GLP10-01-02 ; Interi m Repoi l 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

GLP10-01-02
. Interi m Repor t 13 : Analysi s o fPFBS
. PFHS
. an d PFO S i n Groundwate r Sample s Collecte d a t tir e IWorqa n Count yLandfil l locate d i n Decatur
. A L i n Novembe r201 0 Stud yTitl e Analysi s o fPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc
. 140 0 Westo n Way Westchester , P

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

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

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

6 7

Th e testin g reporte d herei n mee t th e requirement s o fISO/IE C 17025-200 5 "Genera l Requirement s fo rth e Competenc e o fTestin g an d Calibratio n Laboratories", I n accordanc e wit h th e A2I ^

Certificat e #2052.01
. Testin g tha t complie s wit h thi s Intematlona l Standar d als o operat e I n accordanc e wit h IS O 9001:2000
. Certificat e #2052.0 1

Pag e 1 o f6 7GLP10-01-02 : Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements
.

Pag e 2 o f6 7GLP10-01-02 ; Interi m Repoi l 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-02 , Interi m Repor t 13
. Analysi s o

fPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a

t th e Morga n Count

yLandfil l locate d i n Decatur , A L i n Novembe r201 0 Study : Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site Relate d Monitorin g Program
. Thi s analytica l phas e was conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Good Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

•Thes e ar

e environmenta l sample s wher e there i s n o specifi ctest substance , n o specifi ctest syste m an d n o dosin g ofa test system
. •Th e reference substance s 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 detennine d unde rGLPs
.

Gar yHohenstein , Sponso rRepresentative Date

Jaisimh a Kesari , P.E. , DEE , StudyDirecto rDate

Pag e 3 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s ofPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-02 , Interi m Repor t 13
. Analysi s ofPFBS , PFHS , an d PFO S i n Groundwate r Sample s Collecte d a

t th e Morga n Count

yLandfil l locate d i n Decatur , A L i n Novembe r201 0 Study : Analysi s ofPerfluorooctan e Sulfonate (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site Relate d Monitorin g Program
. Thi s repor

t an d th e accompanyin g data were audite d b yth e 3 M Environmenta l Laborator yQualit y Assurance Uni t (QAU) , as indicate d below
. 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 1/5/11-1/7/1 1 Phas e Dat a / Fina l Repor

t Date Reporte d t o

Testin g Facilit y Managemen t 1/20/1 1 Stud yDirecto r 1/20/1 1



### QA U Representative 

# iJMt l Date

Pag e 4 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



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

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

y1 3 7. 1 Method s 1 3 7. 2 Sampl e Collectio n 1 3 7. 3 Sampl e Preparatio n 1 3 7. 4 Analysi s 1 3 8 Analytica l Results 1 5 8. 1 Calibratio n 1 5 8. 2 Syste m Suitabilit y1 5 8. 3 Limi t o

fQuantitatio n (LOQ ) 1 5 8. 4 Continuin g Calibratio n 1 5 8. 5 Blank

s 1 5 8. 6 La b Contro l Spike s (LCSs) 1 6 8. 7 Analytica l Metho d Uncertaint y2 0 8. 8 Fiel d Matri xSpike s (FMS ) 2 0

Pag e 5 o f6 7GLP10-01-02 : Interi m Repor t 1 3 Analysi s ofPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### 9 Data Summar

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

### LIS TO F TABLE S Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Results (Morga n Count yLandfil l Groundwater , Decatur , AL , Novembe r2010 ) 9 Tabl e 2
. Instnjmen t Parameter s 1 4 Tabl e 3
. Liqui d Chromatograph yCondition s 1 4 Tabl e 4
. Mass Transition s 1 4 Tabl e 5
. Limi t ofQuantitatio n (LOQ ) 1 5 Tabl e 6
. Laborator

yContro l Spik

e Recover

y1 7 Tabl e 7
. Analytica l Uncertaint y2 0 Tabl e 8
. Fiel d Matri xSpik e Level s 2 0 Table9
. DALGWMCLMWI B 10111 0 2 1 Tabl e 10
. DA L GWMCLM WI110111 0 2 1 Tabl e 11
. DA L GWMCLM WI S 10111 0 2 2 Tabl e 12
. DALGWMCLMW2 B 10111 0 2 2 Tabl e 13
. DA L GWMCLM W2110111 0 2 3 Tabl e 14
. DA L GWMCLMW3 B 10111 0 2 3 Tabl e 15
. DA L GWMCLM W3110111 0 2 4 Tabl e 16
. DA L GWMCLMW3 S 10111 0 2 4 Tabl e 17
. DA L GWMCLM W4 B 10111 0 2 5 Tabl e 18
. DALGWMCLMW4110111 0 2 5 Tabl e 19
. DA L G WMC L M W4 3 10111 0 2 6 Tabl e 20
. DA L G WMC L MW13 B 10111 1 2 6
Pag e 6 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 21
. DA L GWMCLM W13110111 1 2 7 Tabl e 22
. DA L G WMC L MW13 S 10111 1 2 7 Tabl e 23
. Tri p Blan k

2 8 Tabl e 24
. DA L G W602 S R B 10102 9 2 8

Pag e 7 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



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

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K
. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigato r(clanqeO.mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Kevi n Eich ; Analys t Chelsi e Grochow ; Analys t Jonatha n Steege ; Analys t Stud yDate s StudyInitiation : Marc h 8 , 201 0 Interi m Repor

t 1 3 Experimenta l Tennination : Decembe r15,201 0 Interi m Repor

t Completion : Date ofInteri m Repor t Signin g Locatio n o fArcliive s Al l origina l rawdat a an d th e analytica l repor t have bee n archive d a

t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792
. Th e tes t substanc e an d analytica l referenc e standard reserv e sample s ar e archive d a t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



## 2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t th e Morga n Count yLandfil l locate d i n Decatur , AL , representin g fourtee n differen t samplin g locations
. Atota l of sixt ysampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo rperfluorooctan e sulfonate (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonate (PFBS ) analysis , an d include d duplicat e groundwate rsample s fro m eac h samplin g location
. Sample s als o include d two fiel d matri xspik

e (FMS ) sample s fo reac h location , on e tri p blan k containin g Milli-Q TM water , two tri p blan k spikes , an d on e equipmen t rinseat e blank
. Th e equipmen t rinseate blan k di d no t hav e FM S sample s prepare d fo rdetenninatio n o fPFBS , PFHS , an d PFO S recovery . Th e groundwate rsamples , tri p blank s an d on e equipmen t rinseat e blan k were collecte d b

yWesto n personne l o n Novembe r10-11 , 201 0 an d receive d o n Novembe r12 , 2010
. Al l o fth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r 3 M projec t GLP-10-01-02-13
. 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 an d th e tri p blan k were belo

wth e lowe rlimi t o

f quantitatio n (LLOQ) , indicatin g adequate contro l ofsampl e contaminatio n durin g shippin g an d sampl e collections
. Th e PFB S concentratio n results fo ral l groun d water s range d fro m <0.025 0 ng/m L t o 2.2 6 ng/mL
. Th e PFH S concentratio n results fo ral l groun d water s range d fro m <0.025 0 ng/m L t o 3.2 8 ng/mL
. Th e PFO S concentratio n results fo ral l groun d water s range d fro m <0.025 0 ng/m L t o 14. 8 ng/mL
. Th e metho d uncertaint yfo rPFB S i s ±16% , PFH S ±13% , an d PFO S ±30%
. Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Result s (Morga n Count yLandfil l Groundwater , Decatur , AL , Novembe r2010 ) Sampl e I D DA L G WMC L MW1 B 10111 0 DA L G WMC L MW1110111 0 DA L GWMCLM WI S 10111 0 DA L G WMC L MW2 B 10111 0 DA L GWMCLM W2110111 0 DA L G WMC L MW3 B 10111 0 DA L GWMCLM W3110111 0 DA L G WMC L MW3 S 10111 0 DA L G WMC L MW4 B 10111 0 DA L GWMCLM W4110111 0 DA L G WMC L MW4 S 10111 0 DA L G WMC L MW13 B 10111 1 DA L G WMC L MW13 1 10111 1 DA L G WMC L MW13 S 10111 1 Tri p Blan k

(Milli-Q TM Water

) Equipmen t rinseate blank s Avg
. PFB S

Concentratio n (ng/mL ) ±RP D 2.2 6 ±25 % [a] 0.49 3 ±11 % 1.7 7 ±19 % 1.2 4 ±1.6 % 2.0 6 ±3.4 % 0.038 1 ±12 % 0.027 9 ±0.72 % <0.025 0 <0.025 0 <0.025 0 <0.025 0 0.098 7 ±4.7 % 0.0843 ±7.6 % 0.095 7 ±4.2 % < 0.025 0 < 0.025 0 Avg
. PFH S

Concentratio n (ng/mL ) ±RP D 3.2 8 ±22 % [a] 0.96 6 ±9.1 % 2.2 3 ±20 % 1.3 8 ±2.2 % 1.3 8 ±2.2 % 0.032 6 ±3.7 % 0.032 4 ±8.0 % <0.025 0 <0.025 0 <0.025 0 <0.025 0 0.071 7 ±1.5 % 0.052 6 ±4.4 % 0.055 9 ±8.4 % < 0.025 0 < 0.025 0 Avg
. PFO S

Concentratio n (ng/mL ) ±RP D 7.40 ±30 % [a] 1.4 7 ±13 % 6.42 ±20 % 14. 8 ±2.0 % [b] 5.2 0 ±16 % 0.28 3 ±7.4 % 0.262 ±0.38 % 0.030 6 ±16 % 0.0475 ±15 % 0.144 ±4.9 % 0.25 6 ±5.9 % < 0.025 0 < 0.025 0 < 0.025 0 < 0.025 0 < 0.025 0 N/A ; no t applicabl e [a ] The sample/sample duplicat e RPD wa s S20%
. [b ] Analytical uncertaint

yha s been adjuste

d fo rFM S recover yfo rPFO S t o ±35%
.

Pag e 9 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### 3 Introductio n Thi s analytica l stud ywas conducte d as 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 infonnatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonate (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l studywas conducte d t o analyz e groun d wate rsample s collecte d fro m off-sit e well s locate d i n Decatur , A L fo r PFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on-sit e groundwate rconditions
. Th e 3 M Environmenta l Laborator yprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h were shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling
. Sampl e bottl e sets fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d two fiel d spik e samples
. Eac h empt

ycontaine rfo rgroundwate rsampling s wa s marke d wit h a "fil l t o here " lin e to produce a fina l sampl e volum e of20 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 PFBS , PFHS , an d PFO S prio rt o bein g sen t t o th e fiel d fo rsampl e collection
. Al l sampl e bottle s als o include d th e additio n o finterna l standard s ^^Oa

PFBS , ^^Oa-PFHS , an d "C4-PFO S a t a nomina l concentratio n of1 ng/mL
. Al l sampl e bottle s als o include d th e additio n ofsurrogat e spik e ^^CA-PFO S 

### a

t a nomina l concentratio n o f0. 1 ng/mL
. Se e sectio n 8. 8 ofth e repor

t fo rfiel d matri xspik

e levels
. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detenninatio n ofPerfluorinate d Compound s i n Wate rb yHig h Performance 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 groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples
. Table s 9-2 4 summariz e th e individua l sampl e results an d th e associate d FM S recoveries
. Al l results fo rth e qualit y contro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewher e i n thi s report
. 4 Tes t & Contro l Substance s There wa s no

t a test substance o rcontro l substance s i n th e classi csens e ofa GL P study
. Thi s stud y wa s purel yanalytica l i n nature
.

Pag e 1 0 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



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

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFB S (predominantl ylinear ) Perfluorobutan e sulfonat e C4F9S03 ' Potassiu m Sal t 3 M 1/10/201 7 Froze n 41-2600-8442- 5 TCR-12 1 Whit e Powde r 96.7 % PFH S (linear ) Perfluorohexan e sulfonate C6F13SO3" Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHxSAM0 8 TCR08-001 8 Crystallin e 98 %
Referenc e Substanc e Chemica l Nam e Chemica l Fonnul a Identifie r Source Expiratio n Date Storag e Condition s Chemica l Lo

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO S (linear ) Perfluorooctan e sulfonate CgFiySO s Potassiu m Sal t CA S # 2795-39- 3 Wellingto n 10/18/201 3 Froze n LPFOSKBM0 6 TCR08-000 1 Crystallin e 98 % PFO S (linea r+ branched ) Perfluorooctan e sulfonate CgFiySO s Potassiu m Sal t CA S # 2795-39- 3 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 Whit e Powde r 86.4 %

Pag e 1 1 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "O2-PFB S Labele d - Perfluorobutan e sulfonat e C4F9S[''02]0 - Ammoniu m Sal t RT I Internationa l 3/9/201 5 Froze n 11546-107-2 TCR-1022 , TCR-1028 , TCR 1033 , an d TCR-103 8 Liqui d 99 % "O2-PFH S

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "C,-PFO S Perfluorooctan e sulfonat e ^'CaFiySO a Sodiu m Sal t Wellingto n 04/29/201 3 Froze n MPFC-C-041 0 TCR10-0037 , TCR10-0044 , an d TCR09-007 6 Liqui d NA<^ ' (1 ) Compoun d i s par

t ofa custo m mixtur

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

Pag e 1 2 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



## 6 Tes t Syste m There wa s no

t a test syste m fo rthi s studyi n th e classi csens e o fa GL P study
. Thi s stud ywas conducte d fo ranalysi s ofgroun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b yWesto n Solutions , Inc
. personnel
. Sample s fo rthi s stud yar e "rea l world " environmenta l samples
. Sampl e Descriptio n Ke yCode
. strin g Numbe r Exampl e 1 2 3 4 5
6

7 Strin g Desaipto r Exampl e DA L GWMC L MW4 S 010111 0 Sampl e Locatio n Sampl e Typ e Wel l Locatio n Wel l I D Wel l Leve l Sampl e Typ e
Samplin g Dat e DAL = Decatur , Alabam a GW = Groundwate r MC L = Morga n Count yLandni l Example : MW 4 S = Shallo wwel l 1 = Interfac e wel l B = Bedroc k

wel l 0=primar ysampl e D B = duplicat e sampl e L S = lo wspik e R B = Rinseat e Blan k 10111 0 = Novembe r11 , 201 0


### 7 Metho d Summar y 7. 1 Method s Analysi s fo ral l analyte s wa s complete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detenninatio n ofPerfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
.
_T M , 

## 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene' " (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s were returne d t o th e laborator ya t ambien t condition s o n Novembe r12 , 2010
. Sample s were store d refrigerate d a t th e laborator

yafte rreceipt
. Aset of laborator yprepare d Tri p Blan k

an d Tri p Blan k

fiel d matri xspik

e sample s were sen t wit h th e sampl e collectio n bottles
. 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g it i n a n autovia ! fo r analysis
. 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h perfonnance liqui d chromatography/tande m mass spectrometr y(HPLC/MS/MS)
. Detaile d instrumen t parameters , th e liqui d chromatograph ygradien t program , an d th e specifi cmass transition s analyze d ar e describe d i n th e ra

wdat a har

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

Pag e 1 3 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 2
. Instrumen t Parameters
. instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograpt i Guard colum n Analytica l colum n InjecUo n Volum e Mas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETS MaryAn n ETS-8-044. 0 11/23/1 0 Agilen t 120 0 Pris m R P (2. 1 m m X 5 0 mm) , 5 n Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n

1 0 n L Applie d Biosystem s AP I 500 0 Turtx) Spra

y Turb o io n electrod e Negativ e Analyst 1.4. 2 ETS Ginge r ETS-8-044. 0 12/15/1 0 Agilen t 110 0 Pris m R P (2. 1 m m X 5 0 mm) , 5 ^ ^ Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n

1 0 n L Applie d Biosystem s AP I 500 0 Turb o Spra

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

### Tabl e 3
. Liqui d Chiromatograpii yConditions
. Ste p Numbe r Tota l Tim e

(min ) Flo wRat e

(ftUmin ) Percen t A

( 2 m M ammoniu m acetate ) Percent B (Methano O ETS-8-044. 0 -1 1 /23/1 0 Analysi s 0 1 2 3 4 5 0

2. 0 14. 5 15. 5 16. 5 20. 0 30 0

30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 ETS-8-044.0-12/15/1 0 Analysi s 0 1 2 3 4 5 0

1. 0 11. 0 13. 5 14. 0 17. 0 300

30 0 30 0 30 0 300 300 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 

### Tabl e 4
. IVIas

s Transitions
. Analyt e PFB S PFH S PFO S "CrPFO S Surrogat e Mas s Transitio n Q1/Q 3 299/8 0 299/9 9 399/9 9 399/8 0 499/9 9 499/8 0 499/13 0 503/8 0 Interna l Standar d C'OJPFB S f'OJPFH S ("CJPFO S f'CJPFO S Mas s Transitio n Q1/Q 3 303/8 4 403/8 4 507/8 0 507/8 0 Dwel l tim e wa s 5 0 mse cfo reac h transition
. Th e individua l transition s wer e summe d to produc

e a "tota l io n chromatogram " (TIC) , whic h vi« s use d fo rquantitation
.

Pag e 1 4 of6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### 8 Analytica l Result s 8. 1 Calibratio n Sample s were analyze d against a stabl e isotop e matrix-matche d interna 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 target analyte s into laborator yprepare d syntheti cgroundwate rcontainin g calciu m an d magnesium
. A tota l ofthirtee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 5 0 ng/m L (nominal ) analyze d o n 11/23/1 0 an d te n spike d standard s rangin g fro m 0.02 5 ng/m L t o 5. 0 ng/m L (nominal ) analyze d o n 12/15/10
. Lo w curve points were disable d fo rPFO S o n 11/23/1 0 t o mee t metho d blan k

criteria
. Aquadratic , 1/

x weighted , calibratio n curve o fth e pea k are a counts wa s use d to fi t th e dat a 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 confinne d accurac

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

yrequirements of100±25 % (100±30 % fo rth e lowest curve point) were me t fo ral l analytes
. Th e cortelatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFBS , PFHS , an d PFOS
. 

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

d wa s analyze d fou rtime s a t th e beginnin g o

fth e analytica l sequence t o demonstrat e overal l syste m suitability
. Al l analyte s me t th e acceptance criteri a o fless tha n o requa l t o 5 % relative standar

d deviatio n (RSD ) fo rpea k rati o an d retentio n tim e criteri a ofless tha n o requa l to 2 % RS D wa s me

t fo rPFBS , PFHS , PFOS , an d ^^C4-PF0S
. 

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

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

yrequirements an d fo rwhic h th e are a counts are a t leas t twice thos e ofth e appropriate blanks
. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 5
. Tabl e 5
. Limi t o fQuantitatio n (LOQ)
. Analysi s Dat e 11/23/1 0 12/15/1 0 PFB S

LOQ , ng/m L 0.025 0 N/ A PFH S

LOQ , ng/m L 0.025 0 N/ A PFO S

LOQ , ng/m L 0.25 0 0.025 0 N/ A- No t Applicabl e 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs) were analyze d t o confim 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 reporte d sampl e results were brackete d b yCCV s that me t metho d criteri a o

f100 % ±25 % wit h th e exceptio n ofsamplin g locatio n DA L G WMC L 21101110 , whic h was brackete d b ya CCV fo rPFO S tha

t had a recover

yo f149%
. 

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

fblank s were prepare d an d analyze d wit h th e samples : metho d blanks , tri p blank s an d equipmen t rinseate blanks
. Metho d blan k results were reviewe d an d use d t o evaluate metho d perfonnance t o detennin e th e LOQ fo reac h analyte
. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience
. Equipmen t rinseate blank s are aqueou s sample s that reflec t th e efficienc

yofequipmen t cleanin g i n th e fiel d betwee n differen t sampl e collection s an d are proofofn o cros s contaminatio n o fsample s fro m th e equipment
.
Pag e 1 5 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate rSample s Morga n Count

yLandfill , Decatur , A L - novembe r201 0



### 8. 6 La b Contro l Spike s (LCSs ) 11/23/1 0 Analysis : La b contro l spike s wer e prepare d an d analyze d i n triplicat e a t thre e level s fo rPFBS , PFHS , an d PFOS , an d a t tw o level s fo r^^C4-PF0S
. LCS s wer e prepare d b yspikin g know n amount s o f th e targe t analyte s int o 1 0 m L o flaboratoryprepare d syntheti cgroundwate rt o produc e th e desire d concentration
. Th e spike d wate rsample s wer e the n analyze d i n th e sam e manne ra s th e samples
. Th e metho d acceptanc e criteria , averag e o fLC S a t eac h leve l withi n 100 % + 20 % wit h a n RS D <20% , wer e me t fo rPFBS an d PFHS
. Th e lo wleve l LC S fo rPFO S coul d no t b e calculate d a s th e detecte d concentratio n wa s belo wth e limi t o fquantitation
. Th e mi d an d hig h leve l LC S me t metho d acceptanc e crteria
. 12/15/1 0 Analysis : La b contro l spike s wer e prepare d an d analyze d i n triplicat e a t tw o level s fo rPFOS
. LCS s wer e prepare d b yspikin g know n amount s o fth e targe t analyte s int o 1 0 m L o flaboratoryprepare d syntheti cgroundwate rt o produc e th e desire d concentration
. Th e spike d wate rsample s wer e the n analyze d i n th e sam e manne ra s th e samples
. Th e metho d acceptanc e criteria , averag e o fLC S a t eac h leve l withi n 100 % ±20 % wit h a n RS D <20% , wer e me t fo rPFOS
. A s th e referenc e material s use d fo rquantitatio n o fPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s ar e comprise d o flinea ran d branche d isomers , additiona l LC S sample s o flinea r an d branche d PFO S wer e prepare d a t a minimu m o ftw o concentration s t o evaluat e th e potentia l fo r analytica l bias
. 1 1 /23/1 0 Analysis : Thre e LC S level s wer e prepare d a n anizye d i n tripcalte
. Th e lo wleve l linea ran d branche d LC S coul d no t b e calcualte d a s th e detecte d concentratio n wa s belo wth e limi t o fquantitation
. Th e mi d leve l linea ran d branche d LC S ha d a n averag e recoveryo f136 % an d th e hig h leve l ha d a n averag e recoveryo f133%
. Ane wse t o flinea ran d branche d stoc k standard s wer e prepared , wit h ne w LC S prepare d a t th e sam e thre e concentratio n levels
. Th e ne wLC S wer e analyze d a t th e en d o fth e analytica l ain
. Tw o o fth e lo wleve l linea ran d branche d LC S coul d no t b e calcualte d a s th e detecte d concentratio n wa s belo wth e limi t o fquantitation
. On e replicat e a t th e lo wleve l ha d a recoveryo f152% , whil e bot h th e ne wmi d an d hig h leve l linea ran d branche d LC S me t metho d acceptanc e criteri a wit h averag e recvoerie s o f114%
. