GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o

f PFBS , PFHS , and PFO

S i n Groundwate rSample

s Avenu e AInvestigatio n Area ; Decatur, AL - Ja n 201 1

GLP10-01-02 : Interi m Repor t 1 6 - Analysi s o f PFBS
. PFHS
. an d PFO S i n Groundwate r Sample s Collecte d a s Par t o f th e Avenu e Ainvestigatio n Are a i n Decatur
. A L i n Januar y 201 1 Stud yTitl e Analysi s of Perfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g 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 , P

A1938 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 of signin g Performin g Laborator y 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

y 3 M Center , BId g 260-05-N-1 7 Maplewood , M M 55144 Projec t Identificatio n GLP10-01-02-1 6 Tota l Numbe ro f Page s

6 1

^•• ^ |H[ ^ Tli e testin g reporte d herei n mee t th e requirement

s of ISO/IE C 17025-200

5 "Genera l Requirement

s fo rth e ^d! - ^T ^

Competenc

e of Testin g an d Calibratio n Laboratories" , I n accordanc e wit h th e A2L

ACertificate #2052.01
. [ACCH^ii^ TEP J Testin g tha t complie s wit h thi s Internationa l Standar d als o operat

e I n accordanc

e wit h IS O 9001:2000
. Testin g Cer t #2052.0 1

Page 1 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

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

Pag e 2 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



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

t 1 6 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a s Par

t o fth e Avenu e AInvestigatio n Are a i n Decatur , A L i n Januar y2011
. 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 Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s where there i s n o specifi ctes t substance , n o specifi ctest syste m an d n o dosin g o fa test system
. • Th e reference substance s hav e no t bee n characterize d unde rth e GLP s an d th e stabilit yunde r storag e condition s at th e test sit e hav e not bee n determine d unde rGLPs
.

Gar yHohemstein , Sponso rRepresentative Date % 

# M (

Jaisimh a Kesari , P.E. , DEE , Stud yDirecto rJ i J Date

Pag e 3 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



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

t 1 6 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate rSample s Collecte d a s Par

t o fth e Avenu e AInvestigatio n Are a i n Decatur , A L i n Januar y2011
. 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 findings were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector
.
Inspectio n Date s 3/18/1 1 Phas e

Dat a an d Interi m Repor

t Dat e Reporte d t o Testin g Facilit y Managemen t 3/29/1 1 Stud yDirecto r 3/29/1 1 

# ^-^-( f QA U Representative

Pag e 4 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



### TABL E O F CONTENT S GL P Complianc e statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e ofContent s 5 List ofTable s 6 1 Stud yInformatio n 7 2 Summar

y8 3 Introductio n 8 4 Test & Contro l Substance s 9 5 Reference Substance s 9 6 Test Syste m 1 7 Metho d Summar

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

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

yan d Discussio n 1 8

Pag e 5 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

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

### LIS TO F TABLE S Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Results (Avenu e AInvestigation , Ja n 2011 ) 8 Tabl e 2
. Sampl e Descriptio n Ke yCod e 1 1 Tabl e 3
. Instmmen t Parameter s 1 2 Tabl e 4
. Liqui d Chromatograph yCondition s 1 2 Tables
. Mass Transition s 1 3 Tabl e 6
. Limi t ofQuantitatio n (LOQ ) 1 4 Tabl e 7
. Laborator

yContro l Spik

e Recover

y1 6 Tabl e 8
. Analytica l Uncertaint y1 8 Tabl e 9
. DA L G WSS2 2 27011 1 1 9 Tabl e 10
. DA L G WSS2 4 27011 1 1 9 Tabl e 11
. DA L G W2 1 O R 28011 1 2 0 Tabl e 12
. Tri p Blan k

2 0 Tabl e 13
. Rinseat e Blan k 2 1

Pag e 6 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



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

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari(gwestonsolutions.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@mmm.com) : phon e (65 1 )-733-986 0 Susa n Wolf , 3 M Analys t Chelsi e Grochow ; Analys t Jo n Steege ; Analys t Kevi n Eich ; Analys t Stud yDate s StudyInitiation : Marc h 8,201 0 Interi m Repor

t 1 6 Experimenta l Termination : Marc h 11 , 201 1 Interi m Repor

t Completion : Dat e 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 referenc e substanc e an d analytica l referenc e standar d retai n sample s are archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 7 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s ofPFBS , PFHS , an d PFO S I n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

2 Summar y Th e 3 M Environmenta l Laboratoryreceive d wate rsample s collecte d a s par t o f th e Avenu e A Investigatio n are a i n Decatur , A L fro m thre e samplin g locations
. Atota l o f twenty-on e sampl e bottle s wer e receive d a t th e 3 M Environmenta l Laboratoryfo rperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e wate r sample s fro m eac h samplin g location , a s wel l a s thre e field matri xspik e (FMS ) sample s fo reac h location
. Sample s als o include d on e tri p blan k containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d on e equipmen t rinseate. Th e equipmen t rinseate blan k di d no t hav e FM S sample s prepare d fo rdeterminatio n o fPFBS , PFHS , an d PFO S recovery . Th e samples , tri p blank s an d equipmen t rinseate blan k wer e receive d fro m Westo n personne l o n February1,2011
. Al l wate rsample s fo rthi s projec t wer e logge d unde rGLP10-01-01-16
. Al l o f th e sample s wer e prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l LaboratoryMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP-10-01-02-16
. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s ar e summarize d i n Tabl e 1
. Th e equipmen t rinseate an d tri p blan k wer e belo wth e lowe rlimi t o fquantitatio n (LLOQ ) collecte d wit h th e wate rsample s fo rGLP10-01-02-16 , indicatin g adequat e contro l o f sampl e contaminatio n durin g shippin g an d sampl e collections
. Th e PFB S concentratio n result s range d fro m 3.3 9 ng/m L t o 43. 2 ng/mL
. Th e PFH S concentratio n range d fro m 1.84 ng/m L t o 30 9 ng/mL
. Th e PFO S concentratio n result s range d fro m 8.6 2 ng/m L t o 53 9 ng/mL
. Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Result s (Avenu e AInvestigation , Ja n 2011)
.
Samplin g Locatio n DA L G WSS2 2 27011 1 DA L G WSS2 4 27011 1 DALGW210R28011 1 Tri p Blan k

(Milli-Q TM Water ) Equipmen t rinseat e blan k PFB S Avg
. Cone
. (ng/mL ) ±RP D 3.3 9 ±5.3 % 19. 2 ±3.1 % 43. 2 ±2.8 % <0.025 0 <0.025 0 PFH S

Avg
. Cone
. (ng/mL ) ±RP D 1.8 4 ±6.5 % 14 3 ±2.8 % 30 9 ±1.9 % <0.025 0 <0.025 0 PFO S

Avg
. Cone
. (ng/mL ) ±RP D 8.6 2 ±1.2 % 50 0 ±5.8 % '^ ' 53 9 ±6.3 % '^ ' <0.030 0 <0.030 0 Th e analytica l method uncertaintie s associate d wit h th e reported result s ar e a s follows : PFB S ±20% , PFH S ±22% , an d PFOS ± 33%
. (1 ) Samplin g locatio n di d no t hav e a n appropriate FM S spik e leve l fo rPFOS t o accuratel yassess analyte recovery . (2 ) Sampl e fiel d matrixspik e recover ydi d no t mee t acceptanc

e criteri a of 10

0 ±30 % wit h a recover

yof68.1%
. Th e FM S recover yi s withi n th e analytica l method uncertainty
. 3 Introductio n Thi s analytica l stud ywa s conducte d a s part 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 objectiv e o f th e overal l progra m i s t o gai n informatio n regardin g concentration s o f perfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediment s tha t ar e associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s

Pag e 8 of 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

conducte d t o analyz e groun d wate rsample s collecte d as par t ofth e Avenu e AInvestigatio n i n Decatur , A L fo rPFBS , PFHS , an d PFOS , i n a n effor t t o characteriz e on-sit e groundwate rconditions
. Th e 3 M Environmenta l Laborator yprepare d sampl e container s (25 0 m L high-densit

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

ycontaine rwa s marke d wit h a "fil l t o here " lin e t o produce a final sampl e volum e of20 0 mL
. Container s designate d fo rfield matri xsample s were fortifie d wit h a n appropriat e matri xspik

e solutio n containin g PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o bein g sen t t o th e field fo rsampl e collection
. Se e sectio n 8. 8 o fth e repor t fo rfield matri xspik

e levels
. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detemninatio n o fPerfluorinate d Compound s I n Wate rb yHig h Peri'ormance 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 , tri p blank , an d groundwater-equipmen t rinseate sample
. Table s 9-1 3 summariz e th e individua l sampl e results an d th e associate d FM S recoveries
. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewhere i n thi s repor t 

### 4 - Tes t & Contro l Substance s r'
. .'.: ' = There wa s not a tes t substance o rcontro l substance s i n th e classi csens e o fa GL P study
. Thi s stud y wa s purel yanalytica l i n nature
. 

### [5 Referenc e Substances , ' ^

Referenc e Substanc e Chemica l Nam e Chemica l Fomiul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lot Numbe r TC R Numbe r Physica l Descriptio n Purit y PFB S (predominantl ylinear ) 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 96.7 % PFH S (linear ) Perfluorohexan e sulfonat e CeF-isSOa Sodiu m Sal t Wellingto n 3/25/1 8 Froze n LPFHxSAMOS TCR08-001 8 Crystallin e 98 %

Pag e 9 of 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Chemica l Nam e Chemica l Formul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lot Numbe r TC R Numbe r Physica l Descriptio n Purit y PFOS (linear ) Perfluorooctan e sulfonat e CflFiySO s 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

Perfluorooctan e sulfonat e CsFiySO s Potassiu m Sal t CA S #2795-39- 3 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 Whit e Powde r 86.4 % Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Source Expirat'o n Dat e Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "C,-PFO S Perfluorooctan e sulfonat e CsFi ySO 3 Sodiu m Sal t Wellingto n 9/28/1 3 Froze n 09231 0 TCR10-004 8 Liqui d 98 %

Pag e 1 0 of6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

6 Tes t Syste m Th e test syste m fo rthi s stud yar e surface wate ran d groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L byWesto n Solutions , Inc
. personnel
. Sample s fo rthi s stud yar e "rea l worid " samples , not dose d wit h a specifi clot o ftes t substance
. Tabl e 2
. Sampl e Descriptio n Ke yCode
. Strin g Numbe r Exampl e 1 2 3 4 5 Strin g Descripto r Exampl e DA L SWSS2 4 027011 1 Sampl e Locatio n Sampl e Typ e Locatio n I D Samplin g Dat e Sampl e Typ e DAL=Decatur , Alabam a GW=Gmun(lwate r Example : SS2 4 270111-Januar y27,201 1 0=primarysampl e DB=duplicat e sampl e L S = lo wspik e IVI S = mi d spik e H S = hig h spik e R B = Rinseat e Blan k 

### 7 Metho d Summar y 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Determinatio n o fPerfluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s were retume d t o th e laborator ya t ambien t condition s o n Februar y1 , 2011
. Sample s were store d refrigerate d a t th e laborator

yafte rreceipt
. Th e laborator y prepare d Tri p Blan k

an d Tri p Blan k

fleld matri xspike s were receive d wit h th e sampl e collectio n bottles
. 

### 7. 3 Sampl e Preparatio n Al l groundwate rsample s were initial l prepare d b ydilutin g Im L sampl e wit h 9 mLs o fMilli- Q wate r (dilutio n 1:10)
. Samplin g location s DA L GWSS2 4 an d DA L GW210 R require d furthe rdilutio n fo rPFO S an d were prepare d b

ydilutin g 0. 1 m L o fsampl e wit h 9. 9 mL s ofMill i Q wate r(dilutio n 1:100)
. Tri p Blan k

an d Rinseat e Samples : 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 ranalysis
. Samplin g locatio n DA L G WSS2 2 wa s analyze d fo rPFO S b yremovin g a measure d volum e ofsample , addin g interna l standard , an d placin g a n aliquot ofth e preapre d sampl e into a n autovia l fo ranalysis
.

