GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0 

# 3 M

GLP10-01-02 : Interi m Repor t 0 2 - Analysi s o fPFBS

. PFHS

. an d PFO S i n Groun d Wate rSample s Collecte d fro m Decatur

. A L i n March/Apri l 201 0
Stud yTitl e Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m 

### Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc

. 140 0 Westo n Way Westchester , PA1938 0 Phone:610-701-376 1 

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

### Interi m Repor t Completio n Dat e

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

y 3 M Center , Bld g 260-05-N-1 7 Maplewood , M N 55144 

### Projec t Identificatio n GLP l 0-01-02-0 2 

### Tota l Numbe ro fPage s

5 7

lACCREDITED J Th e testin g reporte d herei n mee t th e requirement s o fANS/1S0/IEC17025:200 5 "Genera l Requirement s fo rth e Competenc e o fTestin g an d Calibratio n Laboratories" , I n accordanc e wit h th e A2L ACertificat e #2052-01

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

. Certificat e #2052-0 1

Pag e 1 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

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

.

Pag e 2 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



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

t 02 Analysi s o fPFBS , PFHS , an d PFO S i n Groun d Wate rSample s Collecte d a

t Decatur , A L i n March/Apri l 201 0 Study : 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 Program

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

• Thes e are environmenta l sample s where there i s n o specifi ctes t substance , n o specifi ctes t syste m an d n o dosin g o fa tes t 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 tes t sit e hav

e no t bee n determine d unde rGLPs

.

Gar yHonensteih , Sponso rRepresentative Dat e 

### \ 

# QZkhkl ^ Jaisimh a Kesari , P.E. , DEE , StudyDirecto r/ Date

Pag e 3 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iWarch/Apri l 201 0



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

t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groun d Wate rSample s Collecte d a

t Decatur , A L i n March/Apri l 201 0 Study : 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 Program

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

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

.

Inspectio n Date s
3/3/1 0 3/25/1 0 6/3/10-6/4/1 0 Phas e
Protoco l In-Phas e Audi t - Bottl e Orde rPre p Interi m Repor

t 0 2 Data an d Repor

t Dat e Reporte d t o

Testin g Facilit y •Managemen t 3/16/1 0 4/5/1 0 6/11/1 0 Stud yDirecto r 3/16/1 0 4/5/1 0 6/11/1 0

y 

# (,-^"7^ 0 QA U Represeirativ e Dat e

Pag e 4 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarch/Apri l 201 0



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

y9 3 Introductio n 1 0 4 Test & Contro l Substance s 1 1 5 Reference Substance s 1 2 6 Tes t Syste m 1 4 7 Metho d Summar

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

s 1 6 8. 6 La b Contro l Spike s (LCSs ) 1 7 8. 7 Analytica l Metho d Uncertaint y1 9 8. 9 Fiel d Matri xSpike s (FMS ) 2 0 9 Dat a Summar

yan d Discussio n 2 0

Pag e 5 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



### 1 0 Conclusio n 3 1 1 1 Data/Sampl e Retentio n 3 1 1 2 Attachment s 3 1 1 3 Signature s 32 LIS TO F TABLE S Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Results (Decatu rGroundwater ,

March/Apri l 2010 ) 1 0 Tabl e 2

. Instmmen t Parameter s 1 5 Tabl e 3

. Liqui d Chromatograph yCondition s 1 5 Tabl e 4

. Mass Transition s 1 5 Tabl e 5

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

. Laborator

yContro l Spik

e Recover

y1 8 Tabl e 6 continued

. Laborator yContro l Spike Recover

y1 9 Tabl e 7

. Analytica l Uncertaint y1 9 Table8

. GW203LQ 1 Y10L F 2 1 Table9

. GW220RQ 1 Y10L F 2 1 Tabl e 10

. GW220LQ 1 Y1 0 L F 2 2 Tabl e 11

. GW222RQ 1 Y10L F 2 2 Tabl e 12

. GW227LQ 1 Y1 0 L F 2 3 Tabl e 13

. GW227RQ 1 Y1 0 L F 2 3 Tabl e 14

. GWGRS04Y10L F 2 4 Tabl e 15

. GW310RQ 1 Y10C P 2 5 Tabl e 16

. GW312RQ 1 Y1 0 C P 2 5 Tabl e 17

. GW317LQ 1 Y10C P 2 6 Tabl e 18

. GW324LQ 1 Y10C P 2 6 Tabl e 19

. GW327RQ 1 Y10C P 2 7 Tabl e 20

. GW328LQ 1 Y10C P 2 7

Pag e 6 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 21

. GW328RQ 1 Y10C P 2 8 Tabl e 22

. G W330LQ 1 Y I 0 C P 2 8 Table23

. GW330RQ 1 Y10C P 2 8 Table24

. GW331SQ 1 Y10C P 2 9 Tabl e 25

. Tri p Blan k

2 9 Tabl e 26

. Rinseat e Blank s 3 0

Pag e 7 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri i 201 0

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

. Westchester , P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator , (clanqe(S)mmm.com) ; phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Jonatha n Steege ; analys t Stud yDate s Stud yInitiation : Marc h 8,201 0 Interi m # 2 Sampl e Collection : Marc h 30,2010-Apri l 14,201 0 Interi m # 2 Experimenta l Termination : Ma y26 , 201 0 Interi m Repor

t Completion : Date ofInteri m Repor t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792

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

Pag e 8 of5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L Marcli/April201 0

Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d i n Decatur , AL , representin g 1 7 differen t samplin g locations

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

. Sample s als o include d low , mi d an d hig h fiel d 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 fiv e equipmen t rinseates. Two additiona l soil-equipmen t rinseates that were collecte d a s par t ofprojec t GLP l 0-01-02
- 0 1 fo ranalysi s ofPFBS , PFHS , an d PFO S i n soil s collecte d fro m th e fomne rsludg e incorporatio n are a (FSIA ) field s a t th e Decatu rsit e i n March/Apri l 2010 , were als o include d i n thi s analysis

. Th e equipmen t rinseate blank s di d not have FM S sample s prepare d fo rdetemriinatio n o fPFBS , PFH S o r PFO S recovery
. Al l groundwate rsample s fo rthi s projec t were logge d unde rGLP l 0-0 1 -0 1 -02

. Th e groundwate rsamples , tri p blan k an d fiv e equipmen t rinseate blank s were receive d fro m Westo n personne l o n Apri l 15 , 2010

. Th e soil-equipmen t rinseate blank s were receive d wit h th e FSI Asoi l shipmen t o n Apri l 01,2010

. 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-10-01-02-02

. Man yofth e groundwate rsample s require d dilutio n t o attai n PFBS , PFHS , an d PFO S concentration s withi n th e rang e ofth e curve , i n som e instance s u p t o a 100-fol d dilutio n were required

. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s are summarize d i n Tabl e 1 Th e equipmen t 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 ofsampl e contaminatio n durin g shippin g an d sampl e collections

. Th e PFB S concentratio n results fo ral l groundwater s range d ove rfou rorder

s ofmagnitud e fro m 0.534 ng/m L t o 447 0 ng/mL

. Th e PFH S concentratio n results fo ral l groundwater s range d ove rfou rorder

s of magnitud e fro m 0.69 1 ng/m L t o 619 0 ng/mL

. Th e PFO S concentratio n results fo ral l groundwater s range d ove rthre e order

s o fmagnitud e fro m 2.44 ng/m L t o 175 0 ng/mL

.

Pag e 9 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVIarch/Apri l 201 0

Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Result s (Decatu rGroundwater , March/Apri l 2010)

.

Samplin g Locatio n GW203LQ 1 Y1 0 L F GW220RQ 1 Y1 0 L F GW220LQ 1 Y1 0 L F GW222RQ 1 Y1 0 L F GW227LQ 1 Y1 0 L F GW227RQ 1 Y1 0 L F GWGRS04Q 1 Y1 0 L F GW310RQ 1 Y1 0 C P GW312RQ 1 Y1 0 C P GW317LQ 1 Y1 0 C P GW324LQ 1 Y1 0 C P GW327RQ 1 Y1 0 C P GW328LQ 1 Y1 0 C P GW328RQ 1 Y1 0 C P GW330LQ 1 Y1 0 C P GW330RQ 1 Y1 0 C P GW331SQ 1 Y1 0 C P Tri p Blan k

(Milli-Q TM Water

) Equipmen t Rinseate Blank s 1 t o 5 , 203 L DA L DF05 SS07 2 001 0 (soi l equipmen t rinseat e blank

) DA L DF l 1 SS0 7 2 001 0 (soi l equipmen t rinseate blank

) PFB S Avg

. Conc

. (ng/mL ) ±RP D 61. 9 ±3.4 % 7.4 6 ±3.5 % 11. 1 ±13 % 12 9 ±3.9 % 342±4.1 % 23.8 ±6.7 % 193 0 ±13 % 38 6 ±8.0 % 122 0 ±0.0 % 0.53 4 ±0.94 % 95. 7 ±2.8 % 75. 8 ±14 % 76. 8 ±1.6 % 36. 0 ±1.9 % 50 4 ±6.0 % 447 0 ±2.5%<^

' 34 9 ±13 % <0.025 5 <0.025 5 <0.025 5 <0.025 5 PFH S

Avg

. Conc

. (ng/mL ) ±RP D 36 0 ±0.83 % 32. 0 ±0.63 % 53. 0 ±4.9 % 84 5 ±1.3 % 63. 7 ±4.7 % 16 9 ±0.0 % 6190±9.0%<^

> 42 4 ±5.4 % 94 6 ±0.74 % 0.69 1 ±0.72 % 10 1 ±5.6 % 154 ±2.6 % 25. 9 ±1.2 % 67. 7 ±6.7 % 40 3 ±1.2 % 25 8 ±5.0 % 42 6 ±13 % <0.025 8 <0.025 8 <0.025 8 <0.025 8 PFO S

Avg

. Conc

. (ng/mL ) ±RP D 85 2 ±1.1 % 46. 0 ±12 % 63. 6 ±3.8 % 97 4 ±4.7 % 28 7 ±13 % 95 6 ±7.4 % 140 0 ±16 % 76 0 ±5.4 % 175 0 ±4.6 % 2.4 4 ±3.7 % 20 3 ±11 % 63 9 ±18 % 14. 5 ±0.69 % 14 6 ±19 % 145 ±14 % 75 9 ±1.1 % 922±21%<^ ' <0.51 0 <0.51 0 <0.51 0 <0.51 0
Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are as follows : PFB S 100 % ±21% , PFH S 100 % ±25% , an d PFO S 100 % ±44%

. (1 ) Samplin g locatio n di d no t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e analyte recovery
. (2 ) Th e RP D di d no

t mee t metho d acceptance criteri a ofS20%

.

Thi s analytica l stud ywa s conducte d a s par t o f th 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 f th e overal l progra m i s t o gai n infomnatio n regardin g concentration s of perfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e

Pag e 1 0 o f 5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

(PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu r^cility

. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d i n Decatur , A L fo r PFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on-sit e groundwate rconditions

. Additionally , tw o aqueou s soil-equipmen t rinseate sample s collecte d a s par t ofth e PFBS , PFHS , an d PFO S assessmen t i n soil s fro m forme rsludg e incorporatio n are a (FSIA ) field s a t th e Decatu rsit e i n March/Apri l 2010 , were als o analyzed

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

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

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

. Eac h empt ycontaine rwa s mari<e

d wit h a "fil l t o here " lin e t o produce a fina l sampl e volum e o f20 0 mL

. Container s designate d fo rfiel d matri xsample s wer e fortifie d wit h a n appropriat e matri xspike 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

. Al l sampl e bottle s include d th e additio n o fO2-PFBS , ^®02-PFHS , an d ^^Cg-PFO S (intema l standards ) a

t a nomina l concentratio n o f1 ng/mL

. Al l sampl e bottle s als o include d th e additio n of^^C4-PF0 S (surrogat e spike ) a t a nomina l concentratio n of0. 1 ng/mL

. 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 , simila rt o soi l sampl e bottle s (se e GLP10-01
- 0 2 Interi m Repor

t 0 1 fo rdetails)

. 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 "Detemiinatio n o fPerfluorinate d Compound s I n Wate rb yHig h Perfomnanc

e 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 8-2 6 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 are reporte d an d discusse d elsewhere i n thi s repor t

There wa s no

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

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

.

