GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

GLP10-01-02 : Interi m Repor t 0 7 - Analysi s o fPFBS

. PFHS

. an d PFO S i n Groun d Wate r Sample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur

. A L i n June/Jul y201 0
Stud yTitl e Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc

. 140 0 Westo n Way Westchester , PA1938 0 Phone : 610-701-376 1 Autho r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor t Completio n Dat e

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

y 3 M Center , BId g 260-05-N-1 7 Maplewood , M N 55144 Projec t Identificatio n GLP10-01-02-0 7 Tota l Numbe ro fPage s

6 8

^ H y^H ^

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 ^ y ^ ^T ^ Competenc e o fTestin g an d Calibratio n Laboratories", I n accordanc e wit h th e A2LACertificat e #2052.01

. lACC'^^l^l^i^P i Testin g tha t complie s wit h thi s Intematlona 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 f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements

.

PAG E 2 O F 3 6 Pag e 2 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

t 0 7 Analysi s o

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

t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n June/Jul y201 0 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site
Relate d Monitorin g Program

. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s wher e 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 hav

e no t bee n detennine d unde rGLPs

. 

# /i 6 Gar yHol/enalein , Sponso rRepresentative Date

Jaisimh a Kesari , P.E. , DEE , StudyDirecto r'Dat e

Pag e 3 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

t 0 7 Analysi s ofPFBS , PFHS , an d PFO S i n Groun d Wate rSample s Collecte d a

t th e Fonne rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n June/Jul y201 0 Study : Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site
Relate d Monitorin g Program

. Thi s analytica l phas e wa s audite d b yth e 3 M Environmenta l Laborator yQualit yAssurance Uni t (QAU) , a s indicate d i n th e followin g table

. Th e findings were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector

.

Inspectio n Date s 10/1,10/4 , an d 10/5/1 0 Phas e Interi m Repor

t 0 7 Dat a an d Repor

t Dat e Reporte d t o

Testin g Facilit y Managemen t 10/11/1 0 Stud yDirecto r 10/11/1 0 

# h /o-;i'^'^ 6 QA U RepresCTitativ

e Date

Pag e 4 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

y9 3 Introductio n 1 1 4 Test & Contro l Substance s 1 1 5 Reference Substance s 1 2 6 Test Syste m 1 3 7 Metho d Summar

y1 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 ofQuantitatio 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 6 8. 7 Analytica l Metho d Uncertaint y1 8 8. 9 Fiel d Matri xSpike s (FMS ) 1 9 9 Data Summar

yan d Discussio n 1 9

Pag e 5 of6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

1 0 Conclusio n 35 1 1 Data/Sampl e Retentio n 35 1 2 /attachments 35 1 3 Signature s 3 6 

### LIS TO F TABLE S Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Results (FSI AGroundwater , June/Jul y2010)

. 1 0 Tabl e 2

. Sampl e Descriptio n Ke yCod e 1 3 Tabl e 3

. Instalmen t Parameter s 1 4 Table4

. Liqui d Chromatograph yCondition s 1 4 Tabl e 5

. Mass Transition s 1 4 Tables

. Limi t ofQuantitatio n (LOQ ) 1 5 Tabl e 7

. Laborator

yContro l Spik

e Recover

y1 7 Tables

. Analytica l Uncertaint y1 9 Tabl e 9

. Fiel d Matri xSpik e Level s 1 9 Tabl e 10

. DA L 130 R 0 2 Y1 0 S F 2 1 Tabl e 11

. DAL130LQ 2 Y10S F 2 2 Tabl e 12

. DA L 130 S 0 2 Y1 0 S F 2 3 Tabl e 13

. DA L 131 R 0 2 Y1 0 S F 2 3 Tabl e 14

. DA L 131 L 0 2 Y1 0 S F 2 4 Tabl e 15

. DA L 131 S 0 2 Y1 0 S F 2 4 Tabl e 16

. DA L 132 R 0 2 Y1 0 S F 2 5 Tabl e 17

. DA L 132 L 0 2 Y1 0 S F 2 5 Tabl e 18

. DA L 132 S 0 2 Y1 0 S F 2 6 Tabl e 19

. DA L 133 R 0 2 Y1 0 S F 2 6 Tabl e 20

. DA L 133 L 0 2 Y1 0 S F 2 7 Tabl e 21

. DAL133SQ 2 Y10S F 2 7

Pag e 6 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 22

. DA L 134 R 0 2 Y1 0 S F 2 8 Tabl e 23

. DA L 134 L 0 2 Y1 0 S F 2 8 Tabl e 24

. DA L 134 S 0 2 Y1 0 S F 2 9 Tabl e 25

. DA L 135 R 0 2 Y1 0 S F 2 9 Tabl e 26

. DA L 135L0 2 Y10S F 3 0 Tabl e 27

. DA L 135 S Q2 Y1 0 S F 3 0 Tabl e 28

. DA L 136 L 0 2 Y1 0 S F 3 1 Tabl e 29

. DA L 136 S 0 2 Y1 0 S F 3 1 Tabl e 30

. DA L 137 L Q2 Y1 0 S F 3 2 Tabl e 30

. DA L 137 S 0 2 Y1 0 S F 32 Tabl e 32

. DA L 138SQ 2 Y10S F 33 Tabl e 33

. DAL138LQ 2 Y10S F 33 Tabl e 34

. Tri p Blan k

34 Tabl e 35

. Rinseat e Blank s 34

Pag e 7 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

1 Stud yInformatio n Sponso r 3 M Compan y Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operafion 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(a)mmm.com) ; phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Jonatha n Steege ; analys t Stud yDate s StudyInitiation : Marc h 8 , 201 0 Interi m 0 7 Experimenta l Tennination : Septembe r17 , 201 0 Interi m Repor

t Completion : Date o

fInteri m Repor

t Signin g Locatio n o fArchive s Al l origina l ra

wdat a an d th e analytica l repor t have bee n archive d a

t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792

. Th e tes t substanc e an d analytica l referenc e standard reserv e sample s ar e archive d a t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

2 Summar y Th e 3 M Environmenta l Laborator yreceive d groun d wate rsample s fro m well s locate d a t th e Fonne r Sludg e Incorporatio n Are a (FSIA ) i n Decatur , AL , representin g twenty-fou rdifferen t samplin g locations

. Atota l ofon e hundre d twenty-fou rsampl e bottle s were receive d a t th e 3 M Environmenta l Laborator y fo rperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e groundwate rsample s fro m eac h samplin g location

. Sample s als o include d a

t least two field matri xspik e (FMS ) sample s fo reac h location , on e tri p blan k containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseates. Th e equipmen t rinseate blank s di d no t have FM S sample s prepare d fo rdeterminatio n ofPFBS , PFHS , an d PFO S recovery
. Th e groun d wate rsamples , tri p blan k an d two equipmen t rinseate blank s were collecte d o n Jun e 30 , Jul y1 an d Jul y2,2010 , an d receive d fro m Westo n personne l o n Jul y6,2010

. Al l ofth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator

yMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP-10-01-02-07

. Man yofth e groun d wate rsample s require d dilutio n t o attai n PFBS , PFHS , and/o rPOFS concentration s withi n th e rang e ofth e curve , i n som e instance s u p t o 100-fol d dilutio n were required

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

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

wth e lowe rlimi t ofquantitatio n (LLOQ) , indicatin g adequat e contro l o

fsampl e contaminatio n durin g shippin g an d sampl e collections

. Th e PFB S concentratio n results fo ral l groun d water s range d ove rthre e order s ofmagnitud e fro m 0.046 3 ng/m L t o 75. 1 ng/mL

. Th e PFH S concentratio n results fo ral l groun d water s range d ove rthre e order s of magnitud e fro m <0.10 3 ng/m L t o 75 4 ng/mL

. Th e PFO S concentratio n results fo ral l groun d water s range d ove rfou rorder

s ofmagnitud e fro m 0.42 7 ng/m L t o 172 0 ng/mL

.

Pag e 9 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Result s (FSI AGroundwater , June/Jul y2010)

.
Samplin g Locatio n DA L 130RQ2Y10S F 10070 1 DA L 130LQ2Y10S F 10070 1 DA L 130SQ2Y10S F 10070 1 DA L 131RQ2Y10S F 10070 1 DA L 131LQ2Y10S F 10063 0 DA L 131SQ2Y10S F 10063 0 DA L 132RQ2Y10S F 10070 1 DA L 132LQ2Y10S F 10070 1 DA L 132SQ2Y10S F 10070 1 DA L 133RQ2Y10S F 10070 1 DA L 133LQ2Y10S F 10070 2 DA L 133SQ2Y10S F 10070 1 DA L 134RQ2Y10S F 10070 2 DA L 134LQ2Y10S F 10070 2 DA L 134SQ2Y10S F 10070 2 DA L 135RQ2Y10S F 10070 2 DA L 135LQ2Y10S F 10070 2 DA L 135SQ2Y10S F 10070 2 DA L 136LQ2Y10S F 10063 0 DA L 136SQ2Y10S F 10063 0 DA L 137LQ2Y10S F 10070 1 DA L 137SQ2Y10S F 10070 1 DA L 138SQ2Y10S F 10063 0 DA L 138LQ2Y10S F 10063 0 Tri p Blan k

(Milli-Q TM Water

) Equipmen t Rinseate Blanks , 137 L an d 131 R PFB S Avg

. Cone

. (ng/mL ) ±RP D 16. 6 ±1.2 % 1.53 ±2.0 % 3.5 7 ±2.0 % 75. 1 ±0.53 % 2.9 4 ±6,8 % 1.06 ±0,95 % 7.6 4 ±1.0 % 10, 0 ±5,2 % 32. 6 ±4,9 % 7,7 0 ±2,1 % 6,7 5 ±1,9 % 12, 7 ±0.79 % 59. 1 ±1.7 % 12. 8 ±0.78 % 0,093 8 ±13 % 83, 0 ±0,48 % 6,3 6 ±0,63 % 0,73 5 ±3,5 % 2,9 1 ±3,8 % 3,4 9 ±1,1 % 0,084 7 ±16 % 0,11 9 ±7,6 % 5,7 2 ±3,3 % 0,046 3 ±27 % '^ ' <0,030 6 <0,030 6 PFH S

Avg

. Cone

. (ng/mL ) ±RP D 11 9 ±0,0 % 13. 0 ±2.0 % 12, 1 ±16 % 34 5 ±1,2 % 19, 3 ±3,6 % 5,4 9 ±1.5 % 36, 0 ±1,9 % 78. 2 ±3,7 % 21 1 ±0,0 % 45, 6 ±1,1 % 39, 4 ±0,76 % 77, 1 ±4,2 % 44 1 ±2.3 % 10 6 ±1,9 % 1.3 3 ±6,0 % 75 4 ±1.9 % 37, 9 ±8,4 % 5,8 8 ±5,4 % 11, 7 ±2.6 % 19, 3 ±1.0 % <0,10 3 <0,10 3 16. 9 ±1,8 % <0,10 3 <0,10 3 <0.10 3 PFO S

Avg

. Cone

. (ng/mL ) ±RP D 53 2 ±8.5 % 74, 4 ±2,3 % <^

' 72, 1 ±0,69 % 172 0 ±1,4 % 33, 6 ±1,6 % 8,2 5 ±3,9 % 26 3 ±0.76 % 24 0 ±2,1%'^'' ^ 86 1 ±0.58 % 77, 5 ±9,2 % 144 ±7.6 % 22 8 ±5,4 % 118 0 ±2,3 % 49 1 ±2,7 % <^

' 12, 6 ±7,2 % 104 0 ±1.8 % 55, 4 ±9,9 % 7,1 6 ±8,1 % 89, 7 ±4,4 % 10 6 ±6.0 % 0,73 4 ±14 % 0,42 7 ±3,7%'^' 21 6 ±0,42 % 0,79 1 ±3,7 % <0,10 2 <0,10 2 Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results ar e a s follows : PFB S 100% ±19% , PFH S 100% ±20% , an d PFO S 100 % ±37% , (1 ) Th e analytica l uncertaint yha s Isee n adjuste d fo rPFO S base d o n FM S recover yfor : DA L 1 SO

L t o 100 % ±45 % an d D/\L 137 S t o 100 % ±38% , Se e discussio n i n sectio n 9 ofth e report

. (2 ) Samplin g locatio n di d no t hav e a n appropriate FM S spil<e leve l t o sufficientl yevaluat e analyte recovery , (3) Th e RP D di d no

t mee t method acceptance criteri a of£20% ,

Pag e 1 0 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

3 Introductio n Thi s analytica l stud ywa s conducte d as par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit

ylocate d i n Decatur , Alabama

. Th e objective o fth e overal l progra m i s t o gai n infonnatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s envinanmenta l medi a suc h a s groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility

. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d a t th e Fornie rSludg e incorporatio n Are a (FSAI ) i n Decatur , A L fo rPFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on sit e groundwate rconditions

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

ypolyethylen e bottles ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o field sampling

. Sampl e container s fo reac h samplin g locafio n include d a field sample , fiel d sampl e duplicate , an d thre e field spik e samples

. Eac h empt

ycontaine rwas mari<e

d wit h a "fil l t o here " lin e t o produce a final sampl e volum e of20 0 mL

. Container s designate d fo rfield matri xsample s were fortifie d wit h a n appropriat e matri xspik

e solutio n containin g PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o bein g sen t t o th e field fo rsampl e collection

. Se e sectio n 8. 8 ofth e repor t fo rfield matri xspik

e levels

. Th e aqueou s equipmen t rinseate sample s were collecte d i n plai n bottle s withou t mari<ings o rfortifications

. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detenninatio n o fPerfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

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

. Table s 10-33 summariz e th e individua l sampl e results an d th e associate d FM S recoveries

. Al l results fo rth e qualit y contro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewher e i n thi s repor t


### 4 Tes t & Contro l Substance s There was no

t a test substance o rcontro l substance s i n th e classi csens e ofa GL P study

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

.

Pag e 1 1 o f6 8

### 5 Referenc e Substance s GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Referenc e Substanc e Chemica l Nam e Chemica l Fonnul 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 CeFiaSO s Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHxSAMO

S TCR08-001 8 Crystallin e 98 %

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 PFO S (linear ) Perfluorooctan e sulfonat e C8F17SO3" Potassiu m Sal t CAS #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 sulfonate C8F17SO3" Potassiu m Sal t CA S # 2795-39- 3 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 Whit e Powde r 86,4 %

Pag e 1 2 o f£GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

6 Tes t Syste m Th e test syste m fo rthi s stud yare groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b y Westo n Solutions , Inc

. personnel

. Sample s fo rthi s stud yare "rea l worid " samples , no t dose d wit h a specifi clot oftest substance

. Tabl e 2

. Sampl e Descriptio n Ke yCode

. strin g Numtie r Exampl e 1 2 3

4 Strin g Descripto r DA L 131 S Q2Y1 0 SF O Samplin g Locatio n Samplin g Poin t Wel l Leve l
Samplin g Dat e Sampl e Typ e Exampl e
DA L = Decatur , A L Example : 131 S R = Residu m shallo wwater-bearin g zon e L = Bedmc k

water-tiearin g zon e S = Epikars t middl e water-bearin g zon e Q2Y1 0 - 2n d Quarter , 201 0 0=primarysampl e 1=duplicat e sampl e L S = lo wspik e M S = mi d spik e H S = hig h spik e
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 Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

.