Pag e 1 1 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



### 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h perfomnanc

e liqui d chromatography

/ tande m mass spectrometr y(HPLC/MS/MS)
. Detaile d instrumen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmass transition s analyze d ar e describe d i n th e ra

wdat a har

d copie s place d i n th e final data packet , an d are briefl ydescribe d below
. Tabl e 3
. Instrumen t Parameters
. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat 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 Polarit y Softwar e ETS Ginge r ETS-8-044. 0 2/11/11,2/28/1 1 Agilen t 1100 Pris m R P (2. 1 m m X 5 0 mm) , 5 n Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n

2or10n L Applie d Biosystem s AP I 500 0 Turb o Spra

y Turb o Io n electrod e Negative Analyst 1.4. 2 ETS Buste r ETS-8-044. 0 3/10/1 1 Agilen t 1100 Betasi l CI S (2. 1 m m X 100 mm) , 5 n Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n

5|i L Applie d Biosystem s AP I 400 0 Turb o Spra

y Turb o io n electrod e Negative Analyst 1.4. 2 Tabl e 4
. Liqui d Chromatograph yConditions
. ste p Numbe r Tota l Tim e

(min ) Flo wRat e

(fiUmin ) Percen t A

( 2 m M ammoniu m acetate ) Percen t B (Methanol } ETS-8-044. 0 Analysi s (ETS Ginger ) 0 1 2 3 4 5 0

2. 0 11. 0 14. 0 14. 5 17. 0 30 0

30 0 30 0 30 0 30 0 30 0 ETS-8-044. 0 Ana h 0 1 2 3 4 5 0

2. 0 11. 0 13. 5 14. 0 17. 0 30 0

30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 /si s (ETS Buster

) 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0

Pag e 1 2 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 5
. IVIas

s Transitions
. Analyt e PFB S PFH S PFO S Mas s Transitio n Q1/Q 3 299/8 0 299/9 9 399/8 0 399/9 9 499/8 0 499/9 9 499/13 0 Referenc e Materia l

Structur e Linea r Linea r Unea r Intema l Standar d N A N A t"CJPFOS" > Mas s Transitio n Q1/Q 3 N A N A 507/8 0 Dwel l tim e wa s 5 0 mse cfo reac h transition
. Th e individua l transition s wer e summe d t o produce a "tota l io n chromatogram " (TIC) , whic h was use d fo rquantitation
. N A= No t Applicable ; interna l standar d no t use d fo rquantitation
. (1 ) PFO S intema l standar d onl yuse d fo r3/10/1 1 analysis
. 8 Analytica l Result s 8. 1 Calibratio n 2/11/1 1 an d 2/28/1 1 Analysis : Sample s were analyze d against a n externa l standar d calibratio n curve . Calibratio n standard s were prepare d b yspikin g know n amounts ofth e stoc k solutio n containin g th e targe t analyte s into prepare d i n Mill i Q wate ro rSyntheti cGroundwater
. Atota l o fsixtee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) were analyzed
. Lo wcurve points were disable d as neede d t o meet calibratio n acceptance criteria
. Aquadratic , 1/ xweighted , calibratio n curve ofth e pea k

are a counts wa s use d t o fit th e data fo reac h analyte
. Th e dat a were no t force d throug h zero durin g th e fitting process . Calculatin g th e standar d concentration s usin g th e pea k are a confinne d accurac yofeac h curve point
. Eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac yrequirements o f100±25 % (100±30 % fo rth e lowest curve point ) an d a correlatio n coefficien t (r) greate rtha n 0.995 , were me t fo rPFBS , PFHS , an d PFOS
. 3/10/1 1 Analysis : Samplin g locatio n DA L G WSS2 2 wa s analyze d against a stabl e isotop e intema l standar d calibratio n curve fo rPFOS
. 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 int o a laboratory-prepare d syntheti cgroundwate r containin g calciu m an d magnesium
. Aseparat e intema l standar d spikin g solutio n wa s prepare d an d a n aliquot wa s adde d a

t th e sam e leve l t o al l calibratio n standard s an d laborator ycontro l sample s a

t a nomina l concentratio n o f1 ng/mL
. Acalibratio n curve rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) wa s analyzed
. Lo wcurve points were disable d fo rPFO S t o meet metho d accurac yo r metho d blan k

criteria
. Th e dat a were no t force d throug h zer

o durin g th e fitting process . Calculatin g th e standar d concentration s usin g th e pea k are a ratio s an d th e resultan t calibratio n curve confinne d accurac yofeac h curve point
. Eac h curve poin t wa s quantitate d usin g th e overal l calibratio n curve an d reviewe d fo raccuracy . Metho d calibratio n accurac yrequirements of100±25 % (100±30 % fo rth e lowes t curve point) an d a correlatio n coeflicien t (r ) greate rtha n 0.995 , were met fo rPFOS
. 

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

d wa s analyze d fou rtime s a t th e beginnin g ofth e analytica l sequence t o demonstrat e overal l syste m suitability
. Th e acceptance criteri a 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 o fles s tha n o requa l t o 2 % RS D was met fo rPFBS , PFHS , an d PFOS
.

Pag e 1 3 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

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

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

yrequirements an d fo rwhic h th e are a counts ar e a t least twic e thos e o fth e appropriat e blanks
. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 6
. Tabl e 6
. Limi t o fQuantitatio n (LOQ)
. Analysi s Dat e 2/11/1 1 2/28/1 1 3/10/1 1 Dilutiort 1 1 0 100 1 PFB S

LOQ , ng/m L 0.025 0 0.25 0 NA NA PFH S

LOQ , ng/m L 0.025 0 0.25 0 NA NA PFO S

LOQ , ng/m L 0.030 0 0.30 0 2.5 0 0.25 0 N A= No t Applicabl e 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen 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 Blank s Thre e type s ofblank

s were prepare d an d analyze d wit h th e samples : procedura l blanks , field/trip blank , an d equipmen t blank
. Procedura l blan k results were reviewe d an d use d t o evaluat e metho d performance an d t o determin e th e LOQ fo reac h analyte
. 8. 6 La b Contro l Spike s (LCSs ) 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 o fth e analyt e into 1 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 ras th e samples
. Th e metho d acceptance criteri a state s that th e averag e ofLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D ^20%
. 2/11/1 1 Analysis : Thre e spike level s were prepare d an d me t metho d acceptance criteri a fo rPFBS , PFHS , an d PFO S (linear)
. 2/28/1 1 Analysis : Thre e spike level s were prepare d an d met metho d acceptance criteri a fo rPFO S (linear)
. 3/10/1 1 Analysis : Two spike level s were prepare d an d met metho d acceptance criteri a fo rPFO S (linear)
. As th e reference material s use d fo rquantitatio n ofPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s are comprise d ofbot h linea ran d branche d isomers , additiona l LC S sample s of PFO S (linea ran d branched ) were prepare d t o evaluat e th e potentia l fo ranalytica l bias
. 2/11/1 1 Analysis : Thre e spike level s LC S (linea r+ branched ) were prepared
. Th e lo wan d mi d set of LC S met metho d acceptance criteria , whil e th e hig h set ofLC S di d not meet metho d acceptance criteri a wit h a n averag e recover

yo f133%
. 2/28/1 1 Analysis : Thre e spike level s LC S (linea r+ branched ) were prepared
. Th e lo wan d mi d set of LC S (linea r+ branched ) met metho d acceptance criteria , whil e th e hig h set o fLC S di d no t meet metho d acceptance criteri a wit h a n averag e recover yof125%
.
Pag e 1 4 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

3/10/1 1 Analysis : Tw o spike level s LC S (linea r+ branched ) were prepare d an d met metho d acceptance criteri a fo rPFOS
. Th e averag e recover

yofth e hig h set o flinea ran d branche d LC S a t 125 % an d 133 % suggests a sligh t bia s whe n quantitatin g branche d isomer s ofPFO S against a calibratio n curve oflinea rPFOS
. Therefore , th e metho d uncertaint yfo rthi s stud yhas bee n set of±33%
. Ametho d deviatio n i s include d wit h th e ra

wdata
. Th e followin g calculation s were use d t o generat e data i n Tabl e 7 fo rlaborator ycontro l spikes
.

, o o D
. n Calculate d Concentratio n .,... , LC S Percen t Recover

y= 100 % Spike Concentratio n LCS % RS D = standar d deviatio n LC S replicate s ,^^^,^ ^ averag e LC S recover

y

Pag e 1 5 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 7
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Analyze d 2/11/1 1
La b I D LCS-110210- 1 LCS-110210- 2 LCS-110210- 3 Averag e ±%RS D LCS-110210- 4 LCS-110210- 5 LCS-110210- 6 Averag e ±%RS D LCS-110210- 7 LCS-110210- 8 LCS-110210- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0.56 3 0.54 2 0.58 1 '/oRecover y

11 3 10 9 11 7 113 % ±3.5 % 4.9 8 4.9 8 4.9 8 5.3 7

5.5 2 5.5 8 10 8

11 1 11 2 110 % ±1.9 % 29. 9 29. 9 29. 9 29. 8

31. 1 32. 0 99. 5

10 4 10 7 104 % ±3.6 % PFH S Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0.60 3 0.59 4 0.59 9 VoRecover y

12 1 11 9 120 120 % ±0.83 % 4.9 8 4.9 8 4.9 8 5.6 1

5.3 6 5.9 6 11 3

10 8 120 114 % ±5.3 % 29. 9 29. 9 29. 9 30. 7

30. 8 32. 7 10 3

10 3 10 9 105 % ±3.3 %
ETS-8-044. 0 Analyze d 2/11/1 1
La b I D LCS-110210- 1 LCS-110210- 2 LCS-110210- 3 Averag e ±%RS D LCS-110210- 4 LCS-110210- 5 LCS-110210- 6 Averag e ±%RS D LCS-110210- 7 LCS-110210- 8 LCS-110210- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0.65 0 0.58 7 0.54 0 VoRecover y

13 0 11 8 10 8 119 % ±9.3 % 4.9 8 4.9 8 4.9 8 5.4 3

4.9 3 5.8 6 10 9

99. 1 11 8 109 % ±8.7 % 29. 9 29. 9 29. 9 30. 8

30. 7 32. 4 10 3

10 3 10 8 105 % ±2.8 % La b I D LCS-110210-1 0 LCS-110210-1 1 LCS-110210-1 2 Averag e ±%RS D LCS-110210-1 3 LCS-110210-1 4 LCS-110210-1 5 Averag e ±%RS D LCS-110210-1 6 LCS-110210-1 7 LCS-110210-1 8 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 0.50 2 0.50 2 0.50 2 Calculate d

Concentratio n (ng/mL ) 0.53 9 0.58 5 0.54 1 VoRecover y

10 7 11 7 10 8 111 % ±5.0 % 5.0 4 5.0 4 5.0 4 6.1 5

5.3 8 5.4 4 12 2

10 7 10 8 112 % ±7.5 % 30. 2 30. 2 30. 2 40. 7

40. 4 39. 6 13 5

134 13 1 133 % ±1.6%'^ ' (1 ) Tti e averag e recover ydi d not mee t metho d acceptance criteri a o f100 % ±20%
.