Pag e 1 1 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 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 Lot Numbe r 1 TC R Numbe r Physica l Descriptio n Purit y PFB S
Perfluorobutan e sulfonat e C4F9SO3 " Potassiu m Sal t 3 M 1/10/201 7 Froze n 41-2600-8442- 5 TCR-12 1 Whit e Powde r 

### 1 96.7 % PFH S (linear ) Perfluorohexan e sulfonat e C6F13SO3 " Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHxSAMO

S | TCR08^01 8 1 Crystallin e 

### 98 % 

### 1

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 PFOS (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 % PFOS (linea r+ branched ) Perfluorooctan e sulfonat e C8F17SO 3 Potassiu m Sal t CAS #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 f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

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

t Numbe r 1 TC R Numbe r Physica l Descriptio n 1 Purity ^^OrPFB S 1 Labele d - Perfluorobutan e sulfonat e C4F9S[^^02]0 ' Ammoniu m Sal t RT I Intemationa l 3/9/201 5 Froze n 11546-107- 2 TCR-101 3 Liqui d 99 % "OrPFH S

Labele d - Perfluorohexan e 1 sulfonat e C6Fi3S[''02]^®0 ' Sodiu m Sal t | Wellingto n 7/24/201 1 1 Froze n MPFHXA0706 | TCR-121 8 Liqui d 

### 98 % 

### 1

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 1 TC R Numbe r Physica l Descriptio n 1 Purity "C^PFO S Perfluorooctan e sulfonat e ^^C;^C4Fi7S0 3 1 Sodiu m Sal t

Wellingto n 1 8/18/201 1

Froze n 1 MPFPS080 8 1 TCR08-004 3

Liqui d 

### 1 98 % "CtfJ»FO S Perfluorooctan e sulfonat e ''C8F17SO 3 1 Sodiu m Sal t

Wellingto n 1 6/17/201 2

Froze n 1 M8PFOS060 9 1 TCR09-004 9

Liqui d 

### 1 98 %

Pag e 1 3 of5 7GLP l 0-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

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 o ftes t substance

. Sampl e Descriptio n Ke yCode

. strin g Numlje r Exampl e 1 2 3

4 Strin g Descripto r GW277 L Q l Y1 0 LF

O Sampl e Typ e Sampl e Locatio n Wel l Leve l
Samplin g Dat e Sampl e Typ e Exampl e GW= Groun d Wate r Example : 227LL F R = Residu m shallo wwater-bearin g zon e L = Bedroc k

water-bearin g zon e S = Epikars t middl e water-bearin g zon e Q1Y10-1s t 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. 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 "Detemiinatio n ofPerfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

. 

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

. Sampl e bottle s were retume d t o th e laborator ya t ambien t condition s o n Apri l 15 , 201 0 Sample s were store d refi-igerate d a t th e laborator

yafte rreceipt

. Aset o flaborator 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 i t i n a n autovia l fo r analysis

. Sample s that require d dilutio n were prepare d b ydilution s of1 m L sampl e wit h 9 mLs o fMill ! Q wate r (dilutio n 1:10)

. Most samplin g location s were dilute d 1:100 byfurthe rdilutin g th e 1:1 0 dilutio n wit h additiona l Mill i Q 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 peri'omnanc

e liqui d chromatography

/ tande m mas s spectrometr y(HPLC/MS/MS)

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

wdat a har

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

.

Pag e 1 4 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 2

. Instrumen t Parameters

. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r io n Sourc e Electrod e Polarll y Softwar e ETS Ginge r ETS-8-044. 0 5/17/201 0 an d 5/26/201 0 Agilen t 110 0 Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n Betasi l C1 8 (2. 1 mm X 100 mm) , 5 n

2,5,or10ti L Applie d Biosystem s AP I 500 0 Tuttj o Spra

y Turb o io n electrod e Negativ e Analyst 1.4. 2 Tabl e 3

. Liqui d Cliromatograph yConditions

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

(min ) 0 1. 0 11. 0 13. 5 14. 0 17. 0 Flo wRat e

(fdJmin ) 30 0 30 0 30 0 30 0 30 0 30 0 Percen M

( 2 m M ammoniu m acetate )

97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 Percent B

(Methanol ) 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 Tabl e 4

. Mas s Transitions

.

/inalyt e

PFB S

PFH S

PFO S Mas s Transitio n

Q1/Q 3 299/8 0 299/9 9 299/13 0 399/8 0 399/9 9 399/13 0 499/8 0 499/9 9 499/13 0 Dwel l tim e wa s 5 0 mse cfo reac h transition

. Th e individua l transition s were summe d t o produce a "tota l io n chromatogram " (TIC) , w/hich wa s use d fo rguantitation

.

Pag e 1 5 o f5 7GLP l 0-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

8. 1 Calibratio n Sample s were analyze d against a n externa l standar d calibratio n curve
. Calibratio n standard s were prepare d b

yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s into prepare d i n Mill i Q water

. Atota l ofthirtee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 5 0 ng/m L (nominal ) were analyzed

. Lo

wcurve points were disable d fo rPFO S t o meet metho d blan k criteria

. Aquadratic , 1/

x weighted , calibratio n curve ofth e pea k are a counts wa s use d t o fit th e dat a fo reac h analyte

. Th e dat a were not force d throug h zero durin g th e fitting process
. Calculatin g th e standar d concentration s usin g th e pea k are a confimned accurac

yo feac h curve point

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

yrequirements o f100±25 % (100±30 % fo rth e lowest curve point) were met fo ral l analytes

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

. Du e t o th e concentratio n ofPFBS , PFHS , an d PFO S detecte d i n th e samples , isotopically-labele d PFBS , PFHS , an d PFO S were no t use d durin g instrumen t calibration

. 8. 2 Syste m Suitabilit y Acalibratio n standar

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

. Th e acceptance criteri a ofles s tha n o requa l t o 5 % relative standar d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a ofles s tha n o requa l t o 2 % RS D wa s met fo rPFBS , PFHS , an d PFOS

. 

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

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

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

. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 4

. Tabl e 5

. Limi t o fQuantitatio n (LOQ)

. Analysi s Dat e 5/17/1 0

5/26/1 0 Dilutio n
1 1 0 100 20 0 PFB S

LOQ , ng/m L 0.025 5 0.25 5 2.5 5 N A PFH S

LOQ , ng/m L 0.025 8 0.25 8 2.5 8 51. 6 PFO S

LOQ , ng/m L 0.51 0 5.1 0 51. 0 N A 8. 4 Continuin g Calibratio n Durin g th e cours e o feac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confimri that th e instalmen t respons e an d th e initia l calibratio n curve were stil l i n control

. Al l CCVs met metho d criteri a of100 % ±25%

. 

### 8. 5 Blanl( s Two type s ofblank

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 evaluat e metho d perfonnance an d t o determin e th e LO Q fo reac h analyt e

Pag e 1 6 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarcli/Apri l 201 0

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

. LCS s were prepare d b yspikin g know n amounts ofth e analyt e into 4 0 m L ofMill i Q wate rt o produce th e desire d concentration

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

. Du e t o th e analytica l reportin g limit , th e lo wset oflinea r PFO S LC S sample s coul d no t b e quantitated

. Th e metho d acceptance criteria , averag e ofLC S at eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <20% , were me t fo rth e PFBS , PFHS , an d linea r PFO S LC S samples

. A s th e reference 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 are comprise d ofbot h linea ran d branche d isomers , additiona l LC S sample s of PFO S (linea r+ branched ) were prepare d a t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias

. Du e t o th e analytica l reportin g limit , th e lo wset o fLC S coul d no

t b e quantitated

. Th e LC S a t th e mi d leve l met metho d acceptance criteria , whil e th e hig h leve l di d no t meet metho d acceptance criteri a wit h a n averag e recover

yo f172%

. A n additona l se t ofmid , mid-high , an d high-leve l LCS , prepare d o n a differen t dat e wit h othe rsamples , were analyze d at th e en d ofth e analytica l ru n t o confir m th e recover yofth e high-leve l LCS

. Th e analysi s ofthes e sample s produce d acceptabl e recoverie s fo rth e mi d an d mid-hig h LCS , wit h th e averag e recover yo fth e high-leve l LC S a

t 130%

. Base d o n th e recover yofth e secon d se t ofhigh-leve l LCS , i t i s th e opinio n ofth e laborator ythat th e recover

yo fth e high-leve l LC S i s du e t o a sampl e preparatio n error , an d no t th e resul t o fan ysignifican t analytica l bias

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

. A metho d deviatio n i s filed wit h th e ra wdat a fo rPFO S (linea r+ branched ) LC S that di d not meet metho d acceptance criteria

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

.

. yer ^

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

y= * 100 % Spiice Concentratio n LCS % RS D = ^*^"^^^

^ '^^^'^''° " ^^ ^

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

y

Pag e 1 7 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVIarcii/Apri l 201 0

Tabl e 6

. Laborator yContro l Spik e Recovery

. ETS-8-044. 0

La b I D LCS-100512- 1 LCS-100512- 2 LCS-100512- 3 Averag e ±%RS D LCS-100512- 4 LCS-100512- 5 LCS-100512- 6 Averag e ±%RS D LCS-100512- 7 LCS-100512- 8 LCS-100512- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0.20 4 0.20 4 0.20 4 Calculate d

Concentratio n (ng/mL ) 0.23 9 0.22 7 0.25 1 %Recover y

11 7 11 1 12 3 117 % ±5.1 % 5.1 0 5.1 0 5.1 0 4.6 8

5.4 2 5.3 5 91. 7

10 6 10 5 101 % ±7.9 % 30. 6 30. 6 30. 6 30. 2

30. 6 29. 3 98. 8

99. 9 95. 8 98.2 % ±2.2 % PFH S Spike d Concentratio n (ng/mL ) 0.20 6 0.20 6 0.20 6 Calculate d

Concentratio n (ng/mL ) 0.24 4 0.24 2 0.25 0 VoRecover y

11 8 11 8 12 1 119 % ±1.5 % 5.1 5 5.1 5 5.1 5 4.7 7

5.4 3 5.4 4 92. 6

10 5 10 6 101 % ±7.4 % 30. 9 30. 9 30. 9 29. 8

29. 1 29. 5 96. 4

94. 3 95. 5 95.4 % ±1.1 %

ETS-8-044. 0

La b I D LCS-100512- 1 LCS-100512- 2 LCS-100512- 3 Averag e ±%RS D LCS-100512- 4 LCS-100512- 5 LCS-100512- 6 Averag e ±%RS D LCS-100512- 7 LCS-100512- 8 LCS-100512- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0.20 4 0.20 4 0.20 4 Calculate d

Concentratio n (ng/mL ) <0.51 0 <0.51 0 <0.51 0 %Recover y

N C N C N C N A 5.1 0 5.1 0 5.1 0 4.9 0

5.4 5 5.5 5 96. 0

10 7 10 9 104 % ±6.7 % 30. 6 30. 6 30. 6 30. 0

30. 2 30. 5 97. 9

98. 7 99. 8 98.8 % ±1.0 % La b I D LCS-100512-1 0 LCS-100512-1 1 LCS-100512-1 2 Averag e ±%RS D LCS-100512-1 3 LCS-100512-1 4 LCS-100512-1 5 Averag e ±%RS D LCS-100512-1 6 LCS-100512-1 7 LCS-100512-1 8 Averag e ±%RS D PFO S (linear+branched )

Spike d Concentratio n (ng/mL ) 0.20 0 0.20 0 0.20 0 Calculate d

Concentratio n (ng/mL ) <0.51 0 <0.51 0 <0.51 0 VoRecover y

N C N C N C N A 5.0 0 5.0 0 5.0 0 5.7 4

5.8 5 5.6 4 11 5

11 7 11 3 115 % ±1.7 % 30. 0 30. 0 30. 0 51. 7

49. 8 53. 4 17 2

16 6 17 8 172 % ±3.5%'^ ' N C = No t Calculated ; Concentratio n detecte d wa s les s tha n tti e analytica l LOQ

. (1 ) Tti e averag e recoveiydi d no t mee t metho d acceptance criteri a of100 % ±20%

.