~T M , 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene' " (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 Jul y 6 , 201 0 Sample s were store d refrigerate d a t th e laborator

yafte rreceipt

. Aset oflaborator yprepare d Tri p Blan k

an d Tri p Blan k

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

. 

### 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g it i n a n autovia l fo r analysis

. Sample s that require d dilutio n were prepare d b ydilution s ofIm L sampl e wit h 9 mL s o fMill i Q wate r (dilutio n 1:10)

. Most samplin g location s were dilute d 1:100 b yfurthe rdilutin g th e 1:1 0 dilutio n wit h additiona l Mill i 0 water

. 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 mass spectrometr y(HPLC/MS/MS)

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

wdata har

d copie s place d i n th e final data packet , an d are briefl ydescribe d below

.

Pag e 1 3 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 3

. Instrumen t Parameters

. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e IVIas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETS OIli e ETS-8-044, 0 7/15/201 0 Agilen t 1100 Betasi l C1 8 (2, 1 m m X 100 mm) , 5 n Betasi l C1 8 (2, 1 m m X 100 mm) , 5 n

2or10ti L /Applied Biosystem s AP I 400 0 Turtx j Spra y Turtj o io n electrod e Negativ e /Analys t 1,4, 2 ETS Mar yAn n ETS-8-044, 0 9/17/1 0 Agilen t 1100 Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n Betasi l C I 8 (2, 1 m m X 100 mm) , 5 n

SorlOu L /\pplie d Biosystem s AP I 500 0 Turtj o Spra

y Turb o io n electrod e Negativ e Analyst 1.4. 2 Tabl e 4

. Liqui d Chromatograph yConditions

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

(min ) 0 1. 0 14. 5 15. 5 16. 5 20. 0 Flo wRat e

(fdJmin ) 30 0 30 0 30 0 30 0 30 0 30 0 Percen t A

( 2 m M ammoniu m acetate )

90, 0 90, 0 10, 0 10, 0 90, 0 90, 0 Percent B

(Methanol ) 10. 0 10, 0 90, 0 90, 0 10. 0 10, 0 Tabl e 5

. Mas s Transitions

.

Analyt e
PFB S

PFH S

PFO S Mas s Transitio n Q1/Q 3 299/8 0 299/9 9 399/8 0 399/9 9 399/13 0 499/8 0 499/9 9 499/13 0 Dwel l tim e wa s 125 o r5 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

.
8 Analytica l Result s
8. 1 Calibratio n Sample s were analyze d against a n extema 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 prepare d i n

Pag e 1 4 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Mill i 0 water

. Atota l offifteen spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) were prepared , however , th e 9/17/1 0 analysi s di d no t contai n th e two highest curve points

. Lo wo rhig h curve points ma yhave bee n disable d t o meet metho d criteria

. Aquadratic , 1/ xweighted , calibratio n curve of th e pea k are a counts wa s use d t o fit th e data fo reac h analyte

. Th e data were no t force d throug h zer

o durin g th e fitting process
. Calculatin g th e standar d concentration s usin g th e pea k are a confirme d accurac yo feac h curve point

. 7/15/1 0 Analysi s fo rPFOS ; Th e calibratio n curve wa s constructe d usin g th e linea risome rofPFO S only

. Since th e sample s were expecte d t o contai n bot h linea ran d branche d isomer s ofPFOS , LC S an d sample s were quantitate d b yprocessin g th e PFO S linea ran d branche d isomer s separatel yan d summin g th e calculate d concentration s togethe rt o generate th e final PFO S concentration

. Thi s was don e t o hel p minimiz e an ypotentia l analytica l bias du e t o quantitatin g linea ran d branche d isomer s of PFO S against a predominatel ylinea rreference standar d fo rPFOS

. 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 PFO. S fo rbot h th e 7/15/1 0 an d 9/17/1 0 analysis

. 

### 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

. Th e acceptance criteri a ofless tha n o requa l t o 5 % relafive standar d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a o fles s tha n o requa l t o 2 % RS D was met fo rPFBS , PFHS , an d PFO S fo rbot h th e 7/15/1 0 an d 9/17/1 0 analysis

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

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

yrequirements an d fo rwhic h th e are a counts ar e a t leas t twic e thos e ofth e appropriat e blanks

. Th e nomina l LOO fo ral l analyte s ca n b e foun d i n Tabl e 6

. Tabl e 6

. Limi t o fQuantitatio n (LOQ)

. Analysi s Dat e 7/15/1 0

9/17/1 0 Dilutio n 1 1 0 100 1 PFB S

LOQ , ng/m L 0.030 6 0,30 6 3,06 0.025 5 PFH S

LOQ , ng/m L 0.103 1,0 3 10, 3 0,025 8 PFO S

LOQ , ng/m L 0.102 1.0 2 10. 2 0.51 0 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confin n tha

t th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control

. Al l CCV s me t metho d criteri a of100 % ±25 % wit h th e exceptio n ofth e following : 7/15/1 0 Analysis ; Twenty-on e CCV s were analyze d durin g th e cours e ofth e ru n wit h thre e CCV s no t meetin g metho d acceptance criteri a wit h recoverie s o f70.8% , 73.6% , an d 73.3 % fo rPFHS

. Reporte d sample s brackete d b

ythes e CCV

s include : 132S , 134R , 135S , an d 135L

. 

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

fblank s were prepare d an d analyze d wit h th e samples : metho d blank s an d field/trip blanks

. Metho d blan k

results were reviewe d an d use d t o evaluate metho d perfomnance'an d t o detemnin e th e LOO fo reac h analyt e

Pag e 1 5 o f6 8GLP10-0i-02 ; Interi m Repor t 0 7 Analysi s ofPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s wer e prepare d an d analyze d i n triplicat e wit h eac h preparatio n set

. LCS s wer e prepare d b yspikin g know n amount s o fth e analyt e int o Mill i Q wate rt o produc e th e desire d concentration

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

. Th e metho d acceptanc e 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 % Acceptanc e criteri a wa s me t fo rth e PFBS , PFHS , an d linea r PFO S fo rLC S sample s analyze d o n 7/15/10

. Acceptanc e criteri a wa s no t me t fo rth e lo wse t o flinea r PFO S LC S analyze d o n 9/17/1 0 wit h a n averag e recoveryo f19 1 %

. Th e mi d an d hig h set s o flinea r PFO S LC S me t metho d acceptanc e criteria , a s di d al l thre e set s o fLC S fo rPFB S an d PFHS

. Th e 9/17/1 0 analysi s include d a numbe ro fsample s tha t containe d PFO S concentration s greate rtha n th e calibratio n range
. I t i s believe d tha t th e hig h recoveryfo rth e lo wse t o fLC S i s du e t o analyt e carry-ove r a s th e lo wse t o fLC S wer e analyze d immediatel yafte rthes e samples

. A s th e referenc e material s use d fo rquantitatio n o fPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s ar e comprise d o fbot h linea ran d branche d isomers , additiona l LC S sample s o f PFO S (linea r+ branched ) wer e prepare d a t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias

. Th e LC S analyze d o n 7/15/1 0 a t th e lo wan d mi d level s me t metho d acceptanc e criteria , whil e th e hig h leve l di d no t mee t metho d acceptanc e criteri a wit h a n averag e recoveryo f122%

. Th e LC S analyze d o n 9/17/1 0 a t th e mi d an d hig h level s me t metho d acceptanc e criteria , whil e th e lo wleve l di d no t mee t metho d acceptanc e criteri a wit h a n averag e recoveryo f125%

. Al l PFO S (linea r+ branched ) LC S wer e use d i n th e determinatio n o fth e analytica l uncertainty

. Ametho d deviatio n i s filed wit h th e ra wdat a fo rPFO S (linea ran d linea r+ branched ) LC S tha t di d no t mee t metho d acceptanc e criteria

. Th e followin g calculation s wer e use d t o generat e dat a i n Tabl e 7 fo rlaboratorycontro l spikes

.

1 /^or , . o Calculate d Concentratio n ..-_. , LC S Percen t Recover

y= 100 % Spil<e Concentratio n LCS % RS D = standard deviatio n LC S replicate s ,^^^,^ ^ averag e LC S recover

y

Pag e 1 6 of6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 7

. Laborator yContro l Spik e Recovery

. ETS-8-044, 0 Analyze d 7/15/1 0

La b I D LCS-100707- 1 LCS-100707- 2 LCS-100707- 3 Averag e ±%RS D LCS-100707- 4 LCS-100707- 5 LCS-100707- 6 Averag e ±%RS D LCS-100707- 7 LCS-100707- 8 LCS-100707- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 0.50 6 0,53 4 0,53 0 YoRecover y

99, 3 10 5 10 4 103 ±3.0 % 5.1 0 5.1 0 5,1 0 5,1 3

4,9 0 5,2 3 10 1

96, 1 10 3 100 % ±3.5 % 30, 6 30, 6 30, 6 28, 4

27, 9 28, 6 92, 7

91, 0 93. 6 92.4 % ±1.4 % PFH S Spike d Concentratio n (ng/mL ) 0,51 5 0,51 5 0,51 5 Calculate d

Concentratio n (ng/mL ) 0.46 3 0.45 5 0.48 0 YoRecover y

89, 8 88, 3 93, 2 90.4 % ±2.8 % 5.1 5 5.1 5 5,1 5 5,6 4

5,5 9 5,7 3 110

10 8 11 1 110 % ±1.4 % 30, 9 30. 9 30, 9 30, 7

29, 9 30, 4 99. 3

96, 7 98. 3 98.1 % ±1.3 %

ETS-8-044, 0 Analyze d 7/15/1 0

La b I D LCS-100707- 1 LCS-100707- 2 LCS-100707- 3 Averag e ±%RS D LCS-100707- 4 LCS-100707- 5 LCS-100707- 6 Averag e ±%RS D LCS-100707- 7 LCS-100707- 8 LCS-100707- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 0,48 0 0,44 7 0,47 0 YoRecover y

94, 1 87, 6 92, 2 91.3 % ±3.6 % 5.1 0 5.1 0 5.1 0 5,4 8

5,4 3 5,4 6 10 7

10 6 10 7 107 % ±0.46 % 30, 6 30, 6 30, 6 30, 1

30, 6 30, 7 98, 4

10 0 10 0 99.6 % ±1.1 % La b I D LCS-100707-1 0 LCS-100707-1 1 LCS-100707-1 2 Averag e ±%RS D LCS-100707-1 3 LCS-100707-1 4 LCS-100707-1 5 Averag e ±%RS D LCS-100707-1 6 LCS-100707-1 7 LCS-100707-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0,50 0 0.50 0 0.50 0 Calculate d

Concentratio n (ng/mL ) 0,49 3 0,43 1 0.41 9 YoRecover y

98, 6 86, 2 83, 8 89.5 % ±8.9 % 5,0 0 5,0 0 5,0 0 5.8 4

5.6 7 5.8 3 11 7

11 3 11 7 116 % ±1.7 % 30, 0 30, 0 30, 0 37, 8

36, 0 36, 3 12 6

120 12 1 122 % ±2.6%" ' (1 ) Th e averag e recover ydi d not meet metho d acceptance criteri a of100 % ±20%

.

Pag e 1 7 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 7 continued

. Laborator yContro l Spik e Recovery

. ETS-8-044. 0 Analyze d 9/17/1 0

La b I D LCS-100916- 1 LCS-100916- 2 LCS-100916- 3 Averag e ±%RS D LCS-100916- 4 LCS-100916- 5 LCS-100916- 6 Averag e ±%RS D LCS-100916- 7 LCS-100916- 8 LCS-100916- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 0.47 4 0.58 3 0.59 2 YoRecover y

93, 0 11 4 11 6 108 % ±12 % 5,1 0 5.1 0 5.1 0 5.0 7

5.9 8 6.1 4 99, 4

11 7 12 0 112 % ±9.9 % 15. 3 15. 3 15. 3 16, 9

16, 1 16, 7 11 0

10 5 10 9 108 % ±2.4 % PFH S Spike d Concentratio n (ng/mL ) 0,51 5 0,51 5 0,51 5 Calculate d

Concentratio n (ng/mL ) 0.46 1 0.56 5 0.56 3 YoRecover y

89, 5 11 0 10 9 103 % ±11 % 5,1 5 5.1 5 5,1 5 4.6 6

5.5 0 5.5 4 90, 5

10 7 10 8 102 % ±9.7 % 15. 5 15, 5 15, 5 15. 7

15. 8 15, 3 10 1

10 2 98. 6 101 % ±1.7 % ETS-8-044, 0 Analyze d 9/17/1 0

La b I D LCS-100916- 1 LCS-100916- 2 LCS-100916- 3 Averag e ±%RS D LCS-100916- 4 LCS-100916- 5 LCS-100916- 6 Averag e ±%RS D LCS-100916- 7 LCS-100916- 8 LCS-100916- 9 Averag e ±%RS O PFO S (linear )

Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 1.1 0 1.0 1 0.82 1 YoRecover y

21 6 19 7 16 1 191 % ±15%'^- ^ 5,1 0 5,1 0 5,1 0 4,3 2

4,9 3 5,1 8 84. 7

96. 8 10 2 94.5 % ±9.4 % 15, 3 15, 3 15, 3 14. 0

14. 7 13. 6 91. 3

96. 1 88. 9 92.1 % ±4.0 % La b I D LCS-100916-1 0 LCS-100916-1 1 LCS-100916-1 2 Averag e ±%RS D LCS-100916-1 3 LCS-100916-1 4 LCS-100916-1 5 Averag e ±%RS D LCS-100916-1 6 LCS-100916-1 7 LCS-100916-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0,50 0 0,50 0 0.50 0 Calculate d

Concentratio n (ng/mL ) 0,67 8 0,66 9 0,52 7 %Recover y

13 6 13 4 10 5 125 % ±14%'' ' 5,0 0 5,0 0 5,0 0 4,8 7

4,9 7 4.8 4 97, 4

99, 4 96, 8 97.9 % ±1.4 % 15, 0 15, 0 15, 0 14, 9

15, 2 15, 0 99, 5

10 2 10 0 101 % ±1.3 % (1 ) Th e averag e recover ydi d no t meet method acceptance criteri a of100 % ±20% , (2 ) Th e hig h recover

yi s mos t lilcelydu e t o carr

yover , whic h i s liicelydu e t o sample s analyze d prio rt o LC S sample s whic h ha d PFO S concentration s exceedin g th e calibratio n range , 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 OC samples

. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto ro

f2 , whicl i con-espond s t o a confidence leve l of95%

. Th e mos t recen t 5 0 data points were use d t o generate th e metho d uncertaint

yvalue s liste d i n Tabl e 8

.

Pag e 1 8 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 8

. Analytica l Uncertainty

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

9.3 9 9.7 6 18. 6 Metho d

Uncertaint y 100%±19 % 100%±20 % 100%±37 % 8. 8 Fiel d Matri xSpike s (FMS ) Low , mi d an d hig h fiel d matri xspike s (FMS ) were collecte d a t eac h samplin g poin t (lowan d hig h FM S onl ya t 131R , 134R , an d 135R) t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix

. Fiel d matri xspike s were generate d b yaddin g a measure d volum e o ffiel 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 of 100±30 % confir m that "unknown " components i n th e sampl e matri xd o no t significantl yinterfer

e wit h th e extractio n an d analysi s ofth e analyte s ofinterest

. Fiel d matri xspik e concentration s mus

t b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike

. Fiel d matri xspike s ar e presente d i n sectio n 9 ofthi s report

. Tabl e 9

. Fiel d Matri xSpik e Levels

. Samplin g Locatio n 136R , 137R , 137s , 137 L 138 L
130L , 131L , 132 U 133R , 134S , 134 U 136S'^ ' 130 R 130S , 131S , 132R , 132 S 133S , 133 U 135S , 135L<^

\ 136 U 138 S '^' , 138 R
131R , 134R , 135 R
Tri p Blan k Spik e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h PFBS , ng/m L

0.102 1.0 2 10. 2 1.0 2 10, 2 10 2 10, 2 10 2 102 0 102 102 0 1,0 2 10. 2 10 2 102 0 PFHS , ng/m L

0.103 1.0 3 10. 3 1.0 3 10. 3 103 10, 3 103 1030 103 1030 1,0 3 10, 3 103 1030 PFOS , ng/m L

0.102 1,0 2 10. 2 1,0 2 10, 2 10 2 10, 2 10 2 102 0 10 2 1020 1,0 2 10, 2 10 2 102 0 (1 ) On e ofth e spike d bottle s i n thi s samplin g set was overfille d b ymor e tha n 10% , Th e fiel d matri xspilc e tru e valu e ha

s bee n adjuste d accordingly

.

- (Sample Concentrationof FM S - Average Concentration : FieldSampl e & Fiel dSampl e Dup. ) Spik e Concentraton 00 %

9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d fiel d matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blanks

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

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

. Fiel d matri xspik

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

Pag e 1 9 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

DA L 1 SO

L - Th e recover

yofth e hig h FM S sampl e fo rPFO S was 54.8%

. Th e mi d spik e wa s no t calculate d sinc e th e detecte d concentratio n wa s lO xhighe rtha n th e expecte d concentration

. Th e analytica l uncertaint

yhas bee n adjuste d fo rPFO S base d o n th e recover yofth e hig h FM S t o 100 % ± 45%

. DA L 132 L - Th e hig h FM S spik e leve l a t 10 2 ng/m L wa s no

t a n appropriat e spik

e leve l t o sufficientl y evaluat e PFO S recovery
. DA L 134 L - Th e hig h FM S spik e leve l a t 10 2 ng/m L wa s no

t a n appropriat e spik

e leve l t o sufficientl y evaluat e PFO S recovery
. DA L 135 L - Th e recover

yo fth e mi d FM S sampl e fo rPFO S was 68.2%

. Th e hig h FM S sampl e di d meet metho d acceptance criteri a wit h a recover yo f91.1%

. Th e mi d spik

e was th e mos

t appropriat e spike leve l a s compare d t o th e sampl e concentration , however , n o adjustmen t wil l b e mad e t o th e analytica l uncertaint

yas th e metho d uncertaint yfo rPFO S i s 100 % ±37%

. DA L 136 L - Th e recover

yofth e mi d FM S sampl e fo rPFO S wa s 65.6%

. Th e hig h FM S sampl e di d meet metho d acceptance criteri a wit h a recover yof79.4%

. Th e mi d spik e wa s th e mos

t appropriat e spik e leve l a s compare d t o th e sampl e concentration , however , n o adjustmen t wil l b e mad e t o th e analytica l uncertaint

ya s th e metho d uncertaint yfo rPFO S i s 100 % ±37%

. DA L 137 L - Th e recover

yofth e lo wFM S sampl e fo rPFH S wa s 149%

. Th e mi d an d hig h FM S sample s di d mee

t metho d acceptance criteri a wit h recoverie s of119 % an d 103% , respectively

. Th e sample s contai n trac e PFH S belowth e metho d LO Q of0.10 3 ng/mL , whic h most likel yaccounts fo rth e hig h recover

yofth e lo wFM S sampl e (spik

e leve l 0.10 3 ng/mL)

. Since th e mi d FM S me t metho d acceptance criteria , an d wa s a n appropriat e spik e leve l as compare d t o th e sampl e concentration , n o adjustmen t wil l b e mad e t o th e analytica l uncertainty

. DA L 137 S - Th e recover yofth e lo wFM S sampl e fo rPFH S wa s 186%

. Th e mi d an d hig h FM S sample s di d mee

t metho d acceptance criteri a wit h recoverie s of123 % an d 108% , respectively

. Th e sample s contai n PFH S jus t belowth e metho d LOO of0.10 3 ng/mL , whic h mos t likel yaccounts fo rth e hig h recover

yo fth e lo wFM S sampl e (spik

e leve l 0.10 3 ng/mL)

. Since th e mi d FM S me t metho d acceptance criteria , an d wa s a n appropriat e spik e leve l a s compare d t o th e sampl e concentration , n o adjustmen t wil l b e mad e t o th e analytica l uncertainty

. Th e recover yofth e mi d FM S sampl e fo rPFO S wa s 61.5%

. Th e hig h FM S sampl e di d mee t metho d acceptance criteri a wit h a recover yo f83.9%

. Since th e mi d spike wa s th e most appropriat e spik e leve l as compare d t o th e sampl e concentration , th e analytica l uncertaint

yhas bee n adjuste d fo rPFO S t o 100 % ±38%

. DA L 1 SS L - Th e recover yofth e lo wFM S sampl e fo rPFH S was 203%

. Th e mi d an d hig h FM S sample s di d meet metho d acceptance criteri a wit h recoverie s of124 % an d 101% , respectively

. Th e sample s contai n PFH S jus t belo wth e metho d LOQ of0.10 3 ng/mL , whic h mos t likel yaccounts fo rth e hig h recover

yo fth e lo wFM S sampl e (spik

e leve l 0.10 3 ng/mL)

. Since th e mi d FM S me t metho d acceptance criteria , an d wa s a n appropriat e spik e leve l as compare d t o th e sampl e concentration , n o adjustmen t wil l b e mad e t o th e analytica l uncertainty

.

Pag e 2 0 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 10

. DA L 130 R Q 2 Y1 0 S F (Sample d 7/1/10 )

3MUMSI D GLP10-01-02-07-00 1 GLP10-01-02-07-00 2 GLP10-01-02-07-00 3 GLP10-01-02-07-00 4 GLP10-01-02-07-00 5 Descriptio n DAL130RQ2Y1 0 SF O DAL130RQ2Y1 0 S F 1 DAL130RQ2Y1 0 S F LS DAL130RQ2Y1 0 S F M S DAL130RQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRPD PFB S Concentratio n (ng/mL ) 16. 5 16. 7 27. 4 NA<^ ' NA<^ > YoRecover

y N A N A 10 6 NA<^ ' NA*^ ' 16. 6 ng/m L ±1.2Y

o PFH S Concentratio n (ng/mL ) 11 9 11 9 13 0 21 8 97 9 YoRecover

y N A N A N C 96. 1 83. 5 11 9 ng/m L tO.OY

o PFO S Concentratio n (ng/mL ) 55 4 50 9 49 8 59 8 135 0 YoRecover

y N A N A N C N C 79. 9 53 2 ng/m L ±8.5Y

o NA= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:10 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s th e spike leve l wa

s no t appropriate as compare d t o th e sampl e concentrations

.

Pag e 2 1 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 11

. DA L 1S0 L Q2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GLP10-01-02-07-01 1 GLP10-01-02-07-01 2 GLP10-01-02-07-01 3 GLP10-01-02-07-01 4 GL P 10-01-02-07-01 5 Averag e Concent i Descriptio n

DAL130LQ2Y1 0 SF O DAL130LQ2Y1 0 S F 1 DAL130LQ2Y1 0 S F LS DAL130LQ2Y1 0 S F M S DAL130LQ2Y1 0 S F H S ratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 1,5 1 1.5 4 2.6 1 46 3 13 0 YoRecover

y N A N A 10 6 NA'^ ' 12 6 1.5 3 ng/m L ±2.0Y

o PFH S Concentratio n (ng/mL ) 12. 9 13. 1 14. 1 43 2 134 %Recover

y N A N A N C NA(^ ' 11 7 13. 0 ng/m L ±1.5Y

o PFO S Concentratio n (ng/mL ) 75. 2 73. 5 75. 2 47 6 13 0 XRecover y

N A N A N C NA<^ ' 54.8'^ ' 74. 4 ng/m L ±2.3Yo'^

> NA= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spik e level

. PFBS , PFHS , an d PFO S wer e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. (1 ) Suspec

t th e sampl e bottl e wa

s prepare d i n correc^tly

. Th e M S concentratio n detecte d i s no t consisten t wit h th e spik

e leve l (nomina l concentratio n o f1 0 ng/mL)

. (2 ) Th e fiel d matri xspik

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

. (3) Th e analytica l uncertaint yfo rPFO S has bee n adjuste d fo rFM S recover yt o 100 % ±45%

.

Pag e 2 2 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 12

. DA L 1S0 S Q 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GLP10-01-02-07-00 6 GLP10-01-02-07-00 7 GLP10-01-02-07-00 8 GLP10-01-02-07-00 9 GLP10-01-02-07-01 0 Averag e Concen t Descriptio n

DAL130SQ2Y1 0 SF O DAL130SQ2Y1 0 S F 1 DAL130SQ2Y1 0 S F LS DAL130SQ2Y1 0 S F M S DAL130SQ2Y1 0 S F H S Titio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 3.5 3 3.6 0 14. 0 NA'^ ' NA'^ ' YoRecover y

N A N A 102 NA<^ ' NA<^ ' 3.5 7 ng/m L ±2.(y'/o PFH S Concentratio n (ng/mL ) 11. 1 13. 0 22. 9 11 3 92 4 YoRecover y

N A N A 105 98. 0 88. 5 12. 1 ng/m L ±16Y

o PFO S

Concentratio n (ng/mL ) 72. 3 71. 8 84. 5 15 2 93 7 YoRecover y

N A N A N C 78. 2 84. 8 72. 1 ng/m L ±0.69Y o N A= No t /Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:10 0 diluton

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s th e spike leve l was no

t appropriate as compare d t o th e sampl e concentrations

. Tabl e 13

. DA L 131 R Q 2 Y1 0 S F (Sample d 7/1/10 )

3MUMSI D GLP10-01-02-07-01 6 GLP10-01-02-07-01 7 GLP10-01-02-07-01 8 GLP10-01-02-07-01 9 Descriptio n DAL131RQ2Y1 0 SF O DAL131RQ2Y1 0 S F 1 DAL131RQ2Y1 0 S F LS DAL131RQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) t YoRP D PFB S Concentratio n (ng/mL ) 74. 9 75. 3 17 9 NA<^ > YoRecover y

N A N A 10 2 NA<^ ' 75. 1 ng/m L ±0.53Y o PFH S Concentratio n (ng/mL ) 34 3 34 7 44 7 116 0 YoRecover y

N A N A N C 79. 1 34 5 ng/m L ±1.2Y o PFO S Concentratio n (ng/mL ) 171 0 173 0 182 0 243 0 YoRecover y

N A N A N C 69. 8 172 0 ng/m L ±1.4Y o N A= No t /Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1 ;10 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d as th e spike leve l was no t appropriate as compare d t o tfi e sampl e concentrations

.

Pag e 2 3 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o f PFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 14

. DA L 1S1 L 0 2 Y1 0 S F (Sample d 6/30/10 )

3 M LIM S I D GLP10-01-02-07-02 5 GLP10-01-02-07-02 6 GLP10-01-02-07-02 7 GLP10-01-02-07-02 8 GL P 10-01-02-07-02 9 Descriptio n DAL131LQ2Y1 0 SF O DAL131LQ2Y1 0 S F 1 DAL131LQ2Y1 0 S F L S DAL131LQ2Y1 0 S F M S DAL131LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 2.8 4 3.0 4 4.1 8 13. 2 88. 4 YoRecover y

N A N A N C 10 1 83. 8 2.9 4 ng/m L ±6.8 % PFH S Concentratio n (ng/mL ) 18. 9 19. 6 20. 7 30. 2 10 4 YoRecover y

N A N A N C 10 6 82. 3 19. 3 ng/m L ±3.6Y o PFO S Concentratio n (ng/mL ) 33. 9 33. 4 34. 9 43. 9 11 2 YoRecover y

N A N A N C N C 76. 9 33. 6 ng/m L ±1.6Y o N A= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2 xtti e spik e level

. PFBS , PFHS , an d PFO S wer e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. (1 ) Adilutio n ofth e sampl e was no t prepare d as th e spik

e leve l wa

s not appropriate as compare d t o th e sampl e concentrations

. Tabl e 15

. DA L ISI S Q 2 Y1 0 S F (Sample d 6/S0/10 )

3 M LIM S I D GLP10-01-02-07-02 0 GLP10-01-02-07-02 1 GLP10-01-02-07-02 2 GLP10-01-02-07-02 3 GLP10-01-02-07-02 4 Averag e Concent i Descriptio n

DAL131SQ2Y1 0 SF O DAL131SQ2Y1 0 S F 1 DAL131SQ2Y1 0 S F L S DAL131SQ2Y1 0 S F M S DAL131SQ2Y1 0 S F H S •atfo n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 1.0 6 1.0 5 11. 0 NA<^ ' NA'^ > YoRecover y

N A N A 97. 5 NA<^ ' NA<^ ' 1.0 6 ng/m L ±0.95Y o PFH S Concentratio n (ng/mL ) 5.5 3 5.4 5 14. 3 NA<^ ' NA<^ ' YoRecover y

N A N A 85. 5 NA<^ > NA<^ ' 5.4 9 ng/m L ±1.5Y o PFO S Concerrtratio n (ng/mL ) 8.4 1 8.0 9 18. 2 NA(^ > NA*^ ' YoRecover y

N A N A 97. 5 NA<^ ' NA'^ ' 8.2 5 ng/m L ±3.9Y o N A= No t Applicabl e PFBS , PFHS , an d PFO S wer e analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s th e spik e leve l wa s no

t appropriate as compare d t o th e sampl e concentrations

.

Pag e 2 4 o f 6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 16

. DA L 1S2 R Q 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GL P 10-01-02-07-03 0 GLP10-01-02-07-03 1 GLP10-01-02-07-03 2 GL P 10-01-02-07-03 3 GLP10-01-02-07-03 4 Descriptio n DAL132RQ2Y1 0 SF O DAL132RQ2Y1 0 S F 1 DAL132RQ2Y1 0 S F LS DAL132RQ2Y1 0 S F M S DAL132RQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 7,6 0 7.6 8 17. 5 NA<^ ' NA'^ ' YoRecover y

N A N A 96. 7 NA<^ > NA<^ ' 7.6 4 ng/m L ±1.0Y o PFHSf^ > Concentratio n (ng/mL ) 36. 3 35. 6 44. 8 13 3 86 5 YoRecover y

N A N A N C 94. 2 80. 5 36. 0 ng/m L ±1.9Y o PFO S Concentratio n (ng/mL ) 26 2 26 4 27 4 33 3 107 0 YoRecover y

N A N A N C N C 79. 3 26 3 ng/m L ±0.76Y o NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S were analyze d o n 7/15/1 0 wit h a 1:10 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s not prepare d a s th e spik e leve l wa s no

t appropriate a

s compare d t o th e sampl e concentrations

. Tabl e 17

. DA L 132 L Q 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GL P 10-01-02-07-04 0 GL P 10-01-02-07-04 1 GLP10-01-02-07-04 2 GLP10-01-02-07-04 3 GL P 10-01-02-07-04 4 Descriptio n DAL132LQ2Y1 0 SF O DAL132LQ2Y1 0 S F 1 DAL132LQ2Y1 0 S F LS DAL132LQ2Y1 0 S F M S DAL132LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 10. 3 9.7 8 11. 2 18. 9 10 2 YoRecover y

N A N A N C 86. 9 90. 2 10. 0 ng/m L ±5.2Y o PFH S Concentratio n (ng/mL ) 76. 7 79. 6 79. 7 84. 9 17 7 YoRecover y

N A N A N C N C 96. 0 78. 2 ng/m L ±3.r/ o PFO S Concentratio n (ng/mL ) 23 8 24 3 25 7 27 0 37 9 YoRecover y

N A N A N C N C N C 24 0 ng/m L tZIYo'^ ' N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

. PFBS , PFHS , an d PFO S wer e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. (1 ) Samplin g locatio n di d no t have a n appropriate FM S spik e leve l t o sufficientl yevaluat e PFO S recovery
.

Pag e 2 5 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 18

. DA L 1S2 S Q 2 Y1 0 S F (Sample d 7/1/10 )

3MUIVISI D GLP10-01-02-07-03 5 GLP10-01-02-07-03 6 GLP10-01-02-07-03 7 GLP10-01-02-07-03 8 GLP10-01-02-07-03 9 Averag e Concent i Descriptio n

DAL132SQ2Y1 0 SF O DAL132SQ2Y1 0 S F 1 DAL132SQ2Y1 0 S F LS DAL132SQ2Y1 0 S F M S DAL132SQ2Y1 0 S F H S -atfo n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 31. 8 33. 4 44. 8 13 5 NA*^ ' YoRecover

y NA NA N C 10 0 NA'^ ' 32.6ng/mL±4.9Y o PFH S Concentratio n (ng/mL ) 21 1 21 1 21 3 28 7 110 0 YoRecover

y N A N A N C N C 86. 3 21 1 ng/m L ±0.0Y

o PFO S Concentratio n (ng/mL ) 86 3 85 8 82 5 87 3 166 0 YoRecover

y N A N A N C N C 77. 9 86 1 ng/m L ±0.58Y

o NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:10 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n o fth e sampl e wa s no t prepare d as th e spik

e leve l wa s no

t appropriate as compare d t o th e sampl e concentrations

. Tabl e 19

. DA L 1SS R Q 2 Y1 0 S F (Sample d 7/1/10 )

3MUMSI D GLP10-01-02-07-04 5 GLP10-01-02-07-04 6 GL P 10-01-02-07-04 7 GLP10-01-02-07-04 8 GLP10-01-02-07-04 9 Descriptio n DAL133RQ2Y1 0 SF O DAL133RQ2Y1 0 S F 1 DAL133RQ2Y1 0 S F LS DAL133RQ2Y1 0 S F M S DAL133RQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 7.7 8 7.6 2 8.8 7 18. 2 NA<^ ' YoRecover

y N A N A N C 10 3 NA'^ ' 7.70ng/mL±2.1Y o PFH S Concentratio n (ng/mL ) 45. 8 45. 3 44. 6 52. 9 12 8 YoRecover

y N A N A N C N C 80. 0 45. 6 ng/m L ±1. 1 Y

o PFO S Concentratio n (ng/mL ) 73. 9 81. 0 71. 0 84. 2 16 0 YoRecover

y N A N A N C N C 80. 9 77. 5 ng/m L ±9.2Y

o NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d as tti e spik

e leve l was no

t appropriate as compare d t o th e sampl e concentrations

.

Pag e 2 6 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 20

. DA L 133 L Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GL P 10-01-02-07-05 5 GLP10-01-02-07-05 6 GLP10-01-02-07-05 7 GLP10-01-02-07-05 8 GLP10-01-02-07-05 9 Averag e Concent i Descriptio n

DAL132LQ2Y1 0 SF O DAL132LQ2Y1 0 S F 1 DAL132LQ2Y1 0 S F LS DAL132LQ2Y1 0 S F M S DAL132LQ2Y1 0 S F H S •atio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 6.8 1 6.6 8 16. 7 NA'^ ' NA<^ ' YoRecover

y N A N A 97. 6 NA<^' NA'^ ' 6.7 5 ng/m L ±1.9Y

o PFH S Concentratio n (ng/mL ) 39. 5 39. 2 48. 3 14 5 91 4 YoRecover

y N A N A N C 103 84. 9 39. 4 ng/m L ±0.76Y

o PFO S Concentratio n (ng/mL ) 13 9 14 9 16 1 27 4 103 0 YoRecover

y N A N A N C 12 8 86. 8 144 ng/m L ±7.6% NA = No t Applicabl e N C = Not Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFOS wer

e analyze d o n 7/15/1 0 wit h a 1:5 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n o

fth e sampl e was no

t prepare d as th e spik

e leve l was no

t appropriate a

s compare d t o th e sampl e concentrations

. Tabl e 21

. DA L 1SSS 0 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GLP10-01-02-07-05 0 GLP10-01-02-07-05 1 GLP10-01-02-07-05 2 GLP10-01-02-07-05 3 GLP10-01-02-07-05 4 Descriptio n DAL133SQ2Y1 0 SF O DAL133SQ2Y1 0 S F 1 DAL133SQ2Y1 0 S F LS DAL133SQ2Y1 0 S F M S DAL133SQ2Y1 0 S F H S Averag e Concerrtratio n (ng/mL ) ±YoRP D PFB S Concerrtratio n (ng/mL ) 12. 6 12. 7 21. 8 NA<^ > NA<^ > YoRecover

y N A N A 89. 7 NA'^ ' NA'^ ' 12. 7 ng/m L ±0.79Y

o PFH S Concentratio n (ng/mL ) 75. 5 78. 7 89. 5 173 99 0 YoRecover

y N A N A N C 93. 1 88. 6 77. 1 ng/m L ±4.2Y

o PFO S Concentratio n (ng/mL ) 22 1 23 4 23 0 33 7 118 0 YoRecover

y N A N A N C 10 7 93. 2 22 8 ng/m L ±5.4Y

o NA= Not /Applicabl e N C = Not Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFOS were analyze d o n 7/15/1 0 wit h a 1:5 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e was no t prepare d a

s th e spik e leve l was no

t appropriate a

s compare d t o th e sampl e concentrations

.

Pag e 2 7 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 22

. DA L 134 R Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-06 0 GLP10-01-02-07-06 1 GLP10-01-02-07-06 2 GLP10-01-02-07-06 3 Descriptio n DAL134RQ2Y1 0 SF O DAL134RQ2Y1 0 S F 1 DAL134RQ2Y1 0 S F LS DAL134RQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) + YoRP D PFB S Concentratio n (ng/mL ) 58. 6 59. 6 15 7 NA<^ ' YoRecover

y N A N A 96. 0 NA<^ ' 59. 1 ng/m L ±I.V/

o PFH S Concentratio n (ng/mL ) 43 6 44 6 52 1 127 0 YoRecover

y N A N A N C 80. 5 44 1 ng/m L ±2.3Y

o PFO S Concentratio n (ng/mL ) 117 0 119 0 114 0 190 0 YoRecover

y N A N A N C 70. 3 1180ng/mL±2.3Y o N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 vwt h a 1:10 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s th e spik e leve l was no

t appropriate a s compare d t o th e sampl e concentrations

. Tabl e 23

. DA L 134 L Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-07 5 GLP10-01-02-07-07 6 GLP10-01-02-07-07 7 GLP10-01-02-07-07 8 GLP10-01-02-07-07 9 Descriptio n DAL134LQ2Y1 0 SF O DAL134LQ2Y1 0 S F 1 DAL134LQ2Y1 0 S F LS DAL134LQ2Y1 0 S F M S DAL134LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 12. 7 12. 8 13. 8 22. 5 NA(^ > YoRecover

y NA NA N C 95. 6 NA<^ ' 12. 8 ng/m L ±0.78Y

o PFH S Concentratio n (ng/mL ) 10 7 10 5 10 7 11 2 18 4 YoRecover

y N A N A N C N C 75. 7 106 ng/m L ±1.9Y

o PFO S Concerrtratio n (ng/mL ) 48 4 49 7 50 3 47 0 53 5 YoRecover

y N A N A N C N C N C 49 1 ng/m L ±2.^/0^^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s tti e spik e leve l was no

t appropriate as compare d t o th e sampl e concentrations

. (2 ) Samplin g locatio n di d no t hav e a n appropriate FM S spik e leve l t o suflicientl yevaluat e PFO S recovery
.

Pag e 2 8 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 24

. DA L 134 S Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-07 0 GLP10-01-02-07-07 1 GLP10-01-02-07-07 2 GLP10-01-02-07-07 3 GL P 10-01-02-07-07 4 Descriptio n DAL134SQ2Y1 0 SF O DAL134SQ2Y1 0 S F 1 DAL134SQ2Y1 0 S F L S DAL134SQ2Y1 0 S F M S DAL134SQ2Y1 0 S F H S Averag e Concerrtratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 0,10 0 0,087 6 1,2 1 10. 9 87. 8 YoRecover

y N A N A 10 9 10 6 86. 0 0.093 8 ng/m L ±13Y

o PFH S Concentratio n (ng/mL ) 1.37 1.2 9 2.4 3 12. 7 91. 4 YoRecover

y N A N A 107 11 0 87. 4 1.3 3 ng/m L ±6.0Y

o PFO S Concentratio n (ng/mL ) 13. 1 12. 2 13. 1 23. 4 10 1 YoRecover

y N A N A N C 10 6 86. 3 12. 6 ng/m L ±7.2Y

o NA = Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFBS , PFH S an d PFO S wer e analyze d o n 7/15/1 0 wit h a 1:5 dilution

. (1 ) Adilutio n ofth e sampl e was no t prepare d a

s th e spik e leve l was no

t appropriate a

s compare d t o th e sampl e concentrations

. Tabl e 25

. DA L 1S5 R Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-06 4 GLP10-01-02-07-06 5 GLP10-01-02-07-06 6 GLP10-01-02-07-06 7 Descriptio n DAL135RQ2Y1 0 SF O DAL135RQ2Y1 0 S F 1 DAL135RQ2Y1 0 S F LS DAL135RQ2Y1 0 S F H S Averag e Concerrtratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 82. 8 83. 2 18 5 NA<^ ' YoRecover

y N A N A 10 0 NA<^ ' 83. 0 ng/m L ±0.48Y

o PFH S Concentratio n (ng/mL ) 76 1 74 7 85 3 161 0 YoRecover

y N A N A N C 83. 1 754 ng/m L ±1.9Y

o PFO S Concentratio n (ng/mL) ^ 103 0 105 0 119 0 189 0 YoRecover

y N A N A N C 83. 2 1040 ng/m L ±1.8Y

o N A= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFOS were analyze d o n 7/15/1 0 wit h a 1:100 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e vra s not prepare d as tti e spik e leve l wra

s no t appropriate as compare d t o th e sampl e concentrations

.

Pag e 2 9 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 26

. DA L 1S5 L Q2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-08 5 GLP10-01-02-07-08 6 GLP10-01-02-07-08 7 GLP10-01-02-07-08 8 GLP10-01-02-07-08 9 Descriptio n DAL135LQ2Y1 0 SF O DAL135LQ2Y1 0 S F 1 DAL135LQ2Y1 0 S F L S DAL135LQ2Y1 0 S F M S DAL135LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 6.3 8 6.3 4 15. 6 NA'^ ' NA'^ ' YoRecover y

N A N A 90. 6 NA'^ ' NA<^ ' 6.3 6 ng/m L ±0.63Y o PFH S Concentratio n (ng/mL ) 36. 3 39. 5 49. 6 13 2 92 2 YoRecover y

N A N A N C 10 3 85. 8 37. 9 ng/m L ±8.4Y o PFO S Concentratio n (ng/mL ) 52. 6 58. 1 62. 2 11 7 98 5 YoRecover y

N A N A N C 68. 2 <^ ' 91. 1 55. 4 ng/m L ±9.9Y o NA= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S were analyze d o n 7/15/1 0 v«it h a 1:100 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s not prepare d as th e spik e leve l wa s no

t appropriate a

s compare d t o th e sampl e concentrations

. (2 ) Th e fiel d matri xspik e di d no t meet method acceptance criteri a of100 % ±30%

. Tabl e 27

. DA L 1S5 S Q 2 Y1 0 S F (Sample d 7/2/10 )

3 M LIM S I D GLP10-01-02-07-08 0 GLP10-01-02-07-08 1 GLP10-01-02-07-08 2 GLP10-01-02-07-08 3 GL P 10-01-02-07-08 4 Descriptio n DAL135SQ2Y1 0 SF O DAL135SQ2Y1 0 S F 1 DAL135SQ2Y1 0 S F L S DAL135SQ2Y1 0 S F M S DAL135SQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concerrtratio n (ng/mL ) 0.74 8 0.72 2 11. 0 NA'^ ' NA<^ ' YoRecover y

N A N A 10 1 NA'^ ' NA'^ ' 0.73 5 ng/m L ±3.5Y o PFH S Concentratio n (ng/mL ) 5.7 2 6.0 4 15. 2 NA'^ > NA'^ ' %Recover y

N A N A 90. 5 NA<^ > NA'^ ' 5.8 8 ng/m L ±5.4Y o PFO S Concentratio n (ng/mL ) 6.8 7 7.4 5 16. 5 NA<^ ' NA(^> YoRecover y

N A N A 91. 6 NA(^ ' NA<^ ' 7.1 6 ng/m L ±8.1Y o NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFBS , PFH S an d PFO S wer e analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d as tti e spik

e leve l wa s no

t appropriate as compare d t o th e sampl e concentrations

.