Pag e 1 6 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 ^alyze d 2/28/1 1
La b I D LCS-110228- 1 LCS-110228- 2 LCS-110228- 3 Averag e ±%RS D LCS-110228- 4 LCS-110228- 5 LCS-110228- 6 Averag e ±%RS D LCS-110228- 7 LCS-110228- 8 LCS-110228- 9 Averag e ±%RS D Spike d

Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 PFO S (linear )

Calculate d Concentratio n (ng/mL ) 0.48 3 0.48 7 0.42 7 VoRecover y

97. 0 97. 7 85. 6 93.4 % ±7.3 % 4.9 8 4.9 8 4.9 8 5.2 7

5.1 7 5.3 4 10 6

10 4 10 7 106 % ±1.4 % 29. 9 29. 9 29. 9 31. 3

31. 7 31. 9 10 5

10 6 10 7 106 % ±0.94 % La b I D LCS-110228-1 0 LCS-110228-1 1 LCS-110228-1 2 Averag e ±%RS D LCS-110228-1 3 LCS-110228-1 4 LCS-110228-1 5 Averag e ±%RS D LCS-110228-1 6 LCS-110228-1 7 LCS-110228-1 8 Averag e ±%RS D PFO S (linea r+ branciied ) Spike d Concentratio n (ng/mL ) 0.50 2 0.50 2 0.50 2 Calculate d

Concentratio n (ng/mL ) 0.46 7 0.47 5 0.49 3 VoRecover y

93. 1 94. 6 98. 2 95.3 % ±2.8 % 5.0 4 5.0 4 5.0 4 4.8 8

5.1 0 4.7 2 96. 7

10 1 93. 6 97.1 % ±3.8 % 30. 2 30. 2 30. 2 40. 4

36. 1 36. 8 13 4

11 9 12 2 125 % ±6.3%'' ' ETS-8-044. 0 Analyze d 3/10/1 1
La b I D LCS-110307- 4 LCS-110307- 5 LCS-110307- 6 Averag e ±%RS D LCS-110307- 7 LCS-110307- 8 LCS-110307- 9 Averag e ±%RS D Spike d

Concentratio n (ng/mL ) 1.9 9 1.9 9 1.9 9 PFO S (linear )

Calculate d Concentratio n (ng/mL ) 2.2 2 2.0 5 2.2 6 VoRecover y

11 1 10 3 11 4 109 % ±5.2 % 9.9 4 9.9 4 9.9 4 11. 1

10. 7 10. 2 11 2

10 7 10 3 107 % ±4.2 % La b I D LCS-110307-1 3 LCS-110307-1 4 LCS-110307-1 5 Averag e ±%RS D LCS-110307-1 6 LCS-110307-1 7 LCS-110307-1 8 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 2.0 1 2.0 1 2.0 1 Calculate d

Concentratio n (ng/mL ) 2.2 4 2.2 3 2.4 0 VoRecover y

11 1 11 1 12 0 114 % ±4.6 % 10. 0 10. 0 10. 0 11. 2

11. 6 11. 0 11 2

11 6 11 0 113 % ±2.7 % (1 ) Th e averag e recover ydi d no t meet mettio d acceptance criteri a of100 % ±20%
. 8. 7 Analytica l IVIetho 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 mos t recen t fifty Q C samples
. Th e expande d uncertaint yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto r o f2 , whic h con-espond s t o a confidence leve l of95%
. Th e metho d uncertaint yfo rPFO S b

yETS-12 - 012- 2 wa s foun d t o b e ±17% , however , since th e hig h set o flinea ran d branche d LC S had a n averag e recover yo f133% , th e analytica l uncertaint yassigne d t o thi s stud ywil l b e ±33%
. Th e metho d uncertaint yvalue s are liste d i n Tabl e 8
.

Pag e 1 7 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 8
. Analytica l Uncertainty
. Analyt e PFB S PFH S PFO S Standar d Deviatio n

10. 1 11. 0 NA'^ ' Metho d

Uncertaint y ±20 % ±22 % ±33 % (1 ) Se e sectio n 8. 6 fo ra discussio n regardin g th e metho d uncertaint yfo rPFOS
. 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 xspik e recoverie s withi n metho d acceptanc e 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 ofth e analyte s o finterest
. Fiel d matri xspik e concentration s must b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e 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 xspik

e was 1. 0 ng/mL , th e mi d field matri xspik e was 1 0 ng/mL , an d th e hig h field mari xspik e wa s 100 ng/m L fo ral l samplin g locations
. ^ , ,_ „ (SampleConcentrationof FMS-Averag e Concentration: FieldSampl e & FieldSampl

e Dup. ) .„,„„„ , FMS Recover

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

### \9 ' Dat a Summar

yan d Discussio n •:-./,• ] Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blan k an d rinseate blank
. Results an d averag e value s ar e rounde d t o thre e significan t figures accordin g t o EP Aroundin g njles
. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspik

e recoverie s meetin g th e metho d acceptance criteri a o f±30% , demonstrat e that th e method(s ) were appropriat e fo rth e give n matri xan d thei rrespective quantitative range s DA L G W2 1 O

R 280111 ; Th e recover

yofth e H S sample , th e onl yappropriat e FM S concentratio n leve l fo rPFOS , wa s 68.1%
. Th e recover ywa s withi n th e metho d uncertaint yfo rPFOS
. DA L G WSS2 4 27011 1 ; Th e H S at 97. 8 ng/m L wa s no t sufficien t t o accuratel yasses s recover yfo r PFOS
.

Pag e 1 8 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tables
. DA L GWSS2 2 27011 1

3 M LIM S I D GL P 10-01-02-16-00 6 GLP10-01-02-16-00 7 GL P 10-01-02-16-00 8 GLP10-01-02-16-00 9 GLP10-01-02-16-01 0 Descriptio n DA L GWSS2 2 0 27011 1 DALGWSS22DB27011 1 DALGWSS22LS27011 1 DALGWSS22IVIS27011 1 DALGWSS22HS27011 1 Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 3.3 0 3.4 8 4.4 5 12. 8 99. 5 VoRecover y

N A N A 106 94. 1 98. 9 3.3 9 ng/m L ±5.3 % PFH S Concentratio n (ng/mL ) 1.7 8 1.9 0 3.1 3 12. 0 104 VoRecover y

NA N A 12 9 102 10 6 1.8 4 ng/m L ±6.5 % PFO S Concentratio n (ng/mL ) 8.5 7 8.6 7 NA<^ ' 16. 5 NA'^ ' %Recover y

N A N A NA'^ > 78. 8 NA'^ > 8.6 2 ng/m L ±1.2 % NA= No t Applicatji e NO = No t Calculated ; Endogenou s concentratio n greate rtha n 2xspik e level
. PFB S an d PFH S were analyze d b yexterna l standar

d calibratio n o n 2/11/11
. PFO S wa s analyze d b yintema l standar

d calibratio n o n 3/10/11
. (1 ) Th e sampl e wa s no

t analyzed
. Tabl e 10
. DALGWSS2 4 27011 1

3MLIIVISI D GLP10-01-02-16-01 2 GLP10-01-02-16-01 3 GLP10-01-02-16-01 4 GLP10-01-02-16-01 5 GLP10-01-02-16-01 6

Averag e Conce r Descriptio n

DA L GWSS2 4 0 27011 1 DALGWSS24DB27011 1 DALGWSS24LS27011 1 DALGWSS24MS27011 1 DALGWSS24HS27011 1 rtration (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 18. 9 19. 5 20. 0 28. 6 11 6 %Recover y

N A N A N C 94. 0 99. 6 19. 2 ng/m L ±3.1 % PFH S Concentratio n (ng/mL ) 14 1 145 14 6 15 4 23 4 VoRecover y

N A N A N C N C 94. 7 14 3 ng/m L ±2.8 % PFO S Concentratio n (ng/mL ) 51 4 48 5 NA<^ > NA<^ ' 54 8 VoRecover y

N A N A NA<^ ' NA<^ ' N C 50 0 ng/m L ±5.8%' ^ NA = No t Applicabl e N C = No t Calculated ; Endogenou s concentratio n greate rtha n 2xspik e level
. PFB S an d PFH S wer

e analyze d 2/11/11
. PFO S wa s analyze d 2/28/11
. (1 ) Th e sampl e was no

t analyzed
. (2 ) Samplin g locatio n di d no t hav e a n appropriate fiel d matri xspike leve l fo rPFOS
.

Pag e 1 9 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 11
. DA L G W2 1 O R 28011 1

3 M LIM S I D GLP10-01-02-16-01 7 GLP10-01-02-16-01 8 GLP10-01-02-16-01 9 GLP10-01-02-16-02 0 GLP10-01-02-16-02 1

Averag e Conce r Descriptio n

DA L GW210 R 0 28011 1 DA L GW210RD B 28011 1 DA L GW210RL S 28011 1 DA L GW210 R M S 28011 1 DA L GW210RH S 28011 1 rtration (ng/mL ) ±VoRP D PFB S Concerrtratio n (ng/mL ) 43. 8 42. 6 52. 5 13 6 94 7 VoRecover

y N A N A N C 95. 5 90. 4 43. 2 ng/m L ±2.8 % PFH S Concentratio n (ng/mL ) 31 2 30 6 32 4 40 2 128 0 VoRecover

y N A N A N C N C 97. 1 30 9 ng/m L ±1.9 % PFO S Concerrtratio n (ng/mL ) 55 6 52 2 NA'^ ' NA'^ > 122 0 VoRecover

y N A N A NA'^ > NA'^ > 68. 1 <^ ' 53 9 ng/m L ±6.3 % NA = Not Applicabl e N C = No t Calculated ; Endogenou s concentratio n greate rtha n 2xspik e level
. PFB S an d PFH S were analyze d 2/11/11
. PFO S was analyze d 2/28/11
. (1 ) Th e sampl e wa s no

t analyzed
. (2 ) Fiel d matrixspike di d no t mee t metho d acceptanc

e criteri a of100 % ±30%
. Tabl e 12
. Tri p Blan k

3 M LIM S I D GLP10-01-02-16-00 1 GLP10-01-02-16-00 2 GLP10-01-02-16-00 3 GLP10-01-02-16-00 4 GLP10-01-02-16-00 5 Descriptio n DAL GWTRI P 0 27011 1 DA L GWTRI P L

S 27011 1 DAL GWTRI P M S 27011 1 DAL GWTRI P M H 27011 1 DAL G WTRI P H S 27011 1 PFB S Concentratio n (ng/mL ) <0.025 0 1.0 4 9.8 8 10 1 98 2 VoRecover

y N A 104 98. 8 10 4 98. 2 PFH S

Concentratio n (ng/mL ) <0.025 0 1.1 8 10. 3 10 8 104 0 %Recover

y NA 11 8 10 3 11 2 104 PFO S

Concentratio n (ng/mL ) <0.030 0 1.03 9.3 7 92. 8 95 0 VoRecover

y N A 10 3 93. 7 94. 9 95. 0 NA= No t Applicabl e

Pag e 2 0 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Tabl e 13
. Rinseat e Blan k

3 M LIM S I D GLP10-01-02-16-01 1 Descriptio n DALGWSS24RB27011 1 PFB S Concentratio n (ng/mL ) <0.025 0 VoRecover y NA PFH S

Concerrtratio n (ng/mL ) <0.025 0 VoRecover y N A PFO S

Concentratio n (ng/mL ) <0.030 0 VoRecover y NA NA= No t /Applicabl e

Pag e 2 1 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



### 10
. Cohclusipn. ' ;' ; . -^ y''•- ' •• ' ^"^^y'; : ty'J ; (Vf:'''' : Laborator ycontro l spike s an d field matri xspike s were use d t o detennin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS
. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein
.



### ' ItjDatwSampimRetention^, , - ^T^:f:i~'e-:'"^-' ' ^'^'j-.-'-* * • -* - -; ' Al l remainin g sample s an d associate d projec t data (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures
.

Attachmen t A : Protoco l Amendmen t 1 6 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d Attachmen t D : Metho d Deviatio n

Pag e 2 2 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1



### ,1 3 Signature s 

# 'Z^) i Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date 

# P

# /f/^ / :k}7 ( Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yDepartmen t Manage rDate



## U
Gar yHohenstein , Sponso rRepresentative 

# Oi^i^'i
. Date



# m Jaisimh a Kesari , Stud yDirecto r Date

Pag e 2 3 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1


### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 2 4 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 6



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

Decatu rPhas e 3 Site-Relate d Monitorin g Progra m
PROTOCO L AMENDMEN TNO
. 1 6

Amendmen t Date : Januar y25 , 201 1 Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

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

GLP10-01-0 2
Samplin g Even t Avenu e AInvestigatio n - Groundwate rSamplin g



# Exact Cop yo fOrigina l initia l Dat e t Pag e 1 o f6 Pag e 2 5 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 6 

### 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
.

AMEN D T

O READ : N o change s t o th e wordin g o fth e protoco l are required
. Thi s amendmen t onl yaddresse s an d document s th e additio n o fth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s fro m Decatur , AL , an d conducte d a s par t 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 o fth e wee k o fJanuar

y 24 , 2011
. Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s projec t GLP10-01-02-1 6 an d reporte d a s interi m report GLP10-01-02-06 , (reflectin g stud yGLP10-01-0 2 an d amendmen t -16)
.
Reason : Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t t o b e conducte d fo rth e 3 M Decatur , A L facility
. Th e GP O i s fou rpage s i n lengt h an d include d as attache d t o thi s amendmen t form
.

Pag e 2 o f6 Pag e 2 6 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 6 Amendmen t Approva l


### y/ / 

# iMi i fffm^^^H ' { " -^ — Gar yHohenstein , Sponso rRepresentative 

## 7 7 

# 'I L Date

fDat e ^ ^ Clesto n C
. Lange , Principa l Analytica l Investigato r 

## ;i.r.j7p ^ s>o'/ / Willia m Reagen/EH S Opn s Environmenta l La b Managemen t 

# fklMMj. : Dat e



# S L Jaisimh a Kbsar i P.E. , DEE , Stud yDirecto r Date

Pag e 3 of6 Pag e 2 7 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2

Amendmen t 1 6
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

Ja i Kesari , Westo n Solution s Charie s Young , Westo n Solution s Ti m Frinak , Westo n Solution s Date : Januar

y25 , 201 1 Subject : Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d

Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 1 6 - Additiona l Avenu e A Sampling ; Januar

y201 1 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r Projec t Schedule/Tes t Date s 3 M Sponso rRepresentativ e Gar yHotienstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul
. M N 55144-100 0 Phone:(651)737-357 0 aatiohenstein(5)mmm.co m 3IVI Environmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S Opns , Environmenta l Laboratory 260-5N-1 7 65 1 733-973 9 wkreaaen®mmnn.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 cclanae(a)mmm.co m Samplin g Coordinato r Timotti yFrina k Westo n Solution s Timothv.frlnak(5)westonsolutions.co m Ptione ; (334)-332-912 3 GLP10-01-02-1 6 Dept #530711 , Project #002267444 9 1 Samplin g sctiedule d fo rth e wee k o fJanuary24 , 201 1 Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHotienstein
.
Pag e 4 o f 6 Pag e 2 8 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 6 

### 2 Backgroun d Informatio n an d Projec t Objective{s ) Th e 3 M EH S Operation s Laborator y(3IV 1 Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m thre e samplin g location s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS)
. an d Perfluorooctanesulfonat e (PFOS ) a s part ofth e Avenu e A Investigation
. Analyse s wil l b e conducte d unde rth e GL P requirement s ofEP ATSC AGoo d Laborator y Practic e Standard s 4 0 CF R 792. Groundwate rsample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k o f Januar y24 , 2011
. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFBS , PFHS , an d PFO S are o fa know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10 - 01-02-16 , 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

ofJanuar y 24,2011
. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo ramva l o n Friday , Januar y21 , 2010
. Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection
. Marti n Smit h \

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

### 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 ofthre e samplin g location s have bee n specified
. Samplin g locatio n description s were not availabl e a t th e tim e ofsampl e bottl e preparation
. Fo reac h samplin g location , a tota l offiv e sampl e bottle s wil l b e collecte d (sample , sampl e duplicate , low-leve l fiel d matri xspike , mid-leve l fiel d matri xspike , an d high-leve l fiel d matri x spike)
. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL
. On e se t o ftri p blank s consistin g o

f reagent-grad e water , a low-leve l tri p blan k spike , mid-leve l fiel d spike , mid-hig h leve l fiel d spike , an d a high-leve l tri p blan k spik e wil l b e prepare d at th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles
. On e additiona l bottl e wil l b e prepare d t o be use d fo rth e preparatio n o fth e equipmen t rinseate blank
. Atota l oftwenty-on e sampl e bottle s wil l b e prepared
. 5 Tes t Method s Sample s wil l b e prepare d an d analyze d byLC/MS/M S followin g ETS-8-044. 0 "Determinatio n ofPerfluorinate d Compound s I n Wate rbyHig h Perfomnanc e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Th e dat a qualityobjective s fo rthes e studie s ar e quantitative results fo rth e targe t analyte s wit h a n analytica l accurac

yo f100+30%
. Fiel d matri xspike s no t yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n th e repor

t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly
. Alternately , sample s ma

yb e analyze d b

yETS 8-154. 3 "Detemninatio n ofPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
.

Pag e 5 of6 Pag e 2 9 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Analytica l Protocol : GLP10-01-0 2 Amendmen t 1 6 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e results fo rth e sample , sampl e duplicate , an d th e thre e fiel d matri xspikes
. Tri p blan k an d tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an y equipment/rinseat e blank s prepare d i n th e field
. Laborator ycontro l spike s ofreagen t wate rprepare d a t th e time o fsampl e extractio n wil l als o b e reporte d an d use d t o evaluat e 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 detemnin e th e method detectio n limit
. Fo rthos e samplin g location s wher e th e fiel d matri xspik

e leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspik

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

Pag e 6 of6 Pag e 3 0 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1


### ATTACHMEN TB : SAMPL E CHROMATOGRAM S AN D CALIBRATIO N CURV E

Pag e 3 1 of 6 1** • Ginge r

AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSamp)<^uit s Name : Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 gll0211a.rd b g1102 1 la.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -8.76e+00 3 x'^ 2 + 1.24e+00 6 x+ 4.17e+00 3 ( r= 0.9995 ) 4.2e 7 4.1e 7 4.0e 7 3.9e 7 3.8e 7 3.7e 7 3.6e 7 3.5e 7 3.4e 7 3.3e 7 3.2e 7 3.1e 7 3.0e 7 2.9e7 - 2.8e7 - 2.7e7 - 2.6e7 - 2.5e 7 2.4e 7 2.3e 7 2.2e7 - 2.1e7 - 2.0e 7 1.9e 7 1.8e7 - 1.7e7 - 1.6e7 - 1.5e7 - 1.4e7 - 1.3e 7 1.2e7- | 1.1e 7 1.0e7 H 9.0e 6 S.OeS 7.0e 6 6.0e 6 5.0e6 - / 4.0e 6 3.0e 6 2.0e 6 I.Oe S 0. 0 -1.0e 6 /

/

1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 3 2 Concentration , ng/m L 3 4 3 6 3 8 4 0 Pag e 4 2 4 4 4 6 4 8 5 0 :^?nffi 1 Printin g Time : 10:21:1 3 A M Printin g Date : Thursday , Marc h17 , 201 1 Pag e 1 o f 1Ginge r

AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSamp*^uit s Name : gii02iia.rd b Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 g1102 1 la.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -3.35e+00 3 x'^ 2 + 6.88e+00 5 x+ 3.41e+00 3 ( r= 0.9997 )
2.7e7 - 2.6e7 - 2.5e7 - 2.4e7 - 2.3e7 - 2.2e7 - 2.1e7 - 2.0e7 - 1.9e7 - 1.8e7 - 1.7e7 - 1.6e7 - 1.5e7 - 1.4e7 - 1.3e7 - 1.2e7 - 1.1e7 - 1.0e7 - 9.0e6 - 8.0e6 - 7.0e6 - e.oes 5.0e6 - 4.0e6 - 3.0e6 - 2.0e6 - 1.0e6 - 0.0 - / ' /

' / /

I ' / / '

I • I 

### / /

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### / / / /

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### /

/ / ' '

1 ' 1 / 

### / / / / / / / / • / / / / / / /

. 1 > 1 > 1 i 1 ' 1 / 

### / / / / /

' 1 • 1 • 1 ' 1 ' - / 

### / / /

1 ' I ' 1 

### /

/ /

1 1 < 1 1 1 1 1 8 1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 3 2 3 4 3 6 3 8 4 0 4 2 4 4 4 6 4 8 5 0 Concentration , ng/m L P^Q^r^r^nfR i Printin g Time : 10:20:4 0 A M Printin g Date : Thursday , Marc h 17 , 201 1 Pag e 1 o f 1Ginge r

AG0133050 9 

# I Sampl e Name : "g110211a019 " Sampl e ID : -10007'27-S ' File : 'g110211a.wif r Pea k Name : TFBS " Mass(es) : "299.0/99. 0 amu,299.0/80. 0 amu " Connmen t '1. 0 ng/m L F C st d i n Mil i Q vratei ' Annotatkin: " Sampl e Index ; I S Sampl e Type : Standar d Cancentration : 1.0 0 ng/m L Calculate dCcnc : 1.0 5 nij/rn L Acq . Date : 2/12/201 1 Acq . Time : 2:20:5 5 A M GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Result s Name : gll0211a.rd b

R T Window : 30. 0 s i Expecte dRT : 10- 6 m : Vs ^ Relativ e RT : N o Int . Type : Hanua l Kenentio nTime : 10. 6 m : Ares : 73352 1 cioun l Height : 165000 . ^-ps 1.6e5 1.6e5 ' 1.S«5 1.5« 5 1.4e5
- 1.4«5
- 1.3*5
- 1.3e5
- 1.2e5 ' 1.2eS l.le S l.1e 5 1.0e5 9.5e4 9.0e4 § • 6.Se4
- I e.0e 4 7.5e4 7.0* 4 6.5e4 6.0e4 5.5e4 5.0e4 4.5e4 4.0e 4 3.5e4 3.0e4 2.5e4
- 2.0e4

1 0 n1 2 1 3 1 4 1 5 1 6 Sampl e Name : "g110211aO11 * Sampl e ID : "Solven t Blank " File ; "g1102 1 la.vuif r • Pea k Name : "PFBS " Ma*«(es) : -299.Dffl9. 0 amu,299.0/80. 0 amu " Commen t •MilliQ\ftfaterTN11-00S2 " Annotation:" " Sampl e Index : 1 1 Sampl e Type :

Dat a printe d byCJ G Printin g Time : 10:16:0 1 A M Pag e 1 o f 6^ * Ginge r

AG0133050 9 

# I Sampl e Name : "g l 10211«032 - Sampl e ID : "LCS-11021[M " File : "g1102 1 la.wi T Pea k Name ; 'PFBS * Maaafes): "299.0^. 0 amu,299.0/80. 0 Amu " Commen t "5pp b LCS " Annotation : " Sampl e Index : 3 2 Sampl e Type : Q C Csncan t cation : A.9 ? ng/m L Calculate dCone ; 5,3 1 ng/m L Acq . Date : 2/12/201 1 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur
. A L - Ja n 201 1 Result s Name : gll0211a.rd b

Acq . Ti m

I Rel a 6:14:5 2 n M
! RT : N o Inc . Type : Manua l Retentio nTime : 10. 6 Area : 360386 9 c . Height : 817000 . Star t Time : 10. 5 En dTime : 11. 2 S.De S 7.8e 5 7.6e 5 7.4e 5 7.2e 5 7.0e 5 6.8e 5 6.6e5
- 6.4e 5 6.2e5
- 6.0e 5 5.8e5
- 5.6e 5 5.4e S 5.2e 5 S.Oe S 4.8a 5 4.6e S 4.4e 5 4.2e 5 4.0e 5 3.8e5
- 3.6e S 3.4e 5 3.2e 5 3.0e 5 2.6e 5 2.6e5
- 2.4e5
- 2.2e5
- Z0e5 ' 1.Se 5 1.6e5 1.4e5 1.2e5 1.0e5 B.0e 4 6.0e4 4.0e4

Tim^ , mif ) SamptoName:"g1102nfl068 " SamptelD:"GLP1(M)1-02-1B-006 " File : •g110211a.M r • Pea k Name : "PFBS " Ma««(e«) : "299.0/99. 0 amu,299.0ffi0. 0 amu " Comment " DALGWSS2 2 0 27011 1 (dil1:10) " Annotation : " Sampl e Index : 6 9 Sampl e Type : Unknow n Concentration : M/ A Calculate dCone : 3.3 0 ng/m L52* 4 Acq . Date : 2/12/201 1 Acq . Time : 5:03:1 1 P M 5^ ^ Mod i fi«d :
Base . Sub , window : p.-ak-Split . Facto r R^po^ t Largas t paa l Hin . Pea k Height : Mln . Pea k Width : Sooothin g Width : R T Window : EKparte d RT : Us e Relativ e RT : alliC'ja i 90 1,0 0 5,0e4
-