Pag e 1 8 of5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 6 continued

. Laborator yContro l Spik e Recovery

. ETS-8-044.0 ; Prepare d with non-stud

ysample s
La b I D LCS-100517-1 6 LCS-100517-1 7 LCS-100517-1 8 Averag e ±%RS D LCS-100517-1 9 LCS-100517-2 0 LCS-100517-2 1 Averag e ±%RS D LCS-100517-2 2 LCS-100517-2 3 LCS-100517-2 4 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 5.0 0 5.0 0 5.0 0 Calculate d

Concentratio n (ng/mL ) 4.9 9 5.2 7 5.1 1 VoRecover y 99. 8 105 102 102 % ±2.6 % 15. 0 15. 0 15. 0 16. 6

16. 9 17. 5 11 1

11 3 11 6 113 % ±2.2 % 30. 0 30. 0 30. 0 37. 4

40. 0 39. 9 12 5

13 3 13 3 130%±3.5%<' ' N C = No t Calculated ; Concentration detecte d wa s les s than th e analytical LOQ

. (1 ) The average recover

ydi d no t mee t metho d acceptanc

e criteri a o f100 % ±20%

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

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

yan d precision

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

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

. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

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

. Th e mos t recen t 5 0 dat a points were use d t o generat e th e metho d uncertaint

yvalue s liste d i n Tabl e 7

. Tabl e 7

. Analytica l Uncertainty

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

10. 5 12. 4 21. 9 Metho d

Uncertaint y 100%±21 % 100%±25 % 100%±44 %

Pag e 1 9 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



### 8. 8 Fiel d Matri xSpike s (FMS ) Low , mi d an d hig h field matri xspike s were collecte d a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix

. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offield 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 xspike recoverie s withi n metho d acceptance criteri a of100±30 % confin n that "unknown " components i n th e sampl e matri x d o no t significantl yinterfere wit h th e extractio n an d analysi s o fth e analyte s o finterest

. Fiel d matri xspike concentration s mus

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

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

. Th e nomina l spike leve l fo rth e lo wfield matri xspike wa s 1. 0 ng/mL , th e mi d field matri xspik e wa s 10 0 ng/mL , an d th e hig h field mari xspik e wa s 100 0 ng/m L fo ral l samplin g locations

. Fo rsom e samplin g locations , th e hig h field matri xspike wa s not appropriat e a s compare d t o th e sampl e concentration

. N o laborator ymatri xspike s were prepared

. Fiel d matri xspike level s wil l b e adjuste d accordingl yfo rth e nex t samplin g event

. Du e t o th e hig h concentratio n ofPFBS , PFHS , an d PFO S detecte d i n th e samples , th e sun-ogat e spike o f^^C4-PF0 S wa s no

t analyzed

.

^

. , „ „ (Sample Concentrationof FMS - Average Concentration : FieldSampl e & FieldSampl

e Dup. ) „,,„„„ , FMS Recover

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

Th e table s belowsummariz e th e sampl e results an d field matri xspike 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 are rounde d t o thre e significan t figures accordin g t o EP Aroundin g rules

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

. Fiel d matri xspike recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges
. G WGRS04Q 1 - Th e recover yofth e hig h FM S sampl e fo rPFO S wa s 134%

. Thi s wa s th e onl y appropriat e field matri xspike leve l fo rPFOS

. Since th e metho d analytica l uncertaint yi s 100 % ±44% , n o adjustmen t wa s mad e t o th e analytica l uncertaint yfo rPFOS

.

Pag e 2 0 o f5 7GLP10-01-02 ; Interi m Repor t 02 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 8

. G W203LQ 1 Y1 0 L F

3MUMSI D GLP10-01-02-02-05 1 GLP10-01-02-02-05 2 GLP10-01-02-02-05 3 GLP10-01-02-02-05 4 GLP10-01-02-02-05 5 Averag e Concen b Descriptio n

GW203LQ 1 Y1 0 LF O GW203LQ 1 Y1 0 LF 1 GW203LQiyi O LFL S GW203LQ1Y1 0 LFM S GW203LQ 1 Y1 0 LFH S •atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 62. 9 60. 8 NA<^ > NA<^ > 122 0 %Recover y

NA NA NA<^ > NA<^ ' 11 4 61. 9 ng/m L ±3.4 % PFH S Concentratio n (ng/mL ) 35 8 36 1 NA'^ ) NA'^ ' 137 0 %Recover y

N A N A NA<^ > NA(^ ' 10 3 36 0 ng/m L ±0.83 % PFO S Concentratio n (ng/mL ) 85 6 84 7 NA<^ ) NA<^ > 170 0 %Recover y

N A N A NA'^ ' NA(^ ' 85. 7 85 2 ng/m L ±1.1 % NA= No t Applicabl e (1 ) Adilutio n oftti e sampl e was no t prepare d a

s th e spik e leve l was no

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

. Tabl e 9. G W220RQ 1 Y1 0 L F

3 M LIM S I D GLP10-01-02-02-08 0 GLP10-01-02-02-08 1 GLP l 0-01-02-02-08 2 GLP10-01-02-02-08 3 GLP10-01-02-02-08 4 Averag e Concen t Descriptio n

GW220RQ 1 Y1 0 LFO GW220RQ1Y1 0 LF 1 GW220RQ1Y1 0 LFL S GW220RQ1Y1 0 LFIVI S GW220RQ1Y1 0 LFH S 'atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 7.5 9 7.3 3 8.8 6 12 2 118 0 %Recover y

NA N A N C 11 2 11 5 7.4 6 ng/m L ±3.5 % PFH S Concentratio n (ng/mL ) 31. 9 32. 1 32. 9 13 8 110 0 %Recover y

N A N A N C 10 8 10 9 32. 0 ng/m L ±0.63 % PFO S Concentratio n (ng/mL ) 43. 2 48. 8 44. 4 13 1 101 0 VoRecover y

N A N A N C 85. 9 97. 4 46. 0 ng/m L ±12 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level

.

Pag e 2 1 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 10

. G W220LQ 1 Y1 0 L F

3IVILIMSI D GLP10-01-02-02-07 1 GLP10-01-02-02-07 2 GLP l 0-01-02-02-07 3 GLP10-01-02-02-07 4 GLP10-01-02-02-07 5 Descriptio n GW220LQ 1 Y1 0 LF O GW220LQ 1 Y1 0 LF 1 GW220LQ 1 Y1 0 LFL S GW220LQ 1 Y1 0 LFM S GW220LQ 1 Y1 0 LFH S Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 10. 4 11. 8 13. 5 12 9 114 0 %Recover y

N A N A N C 11 6 11 1 11. 1 ng/m L ±13 % PFH S Concentratio n (ng/mL ) 51. 7 54. 3 54. 4 15 5 107 0 %Recover y

N A N A N C 10 4 10 4 53. 0 ng/m L ±4.9 % PFO S Concentratio n (ng/mL ) 64. 8 62. 4 65. 8 15 7 91 9 %Recover y

N A N A N C 94. 3 86. 4 63. 6 ng/m L ±3.8 %
N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. Tabl e 11

. G W222RQ 1 Y1 0 L F

3iVILIMSI D GLP10-01-02-02-03 1 GLP10-01-02-02-03 2 GLP l 0-01-02-02-03 3 GLP10-01-02-02-03 4 GLPIO-OI-02-02-03 5 Averag e Concen t Descriptio n

GW222RQ 1 Y1 0 LFO GW222RQ 1 Y1 0 LF 1 GW222RQ1Y1 0 LFL S GW222RQ 1 Y1 0 LFM S GW222RQ 1 Y1 0 LFH S •atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 13 1 12 6 NA'^ ' NA'^ ' 120 0 %Recover y

N A N A NA'^ ' NA<^ ' 10 5 12 9 ng/m L ±3.9 % PFH S Concentratio n (ng/mL ) 83 9 85 0 NA'^ ' NA(^> 188 0 %Recover y

N A N A NA<^ > NA<^ > 105 84 5 ng/m L ±1.3 % PFO S Concentratio n (ng/mL ) 95 1 99 7 NA'^ ' NA<^ > 203 0 %Recover y

N A N A NA'^ > NA'^ > 107 97 4 ng/m L ±4.7 %
N A= No t Applicabl e (1 ) Adilutio n o ftti e sampl e wa s no t prepare d a s th e spik e leve l wa s no t expecte d t o b e appropriat e a s compare d t o th e sampl e concentrations

.

Pag e 2 2 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 12

. G W227LQ 1 Y1 0 L F

3IVILIMSI D GLP l CM)1-02-02-08 5 GLP l 0-01-02-02-08 6 GLP10-01-02-02-08 7 GLP l 0^1-02-02-08 8 GLP10-01-02-02-08 9 Averag e Concen t Descriptio n

GW227LQ 1 Y1 0 LF

O GW227LQ 1 Y1 0 LF 1 GW227LQ1Y1 0 LFL S GW227LQ1Y1 0 LFM S GW227LQ 1 Y1 0 LFH S ratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 34 9 33 5 NA<^ > NA'^ ' 148 0 %Recover y

N A N A NA*^ > NA'^ > 11 2 34 2 ng/m L ±4.1 % PFH S Concentratio n (ng/mL ) 65. 2 62. 2 NA<^ ' NA<^ > 112 0 %Recover y

N A N A NA<^ > NA<^ > 10 8 63. 7 ng/m L ±4.7 % PFO S Concentratio n (ng/mL ) 30 5 26 9 NA'^ ' NA<^ > 126 0 %Recover y

N A N A NA<^ ' NA<^ ' 98. 3 28 7 ng/m L ±13 % NA= No t Applicabl e (1 ) Adilutio n o fth e sampl e wa s not prepare d a s th e spik e leve l wa s not expecte d t o b e appropriat e a s compare d t o th e sampl e concentrations

. Tabl e 13

. G W227RQ 1 Y1 0 L F

3MLIIVISI D GLP l 0-01-02-02-00 1 GLP10-01-02-02-00 2 GLP10-01-02-02-00 3 GLP10-01-02-02-00 4 GLP10-01-02-02-00 5 Descriptio n GW227RQ 1 Y1 0 LF

O GW227RQ 1 Y1 0 LF 1 GW227RQ1Y1 0 LFL S GW227RQ1Y1 0 LFM S GW227RQ1Y1 0 LFH S Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 23. 0 24. 6 NA<^ ' NA'^ ' 117 0 %Recover y

N A N A NA'^ ' NA'^ ' 11 2 23. 8 ng/m L ±6.7 % PFH S Concentratio n (ng/mL ) 16 9 16 9 NA<^ ' NA<^ ' 121 0 %Recover y

N A N A NA<^ > NA<^ > 10 6 16 9 ng/m L ±0.0 % PFO S Concentratio n (ng/mL ) 92 0 99 1 NA<^ ' NA<^ > 195 0 %Recover y

N A N A NA<^ ' NA<^ ) 10 0 95 6 ng/m L ±7.4 % NA= Not Applicabl e (1 ) Adilutio n oftti e sampl e was no t prepare d a s th e spik

e leve l was no

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

.

