GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

GLP10-01-02 : Interi m Report 2 4 - Analysi s o fPFBS . PFHS . an d PFO S i n Groundwate r Sample s Collecte d a

t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur . AL .

Decembe r201 1 Stud yTitl e Analysi s o

fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m Data Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc . 140 0 Westo n Way Westchester , P

A1938 0 Phone : 610-701-376 1 Autho r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor

t Completio n Date Dat e o fsignin g Performin g Laboratory 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 St . Paul , M N 55144 Project Identificatio n GLP10-01-02-2 4 Tota l Numbe ro

fPage s 11 0

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

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Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements .

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### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-02 ; Interi m Repor t 2 4 - Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a

t th e Forme rSludg e Incorporatio n Are a (FSIA ) i n Decatur , AL , Decembe r201 1 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 ctest substance , n o specifi ctest syste m an d n o dosin g o

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

t th e test sit e hav

e no t bee n determine d unde rGLPs .

Gar yHohenstein , Snonso rRepresentative Date

Jaisimh a Kesan , P.E. , DEE , StudyDirecto r

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### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-02 ; Interi m Repor t 2 4 - Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a

t th e Forme rSludg e Incorporatio n Are a (FSIA ) i n Decatur , AL , Decembe r201 1 Study : Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e Sulfonate (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program . Thi s analytica l phas e wa s audite d b yth e 3 M Environmenta l Laborator yQualit yAssurance Uni t (QAU) , as indicate d i n th e followin g table . Th e finding s were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector . Inspectio n Date s Phas e Dat e Reporte d t o Inspectio n Date s Phas e Testin g Facilit y Managemen t Stud yDirecto r 1/16/2012-1/17/201 2 Data / Repor t 1/24/201 2 1/24/201 2



### QA U Representative Date

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### TABL E O F CONTENT S GL P Compliance Statemen t 3 Qualit yAssuranc e Statemen t 4 Tabl e ofContents 5 Lis t ofTable s 6 Attachment s 7 1 Stud yInformatio n 8 2 Summar

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

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

s 1 6 8. 6 La b Contro l Spike s (LCSs ) 1 6 8. 7 Analytica l Metho d Uncertaint y1 8

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8. 8 Fiel d Matri xSpike s (FMS ) 1 9 9 Data Summar

yan d Discussio n 1 9 1 0 Conclusio n 35 1 1 Data/Sampl e Retentio n 35 1 2 Signature s 3 6 

### LIS TO F TABLE S Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Results (FSI AGroundwater , December2011)... . 1 0 Tabl e 2 . Sampl e Descriptio n Ke yCod e 1 3 Tabl e 3 . Instrumen t Parameter s 1 4 Tabl e 4 . Liqui d Chromatograph yCondition s 1 4 Tabl e 5 . Mass Transition s 1 5 Tabl e 6 . Limi t ofQuantitatio n (LOQ ) 1 6 Tabl e 7 . Laborator

yContro l Spik

e Recover

y1 7 Tabl e 8 . Analytica l Uncertaint y1 8 Tabl e 9 . Fiel d Matri xSpik e Level s 1 9 Tabl e 10 . DA L GW130R11120 8 2 0 Tabl e 11 . DA L G W130 S 11120 8 2 0 Tabl e 12 . DA L G W130L11120 8 2 1 Tabl e 13 . DA L G W131 R 11121 4 2 1 Tabl e 14 . DA L G W131 S 11121 4 2 2 Table15 . DA L G W131 L 11121 4 2 2 Tabl e 16 . DA L G W133 R 11121 4 2 3 Tabl e 17 . DA L G W133 S 11121 4 2 3 Tabl e 18 . DA L G W133 L 11121 4 2 4 Tabl e 19 . DA L G W134R11120 9 2 4 Tabl e 20 . DALG W134 S 11120 9 2 5

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### Tabl e 21 . DA L G W134L11120 9 2 5 Tabl e 22 . DA L G W135 R 11121 4 2 6 Tabl e 23 . DA L G W135 S 11121 4 2 6 Tabl e 24 . DA L G W135 L 11121 4 2 7 Tabl e 25 . DA L G W136 S 11121 3 2 7 Table26 . DALG W136 L 11121 3 2 8 Tabl e 27 . DA L G W137 S 11120 9 2 8 Tabl e 28 . DA L G W137 L 11120 9 2 9 Tabl e 29 . DA L G W138 R 11121 4 2 9 Tabl e 30 . DA L G W138 S 11121 4 3 0 Tabl e 31 . DA L G W138 L 11121 4 3 0 Tabl e 32 . DA L G W140R11121 3 3 1 Tabl e 33 . DA L GW141R11121 4 3 1 Tabl e 34 . DA L G W142 R 11121 3 3 2 Tabl e 35 . DA L G W143 R 11120 9 3 2 Table36 . DALG W144 R 11121 3 33 Tabl e 37 . Tri p Blan k

1 3 3 Tabl e 38 . Rinseate Blank s 34 Tabl e 39 . Surrogate Recover y34 ATTACHMENT S Attachmen t A : Protoco l Amendmen t 2 4 3 7 Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s 4 5 Attachmen t C : Analytica l Metho d ETS-8-044. 1 8 6 Attachmen t D : Metho d Deviatio n 10 9

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### 1 Study

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

A1938 0 Phone : (610 ) 701-376 1 Fax : (610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testing Facility 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 St . Paul , M N 55144 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator , (clanqeOimmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow , Analys t Kell yUkes , Analys t Stud yDate s StudyInitiation : Marc h 8 , 201 0 Interi m 2 4 Experimenta l Termination : Januar y5,201 2 Interi m Repor

t Completion : Date o

fInteri m Repor

t Signin g Locatio n o

fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792 . Th e tes t substanc e an d analytica l referenc e standar d reserv e sample s ar e archive d at th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

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## 2 Sutnmary Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t th e Forme r Sludg e Incorporatio n Are a (FSIA) i n Decatur , AL , representin g twenty-seve n differen t samplin g locations . Atota l o

feighty-eigh t sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo r perfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e groundwate rsample s fro m eac h samplin g location . Sample s als o include d a fiel d matri xspike (FMS ) sampl e fo reac h location , a tri p blan k set containin g Miili-Q TM wate r an d appropriat e tri p blan k spikes , an d two equipmen t rinseate blanks . Th e equipmen t rinseate blank s di d no t hav e FM S sample s prepare d fo rdetemninatio n ofPFBS , PFHS , an d PFO S recovery . Th e groundwate rsamples , tri p blank s an d two equipmen t rinseate blank s associate d wit h GLP10-01 - 02-2 4 were receive d fro m Westo n personne l o n Decembe r20 , 2011 . Al l o fth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8 - 044. 1 an d conducte d unde r3 M projec t GLP-10-01-02-24 . Man yofth e groundwate rsample s require d dilutio n t o attai n PFBS , PFHS , and/o rPFO S concentration s withi n th e rang e ofth e curve , i n som e instance s u p t o 100-fol d dilutio n were required . Th e averag e measure d PFBS , PFHS , an d PFO S concentration s are summarize d i n Tabl e 1 . Th e equipmen t rinseate blank s an d th e tri p blan k

sampl e were belowth e lowe rlimi t ofquantitatio n (LLOQ ) fo rPFBS , PFHS , an d PFOS , indicatin g adequat e contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections . Th e PFB S concentratio n results fo ral l groundwate rsample s range d fro m <0.025 0 ng/m L t o 64. 4 ng/mL . Th e PFH S concentratio n results fo ral l groundwate rsample s range d fro m 0.0594 ng/m L t o 82 7 ng/mL . Th e PFO S concentratio n results fo ral l groundwate rsample s range d fro m 0.42 0 ng/m L t o 1570 ng/mL . Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S + 17% , PFH S + 18 % an d PFO S + 19% . Fo rsampl e DA L G W134L , th e metho d uncertaint ywa s expande d fo r PFOS .

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Tabl e 1 . Summarize d PFBS , PFHS , an d PFO S Result s (FSI A Groundwater , Decembe r2011) . PFB S PFH S PFO S Samplin g Locatio n Avg . Cone . (ng/mL) ±RP D Avg . Cone .

(ng/mL) ±RP D Avg . Cone .

(ng/mL) ±RP D DALG W130 R 11120 8 15. 1 ±6.6 % 11 9 ±0.84 % 46 7 ±9.9 % DALG W130 S 11120 8 3.2 7 ±1.8 % 25. 6 ±1.6 % 90. 8 ±10 % DALGW130L11120 8 1.4 9 ±2.0 % 11. 7 ±5.1 % 66. 3 ±1.4 % DA L GW131 R 11121 4 36. 6 ±0.55 % 18 2 ±2.2 % 137 0 ±1.5 % DA L GW131 S 11121 4 0.68 8 ±0.15 % 4.7 8 ±3.6 % 4.5 6 ±3.7 % DA L GW131 L 11121 4 2.8 6 ±1.1 % 18. 8 ±0.53 % 27. 9 ±0.72 % DALGW133R11121 4 2.9 4 ±15 % 20. 9 ±17 % 39. 1 ±10 % DALG W133 S 11121 4 11. 3 ±0.89 % 79. 7 ±1.4 % 17 4 ±2.9 % DA L GW133 L 11121 4 7.9 0 ±2.4 % 58. 7 ±4.1 % 25 2 ±2.8 % DALG W134 R 11120 9 47. 5 ±0.21 % 56 1 ±0.54 % 157 0 ±1.3 % DALG W134 S 11120 9 0.36 4 ±1.6 % 4.2 2 ±1.7 % 17. 5 ±0.0 % DA L GW134 L 11120 9 10. 5 ±1.9 % 10 9 ±0.0 % 43 6 ±1.6 % DALG W135 R 11121 4 64. 4 ±1.6 % 82 7 ±1.6 % 111 0 ±4.5 % DALG W135 S 11121 4 0.99 1 ±6.0 % 7.9 0 ±2.9 % 5.8 1 ±7.6 % DALGW135L11121 4 7.0 9 ±0.85 % 47. 6 ±1.5 % 33. 8 ±7.7 % DALG W136 S 11121 3 1.7 7 ±3.4 % 11. 4 ±3.5 % 59. 4 ±1.7 % DA L GW136 L 11121 3 1.9 1 ±2.6 % 12. 3 ±0.82 % 64. 4 ±3.0 % DALG W137 S 11120 9 0.12 0 ±13 % 0.113±21%<^ > 0.51 7 ±32 % DA L GW137 L 11120 9 0.086 8 ±14 % 0.099 2 ±9.8 % 1.6 2 ±8.0 % DALG W138 R 11121 4 7.4 0 ±0.95 % 35. 3 ±1.4 % 30 0 ±0.0 % DALG W138 S 11121 4 3.6 4 ±4.1 % 17. 8 ±1.7 % 16 0 ±1.3 % DALG W138 L 11121 4 <0.025 0 0.059 4 ±12 % 0.42 0 ±20 % DALG W140 R 11121 3 1.2 7 ±6.3 % 14. 1 ±2.1 % 10 2 ±3.0 % DALG W141 R 11121 4 0.034 2 ±5.3 % 0.25 4 ±4.3 % 4.8 7 ±4.1 % DALG W142 R 11121 3 1.7 7 ±7.4 % 9.9 7 ±4.6 % 94. 4 ±0.32 % DALG W143 R 11120 9 0.71 5 ±1.7 % 2.3 3 ±0.0 % 15. 6 ±6.4 % DALG W144 R 11121 3 2.0 2 ±3.0 % 7.5 4 ±0.66 % 26. 7 ±1.9% ® Tri p Blank s (Milli-Q TM Water ) <0.025 0 <0.025 0 <0.037 1 DALGW140 R R B 11121 3 <0.025 0 <0.025 0 <0.037 1 DALGW133LR B 11121 4 <0.025 0 <0.025 0 <0.037 1 Al l sample s reporte d usin g extema l standar d calibratio n unles s note d otherwise . Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S ±17% , PFH S ±18% , an d PFO S ±19% . (1 ) Th e analytica l uncertaint yha s bee n adjuste d fo rPFO S base d o n FM S recover yfo rDA L G W134 L t o ±39% . (2 ) Th e RP D di d no

t meet metho d acceptance criteri a of<20% . (3 ) Sampl e results reporte d usin g intema l standar d calibration . (4 ) Samplin g locatio n di d no t have a n appropriat e FM S spike leve l t o sufficientl yevaluate PFO S recovery .

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### 3 Introduction Thi s analytica l stud ywa s conducte d a s par t o fth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit

ylocate d i n Decatur , Alabama . Th e objective ofth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility . Thi s analytica l stud ywa s conducte d t o analyz e groundwate rsample s collecte d fro m variou s well s locate d a t th e Forme rSludg e Incorporatio n Are a (FSIA

) i n Decatur , A L fo rPFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on sit e groundwate rconditions . Th e 3 M Environmenta l Laborator yprepare d sampl e container s (25 0 m L high-densit

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

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

s designate d fo rfiel d matri xsample s 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 fiel d fo rsampl e collection . Se e sectio n 8. 8 o fth e repor

t fo rfiel d matri xspike levels . Sampl e bottle s fo rselec t samplin g location s were fortifie d wit h interna l standar d an d surrogat e prio rt o sampl e collectio n t o ai d i n sampl e analysis . Where applicable , interna l standard s were use d t o ai d i n th e data qualit y objectives . Samplin g location s reporte d fo rPFO S usin g interna l standar d calibrato n included : DA L G W 137S , DA L G W137L , DA L G W138L , DA L G W141R , an d DA L G W144R . 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. 1 "Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s I n Wate rb yHig h Perfomrianc

e Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis" . Tabl e 1 summarize s th e averag e PFBS , PFHS , an d PFO S concentration s fo rth e duplicat e sample s collected , th e tri p blank , an d th e aqueou s equipmen t rinseate blan k samples . Table s 10-3 8 summariz e th e individua l sampl e results an d th e associate d fiel d matri xspike recoveries . Surrogate recoverie s fo r sample s quantitate d usin g interna l standar d calibratio n are summarize d i n Tabl e 39 . Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s are reporte d an d discusse d elsewher e i n thi s report . 

### 4 Test & Control Substances There wa s no

t 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 was purel yanalytica l i n nature .

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### 5 Reference

Substances

Referenc e Substanc e PFB S (predominantl y linea r isomer ) PFH S (linea risomer ) PFO S (branche d an d linea r isomers ) Chemica l Nam e Perfluorobutan e sulfonat e Perfluorohexan e sulfonat e Perfluorooctan e sulfonat e Chemica l Formul a C4F9SO3K ' CeFisSO/Na ^ CsFiySO s K * Identifie r Potassiu m Sal t Sodiu m Sal t Potassiu m Sal t CAS#br-PFOS K Us e Targe t Analyt e Referenc e Standar d Targe t Analyt e Referenc e Standar d Targe t Analyt e Referenc e Standar d Sourc e 3 M Wellingto n Wellingto n Expiratio n Dat e 1/10/201 7 3/25/201 8 3/17/201 4 Storag e Condition s Froze n Froze n Froze n Chemica l Lo t Numbe r 10 1 LPFHxSAMO S brPFOSK070 8 TC P Numbe r TCR-12 1 TCR08-001 8 TCR11-001 0 Physica l Descriptio n Whit e Powde r Crystallin e Liqui d Purit y 96.7 % 100 % NA(^ '
Referenc e Substanc e PFO S (branclie d an d linea r isomers ) "C4-PFO S Surrogat e "Cj-PFO S Chemica l Nam e Perfluorooctan e sulfonat e Perfluorooctan e sulfonat e Sodiu m Perfluorooctanesulfonat e Chemica l Formul a CsF-iySO s K* CsFiySOa-Na * "CsFiySOaNa ' Identifie r Potassiu m Sal t CA S #2795-39- 3 Sodiu m Sal t CAS#MPFC-C-051 1 Us e FM S Referenc e Standar d Sun^ogat e Recover y Standar d Intema l Standar d Sourc e Aldric h Wellingto n Wellingto n Expiratio n Dat e 2/4/201 4 9/8/201 3 05/25/201 4 Storag e Condition s Roo m Temperatur e Froze n Froze n Chemica l Lo t Numbe r 1424328 V MPFOS091 0 05241 1 TC R Numbe r TCR11-002 8 TCR10-004 4 TCR11-001 6 Physica l Descriptio n Whit e Powde r Liqui d Liqui d Purit y 99.7 % NA<^ > NA<^ ' (1 ) Reference standar

d a t a concentratio n of5 0 ±2. 5 |jg/m L (2 ) Custo m mixtur

e o fseve n mass-labele d ("C ) perfluoroall<ylcaitioxyli cadds , two mass labele d ("C ) pertiuoroall<ylsulfonates an d on e mass-labele d ('^C ) perfluoro-1-octanesulfonamid e a t a nomina l concentratio n of5 pg/m L

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### 6 Test System Th e test system s fo rthi s stud yare groundwate rsample s collecte d fro m well s locate d i n Decatur , A L b y Westo n Solutions , Inc . personnel . Sample s fo rthi s stud yare "rea l world " samples , no t dose d wit h a specifi clo t oftest substance . Tabl e 2 . Sampl e Descriptio n KeyCode . Strin g Numbe r Strin g Descripto r Exampl e Example DALGW131R 0111214 1 Sampling Location DAL= Decatur, Alabama 2 Well ID GW= Groundwater 3 Sampling Point Example: 131 4 Well Level R = Residuum

shallow water-bearing

zone L= Bedrock water-bearing

zone S = Epikarst middle water-bearing

zone 5 Sampling Date 111214-December 14,2011 6 Sample Type 0=primary sample DB=duplicate

sample FMS = Field Matrix Spike 

### 7 Method

Summary 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 1 "Metho d o

fAnalysi s fo rth e Detemninatio n ofPerfluorinate d Compound s I n Wate rb yHig h Perfomnanc

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

### 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene^' ^ (high-densit

ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory . Sampl e bottle s associate d wit h GLP10-01-02-2 4 were returne d t o th e laborator ya t ambien t condition s o n Decembe r20 , 2011 . Sample s were store d refrigerate d a t th e laborator yafte rreceipt . Aset o

flaborator

yprepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspike s were sen t wit h th e sampl e collectio n bottles . 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis . Sample s that require d dilutio n were prepare d b ydilution s Im L sampl e wit h 9 mLs o fMilli- Q wate r (dilutio n 1:10) . Sample s that require d dilutio n were prepare d b ydilutin g 1m L o

fsampl e wit h 9 mLs o

f Mill i Q wate r(dilutio n 1:10) . Sample s requirin g a 1:10 0 dilutio n were prepare d b ydilutin g 0. 1 m L of sampl e wit h 9. 9 mLs o

fMilli Q wate r Samplin g location s reporte d fo rPFO S usin g interna l standar d calibraton : Durin g th e preparatio n ofth e laborator ycontro l samples , a n aliquot o fa separat e interna l standar d spikin g solutio n wa s adde d t o th e laborator ycontro l sample s (nomina l concentratio n of1 ng/mL) . Th e sample s bottle s were spike d wit h a n interna l standar

d mi xa t a nomina l concentratio n of1 ng/m L prio rt o bein g sen t t o th e fiel d fo rsampl e collection . Pag e 1 3 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 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 mas s spectrometr y(HPLC/MS/MS) . Detaile d instrnmen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmas s transition s analyze d are describe d i n th e ra

wdat a har

d copie s place d i n th e fina l dat a packet , an d are briefl ydescribe d below . Tabl e 3 . Instrumen t Parameters . Instrumen t Nam e ETSKir k ETS Buste r Analytica l Metho d Followe d ETS-8-044. 1 ETS-8-044. 1 Analysi s Dat e 12/27/1 1 - PFBS , PFHS , an d PFO S Extema l standar

d calibratio n 1/4/1 2 - PFO S Intema l standar

d calibratio n Liqui d Chromatograp h Agilen t 129 0 Agilen t 110 0 Guard colum n Betasi l C1 8 (4. 6 m m X 100 mm) , 5 n Pris m R P (2. 1 m m X 5 0 mm) , 5 n Analytica l colum n Betasi l 01 8 (4. 6 m m X 100 mm) , 5 n Betasi l 01 8 (2. 1 m m X 100 mm) , 5 n Injectio n Volum e 1 0 n L 1 0 u L Mas s Spectromete r Applie d Biosystem s fiP\ 550 0 Applie d Biosystem s /\P i 400 0 Io n Sourc e Turb o Spra y Turb o Spra y Electrod e Turb o io n electrod e Turb o io n electrod e Polarit y Negativ e Negativ e Softwar e Analyst 1.5. 2 Analyst 1.4. 2 Tabl e 4 . Liqui d Chromatograph yConditions . ste p Total

Time Flow

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

acetate) (MethanoO ETS-8-044. 1 Analyze d 12/27/1 1 0 0 75 0 97. 0 3. 0 1 2. 0 75 0 97. 0 3. 0 2 14. 5 75 0 5. 0 95. 0 3 15. 5 75 0 5. 0 95. 0 4 16. 5 75 0 97. 0 3. 0 5 20. 0 75 0 97. 0 3. 0 ETS-8-044. 1 Analyze d 1/4/1 2 0 0 30 0 97. 0 3. 0 1 2. 0 30 0 97. 0 3. 0 2 14. 5 30 0 5. 0 95. 0 3 15. 5 30 0 5. 0 95. 0 4 16. 5 300 97. 0 3. 0 5 20. 0 30 0 97. 0 3. 0

Pag e 1 4 o f11 0Tabl e 5 . Mas s Transitions . GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Artalyte Mass Transition Q1/Q3 Reference

Material structure Intemal

standard Mass

Transition Q1/Q3 PFBS 299/80 Linear NA NA 299/99 PFHS 399/80 Linear NA NA 399/99 PFOS 499/80 Branctiedand Linear t^C^PFOS'^' 507/80 PFOS 499/99 Branctiedand Linear t^C^PFOS'^' 507/80 PFOS 499/130 Branctiedand Linear t^C^PFOS'^' 507/80 ["CJPFOS

- surrogate 503/80 Linear t^CalPFOS'^^ 507/80 Dwel l tim e wa s 2 0 o r5 0 mse cfo reac h transition . Th e individua l transition s were summe d t o produce a "tota l io n chromatogram " (TIC) , whic h was use d fo rquantitation . (1 ) Intema l standar

d an d surrogat e wer

e onl yuse d fo rPFO S fo rsamplin g location s DA L G W137S , DA L G W137L , DA L G W138L , DA L G W141R , an d DA L G W144R . 

### 8 Analytical

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

yspikin g know n amounts o fth e stoc k

solutio n containin g th e targe t analyte s into prepare d i n Mill i Q water . Atota l offiftee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) were analyzed . Aquadratic , 1/ xweighted , calibratio n curve ofth e pea k are a counts wa s use d t o fi t th e data fo reac h analyte . Th e dat a were no t force d throug h zero durin g th e fittin g process . Calculatin g th e standar d concentration s usin g th e pea k are a confimned accurac

yofeac h curve point . Fo rsamplin g location s DA L G W137S , DA L G W137L , DA L G W138L , DA L G W141R , an d DA L G W 144 R fo rPFOS : Sample s were analyze d usin g a stabl e isotop e intema l standar d calibratio n curve . Calibratio n standard s were prepare d b yspikin g know n amounts o fth e stoc k

solutio n containin g th e targe t analyte s into a laboratory-prepare d syntheti cgroundwate rcontainin g calciu m an d magnesium . A separat e interna 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 of1 ng/mL . A calibratio n curve rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) was analyze d (0.02 5 ng/m L t o 1 0 ng/m L fo r["CJPFO S surrogate) . Aquadratic , 1/ xweighted , calibratio n curve ofth e pea k are a ratio s wa s use d t o fi t th e dat a fo reac h analyte . Th e data were no t force d throug h zero durin g th e fittin g process . Calculatin g th e standar d concentration s usin g th e pea k are a ratio s an d th e resultan t calibratio n curve confimned accurac

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

yrequirements o

f100±25 % (100±30 % fo rth e lowest curve point) were met fo ral l analytes . Th e con-elatio n coefficien t (r ) wa s greate rtha n 0.995 fo ral l analytes . 

### 8. 2 Syste m Suitability Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofeac h analytica l sequence t o demonstrat e overal l syste m suitability . Th e acceptance criteri a ofles s tha n o requa l t o 5% relative standar d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a ofles s tha n o requa l t o 2 % RS D was met fo rPFBS , PFHS , PFOS , an d f^C4]PF0 S surrogate .

Pag e 1 5 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1


### 8. 3 Limi t o

fQuantitatio n (LOQ ) Th e LOQ fo rthi s analysi s i s th e lowes t non-zer o calibratio n standar

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

yrequirements an d fo rwhic h th e are a counts o rare a rati o are a t leas t twic e thos e ofth e appropriat e blanks . Th e 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) . Ana/ys/s Dat e Dilution PFBS LOQ, ng/mL PFHS

LOQ, ng/mL PFOS

LOQ, ng/mL 12/27/1 1 Analysis extema l standar

d calibratio n 1 0.025 0 0.025 0 0.037 1 12/27/1 1 Analysis - extema l standar

d calibratio n 1 0 0.25 0 0.25 0 0.37 1 12/27/1 1 Analysis extema l standar

d calibratio n 100 2.5 0 2.5 0 3.7 1 1/4/1 2 Analysis intema l standar

d calibratio n 1 NA NA 0.092 8 N A= No t Applicabl e 

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

feac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confin n that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control . Al l CCV s met metho d criteri a o

f100 % ±25 % fo rPFBS , PFHS , PFOS , an d ["CJPFO S surrogate . 