Pag e 3 0 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o f PFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 28

. DA L 1S6LQ2Y1 0 S F (6/30/10 )

3 M LIM S I D GLP10-01-02-07-09 5 GLP10-01-02-07-09 6 GLP10-01-02-07-09 7 GLP10-01-02-07-09 8 GLP10-01-02-07-09 9 Descriptio n DAL136LQ2Y1 0 SF O DAL136LQ2Y1 0 S F 1 DAL136LQ2Y1 0 S F L S DAL136LQ2Y1 0 S F M S DAL136LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 2.9 6 2.8 5 13. 7 NA<^ ' NA<^ > YoRecover y

N A N A 10 6 NA'^ > NA'^ ' 2.9 1 ng/m L ±3.8Y o PFH S Concentratio n (ng/mL ) 11. 8 11. 5 20. 7 10 8 85 6 YoRecover y

N A N A 87. 9 93. 5 82. 0 11. 7 ng/m L ±2.6Y o PFO S Concentratio n (ng/mL ) 87. 7 91. 6 93. 8 15 7 89 9 YoRecover y

N A N A N C 65. 6 '^ > 79. 4 89. 7 ng/m L ±4.4Y o HA

. = No t /Vpplicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFOS were analyze d o n 7/15/1 0 wit h a 1:5 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s tti e spike leve l wa s no

t appropriate a s compare d t o th e sampl e concentrations

. (2 ) Th e fiel d matri xspike di d no t mee t method acceptance criteria

. Tabl e 29

. DA L 1S6 S Q2 Y1 0 S F (Sample d 6/S0/10 )

3 M LIM S I D GLP10-01-02-07-09 0 GLP10-01-02-07-09 1 GLP10-01-02-07-09 2 GLP10-01-02-07-09 3 GLP10-01-02-07-09 4 Descriptio n DAL136SQ2Y1 0 SF O DAL136SQ2Y1 0 S F 1 DAL136SQ2Y1 0 S F L S DAL136SQ2Y1 0 S F M S DAL136SQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 3.4 7 3.5 1 4.7 8 14. 1 NA<^ ' YoRecover y

N A N A N C 10 4 NA'^ ' 3.4 9 ng/m L ±1.1Y o PFH S Concentratio n (ng/mL ) 19. 2 19. 4 20. 0 29. 1 98. 8 YoRecover y

N A N A N C 95. 1 85. 7 19. 3 ng/m L ±1.0Y o PFO S Concerrtratio n (ng/mL ) 10 3 10 9 11 0 11 0 18 3 YoRecover y

N A N A N C N C 83. 9 10 6 ng/m L ±6.0Y o NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFOS wer

e analyze d o n 7/15/1 0 wit h a 1:1 0 dilution

. PFB S was analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d as tti e spike leve l wa s no t appropriate as compare d t o th e sampl e concentrations

.

Pag e 3 1 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 /Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 30

. DA L 137 L Q 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GLP10-01-02-07-10 5 GLP10-01-02-07-10 6 GLP10-01-02-07-10 7 GLP10-01-02-07-10 8 GLP10-01-02-07-10 9 Descriptio n DAL137LQ2Y1 0 SF O DAL137LQ2Y1 0 S F 1 DAL137LQ2Y1 0 S F L S DAL137LQ2Y1 0 S F M S DAL137LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 0.091 4 0.078 0 0.20 3 1.2 1 10. 6 YoRecover y

N A N A 11 6 11 0 10 3 0.084 7 ng/m L ±16 % PFH S Concerrtratio n (ng/mL ) <0.10 3 <0.10 3 0.15 3 1.2 3 10. 6 YoRecover y

N A N A 14 9 <^ > 11 9 10 3 <0.10 3 ng/m L PFO S Concerrtratio n (ng/mL ) 0.68 4 0.78 4 0.88 6 1.8 5 10. 6 YoRecover y

N A N A N C 10 9 96. 5 0.73 4 ng/mL±14Y o N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFBS , PFH S an d PFO S wer e analyze d o n 7/15/1 0 withou t dilution

. (1 ) Th e field matri xspik e di d no t meet metho d acceptance criteria

. Tabl e 31

. DA L 1S7S Q 2 Y1 0 S F (Sample d 7/1/10 )

3 M LIM S I D GLP10-01-02-07-10 0 GLP10-01-02-07-10 1 GLP10-01-02-07-10 2 GLP10-01-02-07-10 3 GLP10-01-02-07-10 4 Descriptio n DAL137SQ2Y1 0 SF O DAL137SQ2Y1 0 S F 1 DAL137SQ2Y1 0 S F L S DAL137SQ2Y1 0 S F M S DAL137SQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 0.12 3 0.11 4 0.23 2 1.3 8 11. 6 YoRecover y

N A N A 11 1 12 4 11 3 0.11 9 ng/m L ±7.6Y o PFH S Concentratio n (ng/mL ) <0.10 3 <0.10 3 0.19 2 1.2 7 11. 1 YoRecover y

N A N A 18 6 <^ ' 12 3 10 8 <0.10 3 ng/m L PFO S Concerrtratio n (ng/mL ) 0.43 5 0.41 9 0.56 2 1.0 5 8.99

. YoRecover y

N A N A N C 61.5'^ > 83. 9 0.42 7 ng/m L ±3.7Yo ^ N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

. PFBS , PFH S an d PFO S wer e analyze d o n 7/15/1 0 withou t dilution

. (1 ) Th e fiel d matri xspik e di d no t meet metho d acceptance criteria

. (2 ) Th e analytica l uncertaint yfo rPFO S has bee n adjuste d fo rFM S recover yt o 100 % ±38%

.

Pag e 3 2 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 32

. DA L 138 S Q 2 Y1 0 S F (Sample d 6/30/10 )

3 M LIM S I D GLP10-01-02-07-11 0 GLP10-01-02-07-11 1 GLP10-01-02-07-11 2 GLP10-01-02-07-11 3 GLP10-01-02-07-11 4 Averag e Concen t Descriptio n

DAL138SQ2Y1 0 SF O DAL138SQ2Y1 0 S F 1 DAL138SQ2Y1 0 S F LS DAL138SQ2Y1 0 S F M S DAL138SQ2Y1 0 S F H S ratfo n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 5.8 1 5.6 2 15. 5 NA<^ ' NA<^ ' YoRecover

y N A N A 10 6 NA<^ ' NA<^ ' 5.72 ng/m L ±3.3Y

o PFH S Concentratio n (rig/mL ) 17. 0 16. 7 27. 8 11 6 88 8 YoRecover

y N A N A N C 96. 3 84. 6 16. 9 ng/m L ±1.8Y

o PFO S Concentratio n (ng/mL ) 21 6 21 7 24 0 31 9 109 1 YoRecover

y N A N A N C N C 85. 7 21 6 ng/m L ±0.42Y

o NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFH S an d PFO S wer

e analyze d o n 7/15/1 0 wit h a 1:5 0 dilution

. PFB S wa s analyze d o n 9/17/1 0 withou t dilution

. (1 ) Adilutio n ofth e sampl e wa s no t prepare d as tti e spik

e leve l was no

t appropriate as compare d t o th e sampl e concentrations

. Tabl e 33

. DA L 138 L Q 2 Y1 0 S F (Sample d 6/30/10 )

3 M LIM S I D GLP10-01-02-07-11 5 GLP10-01-02-07-11 6 GLP10-01-02-07-11 7 GLP10-01-02-07-11 8 GLP10-01-02-07-11 9 Descriptio n DAL138LQ2Y1 0 SF O DAL138LQ2Y1 0 S F 1 DAL138LQ2Y1 0 S F LS DAL138LQ2Y1 0 S F M S DAL138LQ2Y1 0 S F H S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 0.052 5 0.040 1 0.15 3 1.1 9 11. 2 YoRecover

y N A N A 10 5 11 2 10 9 0.046 3 ng/m L ±2r/o'^

^ PFH S Concentratio n (ng/mL ) <0.10 3 <0.10 3 0.20 9 1.28 10. 4 %Recover

y N A N A 203'^ ' 12 4 10 1 <0.10 3 ng/m L PFO S

Concentratio n (ng/mL ) 0.80 5 0.77 6 0.80 5 1.6 6 9.7 1 YoRecover

y N A N A N C 85. 1 87. 5 0.79 1 ng/m L ±3.7Y

o NA=NotApplicat)l e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. PFBS , PFH S an d PFO S wer e analyze d o n 7/15/1 0 withou t dilution

. (1 ) Th e RP D di d no

t mee t method acceptance criteri a ofs20%

. (2 ) Th e fiel d matri xspik

e di d no t meet metho d acceptance criteria

.

Pag e 3 3 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 34

. Tri p Blan k

3 M LIM S I D GLP10-01-02-07-12 4 GLP10-01-02-07-12 0 GLP10-01-02-07-12 1 GLP10-01-02-07-12 2 GLP10-01-02-07-12 3 Descriptio n Tri p Blan k

Sampl e Tri p Blan k

L S Tri p Blan k

M S Tri p Blan k

MH S Tri p Blan k

H S PFB S

Concentratio n (ng/mL ) <0.030 6 1.3 5 12. 7 11 7 117 0 YoRecover

y N A 132 <^ ' 12 5 11 5 11 5 PFH S

Concentratio n (ng/mL ) <0.10 3 1.22 11. 4 10 8 109 0 YoRecover

y N A 11 8 11 1 105 106 PFO S

Concentratio n (ng/mL ) <0.51 0 1.1 9 11. 6 11 4 90 0 YoRecover

y N A 11 7 11 4 11 2 88. 2 NA = NotApplicatJ e (1 ) Th e field matri xspik e di d no t mee t method acceptance criteria

. Tabl e 35

. Rinseat e Blank s

3 M LIM S I D GLP10-01-02-07-06 8 GLP10-01-02-07-06 9 Descriptio n DAL137LQ2Y10SFR B DAL131RQ2Y10SFR B PFB S Concentratio n (ng/mL ) <0.030 6 <0.030 6 PFH S

Concerrtratio n (ng/mL ) <0.10 3 <0.10 3 PFO S

Concentratio n (ng/mL ) <0.10 2 <0.10 2

Pag e 3 4 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

1 0 Conclusio n Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytic:a 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 # 2 (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 35 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

1 3 Signature s

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

# D'/ocr^-o/o Willia m K

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

( ( 

# 'I d Gar yHohenstein , Sponso rRepresentative Date



# m m Jaisimh a P^sari , Stud yDirecto r Jate

Pag e 3 6 o f6 8GLP10-0 1 -02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t AJune/Jul y201 0 , , . ,. , . ., , „^ „ „ ^ « « Analytica l Protocol : GLP10-01-0 2



### Amendmen

t 0 7

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

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

PROTOCO L AMENDMEN TNO

. 0 7

Amendmen t Date : Jun e 16

. 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 Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r

Pag e 1 o f9 Pag e 3 7 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t AJune/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 7 

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

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

PROTOCO L READS : Sectio n 9.2.1 ; Astabl e isotope-labele d surrogat e [(1,2,3,4-"C4)-PFOS ] wil l als o b e adde d at a fixed leve l t o eac h sample , LMS , LCS , pttfcedura i blank , an d at variabl e know n con(»ntration s i n calibratio n standards , an d quantifie d t o evaluat e surrogat e recoveries

. Astabl e isotope-labele d intema l standard , [(1,2,3,4,5,6,7,8-^^C8)-PFOS ] vA Wb e adde d at a fixed concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n o fPFO S an d th e surrogate

. Astatrfe Isotope-labele d intema l standard , [(^®02)-PFHS ] wil l b e adde d at a fixed concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calitH-atio n standar

d fo raidin g quantitatio n ofPFHS

. Astabl e isotope-labele d intema l standard , [(^®02)-PFBS ] wil l b e adde d at a fixed concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n o fPFBS

.

AMEN D T

O READ : Astabl e isotope-labele d sun-c^ate [(1,2,3,4-"C4)-PFOS ] ma yals o b e adde d a

t a fixed leve l t o eac h sample , LMS , LGS , procedura l blank , an d a t variabl e know n concentration s i n calibratio n standards , an d quantifie d to evaluat e surrogat e recoveries.
Astabl e isotope-labele d intema l standard , {(1,2,3,4,5,6,7,8-"C8)-PFOS j ma yb e adde d a t a fixed oDncentratio n to eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n ofPFO S an d ttie surrogate

. Astabl e isotope-labele d intema l standard , [(^*02)-PFHS ] ma yb e adde d at a fixed concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n ofPFHS

. Astabl e isotope-labele d interna ! standand , [(^*02H'FBS ] ma yb e adde d at a fixed concenti^tio n to eac h sample , LMS

. LCS , procedura l blan k an d calibratio n stahdar

d foraidin g quantitatio n o fPFBS

. Th e us e o fintema l standard s an d sun'ogate ar e onl yappropriat e fo rthos e samplin g location s witi i PFBA , PFHS , an d PFO S concentration s i n th e lo wpp b range
. Prio rto eac h samplin g event , i fpreviousl yobtaine d PFBS

. PFHS , an d PFO S dat a i s availabl e fo rth e samplin g points ofinterest , ttie dat a wil l b e reviewe d t o detennin e i fth e us e ofintema l standard s an d surrogat e i s appropriat e fo rth e curren t samplin g even t

Pag e 2 o f9 Pag e 3 8 o f6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t AJune/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 7
PRoreKO 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 ar e 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 (GLP1O-01-02)

. Th e anticipate d sampl e collectio n wil l occu raroun d th e timeframe o fJun e 21,2010

. 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 yLIM S a s project GLP10-01-01-0 7 an d reporte d a s interi m repor t GLP10-01-02-02 , (reflectin g stud yGLP10-01
- 0 7 an d amendmen t -07)

.

/Reason : Th e reaso n fo rthi s amendmen t i s t o documen t tiie Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t t o b e conducte d fo rth e 3 M Decatur , A L facility

. Th e GP O i s fou rpage s i n lengt h an d include d a s attache d to thi s amendmen t fomi

.

Pag e 3 o f9 Pag e 3 9 o f6 8Attachmen t A GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 7 

## Amendmen t Approva l

^

. 