Pag e 2 3 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarch/Apri l 201 0

Tabl e 14

. GWGRS04Y10L F

3IVILIIVISI D GLP10-01-02-02-03 6 GLP10-01-02-O2-03 7 GLP10-01-02-02-03 8 GLP10-01-02-02-03 9 GLP10-01-02-02-04 0 Averag e Concen t Descriptio n

GWGRS04Q1Y1 0 LFO GWGRS04Q1Y1 0 LF 1 GWGRS04Q1Y1 0 LFL S GWGRS04Q1Y1 0 LFM S GWGRS04Q1Y1 0 LFH S •atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 180 0 205 0 NA'^^ ' NA'^ > 273 0 %Recover y

N A N A NA<^ ' NA<2 > 78. 9 193 0 ng/m L ±13 % PFHSf " Concentratio n (ng/mL ) 581 0 636 0 NA<2 ' NA<^ ' 714 0 %Recover y

N A N A NA<^ ' NA<= ' N C 609 0 ng/m L ±9.0%*^ ' PFO S Concentratio n (ng/mL ) 151 0 129 0 NA<^ ' NA<2 ' 273 0 %Recover y

N A N A NA<^ ' NA<^ ' 134 ^ 140 0 ng/m L ±16 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) PFH S reporte d fro m 5/26/1 0 analysis

. (2 ) Adilutio n o fth e sampl e wa s not prepare d a s th e spike leve l wa s not expecte d t o b e appropriate a s compare d t o th e sampl e concentrations

. (3 ) Samplin g locatio n di d no t have a n appropriate fiel d matri xspik e leve l fo rPFHS

. (4) Fiel d matri xspik

e di d no t mee t metho d acceptance criteri a of100 % ±30%

. Since th e metho d analytica l uncertaint yfo rPFO S i s 100 % ±44% , n o adjustmen t was mad e t o th e analytica l uncertainty

.

Pag e 2 4 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 15

. G W310RQ 1 Y1 0 C P

3IVILIMSi D GLP10-01-02-02-02 6 GLP10-01-02-02-02 7 GLP10-01-02-02-02 8 GLP10-01-02-02-02 9 GLP10-01-O2-02-03 0 Averag e Concen t Descriptio n

GW310RQ 1 Y1 0 CP O GW310RQ 1 Y1 0 CP I GW310RQ 1 Y1 0 CPL S GW310RQ 1 Y1 0 CPM S GW310RQ1Y1 0 CPH S •atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 40 1 37 0 NA<^ ) NA<^ > 143 0 %Recover y

N A N A NA<^ ' NA<^ ' 102 38 6 ng/m L ±8.0 % PFH S Concentiatio n (ng/mL ) 43 5 41 2 NA<^ ' NA<^ ' 141 0 %Recover y

N A N A NA<^ ' NA<^ ' 10 0 42 4 ng/m L ±5.4 % PFO S Concentiatio n (ng/mL ) 78 0 73 9 NA'^ > NA'^ > 173 0 %Recover y

N A N A NA<^ > NA<^ > 98. 0 76 0 ng/m L iS.4 % NA= No t Applicabl e (1 ) Adilutio n o fth e sampl e wa s not prepare d a s tti e spik e leve l wa s not expecte d t o b e appropriate a s compare d t o th e sampl e concentrations

. Tabl e 16

. G W312RQ 1 Y1 0 C P

3MLIIVISI D GLP10-01-02-O2-09 0 GLP10-O1-02-02-09 1 GLP10-01-02-02-09 2 GLP10-01-02-02-09 3 GLP10-01-02-02-09 4 Averag e Concen t Descriptio n

GW312RQ1Y1 0 CP O GW312RQ1Y1 0 CP I GW312RQ1Y1 0 CPL S GW312RQ1Y1 0 CPM S GW312RQ 1 Y1 0 CPH S •atio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 122 0 122 0 NA<^ > NA<^ > 224 0 VoRecover y

N A N A NA<^ ' NA*^ ' 100 122 0 ng/m L ±0.0 % PFH S Concentratio n (ng/mL ) 94 9 94 2 NA'^ > NA<^ > 197 0 VoRecover y

N A N A NA<^ > NA<^ > 104 94 6 ng/m L ±0.74 % PFO S Concentratio n (ng/mL ) 171 0 179 0 NA'^ ' NA<^ > 280 0 VoRecover y

N A N A NA<^ ' NA<^ ' 10 6 175 0 ng/m L ±4.6 % NA= No t Applicabl e (1 ) Adilutio n oftti e sampl e wa s no t prepare d as tti e spik

e leve l wa s no

t expecte d t o b e 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 fiel d matri xspike level

.

Pag e 2 5 o f5 7GLP10-01-02 ; Interi m Repor t 02 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 17

. G W317LQ 1 Y1 0 C P

3 M LIM S I D GLP10-01-02-02-02 1 GLP10-01-02-02-02 2 GLP1(W)1-02-02-02 3 GLP10-01-02-02-02 4 GLP10-01-02-02-02 5 Descriptio n GW317LQ1Y1 0 CP O GW317LQ 1 Y1 0 CP I GW317LQ1Y1 0 CPL S GW317LQ1Y1 0 CPM S GW317LQ1Y1 0 CPH S Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 0.53 6 0.53 1 1.7 8 11 6 NA<^ > VoRecover y

N A N A 12 2 11 3 NA'^ ' 0.53 4 ng/m L ±0.94 % PFH S Concentratio n (ng/mL ) 0.68 8 0.69 3 1.8 5 102 NA(^ ' VoRecover y

N A N A 11 8 10 3 NA<^ ' 0.69 1 ng/m L ±0.72 % PFO S Concentratio n (ng/mL ) 2.4 8 2.3 9 2.9 8 76. 2 NA<^ ' VoRecover y

N A N A N C 74. 5 NA<^ ' 2.4 4 ng/m L ±3.7 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

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

e leve l wa

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

. Tabl e 18

. G W324LQ 1 Y1 0 C P

3 M LIM S I D GLP10-01-02-02-00 6 GLP10-01-02-02-00 7 GLP10-01-02-02-00 8 GLP10^1-02-02-00 9 GLP10-O1-O2-02-01 0 Averag e Concen t Descriptio n

GW324LQ1Y1 0 CP O GW324LQ1Y1 0 CP I GW324LQ1Y1 0 CPL S GW324LQ1Y1 0 CPM S GW324LQ1Y1 0 CPH S 'atio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 94. 3 97. 0 NA'^ ' NA<^ ' 117 0 VoRecover y

N A N A NA<^ ' NA<^ > 105 95. 7 ng/m L ±2.8 % PFH S Concentratio n (ng/mL ) 98. 3 10 4 NA'^ ' NA'^ ' 113 0 VoRecover y

N A N A NA<^ > NA<^ ' 105 10 1 ng/m L ±5.6 % PFO S Concentratio n (ng/mL ) 19 2 21 4 NA<^ ' NA<^ ' 99 5 VoRecover y

N A N A NA<^ ) NA W 80. 0 203ng/mL±11 % N A= Not /Applicabl e (1 ) Adilutio n o fth e sampl e was no t prepare d as tti e spik

e leve l was no

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

.

Pag e 2 6 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVIarch/Apri l 201 0

Tabl e 19

. G W327RQ 1 Y1 0 C P

3 M LIM S I D GLP10-01-02-02-06 1 GLP10-01-02-02-06 2 GLP10-01-02-02-06 3 GLP10-01-02-02-06 4 GLP10-01-02-02-06 5 Averag e Concen t Descriptio n

GW327RQ 1 Y1 0 CP O GW327RQ 1 Y1 0 CP I GW327RQ 1 Y1 0 CPL S GW327RQ 1 Y1 0 CPM S GW327RQ 1 Y1 0 CPH S ^tio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 80. 9 70. 6 NA<^ ' NA<^ > 127 0 VoRecover y

N A N A NA'^ ' NA<^ > 11 7 75. 8 ng/m L ±14 % PFH S Concentratio n (ng/mL ) 15 6 15 2 NA<^ ' NA*^ ' 122 0 VoRecover y

N A N A NA<^ ' NA<^ ' 10 9 154 ng/m L ±2.6 % PFO S Concentratio n (ng/mL ) 69 5 58 2 NA<^ > NA<^ ' 149 0 VoRecover y

N A N A NA<^ ' NA<^ ' 86. 0 63 9 ng/m L ±18 % NA = Not/Applicabl e (1 ) Adilutio n o ftti e sampl e wa s no t prepare d as th e spik

e leve l was no

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

. Tabl e 20

. G W328LQ 1 Y1 0 C P

3 M LIM S I D GLP l 0-01-02-02-06 6 GLP l 0-01-02-02-06 7 GLP l 0-01-02-02-06 8 GLP10-01-02-02-06 9 GLP10-01-02-02-07 0 Averag e Concen t Descriptio n

GW328LQ 1 Y1 0 CP O GW328LQ 1 Y1 0 CP I GW328LQ 1 Y1 0 CPL S GW328LQ1Y1 0 CPM S GW328LQ1Y1 0 CPH S ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 77. 4 76. 2 NA(^ ) NA<^ ' 119 0 %Recover y

N A N A NA'^ > NA'^ ' 10 9 76. 8 ng/m L ±1.6 % PFH S Concentratio n (ng/mL ) 26. 0 25. 7 NA<^ > NA<^ ' 107 0 %Recover y

N A N A NA'^ > NA<^ ' 10 6 25. 9 ng/m L ±1.2 % PFO S Concentratio n (ng/mL ) 14. 5 14. 4 NA<^ ' NA'^ ' 86 5 VoRecover y

N A N A NA(^> NA<^ ' 85. 9 14. 5 ng/m L ±0.69 % NA = Not/Applicabl e (1 ) Adilutio n o fth e sampl e wa s no t prepare d as th e spik

e leve l was no

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

.

Pag e 2 7 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Tabl e 21

. G W328RQ 1 Y1 0 C P

3 M LIM S I D GLP1CW)1-02-02-05 6 GLP1CW)1-02-02-05 7 GLP10-01-02-02-05 8 GLP10^1-02-02-05 9 GLP10-01-02-02-06 0 Averag e Concen t Descriptio n

GW328RQ 1 Y1 0 CP O GW328RQ 1 Y1 0 CP I GW328RQ 1 Y1 0 CPL S GW328RQ 1 Y1 0 CPM S GW328RQ 1 Y1 0 CPH S ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 35. 6 36. 3 NA<^ ' NA<^ ' 123 0 VoRecover y

N A N A NA<^ > NA<^ ' 11 7 36. 0 ng/m L ±1.9 % PFH S Concentratio n (ng/mL ) 69. 9 65. 4 NA<^ > NA<^ ' 112 0 %Recover y

N A N A NA*^ ' NA'^ > 107 67. 7 ng/m L ±6.7 % PFO S Concentratio n (ng/mL ) 15 9 132 NA<^ > NA<^ ' 111 0 VoRecover y

N A N A NA<^ ' NA<^ ' 97. 4 14 6 ng/m L ±19 % N A= No t /Applicabl e (1 ) Adilutio n ofth e sampl e was not prepare d as tti e spik e leve l was no

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

. Tabl e 22

. G W330LQ 1 Y1 0 C P

3 M LIM S I D GLP10-01-02-02-01 6 GLP10-01-02-02-01 7 GLP10-01-02-02-01 8 GLP10-01-02-02-01 9 GLP10^1-02-02-02 0 Averag e Concen t Descriptio n

GW330LQ 1 Y1 0 CP O GW330LQ 1 Y1 0 CP I GW330LQ 1 Y1 0 CPL S GW330LQ1Y1 0 CPM S GW330LQ1Y1 0 CPH S •atio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 51 9 48 9 NA<^ ' NA<^ ' 157 0 VoRecover y

N A N A NA<^ * NA<^ ' 105 504ng/m L ±6.0 % PFH S Concentratio n (ng/mL ) 40 5 40 0 NA'^ ' NA'^ ' 146 0 VoRecover y

N A N A NA'^ ' NA'^ ' 10 8 403ng/mL±1.r/ o PFO S Concentratio n (ng/mL ) 15 5 13 5 NA<^ > NA<^ > 110 0 VoRecover y

N A N A NA<^ ' NA<^ > 96. 5 14 5 ng/m L ±14 % N A= No t /Applicabl e (1 ) Adilutio n o fth e sampl e was no t prepare d as th e spik

e leve l wa s no

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

.

Tabl e 23

. G W330RQ 1 Y1 0 C P

Pag e 2 8 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarcii/Apri l 201 0

3 M LIM S I D GLP10-01-02-02-01 1 GLP10-01-02-O2-01 2 GLP10-01-02-02-01 3 GLP10-01-02-02-01 4 GLP10-01-02-02-01 5 Averag e Concen t Descriptio n

GW330RQ1Y1 0 CP O GW330RQ1Y1 0 CP I GW330RQ1Y1 0 CPL S GW330RQ1Y1 0 CPM S GW330RQ1Y1 0 CPH S •atio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 452 0 441 0 NA<^ > NA<^ > NA(^> VoRecover y

N A N A NA<^ ' NA<^ ' NA<^ > 447 0 ng/m L ±2.5%^ ^ PFH S Concentratio n (ng/mL ) 26 4 25 1 NA<^ > NA<^ > 131 0 VoRecover y

N A N A NA<^ > NA<^ ' 10 7 25 8 ng/m L ±5.0 % PFO S Concerttratio n (ng/mL ) 76 3 75 5 NA<^ ' NA'^ ' 171 0 VoRecover y

N A N A NA<^ ' NA<^ ' 96. 1 759ng/mL±1.1 % N A= No t /Applicabl e (1 ) Adilutio n ofth e sampl e was no t prepare d a

s tti e spik e leve l was no

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

. (2 ) Analyt e concentratio n exceede d calibratio n range
. Furthe rdilutio n o fth e sampl e wa s not prepare d as tti e spike leve l wa s no t appropriate a s compare d t o th e sampl e concentration

. (3) Samplin g locatio n di d not hav e a n appropriate field matri xspik e level

. Tabl e 24

. G W331SQ 1 Y1 0 C P

3 M LIM S I D GLP l 0-01-02-02-04 6 GLP l 0-01-02-02-04 7 GLP10-01-02-02-04 8 GLP10-01-O2-02-04 9 GLP10-01-02-02-05 0 Averag e Concen t Descriptio n

GW331SQ 1 Y1 0 CP O GW331SQ 1 Y1 0 CP I GW331SQ 1 Y1 0 CPL S GW331SQ 1 Y1 0 CPM S GW331SQ1Y1 0 CPH S 'atio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 32 7 37 1 NA<^ ' NA<^ > 148 0 %Recover y

N A N A NA'^ ' NA'^ ' 11 1 34 9 ng/m L ±13 % PFH S Concentratio n (ng/mL ) 39 8 45 4 NA<^ ' NA<^ ' 145 0 VoRecover y

N A N A NA<^ ' NA<^ ' 10 4 42 6 ng/m L ±13 % PFO S Concentratio n (ng/mL ) 82 4 102 0 NA<^ > NA<^ > 181 0 VoRecover y

N A N A NA<^ > NA<^ ' 89. 7 92 2 ng/m L ±21%^ ^ N A= No t /Applicabl e (1 ) Adilutio n ofth e sampl e wa s no t prepare d a

s th e spik e leve l was not expecte d t o b e appropriate as compare d t o th e sampl e concentrafions

. (2 ) Th e RP D di d no

t meet metho d acceptance criteri a of^0%

. Tabl e 25

. Tri p Blan k

Pag e 2 9 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

3 M LIM S I D GLP10-01-02-02-07 6 GLP10-01-02-02-07 7 GLP10-01-02-02-07 8 GLP10-01-02-02-07 9 Descriptio n Tri p Blan k

Sampl e Tri p Blan k

FM S Lo w Tri p Blan k

FM S Mi d Tri p Blan k

FM S Hig h PFB S

Concentratio n (ng/mL ) <0.025 5 1.28 12 0 114 0 VoRecover

y N A 12 5 11 8 11 2 PFH S

Concentratio n (ng/mL ) <0.025 8 1.2 1 11 2 107 0 VoRecover

y N A 12 3 11 4 10 9 PFO S

Concentratio n (ng/mL ) <0.51 0 1.2 1 98. 2 92 5 VoRecover

y N A 12 2 99. 2 93. 4
N A= No t /Applicabl e Tabl e 26

. Rinseat e Blank s

3MUMSI D GLP10-01-02-02-04 1 GLP10-01-02-02-O4

2 GLP10-O1-02-02-O4

3 GLP10-01-02-02-044 GLP10-O1-02-02-O4

5 GLP10-01-02-01-00 6 GLP10-01-02-01-03 1 Descriptio n Rinseate Blank i 203 L Rinseate Blank

2 203 L Rinseate Blank

s 203 L Rinseate Blank

4 203 L Rinseate Blank

s 203 L DA L DF05 S S SS0 7 2 001 0 DALDF11SSSS0 7 2 001 0 PFB S Concentratio n (ng/mL ) <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 VoRecover y N A N A N A N A N A N A N A PFH S

Concentratio n (ng/mL ) <0.025 8 <0.025 8 <0.025 8 <0.025 8 <0.025 8 <0.025 8 <0.025 8 VoRecover y N A N A N A N A N A N A N A PFO S

Concentratio n (ng/mL ) <0.51 0 <0.51 0 <0.51 0 <0.51 0 <0.51 0 <0.51 0 <0.51 0 VoRecover y N A N A N A N A N A N A N A
N A= No t Applicabl e

3 0 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Laborator ycontro l spike s an d fiel d matri xspike s were use d t o detemnin e th e anaiytic^a ! 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

.

Al l remainin g sample s an d associate d projec t dat a (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures

.

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 3 1 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L i\/larcl^/Apri l 201 0

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

### ^/?0/^<y/ 0 Willia m K

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



# -7

. 

# tet 1 0 Gar yHoherifeteiri^ponso rRepresentative

StudyDi n 

# \UJi / Dat e



# m o / 7 Date Jaisimh a Kesari , Stud yDirecto r

Pag e 3 2 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2



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

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

PROTOCO L AMENDMEN TNO

. 2



## Amendment

Date : Marc h 24

. 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

GLP l 0-01-0 2

Pag e i o f7 Pag e 3 3 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarch/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2 

### 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 : 

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

.

AUENDTOREAD : 

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

. Thi s amendmen t onl y addresse 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 ofth e 3 M Decatu rPhas e 3 Progra m fo rPFOS

. PFH S an d PFB S (GLP10-01-02)

. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e ofMarc h 26

. 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 2 an d reporte d a s interi m repor t GLPl0-01-02-02

. (reflectin g stud yGLP10-01-0 2 an d amendmen t -02)

.

Reason : 

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

.

Pag e 2 o f7 Pag e 34 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0 

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

t 2 

## Amendmen t

Approval 

# f^ t % ) Gar yHohenstein , Sponso rRepresentative

Clesto n C

. Lange , Principa l Analytica l Investigato r Dat e 

# j/z^/2.i>/ ^ Dat e

^S~'/^-/M<'y^.^ o Willia m Reagen , EH S Opn s Environmenta l La b Managemen t Dat e



# 4S

-
^ /bat e Jaisimh a Kesar i P.E. , DEE , Stud yDirecto r

Pag e 3 ot 7 Pag e 3 5 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IMarch/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2


### Environmenta l Healt h & Safet yOperations , Environmenta l Laborator y

Genera l Projec t Outlin e To : Gar

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

Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charie s Young , Westo n Solution s Ti m Frinak , Westo n Sdution s Date : Marc h 24 , 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 # 2 - Decatu rI* * Quarte r Groundwate rSamplin g 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r ProJQC t Schedulerros t Datv s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S OperatiorJ S 3IVI Buiidin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone : (651 ) 737-367 0 Qahohenstein@mmm.con n 3li a Environmenta l Laborator yManagemen t Willia m I C Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wlcreaQen@mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 ppi^nq^mmmco m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timolhv.frinakiaiwestonsolutions.co m Phone : (334)-332-912 3 GLP1&41-02-0 2 Dept #530711 , Project #002267444 9 Samplin g schedule d fo rth s wss k o fMarc h 29,201 0
Al l verba l an d writtB n correspondenc e wil l b e directe d t o GaryHohenstein

. Pag e 4 o f7 Pag e 3 6 o f5 7GLP l 0-01-02 ; Interi m Repor t 0 2 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2


### 2 Backgroun d Informatio n an d Projec t ObJective(s )
Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m seventee n groundwate rwell s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS)

. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792

. Groundwate rsample s fro m Decatur , A L wil l b e collecte d byWesto n Solution s personne l th e wee k o f Marc h 29 , 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 fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP l 0-01-02
- 02

. 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 fMarc h 29 , 2010

. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l o n Friday , Marc h 26,201 0 t o th e attentio n o fKeit h Schmuck. , 3 M Cordova Environmenta l Engineer

. Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection

. Marti n Smit h \

Westo n Traile r 3 M Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 

### 4 Tes t Parameter s Th e targete d limi t o fquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS , PFHS , an d PFOS

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

. Samplin g locatio n description s were not availabl e a t th e tim e o fsampl e bottl e preparation

. Fo reac h samplin g kx:ation , a tota l o ffive sampl e bottle s wil l b e collecte d (sample , sampl e duplicate , low-leve l field matri xspike , mid-leve l field matri xspike , an d high-leve l fiel d matri xspike)

. Th e lii l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 O m L Fou rset s o ftri p blank s consistin g o freagent-grad e water , a tow-level tri p blan k spike , mki-leve l field spike an d a high-leve l tri p blan k spike wil l b e prepare d a t th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe r bottles

. Th e lowfield matri xspik e wil l b e prepare d at 1 ng/nnL , th e mi d field matri xspik e a t 100 ng/mL , an d th e hig h fiekl matri xspike a t 100 0 ng/mL

. Five additiona l bottle s wil l b e prepare d t o b e use d h rth e preparatio n o f th e equipmen t rinseate blanks

. Atotei l o f106 sampl e bottle s wil l b e prepared

. Al l sampl e bottle s wil l includ e th e additio n o f^*OrPFBS , ^^OrPFHS , an d '^C«-PFOS , 1802.PFB S (intema l standards ) a t a nomina l concentratio n of1 ng/m L Al l sampt e bottle s wil l als o includ e th e additio n o f^'C4-PF0 S (sunnogat e spike ) a t a nomina l concentratio n o f0. 1 ng/mL

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

yHig h Performance Liqui d Chromatography/Mas s Spe(*x3metr yDirec t Injectio n Analysis"

. Th e dat a qualityobjective s fo rthes e studie s ar e quantitativ e results fo rth e targe t analyte s wit h a n analytk^ l accurac

yo f100±30%

. Fiel d matri xspike s not yieldin g recoverie s wi&ii n 1001:30% wil l b e addresse d i n th e repor

t an d th e final acctjrac

ystatemen t mayb e adjuste d accordingly

. Alternately , sample s ma

yb e analyze d b yET S 8-154. 3 "Determinatio n o fPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rBySoli d Phas e Extractto n an d Hig h Performance Liqui d Chromatography/Mas s Spectromefry"

. Metho d Ers-8-15 4 ha s bee n validate d fo rPFOAan d PFO S only ;GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVIarch/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2 however , specifi cqualit

ycontro l sample s analyze d wit h th e sample s wil l b e use d t o detennin e overal l metho d precisio n an d accuracy
. 