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

s were prepare d an d analyze d wit h th e samples : solven t blanks , tri p blanks , an d equipmen t rinseate blanks . Solven t blan k results were reviewe d an d use d t o evaluat e metho d performance t o determin e th e LOQ fo rPFBS , PFHS , PFOS , an d ["CJPFO S surrogate . Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience . Equipmen t rinseate blank s ar e aqueou s sample s that reflec t th e efficienc

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

### 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set . LCS s were prepare d b yspikin g know n amounts ofth e analyt e into Mill i Q wate ro r syntheti cgroundwate rt o produce th e desire d concentration . Th e spike d wate rsample s were the n prepare d an d analyze d i n th e sam e manne ra s th e samples . Th e metho d acceptance criteria , 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% , were met fo rPFBS , PFHS , PFOS , an d [^^C4]PF0 S surrogat e LC S samples . Th e followin g calculation s were use d t o generat e dat a i n Tabl e 7 fo rlaborator ycontro l spikes . LC S Percen t Recover

y Calculate d Concentratio n Spike Concentratio n *100 % LCS % RS D = ^^P"''^*^ ^ ' 100 % averag e LC S recover

y

Pag e 1 6 o f11 0Tabl e 7 . LaboratoryContro l Spike Recovery . GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

ETS-8-044. 1 Analyze d 12/27/1 1 Extema l standar

d calibratio n PFS S PFHS Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) YoRecovery Spiked Concentration (ng/mL) Calculated

Concentration (ng/mL) YoRecovery LCS-111221 ^ 0.49 8 0.59 8 12 0 0.49 7 0.50 6 10 2 LCS-111221- 5 0.49 8 0.58 3 11 7 0.49 7 0.49 6 99. 9 LCS-111221- 6 0.49 8 0.58 4 11 7 0.49 7 0.48 8 98. 2 Averag e ±%RS D 11 8 ±1.5 % 100 % ±1.9 % LCS-111221- 7 49 8 5.7 8 11 6 4.9 7 5.0 3 10 1 LCS-111221- 6 49 8 5.7 0 11 5 4.9 7 4.9 8 10 0 LCS-111221- 9 49 8 5.6 8 11 4 4.9 7 5.0 7 10 2 Averag e ±%RS D 115 % ±0.87 % 101 % ±0.99 % LCS-111221-1 0 29. 9 26. 3 87. 9 29. 9 24. 4 81. 5 LCS-111221-1 1 29. 9 30. 2 10 1 29. 9 28. 9 96. 5 LCS-111221-1 2 29. 9 28. 0 93. 8 29. 9 29. 4 98. 3 Averag e ±%RS D 94.2 % ±7.0 % 92.1 % ±10 % ETS-8-044. 1 Analyze d 12/27/1 1 Extema l standar

d calibratio n PFOS ( 'Branched and Linear) Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) YoRecovery LCS-111221- 4 LCS-111221- 5 LCS-111221- 6 0.46 2 0.46 2 0.46 2 0.39 5

0.38 3 0.37 7 85. 6

82. 9 81. 7 Averag e ±%RS D 83.4 % ±2.4 % LCS-111221- 7 LCS-111221- 8 LCS-111221- 9 4.6 2 4.6 2 4.6 2 5.1 8

5.1 1 5.0 6 11 2

11 1 10 9 Averag e ±%RS D 111 % ±1.4 % LCS-111221-1 0 LCS-111221-1 1 LCS-111221-1 2 27. 8 27. 8 27. 8 23. 2

26. 4 26. 1 83. 5

94. 8 93. 8 Averag e ±%RS D 90.7 % ±6.9 %

Pag e 1 7 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Tabl e 7 continued . LaboratoryContro l Spike Recovery . ETS-8-044. 1 Analyze d 1/4/1 2 Intema l standar d calibration PFOS (Branched

and Linear) ["C^PFOS sunogat

e Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) YoRecovery Spiked Concentration (ng/mL) Calculated

Concentration (ng/mL) YoRecovery LCS-120104- 1 0.184 0.21 4 11 6 0,18 9 0,20 1 106 LCS-120104- 2 0,184 0.19 9 108 0.18 9 0,20 9 11 1 LCS-120104- 3 0.184 0.20 9 11 3 0.18 9 0,21 2 11 2 Averag e ±%RS D 11 2 ±3.6 % 110 % ±2.9 % LCS-120104- 4 1,8 4 2.1 4 11 6 1,8 9 2,1 3 11 3 LCS-120104- 5 1.8 4 2.0 5 11 1 1,8 9 2,0 5 109 LCS-120104- 6 1,8 4 2.0 8 11 3 1,8 9 2,1 1 11 2 Averag e ±%RS D 113 % ±2.2 % 111 % ±1.9 % LCS-120104- 7 18. 4 16. 5 89. 6 LCS-120104- 8 18. 4 17. 3 93. 8 LCS-120104- 9 18. 4 17. 2 93. 6 Averag e ±%RS D 92.3 % ±2.6 % 8. 7 Analytica l Metho d Uncertaint y Analytica l uncertaint

yi s base d o n historica l QC dat a that i s contro l charte d an d use d t o evaluate metho d accurac

yan d precision . Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2 . Th e standar d deviatio n i s calculate d fo rth e set o faccurac yresults (i n % ) obtaine d fo rth e QC samples . Th e metho d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h con-espond s t o a confidence leve l o f95% . Th e most recen t 50 dat a points were use d t o generate th e metho d uncertaint

yvalue s liste d i n Tabl e 8 . Tabl e 8 . Analytica l Uncertainty . Analyte Standard Deviatio n Metho d Uncertaint

y PFB S 8.5 1 ±17 % PFH S 8.9 8 ±18 % PFO S 9.2 9 ±19 %

Pag e 1 8 o f11 0GLP10-01-02 ; interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

8. 8 Fiel d Matri xSpike s (FMS ) Afiel d matri xspik

e (FMS ) wa s collecte d a

t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix . Fiel d matri xspike s were generate d b yaddin g a measure d volum e o f fiel d sampl e t o a containe rspike d b yth e laborator

ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear+branched ) prio rt o shippin g sampl e container s fo rsampl e collection . Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a o f 100±30 % confin n that "unknown " components i n th e sampl e matri xd o no

t significantl yinterfere wit h th e extractio n an d analysi s o fth e analyte s o

f interest . Fiel d matri xspike concentration s mus t be 50 % o

fth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike . Fiel d matri xspike s ar e presente d i n sectio n 9 o fthi s report . Tabl e 9 . Fiel d Matri xSpike Levels . Samplin g Locatio n Spik e Leve l PFBS , ng/m L PFHS , ng/m L PFOS , ng/m L 136R , 137R , 137S , 137L , 138L , 141 R FM S 1.0 1 0,99 8 0.99 8 131S , 134S , 135 S 143 R FM S 20, 2 20. 0 20, 0 130L , 142R , 144 R FM S 50. 5 49. 9 49. 9 130S , 131 U 133R , 1368 , 136L , 140 R FM S 10 1 99. 8 99. 8 133S , 133L , 135L , 138R , 138 S FM S 20 2 20 0 20 0 130R , 134L , CW26C , CW26 L FM S 50 3 49 9 49 9 131R , 134R , 135 R FM S 201 0 200 0 200 0 Tri p Blan k Lo w 1.0 1 0.99 8 0,99 8 Tri p Blan k Mi d 20, 2 20, 0 20. 0 Tri p Blan k Mid-Hig h 10 1 99, 8 99, 8 Tri p Blan k Hig h 50 3 49 9 49 9

(Sampl e Concentratio

no f FMS-Average Concentratio n: Fiel dSampl e & Fiel dSampl e Dup. ) ^ FM S Recover y = —* 100 % Spik e Concentrato

n 

### 9 Mats Summary

adS Discussion Th e table s belowsummariz e th e sampl e results an d fiel d matri xspik e recoverie s fo rth e samplin g location s as wel l a s th e Tri p Blank s an d rinseate blanks . Results an d averag e value s ar e rounde d t o thre e significan t figure s accordin g t o EP Aroundin g rules . Becaus e o f rounding , 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 metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G W134 L - Th e recover yo fth e FM S sampl e fo rPFO S wa s 61.2% . Base d o n th e recover yo fth e FM S sample , th e analytica l uncertaint yhas bee n expande d fo rPFO S to ±39% . DA L G W137 S - Th e sample/sampl e duplicate RP D wa s 2 1 % fo rPFH S an d 32 % fo rPFOS . DA L G W141 R - Samplin g locatio n di d no t hav e a n appropriat e FM S spik e leve l fo rPFO S t o accuratel yasses s recovery .

Pag e 1 9 o f 11 0Tabl e 10 . DA L G W130 R 111208 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFe s PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-00 1 DAL-GW-130R-O-111208 14. 6 NA 11 8 NA 44 4 N A GLP10-01-02-24-002 DAL-GW-130R-DB-11120 8 15. 6 NA 11 9 NA 49 0 N A GLP10-01-02-24-00 3 DAL-GW-130R-FMS-11120 8 48 2 92. 8 55 1 86. 7 87 8 82. 4 Average Concentration

(ng/mL) ± YoRPD 15.1 ng/mL ±6.6Yo 119 ng/mL±0.84Yo 467 ng/mL±9.9Yo NA= No t Applicabl e Sample s dilute d 1:10 0 an d reporte

d fi-o m extemal standar

d calibration . Tabl e 11 . DA L G W1 SO S 111208 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-004 DAL-GW-130S-0-11120 8 3.24 N A 25. 8 NA 86. 1 NA GLP10-01-02-24-00 5 DAL-GW-130S-DB-11120 8 3.30 N A 25. 4 NA 95. 4 NA GLP10-01-02-24-00 6 DAL-GW-130S-FMS-11120 8 97. 7 93. 5 11 0 84. 6 186 95. 4 Average Concentration

(ng/mL) ± YoRPD 3.2 7 ng/m L ±18 % 25.6 ng/mL±1.6Yo 90.8 ng/mLtlOYo NA= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration .

Pag e 2 0 o f11 0Tabl e 12 . DA L G W1 SO L 111208 GLP10-01-02 ; Interi m Repor t 2 4 /^alysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFS S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) %Recovery (ng/mL) YoRecovery GLP10-01-02-24-00 7 DAL-GW-130L-0-11120 8 1.5 0 N

A 11. 4 N A 65. 8 NA GLP10-01-02-24-00 8 DAL-GW-130L-DB-11120 8 1.4 7 N

A 12. 0 N A 66. 7 NA GLP10-01-02-24-00 9 DAL-GW-130L-FMS-11120 8 52. 1 100 54. 7 86. 2 11 0 87. 7 Average Concentration

(ng/mL) ± YoRPD 1.49 ng/mL±2.0Yo 11.7 ng/mL±5.1Yo 66.3 ng/mL±1.4Yo N A= No t /Applicabl e Samples dilute

d 1:1 0 and reporte

d fro m extemal standar

d calibration . Tabl e 13 . DA L G W131 R 11121 4 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-01 0 DAL-GW-131R-0-11121 4 36. 5 N A 18

4 NA 136 0 NA GLP10-01-02-24-01 1 DAL-GW-131R-DB-11121 4 36. 7 N A 180 N A 138 0 NA GLP10-01-02-24-01 2 DAL-GW-131R-FMS-11121 4 202 0 98. 7 1970 89. 4 298 0 80. 5 Average Concentration (ng/mL) ± %RPD 36. 6 ng/m L ±0.55% 182 ng/mL±2.2Yo 1370 ng/mL±1.5Yo N A= No t /Applicabl e Sample s dilute d 1:100 an d reporte d fro m extema l standar d calibration .

Pag e 2 1 o f11 0Tabl e 14 . DA L G W1S1 S 11121 4 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-01 3 DAL-GW-131S-0-11121 4 0.68 8 N A 4.8 6 N A 4.6 4 N A GLP10-01-02-24-01 4 DAL-GW-131S-DB-11121 4 0.68 7 N A 4.6 9 NA 4.4 7 NA GLP10-01-02-24-01 5 DAL-GW-131S-FMS-11121 4 18. 3 87. 2 21. 9 85. 6 20. 2 78. 2 Average Concentration

(ng/mL) ± YoRPD 0.688

ng/mL± 0.15Yo 4.78 ng//nL ±3.6 % 4.56

ng/mL±3.7Yo NA= No t Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m extema l standar

d calibration . Tabl e 15 . DA L G W1S1 L 11121 4 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-01 6 DAL-GW-131L-0-11121 4 2.8 4 N A 18. 8 N A 28. 0 N A GLP10-01-02-24-01 7 DAL-GW-131L-DB-11121 4 2.8 7 N A 18. 7 N A 27. 8 N A GLP10-01-02-24-01 8 DAL-GW-131L-FMS-11121 4 95. 7 91. 9 11 2 93. 4 10 3 75. 3 Average Concentration

(ng/mL) ± YoRPD 2.86

ng/mL±1.1Yo 18.8 ng/mL±0.53% 27. 9 ng/m L ±0.72 % NA= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration .

Pag e 2 2 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Tabl e 16 . DA L G W133 R 11121 4 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-01 9 DAL-GW-133R-0-11121 4 3.1 6 N A 22. 7 N A 41. 1 N A GLP10-01-02-24-02 0 DAL-GW-133R-DB-11121 4 2.7 1 N A 19. 1 N A 37. 1 N A GLP10-01-02-24-02 1 DAL-GW-133R-FMS-11121 4 95. 9 92. 0 11 2 91. 3 12 1 82. 1 Average Concentration

(ng/mL) ± YoRPD 2.9

4 ng/m L ±75 % 20.9 ng/mL±17Yo 39.1 ng/mL±10% NA= No t /Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m extema l standar

d calibration . Tabl e 17 . DA L G W133 S 11121 4 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-02 2 DAL-GW-133S-0-11121 4 11. 3 N A 80. 2 N A 17 6 NA GLP10-01-02-24-02 3 DAL-GW-133S-DB-11121 4 11. 2 N A 79. 1 N A 17 1 NA GLP10-01-02-24-02 4 DAL-GW-133S-FMS-11121 4 20 4 95. 4 27 8 99. 2 31 9 72. 8 Average Concentration

(ng/mL) ± YoRPD 11.3

ng/mL ±0.89Yo 79.7ng»nL±14 % f7 4 ng/m L ±2.9 % N A= No t /Applicabl e Sample s dilute d 1:1 0 an d reporte d fi-o m extema l standar d calibration .

Pag e 2 3 o f11 0Tabl e 18 . DA L G W1S3 L 11121 4 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-02 5 DAL-GW-133L-0-11121 4 7.8 0 N A 59. 9 NA 24 8 NA GLP10-01-02-24-02 6 DAL-GW-133L-DB-11121 4 7.9 9 N A 57. 5 N A 25 5 NA GLP10-01-02-24-02 7 DAL-GW-133L-FMS-11121 4 198 94. 1 24 1 91. 2 41 1 79. 8 Average Concentration

(ng/mL) ± YoRPD 7.9

0 ng/m L ±2.4 % 58.7ng/mL±4.f % 25 2 ng/m L ±2.8 % N A= No t /Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m extemal standar

d calibration . Tabl e 19 . DA L G W134 R 111209 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-02 8 DAL-GW-134R-0-11120 9 47. 4 N A 55 9 NA 158 0 N A GLP10-01-02-24-02 9 DAL-GW-134R-DB-11120 9 47. 5 N A 562 NA 156 0 NA GLP10-01-02-24-03 0 DAL-GW-134R-FMS-11120 9 1870 90. 7 236 0 90. 0 308 0 75. 5 Average Concentration

(ng/mL) ± YoRPD 47.5

ng/mL±0.21Yo 561 ng/mL ±0.54Yo 1570 ng/mL±1.3Yo N A= No t Applicabl e Samples dilute d 1:10

0 an d reporte d fro m extema l standar d calibration .

Pag e 2 4 o f11 0Tabl e 20 . DALG W1S4 S 111209 GLP10-01-02 ; Interi m Repor t 2 4 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concerrtration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-03 1 DAL-GW-134S-0-11120 9 0.36 1 N A 4.1 8 N A 17. 5 N A GLP10-01-02-24-032 DAL-GW-134S-DB-11120 9 0.36 7 N A 4.2 5 N A 17. 5 NA GLP10-01-02-24-03 3 DAL-GW-134S-FMS-11120 9 18. 5 89. 8 22. 2 89. 9 34. 5 85. 0 Average Concentration

(ng/mL) ± YoRPD 0.36

4 ng/m L ±7.6 % 4.22ng'mL±7.7 % 77. 5 ng/m L ±0.0 % NA= No t /Applicabl e Sample s undilute d and reporte

d fro m extemal standar

d calibration . Tabl e 21 . DA L G W134 L 111209 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-034 DAL-GW-134L-0-11120 9 10. 4 N A 109 N A 43 2 NA GLP10-01-02-24-035 DAL-GW-134L-DB-11120 9 10. 6 N A 109 N A 43 9 NA GLP10-01-02-24-03 6 DAL-GW-134L-FMS-11120 9 41 9 81. 2 54 6 87. 6 74 1 61.2 TM Average Concentration

(ng/mL) ± YoRPD 70. 5 ng/m L ±7.9 % 70 9 ng/m L ±0.0 % 43 6 ng/m L ±7.6%' ^ N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level . Samples dilute d 1:10

0 an d reporte d fi-o m extema l standar d calibration . (1 ) FM S di d no

t mee t acceptance criteri a o f100 ±30% . (2 ) Sampl e method uncertaint yi s expande d t o ±39% .

Pag e 2 5 o f11 0Tabl e 22 . DA L G W135 R 11121 4 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-03 7 DAL-GW-135R-0-11121 4 63. 9 N A 82 0 N A 113 0 NA GLP10-01-02-24-03 8 DAL-GW-135R-DB-11121 4 64. 9 N A 83 3 N A 108 0 NA GLP10-01-02-24-03 9 DAL-GW-135R-FMS-11121 4 182 0 87. 3 274 0 95. 7 258 0 73. 8 Average Concentration

(ng/mL) ± %RPD 64. 4 ng/m L ±7.6 % 82 7 ng/m L ±7.6 % 777 0 ng'm L ±4.5 % N A= No t /Applicabl e Sample s dilute d 1:10 0 and reporte

d fro m extemal standar

d calibration . Tabl e 23 . DA L G W135 S 11121 4 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-04 0 DAL-GW-135S-0-11121 4 0.96 1 N A 7.7 8 N A 5.5 9 NA GLP10-01-02-24-04 1 DAL-GW-135S-DB-11121 4 1.0 2 N

A 8.0 1 N A 6.0 3 NA GLP10-01-02-24-042 DAL-GW-135S-FMS-11121 4 19. 1 89. 7 26. 9 95. 0 22. 8 85. 0 Average Concentration (ng/mL) ± YoRPD 0.99

7 ng/m L ±6.0

% 7.9

0 ng/m L ±2.9 % 5.8 7 ng/m L ±7.6

% N A= Not/Applicabl e Samples undilute d an d reporte d fi-o m extema l standar d calibration .

Pag e 2 6 o f11 0Tabl e 24 . DA L G W135 L 11121 4 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-04 3 DAL-GW-135L-0-11121 4 7.0 6 N A 47. 2 N A 32. 5 N A GLP10-01-02-24-044 DAL-GW-135L-DB-11121 4 7.1 2 N A 47. 9 N A 35. 1 N A GLP10-01-02-24-045 DAL-GW-135L-FMS-11121 4 20 0 95. 5 23 2 92. 2 183 74. 6 Average Concentration

(ng/mL) ± YoRPD 7.09

ng/mL±0.85Yo 47. 6 ng/m L ±7.5 % 33. 8 ng/m L ±7.7 % N A= No t /Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m extema l standar

d calibration . Tabl e 25 . DA L G W136 S 11121 3 PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) %Recovery GLP10-01-02-24-04 9 DAL-GW-136S-0-11121 3 1.8 0 N

A 11. 6 N A 59. 9 NA GLP10-01-02-24-05 0 DAL-GW-136S-DB-11121 3 1.7 4 N

A 11. 2 N A 58. 9 NA GLP10-01-02-24-05 1 DAL-GW-136S-FMS-11121 3 106 103 104 92. 8 145 85. 8 Average Concentration

(ng/mL) ± YoRPD 7.7

7 ng/m L ±3.4 % 77.4 ng/m L ±3.5 % 59. 4 ng/m L ±7.7 % NA= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration .

Pag e 2 7 o f11 0Tabl e 26 . DA L G W136 L 11121 3 GLP10-01-02 ; Interi m Repor t 2 4 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-05 2 DAL-GW-136L-0-11121 3 1.8 8 N

A 12. 3 N A 65. 3 N A GLP10-01-02-24-05 3 DAL-GW-136L-DB-11121 3 1.9 3 N

A 12. 2 N A 63. 4 N A GLP10-01-02-24-05 4 DAL-GW-136L-FMS-11121 3 104 10 1 106 93. 9 153 88. 8 Average Concentration

(ng/mL) ± YoRPD 7.97 ng/mL± 2.6% 72. 3 ng/m L ±0.82 % 64. 4 ng'mL ±3.0 % NA = Not/Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m extemal standar

d calibration . Tabl e 27 . DA L G W137 S 111209 PFB S PFH S PFO S Concerrtration Concerrtration Concerrtration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) YoRecovery GLP10-01-02-24-05 8 DAL-GW-137S-0-11120 9 0.12 7 N A 0.12 5 N A 0.60 1 , NA GLP10-01-02-24-05 9 DAL-GW-137S-DB-11120 9 0.11 2 N A 0.10 1 N A 0.433 NA GLP10-01-02-24-06 0 DAL-GW-137S-FMS-11120 9 1.0 9 96. 1 0.94 9 83. 8 1.3 2 80. 5 Average Concentration

(ng/mL) ± YoRPD 0.72 0 ng'mL ±73% 0.77 3 ng/m L ±27% TM 0.577 ng/m L ±32%'^' ^ NA = No t Applicabl e Reporte d result

s fo rPFB S an d PFH S ar

e fro m extema l standar

d calibration . Reporte d results fo rPFO S ar e fro m intema l standar

d calibration . (1 ) RP D di d no

t meet acceptance criteri a o fS20% .

Pag e 2 8 o f11 0Tabl e 28 . DA L G W137 L 111209 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concentration Concentration Concerrtration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-06 1 DAL-GW-137L-0-11120 9 0.092 8 N A 0.104 N A 1.6

8 N

A GLP10-01-02-24-062 DAL-GW-137L-DB-11120 9 0.080 7 N A 0.094 3 N A 1.5

5 N

A GLP10-01-02-24-06 3 DAL-GW-137L-FMS-11120 9 1.1 1 10 1 1.0 0 90. 3 2.5 9 97. 7 Average Concentration

(ng/mL) ± YoRPD 0.0868 ng/m L ±74 % 0.0992 ng/mL ±9.8 % 7.6

2 ng/m L ±8.0 % N A= Not /Applicabl e Reporte d result s fo rPFB S and PFH S ar

e fro m extemal standar

d calibration . Reporte

d result s fo rPFO S ar

e fro m intemal standar

d calibration . Tabl e 29 . DA L G W138 R 11121 4 PFB S PFH S PFO S Concerrtration Concentration Concerrtration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-064 DAL-GW-138R-0-11121 4 7.36 N A 35. 0 N A 30 0 N A GLP10-01-02-24-06 5 DAL-GW-138R-DB-11121 4 7.43 N A 35. 5 N A 30 0 N A GLP10-01-02-24-06 6 DAL-GW-138R-FMS-11121 4 20 2 96. 3 22 0 92. 4 45 1 75. 5 A\^erage Concentration (ng/mL) ± YoRPD 7.4

0 n»'mL ±0.95

% 35. 3 ng/m L ±7.4 % 300 ng/mL±0.0% N A= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration .

Pag e 2 9 o f11 0Tabl e 30 . DA L G W138 S 11121 4 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concerrtration Concentration Concerrtration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) YoRecovery (ng/mL) %Recovery GLP10-01-02-24-06 7 DAL-GW-138S-0-11121 4 3.7 1 N A 17. 9 N A 15 9 N A GLP10-01-02-24-06 8 DAL-GW-138S-DB-11121 4 3.5 6 N A 17. 6 N A 16 1 N A GLP10-01-02-24-06 9 DAL-GW-138S-FMS-11121 4 19 1 92. 8 20 3 92. 6 29 9 69. 5 Average Concentration

(ng/mL) ± YoRPD 3.6

4 ng/m L ±4.7 % 77.8ng/mL ±7.7 % 76

0 ng/m L ±7.3 % N A= No t /Applicabl e Samples dilute

d 1:1 0 an d reporte

d fro m extemal standar

d calibration . Tabl e 31 . DA L G W138 L 11121 4 PFB S PFH S PFO S Concentration Concentration Concerrtration 3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-07 0 DAL-GW-138L-0-11121 4 <0.025 0 N A 0.063 0 NA 0.46 1 N A GLP10-01-02-24-07 1 DAL-GW-138L-DB-11121 4 <0.025 0 N A 0.055 8 NA 0.37 9 NA GLP10-01-02-24-072 DAL-GW-138L-FMS-11121 4 1.0 0 99. 0 0.93 9 88. 1 1.4 0 98. 2 Average Concentration (ng/mL) ± YoRPD <0.025 0 0.0594 ng/mL± 12% 0.42 0 ng/m L ±20 % N A= Not /Applicabl e Reporte d result

s fo rPFB S an d PFH S ar

e fro m extema l standar

d calibration . Reporte d results fo rPFO S ar e fro m intema l standar

d calibration .

Pag e 3 0 o f11 0Tabl e 32 . DA L GW140 R 11121 3 GLP10-01-02 ; Interi m Repor t 2 4 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concerrtration Concerrtration Concerrtration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mLj^ %Recovery (ng/mL) YoRecovery GLP10-01-02-24-07 3 DAL-GW-140R-0-11121 3 1.2 3 N

A 13. 9 N A 100 N A GLP10-01-02-24-074 DAL-GW-140R-DB-11121 3 1.3 1 N A 14. 2 N A 103 NA GLP10-01-02-24-075 DAL-GW-140R-FMS-11121 3 97. 7 95. 5 109 95. 1 18 1 79. 7 Average Concentration

(ng/mL) ± %RPD 7.27 ng/m L ±6.3 % 74.7 ng/mL ±2.7 % 70

2 ng/m L ±3.0 % N A= No t Applicabl e Sample s dilute d 1:1 0 and reporte

d fro m fro m extema l standar

d calibration . Tabl e 33 . DA L G W141 R 11121 4 PFB S PFH S PFO S Concerrtration Concerrtration Concentration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) %Recovery (ng/mL) YoRecovery GLP10-01-02-24-07 6 DAL-GW-141R-0-11121 4 0.035 1 N A 0.25 9 N A 4.9 7 NA GLP10-01-02-24-07 7 DAL-GW-141R-DB-11121 4 0.0333 N A 0.24 8 N A 4.7 7 NA GLP10-01-02-24-07 8 DAL-GW-14 1 R-FMS-11121 4 1.0 0 95. 6 1.1 5 89. 8 5.8 0 N C Average Concentration

(ng/mL) ± YoRPD 0.034

2 ng/m L ±5.3 % 0.254 ng/mL ±4.3 % 4.8 7 ng/m L ±4.7%" ^ N A= Not/Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspil<e level . Reporte d results fo rPFB S an d PFH S ar e fro m extema l standar

d calibration . Reporte d results fo rPFO S ar e fro m intema l standar

d calibration . (1 ) Samplin g locatio n di d no t hav e a n appropriate FM S spik e leve l t o suflicienti yevaluate PFO S recovery .

Pag e 3 1 o f11 0Tabl e 34 . DA L G W142 R 11121 3 GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concerrtration Concerrtration Concerrtration 3M LIMS ID Description (ng/mL) YoRecovery (ng/mL) XRecovery (ng/mL) YoRecovery GLP10-01-02-24-07 9 DAL-GW-142R-0-11121 3 1.8 3 N

A 10. 2 N A 94. 5 N A GLP10-01-02-2408 0 DAL-GW-142R-DB-11121 3 1.7 0 N

A 9.74 N A 94. 2 N A GLP10-01-02-24-08 1 DAL-GW-142R-FMS-11121 3 48. 2 92. 0 53. 8 87. 8 13 1 73. 4 Average Concentration

(ng/mL) ± YoRPD 7.7

7 ng/m L ±7.4 % 9.97 ng/mL ±4.6% 94. 4 ng/m L ±0.32 % NA= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration . Tabl e 35 . DA L G W143 R 111209 PFB S PFH S PFO S Concentration Concentration Concerrtration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) %Recovery (ng/mL) YoRecovery GLP10-01-02-24-082 DAL-GW-143R-0-11120 9 0.70 9 N A 2.3 3 N A 16. 1 N A GLP10-01-02-24-08 3 DAL-GW-143R-DB-11120 9 0.72 1 N A 2.3 3 N A 15. 1 N A GLP10-01-02-24-084 DAL-GW-143R-FMS-11120 9 21. 6 103 19. 6 86. 4 30. 2 73. 0 Average Concerrtration

(ng/mL) ± YoRPD 0.775 ng/m L ±7.7 % 2.33 ng/m L ±0.0 % 15.6 ng/mL±6.4Yo NA= No t /Applicabl e Samples dilute d 1:1 0 an d reporte d fro m extema l standar d calibration .

Pag e 3 2 of11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Tabl e 36 . DA L G W144 R 11121 3 PFB S PFH S PFO S Concentration Concentration Concerrtration 3M LIMS ID Description (ng/mL) XRecovery (ng/mL) YoRecovery (ng/mL) YoRecovery GLP10-01-02-24-08 5 DAL-GW-144R-0-11121 3 2.0 5 N A 7.5 6 N A 26. 4 NA GLP10-01-02-24-08 6 DAL-GW-144R-DB-11121 3 1.99 N A 7.5 1 N A 26. 9 NA GLP10-01-02-24-08 7 DAL-GW-144R-FMS-11121 3 55. 9 107 47. 4 79. 9 70. 0 86. 9 Average Concerrtration

(ng/mL) ± YoRPD 2.02 ng/m L ±3.0 % 7.54 ng/mL±0.66Yo 26.7ng/mL±7.9 % NA= No t /Applicabl e Reporte d result s fo rPFB S and PFH S ar

e fro m extemal standar

d calibration . Reporte

d result s fo rPFO S ar e fro m intemal standar

d calibration . Tabl e 37 . Tri p Blan k

1 PFB S PFH S PFO S Concentration Concerrtration Concentration 3M LIMS ID Description (ng/mL) XRecovery (ng/mL) %Recovery (ng/mL) YoRecovery GLP10-01-02-24-09 4 DAL-GW-TRIP01- 0 <0.025 0 N A <0.025 0 N A <0.037 1 NA GLP10-01-02-24-09 5 DAL-GW-TRIP01-LS 0.99 4 98. 4 0.92 0 92. 2 0.94 3 94. 5 GLP10-01-02-24-09 6 DAL-GW-TRIP01-M S 19. 6 97. 0 18. 5 92. 5 19. 7 98. 5 GLP10-01-02-24-09 7 DAL-GW-TRIP01-MH S 10 1 100 93. 6 93. 8 86. 5 86. 7 GLP10-01-02-24-09 8 DAL-GW-TRIP01-H S 49 9 99. 2 46 7 93. 6 41 2 82. 6 NA= No t /Applicabl e Reporte d result

s fro m extema l standar

d calibration . Th e MH S sampl e was dilute d 1:10 , ttieHS sampl e was dilute d 1:100 .

Pag e 3 3 o f11 0Tabl e 38 . Rinseat e Blank s GLP10-01-02 ; Interi m Repor t 2 4 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

PFB S PFH S PFO S Concerrtration Concerrtration Concentration 3M LIMS ID Description (ng/mL) %Recovery (ng/mL) YoRecovery^ (ng/mL) %Recovery GLP10-01-02-24-09 9 DAL-GW-140R-RB-11121 3 <0.025 0 NA <0.025 0 N A <0.037 1 NA GLP10-01-02-24-10 0 DAL-GW-133L-RB-11121 4 <0.025 0 NA <0.025 0 N A <0.037 1 N A N A= No t /Applicabl e Reporte d results fro m extema l standar d calibration . Tabl e 39 . Surrogat e Recover y 3M LIMS ID Description PFOS surrogate Yo Recovery GLP10-01-02-24-05 8 DAL-GW-137S-0-11120 9 93. 5 GLP10-01-02-24-05 9 DAL-GW-137S-DB-11120 9 106 GLP10-01-02-24-06 0 DAL-GW-137S-FMS-11120 9 10 2 GLP10-01-02-24-06 1 DAL-GW-137L-0-11120 9 10 1 GLP10-01-02-24-06 2 DAL-GW-137L-DB-11120 9 98. 5 GLP10-01-02-24-06 3 DAL-GW-137L-FMS-11120 9 91. 8 GLP10-01-02-24-07 0 DAL-GW-138L-0-11121 4 94. 0 GLP10-01-02-24-07 1 DAL-GW-138L-DB-11121 4 93. 4 GLP10-01-02-24-072 DAL-GW-138L-FMS-11121 4 97. 7 GLP10-01-02-24-07 6 DAL-GW-14 1 R-0-11121 4 93. 7 GLP10-01-02-24-07 7 DAL-GW-14 1 R-DB-11121 4 95. 1 GLP10-01-02-24-07 8 DAL-GW-14 1 R-FMS-11121 4 97. 8 GLP10-01-01-24-08 5 DAL-GW-144R-0-11121 3 10 2 GLP10-01-01-24-08 6 DAL-GW-144R-DB-11121 3 96. 9 GLP10-01-01-24-08 7 DAL-GW-144R-FMS-11121 3 93. 9

Pag e 3 4 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

10 Conclusion Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS . Analysi s was successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 1 describe d herein . 11 Data/Sample

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

Pag e 3 5 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1



### 12 Signatures

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

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



# 2- / 7-Z / Date Gar yHohlenstein , Sponso rRepresentative

Jaisimh a Kesapf, Stud yDirecto r pat e

Pag e 3 6 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 

### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 3 7 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24


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

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

PROTOCO L AMENDMEI^ TNO . 2 4

Amendment

Date: Decembe r1 , 201 1 Performing

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

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

Project Identification GLP10-01-0 2
Sampling

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

Pag e 1 o f7 Pag e 3 8 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24 

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

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

PROTOCOLREADS: N o change s t o th e wordin g ofth e protoco l are required .