# (€ / Y J Gar yHohenstein , SponsorRepresentativ e Dat e


## W/'77^^/ ^ Clesto n C

. Lange , Principa l /^alytica l Investigato r Date 

# />Jt^^A^/ 0 Willia m Reagen , EHSpprt s Environmenta l La b Managemen t

Jaisimh a KesarilEEfljEE , Stud yDirecto r Date



### I I Dat

e

Pag e 4 of9 Pag e 4 0 o f6 8Attachmen t A GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 AnalyUca l Protocol : GLP10-01-0 2 Amendmen t 0 7


### 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 ; Environmente 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 : Jun e 16,201 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 0 7 - Fonne rSludg e Incorporatio n Are a (FSIA ) Groundwate r 

## 1 Genera l Project Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numi>e r Projec t Schedule/Tes t Date s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH 3 Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul

. M N 55144-100 0 Phone:(651)737-357 0 oahohenstein(a!mmm.co m 3I 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 wkreaflSD.i3>ri^mm.con 3 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 cclanqe(a!mmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinakffiwestonsolutions.co m Phone : (334)-332-912 3 GLP10-01-02-0 7 Dep t #530711 , Project #002267444 9 Samplin g schedule d fo rth e wee k o fJun e 21,201 0 |
Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein

. Pag e 5 o f9 Pag e 4 1 of6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t AJune/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 7
2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m twenty-seve n groundwate rwell s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) fro m th e Fonne rSludg e Incorporatio n Are a (FSIA)

. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEP ATSC AGoo d Laborator

yPractic e Standard s 4 0 CF R 792

. Groundwate rsample s fro m Decatur , A L wil l b e Collecte d byWesto n Solution s personne l th e wee k ofJun e 21 , 2010

. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFBS , PFHS , an d PFO S ar e o fa know n precisio n an d accuracy
. Th e final 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
- 07

. 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 fJun e 21 , 2010

. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decaturfo ramva l o n FrWay , Jun e 18,2010

. Sampl e bottle s shoul d b e store d refligerate d on-sit e unfi l sampl e collection

. Marti n Smit h \

Westo n Traile r 3 M Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1
4 Tes t Parameter s Th e targeted limi t o fquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS , PFHS , an d PFOS

. Atotal o ftwenty-seve n samplin g location s have bee n specified

. Fo reac h samplin g location , a sample , sampl e duplicat e an d a minimu m o ftw o fiel d matri xspike s wil l b e collected

. Tabl e 1 indicate s th e wel l I D an d correspondin g fiel d sipik

e levels

. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e botti e wil l b e 20 0 mL

. Thre e sets o ftri p blank

s consistin g ofreagent-grad e water , a low-leve l tri p blan k spike , mid-leve l fiel d spike , mid-hig h fiel d spike , an d a high-leve l tiip blan k spike wil l b e prepare d at th e 3 M Environmente l Laborator yan d sen t to th e samplin g locatio n wit h tiie otiie rbotties

. Two additiiana l bottie s wil l b e prepare d t o b e use d fo rtiie preparatio n o fth e equipmen t rinseate blanks

. Atota l o f145 sampl e bottie s wil l b e pnepaned

.

Pag e 6 o f9 Pag e 4 2 o f6 8Attachmen t A GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 7 

### Tabl e 1

. Samplin g Location s an d Fiel d Matri xSpike levels

. Wel l No

. 136R

. 137R

. 137S , 137L

. 138 L 130L

. 131L , 132L , 133R

. 134S , 134L , 136 S 130R.1303,131S,132R , 132S , 133S , 133L , 135S

. 135L , 136L

. 138S

. 138 R 131R

. 134R , 135 R TnpBlankSe t 1,2 , and 3 Sampl e Leve l Low Mi d Hig h Low Mi d Hifl h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h 

### Hig h Spik e Cone

. (ng/mL ) 0. 1 1. 0 1 0 1 1 0 10 0 1 0 10 0 100 0 10 0 100 0 1 1 0 10 0 100 0



### 5 Tes t Method s Sample s wil l b e prepare d an d analyze d byLC/MS/M S followin g ETS-8-044. 0 "Detenninatio n o fPerfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromat(^raphy/Mas s Specbx)metr yDirec t Injectio n Analysis"

. Th e dat e qualit yobjective s fo rtiiese studie s are quantitative results fo rth e target analyte s witi i a n analytica l accurac

yo f100+30% , Fiel d matri xspike s not yieldin g recoverie s witiii n 100+30 % wil l b e addresse d i n ttie repor

t an d th e 1ina

t accurac ystatemen t ma

yb e adjuste d accordingly

. Alternately , sample s mayb e analyze d byET S 8- 1 &4. 3 "Detenninatio n o fPerfluorinate d Acids , Alcohols , Amides , an d SuJfonafes I n Wate rBySoli d Phas e ExtracAo n ari d Hig h Performance Liqui d Chromatography/Mas s Spectiomelry"
- Metiio d ETS-8-15 4 ha s bee n validate d fo rPFO Aan d PFO S only ; however , specifi cqualitycontro l sample s analyze d witi i ttie sample s wil l b e use d t o detennin e overal l metiio d predsio n an d accuracy
. 

### 6 Reportin g Requirement s Fo reac h samplin g location , th e report wil l contai n tiie results fo rtiie sample , sampl e duplicate , an d field matri x spikes

. Tri p blan k

an d tiip blan k

spike s wril l b e reported fo rth e samplin g even t a s wil l an yequipment/rinseat e blank s prepare d i n th e field. Laborator ycontro l spike s o freagen t wate rprepare d at tiie time o fsampl e preparatio n wil l als o b e reported an d use d t o evaluat e tiie overal l metiio d accurac yan d precision

. Metiio d blank s ofreagen t wate rprepare d a t ttie tirne o fsampl e preparatio n wil l b e use d t o detemnin e ttie metiio d detectio n limi t Fo rttiose samplin g location s where ttie field matri xspike leve l wa s no t appropriate , du e t o highe rtiian expecte d analyt e concenttations , a laborator ymatii xspike mayb e prepare d an d vwl l b e include d i n th e final report 

### 7 Emai l Correspondenc e AttadimentA : Samplin g Botti e Request

Pag e 7 o f9 Pag e 4 3 o f6 8Attachmen t A GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/July201 0

. , . , „ , , ^

. ...^ ^ ^ ^ „ „ Analytica l Protocol : GLP10-01-0 2

Amendmen t 0 7

Projec t Duration : 2 1 Jun e throug h 2 Jul y201 0 Dat e Required : 18-Jun-l O

Shi p Container s to : Westo n Solutions , Inc

. Fiel d Offic e 3 M Decatu rPlan t 140 0 Stat e Dock s Roa d Decatur , A l 35S0 1 256-552-618 9 Attn : Marti n Smit h

Sampl e Medi a Groundwate r Sampl e Containe rRequirement s Sample s 2 7 Duplicat e

Sample s n a Rinsat e Blan k

Set s 2 Tri p Blan k

Sets Se e Not e 1
Not e 1 : On e tri p blan k

wil l b e require d fo reac h shippin g containe rreturne d t o th e laboratory

. I t shoul d b e note d tha t ic e wil l b e require d fo rshipment s o fsoi l / sedimen t sample s whic h mayresul t i n a n increas e i n th e numbe ro fshippin g container s (an d tri p blanks ) required

. Not e 2 : Rinsat e Blan k

Sets shoul d b e accompanie d witi i a n appropriat e volum e o fwate rt o accomplis h th e sampling

. Th e volum e shoul d accoun t fo rspillag e durin g th e rinsin g process
. Not e 3 : Pleas e not e tha t an ybottl e set s no t use d du e t o uniqu e fiel d condition s wil l b e isolate d an d returne d t o th e laboratorylabele d fo rdisposal

.

Pag e 8 o f9 Pag e 4 4 o f6 8Attachmen t A GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 ^^^^^^ ^ ^^^^^ ^

GLP10-01-Q 2 Amendmen t 0 7

Well s Include d i n Thi s Samplin g Event : Wel l No . 130 R 13D S 130 L 131 R I31 S 131 L 132 R 132 3 132 L 133 R 133 S 133 L 134 R 134 S 134 L 135 R 135 S 135 L 136 R 136 S 136 L 137 R 137 S 137 1 138 R 138 5 138 L

Pag e 9 o f 9 Pag e 4 5 o

f 6 8'Ollie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

o100715b.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -3.18e+00 3 x'^ 2 + 4.79e+00 5 x+ 6.13e-H00 3 ( r= 0.9997 )
2.7e 7 2.6e 7 2.5e7- ] 2.4e 7 2.3e7
- 2.2e7
- 2.1e7
- 2.0e 7 1.9e 7 1.8e 7 1.7e 7 1.6e7
- 1.5e7
- 1.4e 7 1.3e 7 1.2e 7 1.1e7
- 1.0e7
- 9.0e6
- 8.0e 6 7.0e 6 6.0e6
- 5.0e6
- 4.0e6
- 3.0e 6 2.0e 6 1.0e 6 0.0- ] O

o

/ 

# X

2 5 3 0 3 5 4 0 0 5 1 0 1 5 2 0 4 5 5 0 5 5 6 0 Concentration , ng/m L 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0
*Dat a wock-u p performe d b yST W Pag e 1 o f 1 Printin g Time : 8:40:4 8 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 4 6 of 6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

o100715b.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -2.96e+00 3 x'^ 2 + 5.97e+00 5 x+ 6.69e+00 4 ( r= 0.9993 )

t o c 

### 8
O S 

# 1 o.oe i 3.4e7
- 3.2e7
- 3.0e7
- 2.8e7
- 2.6e7
- 2.4e7
- 2.2e7
- 2.0e7 n 1.8e7
- 1.6e7
- 1.4e7
- 1.2e7
- 1.0e7
- 8.0e6
- 6.0e6
- 4.0e6
- 2.0e6
- 0.0
- 

### / / / /



### / / X ^

- ^



### ' • •^_ „ .^--- ' 

### o

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 6 0 Concentration , ng/m L 6 5 7 0 7 5 8 0 8 5 9 0 9 5 100
*Dat d work-u p performe d b yST W Pag e 1 o f 1 Printin g Time : 8:41:0 8 AM Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 4 7 o

f 6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

^^

. 0100715 b PFO S linear.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -2.28e+00 3 x'^ 2 + 4.74e+00 5 x+ 5.33e+00 4 ( r= 0.9996 )
2.8e 7 2.7e 7 2.6e 7 2.5e 7 2.4e 7 2.3e 7 2.2e7- ] 2.1e 7 2.0e7
- 1.9e7
- 1.8e7
- 1.7e 7 1.6e7- j 1.5e 7 1.4e 7 1.3e7 H 1.2e 7 1.1e 7 1.0e7 ^ 9.0e 6 8.0e 6 7.0e 6 6.0e 6 5.0e6- | 4.0e 6 3.0e6- | 2.0e 6 1.0e6- | 0. 0 O

0 5 1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 6 0 Concentration , ng/m L 6 5 7 0 7 5 8 0 8 5 9 0 9 5 100
*Dat a work-u p performe d b yST W Pag e 1 o f 1 Printin g Time : 8:37:4 5 A M Printin g Date : Monday , Octobe r 25 , Pag e 4 8 of 6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# T San^ b Narr>e : "ol00715b023
- Sampt e ID : "0 8 008-147-10 " Fito : "o100715b.wi r Pea k Name : "PFBS ' Macs(es) : '298.9)98. 9 amu,298.9/79. 9 amu " Commen t "5. 0 pp b curv e poin t i n MiB I Q Vhia fAnrwtalion : " Sair.pl. i IiiJoj; : 2. ' 3an:j;l e Typa : Stinkar d Cuncentraciun : f-

. It ) nq/m L •Talcuiace d Cone : 5.3 4 ng/m L Acq

. DiZe : 7/15/2: ' Acq

. Ti r 0 3 P M 3.7e5
-

3.6a S
3.5e 5
3.4«5
- 3.3e 5
3.2e 5
3.1e 5
3.0e 5
2.9e5
- 2.ea 5 Z7e 5 Z6a5
- Z5e 5 Z4e 5
2.3e5 '
2.2e 5 Z1e 5

. 2-0e 5

e 1.9e5
- I 1,8e 5
1.7e 5
1.6e S
1.5e 5
1.4* 5
1.3a 5
1.2e 5 l.le S
1.0e 5
9.0e 4 S.0» 4
7.0e 4
6.0e4
- 5.0» 4
4.0»4 '
3.0e 4
2.0e 4
1.0e 4

0. 0 1.9e 5
1.8« 5

S S 1.6e 5
1.5e 5
1.4« 5

n.le S
1.0e 5
9.0* 4
8.0e 4
7.0e 4
6.0e 4
S.0e 4
4.0* 4
3.0* 4
Z0» 4
1.0e 4

*Dat a work-u p performe d byST W Pag e 1 o f 4 Printin g Time : 8:40:1 7 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 4 9 o f6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# I SariM * Nam* : *ol00715b060 " SampI * ID : "Sotven t Blan k (MBH Q Etement) " File : "o100715b.wi r Pea k Name : "PFBS " Ma««(*») : -298.9«8. 9 amu,298.9^. 9 amu " Comment'TN10-0237 " Annotation: "

2750

- 2700 265 0 2600

- 255 0 2500 245 0 2400 235 0 2300 225 0 2200

- 215 0 2100 205 0 2000 ! Riilati '

. . Type :

cp s i rain tnln

1950

-

190 0 1850

- 180 0 1750

- 170 0 1650

- 1600

- 1550

- 1500

- 1450

- 1400

- 1350

- 1300

- 125 0 1200

- 1150

- 1100

- 1050

-



## jijM i 

# I Sampt e Nam* : "o100715b09 rSampt e ID : •GLP10-01-01-07-070 ' Fil* : "olDOTISb.vi , Pea k Name : "PFBS " Mass{es) : "298.9/98. 9 amu,298.9/79. 9 amu ' Comment " DAL134SQ2Y10SF0 ' Annotation: " Sampl e Inda^ : S3 Sampl e Type : Unknow n

.-Spli i apo r Larne ; Hin

. Peak

Height : Min

. Peak

Width : jDiOQthin g Width : Expacca dBT : Us e Relativ e RT : I n t Type i 260 0 255 0 250 0 245 0 240 0 235 0 230 0 225 0 2200
- 215 0 210 0 205 0 200 0 195 0 190 0 185 0 180 0 175 0 170 0

150 0 145 0 140 0 135 0 130 0 125 0 120 0 115 0 110 0 105 0 100 0 95 0 90 0 B50
-



### Jto ^Mail , *Dat awork-u p performe db y ST W Pag e 2 o f 4 Pr i Pr i ntin g Time : 8:40:1 8 A M ntin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 0 o f6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interin n Repor t 0 7 Analysi s o f PFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

riG/ti L S.5 1 ng/m L 7/lE/ZOl O

Expe-ta dRT : 14. C m

.T : N o Bas e T o Bas ' : 14. 1 m liioZi i ciiu n

13. 9 ra 14. 3 m 5.7* 5 5.6* 5 5.5* 5 5,4* 5 5.3* 5 5.2* 5 5.1* 5 5.0* 5 4.9e 5 4.8* 5 4.7* 5 4.6* 5 4.5* 5 4.4* 5 4.3* 5 4.2e 5 4.1e 5 4.0e 5 3.9e S 3.ee 5 3.7e 5 3.6e 5 3.5e S 3.4e 5 3.3e 5 3.2e 5 3.1* 5 3.0* 5 2.9e S 2.8* 5 2.7* 5 2.6* 5 2.5* 5 2.4* 5 2.3* 5 2.2* 5 i1* 5 ZOe S 1.9* 5 1.8* 5 1.7*5

- 1.6* 5 1.5* 5 1.4* 5 1.3* 5 1.2*5

. 1.1* 5 1.0e 5 9.0* 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

- 0.0

- 19.0 7 7/16/201 0 2:22:3 1 ti e Intflll i 5. D : 1 a k : ^

0 0 A M
Qu a 0 0 0 . 0 0 . 0 0

Int

. Type : Ratentio n Tirae : Area : 3 Height : Star t Tin,^ : En d TiroG : Bas e T 30837 B F,.^561 1 13

. H

. Sampl e Nam* : "o100715b037 " Sampt e ID : "LCS-100707-5 " P*a k Name : "PFHS " Masc{e«) : "398.9/98. 9 amu,398.9/80. 0 Commen t "5pp b LCS " Annotation : * " Sampl e Type : O C
5.3B 5 5.2B 5 5. 1 e 5 S.Oe S 4.9* 5 4.8e 5 4.7* 5 4.6* 5 4.5* 5 4.4* 5 4.3* 5 4.2* 5 4.1* 5 4.0* 5 3.9* 5 3.8* 5 3.7* 5 3.6e 5 3.5* 5 3.4* 5 3.3* 5 3J* 5 3.1*5

- 3.0*5

- Z9* S 2.8* 5 2.7*5

- 2.6* 5 2.5* 5 2.4* 5 ^3* 5 2.2* 5 2.1*5

- Z0B5

- 1.9e 5 1.8e 5 1.7* 5 1.6e 5 I.Se S 1.4* 5 1.3e 5 1.2e 5 1.1e 5 1.0e 5 9.0* 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 File:"o100715b.wi r amu,398.9/129. 9 amu '

0. 0 -y^

. *Dat a work-u p performe d b yST W Pag e 3 o f

4 Pr i Pr i ntin g Time : 8:40:1 8 A M ntin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 1 o f 6 8*01iie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s from Decatur , A L June/Jul y201 0 

# r San ^

Nama:*o100715b060 ' Sampt e ID : "Solven t 81anlc(MiI[i Q Elam*nt) ' Fite:-o100715b.Mif r Pea k Name : -PFHS " Mass(es) : "398.9/98. 9 amu.398.9/80. 0 amu.39S.9/129. 9 amu " Convnen t "TN10-0237 " Annotation: " Saffip U InisK : 6 0 San.pl * Type : UnKnow n Acq

. ViKB : ftcq. Time ; Hodified : Ptoc

. ftlgorithm: Ncis « PercTflntH'j e Bas«

. jub

. Kind s P2st:-Split

. Fac t Rapcr r Larges t

P Min

. Peak

Heigli t Hin

. Pea t

Vlidtli : :;pi";thin< ] Width : R T Window : Exp«;-.t9 dRT : Us e BsUtiv e RT : Int

. Type : Ratentio nTime : A.'.'s : 7/16/201 0

2:11:0 4 P

H N o IntsliiQu a : S O v : 1.0 0 or : 5 eak : H

o : 0.0 0 0.0 0 3 30. 0 14. 0 N o Bas e To B

a H . O 473 6 co u 

# r Sampt e Nan« : "ol00715b09 rSampt e ID ; "GLP10-01-01-07-070 ' File : "0100715b.vi« r Pea k Name : "PFHS " Mass<es) : "398.9/98. 9 amu.398.9/80. 0 amu,398.9/129. 9 amu ' Commen t "DA L 134SQ2Y1 0 SFO
- AnnotatJon:"
- Saiapl e Typa : Unknow n C-jncnntiation : N/ A Calculata d Core : 1.3 7 nq/r, L Acq

. Pate : 7/17/201 0 Acq

. Time : 1:45 : 1 1 AM Modified : Proc

. Alaorithn, : ] Nois e Percentage : Base

. Jub

. Window : Peak-Split

. Facto r Repor t Larnas t

Pe a Min

. Peak

Height : Min

. Pea

k Width ; Smoothiri' ] Width : R T Window : Expecte dRT : Us e Relativ dBT ! Int

. Type : B Retentio nTittie : H o

ntelliQ'ja n- MQI

I ? 0 1.0 0 mi n ( : N o 0.0 0 cp s 0-0 0 se c 3 p:.i n 30. 0 se c 14. 0 rain N o as e T = Bas e 14. 0 isin Area : 23055 3 count s H-tight : Star t Time : En dTina : 3276 9 cp s

13. 6 rain 14. 2 rain 3.3* 4
3.2* 4
3.1* 4
3.0* 4
Z9e 4
2.8* 4
Z7* 4
2.6* 4
2.5* 4
2.4* 4
2.3* 4
2.2e 4
2.1* 4
2.0* 4
1.9* 4
1.8* 4
1.7e 4
V.6e 4
1.5* 4
1.4* 4
1.3* 4
1.2e 4

1.1B 4
1.0e 4
9000. 0
8000. 0
7000. 0
6000. 0
5000. 0
4000. 0
3000. 0
2000. 0
1000. 0

n o 1 3

13.76v ^

^_M--v ^ .9 7

16.6 f 

## \ J ^ 19.1 8

i

18.B6 J 

## f
I8.59 J
18.36.^ 1

18.08.- /
^ 1 2 1 4 1 6 1 8 *Dat awork-u p performe db y ST W Pag e 4 o f

4 Printin g Time : 8:40:1 8 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 2 of6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 /Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Sampl e Nam*:-01007151)023 " Sampl a ID : t) B 008-147-10
- Fito:-o100715b.w r • Pea k Nama:-PFOS
- Mass(a8):-499.1Sa.9amu.499.1/79.9arnu.499.1/130.0arT«j ' a Carranant : -5. 0 pp b curv a pain t i n Min i Q Watar
- Annotalion : Samp U InJa>: : 2 i

*Dat a work-u p performe d b yST W Pag e 1 o f 3 Printin g Time : 8:36:4 5 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 3 o

f 6 8*011ie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o f PFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L June/Jul y201 0

I SaiTiptoName:"ol00715M5( rSampl e ID : "LCS-100707-14
- Fito : •ol00715b.wf r j,499.1^79.9amu.499.1/13O.0ami r I Pea k

Name : "PFOS
- Massfes):'499.1^98. 9 a I Cammen t "Spp b LC S ECF ' Annotation : " Sampl e Index : 5 0 Sampi « Type : O C Ccncenttatioii : 5.0 0 ng/a l Calculate dCone : 3.7 0 ng/n. L Acq , r^te : 7/16/201 0 Acq

. Time : 5:56:0 0 W I Modified : R T Window : Expecte dRT : Us e Relativ e Int

. Type : Retentio n T i Area : Height : Star t Time : EndTime : Yf- s 30.00 0 1?.39 5 RT : N

o Manual la : 15. J n752S 0 JJ8il5.l } 15. 3 15. f 3.2e 5

3. 1 e 5

3.0e 5

2.9B 5

2.ee 5

2.7e 5

2.6e 5

2.5e 5

2.4e 5

2.3e 5

2.2B 5

2.1e 5

2.0e 5

1.9e S

1.8e 5

1.7e 5

1.6e 5

1.5e 5

1.4e 5

1.3e 5

1.2e 5

l.le S

1.0e 5

9.0e 4

8.0e 4

7.0e 4

6.0e 4

5.0e 4

4.0e 4

3.0e4 '

2.0e 4

1.0e 4 i ;

15.12..

. .3 5 

# I San ^ Name : -o100715b060 " Sampl e ID : "Solven t Blan k (MiOi Q Element rFile : -o10071Sb.wt r Pea k Name : "PFOS * Mass(es) : '499.1/98. 9 amu.499.1/79. 9 amu.499.1/130. 0 afTu T Commen t *TN1tM237 " Annotation:" "

Hodified : R T Kindov : Expecte dRT : Us e Relativ e R

T Int

. Type : Retentio n Tirae : ;;rea : H-ight : Star t Time : Ye s

30.00 0 15.35 3 th : Manual Ib. t 4220 1 ?319.9& 0 15. 3

*DaC a work-u p performe d byST W Pag e 2 o f 3 Printin g Time : 8:36:4 5 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 4 o f 6 8GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS

. an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Printin g Time : 8:36:4 5 A M Printin g Date : Monday , Octobe r 25 , 201 0 Pag e 5 5 o f6 8 *011ie : U0011040 2 Attachmen t B

San^l e Name : "ol00715b093
- Sampt e ID : -GLP1[>01-01-07-070 rFile : "o100715b.wi r • Pea k Name : -PFOS ' Mass(es) : -499.1/98. 9 amu.499.1/79. 9 amu.499.V130. 0 amu " Commen t 'DM

. 134 S 0 2 YI O S F 0 " Annotation : ~ Samplf l impl aTypo :

R TWindO ! Expecte d Us e Rfl U Unl-. i N/A 1.16e S 1.14e 5 1.12a 5 1.10e5

- 1.08e5

- 1.06e 5 1.04e 5 1.02e 5 I.OOe S 9.80e 4 9.60e 4 S.40e 4 9.20e 4 9.00e 4 8.80D 4 8.60e 4 8.40e 4 S.20e 4 8.00e 4 7.S0e 4 7.60e 4 7.40e 4 7.20e 4 7.00e 4 6.80e 4 6.60*4

- 6.40» 4 6.20e 4 8

- 6.00»4 <

' i 5.80e 4

- I 5.60e 4 5.40e 4 5J20e4

- 5.00O 4 4.80e 4 4.60e 4 4.40e 4 4.20e 4 4.00e 4 3.80e 4 3.60e 4 3.40e 4 3.20e 4 3.00e 4 2.60e 4 2.60e 4 2.40e 4 2.20e 4 2.00e 4 1.B0e 4 1.60* 4 1.40e 4 1.20e 4 LOO M 8000.0 0 6000.0 0 4000.0 0 2000.0 0 0.0 0

*Dat a work-u p performe d b yST W Pag e 3 o f 3•Ollie : U0011040 2 Attachmen t B GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# I T Sanvl e Name : "o100715b050 " Sampl e ID : "LCS-100707-14 " FUe : -o100715b.'Mf r Pea k Name : 'PFOS * Massfes) : '499.1/98. 9 amu,499.1/79. 9 amu.499.1/130. 0 emu * Commen t '5pp b LC S ECF " Annotation : ~ 5 0 Sampl e Type : O C Concentration : i.O O r.-j/nL Calculate dCone : 1.9 1 ng/m L Acq

. rate : 7/16/201 0 Acq

. Time : 5:56:0 0 A M

18021 6 cO'J

i lJ2e9S.47 5 H. 9 r Hodi f R T W i E^pe ^ Us aR Int

. Rete n Area : Heig t i e n d t e * 1 T V

t :

^



### f 3.2e 5
3. 1 e S
3.0e S
2.9e 5
2.8e 5
2.7e S
2.6e 5
2.5e 5
2.4e 5
2.3e 5
2.2e 5
2.1* 5
2.0e 5
1.9e 5
1.8« S
1.7e 5
1.6e 5
1.5e 5
1.4e 5
1.3e 5
1.2e 5
l.le S
I.Oe S
9.0* 4
8.0e 4
7.06 4
6.06 4
5.0« 4
4.0e 4
3.0* 4
2.0* 4
1,0e 4 1 5

15.12. ^

14.93.

. 3 5 Sampl e Name : "o100715b09 rSampl e ID : •GLP1(W]1-01-07-O70 ' File:"o100715b.wiff ' Pea k Name : 'PFOS * Massfes) : '499.1/98. 9 amu.499.1/79. 9 anui,499.1/13D. 0 amu " Commen t 'DA L 134 S 0 2 Y1 0 S F 0 " Annotalion: " Sampl e Sampl e Typo : Unk r N/ A

Hodirifd : R T Windo w Exparte d Ua aRela t Int

. Typ e Retentio n J53H S count s 102609.7S B cp s l.lSe S 1.14«5

- 1.12e5 1.10e5

- 1,08e5 1.06e5 1.04* 5 1.02e5 1.00* 5 9.80* 4 9.60* 4 9.40e4 9.20* 4 9.00* 4 8.80e4 8.6064

- 8.40* 4 8.2064 e.00e4 7.8064 7.60e4 7.40* 4 7.20* 4 7.00* 4 6.80* 4 6.60* 4 6.40* 4 6.20* 4 & 6.00* 4
^ 5.80* 4 I 5.60e4 5.40* 4 5.20* 4 5.00* 4 4.80* 4 4.60* 4 4.40e4

- 4.20* 4 4.00* 4 3.80* 4 3.60* 4 3.40* 4 3.20* 4 3.00* 4 2.80* 4 Z60* 4 2.40* 4 2.20* 4 2.00* 4 1.80* 4 1.60*4

- 1.40* 4 1.20* 4 1.00*4

- 8000.0 0 6000.0 0 4000.00 2000.0 0 0.0 0

*Dat a work-u p performe d b yST W Pag e 1 o f

1 Printin g Time : 8:38:5 6 A M Printin g Date : Monday , Octobe r 25 , 2 01 0 Pag e 5 6 o f6 8DocKBiii(ft*0ifjiPo;!rjfitfewnKgi$3ii.o5 fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 0



# 3 M Emronmenfa l L^iorafioi 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^ ^ ^ j

Approve d By : 

## ^/-j/ a • > 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 5 7 o f6 8Doci®:im«K.i!)ioQ;!rjm'grtniE®rMl,o Wcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 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) , Perfluorononanoi cAci d (PFNA) , Perfluorodecanoi cAci d (PFDA) , Perfluoroundecanoi cAci d (PFUnA) , Perfluorododecanoi cAci d (PFDoA) , Perfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) b yHig h Performance Liqui d Chromatograph ycouple d t o a tande m Mass Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples

. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

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

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

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

. Sampl e collectio n i s not covere d unde rthi s analytica l procedure

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

. Sample s containin g heav y particulat e ma

ynot b e suitabl e fo ranalysi s b ythi s method

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

. Thi s i s a performance-base d method

. Metho d accurac yi s determine d fo reac h sampl e set usin g multipl e laborator ycontro l spike s 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 field matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix

. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l no

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

. Fortificatio n level s fo rfield 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 detemnin 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 instrumen t respons e wit h respec t t o analyt e concentration

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

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

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

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

. 3. 3 Fiel d Blan k

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

. Th e purpos e o fth e F B i s t o determin e i ftest substance s o r othe rinterference s are presen t i n th e field 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 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 8 o f6 8Doc«EC)P3!(«tj-ra2ijMbcmiE®i«:'ct.oM'current , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fron i Decatur , A L Attachmen t C June/Jul y201 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 field an d laborator y procedures

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

. 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s o fth e targe t analyte s ar

e adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e field fo rcollectio n o faqueou s samples

. Aknown , specifi cvolum e o f sampl e must b e adde d t o th e sampl e containe rwithou t rinsing

. Thi s ma yb e accomplishe d b

ymakin g a "fil l t o thi s level " lin e o n th e outsid e ofth e sampl e container

. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample

. I fth e expecte d rang e o fanalyt e concentration s i s unknown , multipl e spike s a t varyin g level s ma

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

e a t a n appropriat e leve l i s made

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

ycomplicat e th e interpretatio n ofth e sampl e analysis

. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t o

fth e collectio n bottles

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

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

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

t th e sam e tim e an d place as eac h FMS

. 