### 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e result s fo rth e sample , sampl e duplicate , an d th e thre e field matri xspikes

. Asingl e tri p blan k an d thre e tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an yequipmen t blank

s prepare d i n th e field. Laborator ycontro l spike s o freagen t wate rprepare d at th e tim e of sampl e extractio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d precision

. Metho d blank

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

. /Mi ylaborator ymatri xspike s that ma

yt> e prepare d wil l als o ti e include d i n th e final report
7 Emai l Correspondenc e Attachmen t /K

: Samplin g Bottl e Request

Pag e 6 o f7 Paff e 3 8 o f5 7GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVIarch/Apri l 201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 2 

# Bottl e Reques t

- GLPlO-01-0 1 /

GLPlO-01-0 2 QU O Decatu r

Groundwate r

Samplin g 02181.129.145.000 1

DAT EREQUESTED : 1 7 Marc h201 0 No

. o f Sample s Sampl e Tvp e Comment 5 Groundwater Anticipate highVO C concentration s 1 2 Groundwater Averag e Sample s 1 Rinseate Sampl e Wil l nee dHPL C water 4 Tri p Blank s Anticipate 1 pe r cooler Note : Some o f

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

. 

# BOTTLE S REQUIRE D B Y 2 6 MARC H 201 0 Shippin g Address : Marti nSmit h\Westo nTraile r 3 M Decatu r

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

Pag e 7 o f7 Paff e 3 9 o f5 7"* * Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , AL^gg^j^j- g Name
March/Apri l 201 0 gl00517a.rd b 

# r Sampl * Nanw : -g100517a02 rSampt e ID : "0 8 008-147-10 " Fite : " g 100517a.wif T Paa k Namo : 'ptbs ' Mass(«s) : -299.0/99. 0 amu,299.0/80. 0 amu,299.0/130. 0 ami T Comman t "5. 0 pp b curv a poin t i n Mi i Q Watsi " Annotation:" " Sarapl e Indey ; 2 7 Satnpl e Type ; Concentration : Calculate dConc : Acq

. Date :
Modified ; R T Window : Expecte dRT : L's e Relativ e RT : ng/m L

Height : Star t T : En d Tim

. 797566 1 c i 2I0OOOO , 10. 2 10. 7 Z1a 6 2.0e 6 1.9a 6 1.ea 6 1.7a 6 1.6a 6 1.5a 6 1.4a 6 1.3a 6 1.2a 6 1. 1 a 6 1.0a 6 9.08 5 8.0a 5 7.0a 5 6.0a 5 5.0a 5 4.0B 5 3.0a 5 2.0a 5 I.Oa S 10.3 7

I 

# I San^aNam8;"g100517a074 ' Sampt e ID:'GLP1(M)1-02-02O01 " Fite ; •g100517a.wi r Paa k Nama : 'ptbs ' Mass(as) : "299.0/99. 0 amu,299.0/80. 0 amu,299.0/130. 0 amu ' Commant-GW227RQ 1 Y1 0 LF0{dil1:100) ' Annotation:- '

1.05a 5 I.OOaS

9.50a4

- 9.00a 4 8.50a 4 8.00a 4 7.50a 4 7.00a 4 6.50a 4

e 6.00e 4 is

- 5.50o 4 S S I 5.00a

4 4.50a4 4.00a4 3.50e 4 3.00a 4 Z50a 4 Z00a 4 1.50a 4 1.00e 4 5000.00

- 0.0 0 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 Ttme

. mi n Sampl e Type : Concentration : Calculate dConc Acq

. Date : Acq

. Time : Modified : R T Window : Expecte dRT : Unknow n H/ A < 0 5/1B/201 0 !:;2:1 3 A

M Ye s 30. 0 10. 4 

# I Sampt e Nanw : -fl100517a059 " Sampt a ID : 'Sotven t btani C Fite : 'g1O0517a.wH r Paa k Nama : 'ptbs " Mass<es) : "299.0/99. 0 amu.299.0/80. 0 amu.299.0/130. 0 amu * ComntanfMiniQWatarTNIOOISS " Annotation: " Sampl e Index : 5 9 5000 480 0 460 0 440 0 420 0 400 0 380 0 360 0 340 0 320 0 3000

- 280 0 260 0 24O 0 220 0 200 0 1800

- 160 0 1400

- 120 0 1000

- 80 0
..•iJ|i-^.i^..,...L,...iii,li i I , I 11 , ifUttp m 

# I Sanpt e Nama : "g100517a168 ' Sampi a ID : "LCS-100517-22
- Fite : "g100517a.v* r Paa k Nama : 'pfba ' M8ss{es) : -299.0^. 0 amu,299.0/S0. 0 amu,299.0/130. 0 ami T Comman t "30pp b LC S EC P Annotation : " Sampl e Index : 16 B Sampl e Tvpe : Concentration : Calculate d Con c Acq

. Date : Acq

. Tirae : Modified : R TWindow : Expecte d RT : L'nknow n N/ A 23. 0 5/13/201 0 5:52:3 0 At Ye s 30. 0 10. 4

Height : Star t ' En dTi r Sampl e Type : Concentration : Calculate d Con c Acq

. Date : Acq

. Time : Modified : R TWindow : Expecte d RT : Us e Relativ e R

T Int

. Type : Retentio n Time : Area ; Height : Q C 0.0 0 0.40 7 5/19/201 C 12:15:4 1 Ye s 30. 0 10. 4 N o Manua l 10. 4 9636 4 C

O 183000

. c ng/m L

ng/m L P H

ss c mi n

mi n jnt s p s

>-"l-8 ' 12.99,13.3 6 ^^ ^ * • ...^WlWWllV

, M

. S
Dat aworke du p b y ST W Printin g Time : 3:24:0 4 P M Printin g Date : Tuesday , Jun e 29 , 201 0 Pag e 1 o f 3 Pag e 4 0 o f 5 7Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , ALj^ggult s Name : gl00517a

. rd b March/Apri l 201 0

• Sampl a Name:'g100517a027 ' Sampt e ID : "0 8 006-147-10 " FBo ; "g100517a

. I Paa k Nama : "pths ' Masa^ea) : -399.0/99. 0 amu,399.0/80. 0 amu,399.Qyi30. 0 amu " I Comman t '5. 0 pp b curv a poin t i n Mi l Q Watar " Annotation : Sampl e Index : Sampl e Type ; Concentration : Calculate dConc : Acq

. Date : Acq

. Time : Modified : Ye s R T Window : 30. 0 Expecte dRT : 11. 8 Us e Relativ e RT : N o

106J125 1 2810000

. 11. 5 Sampt e Nama : •g^0QSi^aQ5S rSampt e ID : "Solven t l>lanI TFite : "g100517a.wi r Pea k Nama : 'pfhs " Maat(ea) : "399.0/99. 0 amu.399.0/80. 0 amu,399.0/130. 0 amu " Commen t 'Mill i 0 Wtato rTN10O153 " Sampl e Index : 5 9 1.20ft4 ' 1.15a 4 1.106 4 1.05e 4 1.00a 4 9500.00 9000.00

s 8500.00 8000.0 0 7500.0 0 7000.0 0 §-6500.0 0 'I'6000.0 0 I 5500.00 5000.00 4500.00 4000.00 3500.00 3000.00 2500.00

- Sampl e Type : Concentratl o Calculate d Con c Acq . Date : Acq . Time : Modified : Proc . Algorith m Nois e Perce n a q Unicnown N/ A 0.0017 9 5/18/201 0 1:22:1 3 A M
N o IntelliCu a : 5 0 Base . Sub
. Window : 1.0 0 P^ah-Split
. Factor : 5 Repor t Larg e Min
. Pea k H e Min
. Pea k W i t Peah : N o

t h Smoothin g Widt h R T Window : Ey.pecte d RT : Us e Relativ e Int . Type : Retentio n T i Area : Height : Star t Time : En d Time : R T

e : : 0.0 0

0.0 0 0 30. 0 11. 6 H o Bas e T o B a 11. 6 4 00 3 CO U 723
. c p 11. 5 11. 7

2000.00 ' 1500.0 0

500.0 0 0.0 0 ^,.1 , , . I I ll f,l,ti,lij l
Sanpt e Name : "glOOSnalSe " Sampt e ID : "LCS-100517-2 rFite : '3100517a.wtf T Pea k Name : "ptha * Maa8(ea) : "399.0/99. 0 aniu.399.0/80. 0 amu.3gg.0/130. 0 ami T Commen t '30pp b LC S EC P Anrmtation : * " Sampl e Index : 15 8 Sampl e Type : Q C Concentration : 0.0 0 ng/m L9.0e 5 Calculate dConc : 1.9 9 ng/m L Acq

. Date : 5/19/201 0 „-^ e Acq

. Time : 12:16:4 1 P M °-^ ° Modified : Ye s 8.0* 5 R T Window : 30. 0 se c

-T : 11. 6 mi n 7.5. 5 v o BT : H

o Manua l 7.0e5 Time : 11. 6 mi n 399832 4 count s 6.5a5 908000

. cp s 11. 4 mi n - 11. 5 mi n ®-°» 5 5.5e 5 I 5.0e 5
#4.5e 5 I

3.0e5
2.5* 5
Z0» 5
1.5* 5
1.0* 5
5.0* 4
0. 0 

# I Sampl * Name : 'g100517a074
- Sampt e ID : "GLP l OOI-02-02-001 ' Fite : -g100517a.M r Pea k Nama : "plhs " Ma8a(ea) : "399.0/99. 0 amu.399.0/80. 0 annu.399.0/130. 0 am f Commant"GW227RQ 1 Y1 0 LFO{dai:100 rAnnotation: " Sampl e Index : 7 4 Sampl e Type : Calculate d Con c Acq . Date : Acq . Time : Modified : R T Window : Expecte d RT : Us e Relativ e int
. Type : Retentio n T i Area : Height : Star t Time : En d Tim- : R T

3 Unknow n N/ A 169
. n g 5/19/201 0 5:52:3 0 A M
Ye s 30. 0 se c 11. 6 mi n N o
Manua l 11. 5 mi n 8200 3 count s 939000
. cp s 11. 3 mi n

1 1 1 2 1 3 1 4 1 5 1 6 Dat aworke du p b y ST W Printin g Time : 3:24:0 4 P M Printin g Date : Tuesday , Jun e 29 , 201 0 Pag e 2 o f 3 Pag e 4 1 o f 5 7Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 0 2 Analysiso fPFBS , PFHS , an d PFO S i n GroundwaterSamplestro m Decatur , A L Result s Name
- gl00517 a rd b March/Apri l 201 0

1 • Sampl * Nanw : "91005178027 " Sampt e ID : "0 8 008.147-10 " Fite:'g100517a.wi r • Paa k Nam* : 'pfoa ' Mass<*B) : '499.0/99. 0 amu,499.0ra0. 0 amu,499.0/130. 0 amu "
• Comman t '5. 0 pp b curv e poin t i n Mi i Q Watar " Annotation: " Sampl e Index : 2 7 Sampl e Type : Standar d Concentration : 5.1 0 ng/m L Calculate d Conc : 5.0 9 ng/m L -J-f i Acq

. Date : S/17/201 0 ^^ ^ Acq

. Time : 3:46:4 8 PM 2.3* 6 Modified : Ye s 2.2* 6 R TWindow : 30. 0 se c Expecte d RT : 12. 4 ni n 2.1* 6 Ua e Relativ e RT : N o jOe B Int

. Type : Manua l 19* 6 Retentio n Time : 12. 4 mi n Area : 972568 5 count s 1.8*6
- Height : 2510000

. cp s Star t Time : 12. 1 mi n 1.7*6
- En d Time : 12. 7 mi n , g^ g 1.5* 6 1 1.3* 6 1 1.2* 6

- 1.1* 6 1.0* 6 9.0* 5 6.0* 5 7.0* 5 6.0*5
- 5.0e 5 4.0e5
- 3.0* 5 2.0*5 ' 1.0* 5

"• ° i 2 3 4 5 " e

• Sampl e Nanrw : 'g100517a074 " Sampt e ID : "GLPltM)1-02-02-001 ' Fite : 'gl00517a.v« r 1 Paa k Name : "ptoa ' Mass(*»):'499.099. 0 amu,499.0/80. 0 amu.499.0/130. 0 amu '
• Comm*nt-6W227RQ1Y1 0 LFO{dK1:100 rAnnotation:
- Sampl e Index : 7 4 Sampl e Type : Uriknow n Concentration : N/ A Calculate d Conc : 920

. ng/m L Acq

. Date : 5/18/201 0 2.2e6 ' Acq

. Tirae : 5:52:3 0 A M 2.1.6
- Modified : Ye s ,- ^ R TWindow : 30. 0 se c^'^ ^ Expecte d RT : 12. 4 mi n 1 9e 6 Us e Relativ e RT : N o 1.ee 6 Int

. Type : Manua l Retentio n Time : 12. 4 mi n 1.7* 6 Araa : 1717574 4 count s Height : 2300000

. cp s 1.6*6
- Star t Time : 12. 0 mi n En d Time : 12. 6 mi n 1.5*6
- 1.4*6
-

1 1.1* 6

- 1.0*6 ' 9.0* 5 • 8.0*5
- 7.0*5
- 8.0*5
- 5.0*5
- 4.0*5
- 3.0*5
- 2.0*5
- 1.0*5
- 0.0- J • • • • • • • 1

. 1 • r

1 2 3 4 5 6 12-4 2

I 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 Time , mi n

124 1

12.2&,

.

1Z16

. h 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 • Sampt e Name:'g100517a05 ? Sampt e ID:'Sohen t tilani rFBa:-g100517a.<M r • Paa k Nama;'pfos
- Ma«a<es) : "499.0199. 0 amu,499.0ffi0.0amu,499.0/130. 0 amu "
• Comman t "Min i 0WatefTN10«15 rAnnotation : " Sampl e Index : S 9 Sampl e Type : Unknow n Concentration : N/ A Calculate d Conc : 0.14 4 ng/m L 650 0 Acq

. Date : 5/18/201 0 Acq

. Time : 1:22:1 3 A M gQQ
Modified : Ye a R TWindow : 30. 0 se c750 0 Expecte d RT : 12. 4 mi n Us e Relativ e RT : N o y^j ^ Int

. Type : Manua l Area : 3146 7 count s Height : 8020

. cp s p-_ - Star t Time : 12. 2 mi n ^°° ° En d Time : 12. 5 mi n 550 0
500 0 1

> , 450 0
1 400 0
350 0
300 0
250 0
200 0
150 0
100 0
50 0 1 ,*,jJL-..L_L.li.i^*._iJL-. j 1 h

. uiuJHi i 

## J 1 1



# i .f l i l i 

# m \ 1 lu W" 

# I ,]J r W r1 w ^ iji f- " 1 .i^jtm m \ \ mm^"' ^ V i 2 3 4 5 6 7 8 9 1 0 i' l 1 2 1 3 1 4 1 5 1 6 |

• Sampt e Name:'gl00517a168 ' Sampt e ID : •LCS-100517-22 ' Fite:'g100517a.wi r • Pea k Name:'pfoa ' Ma**(*»):-499.0ira9.0amu,499.0/80.0amu,499.0r t 30. 0 amu "
• Comman t -30pp b LC S EC P Annotation : " ' Sampl e Index : IS B Sampl e Type : QC Concentration : 30. 0 nq/m L Rn» e Calculate d Conc : 37. 4 ng/m L o.iw
- Acq

. Date : 5/19/201 0 Acq

. Time : 12il6:4 1 P M 7.5^ 5 Modified : Ye s R TWindow : 30. 0 se c7.0* 6 Expecte d RT : 12. 4 mi n Ua e Relativ e BT : N o Int

. Type : Manua l Retentio n Time : 12. 4 mi n 60* 6 Area : 5362241 7 count s Height : 6140000

. cp s Star t Time : 12. 0 mi n 5.5* 6 En d Time : 12. 8 mi n 5.0* 6 1 4.5* 6 J f 1 4.0* 6 1 3.5* 6
a0a 6
Z5* 6
Z0* 6
1.5* 6
1.0* 6
5.0* 5

°' ° i 2 3 4 1 Time , mi n

12.4 5

12.32s

.

12.2 0 1 1 1 6 7 8 9 1 0 i' l 1 2 1 3 1 4 1 5 1 6 | | ^ Jm^ m I I Dat aworke du p b y ST W Printin g Time : 3:24:0 5 Printin g Date : Tuesday , Pag e 3 o f 3 P M Jun e 29 , 201 0 Pag e 4 2 o f 5 7Ginge r AG0133050 9 GLPlO-01-02 ; Interi m Repor t 0 2 Analysiso fPFBS , PFHS.an d PFOSinGroundwaterSamplesfro m Decatur , A L Result s Name : gl00517 a rd b March/Apri l 201 0 g100517a.rd b (pfbs) : "Quadratic " Regressio n (" 1 Ix " weighting) : y= -1.3e•^004 x'^ 2 + 1.71e•^00

6 x• ^ 3.98e+00 3 ( r= 0.9996 )

- T' 1 ~ ~ l 1 T " 0 8 " T' r ~ " T ' r ^ 1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 32 3 4 3 6 3 8 4 0 4 2 4 4 4 6 4 8 5 0 Concentration , ng/m L Dat a worke d up byST W Printin g Time : 3:24:2 6 P M Printin g Date : Tuesday , Jun e 29 , 201 0 Pag e 1 o f 1
Pag e 4 3 o t 5 7Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 0 2 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L Result s Name : gl00517a

. rd b March/Apri l 201 0

Dat aworke du p b y ST W Printin g Time : 3:24:4 5 P M Printin g Date : Tuesday , Jun e 29 , 201 0 Pag e 1 o f 1 Pag e 4 4 o f5 7»* * Ginge r AG0133050 9 GLPlO-01-02 ; Interi m Repor t 0 2 Analysiso fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L Result s Name
- gl00517 a rd b Marcti/Apri l 201 0

Dat aworke du p b y ST W Printin g Time : 3:25:0 7 P M Printin g Date : Tuesday , Jun e 29 , 201 0 Pag e 1 o f 1 Pag e 4 5 o f5 7GLPlO-01-02 ; Interi m Re9o9SiJiTi®n t "is y'o B usGcl , I fcufrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



# Environmenfa l Laboratory

l\/letiio d Metiio d o fAnalysi s fo rtti e Determinatio n o fPerfluorinate d Compound s i n Wate r b yLC/MS/MS ; Direc t Injectio n Analysi s Mettio d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q ^

1(2 , f o " 1

Approve d By : 

# 4^//^/ o y Willia m K

. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 Metiio d o fAnalysi s fo rth e Detenminatio n o fPerfluorinate d Conipound s i n Wate rb yLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 6 o f5 7GLP10-01-02 ; Interi m ReP)f?S^iJrnen

t ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 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 "Detemninatio n of Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"

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

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

. Sampl e collectio n i s no

t covere d unde rthi s analytica l procedure

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

. Sample s containin g heav y particulat e ma

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

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

. Thi s i s a perfomnance-base d method

. Metho d accurac yi s determine d fo reac h sampl e se t usin g multipl e laborator ycontro l spike s a

t multipl e concentrations

. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix

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

ystatements) , o rwil l no

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

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

. 

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

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

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

. 

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

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

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

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

. 3. 3 Fiel d Blan k

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

. Th e purpos e ofth e F B i s t o determin e i ftes t substance s o r othe rinterference s are presen t i n th e fiel d environment

. Thi s sampl e i s als o refen-ed t o a s a Tri p Blank

. ETS-8-044. 0 Pag e 2 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 7 of5 7GLPlO-01-02 ; Interi m R^of?S|Jrnen t ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e at th e sam e tim e fi-om th e sam e locatio n a s th e sample

. Th e FD S i s handle d unde ridentica l circumstance s an d treate d exactl yth e sam e throughou t field an d laborator y procedures

. Analysi s o

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

. 

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

. Aknown , specifi cvolum e of sampl e must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

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

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

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

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

t a n appropriat e leve l i s made

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

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

. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sampie , FSCS ) A n aliquot o fAST 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 determin e i fth e metho d i s i n contro l an d whethe ra los s o fanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues

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

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

t th e sam e tim e an d place a s eac h FMS

. 

### 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator ya t th e tim e ofsampl e extraction

. At least 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 xspik

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

. Th e LM S i s analyze d exactl ylike a laborator ysampl e t o detennin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results

. Th e endogenou s concentration s o fth e analyte s i n th e sampl e matri xmust b e 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 o fa sampl e receive d fro m th e field fo rtesting

. 

### 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits 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 LLOQ s are matrix-dependent

. Th e uppe rlimi t ofquantitatio n (ULOQ ) fo ra dataset i s th e highest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits ofprecisio n an d accurac ydurin g routin e operatin g conditions

. Th e highest standar

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

.

ETS-8-044. 0 Pag e 3 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 8 of5 7GLP10-01-02 ; Interi m R^oQQjJiTien t "la yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L IVlarcti/Apri l 201 0

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

ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that are use d wit h othe rlaborator ysamples

. Th e metho d blan k i s use d t o detemnin e i ftes t substance s o rothe rinterference s are presen t i n th e laborator y environment , th e reagents , o rth e apparatus

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

. 3.1 3 Stoc k

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

. 

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

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

. I fused , sun'ogate(s ) are adde d t o al l sample s an d qualit y contro l samples

. Sun'ogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedure includin g sampl e collection , preparation , an d analysis

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

e an d i s NO

Trequired

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

. 