AMEND TO 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 ofth e Genera l Projec t 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 durin g th e wee k of Decembe r5 , 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 project GLP10-01-02-2 4 an d reporte d a s interi m repor t GLP10-01-02 - 24 , (reflectin g stud yGLP10-01-0 2 an d amendmen t -24) .
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 of7 Pag e 3 9 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24 

### Amendmen t Approva l 

# n Gar yHohensteri , Sponso rRepresentative Date

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

Willia m Reagen , EHSppn s Environmenta l La b Managemen t Date 

# mil Jaisimh a Kesar i f*-

^ , DEE , StudyDirecto r D^ e

Pag e 3 of7 Pag e 4 0 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24 ^IM i 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 Clesto n Lange , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Decembe r1,201 1 Date : Subject : Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d

Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 2 4 - Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r- Decembe r201 1 Samplin g 1 Genera l Projec t Informatio n 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone : (651 ) 737-357 0 Qahohenstein(5)mmm.co m 3W 1 Environmenta l Laborator yManagemen t Willia m K

. Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 Contact s wkreaaen(3!mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanaeOmmm.co m Samplin g Coordinato r Timoth yFrinal < Westo n Solution s Timothy.frinakOwestonsolutions.co m Phone : (334)-332-912 3 La b Reques t Numbe r CLP10-01-02-2 4 Si xDigi t Departmen t Numbe r Dept #530711 . Project #002267444 9 Projec t Schodule/Tes t Date s Samplin g schedule d fo rth e weel < o fDecembe r5 , 201 1 All verbal and written correspondence

will be directed to Gary Hohenstein.
Pag e 4 of7 Pag e 4 1 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m twenty-seve n groundwate rwell s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) fro m th e Forme rSludg e Incorporatio n Are a (FSIA) . Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792 . Groundwate rsample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k of Decembe r5 , 2011 . Th e 3 M Environmenta l Laborator yv/il l prepar e th e sampl e bottle s wit h al l require d spike s to ensur e tha t result s fo rPFBS , PFHS , an d PFO S ar e o fa know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10 - 01-02-24 . 3 Projec t Schedul e Sampl e collectio n bottle s wil l be prepare d b y3 M Environmenta l Laborator yfo rsamplin g th e wee k

ofDecembe r 5 , 2011 . Sampl e bottle s wil l be shippe d i n cooler s to 3 M Decatu rfo rarriva l b yMonday , Decembe r5 , 2011 . Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection . Marti n Smit h \

Westo n Traile r 3 M Decatu rPlan t 140 0 Stat e Docks Roa d Decatur , Alabam a 3560 1 4 Tes t Parameter s Th e targete d limi t ofquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS , PFHS , an d PFOS . Atota l o fthirty-on e samplin g location s hav e bee n specified . Fo reac h samplin g location , a sample , sampl e duplicat e an d fiel d matri xspik e wil l be collected . Tabl e 1 indicate s th e wel l I D an d correspondin g fiel d spik e level . Th e "fil l to here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l be 20 0 mL . On e sets oftri p blank s consistin g of reagent-grad e water , a low-leve l tri p blan k spike , mid-leve l fiel d spike , mid-hig h fiel d spike , an d a high-leve l tri p blan k spik e wil l b e prepare d a

t th e 3 M Environmenta l Laborator yan d sen t to th e samplin g locatio n wit h th e othe rbottles . Based o n previou s samplin g ofth e FSI A(GLP10-01-02-07 , GLP10-01-02-011 , an d GLP10-01-02-18) , mor e tha n hal fo

fth e sampl e location s ar

e expecte d to hav

e PFH S and/o rPFO S level s greate rtha n 100 ng/mL . To ai d i n th e quantitatio n o

fsamplin g location s wit h PFBS , PFH S an d PFO S level s at expecte d concentration s o f <50 ng/mL , sampl e bottle s wil l contai n th e additio n o finterna l standard s '^02-PFBS , ^^Ca-PFHS , an d ^^CgPFOS , a s wel l a s '^C4-PF0 S surrogate . Th e tri p blan k sample , tri p blan k

lo wan d mi d spike s wil l als o includ e th e additio n o

finterna l standar

d standard s '^Oz-PFBS , '^Ca-PFHS , an d ^^Cs-PFOS , a s wel l a s '^C4-PF0 S surrogate . Two additiona l bottle s wil l be prepare d to b e use d fo rth e preparatio n ofth e equipmen t rinseat e blank s an d wil l als o contai n th e additio n o fintema l standard s '*02-PFBS , ^'Ca-PFHS , an d '*CB-PF0S , a s wel l as '^C^-PFO S surrogate . A1 - L bottl e o flaborator

yreagen t wate rwil l b e provide d t o be use d to collec t th e rinseate blanks .

Pag e 5 o f7 Pag e 4 2 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Analytical

Protocol:

GLP10-01-02 Amendment

24 Tabl e 1 . Samplin g Location s an d Fiel d Matri xSpik e levels . Set # Wel l No . Spik e Cone . (ng/mL) 1 * 136R , 137R , 137S , 137L ,

138L , 141 R 1. 0 2 * 131S,134S,135S,143 R 2 0 3 * 130L , 142R , 144 R 5 0 4 1308 , 131L , 133R , 136S ,

136L , 140 R 10 0 5 1338 , 133L , 135L , 138R , 138 8 20 0 6 130R , 134L , CW26C , CW26 L 50 0 7 131R,134R,135 R 200 0 Tri p Blan k 1 * 2 0 * Tri p Blan k 10 0 Tri p Blan k 50 0 surrogate . 5 Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 1 "Metho d ofAnalysi s fo rth e Determinatio n o

fPerfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr

yDirec t Injectio n Analysis" . Th e data qualit yobjective s fo rthes e studie s are quantitative results fo r th e target analyte s wit h a n analytica l accurac yof100±30% . Fiel d matri xspike s not yieldin g recoverie s withi n 100±30 % wil l be addresse d i n th e repor t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly . Based o n th e results fro m previousl ycollecte d sample s fro m th e FSIA , most samplin g location s wil l require dilutio n wit h laborator yreagen t wate rprio rto sampl e analysi s b yETS-8-044.1 . 

### 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 field matri x spike . 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 yequipment/rinseat e blank s prepare d i n th e field. Laborator ycontro l spike s o

freagen t wate rprepare d a t th e tim e ofsampl e preparatio n wil l als o be reporte d an d use d t o evaluate th e overal l metho d accurac yan d precision . Metho d blank s ofreagen t wate rprepare d a t th e tim e ofsampl e preparatio n wil l b e use d t o determin e th e metho d detectio n limit . Fo rthos e samplin g location s wher e th e field matri xspik

e leve l was no

t appropriate , du e to highe rtha n expecte d analyt e concentrations , a laborator ymatri xspik

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

### 7 Emai l Correspondenc e Attachmen t A : Samplin g Bottl e Reques t

Pag e 6 o f7 Pag e 4 3 o f11 0GLP10-01-02; Interim Report 24 Analysis of PFBS, PFHS, and

PFOS in Groundwater Decatur, AL-

December

2011 Analytical

Protocol:

GLP10-01-02 Amendment

24 Attachmen t A



### Bolll e reques

t fo r 4lhquarte

r 201 1 FSI Awel l samplin

g Young , Charles T . to:stwolf(^inmm.co m 11/29/201 1 03:1 0 P

M Cc:"Frinak, Timolh

y R." , "Smil LMartin " From : "Young , Charles T. " <Charles.Young@WestonSolutions.com > Sue : Ti m Frina k

an d Marti n Smit h are settin g u p fo rgroundwate rsamplin g commencin g nex t wee k at th e followin g Forme rSludg e Incorporatio n Are a monitorin g wells :

130 R 133 L 136 S 140 R 130 S 134 R 136 L 141 R 130 L 134 S 137 R 142 R 131 R 134 L 137 S 143 R 131 S 135 R 137 L 144 R 131 L 135 S 138 R CW26 C 133 R 135 L 138 S CW26 L 133 S 136 R 138 L Ca n yo u prepare a bottl e se t fo rshipmen t t o Marti n Smith' s attentio n at Decatu rwit h arriva l b yTuesday , Decembe r6 , 2011 ? A s wit h eartie rrounds , analysi s wil l b e performe d unde rGLP10-01-0 1 an d GLP10 - 01-02 . Du e t o th e relativel ylowG Wlevel s at th e site , som e ofth e abov e well s ma yb e dr yan d therefor e wil l not b e sampled . Marti n wil l retur n an yunuse d bottl e set s shoul d som e ofth e location s hav e insufficien t wate r fo rsampling . Thanks , Charti e Charle s T . Youn g Technica l Directo r Westo nSolutions , Inc . 140 0 Westo nWay (5-2 ) Wes t Chester , P

A1938 0 (610 ) 701-378 7 Fa x (610 ) 701-340 1 

### CONFlDENTIALrrY : Thi s emai l an dattaclmient

s ma y containinformatio nwhichi s confidentia

l an dproprietary . Disclosur

e o r us e o f an y suc hconfidentia

l o r proprietcir

y infonnatio nwithout

th e writtenpermissio

no f Westo nSolutions , Inc . i s strictly prohibited . I f yo u receive dthi s emai

l inerror, pleas

e notif y th e sende r b y retur ne-mai l an ddelet e thi s emai

l fro m you r system. Than

k you .

Pag e 7 of7 Pag e 4 4 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 

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

Pag e 4 5 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Workstation : ETSKIR K Result s Name : klll227a.rd b k111227a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -84 2 x'^ 2 + 9.99e+00 5 x+ 2.63e+00 4 ( r= 0.9998 ) 8.5e 7 8.0e 7 7.5e7 7.0e 7 6.5e7 6.0e 7 5.5e 7 5.0e7 4.5e7 i u 4.0e7 < 3.5e

7 3.0e 7 2.5e 7 2.0e 7

0. 0 1 5 2 0 2 5 3 0 35 4 0 4 5 5 0 Concentration , ng/m L 5 5 6 0 6 5 7 0 7 5 8 0 85 9 0 Dat a worke d up b yKJ U Printin g Time : 9:46:0 2 A M Pag e 1 o f 1 Printin g Date : Wednesday , Januar y04 , 201 2 Pag e 4 6 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Workstation : ETSKIR K Result s Name : klll227a.rd b

Dat a worke d u p b yKJ U Printin g Time : 9:46:3 2 A M Pag e 1 o f 1 Printin g Date : Wednesday , Januar y04 , 201 2 Pag e 4 7 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analyst s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Workstation : ETSKIR K Result s Name : klll227a.rd b

Dat a worke d u p b yKJ U Printin g Time : 9:45:1 6 A M Pag e 1 o f 1 Printin g Date : Wednesday , Januar y04 , 201 2 Pag e 4 8 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

Sampl e Nam e 1(11122To018 " Sampl e ID : '11012-10-9 - File ' "k 1 n227a.*t r Pea k Nan>« . -PF8S ' Mass(as) : *299.00a«0.00 0 Oa,299.00a/99.00 0 Da Comment . "2. 5 ntj'm L F

C std I n Mill i O Watof " Armotaliofi ; ~ Sampl e Index : I B

Dat a printe d b yST W Thursday , Januar y26 , Pag e 1 o f 2 7 Pag e 4 9 o f11 0GLP10-01-02 : Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I Sampl e Name,-1(1112270035 ' Samptel D -LCS-111221-10 - Fil e "kl l Pea k Name : -PFBS - Massfes) - -299.D00/SD.000 Da,299.000/99.00 0 Da Comment.-30pp b LCS " Annolano n - :ample Index: 3b 2 9. 9 ng/m L 2 6. 3 ng/mL 12/28/201 1 12-03:5 5 A

M
Peak-Split . Facto i Repor t Larges t

Pe ; Min . Pea

k Height : Hln . Pea

k Hldth : Snoothin g Width : fir Hindow : Expecte dRT : 7 0 1.0 0 I

iHel i ! RT : Manua l

• : 12. 8 23S590S 3 t 

# I SampleNam e •k111227aCM2 - Sampl e I D -GLP10-01-02-24-099 - Fie , Pea k Name : 'PFBS " Mass(es) : '299.000/80.00 0 Da,299.000/99.00 0 Da Commen L "DAL-GW-WOR-RB- " Annotatio n ~ Sampl e Index ' 4 2 Sampl e Type : Unknow n Concentration : ll/ A Calculate d Cone : < 0 Acq . Date : 12/2B/201 1 Acq . Time : 2:28-3 4 A M Modified : ll o Proc . Algorithm
- Specif y Paramet t Baae. Sub. Window: 1.00ain Peak-Split . Factei : 3 Repor t Larges t

Peak : Ye s Hin . Pea

k Height : 0.O O cp t Min . Pea

k width : 0.0 0 se t n g width . R T h Expecte dF 30C 12. 8 itlv e BT ; ll o Int . Type : Bas e T o Bas e Retentio nTime : 12. 8 rain Area : 365 4 count s



### ( Sampl e Name ' -k111227a043 - Sampl e ID : -GL P 10^) 1 •02-24-100 - RI e Poa k Name ' 'PFBS ' M3ss(es) - '299.000/80.00 0 Da.299.000/99.00 0 Da ' CommenL-DAL-GW-lSSL-RB- " Annotatio n " Sampl e Index ; 4 3 Sampl e Typ e Calculate dCone : K/ A

Proc . Algorithm : Specif y f Base . Sub . Hindou : l.O C Peak-Split . Factor : 3 Repor t Larges t

Peak : Ye : tlin . Pea

k Height : O. f Min . Pea

k Width : O.

C Smoothin g width : 3 R T Kindow ; 30. 0 Expecte dKT i 12. 3 Us e Relativ e RT : N o Retent i Height : 6,51e-*00 2 CP S 

# I SampleNam e •kin227a046 ' Samplel D 'GL P1CK>1-02-24-096 " Flo : Pea k Name : 'PFBS ' Massfes ) '299.000/80.00 0 Da.299.000/99.00 0 Da
Comment

-DAL-QW-TR1P01-MS-
- Annotation ' - Sampl e Index : i 6 Sampl e Type : Unknow n

,r s - H Q I Modified . ll o Proc . Algorithm
- Specif yParamet i Nois e Percentage : 7 0 Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor : 3 Repor t Larges t Peak : Ye s Min . Pea k Height : 0.0 0 cp : Hin . Pea k width : 0.0 0 se c Smoothin g Width
- 3 point s 2 0e6 ' R T Window : 30. 0 se c Expecte d RT : 12. 8 Di n Us e Relativ e RT : H o Int . Type : Valle y

10. 5 11. 0 11, 5 12, 0 12, 5 13. 0 13. 5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 2 o f 2 7 Pag e 5 0 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll22'7 a . rd b 

# I Sampl e Name : •k111227a049 ' Samplel D 'GLP10-01-02-24.001 - Flte''k111227a.wrf r Pea k Nam e "PFBS " Mass{es ) '299.000/80.00 0 Da,299.000/99.00 0 Da Comment - "DAL-GW-130R-0- " Annolation . ~

Base . Sub . Window : Peak-Split . Factor : Repor t Larges t

Peak : Min . Pea

k Height ; Hin . Pea

k width : in g Width : 2.5e 4 2/4e4 2.3e 4 2.2e 4

R T Window : 1.Se 4 1.7e 4 1,6e4 ' 1.5e 4

7000.0 - 6CK».0 ' SOOO.O4000. 0 3000.0 - 2000. 0 1000. 0 0.0 - 12. 5 13. 0 13. ! 

# I Sampl e Name : •k111227B056 ' Sampl e ID . 'GL P 1001-02-24-004 ' Fte ' " I Pea k Name . 'PFBS - Massfes) , -299.000/80.00 0 Da,299.000/99.00 0 Da Commen t 'DAL-GW-130S-0- ' Annotatron . "
S.0e 4 4.Sa4 ' 4.6e4 4.4^ ' 4.2e4 - 4.0e 4 3.8e4 ' 3.6e 4 3/4e 4 3.2e 4 3.0*4 - 2.8e4 - Proc . Algorithm : S i Base . Sub . Window : Peak-Split . Factor : Repor t Larges t

Pea l Kin . Pea

k Height : Kin . Pea

k Width : Smoothin g width : R T Window : Expecte dRT : Bas e T o Bas e

2.4« 4 2.2e4 > 2.0a 4

1.0e4 - BOOO.0 - 6000.0 - 4000.0 - 2000.0 - 0.0 - 

## ( Sampl e Name : 'k111227a0S9 * Sampl e ID ' *GLP1041-02-24-007 ' Fil e ' Pea k Name . -PFBS " Mass(es) . -299.000/B0.00 0 Da,299.000/99.00 0 Da Comment . "DAL-GW-130L-O- - Annotation , " Sampl e Index : 5 9 Sampl e Type : Unknow n Calculate dCone : 1.S O ng/m L Acq , Date : 12/28/201 1 2,3ft4
- Acq , Time : 8:19:5 1 A M 2.2*4
- Modified : ye s 2.1e4 - Proc . Algorithm
- Specif y Parameter s - H Q 11 1 

# I SampteNam6;'k111227a062 ' SamptoID:•GLPHM)1-O2-24-010 ' Fie:'k111227a.wrf r Pea k Name . 'PFBS ' Mas5(es} , -299.000/80.00 0 Da,299,000^9.00 0 Da " Commen t 'DAL-GW-ISIR-O- ' Annotation. " Sampl e Index : 6 2

lin g Mid i .« dRT :

15272 0 c c

2.41e-f00 4 12. 6 1.6»4 < 1.5»4 - 1.4e4 < 1.3M 1.2e4 - 1.1*4 - 1.0e4 - 9000.0 -

6000.0 - 5000.0 - 4000.0 - 3000.0 - 2000.0 - 1000.0 - co-bftf ^ 10. 5 Dat a printe d b yST W Thursday , Januar y26 , Pag e 3 o f 2 7 Pag e 5 1 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I SampleNam e "k l 11227b0G9 " Sampl e ID : "GLP10-01-02-24-013 ' Fil e Pea k Name ' "PFBS " Mass(es) ' "299.000/60.00 0 Da,299.000/99.00 0 Da " Commen I "DAL-GW-1 3 IS* ' Annotatio n " Sampl e Index : 5 Sampl e Type : Unknow n Concentration : N/ A Calculate dCone : 0.68 8 ng/m L Acq . Dat e 12/29/201 1 Acq . Time : 11:10:4 3 A M 1.6a 4 15e 4

. Algorithm : Specif y Paramet c Peak- :

Manua l 13. 3 "7536 3 < 1.3* 4 12e4 - 1.1e4 - 1.0e4 - 9000.0 - 8000.0 - 7000.0 - 6000. 0

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

# I SampteNaine'"k111227t)072 " Samplel D "GLPIMl-02-24-016 ' Fie ' Pea k Name ' "PFBS " Mass(es) , "299,000/80.00 0 Da,299,000/99.00 0 Da Comment : •DAL-GW-131L-0- " Annotatio n - Sampl e Index : S Sampl e Type : Unknow n Calculate dCone : 2.8 4 ng/m L 12/29/201 1 12:12: ' Acq . Tira i Modified : Ye s Proc . Algorithm : Specif yPar i Nois e Percentage : 7 0 Base . Sub . Window : 1.0 0 Peak-Split . Factor : 3 Repor t Larges t Peak : Ve s Hin . Pea k Height
- 0,0 0 Hin . Pea k Width : O.O O Smoothin g Width : 3 R T * Expected RT; 13. 3

Bas e T o E : : 13. 3 27907 3 c i

13, 0 13. 5 14. 0 14. 5 

# I Sampl e Name : -k l 112271)075 ' Sampl e ID . -GLP1CM)1-02-24-019 ' File : 'k111227b,wi r Pea k Name : TFES ' Massfes) : '299.000/80.00 0 Da,299.000/99.00 0 Da Comment:-DAL-GW-133FW>- - Annotattoo: -

Peak-split . Factor : Repor t Larges t Peak : Min . Pea k Height : Min . Pea k Hldth :

Bas e T o Bas e Height : Star t T l En dTim * 

# I SampleNam e •k111227t)0e2 " Sampl e ID'•GLP1CWH-02-24-022 " F< e •k111227b.wt r Pea k Nam e "PFBS " Ma»s(e») : "299.000ffl0.00 0 Da599.000«9.00 0 Da Commen t "DAL-GW-133S-0- " Annotation. " Sampl e Index ; 1 6 Sampl e Type : Unknow n 1.7e 5 1.6e 5 1.50 5 1.4e 5 1.3e 5 1.2o5 l.le S 1.0a 5 9.0e 4 a.0e 4 7.0e4 6.0e4 5.0* 4 4.0e 4 3.0« 4 2.0e 4 1.0« 4 12. 5 13. 0 13. 5 14, 0 Time , mi n Dat aprinte db y ST W Thursday , Januar y26 , 201 2 Pag e 4 o f 2 7 Pag e 5 2 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 5 o f 2 7 Pag e 5 3 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS . an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

## ( Sampl e Name , -k111227bl01 " Sempte ID : -GLP10-01-02-24-037 - FIte : Pea k Name : -PFBS - Masses) : -299.000ra0.00 0 Da,299.000/99.00 0 Da Comment : •DAL-GW-135R-0- - Annotatio n " Sampl e Index : • 3 7 Sampl e Typ e Calculated

Cone K/h

63. 9 ng/ r

Base . Sub . Window : Peak-Split . Facto r Repor t Larges t Pea l Kin . Pea k Height : Min . Pea k Width ; Smoothin g Width : R T Kindow : Sampl e Name ' -V111227b108 ' Sampl e t O 'GLPI0-01-02-24-040 " FN ' 'k l 11227b.wi r •Pea k Name ' "PFBS * Massfes) : '299,000/BO.OO O Da,299.000i/99.00 0 Da ' I Commen t "DAL-GW-IKS-O- - Amwtation : " Sampl e Index : 4 4 Sampl e Type : Unknow n Concentration . ll/ A15eS
Calculate d Cone : 0.96 1 ng/m L Acq . Date : 12/30/201 1 Acq . Tine
- 12:35:5 0 A M Ho d I I Noi : Algorithm : t

.age :

. Sub . Min t Peak-Split . Factor ' Pepor t Larges t Peak . Hin . Pea k Height : Hin . Pea k width : Smoothin g Width : BT Window : ; Expecte d RT ; Us e Relativ e RT : Bas e T o Bas e

:: 13.2 lain 91997 5 count s 1.52e+00 5 cp s

12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 

# I Sampl e Name ' -k111227b111 ' Sampl e ID : 'GL P 1041-02-2 ' Pea k Name : -PFBS - Mass(es) : -2S9.000/80.00 0 Da,299.00C Commen i "DAL-GW-135L-0- ' Annotatkin, -

Mois e Percentage : Base . Sub . window : Peak-Split . Factor ; Pepor tLarges tPeak ; Min . PeakHeight : Min . PeakWidth : Smoothin g width : R T Window : 30 Expecte d RT ; 1 . Us e Relativ e RT : K i • : •k11l227b.wtf r 

### ( Sampl e Name ' "kt11227b114 - Sampl e ID ' ' G L P tIM)1-02-24-049 * Fie: ' Pea k Nam e -pFBS " Maas(es] ' '299.000/80.00 0 Da,299.000/99.00 0 Da Commen t "DAL-GW-136S-(V " /\nr>otal)Oo : " Sampl e Indej c 5 0

Type ; Bas e T o Bas e l.05e5
- 1.00e5
- 9.50e4
- 9.00e4
- S.50e4
- 8.00e4
- 7,SOe4
- 7.00e4
- S.50e4
- 6.00«4 '

4,50e 4 4.00e4 ' 3.50e4
- 3.00* 4 2.50e4 ' 2,00e4 ' 1,50*4
- 1.0OM
5000.00
- 0.00
- Sampl e Type : ll/ A

Base . Su b Peak-Split . Factor : 3 Repor t Larges t Peak ; ' Hin . Pea k Height ; I Min . Pea k Width ; I Smoothin g width ; R T Window : 30. 0 Expecte d RT ; Specif yParameter s - M Q 11 1 7 0 <: 1.0 0 mi n

! Rela l Int . Type : Retentio n 1 Height : ! RT : ll o 3.0e 4 2.Se 4 2.6e 4

1.8e 4 1.6o 4

1.0e 4 6000.0 6000. 0 4000. 0 2000. 0 0.0- 12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 Tima . mi n Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 6 o f 2 7 Pag e 5 4 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

Dat aprinte db y ST W Thursday , Januar y 26 , 201 2 Pag e 7 o f 2 7 Pag e 5 5 o f 11 0GLPIO-01-02 : Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•SampteNam6:"k111227b13T - Sampl e ID'•GLP1CW)l-02-24-06 rFBe . "kl11227b.wrf r •Pea k Name:-PFBS " Ma£s(ei):*2e9,000/80.000Da,299.000J99.000Da ' I Commeni:-DAL-GW>13eS-0- ' AnnoOUon:* * Sanpl e Index : 7 3

Proc . Algorithm : Spe c Nois e Percentage : Base . Sub . window ; Peak-Split . Factor
Repor t Larges t

Peak ; Kin . Pea

k Height : Min . Pea

k width ; 0.0 0 cp s R T Window : (idth :

. 0 14. 5 15. 0 15. 5 

## ( Sampl e Name : -kil l 227bl40 " Sampl e ID , • < Pea k Name . -PFBS ' Mass(es) . "299.000/80.0 ( Commen t "DAL-GW-1381-0- " Anrwtatkin," " Sampl e Index : 7 6 Sanpl e Type ; Unknow n Concentration : ll/ A Calculate dCone : 0.012 1 ng/m L

Peak-Split . Factor ; Hin . Pea

k Height :

I t Type
ftentio nT ] sight : Bas e T o Bas e

2159 1 count s 1.25e4 1.20e4 1.15e4 1.10e4 1.05«4 1.00e4 9500.0 0 9000.0 0 &S00.00 8000.0 0 7500.0 0 § •7000.0 0 ^6500.0 0 I 6000.0 0

~ 5500.0 0 5000.0 0 4500.0 0 4000.0 0 3500.0 0 3000.0 0 2500,0 0 2000.0 0 1500.0 0 1000.0 0 500.0 0 0.0 0 

# I SampteNam e •kl11227b14 rSampl e ID:•GLPlOfll-02-24-073 * File : Pea k Name ' "PFBS " Mas»(es) . "299.000/80.00 0 Da.299.000«9.00 0 Da " Commen f"DAL-GW-140R-0- " Annotation . ~ Sampl e Index ; 8 3 Sampl e Type : Unknow n Concentration : N/A Calculate d Cone : 1.2 3 ng/Ri L Acq . Date : 12/30/201 1 2.0* 4 Acq . Tine : 2:01;4 1 P K 15e 4 Modified : Ye s I I 1.ee4 1.70 4 •k111227b.viiit r

Proc . Algoc i Nois e Perce r hn : Specif y Parametet i

Min . Pea

k Height ; Min . Pea

k Width : Smoothin g Width ;

5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 

## ( Sampl e Name : "k l n227b150 - Sampte ID : " i Pea k Name , "PFBS " Ma5S(es) , -299.000/80.0 1 Commen t T)AL-GW-141R-0- - Annotation. " Sampl e Index : 3 6 0.035 1 r 12/3D/201 1 3:03: 4 1 P

M s"K111227b.wrt r

. Peak Width . .thin g R T Hindo i

11,6 5 7.65e+00 3 1.3»4 1.3*4 - 1.2e 4 1.2»4 ' 1.1e4 - 1.1e4 ' 1.0e4 ' 9500.0 - 9000.0 - 8500.0 - 800 0 0 - 7500.0 -

. 7000.0 - 6500. 0 6000.0 - 550 0 0 - 5000. 0 4500.0 - 4000. 0 3500.0 - 3000. 0 2500.0 - 2000.0 - L 13.8 8 11. 5 12, 0 12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 8 o f 2 7 Pag e 5 6 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I Sampl e Name : "k111227bl53 - Sampl o ID ' "GLP10-01-02-24-079 " Fite ' •kll1227b.wrf r Pea k Name : "PFBS * Mass{es) ' -299,000/80,00 0 Da,299.000/99.00 0 Da Comment : "DAL-GW-142R-0. * Annotation : " * Sampl e Index : 8 9 0.70 9 r 12/30/201 1 6 ; 30;2 3 P

M

. PeakHeight ; 

# I Sampl e Name . •kin227b160 - Samplel D " G L P 1 CM)1-02-24-082 - Flo : "kil l 227b.wrf r Pea k Name . "PFBS " Mass{es) : "299.000/80,00 0 Da,299.00IV99.00 0 Da ' Commen t "DAL-GW-143R-0- - Ajwiotatwn *



## ( Sampl e Name ' "kl l 1227b163 - Sampl o ID : 'GL P IW)1-02-24-085 " File . Pea k Name : "PFBS " M3*s(es) . "299.000/80.00 0 Da.299.000/99.00 0 Da Commen t "DAL-GW-mR-O- - Annotation:" * Sampl e Index : 9 9 Sampl e Type ; Unknown Concentration ; N/ A Calculate d Cone : 2.0 5 ng/n L Acq . Date ; 12/30/201 1 Acq . Tine : 7:32:2 3 P H

Peak-Split . Factor ; Pepor t Larges t Pea l Hin . Pea k Height : SDOOthln g Hi d Expecte d RT ;

Height : Star t 1 En d Ti n 

## ( Sampl e Name ; •k111227a018 " Sampl e I D "11012-10-9 " FBe ' •k111227a.iiw r Pea k Name : "PFHS " Maasfes) ' '399.000/99.00 0 Da,399.000/80.00 0 Da ' Commen t "2. 5 ng/m L F

C «td i n Mil i Q Water " Annotation. " Sampl e Index : 1 8 Sampl e Type ; Standar d Concentration : 2.5 0 ng/mL Calculate d Cone : 2.7 3 ng/mL Acq . Date : 12/27/201 1 Acq . Time : 6:12;< 3 P M Modified : ll o Proc . Algorithm : Specif y Parameter s - M Q II I Nois e Percentage : 50 Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor ; 2 Repor tLarges tPeak ; Ve s Min . Pea kHeight ; 0.0 0 cp s Min . PeakMldth ; O.O O se c 1 RT :

3.94e-t00 5 cp s

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e Pag e 5 7 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•Sampl e N8me"k111227a028 - Sampl e ID . "Solven t Blank ' Fie . "kl l 1227 a wtf T I Pea k Name , "PFHS " Mas«(es} . "399.000/99.00 0 Da,399.000/80.00 0 Da " I Commen t "MBiQWaterTNll-0437 ' Annotatio n - Sampl e Index : 2 B Sampl e Type ; Unknow n Concentration : H/ A Calculate d Cone : < 0 Ac q Date : 12/27/201 1 Acq , Tiroe : 9-39:1 9 P H 8500 - 9000

Min . PeakHeight : MinPea kNidth . Smoothin g Midth : 0.0 0 se c 3 point !