4.9e4
- 4.ee4
- 4.7e4
- 4.6e4
- 4.Se4 ' 4.4e4 ' 4.3e4 4.2e4 4.1e4 4.0e4 3.9e4 3.8e4 3.7e4 3.6e4 3.5e4 3.4e4 3.3e 4 3.2e4 3. 1 e4 3.0e 4 Z9s 4 2.8e 4 2.7e4 2.6e 4 2.5e 4 2.4e4 2.3e 4 2.2e 4 2. 1 e4 2.0e 4 1.9* 4 1,8*4 1.7e4
- 1.6e4
- 1.Se 4 1.4e 4 1.3e 4 1.2e 4 1.1e 4 1.0e 4 9000. 0 8000. 0 7000. 0 6000, 0 S000.D 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 '-<v_- , Dat aprinte dby CJ

G Printin g Time : 10:16:0 1 A M Pag e 2 o f 6 TiTM.mi n Pag p :^R n ffi1Ginge r

AG0133050 9

• Sampl e Name:-g110211a07 rSampl e ID : "GLP1(H)1-02-16-012 " File:-g110211a.<Mf r I Pea k Name : "PFBS * Mass<es) : -239.0i«9. 0 amu,299.W80. 0 • Comment*D/U.GWSS24027011 1 {dil1;10) " Annotation : Samplf l Index : 7 7 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Result s Name : gll0211a.rd b

Sampl e Tvpe : Csncar^tration : Calculate dCone : Acq . Date : Acq . Tirae : Hidified ; Proc . Algorithm : Ncis e Percentag e Base . Sub
. Wind o Unknow n N/ A IS. 6 2/12/201 1 7:<5:3 2 P

H Ye s InteiliQu a 9 5 * : 1.0 0 Peak-Split
. Factor : 4 Kspor t Larges t

Peak : N" . Min
. Peak

Heigh t Hin
. Peak

Width : Smoothin g Width : R T Window : Expflcte dRT : Us ^ Relativ e RT : Int , Type : Retentio nTin.e : 0.0 0 0.0 0 i 30. 0 10. 6 N o Bas e T o B a 10. 5 Area : 12540< £co u Height : Star t Time : En dTime : 77000 . cp

10. t U . 2 Concentratl o Calculate dC Acq . [?at« : Acq . Tim? : Modified : n : H/ A one : 4 3, 6 2/U/201 1 10:r-:i5 S Ve s Sampl e Name : •g110211aOee - Sampl e ID : "GLP10-01-02-lW)17 - File : "g110211a.w r Pea k Name : "PFBS " Ma«c(e«) : "2S9.0/99. 0 amu,299.0/80. 0 a - Comment'DALGW210R028011 1 (dil1:10 rAnnotation:" ' Sampl p Index : 9 6 6.4e 5 6.3e 5 6.2e5
- 6. 1 e S B.Oe S 5.9e 5 5.ee 5 5.7e 5 S.6e 5 5.5e 5 5.4e 5 S.3e5 5.2e 5 5. 1 e 5 S.Oe S 4.9e 5 4.8e 5 4.7e 5 4.6e 5 4.5e S 4.4e5
-

Dat a printe d b

yCJ G Printin g Time : 10:16:0 1 A M Pag e Time-'"' " Pag g -^ R n f fij_Ginge r

AG0133050 9

• SampleNarTM:'g110211a019 " Satr^t e ID : I Pea k Name:-PFHS * Maea(e») : "399.0/99. 0 I Commen t '1. 0 ng/m L F C st d t n Ui B Q water " Sampl e Index : 1 9 Sampl e Type : Standar d Concentration : 1,0 0 ntj/m L Calculate dCone : 1.O S ny/m L Acq . Date : 2/12/201 1 Acq . Time : 2:20:5 5 A M fie i

Repor t Large : m

: Inte l litiua n - MQI l

Min . Pea k Haiuh' : Min . Pea k Width : Smoothin g Width : R T Window : Expecte d RT : U= - Relativ e RT : lr,t . Type : Retentio n Tini« : : 0 J 30. 0 11. 7 N o Baa a T o 11, 7 Area : 129527 C Height : •&6000 . 0 0 0 0

B a :o u c p '10007-27-8 " FUe:"g110211a.wi r

amu,399.0/80. 0 ami T Arviotation : ~ 3. 1 e S 3.0e 5 3.0e S Z9e 5 2.9e5 i 2.8e S 2.8e S Z7e 5 2.7e 5 ZSe S Z6e 5 ZSe 5 ZSeS : Z4e 5 Z4e 5 2.3e 5 2.3e S 2.2e 5 2,2e 5 Zle S ZleS r ZOeS ZOe S 1.9e 5 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur
. A L - Ja n 201 1 Result s Name : gll0211a.rd b

1.7e5
- 1.7e5
- 1.6e5
- 1.6e5
- 1.5e 5 1.5e5 1.4e5 1.4e5 1.3e5 1.3e5 1.2e5 ^2t>S 1,1e 5 l.leS

1.0e5 9.Se 4 9.0e4 8.5e4
- S.0e 4 7.5e 4 7.0e4 6.5e4 6.0e4 5.5e4 5.0e4 4.5e4 4.0e4 3.5e4 3.0e4 2.5e4 2,0e4 1.5e 4 1.0e 4 5000. 0 0. 0 Sampl e Name : "g110211a011 " Sampl e ID : "Solven t Kank " File : "g l 1021 la.wf T Pea k Name : "PFHS * Masa(es) : "399.0/99. 0 amu.399.(V80. 0 amu ' Commen t 'Mill ) Q Wate rTN11-0052 " Annotation : Sampl e Index : 1 1 Sampl e Type : Unt: j Calculate d Cone : Acq . L'ate : Acq . Time : Modified : Proc . Algcrithm : Mois a Percentag e Base . Sub . Wind o < c , 2/11/201 1 11:57:1 5 P N o InteiliQu a 5 0 • i : 1,0 0 P-ak-Split . Factor : 2 R-.pc.r t Larges t Peak : N o Min . Pea k Heigh t Min . Pea k Width : Smoothin g Width : R T Window : Expecte d RT : Us e Relativ e RT : Int . Type : Retentio n Time : Area : Height : Star t Time : 0.0 0 0.0 0 3 30. 0 11. 7 N o valle y 11. 7 156 7 co u 26J . c p 11, 6

Dat aprinte db y CJ

G Printin g Time : 10:16:0 1 A M Pag e 4 o f 6'^* * Ginge r

AG0133050 9 

# I Sampt e Name : "g110211a03 rSampl e 10 : "LCS-110210-4 " Pea k Name : "PFHS * Ma»»(e«) : -399.Q«9. 0 amu.399.0/80. 0 Commen t 'Spp b LCS " Annotation : ~ GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o f PFBS
. PFHS
. an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur
. A L - Ja n 201 1 Result s Name : gll0211a.rd b

Inde j 3 2 Sampl e Type : Q C Concentration : 4.9 B ng/m L Calculate dCone : 5.6 1 ny/m L Acq . Date : 2/12/201 1 Acq . Time : 6: H : 5 2 A M M:jdified : Ye s Proc . Algorithm : IntelliQua n- MQ ! Base , Sub
. Window : Peak-Split , Facto r Repor t Larges t

Pe a Hin , Pea k

Height : Min , Pea k

Width ; Smoothin g Width : R T Window : Expecte dRT : Us ^ Relativ e RT : Int . Type : Retentio nTime : 1.0 0 ra 1 0,0 0 c 0,0 0 s i 30. 0 38 C 11. 7 mi n N o 'alle y 11. 7 mi n Area : 66^165 1 count s H«ight : 1610000 . cp u Star t Tine : En dTime : 11. 5 rain 12. 1 rain p s

point s 1.5e 6

1,4e 6
1.4e 6
1.3e 6 Samptof4ame;"gl10211a068 - Sampl e ID : "GLP1(W1-02-1&O06 " Fite : •gll0211a.M r Pea k Name : "PFHS " Masc(es) : "399.0/99. 0 amu,399.0/80, 0 amu ' Comment'DALGWSS2 2 0 27011 1 ((SI1:10) " Annotation: - sampl e Index : 6 ^ Sampl e Type : Unknow n 4.ae 4 4.7e4 - 4.6e 4 4.Se4 - 4.4e 4 4.3e4 ' 4Ze 4 4. 1 e 4 4.0e 4 3.9e 4 3.8e 4 3.7e 4 3.6a 4 3.5e 4 3.4e 4 3.3e 4 3.2e 4 3.1e 4 3.0e 4 Z9e 4 ZSe4 ' Z7e 4 Z6e 4 2.Se 4 2.4e 4 Z3e4 - 2.2e 4 Zle4 - Z0e 4 1.ge 4 1.8e 4 1.7e 4 1.6e 4 1.5e4 - 1. 4

1.3*4 ' 1.2*4
- 1.1*4
- 1.0e4
- 9000.0
- B000.0
- 7000.0
- 6000.0
- 5000. 0 4000. 0 3000.0
- 2000. 0 1000. 0 0. 0 J\^^-^^' ^ .^,)A »
1 0 1 1 1 2 1 3 1 4 1 5 1 8 1 7 Dat aprinte db y CJ G Printin g Time : 10:16:0 2 A M Pag e 5 o f 6Ginge r

AG0133050 9 

# 1 Sampl e Name : "91102118077 " Sampl e ID : 'GLPI0-01-02-16-0 1 rFile : "81102 1 la.wi T Pea k Mame : "PFHS " Mass<es) : "399.0/99. 0 amu,399.0/80. 0 amu " Commen t "DA L G W SS2 4 0 27011 1 (di l 1:10 rAnnotation : " " Sampl e Index : 7 7 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Result s Name : gll0211a.rd b

Unk i N/ A Acq . Date : Acq . Time : Modified : K T Window : E.xpecte dRT : Us e Relativ e Int . Type : Retentio nT i Area : Height : K

T

me : 2/12/201 1 7:^5:3 2 P

M Ye s 30, 0 11. 7 n N o Manual 11. 7 t i 15-'6S4: 8 : o 3050000 . c 3.0* 6 3.0* 6 Z9* 6 Z9* 6 Z8e 6 2.B« 6 2.7* 6 2.7* 6 2.6* 6 2.6e 6 2.5e 8 2.5e 6 2.4e6 : Z4e 6 2.3*6
- Z3e 8 2.2e 6 Z2e 6 Z1e 6 Z1e 6 2.0e 6 2.0* 6 1.9* 6 1.9* 6 1.8e6 1.3e 6 1.7* 6 1.7e6 1.6* 6 1.6e6 l.Se 6 1.5* 6 1.4* 6 1.4* 6 1.3*6
- 1.3e 6 1.2e6
- 1.2e6 1.1e 6 1.1e6
- 1.0e6
- 9.5* 5 9.0* 5 8.5* 5 8.0* 5 7.5e 5 7.0e 5 6.5e S e.OeS 5.5e 5 S.Oe S 4.5e S 4.0e 5 3.5*5
- 3.0* 5 2.5* 5 ZOeS I.SeS
1.0* 5 5.0* 4

0. 0 

## mI Sampl e Name : "g l 1021 1 aOSff- Sampl e ID : 'GL P 1(MH-02-1B-0 1 rFile : "g110211a.wif r i Pea k Name : "PFHS " MaM(*s) : "399.0/99. 0 amu,3g9.0/80. 0 amu ' I Comment " DALGW210R028011 1 (di!1:10) " Annotation : ~ impl e Type : mcantrati o Unk f N/ A Calculate dCon e Acq . fate : Acq . Time : l1odiii«d : R T Window : E:<pacte dRT : U36 Relativ e Int . Type : Retentio nT i Area : Height : Star t Tin,e : En dTime : R

T 312 . 2/12/20 ! 10:27:£ B Ye s 30, 0 11. 7 H o Manual 11. 7 30135E9 3 5370000 , 11. 3 12. 4 1 P

