroughl ydocumente d i n th e ra wdata

. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfi t ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-detemnine 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 o fdeterminatio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o requa l t o 0.990

. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 3 o f5 7Docimwxtl-9TSBj\kmm'mi4>miccmien t fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S I n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0

b e withi n ±30%

. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata

. Aminimu m of6 points wil l b e use d t o constmc t th e calibratio n curve . I fth e calibratio n curve doe s no t meet acceptance criteria , perfon n routin e maintenance o rprepar e a ne wstandar d curve (i 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 las t passin g CCV wil l the n bracket acceptabl e samples

. Multipl e CCV level s ma yb e used

. Sample s containin g analyte s that 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 yContro l
10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e data 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 belo wwil l b e documente d i n th e ra wdata an d footnote d i n th e fina l report
. 

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

s must b e prepare d wit h eac h analysi s batch

. At least fiv e metho d blank s must b e prepared

. Metho d blank

s ma yb e injecte d multipl e times , bu t n o mor e tha n 3 injection s shoul d b e remove d fro m a singl e metho d blank

. At a minimum , metho d blank s are analyze d prio rt o instrumen t calibration , prio rt o th e analysi s of CCV samples , an d a

t th e en d ofth e analytica l mn . Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % 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 firs t 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 detennin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made

. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field

. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo r replicate s exclude s fiel d blanks

. 

### 10. 4 Surrogat e Spike s 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 oftwo differen t concentration s are t o b e prepare d wit h eac h preparatio n batch

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

d deviatio n ofth e contro l spike s evaluate d independentl ya t eac h concentratio n leve l mus t b e les s tha n o requa l t o 20 % an d th e averag e recover ymus t b e 80-120%

. I fth e above criteri a ar e no t met , th e entir

e set o fsample s shoul d b e re-injecte d o rre-prepare d as appropriate :

ETS-8-044. 0 Pag e 9 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 4 o f5 7Docum.9«A-€-rmj\kmrmmt^!>0XKurrenl , fo r1 4 day s fro m 01/03/20' ^ Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0

10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s o

ffiel d matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % o fth e fortifie d levels

. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d as suc h (wit h expande d accurac ystatements) , o rwil l 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 % o fth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o determin e th e statemen t ofaccurac yfo ranalytica l results

. Th e averag e ofth e sampl e an d th e fiel d duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t o fanalyt e foun d (i n ng/mL , base d o n pea k area) usin g th e standar d curve (linea rregressio n parameters ) generate d iD ya n appropriat e software program : A1 1 rJ /

, , x(Pea k

Area-Intercept ) ^r Analyt e foun d (ng/mL ) = - ^ ^-^

xD F Slop e D F = facto rb

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

_Tota l analyt e foun d (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) Analyt e adde d (ng/mL )
1 2 Metho d Performanc e An ymetho d perfonnanc e parameter s that ar e no t achieve d must b e considere d i n th e evaluatio n o fth e data

. Nonconfonnance t o an yspecifie d parameter s mus t b e describe d an d discusse d i fth e Technica l Manage r(non
GL P study) o rStud yDirecto r(GL P study ) choose s t o repor

t th e data

. I fcriteri a liste d i n thi s metho d perfomnanc e sectio n are no

t met , maintenance ma

yb e performe d o n th e syste m an d sample s reanalyzed , o rothe raction s take n as appropriate

. Documen t al l action s i n th e ra wdata

. I fdat a are t o b e reporte d whe n perfonnance criteri a hav e no t bee n met , th e dat a must b e footnote d o n table s an d discusse d i n th e tex

t 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 ar

e injecte d a

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

. Th e syste m suitabilit yinjection s mus

t have are a counts wit h a n RS D of25 % 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 mus t b e greate rtha n o r equa l t o 0.990

. Eac h poin t i n th e curve mus t b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

yb e withi n ±30%

. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence ar e evaluate d as continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac 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 tha t ar e brackete d b

yCCVs no

t meetin g thes e criteri a must b e reanalyzed

.

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 5 o f5 7Docu:©ii?!rrt-(o-ft62/ib@-ira8isl),rtff(cuiTent , fo r1 4 day s fro m 01/03/201 1 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Attachmen t C Octobe r201 0

Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

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

. 12. 3 Sensitivit y Th e targete d limi t ofquantitatio n fo ral l analyte s i s 0.02 5 ng/mL

. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n o fappropriat e blank

s an d th e accurac

yofth e low-leve l calibratio n curve points

. Refe r t o Sectio n 1 0 fo radditiona l details

. 

### 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s are designe d t o generat e data that are accurat e t o +/-30%

. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d accurac yo flaborator

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

ymatri xspikes

. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field

. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo rreplicate s exclude s fiel d blank s o rrinse blanks

. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d precisio n oflaborator ycontro l spikes

. 

### 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfomriin g thi s metho d wil l b e dispose d o fappropriately

. Th e origina l sample s wil l b e archive d a

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

. 1 4 Record s Eac h dat a packag e generate d fo ra stud ymus t includ e al l supportin g informatio n fo rreconstructio n ofth e data

. Informatio n fo rth e dat a packag e mus t include , bu t i s no

t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

ypages) , instmmen t results files , chromatograms , calibratio n curves , an d dat a calculations

. 1 5 Affecte d Document s None

. 1 6 Revision s Revisio n Numbe rSummar yo fChange s

ETS-8-044. 0 Pag e 1 1 of1 1 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 6 o f5 7

### ^McfffflS^l^ntia l GLP10-01-02 ; Interi m Repor t 1 0 Analysi s fo rPFBS , PFHS , an d PFO S i n Groundwate rfro m Decatur , A L Octobe r201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/

. Identificatio n Stud y/ Projec t No

. GLPlO-01-02-1 0 Date(s ) o fOccurrence : 11/8/10-g101108 a I Documen t ! ETS-8-04 4 Number :

0 Deviatio n typ e 0 SO P D Equipmen t Procedur e IZ i Metho d (Chec k one ) D Protoco l D GP O D Other :



### //

. Descriptio n (attac h extr a pages a s needed ) Metho d Requirements : (1 ) Syste m suitabilityare a coun t RS D <5% , retentio n tim e RS D <2 % (2 ) LC S averag e recover yo f100 % ±20%

. (3 ) Sample/Sampl e Duplicat e RP D <20%

. 

### Actua l procedure/p^^^^^^

^ (1 ) Are a ratio s were use d i n plac e o fare a count s sinc e th e calibratio n curv e wa s generate d usin g Interna l standard are a ratios

. Th e are a rati o RS D fo rPFH S wa s jus t outsid e metho d acceptanc e criteri a at 5.9%

. (2 ) LC S averag e recover yfo rbot h set s oflinea ran d branche d PFO S were outsid e metho d acceptanc e criteri a wit h averag e recoverie s o f126 % an d 122%

. (3 ) Th e RP D valu e fo rsevera l samplin g location s wer e >20 % 

### II L Action s Take n (suc h a s amendmen t issued

. SO P revision , etc. ) 

### Correctiv e Actio n ( D Ye s 0 No) Reference : Acceptabilityo fth e nonconformin g work : 1 ) Syste m suitability- Othe rQ C item s were use d t o asses s dat a accurac yfo rPFHS , whic h ha d are a rati o RSD s outsid e metho d acceptanc e criteri a - calibratio n curv e poin t accuracy , curv e fi t criteria , CCV , an d LC S an d FM S recoveries , al l meetin g metho d acceptanc e criteria

. 2 ) I n general , th e EC F LC S fo rPFOAan d PFO S have bee n runnin g 1.5-20 % highe rwhe n quantitate d usin g linea rPFOAan d PFOS

. LC S recoverie s <130 % fo rEC F PFOAan d PFO S are withi n FM S acceptanc e criteri a of100 % ±30 % fo rETS-8-044.0

. Al l LC S were use d i n th e determinatio n ofmetho d uncertainty

. 3 ) Samplin g location s wit h RP D value s >20 % wil l b e footnote d i n th e dat a tables

. Actions : D Haltin g o fWor k D Clien t Notificatio n D Wor k Recal l D Withholdin g o fRepor t IZ I Other : Deviation s wil l b e note d i n fina l repor t 

# M l Project Lead/PA ! Approval : S Stud yDirecto r(i fGLP) : Dat e ^ 1 1 Date : Sponso rApprova l (fo rGL P protoco l deviations) : N A Date : N A Technica l Reviewe r(optional) : NA Date : NA Laborator yDepartmen t Manage rApproval : Date :

ly

. Authorizatio n t o Resum e Wor k Where haltin g o fwori < occurred , resumptio n o fworl < mus t firs t b e approve d b yLaborator yManagemen t 

### Laborator yDepartmen t Manage rApproval : N AI Date : N A Deviatio n No

. (assigne d b yStud yDirecto ro rTea m Leade ra t th e en d o fstud yo rproject )

Attachmen t AETS-4-008. 7 Pag e l^of j

Documentatio n o fDeviation s an d Contro l o fNonconformin g Testing , Pag e 5 7 o f5 7