Area : 26 9 count : Height ; 2.71e*00 2 cp : 8000 7500 700 0 eso o 600 0 550 0 a 500 0 I " 450 0

- 400 0 3S00 300 0 250 0 200 0 150 0 100 0 50 0 

# I SampteName-1(1112278028 - SamplelDT.CS-111221-4 - Fie : Pea k Name : 'PFHS ' Uass(es ) -399.000/99.00 0 Da,399.000/80.00 0 Da ' Commen t -O.Sppb LCS - Annotation ' " Sampl e Index . 29 Sampl e Type ; Q C Concentration ; 0.49 7 ng/m L Calculate d Cone : 0.50 6 ng/m L Acq . Date ; 12/27/201 1 Acq . Time : 9:59:5 8 P M
Peak-Split . Factor : 2 Repor tLarges tPeak ; Ye i Min . Pea kHeight : O. C Min . Pea kWidth ; O. C Smoothin g Width : 3 R T Window : 30. 0 Expecte d RT ; li. A Us e Relativ e RT : M o mt. Type: Valley Retention Time; 11.4 Area; 42Se56 c< Height : 7.54e'O0 4 Star tTime ; H. 2 En d Time ; H. 6

12. 0 12. 5 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 

# I Sampto Name : -k l 11227a03 rSampt e ID : TCS-111221- rRte : -k l 1 1 Pea k Name : "PFHS " Mass(as) : -asg.OOO^g.OO O Da.399.OOQreO.00

0 Da Comment : -5pp b LCS " Annotation , " * Calculate d Cone : Acq . Time : 5.0 3 ng/m L 1/27/201 1 :01:5 7 P

M Modified : N o Proc . Algorithm ; Specif y Par ; Nois e Percentage : 5 0

Int . Type ; Valle y Retentio n Time ; H. 4

16855 3 7 . n e + 00 5 cp s 

# I Sampt e Name : 1(111227a035 " Sampl e ID ' -LCS- l 11221-10 - Fie : "k l 1 P»a k Name : -PFHS " Mass(es ) '399.000/99.00 0 D a .399.000^0.00 0 Da Commen t "30pp 6 LCS " Annotation : ~ Sampl e Index : 3 5

Proc . Algorithm : Specif y Paramet ' Nois e Percentage ; 50 Base . Sub . Window : 1.0 0 min Peak-Split . Factor ; 2 Repor tLarges tPeak : Vs a Min . Pea kHeight : 0.0 0 Min . Pea kWidth ; 0.0 0 Smoothin g Width : 3 R T Window ; 30. 0 Expecte d RT : H. A i

15.0 15.5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 0 o f 2 7 Pag e 5 8 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I SampteNam e "kl11227B042 " Sampte ID , "GLP10^1-02-24-099 " Fil e •k111227a.wi r Pea k Name . "PFHS " Mass{es) , "399.000/99.00 0 Da,38S.000/80.00 0 Da Comment : "DAL-GW-140R-RB- " AnnotaOon , -

Acq . Time : Modified ; Proc . Algorithm : Nois e Percentag e Base . Sub . Hindc i Peak-Split . Fact i Repor t Larg < 5 0

r : 1.0 0 Pes ) : Height ; Min . Pea k width ; Smoothin g Width : R T Window :

Bas e T o Bas e 9000
- 8500
- 8000
- 7500
- 7000
- 6500
- GOOO
5500
- 5000
-

250 0 200 0

14m, J ^^15.0 8 1 5 6 6 ^^^ ^ ^^^ ^

12. 0 12. 5 13. 0 13. 5 15. 0 15. 5 16. 0 16. 5 

# I Sampl e Name ' •kl11227a043 " Sampte ID ' "(SLPl0-01-02-24-100 " Fia : •klll227a.wi r Pea k Name ' 'PFHS - Mass(es} ' -399.000/99.00 0 Da,399.000/80.00 0 Da " Commen t -DAL-GW-133L-RB- * Annotation ' ~

7500
- 7000
-

Smoothin g Wi t R T Window : Expecte dBT : 6000
- 5500
- SOOO
4500
- 4000
- 3500
- 3000
- 2500
- 2000
-

15. 5 ia. 0 

# I Sampte Name:'k111227a046 - Sampl e ID:-GLP10-01-02-24-096 - Fil e Pea k Name . "PFHS ' Mas£(es } -399.000/99.00 0 Da.39g.000/80.00 0 Da Comment , "DAL-GW-TRIPOl-MS- ' Annotation ' ~ Sampl e Index ' 4 6 Sampl e Type : Unknow n 18. 5

Pro c Algor i Specif y 5 0 indow : l. C Peak-Split . Factor ; Repor t Larges t

Peak Hin . Pea

k Height : Min . Pea

k width : Sxpocto dRT : Us e Relativ e Retentio n Ti n IT : N o Valle y ! . H. 4 1475945 0 ( 2.516*00 6 14. 2 

# I Sampte Name : *kl11227a049 " Sampte ID : 'GL P 1041-02-24-001 ' Fie : Pea k Name , "PFHS - Mass(es ) '399.000/99.00 0 Da,399,000/80.00 0 Da ' Commen t •DAL-GW-130R-*- * Annotation : ~ Sampl e Index ; 4 9 sampl e Typ e ng/ r Modified : Proc . Algorithn : S ] Nois e Percentage ; Base . Sub . window ; Peak-Split . Facto r Hin . Pea

k Height : Min . Pea

k Hldth ; Smoothin g Hldth :

15, 5 18. 0 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 1 o f 2 7 Pag e 5 9 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

Sampte Name , "kl l 12Z7a056 " Sampte I D "GL P 1041-02-24-004 " File , -k111227a.»« r I Pea k Name . TFH5 " Massfes) : -399.000/99.00 0 Da ,399.000/80.00 0 Da ' Comment,-DAL-GW-130S.O- - Annotetio n - Sampl e Index : 5 6 Sampl e Typ e N/ A 25. 8 ';17:5 2 / Modified; Yes Proc. Algorithm: Specify Pars Noise Percentage; 50 Base. Sub. Window; 1.00 Peak-Split. Factor; 3 Report Largest Peak; Yas Min. PeakHeight: 0.00 Min. PeakHldth; 0.00 Smoothingwidth; 3 RT Window30.0 at

Int . Type : Retentio n 1 Height : Manua l

i e ; 14 . l 215446 3 c <

14. 0 14. 5 rSampteNam e •kl11227a059 " Sampt e ID . "GLP10-01-02-24-007 " Fie,-kl11227a.wtf r

• Pe n 8:19:5 1 A M •ithm : Specif yPa i Peak-Split . Factor : Pepor t Larges t Peak : Hin . Pea k Height : Mi n Pea k Width ; Smoothin g width : R T Window : I C ielat J i BT :



# I Sampte Name : "k l 11227a062 " Sampte ID : "(JLP10-01-02-24-010 " Fito Pea k Name : TFHS * Massfes) : -399.000/99.00 0 Da,399.000/80.00 0 Da Commen t "D/U.-<JW-131R-<K " Annotation' -

, Window ; L . Facto i Larges t Peak : Min . Pea k Height ; Min . Pea k Width . Smoothin g Width : R T Kindow :

• Relat I 1 RT ; ! RT : 

# I Sampt e Name : •k11!227b069 " Sampt e ID : "GLPICKI1-02-24-013 " Fie : -k111227b.wt r Pea k Nam e -pFHS " Mass(es ) "399.000/99.00 0 Da,399.000/e0.00 0 Da ' Commen t "DAL-GW-131S-0- " Annotatio n " Sampl e Index : 5 Sampl e Type : Unknow n Concentration . tl/ A Calculate d Cone ; 4.8 6 ng/mL Acq . Date ; 12/29/201 1

: Larges t Pea k

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 2 o f 2 7 Pag e 6 0 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

m SampteName''k111227b072 - Sampte ID.-GL P lOJ]1-02-24-016 " •Pea k Name - "PFHS " Mass(es) . "399.000/99.00 0 Da,399.000/80.00 0 Da ' m Comment'"DAL-GW-ISIL-O- " Annotation. - •k111227b.wt r

•Type : N/ A

. Algorithm : Specif yPar a ! Percentage ' 5 0

. Sub Window : 1.0 0 -Split . Factor ; 2

- t Larges t Peak : Ye s Pea k Height
- 0 0 0 Pea k Hldth ; 0 0 0 2.4e 5 2.3e 5 2. 2 65 2. 1 e5 - 2.0e 5 1.9e5 ' 1.8e5 ' 1.7e5 1.&e5 - 1.5e5 1.4e5 ' 1.3e5 - 1Je 5 1.1e5 ' 1.0e5 ' 9.0e4 ' 8.0M ' 7.0e4 - 6.0*4 - 5.0»4 - 4.0e4 - 3.0*4 - 2.0e4 ' 1.0*4 - 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 

# I Sampte Name . •k111227b075 - Sampt e ID:-GLP10-01-02-24-019 " Fie " "k111227b.wi( r Pea k Name . 'PFHS " Mass(es ) "399.000/99.00 0 Da,399.000/80.00 0 Da " Commen t "DAL-GW-133R-0- - Annotatx m -

irithn : Specif y Pa i window ; 1.0 0

Smoothin g width ; R T Window : Expecte dRT : Us e Relativ e RT . Height : Star t Tim e En dTine :



# I Sampte Name : *k111227b082 " Sanvfi e ID ' Pea k Name . -PFHS ' Mass(es) . Comment."DAL-GW-ISSS-O- ' Annotation ' Sampl e Index : 1 8 sampl e Type - Unknow n Calculate dCone : 80. 2 ng/mL Sampte Name : "k l 112271)085 ' Sampt e ID : 'GL P 10J31-02-24-025 ' Fi e Pea k Name . 'PFHS " Ma»5(Bs) : '399.000/99.00 0 Da.399.000/80.00 0 Da ' Commen L •DAL-GW-133L-0- * Annotatian. " Sampl e Index : 2 1 Sarjpl e Type ' Unknow n

Dat a printe d b yST W Thursday , Januar y26 , Pag e 1 3 o f 2 7 Pag e 6 1 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

I SampteNam e -k111227b08e - Sampte ID'•GLP10-01-02-24-028 ' File . •k111227b.wt r Pea k Nam* . "PFHS ' Mass{ss) ' '399.000/99.00 0 Da,399.000/80.00 0 Da ' I Commen t TJAL-GW-134R-*- - Annotatio o ~
Calculate dCone : 559 . Acq . Date : 12/29/2 1 Ac g Tine ; 5;43;0 1

Min . Pea

k Height : Min . Pea

k Width : Sooothm g width :

. Type : Manua l intto nTime ; 14. 7 i : 462309 2 c i

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

# I Sampt e Name , "k l n227b095 " Sampt e I D Pea k Name,-PFHS - Mas«(as ) '399.000/99 , Commen t •DAL-GW-134&.0- " Annotation : - Sampl e Index : 3 1 Sampl e Type ; Unknow n Calculate dCone : 4.1 8 Acq . Date : 12/29/201 1 Acg . Tine ; 8:07-2 9 P M

lOthin g Width : 5.0O 5 4.8e 5 4.6e 5 4.4« 5 4.28 5 4.0e 5 3.8e 5 3.6e 5 3.4« 5 3.2e 5 3.0e 5 2.ae 5 2.8e 5 2.4e S 2.2e 5 2.0o 5 1.8e5 1.6e5

8.0e 4 6.0e 4 4.0e 4 2.0* 4 

## [ Sampte Name : 'k l 11227b098 - Sampt e ID ; Pea k Name : 'PFHS ' Mass(es) : •399.f" " ' Comment : "DAL-GW-mL-O- - Annotation , Sampt e Nam* : "k l 11227b101 " Sampl e ID ' "GLP I &<I1-02-24-03 rFi e Pea k Name . "PFHS - Masa(es) - '399.000/99.00 0 Da.399.000/30.00 0 Da Commen t "DAL-GW-ISSR-^J. " Annotation : ~ Sampl e Index : 3 7 Sampl e Type : Unknow n

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 4 o f 2 7 Pag e 6 2 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 *ETS-Kir k Result s Name : klll227a.rd b 

# r Sampte Name , "k l 11227 b 108 ' Sampt e ID . 'GLP10-01-02-24-040 - Fite * "k111227 b Pea k Name ' TFHS " Massfes) : "399.000»9.00 0 Da.399.000/80.00 0 Da Commen t "DAL-GW-ISSS-O- - Annotation: " Sampl e Index : 4 4 Saopl e Type ; Unknow n Concentration ; N/A Calculate d Cone : 7.7 8 ng/mL Acq . Date - 12/30/201 1 Acq . Time
- 12:35:5 0 A M

.-Split . Factor : >r t Larges t Peak : Pea k Height ; Pea k Width :

Height : Star t Ti l En d Tim e 9.0* 5 e.5e 5 e.0e 5 7.5* 5 7.0e 5 6.5e 5 6.0e 5 5.5* 5 S.0e 5 1 4.5* 5 4.0e S 3.5* 5 3.0* 5 2.5* 5 2.O0 S 1.5* 5 1.0* 5 5.0* 4 3. 5 14. 0 14, 5 15. 0 15. 5 16. 0 16. 5 

# I Sampt e Name''k111227bl11 - Sampte ID.-GLPIOfll-02-24-043 ' Fie-"kl l 1227b . Pea k Nam* ' "PFHS * Mass(*s) , "399.000/99.00 0 Da,399.000/80.00 0 Da Commen t "DAL-GW-135L-(^ " Annotation . - Sampl e Index ; 4 7 Sampl e Type : Unknow n Concentration : ll/ A Calculate dCone ; 47. 2 ng/m L Acq . Date : 12/30/201 1 Acq . Tine : 1:37;4 8 A H

: Larges t

Peak : Smoothin g Width : R T Window : Expecte dRT ; Us e Relativ e BT ;

le : 14. e nl n 391194 0 count s 5.6S e + O0

5 cp s



# I Sampte Name ' *k111227b114 ' Sampt e ID ' "GLP10-01-02-24-049 ' Fito . -k l 11227b,wi r Pea k Name , "PFHS " Ma3S(es) : '399.000/99.00 0 Da,399.000/80.00 0 Da Comment , •DAL-GW-136S-0. - Annotation: - Sampl e Index : 5 0 sampl e T-yp

e - Unknow n Concentration : N/ A Calculate d Cone : 11. E ng/n L Acq . Date : 12/30/201 1 Acq . Time : 2:39:4 4 A M Modified : Ye s Proc . Algorithm : Specif yPa . Nois e Percentage ; 5 0 Base . Sub . Nindew : 1.0 0 Peak-Split . Factor ; 2 Repor t Larges t Peak ; Ye s Hin . Pea k Height . 0.0 0 Min . Pea k Width ; 0.0 0 Smoothin g Width ; 3 R T Window : 3 0 0 Expecte d RT - 14. ' 

# I SampleNarrw-k111227b12 rSampte ID''GLP10-01-02-24-052 " Fie : Pea k Name : 'PFHS ' Ma5s(e4) , "399.000/99.00 0 Da,399.000/B0.00 0 Da Comment:-DAL-GW-136L-0- * Annotatio n " Sampl e Index : 5 7 Sampl e Type ; Unknow n Concentration : N/ A Calculate d Cone : 12. 3 ng/m L Acq . Date : 12/30/201 1

. Tim « 14 ;17 I Modified : Ye s Pro c Algorithm ; Specif y Paramet i Nois e Percentage : 5 0 Base . Sub . Window : 1.0 0 mi n Peak-Split . Factor : 2 Repor t Larges t

Peak ; Ye s

i t . Type : Manua l ea : 103169 7 c i

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 5 o f 2 7 Pag e 6 3 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I Sani[teName.-k111227b124 - Samff a ID:-GLP1CMH.02-24-058 - Fil e -k111227b.wi r Pea k Nam* . -PFHS " Mass(BS) : '399.000/99.00 0 Da,399.00fl/80.00 0 Da " Comni«nt.-OAL.CW.137S^ - AanotaUofi , - Sampl e Index . 60 Sampl e Type ; Unknown Calculate dCone . 0.12 5 ng/m L Ac qDate ; 12/30/201 1 Acq . Time : 6:0S;1 5 A H 1.5* 4 1.4*4 Modified ; tl o Proc . Algorithra : Specif y Parameter s Nois e Percentage
- 5 0 - M O II I 1.3*4 Base . Sub . window : 1.0 0 mi n Peak-Split . Factor ; 2 Repor t Larges t

Peek : Ye s Hin . Pea

k Height : 0.0 0 cp s Hin . Pea

k width : 0.0 0 se e Sooothin g Width : 3 poi n R T Window ; 30. 0 se c Expecte dRT ; 14. 4 mi n Us e Relativ e RT ; H o Int . Type ; Valle y Retentio nTime : 14. 6 mi n Area ; 109B9 7 count s 1.2*4 1.1*4 1.0*4 9000. 0 &

" 8000. 0 £ • Height ; 1.52e»00 4 cp s 1.2*4 1.1*4 1.0*4 9000. 0 &

" 8000. 0 £ • 1 7000. 0 6000. 0 50O0. 0 4000. 0 3000. 0 2000. 0 1000. 0 

# J

Ll5^ 5 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 

# I Sampt e Name , 'kl11227b127 - Sampte ID ' -GL P 10-01-02-2 < Pea k Name - -PFHS - MaSE(Bs) : -399.000/99.00 0 Da,399.0r ' Commen t -DAL-GW-137L-0- - Sampl e Index : 6 3 Sampl e Type : Unknow n Calculate dCone : 0.10 ^ Acq . Date : 12/30/201 1 Acq . Time ; 7:0 8 ;1 4 A H Proc . Algorithm : Specif y Kois e Percentage : 5 0 Baae . Sub . Uindow ; I.O i Peak-Spilt . Factor ; 2 Repor t Larges t

Peak : Ye : Hin . Pea

k Height : O. i Kin . Pea

k width : O. i Smoothin g Width : 3 R T Window : 30. 0 Us e Relativ e RT ; ll o Type ; l a l 9000. 0 8500. 0 8000. 0 g 7500.0
- ^ 7000. 0 I6500. 0

- 6000. 0 5500. 0 5000.0
- 4500.0
- 4000. 0 3500.0
- 3000.0
- 2500.0
- 2000.0
- 1500.0 - 1000.0 - 500.0 - coistW . 1.0 5 L i 5.0 9

12. 0 13. 5 14. 0 14. 5 15. 0 15. 5 18. 0 16. 5 

# I Sampte Natne : 'k l 11227bl34 - Sampte ID : 'GLP1041-02-24-064 ' Rte Pea k Nam* ' -pFHS ' Man(es) : -399.000/99.00 0 Da,399.000/80.00 0 Da ' Comment : "DAL-GW-138R-(V ' Annotation ' ~ Sampl e Index : 7 0 Sampl e Type ; Unknown Calculate dCon e Acq . Time ; Modified :

Smoothin g I R T Window : 12/30/201 1

9;32.5' i A

H Ye s Specif y Par i SampteName'-kl11227b13 rSampte ID''GLP1OO1-02- Z Pea k Nam e 'PFHS ' Mass[es) ' -399.000/99.00 0 Da.39g.0C Commeni:'DAL-GW-138S-(^- ' /\nnoiatton: " Sampl e T>-pe : Calculate dCone : Modifie dVe s Proc . Algorithm : Specif y Par a Nois e Percentage ; 5 0 Base . Sub . window ; 1.0 0 Peak-Split . Factor : 2 Repor t Larges t

Peak ; Ve s Hin . Pea

k Height : 0.0 0 Hin . Pea

k Width : O.O

O Smoothin g width ; 3 R T Window : 30. 0 s e Expecte dRT ; li. 4 mi Us e Relativ e RT ; tl o In LType ; Manua l 2.20 5 2.1e5 ' 2.0e5 '

1.7e5 - 1.6*5 -

Height ; Star t Ti l En dTim e 9.0* 4 e,0e 4 7.0e 4 6.0e 4 5.0* 4 4,0* 4 3.0* 4 2.0* 4 1.0* 4 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 6 o f 2 7 Pag e 6 4 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

Peak-Split . I Repor t Large ! Min . Pea

k He i Min . Pea

k width ; R T Windo *

1 RT : 

# I Sampt

e Name . 'kl11227b140 ' Sempt e ID , 'GLPI001-02-24-070
- Fite : 'k l 11227b.wtf r Pea k Name . 'PFHS ' Massfes) : '399.000/99.00 0 Da,399.000«0.00 0 Da
Comment.-DAL-GW-mL-O-
- AnnotalK W- Sampl e Index : 7 6 Sampl e Typo ; Unknow n Concentration ; H/A Calculate dCone : 0.063 0 ng/m L Acq . Date ; 12/30/201 1 800 0 Acq . Time : 11:36:5 7 A M Hoaiii.d , Proc . Algorithm : Specif yParameter s - M O II I Nois e Percentage : 5 0 7000 . " 0 mi n s 650 0 0 0 se e 6000 , point s i..i n5500
- 500 0 ount s & 4500
- m^ n 1 <000

- 350 0 3000
- 2500
- 2000
- 1500
- 1000
- ! Rela i

i l,15.2 7 15.7 6 

# I SampteName -k l 11227bl47
- Sampt e ID'•GLP10-01-02-24-073 ' Fie.-k111227b.wif r Pea k Nam e 'PFHS ' Mass(es ] "399.000/99.00 0 Da,399.000/80.00 0 Da ' Co(nm*n t

"DAL-GW-mR-O- ' Annotation ' " Sampl e Index ; 8 3 Sampl e Type : Unknow n Concentration ; ll/ A Calculate dCone ; 13. 9 ng/m L

rithra ; Specif y Pa i Base . Sub . Windo w Peak-Split . Facto : Repor t Larges t

Pei Min . Pea

k Height : Min . Pea

k Hidth . Smoothin g Width :



# I Sampt

e Name : •kl11227b150 ' Samfi e ID : 'GL P1001-02-24-076
- Rte ' "k111227b.wif r Pea k Name : 'PFHS ' Mass(es) : '399.000/99.00 0 Da,399,000/80.00 0 Da
Comment:-DAL-GW-WIR-O- ' Annotation,
- Sampl e Index : 8 6 Sampl e Type
- Unknow n Concen t

1atlon ; N/ A Calculate dCone : 0.25 9 ng/m L Acq . Date ; 12/30/201 1 Acq . Tine ; 3:03;4 1 P H Modified : Ye s Proc . Algorithm : Specif y Paramet t Hois e Percentage ; 5 0 Base . Sub . Window ; 1.0 0 mi n Peak-Split . Factor ; 2 Repor t Larges t

Peak ; Ye s Min . Pea

k Mldth ; 0.0 0 se t

Height : Star t 1 En dTi n 3.4* 4 3.2* 4 3.0* 4 2.8e 4 2.6* 4 2.4* 4 2.2* 4 2.0* 4 1.6* 4 1.6* 4 1.4*4
- I5e 4 1.0e 4 8000.0
- 6000.0
- 4000.0
- 2000.0
- 0. 0 

# I Sampt o Name : 'k1l1227bl53 ' Sampt e ID ' -GLP1001-02- : Pea k Name , 'PFHS ' Ma&s(«s ) '39 9 000/9 9 00 0 Da.399.0 C Commen t

•D/U.-GW-142R-0- * /SjinotaBo n - Sampl e Index ; 8 9 Sampl e Type ; Unknow n Calcul i 10. 2 ng/m L

Proc . Algor i
Pea l NOl !
Min . Pea

k Heigh t Min . Peak

Width ; Smoothin g Hidth : R T Hindow ; in : Specif y Par ;

:age : 5 0

iRela t

En dTine : ! RT :

14.9 9



# _ft

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 7 o f 2 7 Pag e 6 5 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•SampteNam9:-k111227t)160 ' Sampte lD"GLP10-01-02-24-082 " File*•k111227b.viffl - •Pea k Name : 'PFHS - Mass(as} ' -399.000/99.00 0 Da,399.000/80.00 0 Da ' •Comment : •OAL-GW-143R-*- * Annotation' - Sample Index; 96 Sanple Type: Unknown Concentration: ll/A

i f yPa i 5 0 1.0 0

Us e Relativ f Int . Type ; 2.91e*00 4

4000. 0 20O0.O12. 0 12. 5 13. 5 14. 0 

# I SampteName:-k111227b163 - Sampte I D * G LP10-01-02-24-085 ' Fie : Pea k Name , 'PFHS ' Mass{es) : '399.000/99.00 0 Da.399.000/B0.00 0 Da ' Commen c'0AL-GW-144R-0- - Annotation : ~ Sanpl e Index : 9 9 Sampl e Typ e Il/ A ng/m L Mod i fled : Proc . Algorithm Nois e Percentage : Base . Sub . Windo

v Peak-Spilt . Fact e Repor tLarges tP

( Min . Pea

kHeight Min . PeakWidth : Smoothin g width : R T Window : Expecte d RT :



# I Sampte Nam* : *k l 11227a018 * Sampte ID : '11012-10-9 * Fite : "k l 11227 a wifT Pea k Name : 'PFOS - Mass(*s) . -499.000/90.00 0 Da.499.000/99.00 0 Da.499.000/130.00 0 Da ' Comment . "2. 5 ng/m L F

C std i n Mil S O Water ' Annotation , " Sampl e Index : I S

Hoi ! Per < itage :

lindo w Specif yParamet i Base . Sub Poak-Spli ' Repor t Larges t Pe . Hin . Pea k Height : Mill . Pea k width : Smoothin g Hldth : R T Window
1 RT ; ; RT : 

# I Sampto Name ' It l 11227a028 ' SiBiipt e ID : 'Solven t Blank ' Fl* : 'k l 11227a.wlt r P*a k Ham t TFOS ' Mass<es) "499.000/80.00 0 Da.499.000/99.00 0 Da.499.000/130.00 0 Da ' Common L "MK i Q Wate rTN I l-043 rAnnolatte n " Concentration ; Calculate d Cone ;

. Window : • . Factor : Smoothin g Ml

c R T Window : Us e Relativ e

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 8 o f 2 7 Pag e 6 6 of11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•SampteName . "kl l 1227a029 " SamptelD.TCS-111221-4 " Fit e •kl11227a.wrt r I Pea k Name . "PFOS " Mass(*s ) -499.000/80.00 0 Da,499.OO0/99.OO 0 Da.499.000/130.00 0 Da " •Comment ' *0.5pp b LCS " Annotation , - Sampl e Index : 2 9 Saopl e Type ; Q C Concentration ; 0.46 2 ng/m L Calculate d Cone : 0.39 5 ng/m L Acq . Date ; 12/27/201 1 Acq . TI P 9:59:5 8 P M Ye s Proc . Algorithm : Specif yPar ; Kois e Percentage ; 5 0 Base . Sub . Window ; 1.0 0 Peak-Split . Factor : i Repor t Larges t Peak ' Ye s Kin . Pea k Height ; 0.0 0 Min. Peakwidth; 0.00 SmoothingWidth; 3 RT Hindow: 30.0 si Expecte d RT : IS. 4 m i Us e Relativ e RT ; K o In tTyp e Tine : 15. 3