### 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot o

fcontro l matri xt o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator ya t th e tim e ofsampl e extraction

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

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

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

. 

### 3. 8 Laborator 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 detennin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results

. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e determine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations

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

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

. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t o

fquantitatio n (LLOQ ) fo ra dataset i s th e lowes t concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac

ydurin g routin e operatin g conditions

. To simplif ydat a reporting , th e LLO Q i s generall yselecte d a s th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria

. Sampl e LLOQs are matrix-dependent

. Th e uppe rlimi t o

fquantitatio n (ULOQ ) fo ra dataset i s th e highest concentratio n tha t ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac

ydurin g routin e operatin g conditions

. Th e highest standar

d i n th e calibratio n curve that meets metho d criteri a i s define d as th e ULOQ

.

ETS-8-044. 0 Pag e 3 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 9 of6 8Doci®mwt)-H}3"j«fesnifi??!|fcii,ol fcurrent , fo r1 4 day s fro m 10/26/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 0



### 3.1 1 Metho d Blan k A n aliquot ofcontro l matri xtha t i s treate d exactl ylik

e a laborator

ysampl e includin g exposur e t o al l glassware , equipment , solvents , an d reagents that 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 yo fmateria l intende d t o represen t th e origina l source material

. 

### 3.1 3 Stoc k

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

. 

### 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t nonnall y foun d i n th e sample(s)

. Asunogat e compoun d i s typicall ya target analyt e wit h a t leas t on e ato m containin g a n isotopically-labele d substitution

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

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

. Inclusio n ofa sun'ogate analyt e i s a n optiona l qualit ycontro l measure an d i s NO Trequired

. 

### 3.1 5 Workin g Standar d (WS ) Asolutio n ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o 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 ydeteimined ; however , eac h shoul d b e treate d a s a potentia l healt h hazard

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

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

. Th e laborator

yi s responsibl e fo rmaintainin g a saf e wor k environmen t an d a curren t awarenes s ofloca l regulation s regardin g th e handlin g ofth e chemical s use d i n thi s method

. Areference file ofmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses

. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems

. Refe rt o th e appropriat e equipmen t procedur e o roperato rmanua l fo radditiona l infonnatio n an d cautions

. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware

. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m intert^erence s unde r condition s ofanalysi s b

yrunnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 of1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 0 o f6 8Attachmen t 0 )oci«ra:wi!)iR03MMWmKi!rToM,o'? fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 o fpumpin 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 L connecte d t o a tande m Mass Spectromete r (LC/MS/MS)

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

t ra wdat a fo rpea k

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

. Gas tigh t syringes , 25pL , 50pL , 100(JL , 250|JL , 500pL , lOOOpL

. 1 m L plasti cHPLC autovial

. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e ofspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm
. 

### 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C18,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

Are a - quadrati ccurve flt, 1/ xweighted

. Ru n Time : ~ 1 7 minutes

. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met

.

ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 1 o f6 8Attachmen t 0 Docmsmmbwzi'pkmmimy! ^ current , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 PFBA PFPeA 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 9 313- > 26 9 an d 31 3 ^11 9 36 3 ^ 319 , 36 3 ^

16 9 an d 36 3 ^

11 9 41 3 ^ 369 , 41 3 ^

21 9 an d 41 3 ^

16 9 46 3 - » 419 , 46 3 - ^

16 9 an d 46 3 - > 21 9 51 3 - ^ 469 , 51 3 - > 21 9 an d 51 3 - ^ 26 9 56 3 ^ 519 , 56 3 - > 26 9 an d 56 3 - > 21 9 61 3 - > 569 , 61 3 - ^

16 9 an d 61 3 ^

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

9 9 39 9 ^ 8 0 an d 39 9 ^

9 9 49 9 ^ 80 , 49 9 ^

9 9 an d 49 9 - > 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n o fisomers tha t more closel ymatche s NM R dat a an d ma yhave th e adde d benefi t of 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 a s a guide , altemat e instalment s an d equipmen t ma yb e used

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

. Reagen t Grad e 

### 7. 2 Standard s Perfluorobutanoi cAci d (PFBA
- C4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFH A- C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFO A- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFN A- C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C l 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 of1 1 Metho d ofAnalysi 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 6 2 o f6 8DocKSttK»f)«2rjfitertn»8^ii,o Wcurreot , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 0

Th e previou s informatio n i s intende d a s a guide

. Reagent s an d standard s fro m alternat e source s ma yb e used

. 

### 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—^Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t water

. Note : Alternative volume s ma yb e prepare d as lon g as th e ratio s ofth e solven t t o solut e ratio s ar e maintained

. 

### 7. 4 Stoc k

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

d preparatio n procedur

e serve s a s a n example

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

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

solution s t o appropriat e levels

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

d (correcte d fo rpercen t sal t an d purity ) an d dilut e t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cfiask. 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 con-ectio n i s give n belowfo rPFOS

. ^

. , ^ molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t o fsal t 49 9 PFO S (K- ^ )sal t correctio n facto r= - ^ = 0.927 5 53 8 1 0 m g CSFITSOS'K " wit h purit y90 % = 8.35m g CsFiySOa " (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 fiask an d brin g u p t o volum e wit h solvent

. 25 0 ng/m L mixe d woricin g standard^Ad d 1.25m L ofth e 5 pg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflask

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

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

. Storag e Conditions—Stor e al l SSS s an d worthin g standard s i n accordance wit h laborator ystandar d operatin g procedur e o ri n a refrigerato ra

t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e 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 6 3 o f6 8Attachmen t C DocL(SB:vRst5if)iqo3'jhtteirmiBi8^#io Wcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L June/Jul y201 0

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

. Note : Volume s o fwate ran d worthin g standard s ma y b e adjuste d t o meet th e data qualit yobjective s addresse d i n th e genera l projec t outline

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

.

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

.

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 yoffluorochemical stickin g t o th e glass

. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water

. Prepar e metho d QC sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials

. Prepar e a t least five metho d blanks

. 

### 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

d curve prio rt o eac h set o fsamples

. Th e standar

d curve ma

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

xo runweighted , o rb

yquadrati cfli (

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 be thoroughl ydocumente d i n th e ra wdata

. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e data o rbecaus e theydi d no t mee t th e pre-detennine d acceptance criteria

. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are no t a t least twic e that ofth e metho d and/o rsolven t blanks

. Th e coefficien t ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o requa l t o 0.990

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

t Injectio n Analysi s Pag e 6 4 o f6 8Doc«B!>WG(il)«ayiteBnirop:ai.oM ' current , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S I n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 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 cun/e

. 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 ar e 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 dat a accurat e t o ±30 % wit h a targete d LOQ of0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e final report

. 10. 2 Metho d Blank s Metho d blank

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

. At least five metho d blank s mus t b e prepared

. Metho d blank

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

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

t th e en d ofth e analytica l 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 o

fth e LOQ standard

. Th e standar

d deviatio n ofth e are a counts ofthes e metho d blank s shoul d b e calculate d an d reported

. I f th e mea n are a counts ofth e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ mus t b e raise d t o th e flrst standar

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

. 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

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

. Th e requiremen t fo r replicate s exclude s field blanks

. 

### 10. 4 Surrogat e Spike s Sun-ogat e spike s are no

t require d bu t ma

yb e use d o n projec

t specifi crequirements

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

ftwo differen t concentration s are t o b e prepare d wit h eac h preparatio n batch

. Lo wla b contro l spike s shoul d b e prepare d a t concentration s i n th e rang e offive t o te n time s highe rtha n th e targete d LO Q an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t 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 are no t met , th e entire set ofsample s shoul d b e re-injecte d o rre-prepare d a s appropriate

.

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

t Injectio n Analysi s Pag e 6 5 o f6 8DocK3ttBwt)«aMhtbim!K»pBil.o Wcurreot , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 0



### 10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s o ffleld matri xspike s an d laborator ymatri xspike s ar

e anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels

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

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

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

. Th e targete d fortificatio n level s shoul d b e a t 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 withou t justificatio n t o detennin e th e statemen t o faccurac yfo ranalytica l results

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

. , ^ , . , , , , (Pea k

Are a - Intercept ) ^ ^ Analyt e foun d (ng/mL ) = - ^ ^-^

xD F Slop e D F = facto rb

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

_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

. Nonconfomnanc

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

. I fcriteri a liste d i n thi s metho d perfonnance 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 ar e 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 o fth e report

. 

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

ystandard s are no

t a require d componen t ofthi s method

. I frequire d b yprotoco l o rb

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

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

. Th e syste m suitabilit yinjection s mus

t have are a counts wit h a n RS D ofS5% an d a retentio n tim e RS D of^2 % 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 o f th e LLOQ , whic h ma

yb e withi n ±30%

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

t b e withi n 25 % ofth e theoretica l valu e (withi n 30 % fo rlowest curve point)

. Sample s that are brackete d b

yCCVs no

t meetin g thes e criteri a must b e reanalyzed

.

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

t Injectio n Analysi s Pag e 6 6 o f6 8DocifSttftcwfjinoaihfeanWiSiil.o-r fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L Attachmen t C June/Jul y201 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 yspecifl canalyt e ma yvar y dependin g o n th e evaluatio n ofappropriat e blank s an d th e accurac

yo fth e low-leve l calibratio n curve points

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

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

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

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

ymatri xspikes

. 

### 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

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

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

. Sectio n 1 0 contain s additiona l 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 performin 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 interna l procedures

. 1 4 Record s Eac h data packag e generate d fo ra stud ymust includ e al l supportin g infonnatio n fo rreconstmctio n ofth e data

. Informatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

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

. 

### 1 5 Affecte d Document s None

. 

### 1 6 Revision s Revisio n Numbe rSummar vo fChange s

ETS-8-044. 0 Pag e 1 1 of1 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 6 7 o f6 8

### SMcffM^ntia l GLP10-01-02 ; Interi m Repor t 0 7 Analysi s o fPFBS , PFHS , and PFO

S I n Wate rSample

s fro m Decatur, AL June/July201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/

. Identificatio n Stud y/ Projec t No

. GLP10-01-02-0 7 Date(s ) o fOccurrence : 0100715 b an d m l 00917 a Documen t Number : ETS-8-044. 0 Deviatio n typ e D SO P D Equipmen t Procedur e 1 3 Metho d (Ciiecl fone ) D Protoco l B GP O D Other :



### //

. Descriptio n (attac h extr a pages a s needed ) M9^h9AB'^'^\''^JPTf}^D^^ l (1 ) CC V recover

ywithi n 100 % ±25%

. (2 ) LC S averag e recover yof100 % ±20%

. (3 ) Sample/Sampl e Duplicat e RP D S20%

. (4 ) FM S recover

yo f100 % ±30%

. 

### Actua l procedure/process : (1 ) (2 ) (3 ) (4 ) Twenty-on e CCVs wer e analyze d durin g th e cours e ofth e ru n wit h thre e CCVs not meetin g metho d acceptanc e criteri a wit h recoverie s o f70.8% , 73.6% , an d 73.3 % fo rPFH S (o100715b)

. LG S averag e recover

yfo rth e hig h se t o flinea ran d branche d PFO S wa s 122 % (s100715b)

. LC S averag e recover

yfo rth e lowse t oflinea rPFO S wa s 121 % an d 125 % fo rth e lowse t oflinea ran d branche d PFO S (m100917a)

. Th e RP D valu e fo rPFB S fo r138 L wa s 27%

. Th e followin g location s di d not have a n appropriat e FM S leve l fo rPFOS : DA L 132 L an d DA L 134L

. Th e followin g FM S leve l di d not mee t metho d acceptanc e criteria : th e hig h FM S fo rPFO S o n DA L 130 L (54.8%) , th e mi d FM S fo rPFO S DA L 135 L (68.2%) , th e mi d FM S fo rPFO S o n DA L 136 L (65.6%) , th e lowFM S fo rPFH S o n DA L 137 S (149%) , th e lowFM S fo rPFH S o n DA L 137 S (186%) , th e mi d FM S fo r PFO S o n DA L 137 S (61.5%) , an d th e lowFM S fo rPFH S o n DA L 138 L (203%)

. 

### ///

. Action s Take n (sucl i a s amendmen t issued , SO P revision , etc. ) 

### Correctiv e Actio n ( D Ye s 0 No) Reference : Acceptabilit yo fth e nonconformin g work : 1 ) 2 )
3 ) 4 ) Reporte d sample s brackete d byth e thre e CCVs fo rPFH S tha t di d not mee t metho d acceptanc e criteri a (132S , 134R , 135S , an d 135L) wil l b e note d i n th e fina l report

. Th e 9/17/1 0 analysi s include d a numbe rofsample s tha t containe d PFO S concentration s greate rtha n th e calibratio n range
. I t i s believe d tha t th e hig h recover yfo rth e lowse t ofLC S i s du e t o analyt e carry ove ras th e lowse t ofLC S were analyze d immediatel ythes e samples

. Th e RP D valu e fo rPFB S fo r138 L wit h a valu e >20 % wil l b e footnote d i n th e dat a tables

. Samplin g location s withou t a n appropriat e spike leve l fo rPFO S wil l b e footnote d i n th e fina l repor t (DA L 132 L an d DA L 134L)

. Samplin g location s DA L 135 L an d 136 L ha d FM S recoverie s fo rPFO S tha t di d not mee t metho d acceptanc e criteri a (68.2 % an d 65.6%) , however , sinc e th e metho d analytica l uncertaintyfo rPFO S i s 100 % ±37% , n o adjustmen t wa s mad e t o th e analytica l uncertainty

. Samplin g location s DA L 137L , DA L 137S , an d DA L 138 L ha d hig h recoverie s fo rth e lowFM S fo rPFHS , however , th e sample s containe d PFH S jus t belo wth e metho d LO Q o f0.10 3 ng/mL , whic h mos t likel yaccount s fo r th e hig h recover

yofth e lowFM S samples

. Th e mi d an d hig h FM S level s fo rthes e samplin g location s me t metho d acceptanc e criteria

. Fo rsamplin g location s DA L 130 L an d DA L 137S , th e analytica l unc^rtairit ywil l b e adj^u^^ ^ o n th e recover yofth e mos t appropriat e spik e level

. 

### Actions : D Haltin g o

fWor k D Clien t Notificatio n D Wori < Recal l D Withholdin g o fRepor t 0 Other : Deviation s wil l be noted i n fiop i report

. Project Lead/PA I Approval : Stud yDirecto r(FGLP) ^ 

### Sponso rApprova l (fo rGLP^rotoco l deviations) : N A Date : N A Technica l Reviewe r(optional) : NA ! Date : NA Laborator yDepartmen t Manage rApproval : 1 Date :

IV

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

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

. Attachmen t A (assigned byStudyDirecto ro rTea m Leade ra

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