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

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

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

. Th e laborator

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

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

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

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

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

. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s o fanalysi s b

yrunnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 4 9 o f5 7GLP10-01-02 ; Interi m RePoR?i-"Tient ma yb e used , i f current , fo r1 4 day s fro m 06/29/201 0 Analysi s of PFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 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 ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes

. 

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

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

t ra wdat a fo rpea k

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

. Ga s tigh t syringes , 25^1 , 50|JL , lOOpL , 250IJL , 500pL , 1000|JL

. 1 m L plasti cHPLC autovial

. Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e o fspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm
. 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 |j m Analytica l Column : Betasi l CI8,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

Are a - quadrati ccurve fit, 1/ xweighted

. Ru n Time : ~ 1 7 minutes

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

.

ETS-8-044. 0 Pag e 5 o f 1 1 Metho d o fAnalysi s fo rth e Determinatio n o f Perfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 0 o f 5 7GLPlO-01-02 ; Interi m ReQjffffi-'rnen t ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



### 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e bn , MR M mode , monitorin g th e followin g transitions : Analyt e PFBA PFPeA PFH A PFHp A PFOA PFN A PFD A PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 31 3 ^26 9 an d 31 3 ^11 9 36 3 ^ 319 , 36 3 ^

16 9 an d 36 3 ^11 9 41 3 ^ 369 , 41 3 ^

21 9 an d 41 3 - ^

16 9 46 3 - ^ 419 , 46 3 - ^

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

21 9 an d 51 3 ^

26 9 56 3 - > 519 , 56 3 ^

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

16 9 an d 61 3 - ^

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

9 9 39 9 - > 8 0 an d 39 9 ^

9 9 49 9 ^ 80 , 49 9 ^

9 9 an d 49 9 ^

13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n o fisomers tha t more closel ymatche s NM R dat a an d ma yhav e th e adde d benefi t o f increase d sensitivity

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

. Th e previou s informatio n i s intende d a s a guide , alternat e instalment s an d equipmen t ma yb e used

. 

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

. Reagen t Grad e 

### 7. 2 Standard s Perfiuorobutanoi cAci d (PFBA-C 4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n a s NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r 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 (PFOA- 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
- C1 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 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 1 o f5 7GLPlO-01-02 ; Interi m RePoffS" ^ m e n t ms yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L Marcli/April201 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 mayb e used

. 

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

. Note : Alternative volume s ma yb e prepare d a s lon g a s th e ratio s o fth e solven t t o solut e ratio s are maintained

. 

### 7. 4 Stoc k

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

d preparatio n procedure serve s a s a n example

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

. Fo rexample , p L volume s ma yb e spike d int o 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 cflask. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container

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

. Expiratio n date s an d storag e condition s ofstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure

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

.

, . X

. rX molecula rweigh t o fanio n sal t correctio n facto r= ^ moclecula rweigh t o fsal t

49 9 PFO S (K- ^ )sal t correctio n facto r= ^^ ^ = 0.927 5 53 8 1 0 m g CsFiySO

s K * wit h purit

y90 % = 8.35m g CsFuSOa" (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 (jg/m L (500 0 ng/mL ) mixe d workin g standard-^d d O.Sm L eac h ofth e lOOpg/m L SSS s t o a lOm L volumetri c flask an d brin g u p t o volum e wit h solvent

. 25 0 ng/m L mixe d workin 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 procedure o ri n a refrigerato ra t 4''±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation

.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 2 o f5 7GLPlO-01-02 ; Interi m RepoRSi^ment ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



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

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

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

.

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

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

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

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

Calibratio n Standard , ng/m L (ppb ) i n AST M Typ e 1 Water , o rothe rsuitabl e wate r 0.02 5 0.037 5 0.05 0 0.07 5 0.10 0 0.25 0 0.50 0 1.00 2.5 0 5.0 0 10. 0 

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

. Sample s containin g heav yparticulat e ma

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 centrifijg e prio rt o removin g a sampl e aliquot , o rfiltered. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial

. Plasti ci s prefen-ed ove rth e us e ofglas s autovials , t o preven t th e possibl yoffiuorochemical stickin g t o th e glass

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

. Prepar e metho d Q C sample s an d multipl e metho d blank s an d aliquot int o labele d plasti cautovials

. Prepar e a t least fiv e metho d blanks

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

d curve prio rt o eac h set ofsamples

. Th e standar d curve ma

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

xo runweighted , o rb

yquadrati cfli (

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

xo runweighted , usin g suitabl e software

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

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

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

. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfi t ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-detemnine d acceptance criteria

. Low-leve l curve points shoul d als o b e exclude d i fthei rare a count s are no t a t least twic e that ofth e metho d and/o rsolven t blanks

. Th e coefficien t ofdeterminatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.990

. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n o fth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Detemiinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 3 o f5 7GLPlO-01-02 ; Interi m R^offS^men t ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 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 , perfor m routin e maintenance o rprepare a ne wstandar d curve (i fnecessary) an d reanalyze

. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

yofth e calibratio n curve
. Analyz e a mid-rang e calibratio n standard , on e ofth e sam e standard s use d t o constmc t th e calibratio n curve , a

t a minimu m afte rever ytent h sample , not includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set

. Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable

. Th e calibratio n curve an d th e last passin g CCV wil l the n bracket acceptabl e samples

. Multipl e CCV level s ma yb e used

. Sample s containin g analyte s that 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 LO Q of0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e final report

. 10. 2 Metho d Blank s Metho d blank

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

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

. Metho d blank

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

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

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

. Th e standar

d deviatio n ofth e are a count s o fthes e metho d blank s shoul d b e calculate d an d reported

. I f th e mea n are a count s o fth e metho d blank s excee d 50 % o

fth e LOQ standard , the n th e LOQ must b e raise d t o th e first standar

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

. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l not b e exclude d fro m reporting

. Th e requiremen t fo r replicate s exclude s fleld 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

ftw o 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 o ffive 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 at concentration s nea rth e mid-poin t ofth e curve
. Th e relative standar

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

. I fth e above criteri a are no t met , th e entire se t o fsample 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 Detemiinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 4 o f5 7GLPlO-01-02 ; Interi m ReQjQSi'J'Tient ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0



### 10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s offield matri xspike s an d laborator ymatri xspike s are anticipate d t o b e betwee n 70 % an d 130 % ofth e fortifie d levels

. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagged a s suc h (wit h expande d accurac ystatements) , o rwil l no

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

. Th e targete d fortificatio n level s shoul d b e a t least 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o detennin e th e statemen t ofaccurac yfo ranalytica l results

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

. t .1 , /

IV (Pea k

Area-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 are not achieve d must b e considere d i n th e evaluatio n ofth e data

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

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

t met , maintenance ma

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

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

. I fdat a are t o b e reporte d whe n perfonnance criteri a have not 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 are 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 must have are a count s wit h a n RS D o f^5 % an d a retentio n tim e RS D o f^ % t o b e compliant

. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.990

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

yb e withi n ±30%

. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve
. Th e accurac yof eac h curv e poin t must b e withi n 25 % o fth e theoretica l valu e (withi n 30 % fo rlowest curve point)

. Sample s that are brackete d b

yCCVs no

t meetin g thes e criteri a must b e reanalyzed

.

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o fAnalysi s fo rth e Detenninatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 5 of5 7GLPlO-01-02 ; Interi m Repo(?Sil-imen

t ma yb e used , i fcurrent , fo r1 4 day s fro m 06/29/201 0 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L March/Apri l 201 0

Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

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

. 

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

. Th e LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n o fappropriat e blank s an d th e accurac

yo fth e low-leve l calibratio n curv e points

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

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

. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d accurac 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 fleld blank s o rrinse blanks

. Sectio n 1 0 contain s additiona l infomiatio 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 perfonnin g thi s metho d wil l b e dispose d ofappropriately

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

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

. 

### 1 4 Record s Eac h dat a packag e generate d fo ra stud ymust includ e al l supportin g infomiatio n fo rreconstmctio n o fth 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 , instmmen t acquisitio n method , summar

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

. 1 5 Affecte d Document s None

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

ETS-8-044. 0 Pag e 1 1 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 6 o f5 7GLPlO-01-02 ; Interi m Repor t 0 2 3 M Confidentia l Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s fro m Decatur , A L iVIarch/Apri l 201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/

. Identificatio n stud y/ Projec t No

. Date(s ) o f Occurrence : Documen t Number

. GLP10-01-02-0 2 j100517 a ETS-8-044. 0 Deviatio n typ e D SO P D Equipmen t Procedur e 0 Metho d (Chec k one ) D Protoco l IZ l GP O D Other

.

//

. Descriptio n (attac h extr a page s a s needed ) 

### Metho d Requirements : 1

. LC S averag e recover yo f 100 % ±20%

. 2

. Sample/Sampl e Duplicat e RP D S20%

. 3

. FM S recover yo f 100 % ±30%

. 

### Actua l procedure/process : (1 ) LC S averag e recover yfo rbranche d PFO S wa s >120%

. (2 ) Th e RP D fo rPFO S fo rsamplin g locatio n 331 S wa s 21%

. (3 ) Th e recover yo f th e FM S Hig h sampl e fo rGRS0 4 fo rPFO S wa s 134%

. 

### ///

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

### Correctiv e Actio n ( D Ye s 0 No ) Reference : Acceptabilit yo fth e nonconfonnin g work : 1 ) Th e branche d PFO S whe n quantitate d agains t calibratio n curv e poin t prepare d fro m linea r PFO S hav e bee n quantitatin g aroun d 15-20 % higher

. Th e se t o f 3 0 pp b branche d LC S prepare d wit h th e sample s produce d recoverie s -170%

. Th e 5 pp b branche d LC S recover y wa s withi n acceptanc e criteria , suggestin g tha t th e 3 0 pp b averag e recover yma yb e i n error
. Thre e replicate s o f branche d LC S a t 5 ppb , 1 5 ppb , an d 3 0 ppb , prepare d wit h non-stud y samples , wer e analyze d wit h th e stud ysample s t o confir m th e highe rrecovery
. Th e result s o fth e additiona l sample s wer e withi n th e field matri xspik e acceptanc e criteri a o f 100%±30%

. Al l LC S wer e use d i n th e detenninatio n o f th e analytica l uncertainty

. 2 ) Th e RP D valu e fo rPFO S fo rsamplin g locatio n 331 S wil l b e footnote d i n th e dat a tables

. 3 ) Sinc e th e metho d analytica l uncertaintyfo rPFO S i s 100 % ±44% , n o adjustmen t wa s mad e t o th e analytica l uncertaint yfo rPFO S o n GRS04

.
Actions : D Haltin g o f Wor k D Clien t Notificatio n D Wor k Recal l D Withholdin g o f Report E I Other : Deviation s wil l b e note d i n final report

. Projec t Lead/PA I Approval : Suja n Wol f H ^ Date : . Stud yDirecto r(i f GLP) : KUXfyj-J / ^

D^^®
- Sponso rApprova l (fo rGL P protoco l deviations) : N A Date : N , Technica l Reviewe r(optional) : N A Date : N A 

# W

Laborator yDepartmen t Manage rApproval : Date : 

## c:/SoAo/r J IV

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

occurred , resumptio n o fwor k mus t firs t b e approve d b yLaboratoryManagemen t Laborator yDepartmen t IVIanage rApproval : N ADate : N A 

### Deviatio n No

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

Attachmen t A ETS-4-008. 7 Pag e 1 o f 1

Documentatio n o f Deviation s an d Contro l o f Nonconformin g Testin g Pag e 5 7 o f5 7