42066 4 c

<

14. 5 15. 0 15. 5 16. 0 16. 5 1 7 0 17. 5 

# I Sampte Name'•k111227a032 - Sampte ID'TCS-111221-7 " Fle."k111227a.wif r Pea k Name ' 'PFOS * Mass(es) ' "499.000/80.00 0 D a ,499.000/99.00 0 Da.499.000/130.00 0 Da " Commen t "Spp b LCS " Annotation : - Sampl e Index ; 3 2 Sampl o Type ; O C Concentration : 4.6 2 ng/n L Calculate d Cone ; 5.I B ng/m L Acq . Date : 12/27/201 1 Acq . Tine : 11-01:5 7 P M

Base . Sub . Window : Peak-Split . Facto i Repor tLarges tPe ; Hin . PeakHeight ' lln . Pea kWidth ; R T Wind t

le : 15. 3

517351 7 e

t

4. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 I Sampte Name''k111227a035 " SamptelD'-LCS-l11221-lO - File : "M l 1227a . Pea k Name . -PFOS - Mass{es ) -499.000/SO.OO O Da.499.000/99.00 0 Da,499.000/130.00 0 Da ' I Commeni , *30pp b LCS ' Annotation : - 2 3. 2 ng/m L 12/28/201 1 12;03;5 5 A

H Algo l ! Perc i Ho i Base . Sub . window : Peak-Split . Factor : Repor tLarges tPeak ; Hin . PeakHeight : Min . Peakwidth ; Smoothin g Width ; BT Hindow ; Expe c Us e Rela t Int . Type ;

iRT. ! RT ;
3.27e+00 6 I Sampte Name.-kil l 227a042 - Sampte ID-GLP1CM)1-02-Z4-099 " Fie: * Pea k Nam e -PFOS * Mass(es ) '499.000/80.00 0 Da,499.000/39.00 0 Da,4 : I Commen t •DAL-GW-140R-RB- " Annotatio n - Sampl e Type :

Smoothin g Hidth : R T Window : Expecte d RT ; Us e Relativ e BT : Int . Type ; Area . Height : 2.6* 4 2.5* 4 2.4e 4 2.3a4 2.2e 4 2.1* 4 2.0* 4 1.9*4 - 1.8* 4 1.7* 4 1.6*4 - 1.5*4 -

- 1.4*4 - 1.3*4 - 1.2* 4 1.1*4 - 1.0*4 - 9000.0 - eooo.0 - 7000. 0 6000. 0 5000.0 - 4000.0 - 3000.0 - 2000.0 - 10OO.0 - 0. 0 15.3 2 J 17.0 8

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 1 9 o f 27 Pag e 6 7 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•SampteNam*:'k111227a043 ' Sampte ID:'GLP10^1-02-24-100 ' Fil e •k111227a.¥ ^ •P*8 k Name : TFOS ' Mass(**) ' '499.000^0.00 0 Da,499.000/99.00 0 Da,499.000/130.00 0 Da I CofTMii*nt.-DAL-GW-133L-RB- " Amotatwn . " Sampl e Index : Sampl e Type ; Concentration : Calculate dCone ; H/ A

1 . Hindow : t . Factor : itqes t Peak '

Hanua l 1 5 3 1246 0 c t 2.3* 4 2.2* 4 2.1*4
- 2.0*4
-

1.7* 4 1.6* 4 1.5*4
- 1.4* 4 1.3*4
- 12*4
- 1.1*4
- 1.0*4
- 9000. 0 8000. 0 7000.0
- 6000. 0 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 

# I SampteNam e •kll12278046 - Sampte I D 'GLP10-01-02-24-096 ' Fie,-k111227a.w1f P Pea k Nam * -PFOS - Mass{es) ' '499.000/80.00 0 Da,499.000/99.00 0 Da,499.000/130.00 0 Da Comm*n t -DAL-GW-TRIPOl-MS- ' Annotatio n " Sampl e Index ; 4 6 Sampl e Type : Unknow n ng/m L
Hodified ; Ye s Proc . Algorithm ; Specif y: Mois e Percentage : 5 0

Pea k Height : Sinoothin g Wi c R T Hindow ; Expecte dRT : 2.5*6 - 2.4e6 - 2.3e S 2.2e 6 2.1e6 - 2.0*6 - 1.9* 6 1.ee6 ' 1.7*6 - 1.6* 6 1.5* 6 1.4* 6 1J« 6 1Je 6 1.1e 6 1.0e 6 9.0* 5 8.0* 5 7.0e 5 6.0e 5 5.0e 5 4.0* 5 3.0e 5 2.0e 5
14. 5 15. 0 15. 5 16. 0 1B. 5 17. 0 17. 5 

# I SampteNam e 'kl11227a049 ' Sampte ID''GLP10^1-02-24-001 ' FIto : Pea k Nam e 'PFOS ' Massfes) : -499.000/80.00 0 Da,499.000/99.00 0 Da. ' Commen t -DAL-GW-ISOR-O- ' Annotation ' ~ Sanpl e Index ; 1 9 Sampl e Type ; Unknow n Concentration ; N/ A Calculate d Cone ; 444 . ng/m L Acq . Date : 12/2B/201 1 

# I Sampl e Name ' T d 11227a056 ' Sampt e ID : *GLP10-01-02-24-004 ' Fie : 'k l 11227a.wi r Pea k Nam e -PFOS " Massfes) . "499.000/80.00 0 Da,499.000/99.00 0 Da,499.000/130.00 0 Da Commen t "DAL-GW-ISOS-O- - Annotation . -

Acq . Tine ; 4:53;1 '

It. lypt-^ 3.6* 5 3.4* 5 32e 5 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0* 5 1.6* 5 1.6* 5 1.4* 5 12* 5 1.0* 5 8.0* 4 6.0* 4 4.0* 4 2.0* 4 12/28/201 1

Sub . Window ;

- t Larges t Peak : Pea k Height ; Smoothin g Wid I R T Hindow : Expecte d RT Manua l

l e ; 15. 2 856724 3 c <


# m i 7.0*5
- 6.5e5
- 6.0e5
- 5.5e5 - 5.0*5
- 4.5*5
- 4.0e5
- 3.5e5
- 3.0eS
2.5*5
- 2.0*5
- 1.5*5
- 1.0*5
- 5.0*4
- 13. 0 13. 5 14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 2 0 o f 2 7 Pag e 6 8 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS . an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 *ETS-Kir k Result s Name : klll227a.rd b 

# I Sampt e Name , "k l 11227*059 " Sempt e ID : "GL P 1001-02-24-007 " File ' "k111227 a wt r Pea k Name : "PFOS " Mass(es) . "499.000/80.00 0 Da.499.000/99.00 0 Da,499.000/130.00 0 Da Commen t "DAL-GW-130L-O- - Annotation : - Sampl e Index : 5 9 Sampl e Type ; Unknow n Concentration ; M/ A Calculate d Cone : 65. 8 ng/mL

Proc . Algorithm : Specif yPar s Repor t Larges t P

e Hin . Pea k width : Smoothin g Hldth : R T Window
Expecte d RT : Us e Relativ e RT ;

14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Algorithm
- Spe c Baae . Sub . Hind i Kin . Pea k Height
Min , Pea k Width . Smoothin g Width . R T Hindow : i f yPar a 5 0 1.0 0 

# I SampteName:H111227a062 - Sampte ID.•GLPlO-01-02-24-010 - Fi e " I Pea k Nam e "PFOS " Mass(es ) "499.000/80.00 0 Da,499.000/99.00 0 Da,4S Commen t 'DAL-GW-iaiR-O- " Annotttion. - Sanpl e Index : 62 1.10* 6 1.05e 6 1.00e 6 9.50e 5 9.00* 5 150* 5 8.00* 5 7.50* 5 7.00* 5 6.50* 5 6.00e 5 5.50* 5 5.00* 5 4.50* 5 4,00* 5 3.50* 5 3.00* 5 2.50* 5 2,00* 5 1.50* 5 I.OOe S 5.00* 4 0.0 0 Manua l lb. 2 1346618 5 <

14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5

IPe n itage :

; Specif y ParatneC

Int . Type ; Retentio n1 Area : Star t Time : EndTims ; :plit . factor ;

. Larges t

Peak : 'ea k Height
- '«a k Hidth : lin g Width ; idow : 3 ( 1 RT ; 1 

# I Sampt e Name ' "k l 11227b069 " Sampte ID : "GLP10-01-02-24-013 ' FIto: ' Pea k Nam* ' -pFOS ' Mass(»s) . '499.000/80.00 0 Da.499.OO(V99.O0 0 Da,4 < Commen t "DAL-GW-ISIS-O- - Annotation. " Sampl e Index ; S Sanpl e Type : Unknow n 5.0* 4 4.8* 4 4.6* 4 4.4* 4 4.2* 4 4.0e 4 3.6* 4 3.6* 4 3.4*4 - 3.2* 4 3.0* 4 2.8* 4 2.5* 4 2.4* 4 2.2* 4 2.0* 4 1.B M 1.6* 4 1.4* 4 1.2* 4 1.0* 4 8000. 0 SampteNamB:"M11227b07 rSampte ID:-GLPlOO1-02-24-016 - Fie : •k111227b.wt r Pea k Nam* . TFOS ' Mass(ea ) "499.000/80.00 0 Da ,499.000/99.00 0 Oa.499.000/130.00 0 Da Comment;-DAL-GW-131L-0- ' AnnolaBon: - Sampl e Index : 8 Sampl e Type ; Unknow n Calcula t 28. 0 n ^ 12/29/201 1 12:12:4 3 P

M Algorithm : Specif yPar s

Smoothin g Hidth ; 3 R T Hindow ; 30. 0 Expecte d RT ; 15. 4 Us e Relativ e RT : ll o Int . Type ; Manua l Retentio n Time : 15. 5 Area : 2S1912 B c t Height : 2.96e*00 5

-.15.6 8 2.8*5
- 2.6*5
- 2.4eS
2.2*5
- 2.0*5
- 1.8*5
- g - 1.6*5
- g 1.4*5
- 15e5
- l.OeS
8.0* 4 6.0* 4

Dat a printe d b yST W Thursday , Januar y26 , Pag e 2 1 o f 2 7 Pag e 6 9 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

•Sampte Nam* : -k l 11227b075 " Sampte ID : - ( •P*B k Nam* : -PFOS - M3SS(*£) - -499.0DO/80.D ( I Comm*n t T>AL-GW-133R-t^- - Annotation' " Sanpl e InJex : 1 1 Saapl e Type : N/ A Calculate d Cone ; 41. 1 Acq . Date : 12/29/201 1 Acq , Time : 1;14:4 0 P ^

Smoothin g wtd l R T Window : Expecte d RT : ng/ r

Hanua l 15. 5 1116483 CO

L 3.77e-fO0 S 3.6* 5 3.4* 5 3.2* 5 3.0* 5 2.8* 5 2.6* 5 2A« 5 2.2* 5 2.0* 5

1.2*5 - 1.0*5 - eo»4 > 60e 4 4,0* 4 2.0*4 - 14, 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 

# I Sampte Name : 'K1l1227b082 - Sampte ID , - < Pea k Nam e 'PFOS - Mass(es):'499.000/8 0 Comment : •DAL-GW-133S-0- ' Annotatio n ' Sampl e Index ; I B Sampl e Type : Unknow n Concentration ; ll/ A Calculate d Cone : 176 . ng/n L Acq . Date ; 12/29/201 1 Acq . Tine : 3:39:0 8 P H Hodified ; Ye s

Ki nPea kHeight : Hin . Pea kHldth ; Smoothin g Hidth ; R T Window1.6e 6 1.5e6 1.4e 6 1.3e 6 1.2e 6 1.1e6 1.0*6 § •9.0e 5 t 1 6.0* 5 7.0e 5 6.0e 5 5.0* 5 4.0* 5 3.0* 5 2.0e5 1.0e 5 14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 

# I Sampte Name : "k l 11227b085 - Sampte ID : - i Pea k Name : TFOS - Massfes ) -499.000^80.0 1 Comment : "DAL-GW-133L-(V " Annotation . ampl e Index : 2 1

. Algorithm : :

. Sub . Window ; 

# I Sampt e Nam* : "V l 11227t>088 " Sampte ID ' " i Pea k Nam e "PFOS " Mass(es ) "499.000/80.0 1 Commen L -OAL-GW.134R.O- ' Annotation : - Sampl e Index : 2 4

Smoothin g Hid ! R T Hindow ; Expecte d RT ;
Height . Star tTim e En d Tlma : 9.0* 5 8.0* 5 7.0* 5 6,0* 5 5.0* 5 4.0e5 3.0* 5 2.0* 5 1.0*5 Hoi : Per t Baae . Su l Repor tL t Factor ;

S tPeak : Hin . Pea kHidth ; Smoothin g Hldth : R T Hindow ; 3 C iRela l ! RT :

1.42e+00 6 cp s

,33^ ^ 1.3e6 - 1.2e6 - 1.1*6 - 1.0*6 - 9.0e5 - 8.0eS 7.0e 5 6.0e 5 5.0e5 - 4.0*5 - 3.0*5 - 2.0e5 -

4. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Thursday , Januar y26 , Pag e 2 2 o f 2 7 Pag e 7 0 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b

• Sampt

e Nam* ' 'k l 11227b095 ' Sampt e ID : 'GL P1001-02-24-031 ' Rte ' "k l 11227 b w4 r IP*B k Nam* . 'PFOS
- Mass(*f) : -499.000/8a00 0 Da.499,000/99.00 0 Da.499.000/130.00 0 Da ' • Commen

t "DAL-GW-134S-0-
- Annotatto n - Sampl e Index ; 3 1 Sampl e Type : Unknow r H/A 17. 5

[-Split . Fact ;

. Pea k height : 1.5*6
- 1.4*6
- 1.3*6
- 1.2e6
- 1.1*6
- 1.0e6
- 9.0e5
- 8.0*5
- 7.0e5
-

4.0*5 - 3.0*5 -

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

# I Sampt e Nam* . T(111227ti098
- Sampt e ID : -GL P1(M)1-02-24-034 " Fte: I Pea k Nam* . "PFOS
- M8S5(*s) ' -499.000/80 ^ Da.499.000/g9.00 0 Oa,4 r Comm*nt : -DAL-GW-134L-^)-
- Annotatton * ~ Sanpl e Index : 3 4 Sampl e Type
- Unknow r Calc i o dCon

e ll/ A 4 32 . Modified ; Ye s Proc . Algorithm : Specif y Parj Base . Sub . window ; I.0 0 Peak-Split . Factor : 4 Repor t Larges t

Pea k Ye s Min . Pea

k Height
- 0.0 0 Hin . Peak

Hldth : 0.0 0 Smoothin g width ; 3 R T Window : 30. 0 a t Expecte dRT : 15. 4 m ] Us e Relativ e RT ; N o Int . Type ; Manua l Retentio n Time : 15. 6 m : Area : 432184 9 coun t Beight : 3.65B-*00 5 C [ Start Time: 15.1 lai End Time: 15.8ml 3.6*5 ' 3.4*5
- 3.2*5
- 3.0e5
- 2.8*5
- 2.6e5
- 2.4* 5 2.2e5
- 2.0*5
- 1.8*5
- 1.6*5
- 1.4*5
- 1.2*5
- 1.0e5
- 8.0e4
- 6.0*4
- 4.0*4
- 2.0*4
- 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 ISampteName--k11l227b101
- Samptel D " ! Pea k Nam*''PFOS
- Mass(es)''49 9 000/SO.O ( ICommeni "D/y.-GW-135ltO- ' Annotation:" '
alculate dCo

r

Peak-Split . Fflct t Mi nPea

k Height ; Min . Pea

k Hidth : Smoothin g Width : R T Hindow : Expecte dRT : Us e Relativ e RT ; Typo ; Rete r Area ; Height : Star t 1 En d Ti n .12e«00 6 cp s l.lOe e 1.05* 6 1.00e 6 9.60e 5 9.00* 5 8.50* 5 6.00* 5 7.50*5
- 7.00*5
- 6.50* 5 6.00*5
- 5.50*5
- 5.00*5
- 4.50e5
- 4.00*5
- 3.50*5
- 3.00*5
- 2.50©5
- 2.00*5
- 1.50*5
- LOOeS
5.00*4
- 0.00
- 

# I SampI * Name : 'k111227b108 ' Sampl e ID : 'GLP l 041-02-24-040 ' Fie ' ' I Pea k Nam e 'PFOS
- Mass(as) ' '499.000/8 0 000 Da,499.000/99.00 0 Da,4 9 Comman L''DAL-GW-135S.C
- Annotation' " Sampl e Index ; 4 4 4.8* 5 4.6* 5

, Algo ) : Perc < Moi ; Base . Sub . window ; Peak-Split . Facto r Repor t Larges t

Pe a Hin . Pea

k Height : Hin . Pea

k Width : Smoothin g width : R T Hindow :

1 RT ; Hanua l

558140 2 count s 4.92e'00 5 cp s 4.2* 5 4.0e 5 3.8* 5 3.6* 5 3.4*5
- 3.2* 5 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0eS
1.8e S 1.6e5
- 1.4e5
- 12e5
- 1.0*5
- 8.0* 4 6.0* 4

15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 TTm* . min 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 2 3 o f 2 7 Pag e 7 1 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 *ETS-Kir k Result s Name : klll227a.rd b 

# I SampteName:"kl11227b111 - Sempte I D •GLP10-01-02-24-043 * Fite'•k111227b.wrf P PeakNam e -PFOS * Massfes):'499.000/80.00 0 Da,499.000/9g.OOODa,499.000/130.00 0 Da ' Comment'XAL-GW-135L-a- ' Annotatio n ~ Sampl e Index : 4 7 inpl e Type ; Concentration : H/ A Calculate d Cone ; 32. 5 r Acq . Date ; 12/30/201 1 Ac qTime ' 1;37;4 8 A H lified : Nois e Per t

. Sub . :age :

Peak : Facto j Pepor t Larg i Hin . Pea k Height ; Hin . Pea k Hidth ; Smoothin g Hidth ; R T Window : Expecte d RT : Us e Relativ e RT ; 1.0 0 tnl n

15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 I Sampt e Name : -k1l1227b114 - Sampt e ID ' 'GLP10-01-02-24-049 ' Fi e •kl11227 b wffT I Pea k Nam * "PFOS " M3£S(BS) : "499.000/80.00 0 Da,499.000/99.00 0 Da,499.000/130.00 0 Da ' I Comment : •0AL-GW-136S-0- - Annoiabon: -



# I Sampte Nam* : 'k111227b12 rSampte ID'*GLPlCM)1-02-24-05 rRta:"k111227b.wfl r Pea k Name : "PFOS " Mas»(*s) : "499.000/80.00 0 Da.499.000/99.00 0 D».499J»0/130.00 0 Da Comment . "DAL-GW-ISeL-O- * AnnoUtion . "
Calculate d Cone ; 65. 3 r Acq . Date ; 12/30/201 1 Acq . Time ; 5:04:1 7 A M Modified : Ye s Proc . Algorithm ; Specif yPar a Nois e Percentage : 5 0 Base . Sub . Hindow ; 1.0 0 Peak-Split . Factor ; 4 Repor t Larges t Peak : Ye a Hin . Pea k Height : 0.0 0 Mm . Pea k Width : 0.0 0 Smoothin g Width : 3 R T Hindow ; 30. 0 s e

1 RT : ; RT :

6.32e->00 5 ep s 

# I Sampt e Name : "k l 11227bl24 " Sampte ID ' "GLP1001-02-24-058 " Fte . "k l 11227lJ.wt r Pea k Nam* ' -pFOS " Mass(es) : '499.000/80.00 0 Da,499.000.199.000 Oa.499.000/130.00 0 Da ' Conwnen t "DAL-GW-137S^>- " Annotation ; " Sampl e Index ; 6 0 Saapl e Type : Unknow n Concer n Calcul B Acq . Da i Acq . Ti n 0.587 6;0£:15 t ng/m

L

Proc . Algorithm ; Specif yPara n 1 Perc f Base . Sub . Hindow ; Peak-Split . Factor : Repor t Larges t Peak ; Min . Pea k Height ; Kin . Pea k Midth ; R T Hindow ; 3 1 Expecte d RT Us e Relativ e HT ; l Int . Type ; Ma i Retentio n Time . Area : 61191 : Height ; 6.II 1

5. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Thursday , Januar y26 , Pag e 24 o f 2 7 Pag e 7 2 of 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rcl b

Dat a printe d b yST

W Thursday , Januar y26 , 201 2 Pag e 2 5 o f 2 7 Pag e 7 3 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS . an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Result s Name : klll227a.rd b 

# I Sampl e Nam* . "kl11227t>14 rSampl * ID:-GLP10-01-02-24-073 ' File : •kll1227b.v« r Pea k Name : "PFOS " Mass(*s) : '499.000/80.0D O Da.499.000/99.00 0 Da,499.000/130.00 0 Da ' Comm*nI , "DAL-GW-1401^0- ' Armoiatxt n Sampl e Index : 8 3 Saapl e Typ e Calcula l H/ A

jrithm : Specif y Pa i

, Window ; 1.0 0 Min . Pea

k Hidth : Smoothin g width : R T Hindow : Manua l

le : 15. 3 997248 0 C

(

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

# I SampleNam e -kl11227bl50 ' Sampl e ID'"GLP10-01-02-2 ' Pea k Nam * 'PROS ' M3ss(es) ' "499.000/80.00 0 Da,499.0 r Comman t 'DAL-GW-141R-0- ' Anootatton: "

Algorithm
- Specif y Pa i

Smoothin g width : R T Hindow : Expecte dRT : 3.ae5 3.6e5
- 3.4*5
- 3.2*5
- 3.0*5
- 2.6* 5 2.6* 5 2.4e5
- 2.2eS
2.0e5
- 1.8* 5 1.6e 5 1.4*5
- 1J*5
- 1.0*5
- 60*4 ' 60*4 ' 4.0*4
- 2.0*4
- 14. 5 1 5 0 15. 5 16. 0 16. 5 17. 0 17. 5

Proc / Noise I irithm : Specif y Par ;

rentage : 5 0

. Window : 1.0 0

Smoothin g width ; R T Hindow : Expecte dRT ; 

# I Sampl e Nam* : "kl l 1227b153 ' Sampl e ID : *GLP 1 CM]1-02-24-079 ' File : ' I Pea k Name . TFOS ' Mass{*s) : •499.000«0.00 0 Da,499.000i'M.OOO Da.4S Commeni : •DAL-GW-142R-0- * Annotation . " * Sampl e Index : S9 1.10* 6 1.05* 6 1.00* 6 9.50* 5 9.00* 5 B.50* 5 S.00eS 7.50* 5 7.00* 5 6.50* 5 e.00e S 5.50* 5 5.00* 5 4.50* 5 4.00* 5 3.50* 5 3.00* 5 2.50* 5 2.0De 5 1.50e5
- 1,00*5
- 5,00*4
- 0.00
- 

# I Sampl e Name - 1(111227t>160 " Sampl * ID : "GL P 1 CM ) 1-02-2 ' Pea k Nam e "PFOS " Mass(es) : '499.000/80.00 0 Oa,499.0 f Commen t "DAL-GW-143R-0- " /Annotation . " Sampl e Type : Calc i n/A 12/30/201 1 Algorithm ; Spe t Sub . Window ; Uln . Pea k iight ;

Width ; Smoothin g Hidth : R T Hindow : Expecte d RT ; Us e Relativ e RT : Int , Type ; 1.6*5
- 1.5*5
- 1.4o5
- 1.3*5
- 1.2e5
- l.leS
1.0e5
- g 9.0*4
- t 8.0*4
- 

### I
7.0*4
- 6.0*4
- 5.0e4
- 4.0*4
-

14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 2 6 o f 2 7 Pag e 7 4 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 *ETS-Kir k Result s Name : klll227a.rd b 

# I SampleNam e "klll227l>163 " Pea k Nan>e : "PFOS ' Mass( M Commen t -DAL-GW.144R-0- ' Sanpl e Index : 99 Sanpl e Type : Unknow n

Repor tLarges tPe

i Min . Pea kHeight ; Min . Pea kWidth : 1.15*5 - 1.10*5 - 1.05*5 - 1.00*5 - 9.50*4 - 9.00*4 - 8.50*4 - 8.00*4 - 7.50*4 - 7.00*4 - ^ S.50»4 - 6.00*4 - I 5 50*4 -
" 5.00*» - 4.50*4 - 4.00*4 - 3.50*4 - 3.00*4 - 2.50*4 - 2.00*4 - 1.60*4- i 1.00*4 - 5000.00 - 0.00 - 13. 0 13. 5 14. 0 14. 5 15. 0 15. 5 16. 0 16. 5

Dat a printe d b yST W Thursday , Januar y26 , 201 2 Pag e 2 7 o f 2 7 Pag e 7 5 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Workstation : ETSBUSTE R Batc hName : bl20104a.da b

*Dat a worke d u p b yKJ U Pag e l o f 1 Printin g Time : 3:41:0 6 P M Printin g Date : Thursday , Januar y05 , 201 2 Pag e 7 6 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Decatur , A L - Decembe r201 1 Workstation : ETSBUSTE R Batc hName : bl20104a.da b

*Dat a worke d up b yKJ U Pag e 1 o f 1 Printin g Time : 3:41:3 0 P M Printin g Date : Thursday , Januar y05 , 201 2 Pag e 7 7 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Buste r J293020 3 Batc hName : bl20104a.da b 

# I SampleNamet)120104a0i rSampl e ID,'11012-e4 ' Flei' l P*akNam e -13C4PFOS-SUR ' Masses ) •503.0W).0ami T Ckimmeni;*1.0n9'mLF C stdi n Synth . Watai * Annotation' -
3.2e 4 3.0e 4 2.Be 4 Snoothin g Hidth ; 3 R T Window : 30. 0 Us e Relativ e RT ; N o liQua n - 1 0 0 cp s 0 0 sa c
2.4e 4 2.2* 4 2.0* 4

1.4* 4 1.2* 4 1.0* 4 eooo. 0 6000. 0 4000. 0 2000. 0

' 0. 0 164 5 16.76 17.1 3 17.5 0 15. 5 16. 0 

# I Sampl e Name''b120104a02a ' SamplelD'11010^04 ' F)e-b120104a.wi r Pea k Name : •13C4PFOS-SUR ' MaM{es) : '503.0/BO. O amo ' Commen L 'Metho d Blank ' Annotatio n * * Concentratl < Calculate dC Acq . Date : Acq . Time : : 0.0037 3 n t 1/4/201 2 11:21:3 6 P

M

il, .l.h.i... .iiM, i4ii,.i . 

# I Sampte Nam e 'b120104a029 " Sampte ID . •LCS-120104-1 ' Fie ; •t>120104a.wi( r Pea k Nam* : •13C4PFOS-SUR ' M3ss(es) - '503.0/80. 0 amu ' Comment . '0.2pp b LCS * Annotatio n - Sampl e Index ; 2 9 Calculate d Cone : 0.20 1 n g Acq . Date : 1/4/201 2 Acq. Tine: 11:12:44 PH Modified : N o Proc . Algorithn : IntelliOua n - Mm . Pea k Height : 0.0 0 cp s Min . Pea k width ; 0.0 0 sa c 15. 4 Valle y 15. 4 3205 8 c c 7.04e+00 3 15. 3 15. 6 

# I Sampte Name : •bl20104a032 " Sampt e ID : •LCS-120104-4 ' File''b120104a.wif r PeakNam e '13C4PFOS-SUR ' Massfes):"SOSCBO.Oamu ' Commen t '2pp b LCS ' Annotation- " SaiDpl e Index . 3 2 Sampl e Type ; Q C Concentiatlon : 1.8 9 ng/n L Calculate d Cone : 2.1 3 ng/n L Acq . Date : 1/5/201 2

Proc . Algorithn : Hin . Pea k Height : Hin . Pea k Uldth : Snoothin g Mldth . R T Mindow : ixpe c

Height : Star t TJ En d Ti m ! RT :

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26,
- 201 2 Pag e 1 o f Pag e 7 8 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Buste r J293020 3 Batc hName : bl20104a.da b 

# I San^t o Name . "61201048035 ' Sampl * ID ' -LCS-120104- rFie : 'b120104a.wi r Pee k Nam* . '13C4PFOS-SUR ' Mau{tts} ' -503.0/BO. O amu " Commeni : "2 0 pp b LCS " Annotation ' - Saople Index: 3b Sanpl e Type ; Q C Concentration : 0.0 0 ng/n L Calculate d Cone : 0.0025 7 ng/nt . Acq . Date ; l/S/201 2 Acq . Tine ; 1;49;1 1 A M Proc . Algorithn ; 1 Min . Pea kHeight Hin . PeakWidth ; Snoothin g Width : R T Klndoa ; Us e Relativ e RT : Height ; Star tT J End Timt lelliQua n - ID A 0.0 0 cp s 0.0 0 se c 

# I SampteNam e •bl20104a042 ' Sampte I D •GLP10-01-02-24-05a ' F**t>1201O4a.wrf r Pea k Name : '13C4PFOS-SUR ' Massfes) : '5O3.(V80. 0 amu ' Comman t •DAL-GVV^137S-0- ' Annotatio n -

I . Pea kHeight ; I . Pea kWidth ; lOthin g Width -

: . Type ; .elliQua n - IQ J

14. 0 14. 5 16.1 4 16.51^16.6017.0 2 17.47. . 17.87..^ 6. 0 16. 5 17. 0 17. 5 

# I Sampt e Name : *b12O104aO45 ' Sampte ID ; *GLP10-01-02-24-061 * Fie - 'b1201O4a.wtr r Pea k Nam*.'13C4PFOS-SUR ' Mass(*s),'503.0/80. 0 Comment : •DAL-GW-137L-0- ' Annotation . - Sanpl e Index : Sanpl e Type ; Unknow n Concentration ; H/ A Calculate d Cone : 0.096 5 Acq . Date ; 1/5/201 2 Acq . Time : 

# I Sampt e Name ' 'b1201D4BO48 * Sampte ID : 'GL P I CM)1-02-24-070 ' Fite ' 'bl20104a.wi r PeakName'13C4PFOS-SUR ' MaM(es)-'503.0/80. 0 Comment:'DAL-GW-13eL-0- * Annotatks n -

R T Mindo- : c p s 1( 0 ntelliQua n 0.0 0 0.0 0 3 30. 0 15. 4 H o 1S10 3 count s 3 . •ieo'00 3 cp s 15. 3 Hi n

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e 2 o f Pag e 7 9 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Buste r J293020 3 Batc hName : bl20104a.da b

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e 3 o f 8 Pag e 8 0 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Buste r J293020 3 Batc hName : bl20104a.da b

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e Pag e 8 1 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Buste r J293020 3 Batc hName : bl20104a.da b

Dat a printe d byST

W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e 5 o f 8 Pag e 8 2 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Buste r J293020 3 Batc hName : bl20104a.da b 

# I Sampte Nam* : 'b120104a017 ' Sampte ID . "11012-6-8 ' Fie . 't)120104a.wi r Pea k Nam * 'PFOS ' Mass(*£} ' '499.0/130. 0 amu.499.0/99. 0 am u ,499.0/80. 0 Commen t '1. 0 nglml . F

C std I n Synth . Water* Annotation . 0.94 8 l/</201 Z 7:29;4 7 P

H



# I Sampt o Narr w'b120I04a029 ' Sampte ID : *LCS-120104-1 " Fie ' 'bl20104a.wi r Pea k Nar w'PFOS ' Mass{es) - '499.0/130. 0 amu.499.0» 9 0 amu,499.0/BO. O amu ' Commeni-"0.2pp b LCS * Annotatkin' "

Modified ; R T Window ; Expecte d RT :

Height ; Star t Ti f En d Time ' 9.276*00 3 cp s 

# I Sampto Name:'b120104a032 ' Sampto ID:'LCS-120104-4 ' F Pea k Name . 'PFOS ' Ma£s(»a) ' "499.0/130. 0 amu,499.0/99. 0 a i Commen L '2pp b LCS ' Armotatkin ' " Sampl e Index ; 3 2 Sampl e Type ; Q C Concentration ; 1.8 4 ng/n L95*4
- Calculate dCone ; 2.1 4 ng/n L Acq . Date ; 1/5/201 2 »,-< T Tine
- I3;*fi:0 0 I M 9.0*4
- 8.5*4
- 8.0*4 ' 7.5*4
- 7.0*4
- 6.5e4 ' 6.0*4
- 5.5*4
- I 5.0*4
- I 4.5*4
- Expecte d RT : Us e Relativ e Int . Type : Retentio n Ti n Aiea : Height : Star t Time ; En d Time : : 15. 4

59640 9 c i

2.5*4
- 2.0*4
- 1.5*4
- 1.0*4
- 5000.0
- 0.0
- Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e 6 o f Pag e 8 3 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Buste r J293020 3 Batc h Name : bl20104a.da b

I Sampt e Nam*:'b120104a035 ' Sampt e ID'TCS-120104. rFl* . 1)120104a.wvf r I _. . . iu,499.0/99.0amu,499.0/80.0amu ' 7.5e 5 7.0*5 - 6.5*5 - 6.0* 5 I t . Type : itentio n 1 5.5* 5 5.0e 5 4.Se S § " 4.0*5 - I 3.5*5

-

15.25-. .

14. 5 15. 0 15. 5 16. 0 16. 5 17. 0 17. 5 

# I Sampt e Name ; 'bl20104o042 " Sampt e ID : 'C3LP10-01-02-24-^)58 " Fite : •bl20104a.wi r P*a k Nam* : 'PFOS ' Mats(*») . '499.0/130. 0 amu.499.0/99. 0 amij,499.0/B0. 0 amu ' Comman L 'DAL-GW-13 7 S-0- " Annotation : - Sampl e Index : 1 2 Sampl e Type : Unknom n Calculate d Cone . 0.60 1 r 1/5/201 2 4:1 7 :0 1 A

H 2.1* 4 2.0e 4

2.19**00 4 cp s

1.0* 4 9000.0 - 8000.0 - 7000.0 - 6000.0 - 5000.0 - 4000.0 - 3000.0 - 2000.0 - 1000.0 - 0.0 - 13. 0 13. 5 14. 0 14, 5 15. 0 15. 5 16. 0 16. 5 I Sampt e Nam* . •b120104aO45 ' Sampt e ID : 'GLP10^)1-02-24-061 ' fie : "b120104a.wrt r Pea k Name - "PFOS ' Mass{es) : '49 9 0/130. 0 a i •Commen t "D/U.-GW-137L-0- ' Annotation: - Saiapl e Index : I S j,499.0/99. 0 amu.4g9.0/S0. 0 a r I Sampt e Nam* : "^201043048 ' Sampt e ID : 'GLP10-01-02-24-070 * Fito ' 'b1201O4a.w l I _. iu.499.0/99.0amu.499.0/80.0amu '

Manual 15. 4 11690 2 c < 1.00*5 '

9.50*4 - 9.00*4 8.50*4 - a.00»t ' 7.50*4 - 7.00*4 - 6.50*4 - 6.00*4 - ^ 5.50*4 - i 5.00e4 ' E

= 4.50* 4 - 4.00*4 ' 3.50*4 - 3.00*4 - 2.50*4 - 2.00*4 - 1.50*4 - 1.00*4 - 5000.0 0 0.00 - Hodifled : K T Hindow : Expecte d RT : 0.461 1/5/2012 6:23:26 >

1.30e*00 4 cp s 1.0*4 - 9500.0 ' 9000.0 - 8500.0 ' 8000.0 ' 7500.0 ' ^ 7000.0 ' ^ 6500.0 -

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 4. 5 15. 0 15. 5 16. 0 1 6 J 17. 0 17. 5 5500.0 ' 5000.0 ' 4500.0 ' 4000.0
- 3500.0 ' 3000.0 ' 2500.0 ' 2000.0 ' 1500.0 ' 500.0 ' 0.0 ' 

# J

Pag e 7 o f Pag e 8 4 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Buste r J293020 3 Batc hName : bl20104a.da b 

# I SampteNam e -61201048055 ' Sampte ID:'GLP10-01-02-24-076 ' Fie'tj120104a.wi r Pea k Nam* ' 'PFOS ' Mass(es) - '499.0/130. 0 Bmu,499.0«9. 0 amu,499.0/80. 0 amu ' Comment : •DAL-GW-141R-0- ' Annotation . ~ 4.9 7 ng/m L
Modified ; R T Window : Expecte d RT ;

Star tTime : 1X1*5 ' 9.0*4 - B.0»4 - 7.0*4 6.0*4- 5.0*4 4.0a 4 3.0*4 - 2.0*4 - 

# I Sampt o Name'"61201048058 " Sempte ID-•GLP10-01-01-24-085 " Fit e •b120104a.w( r Pea k Nam* ' 'PFOS ' MBSS{*S) . '499.0/130. 0 amu,499.0/99. 0 annu,499.0/BO. O Commoni : "DAL-GW-WR-O- "
Calculate d Cone . Acq . Time ; Modified : R T Mindow
Us e Relaclu e RT :
Height : Star t T i En d Ti m 26. 4 l/S/201 2 9:54:1 4 M

^ 3.5*5
-

I 3.0e5
-

13. 0 13. 5 14. 0 14. 5 1 5 0 15. 5 16. 0 16. 5 17. 0 17. 5

Dat a printe d b yST W Printin g Time : 1:29:0 3 P M Printin g Date : Thursday , Januar y26 , 201 2 Pag e 8 o f 8 Pag e 8 5 of 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 

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

Pag e 8 6 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1


# 3IV I Environmenta l Laborator y Method Method of Analysis

for the Determination

of Perfluorinated

Compounds

in Water by LC/MS/MS;

Direct Injection

Analysis Method Number:

ETS-8-044.1 Adoption

Date: 4/12/07 Effectiv e Date : /l/f// / Approve d By :

Willia m K . Reagen , Technica l Director , Environmenta l Laborator yDat e

ETS-8-044. 1 Pag e 1 of2 2 Method 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 8 7 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1


### 1 Scop e an d Applicatio n Thi s metho d describe s th e direc t injectio n analysi s o

fperfluorinate d compound s (PFCs ) fro m wate rmatrice s usin g high-perfoimance liqui d chromatograph ytande m mas s spectrometr y (HPLC/MS/MS) . Th e metho d i s generall yapplicabl e bu t no t limite d t o th e measuremen t of perfluoroalky l sulfonamide s an d perfluorinate d alky i acid s (PFAAs ) suc h as perfluorosulfoni c acid s (PFSAs ) an d perfluorocarboxyli cacid s (PFCAs ) (Tabl e 1) . Wate rsample s containin g heav yparticulat e ma

yrequir e preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Detenninatio n ofPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Perfonnance Liqui d Chromatography/Mas s Spectrometry" . Th e metho d i s applicabl e t o bot h extema l standar d an d intema l standar

d calibratio n V Tabl e 1 . Representativ e Targe t Analyte s Acronym Analyte Chemical Abstract Services Registry Number

(CASRN) PFBA(C 4 Acid ) Perfluorobutanoi caci d 375-22- 4 PFPeA(C 5 Acid ) Perfluoropentanoi caci d 2706-90- 3 PFHx A(C 6 Acid ) Perfluorohexanoi caci d 307-24- 4 PFHpA(C 7 Acid ) Perfluoroheptanoi caci d 375-85- 9 PFOA(C 8 Acid ) Perfluorooctanoi caci d 335-67- 1 PFN A(C 9 Acid ) Perfluorononanoi caci d 375-95- 1 PFD A(CI O Acid ) Perfluorodecanoi caci d 335-76- 2 PFUnA(C1 1 Acid ) Perfluoroundecanoi caci d 2058-94- 8 PFDoA(C12Acid ) Perfluorododecanoi caci d 307-55- 1 PFTrDA(C1 3 Acid ) Perfluorotridecanoi caci d 72629-94- 8 PFB S (C 4 Sulfonate ) Perfluorobutanesulfoni caci d 375-73- 5 PFH S (C 6 Sulfonate ) Perfluorohexanesulfoni caci d 355-46- 4 PFO S (C 8 Sulfonate ) Perfluorooctanesulfoni caci d 1763-23- 1 FBS A(C 4 Sulfonamid e Perfluorobutanesulfonamid e 30334-69- 1 FOS A(C 8 Sulfonamide ) Pefluorooctanesulfonamid e 754-91- 6 Th e Minimu m Reportin g Leve l (MRL) i s th e Limi t ofQuantitatio n (LOQ ) that meets Data Qualit yObjective s (DQOs ) that ar e develope d base d o n th e intende d use o fthi s method . Metho d Flexibilit

y- Thi s i s a perfonnance-base d metho d an d ma yb e generall yapplie d t o th e determinatio n ofperfluorinate d compound s i n wate rmatrice s whe n analysi s batc h qualit y contro l (QC ) criteri a are met^ . Eac h set o fsample s are prepare d i n a n analysi s batc h wit h calibratio n standards , LCSs , blanks , an d continuin g calibratio n chec k standard s analyze d o n th e sam e instrumen t durin g a tim e perio d that begin s an d end s wit h th e analysi s ofth e appropriat e continuin g calibratio n chec k standards . Th e laborator yi s pemnitted t o modif

yth e L C column , mobil e phas e composition , L C conditions , an d MS/M S conditions . Metho d modification s shoul d b e considere d t o improve metho d perfomnanc e o rt o meet data qualit

y objective s fo rth e study . I n al l case s wher e metho d modification s are implemented , th e batc h

' Th e metho di s supporte

db y validationwit

hintema l standar dcalibrationfo r

C4-C1 3 PFCAs , C4 , C6 , an dC8 PFSAs , an dC8 perfluoroalkan

e sulfonamid

e i nlaborator

y control sample

s unde r 3 M metho

dvalidationE l 1-0667 . ^ Guidanc e fo r establishin

g metho dQ C Criteri abase

do na. ) FDAMa

y 2001 , "Guidanc

e fo r Industry , Bioanalytica

l MethodValidation" , b. ) EP AMethod537 , an

dc. ) Europea

nCommission : Guidanc

e fo r Generatin

g an dReportin

g Method s o f Analysi s mSuppor

t o f Pre-registratio

nDat aRequirement

s fo r Anne x I I(Par t A , sectio n4 ) an dAnne x H I (Par t A,sectio n5 ) o f Directive 91/414 , SANCO/3029/99 rev . 4 (11/07/00) . ETS-8-044. 1 Pag e 2 of2 2 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc t Injectio n Analysi s Pag e 8 8 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 analytica l QC s (sectio n 9 ) must b e complete d an d pas s Q C acceptance criteri a (sectio n 13) i f th e dat a fro m th e analytica l batc h ar e t o b e reported . 2 Metho d Summar y Wate rsample s are analyze d a s nea t aqueou s sampl e o ra s solven t dilute d aqueou s sample s b ydirec t injectio n usin g LC/MS/MS . Sample s containin g heav yparticulat 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 centrifuge d o rfiltere d prio rt o removin g a sampl e aliquot o rdilutin g wit h solvent . Th e wate r sampl e i s mixe d wel l prio rt o removin g a n aliquot o rdiluting , i fnecessary , wit h AST M Typ e I water , HPLC water , othe rsuitabl e water , o rsolven t (methanol) . Quantitatio n i s b

ystabl e isotop e interna l standar d calibratio n i n laborator

yreagen t water . Al l perfluorinate d compound s (PFCs ) targe t analyt e concentration s ofperfluorosulfoni cacid s (PFSAs ) an d perfluorocarboxyli cacid s (PFCAs ) are reporte d a s anion s an d correcte d fo r thei rsal t o rfre e aci d fomns . Alternatively , quantitatio n ma yb e perfomried b

yextema l standar d calibration . Thi s i s a perfomnance-base d method . Metho d uncertaint yfo reac h target analyte i s detennine d fo reac h analytica l batc h 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 . Calibratio n standard s fo rPFUnA , PFDoA , PFTrDA , an d FOS Ahav e bee n foun d t o b e unstabl e fo rmor

e tha n 2 days i n 100 % water . Sample s requirin g analysi s fo rthes e compound s b

ythi s metho d shoul d b e dilute d 1: 1 wit h methano l an d analyze d against a calibratio n curve prepare d i n 1: 1 syntheti cgroundwaterMeOH . 3 Definition s 3. 1 Analysi s Batch i Aset ofstud ysample s that are prepare d wit h calibratio n standards , laborator ycontro l samples , an d procedura l blanks , an d analyze d o n th e sam e instrumen t durin g a tim e perio d that begin s an d end s wit h th e analysi s o fth e appropriat e continuin g calibratio n chec k standards . 3. 2 Analytica l Sampl e Aportio n ofa laborator

ysampl e prepare d fo ranalysis . 3. 3 Calibratio n Standar d Asolutio n prepare d b

yspikin g a know n volum e ofth e Workin g Standar d (WS ) into a predetemnined amoun t o

fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e wate r(i.e . matri xwater) , an d analyze d accordin g t o thi s method . Calibratio n standard s ar e use d t o calibrat e th e instrumen t respons e wit h respec t t o analyt e concentration . 3. 4 Laborator yDuplicat e Sampl e (LDS , o rLa b Dup ) Alaborator

yduplicat e sampl e i s a separat e aliquot o fa sampl e take n i n th e analytica l laborator ythat i s analyze d separatel ywit h identica l procedures . Analysi s o fLDS s compare d t o tha t ofth e firs t aliquot give a measur e o fth e precisio n associate d wit h laborator y procedures , bu t no

t wit h sampl e collection , preservation , o rstorag e procedures . ETS-8-044. 1 Pag e 3 of2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 8 9 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
3. 5 Fiel d Blan k

(FB)/Tri p Blan k

(TB ) AST M Typ e 1 , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator yan d treate d a s a sampl e i n al l respects , includin g exposur e t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures . Th e purpos e ofth e T B i s t o detennin e i ftes t substance s o rothe 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 . 3. 6 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 field an d laborator

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

yprocedures . 3. 7 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s o fth e targe t analytes , IS s an d SRS s are adde d t o th e sampl e bottl e i n th e laborator ybefor e th e bottle s ar

e sen t t o th e field fo rcollectio n o faqueou s samples . Aknown , specifi cvolum e ofsampl e must b e adde d t o th e sampl e containe r withou 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 of th e sampl e container . Th e FM S i s analyze d t o ascertai n i fan ymatri xeffects , interferences , o rstabilit yissue s ma

ycomplicat e th e interpretatio n ofth e sampl e analysis . 3. 8 Tri p Blan k

Matri xSpik e (TBMS ) A n aliquot ofAST M Typ e 1 , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analytes , IS s an d SRS s are adde d i n th e laborator yprio rt o th e shipmen t o

fth e collectio n bottles . Th e TBM S i s analyze d exactl ylik e a stud ysampl e t o hel p determin e i fth e metho d i s i n contro l an d whethe ra los s ofanalyt e o ranalytica l bia s coul d b e attribute d t o sampl e holdin g time , sampl e storag e and/o rshipmen t issues . Alo wan d hig h TBM S are appropriat e whe n expecte d sampl e concentration s are no t know n o rma

yvary . 3. 9 interna l Standar d (IS ) Acompoun d adde d t o eac h stud ysample , calibratio n standard , laborator ycontro l samples , an d procedura l blank

s a t a consisten t leve l (typicall yaroun d 1 ng/mL) . Th e intema l standard(s ) are stabl e isotop e labele d version s o fth e targe t analytes . Th e are a coun t rati o of th e targe t analyt e t o th e interna l standar d i s use d fo rcalibration . Surrogate IS s ar e applie d whe n stabl e isotop e IS s oftarge t analyte s ar e unavailable . Asurrogat e I S i s no t necessaril y a stabl e isotop e labele d versio n ofth e targe t analyte , bu t i s treate d a s a n intema l standar d fo r quantitation . 3.1 0 Laborator yContro l Sampl e (LCS ) A n aliquot ofcontro l matri xt o whic h know n quantitie s ofth e target analytes , IS s an d SRS s (whe n applicable ) are adde d i n th e laborator ya t th e tim e whe n sample s are aliquotted . At leas t thre e level s (two level s fo rSRSs ) i n triplicat e ar e included , on e generall ya t th e lo wen d o fth e calibratio n curve an d on e nea rth e mi d rang e an d th e uppe ren d o fth e curve . Th e LCS s are analyze d exactl ylike a laborator ysampl e t o determin e whethe rth e stabilit yofth e standards . LCS s shoul d b e prepare d eac h da ysample s are aliquoted . 3.1 1 Laborator yMatri xSpik e (LMS ) Alaborator

ymatri xspike i s a n aliquot o fa sampl e t o whic h know n quantitie s oftarge t analytes , IS s an d SRS s (whe n applicable ) are adde d i n th e laboratory . Th e LM S i s analyze d exactl ylike a laborator

ysampl e t o detemnin 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 x must 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 r thes e concentrations . LMS s ar e optiona l fo ranalysi s o

faqueou s samples . ETS-8-044. 1 Pag e 4 of2 2 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 9 0 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
3.1 2 Laborator ySampl e Aportio n o raliquot ofa sampl e receive d fro m th e field fo rtesting . 3.1 3 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra n analytica l batc h i s th e lowes t concentratio n that ca n b e reliabl yquantitate d withi n th e specifie d limits o fprecisio n an d accuracy . 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 tha t meets metho d acceptance criteria . Th e LLO Q fo reac h target analyt e i s establishe d fo reac h analysi s batc h as th e lowest calibratio n standar d wit h are a counts a

t least twic e tha

t o fth e averag e are a counts ofth e procedura l blanks . Th e uppe rlimi t ofquantitatio n (ULOQ ) fo ra n analytica l batc h i s th e highest concentratio n that ca n b e reliabl yquantitate d withi n th e specifie d limits o fprecisio n an d accuracy . Th e highest standar d i n th e calibratio n curve that meets metho d acceptance criteri a i s define d a s th e ULOQ . 3.1 4 Method/Procedura l Blan k A n aliquot o fcontro l matri xthat i s treate d exactl ylik e a laborator

ysampl e includin g exposur e t o al l glassware , equipment , solvents , an d reagents that are use d wit h othe rlaborator y samples . Th e metho d blan k i s use d t o detennin e i ftest substance s o rothe rinterference s are presen t i n th e laborator

yenvironment , th e reagents , o rth e apparatus . 3.1 5 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yo fmateria l intende d t o represen t th e origina l source material . 3.1 6 Stoc k

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

### 3.1 7 Surrogat e Interna l Standar d A n I S that i s no

t necessaril ya stabl e isotopicall ylabele d targe t analyte , bu t i s treate d a s a n intema l standar

d fo rquantitation . Sun-ogat e IS s are use d whe n isotopicall ylabele d counterparts ofth e targe t analyt e ar e no t commerciall yo rreadil yavailable . 3.1 8 Surrogat e Recover yStandar d (SRS ) A n isotopicall ylabele d standard , no t use d as a n intema l standard , that i s adde d t o eac h sampl e an d appropriat e Q C sampl e as a mean s t o evaluat e th e metho d performance fo ra chemica l clas s o

fcompound s (e.g. , PFSAs , PFCAs) . 

### 3.1 9 Workin g Standar d (WS ) Asolutio n o

fsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d a s neede d t o 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 yo fth e standard s fo rthi s metho d hav e no t bee n precisel y detennined ; 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 exposur e t o chemical s tha

t migh t b e present . ETS-8-044. 1 Pag e 5 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 1 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
Th e laborator

yi s responsibl e fo rmaintainin g a saf e wor k environmen t an d a curren t awarenes s o

floca l regulafion s regardin g th e handlin g o fth e chemical s use d i n thi s method . Areference file ofmateria l safet ydat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses . 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems . Refe rt o th e appropriat e equipmen t procedur e o roperato rmanua l fo r additiona 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 rcondition s o fanalysi s b

yrunnin g metho d blanks . Parts an d supplie s tha

t contai n Teflon®

shoul d b e avoide d o rminimize d du e t o th e possibilit y ofinterference 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 Material s 6. 1 Instrumentatio n Analytica l balance capabl e ofreadin g t o 0.000 1 g HPLC/MS/M S o rHPLC/M S system , a s describe d i n Sectio n 10 . 6. 2 Supplie s an d Material s Sampl e collectio n bottles—HDP E (e.g. , NalgeneTM ) wide-mout h bottle s wit h screwcap . Note : D o no

t us e fluorinated o rTeflon® bottle s o rline d caps . Cooler s o rboxe s fo rsampl e shipment . 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes . Clas s Apipette s an d volumetri cflasks, various . 2 m L HPLC autovial s Disposabl e pipettes , polypropylen e o rglas s a s appropriat e Centrifug e capabl e ofspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 

### 7 Reagent s an d Standard s Note : Supplier

s an d catalo g number

s are fo rillustrative purpose s only . Equivalen t perfomnanc

e ma yb e achieve d usin g chemical s obtaine d fro m othe rsuppliers . D o no t us e a lesse rgrad e ofchemica l tha n thos e listed . 7. 1 Chemical s Wate r- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Calciu m Acetat e - A.C.S . Reagen t Grad e ETS-8-044. 1 Pag e 6 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 2 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Magnesiu m Acetat e - A.C.S . Reagen t Grad e Methano l - HPLC grad e Ammoniu m Acetat e - A.C.S . Reagen t Grad e 

### 7. 2 Representativ e Target Analytes , ISs , an d SRS s PFBA , Heptafluorobutyri cAcid , (C 4 Perfluorinate d Acid ) PFPeA , Nonafluoropentanoi cAci d (C 5 Perfluorinate d Acid ) PFHxA , Perfluorohexanoi cAci d (C e Perfluorinate d Acid ) PFHpA , Tridecafluoroheptanoi cAcid , (C 7 Perfluorinate d Acid ) PFOA , Ammoniu m perfluorooctanoate , (C s Perfluorinate d Acid ) PFNA , Heptadecafluorononanoi cAcid , (C g Perfluorinate d Acid ) PFDA , Nonadecafluorodecanoi cAci d (C1 0 Perfluorinate d Acid ) PFUnA , Perfluoroundecanoi cAcid , (C n Perfluorinate d Acid ) PFDoA , Perfluorododecanoi cAcid , (C1 2 Perfluorinate d Acid ) PFTrDA , Perfluorotridecanoi cAcid , (C1 3 Perfluorinate d Acid ) FBSA , Perfluorobutanesulfonamid e FOSA , Perfluorooctanesulfonylamid e PFBS , Potassiu m Perfluorobutanesulfonat e PFHS , Perfluorohexanesulfonat e PFOS , Potassiu m perfluorooctanesulfonat e PFO A[1,2 , 3,4-"C] , "C4-isotopicall ylabele d perfluorooctanoi caci d (SRS ) PFO S [1,2 , 3,4-"C] , "C4-isotopicall ylabele d Perfluorooctanesulfonat e (SRS ) PFUn A[1,2-"C] , "C2-isotopicall ylabele d Perfluoroundecanoi caci d (SRS ) Acusto m mi xo

fIS s i n a methanoli csolutio n containin g ([1,2,3,4-"C4]PFBA , [1, 2 - "CJPFHxA , [1,2,3,4,5,6,7,8-^^C8lPFOA , [1,2,3,4,5,6, 7 8,9-^^C9]PFNA , [1, 2 -^^CJPFDA , [1,2,3,4,5,6,7-"CyjPFUnA , [1, 2 -"CJPFDoA , [1,2, 3 -^^CajPFHS , [1,2,3,4,5,6,7,8-^^C8]PFOS , an d [1,2,3,4,5,6,7,8-"C8]PFOS A(Wellingto n Laboratories , Guelph , ON ) i n combinatio n wit h adde d ([1,2,3,4,5-"C5]PFPeA , ([1,2,3,4-^C4]PFHpA , an d [^^OJPFB S ca n b e use d t o prepar e a stoc k I S solution . Alternatively , individua l stabl e isotop e IS s ca n b e use d t o prepar e a stoc k I S mixture . Othe rIS s ca n b e applied . 

### 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—^Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L ofreagen t water . Syntheti cGroundwate r(containin g 2 5 pp m C a an d Mg ) - Weig h 0.6 1 g o fCalciu m Acetat e an d 0.92 g ofMagnesiu m Acetat e an d dissolve i n 6. 0 L o freagen t water . Note : Alternative volume s ma yb e prepare d a s lon g a s th e ratio s ofth e solven t t o solut e rafio s are maintained .
ETS-8-044. 1 Pag e 7 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 3 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
7. 4 Stoc k

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

d preparatio n procedur

e serve s as a n example . Weighe d amounts an d flnal volume s ma

yb e change d t o sui t th e need s ofa particula rstudy . Fo rexample , p L volume s ma

yb e spike d into volumetri cflasks whe n dilutin g stoc k solution s t o appropriat e levels . 10 0 pg/m L targe t analyt e SSSs—Weig h ou t 1 0 m g ofanalytica l standar d (correcte d fo r percen t salt , aci d [ETS-4-031 ] an d purity ) an d dilut e t o 100 m L wit h methano l o rothe r suitabl e solvent , i n a 100 m L volumetri cflask. Transfe rt o a 125 m L LDP E bottl e o rothe r suitabl 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 y standar d operatin g procedure . A n exampl e ofpurit yan d sal t correctio n i s give n belo wfo r PFOS . ^

. rL molecula rweigh t ofanio n sal t correctio n facto r= = moclecula rweigh t ofsal t

49 9 PFO S (K-')sal t correctio n facto r= —= 0.927 5 53 8 1 0 m g CsFiySOa'K

* wit h purit

y90 % = 8.35 m g C8F17SO3 ' (1 0 mg*0.90*0.9275=8.3 5 mg ) 1 0 MQ/m L (10,00 0 ng/mL ) mixe d workin g standard—Ad d 5. 0 m L eac h ofth e 100 pg/m L SSS s t o a 5 0 m L volumetri cflask an d brin g u p t o volum e wit h solvent . 1 (jg/m L (1,00 0 ng/mL ) mixe d worl<in g standard—Ad d 0. 5 m L o fth e 100 pg/m L SSS s t o a 5 0 m L volumetri cflask

an d brin g u p t o volum e wit h solvent . 0. 1 MQ/m L (10 0 ng/mL ) mixe d standard—Ad d 0.05 m L ofth e 100 pg/m L SSS s t o a 5 0 m L volumetri cflask

an d brin g u p t o volum e wit h solvent . Storag e Conditions—Stor e al l SSS s an d wori<in g standard s i n accordance wit h laborator y standar 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 . 