M

s

m CO- J m m 5,3*6
-

5.2* 6 5.1* 6 5.0* 6 4.9*6' 4.8*6
- 4.7* 6 4.6* 6 4.5* 6 4.4* 6 4.3* 6 4.2* 6 4.1* 6 4.0* 6 3.9* 6 3.6* 6 3.7* 6 3.6e 6 3.5* 6 3.4* 6 3.3* 6 3.2* 6 3.1* 6 3.0* 6 Z9* 6 Z8e 6 Z7* 6 Z6* 6 Z5e 6 Z4* 6 Z3*6 ' 2.2* 6 Z1*6
- Z0*6
- 1.9* 6 1.6*6
- 1.7* 6 1.6e6 1.5e6 1.4e6
- 1.3e6 ' 1,2e6 1.1*6
- 1.0*6
- 9.0e S 6.0* 5 7.0* 5 6.0* 5 S.Oe S 4.0e S 3,0* 5 Z0* 5 1.0* 5 0. 0
Dat a printe d b yCJ G Printin g Time : 10:16:0 2 A M Pag e 6 o f 6 -IJiaSJDi Q Parj g -^ Q n f R 1»* * Ginge r

AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSampt^uit s Name : Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 gll0228a.r<a b

• g110228a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -6.87e-H00 3 x'^ 2 + 1.12e-H00 6 x-

K-4.99e-t-00 3 ( r= 0.9998 ) 4.0e7 - 3.9e7 - 3.8e7 - 3.7e7 - 3.6e7 - 3.5e7 - 3.4e7 - 3.3e7 - 3.2e7 - 3.1e7 - 3.0e7 - 2.9e7 - 2.8e7 - 2.7e7 - 2.6e7 - 2.5e7 - 2.4e7 - 2.3e7 - 2.2e7 - 2.1e7 - 2.0e7 - 1.9e7 - 1.8e7 - 1.7e7 - 1.6e7 - 1.5e7 - 1.4e7 - 1.3e7 - 1.2e7 - 1.1e7 - 1.0e7 - 9.0e6 - 8.0e6 - 7.0e6 - 6.0e6 - 5.0e6 - 4.0e6 - 3.0e6 - 2.0e6 - 1.0e6 - 0.0 - • / 

### f i 

# i / 

### / / / / ,-• / / / 

### / / / ' / 

### / / • / / / 

### / / / / 

### / / / / / / / 

### / / / / 

### / / / / / / / / / / / / / / / / / / / /



### / / / 

### ,.- •

^-' '

8 1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 Concentration , ng/m L 3 2 3 4 3 6 3 8 4 0Pag p 4 2 4 4 4 6 4nnffi 1 4 8 5 0 Printin g Time : 10:24:1 3 A M Printin g Date : Thursday , Marc h 17 , 201 1 Pag e 1 o f 1* * Ginge r

AG0133050 9

• Sampl e Name ; •a110228a019 ' Sampl e ID : "10007-27-8 " File ; "g110228a.wif r Pea k Name : "PFOS " Maac{*s) : '49S.O/S9. 0 amu.499.0/BO. O amu.499.0/130. 0 amu " Commen t '1, 0 ng/m L F C st d i n Mifl i Q water " /Annotation : " Sampl e Index : 1 9 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Result s Name : gll0228a.rd b

impl a Type ! 1.0 0 ng/m L Calculate d Cone : Acq . Date : Acq . Time : Hodilied : Proc . Algorithm : Nc-is e Petcencage ; Base . Sub . Windo w Peak-Split . Fact o Repor t Larges t P e Min . Pea k Hei^iht : Min . Pea k Width : Smoorliin g WiJth : K T Window : Expscte d RT : 0.95 1 2/28/201 1 9:40:2 0 P N o ntelllQ u 5 0 1.0 0 r : 2 ak : N:: . 0. 0 0. 0 0 30. 0 12. 5 3.2* 5 3.1*5
- 3.1*5
- 3.0*5
- 3.0* 5 Z9*5
- 2.9* 5 2.6* 5 2.8*5
- Z7* 5 Z76 5 2.6* 5 2.6* 5 2.5* 5 2.5* 5 2.4* 5 2,4* 5 2.3* 5 2,3*5
- 2.2* 5 2.2* 5 ZleS

Z1* 5 2.0* 5 2.0* 5 1.9* 5 Sampl e Nam* : "g l 10228a011 ' Sampl e ID : 'Solven t B Pea k Name : "PFOS " Ma«*{ee) ; *4£ * ' " " Commen t "Mil U Q V\bterTN11-007 rAnnotation : ~

Dat a printe d b

yCJ G Printin g Time : 10:23:1 7 7U 4 Pag e 1 o f 3 limsjm ] pRgp4 1 n ff> 1** * Ginge r

AG0133050 9

• Sampl e Name ; -g11022Sa03 rSampl e ID : "LCS-11022&4 " Pea k Name : "PFOS " Ma»s(es) : "499.0/99. 0 an)u.499.0/BO. 0 Commen t *5pp b LCS * Annotation : " Sampl e Index : 3 2 Sampl e Type : Q C Concentration : 4.9 B ng/m L Calculate dCone : 5.2 7 ny/m L Acq . Date : 3/1/201 1 Acq . Tine : !2:? 4 •.2 i A H GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS
. PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Result s Name : gll0228a.rd b

llDdilied : N o Proc . Algorithm : IntalliQua n- MQl ! Ntis B PeLcentaqo : 5 0 Base . Sub
. Window : 1.0 0 mi n Peak-Split
. Factor ; 2 Repor t Larges t

P«ak : Nc

Hin
. Pea k

Height : 0.0 0 cp a Hin
. Peak

Width : 0.0 0 se c Sn-aothin g width : 0 point ; R T Windov : 30. 0 se c Expecte dRT : 12. 5 mi n \}c ^ Relativ e RT : H o 1.7* 6 1.6* 6

t . Type : alle y 1.6* 6 1.5*6
- 1.5* 6
1.4* 6
1.4e 6 1.3e 6 1.3e6
- 1.2e 6
1.2* 6 1.1e6 < l.leS

1.0e 6 9.5e 5 9.0e 5 i

" 8.0e 5 7.5e 5 7.0e 5 S.Se 5 6.0* 5 5.5* 5 5.0* 5 4.Se 5 4.0* 5 3.5* 5 3.0* 5 2.5* 5 ZO* S 1.5* 5 1.0* 5 5.0* 4 0. 0 

# J Sampt e Name : "g11022Ba041 - Sampl e ID : "LCS-110228-13 - File : -g110228a.<M r Pea k Name : "PFOS " Uaaa{ea) : "499.0/99. 0 amu,499.0/80. 0 amu,499.0/130. 0 amu " Commen t "Spp b LC S ECF " Annotation:" " :ampl e Sampl * Type : Calculate dCo i Acq . L'ate : Acq . Time : Modified : R T Windo-v : E:;pect8 dRT : Us e Relativ e I
Hfliyht : Star t T : En dTim i CC 5.0 4 1.02*6
- 1.00*6
- 9.80* 5 9.60* 5 9.40* 5 9.20* 5 9.00* 5 8.B0e 5 8.60e 5 8.40e 5 8.20e5
- 8.00* 5 7.80* 5 7.60*5
- 7.40e 5 7.20e 5 7.00* 5 6.80* 5 6.60* 5 6.40*5
- 6.20* 5 6.00* 5 5.80* 5 5.60* 5 5.40* 5 5.20* 5 5.00* 5 4.80* 5 4.60* 5 4.40* 5 4.20*5
- 4.00* 5 3.80* 5 3.60* 5 3.40*5
- 3.20* 5 3.00* 5 2,80*5
- 2.60e 5 2.40e 5 2.20e 5 2.00* 5 1,80* 5 1.60* 5 1.40* 5 1.20e 5 1,00e 5 8.00* 4 6,00* 4 4.00* 4 Z00* 4 0.0 0 Dat a printe d b

yCJ G Printin g Time : 10:23:1 8 A M Pag e 2 o f 3 agp4?nffi 1** * Ginge r

AG0133050 9 

# T Sanpl e Name : "g l 10228a066 - Sampl e ID:"GLP10-01-02-1fr0i rFile : "g l 10228a.wr T Pea k Name ; 'PFOS ' Mass(**) : "49S.0/99. 0 amu.499.0/80. 0 amu,499.0/130. 0 amu " Comm*n t "DA L GWSS2 4 0 27011 1 (d a 1:100) " Awiotalion : " GLP I 0-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur
. A L - Ja n 201 1 Result s Name : gll0228a.rd b

Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 51') . ng/m L Acq , Date : J/1/201 1 Acq , Time : 10:47:2 5 A M Modified : R T window- : E.tpecta dRT : V mRelativ e
Heigh t Star t : En dTi r Ye s

IBEOOO . cp s 12, 1 mi l IZ.- J mi l

1 

# i 1 7.8* 5 7.6* 5 7.*, 5 7Ze 5 7.0* 5 6.8* 5 6.6* 5 6.4* 5 6.2* 5 6.0* 5 5,8* 5 5,6* 5 5,4* 5 5.2* 5 5.0* 5 4.8* 5 4,6*5
- 4.4*5
- 4,2.5
- 4.0*5
- 3.8*5
- 3.6*5
- 3.4*5
- 3.2*5
- 3.0*5
- Z8e5
- Z6e 5 Z4*5
- 2.2e5
- Z0e 5 1.8e 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6,0* 4 4.0* 4
2.0* 4 O D 1 2

1Z40 ^

12.30 ^ 5 2

h---n
. Sampl e Inde x Sampl e Type : Concantrati o Calculate d Con e Acq
. Dace : Acq
. Time : Hodified : R TWindow : E;:pocte d RT : Us e Relativ e Int
. Type : Retentio n T i Haiulit : Star t Tin,« : R

T 7 0 Unkno^- n N/ A 556
. 3/1/20 1 11:59: J Ye s 30, 0 12. 5 N o Manua l 12. 5 601B60 1 1110000
. 12. 2 

# I SampI * Name : 'gl10228a070 - Sampl e ID : 'GLP I 001-02-16-017 " File : "g l 10228a.wtf r Pea k Mame ; "PFOS " Massfee) : "499.0/99. 0 amu,499.0/80. 0 amu,499.0/130. 0 amu " Commen t "DA L GW210 R 0 28011 1 (d U 1:100) " Annotation; - 1,10*6
- 1.08*6
- 1.06* 6 1.04* 6 1.02*6
- 1.00* 6 9.80* 5 9.60* 5 9.40* 5 9.20*5
- 9.00* 5 8.80*5
- 8.60* 5 8.40* 5 8.20* 5 8.00* 5 7.80* 5 7.60* 5 7.40* 5 7.20* 5 7.00* 5 6.80* 5 6.60* 5 6.40* 5 6.20* 5 6.00* 5
^ 5.60* 5
^ 5.60* 5 I5.40* 5 5.20* 5 5.00* 5 4.80* 5 4.60* 5 4.40* 5 4.20*5
- 4.00* 5 3.80* 5 3.60*5
- 3.40*5
- 3.20*5
- 3.00* 5 Z80e 5 Z60e 5 Z40* 5 220* 5 200* 5 1.80* 5 I.eOe S 1.40e 5 1.20* 5 1.00* 5 8.00* 4 6.00e 4 4.00* 4 2.00* 4 0.0 0 Dat aprinte db y CJ G Printin g Time : 10:23:1 8 /\ M Pag e 3 o f 3 TiT^e.mi n Pgj g il' ^ n f R 1Buste r J293020 3 GLP I 0-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Batc hName : bll0310a.da b
b110310a.rd b (PFOS) : "Quadratic " Regressio n (" 1 /x " weighting) : y= -0.0004 8 x'^ 2 -H.3 4 x•

^ 0.051 4 ( r= 0.9998 )

( D < W 

### < ( 0 135 - 130 - 125 - 120 - 115 - 110 - 105 - 100 - 95 - 90 - 85 - 80 - 75 - 70 ^ 65 - 60 -



### . • 55 :



### . 5 0 J ] 45 - 40 - 35 - 30 : 25 : 20 - 15 - 10 - 5 - 0 - 

### ,.•' ' , ' ,-• ' ^ ,*/" '

, ' ,-'' ' /.•-" " / ' '

./ ' , '

y "

• • ,x' '



### / ' -' ' _-•• •



### ^' ' ,^ ' ^ x 

### ,.- 4

^,-'' y '



### /' ' ,/^' ' ^z' ' 

### '' ' ^ ^ y''' ' 

### •,. "

,,-'' ' X

/ ,,--- ' '-•' ' ^ y ' 

### / " • ,,•'' '

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 6 0 6 5 7 0 7 5 8 0 Analyt e Cone . / I S Cone . 8 5 9 0 9 5 10 0 Dat a printe d byST W Printin g Time : 9:46:1 7 A M Printin g Date : Thursday , Marc h 17 , 201 1 Pag e 1 o f 1 Pag e 4 4 o f 6 1' • Buste r

J293020 3

Proc . Algorithm : Nois e Pei-centage : Base . Sub
. Hindc v Peak-Split
. Fact o Repor t Larges t

P e M m . Pea k

Heiyht : Hin
. Pea k

Width : Smootliin g Widtli : K T Windov : Expecte dRT : ntelUQu a
k :
J U 1 2 5 0 1.0 0 1 Nt . 0.0 0 0.0 0 0 0 • 9 T : •^a s V3lU y : 12. 7 30172 7 c

< 12. 7 • Sampl e Name : "61103103022 * Sampl e ID : "10007-32-10 " Fil* : "b110310a.wif r I Pea k Name : "PFOS " Mau(*c) : "499.0/130. 0 amu.499.0/99. 0 amu,499.0/80. 0 amu " I Comm*n t "5. 0 ng/m L F C M d i n Synth
. Water " Annotation ; ~ Sampl e Index : 2 2 Sampl e Type : Standar d Concentration : 5.0 0 ng/m L Calculate dCone : A.' l mj/m L84* 4 Acq . Date : 3/10/201 1 Acq . Time : 11:11:0 2 P M 8.2* 4

7.8* 4 7.6e4
- 7.4* 4 7.2e 4 7.0e 4 6.8* 4 6.6* 4 6.4* 4 6Z*4
- 6.0*4
- 5.6*4
- 5.6* 4 5,4* 4 5.2* 4 5,0* 4 4.8* 4 4.6* 4

^ 4.4* 4 I 4,2* 4 I 4.0e4 - 3.8*4 - 3.6e4 ' 3.4e 4 3.2* 4 3.0* 4 Z8e4 - ZSe 4 Z4* 4 Z2* 4 2.0* 4 1.8* 4 1.6*4 '

1.0* 4 6000. 0 6000. 0 4000. 0 2000. 0 0.0-1
- GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS
. PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur
. A L - Ja n 201 1 Batc hName : bll0310a.da b



# Jk : Printin g Time : 10:27:2 7 7V M Printin g Date : Thursday , Marc h17 , 201 1 SampI * Nam* : "51103103012 " Sanpl e ID : "10010-213 * File : "b l 10310a.*rt r 

### I P*a k Nam* : 'PFOS * llrtaea(**) ; "499.0/130. 0 amu,499.0/99. 0 amu,499.0/80. 0 amu " Commen t "Metho d Bbnl TAnnotation : ~ Sampl e Index : 1 2 Unkn i N/ A 0.01S 9 n<j/m L 3/10/201 1 Sampl e Type :

tio i dC i Calcu l Acq . L ' Acq . T

Base
. Sub
. Window : P-?ak-Split , Factor : B-ipor t Larges t Paa k Min
. pea k

Height : Min
. Pea k

Width : Smoorhin q Width : R TWindow : Expecte d RT : Us e Relativ e RT : 1.0 0 2 N o 0,0 0 0.0 0 0 30. 0 12. e ¥ 3 3 Int
. Type : Valle y Retentio n Time : Area : 3 6 H-iight : 1. 1 Star t Time : En d Time : 12. B 1 0 co u i-e»0O: « 12. 7 12. e

Pag e 1 o f 3' * Buste r

J293020 3
I Sampt e Name ; -bl10310a038 " Sampl e ID:"LCS-110307- rFil* ; 'bl10310a.vflf r I P*» k Nam* : "PFOS " Mau(*s} : "499.0/130. 0 amu.499.0/99. 0 amu.499.0/80. 0 amu " I ConuTwn t "lOppbLCS " Annotation: ' Sampl e Index : 3 5 GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

Sampl e Type : Q C Concentration : 9.9 4 ng/m L Calculate dCone : 11. 1 na/m L Acq . Date : 3/11/201 1 Acq . Time : 3:59:3 6 A M Hoditied : N o Proc . Alqorithm : IntelliOua n- MO H Nois e Peicentage : 5 0 Base . Sub
. Window : 1.0 0 mi n Peak-Split
. Factor : 1 Repor t Larges t

Peak : Nf

. Hin
. Pea k

Heioht : 0.0 0 cp s Hin
. Pea k

Width : 0.0 0 se e Smootliin g Width : 0 point s R T Window : 30. 0 se c Expecte dRT : 12. 8 mi n Usf l Relativ e RT : Ye s Int . Type : Valle- / Retsntio nTims : 12. 7 mi n Area : 59655 5 count s Height : ?.01e*00 5 cp s Star t Tirae : 12. 5 mi n En dTime : 12. 6 mi n 3.0* 5 3.0* 5 2.9* 5 Z9e 5 2.6* 5 2.8* 5 Z7e 5 2.7* 5 2.6* 5 2.6* 5 2.5* 5 Z5e 5 Z4* 5 24e 5 Z3e 5 23* 5 2.2e 5 2.2* 5 Z1e 5 Z1e5
- ZOe S Z0* 5 SampI * Nam* : "bn0310a048 " Sarr ^ 10 : "LC&-110307 - P*a k Name : "PFOS " Mas*(es) : "499.0/130. 0 anui,499.0/ 5 Commen t "lOpp b LC S ECF " Annotalion:" " Sampl e Index : J 9 10. 0 ng/m L Calculate d Acq , L'ate : Acq , Time : Modified : R TWindo-^ : Expecte d R

T Con e ! 11. 2

3/11/201 1 7:00:0 6 AM V9 S 30. 0 12. e Batc hName : bll0310a.da b
i rFile:"b110310a.wf r 19. 0 amu.499.0/a0. 0 amu "

1.26*5 - 1.24*5 - 1.22*5 - 1.20e5 - 1.18*5 - 1.16*5 - 1.14*5 - 1.12*5 - 1.10*5 - 1.08*5 - 1.06*5 - 1.04*5 - 1.02*5 - 1.00*5 - 9.80*4 - 9.60*4 - 9.40*4 - 9.20*4 - 9.00*4 - 8.80*4 - 8.60*4 - 8.40*4 - 8.20*4 - 8.00*4 - 7.80*4 - 7.60*4 - 7.40*4 - 7.20*4 - 7.00*4 - 6.80*4 - !
. 6.60*4 - ^ 6.40*4 - j 6.20*4 -
' 6.00*4 - 5.80* 4 5.60*4 - 5.40*4 - 5.20*4 - 5.00*4 - 4.80*4 - 4.60*4 - 4.40*4 - 4.20*4 - 4.00*4 - 3,60*4 - 3,60*4 - 3.40*4 - 3.20*4 - 3.00*4 - Z80*4 - 2,60*4 - Z40e4 - Z20*4 - 2.00*4 - 1.80* 4 1.60*4 - 1.40* 4 1.20* 4 1.00* 4 8000.0 0 6000.0 0 4000.0 0 2000.0 0 0.0 0 

## Jk ^ Printin g Time : 10:27:2 7 A M Printin g Date : Thursday , Marc h17 , Pag e 2 o f 3 Tim , mi n Pajo^Rn f R1Buste r

J293020 3
I Sampl e Nam* : "b110310a055 " Sampl e ID : "GLP1(>O1-O2-16-006 " File : "bllOaiOa.wif r I Pea k Name : "PFOS " Mass(*«) : "499.0/130 0 amu.499.0/99. 0 amu.4d9.OQ0. 0 amu " • Comment"D/U.GWSS22027011 1 w/IS " Annotation: - Sampl e Index : 5 5 Sampl e Type : GLP10-01-02 : Interi m Repor t 1 6 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1 Batc hName : bll0310a.da b

N/A Calculate d Con e Acq
. Date : Acq
. Time : : ?-5 7 3/11/201 1 9:0£:2 1 A

M

: 12. 7 7 0 4 7 0 7 C i 9.eSetOO J 9.8* 4

9.2* 4 9.0* 4 8.8* 4 8.6* 4 6.4* 4 8.2* 4 8.0* 4 7.8* 4 7.6* 4 7.4* 4 7.2* 4 7.0B 4 6.8* 4 6.6*4
- 6.4* 4 6.2* 4 6.0* 4 5.8e4
- S.6e 4 5.4* 4 5.2* 4 5.0* 4 4.8* 4 4.6*4
- 4.4* 4 4.2* 4 4.0* 4 3.8* 4 3.6* 4 3.4* 4 3.2* 4 3.0*4
- Z8e 4 Z6* 4 2.4* 4 Z2* 4 Z0* 4 1.8* 4 1.6* 4 1.4*4
- 1.2* 4 1.0e 4

eooo. o 6000. 0 4000. 0 2000. 0 I nMniiiiiidi^i.
. 1 0 1 1 1 2 1 3 1 4 I S 1 6 1 7 Printin g Time : 10:27:2 7 A M Printin g Date : Thursday , Marc h 17 , 201 1 Pag e 3 o f 3 Pag e 4 7 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1


### ATTACHMEN TC : ANALYTICA L METHO D

Pag e 4 8 o f6 1Ana^Js°S°pi^BsW^®S'pF0§f,>3teSh<^^^^^ ^ for1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1


# 3 M Environmenta l LaboiafxN y

l\/letho d Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate r b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e D a te : Q U 1( 1 f o 7
Approve d By :


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

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

t Injectio n Analysi s Pag e 4 9 o f e iGLP10-01-02 ; Interi m Repor t 16
. , . . , * c . < ^ i s n^/Az-znA^- i Analysi s o f PFBs}^WismPvo§^^G}^m^siLf\mer) l for1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

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

yrequire preparatio n b

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

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

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

t multipl e concentrations
. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix
. Sampl e results fo rspike s outsid e o f70 % t o 130% , ma yb e flagge d 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 a t least 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o determin e th e statemen t of accurac yfo ranalytica l results
. 

### 3 Definition s 3. 1 Calibratio n Standar d Asolutio n prepare d byspikin g a know n volum e ofth e Wori<in g Standar d (WS ) int o a predetermine d amoun t o fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method
. Calibratio n standard s are use d t o calibrat e th e instrumen t respons e wit h respec t t o analyt e concentration
. 3. 2 Laborator yDuplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

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

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

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d 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 referre d t o a s a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 0 o f6 1AZlisl!'pFBsWMlm%6^%]Gh§^^^^ ^ for1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n 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 fiel d an d laborator y procedures
. Analysi s ofth e FD S compare d t o that ofth e firs t 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 (FIVIS ) Asampl e t o whic h know n quantitie s o fth e targe t analyte s ar e adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d 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 o fth e sampl e container
. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample
. I fth e expecte d rang e ofanalyt e concentration s i s unknown , multipl e spike s a t varyin g level s ma

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

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

ycomplicat e th e interpretatio n o fth e sampl e analysis
. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot 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 ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s o fanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s are no t know n o rma

yvary . At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d place 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
. A t 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 ylike a laborator

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

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

ysampl e t o determin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results
. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e determine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations
. LMS s are optiona l fo ranalysi s ofaqueou s samples
. 3. 9 Laborator ySampl e Aportio n o raliquot ofa sampl e receive d fro m th e fiel d fo rtesting
. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e 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
. T o simplif ydat a reporting , th e LLOQ 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 o fquantitatio 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 o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 1 o f6 1