### 7. 5 Calibratio n Standard s Calibratio n ca n b e perfonne d b yI S o rexterna l calibration . Usin g th e wori<in g standard s describe d above , prepar

e calibratio n solution s i n AST M Typ e 1 water , HPLC water , othe r suitabl e water , o ra mixture o fsolven t an d wate rusin g th e infomnatio n i n Tabl e 2 a s a guideline . Note : Volume s ofwate ro rwater/solven t mixture s an d wori<in g standard s ma yb 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 rtha n thos e liste d belowca n b e prepare d a s needed . Fo rth e quantitatio n ofPFO Aan d PFOS , reference material s ofcertifie d mixe d linea ran d branche d isome rar

e preferred . Alternately , reference material s ofprimaril ylinea risomer s o f PFO Aand/o rPFO S ma

yb e used , however , whe n quantitatin g wit h predominantl ylinea r reference standards , additiona l LC S sample s containin g bot h linea ran d branche d isomer s o f PFO Aan d PFO S are required^ . 7.5. 1 Intema l Standard (IS ) an d Surrogat e Recover yStandard (SRS) Fo rI S calibration , stabl e isotop e intema l standard s o feac h target analyt e o rappropriat e surrogat e IS s shoul d b e spike d a t th e sam e leve l i n al l calibratio n standards . Once th e calibratio n standard s have bee n prepare d a s state d above i n Sectio n 7.5 , al l calibratio n standard s are spike d wit h a separat e interna l standar d spikin g solution . Typicall yth e

' Arepor t summarizin

g a nassessmen

t o f th e us e o f referenc e standard

s containin

g certifie dlinea

r an dbranche disomer s o f PFOA/PFO

S ca nb e foundi n3 M repor

t Ell-0560 . ETS-8-044. 1 Pag e 8 of2 2 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 9 4 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 concentratio n o

fth e interna l standar

d i s consisten t wit h th e interna l standar d concentratio n expecte d i n th e sample s bein g prepared , usuall y1 ng/mL . Th e concentratio n o fth e intema l standar d spikin g solutio n i s typicall y2 pg/mL . Aseparat e zer o poin t o rmetho d blan k

i s typicall yprepare d a

t th e sam e tim e a s th e calibratio n standards , usin g th e sam e solutio n use d t o prepare th e standard s (AST M Typ e 1 water , HPLC water , othe rsuitabl e water , o ra solvent/wate rmixture) , an d i s spike d wit h th e intema l standar d a t th e sam e concentrafio n a s th e calibratio n curve , typicall ya t 1 ng/mL . I fth e sample s bein g analzye d were pre-spike d wit h SRSs , th e calibratio n curve prepare d i n Sectio n 7. 5 i s spike d wit h a separat e SR S spikin g solution . Typically , th e sampl e bottle s are spike d wit h a SR S a

t 0. 1 ng/mL . Th e final calibratio n curve must consist ofa t least si x calibratio n points afte ranalysis . Th e followin g tabl e provide s a n exampl e ofspik e concentration s an d volume s use d t o achieve a multi-poin t extracte d calibratio n curve wit h interna l standar

d an d sun'ogate standard . Tabl e 1 lists recommende d stabl e isotop e interna l standard s fo rsevera l PFS Aan d PFCA target compounds . Acusto m mi xofisotopicall ylabele d targe t analyte s i n a methanoli c solutio n containin g ([1,2,3,4-"C4]PFBA , [1, 2 -^^CJPFHxA , [1,2,3,4,5, 6 7,8-"C8]PFOA , [1,2,3,4,5,6,7,8,9-X9]PFNA , [1,2,3,4,5, 6 -"CejPFDA , [1,2,3,4,5,6, 7 -''XylPFUnA , [1, 2 - "CJPFDoA , [1,2,3-"C3]PFHS , [1,2,3,4,5,6,7,8-"C8]PFOS , an d [1,2,3,4,5,6,7,8-"C8]FOS A (Wellingto n Laboratories , Guelph , ON ) i n combinatio n wit h adde d ([1,2,3,4,5-"C5]PFPeA , ([1,2,3,4-"C4]PFHpA , an d [^^OJPFB S ca n b e use d t o prepare a stoc k I S solution . Alternative source s ofcertifie d stabl e isotop e labele d targe t analyte s are applicable . Alternatively , individua l stabl e isotop e IS s ca n b e use d t o prepar e a stoc k I S mixture . Th e tabl e belowlists th e recommende d stabl e isotop e IS s an d SRS s applie d i n th e method . Othe rstabl e isotop e IS s an d SRS s oftarge t analyte s no t liste d i n th e tabl e ma

yb e use d i f supporte d b

yvalidatio n and/o ranalysi s batc h QC s meetin g metho d acceptance criteri a (e.g. , [^^CJ-PFOA) . Th e sam e intema l standar d shoul d b e use d fo ra give n analyt e throughou t th e entire project/study . Note : som e o fth e compound s liste d belo ware appropriat e t o us e a s surrogat e IS s whe n a stabl e isotop e I S ofa targe t analyt e i s no t available . Generally , surrogat e isotopicall ylabele d PFCA s are use d fo rPFCAs , an d surrogat e isotopicall ylabele d PFSA s are use d fo rPFSAs . Tabl e 2 provide s example s o fspik e concentration s an d volume s use d t o achieve a multi-poin t calibratio n curve wit h IS s an d SRSs .

ETS-8-044. 1 Pag e 9 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 5 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Tabl e 1 . Stabl e Isotop e PFCA s an d PFSA s use d fo rIS s an d SRS s Compound

Natne Synonym orAcronym Analytical Purpose Reference Standard

Source "C4-Perfluorobutanoic acid [1,2,3,4-"C4]PFB A I S fo r PFB A Wellingto nLabs

(Mi x o r Individual ) "C4-Perfluoropentanoi

c acid [l,2,3,4,5-"C5]PFPe A I

S fo r PFPe A Wellingto nLabs

(Mi x o r Individual ) "C2-Perfluorohexanoi

c acid [l,2-"C2]PFHx A I S fo r PFHx A WellingtonLabs

(Mi x o r Individual ) "C4-Perfluoroheptanoi

c acid [l,2,3,4-"C4]PFHp A I S fo r PFHp A Wellingto nLab s

(Mi x o r Individual ) '^Cg-Perfluorooctanoi

c acid [l,2,3,4,5,6,7,8-"C8]PFOA I S forPFO Aan

d[1,2,3, 4 "C4]PFO A Wellingto nLabs

(Mi x o r Individual ) "Cg-Perfluorononanoi

c aci d [1,2,3,4,5,6,7,8,9-"C9]PFN A I S fo r PFN A Wellingto nLabs

(Mi x o r Individual ) "Ce-Perfluorodecanoi

c acid [1,2,3,4,5,6-"CslPFD A I S fo r PFD A Wellingto nLab s

(Mi x o r Individual ) "C7-Perfluoroundecanoi

c acid [1,2,3,4,5,6,7-"ClPFUn A I S fo r PFUn A Wellingto nLabs

(Mi x o r Individual ) "C2-Perfluorododecanoi

c acid [l,2-"C2]PFDo A I S fo r PFDoA , *PFT

A Wellingto nLabs (Mi x o r Individual ) "Oi-AmmoniumPerfluorobutan e sulfonat e ["02]PFB S I S fo r PFB S RT IInternationa l (Individual ) "Cs-Ammoniu

mPerfluorohexan

e sulfonat e [1,2,3-"C3]PFHS I S fo r PFH S Wellingto nLabs

(Mi x o r Individual ) "Cs-Sodiu mPerfluorooctan

e sulfonat e [l,2,3,4,5,6,7,8-"C8]PFO S I S fo r PFO S an d PFOS[l,2,3, 4 "C4] , Wellingto nLabs (Mi x o r Individual ) ''Cs-Perfluorooctanesulfonamid e [l,2,3,4,5,6,7,8-"C8]FOS A I S fo r FOSA Wellingto nLabs (mix )

RT IInternationa

l (Individual ) "C4-Perfluorooctanoic acid [l,2,3,4-"C4]PFO A SR S fo r al l PFCAs : C4-C 8 Wellingto n "Cj-Perfluoroundecanoic acid [l,2-"C2]PFUn A SR S fo r all PFCA s C9-C1 3 Wellington "Cg-Perfluorooctan

e sulfonat e [1,2,3,4-"C4]PFO S SR S fo r al l PFSAs : C4 , C6 , an dC8 Wellingto n

ETS-8-044. 1 Pag e 1 0 of2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 6 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

Tabl e 2 . Exampl e Preparatio n o fCalibratio n Curv e wit h IS s an d SRS s Sample Description Concentration

ofWS.tig/mL Volume of WS.fd. Volume

of IS (2 i/g/mL), fd. Concentration of Surrogate, fig/mL Volume of Surrogate, id. Volume of ASTM Type 1 Water, or other suitable solvent mL 0.02 5 ng/m L curv e poin t 0.1 0 2 5 5 0 0.2 0 12. 5 10 0 0.03 0 ng/m L curv e poin t 0.1 0 3 0 5 0 0.2 0 1 5 10 0 0.0 4 ng/m L curv e poin t 0.1 0 4 0 5 0 0.2 0 2 0 10 0 0.0 5 ng/m L curv e poin t 0.1 0 5 0 5 0 0.2 0 2 5 10 0 0. 1 ng/m L curv e poin t 0.1 0 10 0 5 0 0.2 0 5 0 10 0 0.2 5 ng/m L curv e poin t 0.1 0 25 0 5 0 0.2 0 12 5 10 0 0. 5 ng/m L curv e poin t 1. 0 5 0 5 0 0.2 0 25 0 10 0 1 ng/m L curv e poin t 1. 0 10 0 5 0 0.2 0 50 0 10 0 2. 5 ng/m L curv e poin t 10. 0 2 5 5 0 10. 0 2 5 10 0 5. 0 ng/m L curv e poin t 10. 0 5 0 5 0 10. 0 5 0 10 0 10. 0 ng/m L curv e poin t 10. 0 10 0 5 0 10. 0 10 0 10 0 25. 0 ng/m L curv e poin t 10. 0 25 0 5 0 10. 0 N A 10 0 50. 0 ng/m L curv e poin t 10. 0 50 0 5 0 10. 0 N A 10 0 75. 0 ng/m L curv e poin t 10. 0 75 0 5 0 10. 0 N A 10 0 10 0 ng/m L curv e poin t 10. 0 100 0 5 0 10. 0 N A 10 0 N/ A- Not Applicabl e (1 ) Sample s requirin g analysi s fo rPFUnA , PFDoA , PFTrDA , an d FOS Ashoul d b e analyze d agains t a calibratio n curv e prepare d i n 1: 1 syntheti cgroundvrater:MeOH .

ETS-8-044. 1 Pag e 1 1 o f2 2 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 7 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

8 Sampl e Collectio n an d Bottl e Preparatio n Sampl e collectio n bottle s are prepare d by3 M Environmenta l Laborator y(o rsubcontrac

t supplier ) personne l fo r shipmen t a

t ambien t temperature t o th e collectio n site . Typically , fou rseparat e collectio n bottle s are associate d wit h a singl e collectio n site : sample , field duplicat e sample , lo wfield matri xspike , an d hig h field matri xspike . Altematively , th e sampl e an d field duplicat e sampl e ma ycontai n SRS s i n lie u o

fadditiona l targe t analyt e lo wfield matri xspik

e an d targe t analyt e hig h field matri xspike samples . Dependin g o n th e scop e of th e project , additiona l replicate s o fth e field sampl e an d field matri xspike s ma yb e added . Also , i t i s no t uncommo n fo radditiona l mid-leve l field matri xspike s t o b e collecte d i fth e expecte d sampl e concentration s are tnji yunknow n o rcoul d spa n a larg e concentrafio n range . High-densit

ypolyethylen e (HDPE ) wide-mout h Nalgen e bottle s are use d fo rth e sampl e collectio n containers . (Volume s ofth e bottle s ma yvar ydependin g o n ho

wmuc h sampl e i s require d t o meet data qualit yobjectives. ) Sampl e collectio n volume s are projec t specifi can d base d o n dat a qualit yobjectives . Th e Nalgen e bottle s d o no t requir e an ypretreatmen t prio rt o use . Typically , placemen t ofa sampl e bottl e volumetri c"fil l t o here " lin e i s don e b yusin g a sampl e bottl e marke rtemplate . Alternatively , bottle s ma yb e weighe d prio rt o bottl e preparatio n an d weighe d agai n afte rsample s hav e bee n collected . Al l bottle s shoul d b e cleari ylabele d t o indicate its intende d us e as a sample , field sampl e duplicate , lowfield matri xspike , hig h field matri xspike , sample/SR S field matri xspike , field duplicat e sample/SR S field matri x spike , tri p blank , o rtri p blan k matri xspike . I feac h locatio n ha s differen t designate d spik e levels , th e labe l shoul d als o cleari yindicat e th e sampl e locatio n designation . Generally , a set ofbottle s fo ra give n collectio n sit e are prepare d the n groupe d togethe ri n plasti cbag s fo rorganizationa l purposes . Fo reac h sampl e collectio n event , a

t least on e set oftri p blan k an d tri p blan k

matri xspike s ar

e prepared . Bottl e preparatio n shoul d b e documente d i n a Note t o Fil e o ro n a sampl e preparatio n worksheet an d shoul d includ e th e followin g infonnation : dat e prepared , tota l numbe ro fbottle s prepared , numbe rofsampl e sites , th e standar d identificatio n number

s an d spike volume s use d t o prepar e spike d bottles , th e "fil l t o here " volume , an d an yothe rpertinen t infomriafio n neede d fo rreconstnjctibilit yo fth e data . Th e Note t o Fil e wil l b e include d i n th e final data packag e fo rth e project . Sample s ar

e collecte d i n th e field an d shippe d t o th e laborator ya t ambien t temperature . 8. 1 Fiel d Matri xSpik e Sampl e (FMS ) Fiel d matri xspike sample s ar e a requiremen t ofth e method . AFM S sampl e i s define d a s a Q C sampl e t o whic h know n quantitie s ofappropriat e targe t analyte s are adde d t o th e sampl e bottl e i n th e field o ri n th e laborator ybefor e th e bottle s ar

e sen t t o th e field. Th e sampl e an d field duplicat e sampl e ma ycontai n appropriat e SRS s i n lie u oftarge t analyt e FM S samples . Sampl e quantitie s are determine d volumetricall yo r gravimetrically . Aknown , specifi cvolum e o rweigh t ofsampl e i s adde d t o th e sampl e containe rwithou t rinsing. Volumetri csampl e measurements ma yb e acquire d b

ya laborator

yapplie d "fil l t o thi s level " lin e o n th e outsid e ofth e sampl e container . Target analyt e FM S sample s shoul d b e spike d a t approximatel y0.5-1 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 . Typicall ya lo

wan d a hig h target analyt e spike are prepare d fo reac h samplin g location . I n thos e instance s where SRS s are t o b e use d i n lie u oftarge t analyt e FM S samples , th e sampl e an d field duplicat e sampl e are spike d a

t approximatel y2- 5 time s th e target LOQ . Th e FM S i s analyze d t o ascertai n i fmatri x effect s o rsampl e holdin g tim e contribute s bias t o th e analytica l results . Fo rth e sampl e bottle s designate d fo r matri xspikes , a n appropriat e volum e ofmatri xspikin g solutio n i s adde d t o th e empt ybottl e prio rt o sampling . Th e volum e o

fspike solutio n adde d shoul d produce th e desire d final concentratio n oftarge t analyte s onc e th e bottl e i s filled wit h sampl e t o th e "fil l t o her e line" . Th e matri xspikin g solution(s ) shoul d b e prepare d i n a suitabl e solven t an d contai n al l o fth e appropriat e targe t analytes , ISs , an d SRSs . Th e targe t analyt e matri x spikin g solutio n i s ofte n th e sam e as th e workin g standard s use d t o creat e th e calibratio n standards . A n exampl e ofa bottl e spike i s give n below . "Fil l t o here " volum e = 20 0 m L ( A25 0 m L Nalgen e bottl e i s used ) Desire d Fiel d Spike Concentrafio n = 0.2 5 ng/m L ETS-8-044. 1 Pag e 1 2 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 8 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
50 0 n L ofa 0. 1 ng/m L spikin g solutio n (containin g th e targe t analytes ) i s adde d t o th e bottl e an d th e bottl e ca p promptl ysealed . 8. 2 Interna l Standar d an d Surrogat e Recover yStandar d I fanalysi s ofa sun-ogat

e recover ystandar d (SRS ) i s include d i n th e projec t objectives , a n appropriat e volum e ofa surrogat e standar

d solutio n i s adde d t o al l th e bottle s prio rt o samplin g an d SPE . Typicall ysampl e bottle s are spike d wit h surrogat e recover ystandard s a

t a final desire d spike concentratio n of0. 1 ng/mL . I fquantitatio n b

yintema l standar

d (IS ) i s include d i n th e projec t objective , a n appropriat e volum e ofinterna l standar d solutio n i s adde d t o al l th e bottle s prio rt o samplin g an d SPE . Typicall ysampl e bottle s are spike d wit h interna l standar

d a t a final desire d spike concentratio n o f1 ng/mL . Fo rth e tri p blank , th e SR S spik e an d I S spik

e i s adde d t o th e bottl e an d the n AST M Typ e I wate r(HPLC grad e reagen t wate ro rothe rsuitabl e wate rma yused ) i s adde d t o th e "fil l t o here " line . Th e bottl e i s cappe d an d sealin g tap e ma

yb e place d aroun d th e oute redg e ofth e cap . Tri p blan k matri xspike s are prepare d b yaddin g th e appropriat e volum e oftarget analyt e spikin g solution , IS , an d SR S spikin g solution s an d filling th e bottl e t o th e desire d volum e wit h th e appropriat e wate ran d cappin g an d sealin g th e cap . 9 Qualit y Contro l an d Dat a Qualit y Objective s 9. 1 Dat a Qualit y Objective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LOQ of0.02 5 ng/mL . An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra

wdata an d footnote d i n th e final report . 9. 2 Method/Procedura l Blank s Th e method/procedura l blan k i s zer o poin t calibratio n standar d (whic h include s ISs ) analyze d i n a regula rbasi s wit h eac h analysi s batch . A t a minimum , metho d blank s ar e analyze d prio rt o instalmen t calibration , prio rt o th e analysi s ofCCV samples , afte rever y1 0 sampl e injections , an d a t th e en d ofth e analytica l mn . Th e mea n are a coun t o rare a ratio s whe n usin g intema l standar d calibrafion , fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % ofth e are a coun t counts o rare a ratio s whe n usin g interna l standar d calibration , ofth e LOQ standard . Th e standar d deviatio n ofth e are a counts , o rare a ratio s whe n usin g intema l standar d calibration , ofthes e metho d blank s shoul d b e calculated . Aspecifi c%RS D acceptance criteri a i s no t specifie d bu t i s assesse d o n a n analytica l batc h basis . I fth e mea n are a counts o rare a ratio s whe n usin g intema l standar d calibration , ofth e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ must b e raise d t o th e first standar

d leve l i n th e curve that meets criteria . Metho d blank s ma yb e eliminate d i ftechnica l justificatio n ca n b e provide d (e.g . th e procedura l blan k wa s analyze d afte ra n unexpectedl yhig h leve l sample) . I fan yprocedura l blank

s are remove d fro m th e LOQ detemninafion , documen t i n th e ra wdat a an d repor

t a s appropriate . Laborator

ySampl e Replicate s /

Fiel d Duplicat e Sampl e Typically , sample s are collecte d i n duplicate s i n th e field. Th e relative percen t difference (RPD ) ofduplicat e sample s shoul d b e ^20 % fo rth e precisio n o fsampl e preparafio n an d analysi s t o b e considere d i n control . Replicate sample s no

t meetin g th e <20 % RP D criteri a are flagge d an d reporte d a s outsid e o fQ C acceptance criteria . 9. 3 Laborator yMatri xSpike s (LMSs ) LMS s ma yb e performe d i n lie u ofFMS s i fFMS s hav e previousl ybee n perfonne d fo rth e sampl e matrix . Additionally , LMS s ma

yb e perfonne d i n lie u ofFMS s fo ra sampl e matri xi fth e FM S level s were no t appropriat e fo rdetemninin g spike recoverie s relative t o endogenou s level s o ftarge t analyte s an d appropriat e SRSs . Generally , eac h sampl e locatio n represents a differen t sampl e an d sampl e matrix . LMS s ar e prepare d fo reac h sampl e an d analyze d t o detennin e th e matri xeffec t o n spik e recover yefficienc yofeac h targe t analyt e an d appropriat e SRSs . LMS s shoul d b e prepare d at a minimu m ofon e leve l an d i n duplicate . LM S concentration s shoul d b e prepare d a t approximatel y0.5-1 0 time s th e endogenou s concentratio n o r approximatel y4-1 0 time s th e LOQ concentratio n ofeac h target analyte . ETS-8-044. 1 Pag e 1 3 of2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 9 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1
La b matri xspike recoverie s shoul d fal l withi n ±30 % o fexpecte d values . Sampl e dat a wit h LM S recover y outsid e of±30 % bu t withi n ±50 % ofth e expecte d valu e ar e fiagged an d reporte d a s outsid e o fQ C acceptance criteria . Data wit h LM S recover youtsid e o

f±50 % o fth e expecte d valu e ar e reporte d a s NR , where N R i s define d a s "Not Reportable " dat a outsid e ofQC acceptance criteria . 9. 4 La b Contro l Sampl e La b contro l spike s are prepare d fo reac h analysi s batc h t o detennin e metho d accurac yan d precision . LCS s shoul d b e prepare d a

t thre e level s i n triplicat e fo reac h targe t analyt e an d a t a minimu m oftwo level s i n triplicat e fo rappropriat e SRSs . Lo wla b contro l spike s shoul d b e prepare d a t a concentrafio n i n th e rang e of approximatel yifou rt o te n time s highe rtha n th e targete d lowe rLOQ , th e mi d la b contro l spike s shoul d b e prepare d a

t a concentratio n nea rth e mid-poin t ofth e calibratio n curve an d th e hig h la b contro l spike s a t approximatel y80 % ofth e uppe rLOQ . Fo reac h targe t analyt e an d SRSs , th e percen t relative standar d deviatio n (metho d precision ) fo reac h contro l spike leve l must b e les s tha n o requa l t o 20 % an d th e averag e recover y(metho d accuracy) fo reac h contro l spik e leve l must b e 80-120% . Sampl e dat a fo rtarge t analyte s outsid e ofth e laborator

ycontro l spike acceptance criteri a wil l b e handle d as follows : I fth e averag e recover

yofa spikin g leve l fall s outsid e metho d acceptance , bu t a t leas t 67 % ( 6 ou t o

f9 ) o fLC S sample s are withi n 20 % ofthei rrespective nomina l valu e (33 % o fth e QC samples , no

t al l replicate s a

t th e sam e concentration , ma

yb e outsid e 20 % o

fnomina l value) , th e averag e recover ywil l b e fiagged as outsid e metho d acceptance criteria . Al l LC S sample s wil l b e contro l charte d as pe rETS-4-026 . I fth e averag e recover yofon e ofth e spikin g level s exceede d th e analytica l metho d uncertaint yas determine d b

yETS-12 - 012 , that analytica l batc h uncertaint ywil l b e expande d fo rthat particula rstudy . I fmor e tha n 67 % ofth e LC S sample s fai l t o meet metho d acceptance criteria , th e dat a wil l no t b e reported . Calibratio n standard s consistin g ofmixe d branche d an d linea risome rPFOS/PFO Aar e preferred . However , fo rPFOS/PFO

Atarge t analytes , i fth e calibratio n standard s ar e comprise d ofpredominantl ylinea risomer s only , a t least on e leve l oftriplicat e LCS s shoul d b e prepare d usin g PFOS/PFO Awhic h contain s a mi xo flinea r an d branche d isomers . Thes e LCS s wil l b e use d t o demonstrat e quantitative equivalenc y(o rquantitative bias ) o fth e isomeri cmi xwhe n usin g a predominantl ylinea rstandar d fo rcalibration . Th e mixe d linea ran d branche d isome rPFOS/PFO

ALCS s recoverie s shoul d fal l withi n ±30 % o fexpecte d values . Alternatively , i n lie u of mixe d branche d an d linea risome rPFOS/PFO ALCSs , mixe d branche d an d linea risome rPFOS/PFO A TBMS s ma

yb e applie d t o demonstrat e metho d accurac yan d precision . 

### 9. 5 Fiel d Matri xSpike s (FMSs ) / Surrogat e RecoveryStandard s (SRSs ) FMS s are prepare d fo reac h samplin g locatio n an d analyze d t o determin e th e matri xeffec t an d sampl e holdin g tim e o n th e spike recover yo feac h targe t analyt e and/o rappropriat e SRS . Generally , eac h sampl e locatio n represents a differen t sampl e an d sampl e matrix . FMS s are Q C sample s t o whic h know n quantitie s ofappropriat e target analyte s are adde d t o th e sampl e bottl e i n th e laborator

ybefor e th e bottle s are sen t t o th e field. Typicall ya lo wan d a hig h targe t analyt e FM S are prepare d fo reac h samplin g locafion . Th e sampl e an d field duplicat e sampl e ma ycontai n appropriat e SRS s i n lie u oftarge t analyt e lo

wfield matri xspike an d targe t analyt e hig h field matri xspike samples . Fiel d matri xspike metho d acceptance criteri a ar e recoverie s withi n ±30 % o fth e expecte d value . I fFM S recover y(target analyt e o rSR S spike ) i s outsid e o f±30 % ofth e expecte d valu e o rcoul d no t b e assesse d becaus e th e FM S (target analyte ) was spike d a t a n inappropriat e level , th e sampl e resul t i s reporte d a s follows : 1 . ) I ftarget analyt e FM S recover ycoul d no

t b e assesse d becaus e th e FMS' s were a t a n inappropriat e level , the n Laborator

yMatri xSpike s (LMS ) ma yb e substituted . I fLM S recoverie s ar e withi n ±30 % th e dat a are reportabl e an d flagged t o indicat e that th e FM S spike s level s were inappropriate . 2 . ) I fmultipl e targe t analyt e FMS' s were prepare d o n a sampl e an d th e closest FM S leve l t o th e reporte d sampl e meets th e ±30 % acceptance criteri a bu t additiona l FMS' s are outsid e th e ±30 % acceptance range , th e data ar e reportabl e an d flagged t o indicat e that whil e there were failin g FMS's , th e uncertaint ywil l no t b e expande d since th e most appropriate spike leve l passed . ETS-8-044. 1 Pag e 1 4 o f2 2 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 10 0 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 3 . ) I fth e target analyt e FM S recoverie s ar e outsid e ofth e ±30 % acceptance rang e bu t a t leas t 3 0 acceptabl e historica l reportabl e FM S sampl e results are available , th e data ma yb e reporte d bu t flagged wit h a n expande d uncertaint yan d a s no

t meetin g FM S criteria . 4 . ) Sampl e data wit h FM S recover youtsid e o

f±30 % bu t withi n ±50 % o fth e expecte d valu e ar

e flagged an d reporte d a s outsid e ofQ C acceptance criteri a wit h a n expande d uncertainty . 5 . ) I fFM S recover

yi s outsid e o

f±50% , th e sampl e resul t i s reporte d a s NR , where N R i s define d a s "No t Reportable " du e t o noncomplian t Q C results . 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 determin e th e statemen t o faccurac yfo ranalytica l results . Note : I t i s possibl e fo rbottle s utilize d fo rFiel d Matri xSpik e sample s t o b e under-fille d o rover-fille d durin g sampl e collection . Since thi s scenari o wil l effec t th e actua l concentrafio n o fth e FM S sampl e (sun-ogat e an d intema l standar

d concentration s wil l als o b e effected , i fused) , i t i s importan t that an yobviou s under-fillin g o r over-fillin g ofsampl e bottle s b e documente d i n th e dat a packag e an d take n into accoun t i n th e FMS , ISs , o r SRS s recover

ycalculations . Sample s over-fille d o runder-fille d b ymor e tha n 10 % wil l b e requir

e recalculatio n o fth e FMS , ISs , an d SR S tru e values . Th e averag e o

fth e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 1 0 Procedure s 10. 1 Wate rSampl e Preparatio n Thi s metho d i s applicabl e t o wate rsamples . Sample s containin g heav yparticulat e ma

ynot b e suitabl e fo r analysi s b ythi s method . Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered. •Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d autovial . •Dilut e sample , i fnecessary , wit h AST M Typ e I water , HPLC water , othe rsuitabl e water , o rsolven t (methanol) . •La b contro l spike s are prepare d fo reac h analysi s batc h t o detennin e metho d accurac yan d precision . LCS s shoul d b e prepare d a t thre e level s i n triplicat e fo reac h targe t analyt e an d a t a minimu m oftwo level s i n triplicat e fo rappropriat e SRSs . Lo wla b contro l spike s shoul d b e prepare d a t a concentrafio n i n th e rang e ofapproximatel yfou rt o te n time s highe rtha n th e targete d lowe rLOQ , th e mi d la b contro l spike s shoul d b e prepare d a t a concentratio n nea rth e mid-poin t o fth e calibratio n curve an d th e hig h la b contro l spike s a

t approximatel y80 % ofth e uppe rLOQ . Fo rI S quantitation , stabl e isotop e interna l standard s o

feac h targe t analyt e o rappropriat e sun'ogate IS s shoul d b e spike d a t th e sam e leve l a s th e sample s bein g analyzed , i n al l LCSs . •I fLCS s are bein g prepare d usin g syntheti cgroundwater , allowth e LCS s sample s t o equilibrat e fo ra minimu m o f4 hour

s befor e aliquotin g fo ranalysi s o rdilutin g wit h solven t (methanol) . 

### 1 1 Sampl e Analysi s - LC/MS/M S 11. 1 Instrumen t Setu p Note : I n thi s example , a n Applie d Biosystem s SciexAP I 400 0 (AP I 500 0 o rAP I 5500 ) Tande m Mass Spectromete r(LC/MS/MS ) i s used . Othe rbrands/model s ofLC/MS/M S instruments a s wel l a s singl e quadrupol e mas s spectrometer s (LC/MS ) ma

yb e use d a s lon g as th e metho d acceptance criteri a are met . Bran d names , suppliers , par t numbers , an d model s are fo rillustrative purpose s only . Equivalen t perfonnance ma yb e achieve d usin g apparatu s an d material s othe rtha n thos e specifie d here , bu t demonstratio n of equivalen t perfonnance tha t meets th e requirements ofthi s metho d i s th e responsibilit yofth e laboratory . Th e operato rmust optimiz e an d documen t th e equipmen t an d setting s used . ETS-8-044. 1 Pag e 1 5 o f2 2 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 10 1 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Establis h th e LC/MS/M S syste m an d operatin g condition s equivalen t t o th e following : Mass Spec : Applie d Biosystem s AP I 4000 , AP I 5000 , o rAP I 550 0 Io n Source : Turb o Io n Spra y(ABS ) Mode : Electrospra

yNegative Sca n Type : MR M (Multipl e Reactio n Monitoring ) Computer : Del l DH M Software : Windows 200 0 o rWindow s XP , Analyst 1.4. 2 o rhighe rversion s HPLC : Agilen t Serie s 1100,1200 , o r129 0 Agilen t Quaternar

yPum p Agilen t Vacuu m Degasse r Agilen t Autosample r Agilen t Colum n Ove n Note : On e o rmor

e C1 8 HPLC analytica l column s (2. 1 m m x100 mm , 5|a m o r2. 1 m m x5 0 mm , 5nm ) ma yb e attache d on-lin e afte rth e purg e valve an d befor e th e sampl e injectio n por t t o retar d an d separat e an yresidu e contaminants that ma

yb e i n th e mobil e phas e and/o rHPLC system . HPLC Column : Betasi l C18,4.6m m x100mm , 5(x m (ThermoElectro n Corporafion ) Colum n Temperature : 35° C Injectio n Volume : 5p L Mobil e Phas e (A) : 2m M Ammoniu m Acetat e i n AST M Type I wate r(Se e 7.3 ) Mobil e Phas e (B) : Methanol Tabl e 3 . Liqui d Chromatograph yGradien t Program . Step Number Total

Time (min) 0 Flow

Rate (fiUmin) Percent A (2 mM ammonium acetate) Percent B (Methanol) 0 Total

Time (min) 0 75 0 97. 0 3. 0 1 2. 0 75 0 97. 0 3. 0 2 14. 5 75 0 5. 0 95. 0 3 15. 5 75 0 5. 0 95. 0 4 16. 5 75 0 97. 0 3. 0 5 20. 0 75 0 97. 0 3. 0 Note : Othe rHPLC gradients ma yb e use d as lon g a s th e metho d criteri a an d projec t dat a qualit

yobjective s are met . I t ma yb e necessar

yt o adjust th e HPLC gradien t i n orde rt o optimiz e instrumen t perfonnance . Column s wit h differen t dimension s (e.g . 2.1m m x30mm ) an d column s fro m differen t manufacturer s (Keyston e Betasi l C1 8 etc. ) ma yb e used .

ETS-8-044. 1 Pag e 1 6 of2 2 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 102 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 Tabl e 4 Suggeste d MR M Transition s fo rTarge t Analytes , Surrogates , an d Interna l Standard s

Analyte Analyte Description Mass Transition 01 (amu) Mass Transition

03 (amu) PFB A(C 4 Acid ) Targe t 21 3 16 9 PFPe A (C5 Acid ) Targe t 26 3 21 9 PFHx A(C 6 Acid ) Targe t 31 3 269 , 11 9 PFHp A(C7 Acid ) Targe t 36 3 319 , 16 9 PFO A (C 8 Acid ) Targe t 41 3 369,219,16 9 PFN A(C9 Acid ) Targe t 463 419 , 169,21 9 PFD A(CIO Acid ) Targe t 51 3 469,269,21 9 PFUn A(C1 1 Acid ) Targe t 56 3 519,269,21 9 PFDo A(C1 2 Acid ) Targe t 61 3 569 , 169,31 9 PFTA(C1 3 Acid ) Targe t 66 3 619 , 369,31 9 FBS A(C 4 Sulfonamide) Targe t 29 8 7 8 FOSA (C 8 Sulfonamide) Targe t 49 8 7 8 PFB S (C 4 Sulfonate) Targe t 29 9 99 , 8 0 PFH S (C 6 Sulfonate) Targe t 39 9 99 , 8 0 PFO S (C 8 Sulfonate) Targe t 499 80,99 , 13 0 [1,2,3, 4 -"C4IPFB A I S fo r PFB A 21 7 17 2 [1,2,3,4,5-"CslPFPe

A I S fo r PFPe A 268 22 3 [l,2-"C2lPFHx A I S fo r PFHx A 31 5 270 [1,2,3,4
- "C4IPFHP

A I S fo r PFHp A 36

7 32

2 [l,2,3,4,5,6,7,8-"C8lPFOA I S fo r PFO A 42 1 376 [1,2,3,4,5,6,7,8,9-"C9IPFN A I

S fo r PFN A 472 42 7 [1,2,3,4,5,6-"CslPFD A I S fo r PFD A 51 9 47 4 [1,2,3,4,5,6,7-"ClPFUn A I S fo r PFUn A 570 52 5 [l,2-"C2lPFDo A I S fo r PFDo Aan dPFT A 61 5 57 0 ["O2IPFB S I S fo r PFB S 30 3 8

4 [l,2,3-"C3lPFH S I S fo r PFH S 40

2 8

0 [1,2,3,4
- "C4IPFOS I S fo r PFO S 50

3 8

0 [l,2,3,4,5,6,7,8-"C8lFOS A I S fo r FOSA 50 7 8

0 [l,2,3,4-"C4lPFO A Surrogat e (C4-C 8 Acids ) 41 7 372 [1,2,3,4
- "C4]PFO

S Surrogate(Sulfonates , FOSA ) 50

3 8

0 [l,2-"C2lPFUn A Surrogat e (C9-C1 3 Acids ) 56 5 52

0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option . Th e us e ofon e daughte rio n i s acceptabl e i fdat a sensitivit yan d selectivit

yi s achieve d an d provide d that retentio n tim e criteri a ar e met t o assure adequat e specificity . Whil e th e daughte rion s ma yb e chose n a

t th e discrefio n ofth e analyst , mas s transitio n 9 9 i s suggeste d fo rPFOS . Quantitatio n ma yb e perfonne d usin g th e tota l io n chromatogra m (TIC , o rsumme d MRMs ) fo ra give n analyte . Fo rexample , th e PFO ATI C woul d su m al l thre e ofth e monitore d transitions . Us e o fth e suggeste d primar

yio n i s recommended . Retentio n time s ma yvar yslightly , o n a day-to-da

ybasis , dependin g o n th e batc h ofmobil e phas e an d th e gradient , column , guar d column(s ) use d etc . Drif t i n retentio n fimes i s acceptabl e withi n a n analytica l run , a s lon g a s th e drif t continue s throug h th e entire analysi s an d th e standard s are intersperse d throughou t th e analytica l run . 

### 11. 2 Calibratio n Curv e Quantitatio n i s b

yintema l standar

d o rextema l standar

d calibration . Calibratio n standard s ma yb e prepare d i n AST M Typ e 1 , HPL

C water , othe rsuitabl e water , o ra solvent/wate rmixture . I fintema l standar d calibratio n doe s no t meet calibratio n acceptance criteria , extema l calibratio n ca n b e applied . Se e Tabl e 1 fo r ETS-8-044. 1 Pag e 1 7 o f2 2 Metho d o fAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 10 3 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 recommende d applicafio n o f availabl e intema l standards . Quantitatio n o f PFO Aan d PFO S i s b

ysumme d analyte-specifi cmas s transitions . Analyz e th e standar

d curve prio rt o eac h set o f samples . I f intema l standard s were adde d t o th e calibratio n standard s are a ratio s are use d t o generat e th e calibratio n curve . Th e standar d curve ma

yb e plotte d usin g a linea rregressio n (

y= m x+ b) , weighte d 1/

xo runweighted , o rb

yquadrati cfit (

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

xo r unweighted , usin g suitabl e software . 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 calibrafio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-determine d acceptance criteria . Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts (o rare a rafi o i f quantitatin g b yIS ) are no

t a t least twic e that o fth e averag e are a counts (o rare a rati o i f quantitatin g b yIS ) of metho d and/o rsolven t blanks . Th e coefficien t o fdeterminatio n (r^

) valu e fo rth e calibratio n curve must b e greate rtha n o requa l t o 0.99 0 (o ra con-elatio n coefficien t (r

) of 0.995) . Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n o

fth e LLOQ , whic h ma

yb 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 no t meet acceptance criteria , perfor m routin e maintenance o rprepar e a ne w standar d curve (i f necessary

) an d reanalyze . 11. 3 Continuin g Calibratio n Verificatio n (CCV ) 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 o fth e sam e standard s use d t o construc t th e calibratio n curve , at a minimij 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 must b e brackete d b

ypassin g CCVs o rth e calibratio n curve an d a passin g CCV t o b e reportable . 11. 4 Syste m Suitabilit y Aminimu m ofthre e syste m suitabilit ysample s shoul d b e injecte d a t th e beginnin g o

f eac h analytica l njn , prio r t o th e analysi s o fth e calibratio n curve . Typicall ythes e sample s are a t a concentratio n nea rth e mid-leve l ofth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial . I t i s suggeste d that th e syste m suitabilit yinjection s hav

e are a counts o rare a ratio s whe n usin g interna l standar d calibration , wit h a targe t RS D o f<5 % an d a targe t retentio n tim e RS D o f <2% . There i s n o define d acceptabilit ylimi t o n thes e results a s th e %RS D valu e i s dependen t o n th e numbe ro fMR M transition s bein g monitore d i n th e LC/MS/M S ru n o rtim e period . Ultimately , an yeffect s o n thes e parameter s fo rth e Syste m Suitabilit ysample s wil l als o b e eviden t o n al l standard s an d QC sample s analyze d a s part o fth e analysi s batch . An yeffec t o fsyste m suitabilit

yi s incorporate d withi n Q C acceptance criteria . 11. 5 Sampl e Analysi s an d QC s Fo reac h analysi s batch , th e instrumen t analysi s ru n sequence shoul d includ e a n initia l calibratio n curve , samples , FDSs , intersperse d blanks , intersperse d CCVs , appropriat e QC s (i.e. , LCSs , LMSs , FMSs , TBMSs , an d TBs) , an d a final CCV o rcalibratio n curve bracketin g sample s an d appropriat e QC s Injec t th e sam e volum e (betwee n 5 -10OpL) ofeac h standard , analytica l sampl e an d blan k into th e instrumen t (unles s a n on-instmmen t sampl e dilutio n i s desired) . Sample s containin g analyte s that are quantitate d above th e concentratio n ofth e highest standar d i n th e curve shoul d b e furthe rdilute d an d reanalyzed .

' 3 M Environmenta

l Laborator

y stud y E08-009 6 evaluate

dth e effec t o nthes e result s a s afunctio no f

th e numbe r o f MRM s bein

g monitored . ETS-8-044. 1 Pag e 1 8 of 2 2 Metho d of Analysi s fo rth e Determinatio n of Perfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 104 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 

### 1 2 Data Analysi s an d Calculation s Th e chromatograph yanalysi s software wil l typicall ycalculat e th e amoun t o ftarge t analyt e i n th e sampl e extracts usin g th e establishe d calibratio n curve . Calculat e th e percen t recover yofth e LC S usin g th e followin g equation : LCS Concentration {—) LCS % recover

y = ISi ^ * 100 % n g Spik e Concentratio

n(—^ ) m L Calculat e th e percen t recover yofth e LM S usin g th e followin g equation :
LMS Concentration

{-^) - Concentration

of Sample (-^) LM S % recovery= * 100 % Spik e Concentratio n (-2S- )

m L Fo rsample s fortifie d wit h know n amounts o fanalyt e prio rt o extraction , use th e followin g equatio n t o calculat e th e percen t recovery . Recover y- 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 3 Analysi s Batc h Method Performanc e Criteri a An ymetho d perfonnanc 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 n th e final repor t i fth e Technica l Manage r(non-GL P study) o rStud yDirecto r(GL P study) choose s t o repor t th e data . I fcriteri a liste d i n thi s metho d perfonnance sectio n are no t met , maintenance ma

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

t o fth e report . 

### 13. 1 Syste m Suitability- Analysi s Batc h Aminimu m ofthre e syste m suitabilit ysample s shoul d b e injecte d a t th e beginnin g o

feac h analytica l run . Thes e sample s are ru n prio rt o th e calibratio n curve . I t i s suggeste d that th e syste m suitabilit yinjection s hav

e are a counts wit h a targe t RS D ofS5 % an d a targe t retentio n tim e RS D of22% . There i s n o define d acceptabilit

ylimi t o n thes e results a s th e %RSD s are dependen t o n th e numbe rofMR M transition s bein g monitore d i n th e LC/MS/M S ru n o rtim e period . An yeffec t o fsyste m suitabilit

yi s incorporate d i n th e Q C acceptance criteria . 

### 13. 2 Calibratio n an d Limi t ofQuantitatio n (LOQ ) - Analysi s Batc h Calibratio n Curve : Th e coefficien t o fdetenninatio n (r^

) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.99 0 con-espondin g t o a correlatio n coefficien t (r ) = 0.995 . Each 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 yb e withi n ±30% . CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac y ETS-8-044. 1 Pag e 1 9 o f2 2 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 10 5 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

ofeac h curve poin t must b e withi n 25 % ofth e theoretica l valu e (withi n 30 % fo rlowes t curve point) . Sample s that ar e brackete d b

yCCVs no

t meetin g thes e criteri a mus t b e reanalyzed . Limit s o fQuantitatio n (LOQ) : Th e lowe rLOQ (LLOQ ) i s th e lowest non-zer o active standar

d i n th e calibratio n curve ; th e pea k are a o fth e LLOQ must b e a

t least 2 X that ofth e averag e are a counts fo ral l prepare d procedura l blank(s) . B ydefinition , th e measure d valu e o fth e LLO Q must b e withi n 30 % ofth e theoretica l value . 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 . 13. 3 Blank s - Method/Procedura l Blank s an d Tri p Method/Procedura l Blanks : Multipl e procedura l blank s shoul d b e intersperse d throughou t th e analysi s batc h an d th e analytica l sequence . At a minimum , metho d blank s are analyze d prio rt o instalmen t calibration , prio r t o th e analysi s o

f CCV samples , afte rever y1 0 sampl e injections , an d a t th e en d o

fth e analytica l run . Th e mea n are a counts (o rare a ratio s whe n usin g I S calibration ) fo reac h analyt e must b e les s tha n 50 % o fth e are a coun t o

fth e LOQ standard . I fth e are a counts o fth e procedura l blank

s excee d 50 % ofth e LOQ standard , the n th e LOQ must b e raise d t o th e first standar d leve l that meets criteria . Tri p Blani cAtri p blan k

ofAST M Typ e I wate r(o rla b equivalent) i s prepare d i n a sampl e containe ri n th e laborator yan d treate d a s a sample , includin g exposur e t o shipping , samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures . Th e tri p blank s results fo reac h analyt e ar e include d wit h th e reporte d sampl e results . 

### 13. 4 Data Accurac yan d Precisio n - Analysi s Batc h La b Contro l Spil^es : Th e averag e recover ya t eac h LC S leve l fo reac h targe t analyt e an d appropriat e SR S shoul d b e withi n 80-120 % an d th e percen t relative standar d deviatio n o

fth e recoverie s must b e les s tha n o r equa l t o 20% . I fth e averag e recover yo f a spikin g leve l fall s outsid e metho d acceptance , bu t a t leas t 67 % ( 6 ou t o f 9 ) o f LC S sample s are withi n 20 % ofthei rrespective nomina l valu e (33 % ofth e QC samples , no t al l replicate s a

t th e sam e concentration , ma yb e outsid e 20 % of nomina l value) , th e averag e recover ywil l b e flagged as outsid e metho d acceptance criteria . Al l LC S sample s wil l b e contro l charte d a s pe rETS-12-012 . I f th e averag e recover

yofon e ofth e spikin g level s exceede d th e analytica l metho d uncertaint ya s determine d b

y ETS-12-012 , that analytica l batc h uncertaint ywil l b e expande d fo rthat particula rstudy . Th e averag e recover y a t eac h LC S leve l fo rmixe d branched/linea risome rPFO Aan d PFO S shoul d b e withi n 70-130 % an d th e percen t relative standar

d deviatio n o

fth e recoverie s must b e les s tha n o requa l t o 20% . Fiel d Duplicates : Th e relative percen t difference (RPD ) o fduplicat e sample s shoul d b e les s tha n 20 % fo rth e precisio n o

fsampl e preparatio n an d analysi s t o b e considere d i n control . Replicate sample s no t meetin g th e 20 % RP D criteri a are flagged an d reporte d a s outsid e ofQ C acceptance criteria . Fiel d IVIatri xSplices : FM S acceptance criteri a are recoverie s withi n ±30 % ofth e expecte d valu e fo reac h target analyt e an d appropriat e SRS . Sampl e dat a wit h FM S recover youtsid e of±30 % bu t withi n ±50 % ofth e expecte d valu e are flagge d an d reporte d a s outsid e of Q C acceptance criteria . Data wit h FM S recover y outsid e of±50 % o

fth e expecte d valu e are reporte d a s NR , where N R i s deflne d a s "No t Reportable " dat a outsid e of QC acceptance criteria . I fFM S recover ycoul d no

t b e assesse d becaus e FMS s were a t a n inappropriat e level , the n Laborator yMatri xSpike s (LMSs ) ma yb e substituted . I f LM S recoverie s are withi n ±30 % fo reac h targe t analyt e an d SRS s th e data are reportabl e bu t flagged as no t meetin g th e FM S metho d acceptance criteria . 

### 13. 5 Analytica l Method Uncertainty Analytica l metho d uncertaint yfo reac h targe t analyt e an d SR S i s detennine d wit h contro l charte d historica l analysi s batc h LC S dat a fo rth e metho d an d reporte d wit h eac h analysi s batch. ^ Uncertaint

ydetennination s

' Methoduncertaint

y base do nINTERNATIONALANS/ISO/IE D STANDAR

D 1702 5 referenc e (GUM , Guid

e t o th e Expressio

no f Uncertaint y i nMeasurement) . Methodapplicationdemonstrate di nETS-12-012 , citin g references : a. ) EURACHEM/CITAC Guide , "Quantifyin g Uncertaint

y i nAnalytica

l Measurement, " Secon

dEdition ; Editors : S.L.R . Ellison , M . Rosslein , an dA . Williams . b.)Georgian , Thomas , "Estimationo f Laborator y Analytica

l Uncertaint

y Using Laborator

y Control Samples, " Environmenta l Testin g & ETS-8-044. 1 Pag e 2 0 o f2 2 Metho d o f Analysi s fo rth e Determinatio n o f Perfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 10 6 o f 11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

ar e base d o n INTERNATIONA L ANS/ISO/IE D STANDAR D 1702 5 reference (GUM , Guid e t o th e Expressio n ofUncertaint

yi n Measurement) an d describe d i n ETS-12-012 . At leas t thirt ydata points are require d fo r determinin g analytica l metho d uncertainty . Th e metho d uncertaint yi s define d as 2xth e standar d deviatio n of th e percen t recoverie s ofth e poole d la b contro l spikes . Whil e al l LC S data points ar e contro l charted , onl yth e mos t recen t fiftydat a points are use d fo rdetemninin g th e metho d uncertainty . Whe n les s tha n thirt

yLC S dat a points hav

e bee n generate d fo ra give n analyte , th e analysi s batc h LCS s are use d t o detennin e th e dat a uncertainty . I f FMS s meet th e ±30 % recover ycriteri a a

t a leve l appropriat e t o th e endogenou s level , an d th e LC S meet th e ±20 % recover ycriteria , the n th e uncertaint yofth e dat a i s detennine d as withi n 100±20% . Analysi s batc h sampl e dat a wit h FM S recover youtsid e of ±30 % bu t withi n ±50 % o fth e expecte d valu e are fiagged an d reporte d as outsid e ofQ C acceptance criteri a wit h expande d uncertainties . Data wit h FM S recover youtsid e of±50 % ofth e expecte d valu e are reporte d a s NR , where N R i s define d a s "No t Reportable " data outsid e of Q C acceptance criteria . I f FM S recover ycoul d no

t b e assesse d becaus e FMS s were a t a n inappropriat e level , the n Laborator yMatri xSpike s (LMSs ) ma yb e substituted . I fLM S recoverie s are withi n ±30 % fo reac h targe t analyt e an d appropriat e SRS s th e dat a are reportabl e bu t flagged as no t meetin g th e FM S metho d acceptance criteri a wit h uncertaintie s of±30% . I fFM S d o no t meet th e ±30 % recover

ycriteria , an d historica l FM S dat a doe s no t exist , th e analytica l uncertaint yi s evaluate d o n a sample-by-sampl e basis , th e dat a ma

yb e reporte d wit h expande d uncertaint yan d are flagged. 

### 13. 6 Quantitatio n o

fPFOA/PFO S - Analysi s Batc h Calibratio n standard s consistin g ofmixe d branche d an d linea risome rPFOS/PFO Aar e preferred . Quantitatio n i s perfonne d b yintegratin g th e linea ran d branche d isomer s together . Alternately , th e linea ran d branche d isomer

s ca n b e integrate d separately , applyin g th e appropriat e tai e valu e t o eac h calibratio n curve poin t fo reac h isomer . Th e LC S an d sample s are the n quantitate d b yintegratin g th e linea ran d branche d isomer s separatel y(require s separat e analytica l results files) an d quantitatin g th e resultin g pea k against th e linea ro rbranche d calibratio n curve . Th e results fro m bot h integration s are the n summe d t o produce th e final result . Integratin g th e linea ran d branche d isomer s separatel yma

yb e helpfu l fo rthos e sample s where th e linear/branche d ratio s d o no t closel ymatc h thos e o

fth e reference standards . However , fo rPFOS/PFO

Atarge t analytes , i fth e calibratio n standard s ar e comprise d of predominantl ylinea r isomer s onl yth e metho d require s th e additio n o f LCS s o f mixe d branched/linea risome rPFOS/PFOA . Th e purpos e of includin g thes e LCS s i s t o demonstrat e quantitative equivalenc y(o rquantitative bias ) ofth e isomeri cmi xwhe n usin g a predominantl ylinea rPFO S o rPFO Astandar d fo rcalibration . Altematively , i n lie u o fmixe d branche d an d linea risome rPFOS/PFO ALCSs , mixe d branche d an d linea risome rPFOS/PFO A TBMS s ma

yb e applie d t o demonstrat e metho d accurac yan d precision . A n alternat e metho d o

fquantitatio n ca n b e perfonne d wherebyonl yth e linea risome rof PFOS/PFO Ai s integrate d an d use d fo rgeneratin g th e calibratio n curve . Th e LC S an d sample s ar e the n quantitate d b

y integratin g th e linea ran d branche d isomer s separatel y(require s separat e analytica l results files) an d quantitatin g th e resultin g pea k against th e linea rcalibratio n curve . Th e results fro m bot h integration s are the n summe d t o produce th e final result . Integratin g th e linea ran d branche d isomer s separatel yreduce s th e on colum n concentratio n fo rthos e sample s that contai n bot h linea ran d branche d isomer s o f PFOA/PFOS . Thi s ensure s that th e concentratio n detecte d i s withi n th e a rang e o fth e calibratio n curve that i s comparabl e regardles s ofwhethe rth e calibratio n curve wa s generate d usin g predominantl ylinea risomer s of PFOS/PFO

A o rlinea rplu s branche d isomer s ofPFOS/PFOA . 

### 1 4 Pollutio n Preventio n an d Wast e IVIanagement Wast e generate d whe n perfonnin g thi s metho d wil l b e dispose d o f appropriately . 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 . Analysis , November/Decembe r 2000 . c.)Taylor, B.N . an dCE . Kuyatt , NIS T Technica l Not e 1297 , 199

4 Edition : "Guideline s fo r Evaluatin g an dExpressin

g th e Uncertaint

y o f NIS T Measuremen

t Resuhs."d.)Adams , T.M. , "A2L AGuid e fo r th e Estimationo f Measuremen

t Uncertaint

y i nTesting" , Jul

y 2002 . ETS-8-044. 1 Pag e 2 1 O f2 2 Metho d o f Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 10 7 o f 11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1

1 5 Record s Eac h dat a packag e generate d fo ra stud ymust includ e al l supportin g infonnatio n fo rreconstmctio n ofth e data . Infonnatio n fo rth e data 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 m n lo g (instrumen t batc h records , instalmen t acquisitio n method , summar ypages) , instrumen t results files, chromatograms , calibratio n curves , an d dat a calculations . 1 6 Affecte d Document s None. 1 7 Revision s Revisio n Numbe rSummar vo fChange s 1 Section

1. Included

the use of internal standard

calibration

by this method. Section 2. Included

the use of internal standard

calibration

by this method. Included

the use of a solvent/water

mixture when analyzing

for PFUnA, PFDoA, PFTrDA, and FOSA. Section 3. Added

definitions

for internal standard, surrogate

internal standard, and surrogate

recovery

standard. Section 6. Removed

the details regarding

the instrument

parameters

to section 10 of the method. Section 7. Updated

reference

standards

to include intemal standards

and surrogates. Changed concentration

levels for working standards

and included the use of internal standards

and surrogates. Section 8. Inserted

a new section on sample bottle preparation. Section 9 Quality Control. This

section was previously

section 10 in ETS-8-044.0. Updated QC criteria to be consistent

with method ETS-8-154.4. Section 10 Procedures. This

section was previously

section 8 (Sample Handling)

in ETS-8- 044.0. Added

detail regarding

the preparation

of LCSs. Included

the use of methanol

as a dilution solvent. Section 11 Sample

Analysis. This

section was previously

section 10 in ETS-8-044.0. Included the details regarding

the instrument

parameters. Section 12 Data Analysis and Calculations. This

section was previously

section 11 inETS8-044.0. Removed

the equation

for calculating

the analytes concentration, indicating that this is done by the instrument

software. Section 13 Method Performance. This

section was previously

section 12 in ETS-8-044.0. Updated QC criteria to be consistent

with ETS-8-154.4. Added

information

on the determination

of analytical

method uncertainty

and quantitation

of PFO/VPFOS. Section 14 Pollution

Prevention. This

section was previously

section 13 in ETS-8-044.0. Section 15 Records. This

section was previously

section 14 in ETS-8-044.0. Section 16 Affected Documents. This

section was previously

section 15 in ETS-8-044.0. Section 17 Revisions. This

section was previously

section 16 in ETS-8-044.0.

ETS-8-044. 1 Pag e 2 2 of2 2 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 10 8 o f11 0GLP10-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r

Decatur , A L - Decembe r201 1 

### ATTACHMEN TD : DEVIATION(S )

Pag e 10 9 o f11 0GLPIO-01-02 ; Interi m Repor t 2 4 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate r Decatur, AL - Decembe r201 1 

## RECOR D O F DEVIATION/NONCONFORMANC E

/. Identification Stud y/ Projec t No . GLP10-01-02-2 4 Date(s ) o fOccurrence : 12/27/11 , 1/4/1 2 Documen t Number : ETS-8-044. 1 Deviatio n typ e •SO P •Equipmen t Procedur e 0 Metho d (Chec k one ) •Protoco l •GP O •Other :

/ / . Description

(attach

extra pages as needed) 

### Metho d Requirements : 1 . FM S recover

ywithi n ±30 % (sectio n 13.4) . 2 . RP D value s <20 % (sectio n 13.4) . 

### Actua l procedure/process : 1 . Th e samplin g locatio n DA L G W134 L ha d a PFO S FM S recover yof61.2% . 2 . Th e samplin g locatio n DA L G W137 S ha d a sample/sampl e duplicat e RP D o f21 % fo rPFH S an d 32 % fo r PFOS . 

### ///. Actions Taken (such as amendment

issued, SOP

revision, etc.) 

### Correctiv e Actio n ( •Ye s 0 No ) Reference : Acceptabilit yo fth e nonconformin g work : 1 . Th e samplin g locatio n wit h a FM S recover youtsid e metho d acceptanc e criteri a wil l b e flagge d i n th e repor t an d th e analytica l uncertaintyfo rDA L G W134 L wil l b e expande d t o ±39 % fo rPFOS . 2 . Th e non-complian t RPD s wil l b e flagge d i n th e fina l report . Actions : •Haltin g o fWor k •Clien t Notificatio n •Wor k Recal l •Withholdin g o fRepor t 0 Other : Deviation s wil l b e note d i n fina l report . 

### Project Lead/PA I Approval : Stud yDirecto r(i fGLP) : Sponso rApprova l (fo rGL P protoco l deviations) : N A Date: / i 

### Date : Date : Technica l Reviewe r(optional) : NA Date : NA Laborator yDepartnnen t Manage rApproval : Date :

IV. Authorization

to Resume

Work Where halting of work occurred, resumption

of work must first be approved

by Laboratory

Management 

### Laborator yDepartmen t Manage rApproval : NADate : NA Deviation

No. (assigned

by Study Director

or Team Leader at the end of study or project)

ETS-4-008. 7 Pag e 1 o f1 Documentatio n o fDeviation s an d Contro l o fNonconformin g Testin g iioo fn o