### ^!^sl!?F^^M!mkm^^^<ii^si^m^en t fo r1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

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

ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that ar e use d wit h othe rlaborator ysamples
. Th e metho d blan k i s use d t o detennin e i 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 no t normall y foun d i n th e sample(s)
. Asurrogat e compoun d i s typicall ya targe t analyt e wit h a t least on e ato m containin g a n isotopically-labele d substitution
. I fused , surrogate(s ) 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 procedur e includin g sampl e collection , preparation , an d analysis
. Inclusio n ofa sun'ogate analyt e i s a n optiona l qualit ycontro l measure an d i s NO Trequired
. 3.1 5 Workin g Standar d (WS ) Asolutio n ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o prepar e calibratio n standard s an d othe rrequire d analyt e solutions
. 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yofth e standard s fo rthi s metho d have not 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 fil e ofmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l informatio n an d cautions
. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware
. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s 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 ; Direc

t Injectio n Analysi s Pag e 5 2 o f 6 1GLPI0-01-02 ; Interi m Repor t 16 ^ , , . , . x : ^ j ^ , r

. r\M/y AI'-sr^

^ A Analysi s o f PFBs,LpRTsJg?,SPFdr:?i?.>3fe§i(i^%fe^safn^fc^ ^ for1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1
Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination
. Thes e ma yinclude , bu t are no

t limite d to : was h bottles
. Teflon ® line d caps , autovia l caps , HPLC parts , etc
. Th e us e ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h perfomnanc

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

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25pL , 50pL , lOOpL , 250|JL , 500pL , 1000|JL
. 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s as appropriat e Centrifug e capabl e ofspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 \x m Analytica l Column : Betasi l C18,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

Area-quadrati ccurve fit , 1/ xweighted
. Ru n Time : ~ 1 7 minutes
. Th e previou s informatio n i s intende d a s a guide ; alternat e condition s an d equipmen t ma yb e use d provide d tha t dat a qualityobjective s ar e met
. ETS-8-044. 0 Pag e 5 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 3 o f 6 1GLPI0-01-02 ; Interi m Repor t 16 , , , . , , . i : Aj i i rnAinAi'-.nA i Analysi s o f PFBs.Lr^Fi-TsJ^iS^PTO^iPtefeSncJ^^fefisafn^^^^ ^ for1 4 day s fro m 04/04/20 1 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e PFBA PFPe A 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 mayhave th e adde d benefi t of increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a are 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 instmments an d equipmen t ma yb e used
. 7 Reagent s an d Standard s 7. 1 Chemical s Water - Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A
. C.S
. Reagen t Grad e 7. 2 Standard s Perfluorobutanoi cAci d (PFBA-C 4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfiuorooctanoi 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-C1 0 acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C I 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 ; Direc t Injectio n Analysi s Pag e 5 4 o f 6 1GLP10-01-02 ; Interi m Repor t 16
. , , . , xr. < ^ i ^

n Atr

^ Am^ AA Analysi s o f PFBS,lr>FfW@?,Sii#6T§f,)Gte§i(i^1.fe^s^fnpl;^rrent , fo r1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1
Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s ma yb e used
. 

### 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—Weig h 0. 3 g o fAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t water
. Note : Alternativ e volume s ma yb e prepare d a s lon g as th e ratio s o fth e solven t t o solut e ratio s ar e maintained
. 

### 7. 4 Stoc k

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

d preparatio n procedur

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

solution s t o appropriat e levels
. 100 |jg/m L targe t analyt e SSSs—^Weig h ou t 1 0 m g ofanalytica l standar d (correcte d fo rpercen t sal t an d purity ) an d dilut e t o 10Om 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 connectio n i s give n belowfo rPFOS
.

, ^ ^ - r^ molecula rweigh t o fanio n sal t correctio n facto r= = moclecula rweigh t o fsal t

4g Q PFO S (K^ - )sal t correctio n facto r= ^^ ^ = 0.927 5 53 8 1 0 m g CsFiySOa'K

* wit h purit

y90 % = 8.35m g CsFiySOs " (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 Mg/m L (500 0 ng/mL ) mixe d workin g standard—^Ad d 0.5m L eac h ofth e 100pg/m L SSS s t o a 10m L volumetri c flas k an d brin g u p t o volum e wit h solvent
. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L o fth e 5 pg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflas k

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m L mixe d standard—^Ad d 625p L ofth e 5 pg/mL-mixe d wori<in g standar d solutio n t o a 25m L volumetri c flas k an d brin g u p t o volum e wit h solvent
. Storag e Conditions—Stor e al l SSS s an d wor1<in g standard s i n accordance wit h laborator ystandar d operatin g procedure o ri n a refrigerato ra t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation
.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 5 o f6 1GLP10-01-02 ; Interi m Repor t 16 ^ , , . , ^ r^ j , x

- njiir^Ai-^n^ A Analysi s o f PFBS,Lp?i-T^JS'iS>pF%1?f,tefefncJiafef^sa'fe¥rent , fo r1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

7. 5 Calibratio n Standard s Usin g th e wori<in g standard s describe d above , prepar e 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 ofwate ran d worthin g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline
. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d a s needed
. Concentratio n o fWS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS,/J
.

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 f AST 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 centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial
. Plasti ci s prefen-ed ove rth e us e o fglas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass
. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water
. Prepare metho d Q C sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials
. Prepare 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 cfi l (

y= ax ^ •• • b x•* - c) , weighte d 1/

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

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

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfi t ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t mee t th e pre-determine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts ar e no t a t least twic e that o fth e metho d and/o rsolven t blanks
. Th e coefficien t ofdetemninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 6 of6 1Al^Bi°s\so°SsWMimkoS^^ ^ for1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

b e withi n ±30%
. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata
. Aminimu m o f6 points wil l b e use d t o construc t th e calibratio n curve . I fth e calibratio n curve doe s not meet acceptance criteria , perfor m routin e maintenance o rprepar e a ne wstandar d curve (i fnecessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

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 constnjct th e calibratio n curve , a t a minimu m afte rever ytent h sample , no

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

d i n th e curve shoul d b e furthe rdilute d an d reanalyzed
. 1 0 Qualit yContro l 10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LOQ of0.02 5 ng/mL
. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e fina l report
. 

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

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

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

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

d deviatio n o fth e are a counts ofthes e metho d blank s shoul d b e calculate d an d reported
. I f th e mea n are a count s ofth e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ mus t b e raise d t o th e firs t 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 determin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made
. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field
. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s fiel d blanks
. 10. 4 Surrogat e Spike s Surrogat e spike s are no

t require d bu t ma

yb e use d o n projec

t specifi crequirements
. 10. 5 La b Contro l Sampl e Triplicat e la b contro l spike s a t a minimu m 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 offiv e t o te n time s highe rtha n th e targete d LO Q an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t ofth e curve . Th e relative standar

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

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

t Injectio n Analysi s Pag e 5 7 o f 6 1GLP10-01-02 ; Interi m Repor t 16
. , ,. ^ , . t ^

y i ^ Kn>i/n/i/TA ^ ^ Analysi s o fPFBs,ir-Ft-Tsief',^i5r6'§f.>3feSh(j^%fe0safniSi6i«'re n fo r1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1

10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s offiel d 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 flagge d as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targete d fortificatio n level s shoul d b e a t leas t 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 fiel d duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t 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 : A
. X rJ /

, .X (Pea k

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

^ xD F D F = facto rb

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

„ _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 perfomrianc

e parameter

s that are no

t achieve d must b e considere d i n th e evaluatio n ofth e data
. Nonconfonnance t o an yspecifie d parameter s must b e describe d an d discusse d i fth e Technica l Manage r(non GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data
. I fcriteri a liste d i n thi s metho d performance sectio n are no t met , maintenance ma

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

t ofth e report
. 12. 1 Syste m Suitabilit y Syste m Suitabilit

ystandard s are no

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

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

t th e beginnin g ofeac h analytica l nj n prio rt o th e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mi d leve l o fth e calit)ratio 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 of55 % an d a retentio n tim e RS D o f52 % t o b e compliant
. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t ofdeterminatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

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

yCCVs not meetin g thes e criteri a must b e reanalyzed
. ETS-8-044. 0 Pag e 1 0 o f 1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 8 o f6 1GLP10-01-02 ; Interi m Repor t 16, , , .. . . rAj , , rn.Ai^Ai'-^r^A A Analysi s o f PFBS,k5i?i-TsJg?,S:pFGl§fi>3feg-ici4%fe?Ssa".ti^t|rrent, fo r1 4 day s fro m 04/04/201 1 Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1
Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % o f standard ) an d th e mas s spectra l respons e ofuniqu e ions
. 12. 3 Sensitivit y Th e targete d limi t ofquantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n ofappropriat e blank s an d th e accurac

yo fth e low-leve l calibratio n curve points
. Refe r t o Sectio n 1 0 fo radditiona l details
. 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s ar

e designe d t o generat e data that are accurat e t o -H/-30%
. Sectio n 1 0 contain s additiona l infomnatio n regardin g th e require d accurac yoflaborator

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

ymatri xspikes
. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field
. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s fiel d blank s o rrinse blanks
. Sectio n 1 0 contain s additiona l infomiatio n regardin g th e require d precisio n o flaborator ycontro l spikes
. 

### 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfomiin g thi s metho d wil l b e dispose d ofappropriately
. Th e origina l sample s wil l b e archive d a

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

d pre p sheets/records , instrumen t ru n lo g (instrumen t batc h records , instalmen 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 Detenninatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 9 o f6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Avenu e AInvestigatio n Area ; Decatur , A L - Ja n 201 1


### ATTACHMEN TD : DEVIATION(S )

Pag e 6 0 o f 6 1GLP10-01-02 ; Interi m Repor t 1 6 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate rSample

s 

# REC0*frcJfi^tl'imW^/W6^SSS^0RMANC E

/
. Identificatio n Stud y/ Projec t No
. GLP10-01-02-1 6 Date(s ) o f Occurrence : g110228 a an d g110211 a Documen t Number : 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 D GP O D Other :



### //
. Descriptio n (attac h extr a pages a s needed ) Metho d Requirements : 1
. LC S averag e recoverie s withi n ±20 % (sectio n 10.5)
. 2
. FM S recover

ywithi n ±30 % (sectio n 10.6)
. 

### Actua l procedure/process : 1
. Th e averag e PFO S recover yfo rth e 3 0 pp b LC S (linear-^ branched ) wa s 133 % (g1102 1 la)
. Th e averag e PFO S recover

yfo rth e 3 0 pp b LC S (linea r• ^ branched ) wa s 125 % (g l 10228a)
. 2
. Samplin g locatio n 210R ; th e recover yo fth e FM S Hig h sampl e fo rPFO S wa s 68.1 % (g l 10228a)
. 

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

### Correctiv e Actio n ( D Ye s 0 No

) Reference : Acceptabilit yo fth e nonconformin g work : 1
. Th e recoverie s fo rth e 3 0 pp b LC S (linea r+ branched ) at 133 % an d 125 % wil l b e flagge d I n th e fina l report
. Th e las t fiftyLCS s fo rPFOS , includin g th e LC S prepare d wit h thi s study , wer e evaluate d b yETS-12-01 2 t o determin e th e metho d analytica l uncertainty
. Th e analytica l uncertaintywhe n evaluate d byETS-12-01 2 wa s determine d t o b e ±17 % fo rPFOS
. However , th e analytica l uncertaintyfo rthi s stud ywil l b e se t at ± 33% , base d o n th e recover yo fth e hig h set s of linea r+ branche d LCS
. 2
. Th e FM S Hig h recover yfo rPFO S wil l b e flagge d i n th e fina l report
. Th e recover yi s withi n th e metho d uncertaintyo f±33%
. Actions : D Haltin g o fWor k D Clien t Notificatio n D Wori < Recal l D Withholdin g o f Repor t 0 Other : Deviation s wil l b e note d i n fina l report
. 

### Project Lead/PA I Approval : Date : Stud yDirecto r(i fGLP) : Date : Sponso rApprova l (fo r(St P protoco l deviations) : N A fechnica i Reviewe r(optional) : N A Date : Date : N A Laborator yDepartmentJ^dafvage rApproval : Date :

IV
. Authorizatio n t o Resum e Wor k Wher e tialtin g o fwor k

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

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

yStud yDirecto ro rTea

m Leade ra

t tli e en d ofstudyo rproject ) 

### ETS-4-008. 7 Page 1„o f1 Documentatio n o

fDeviation s an d Contro l o fNonconformin g Testin & Pag e 6 1 o f 6 1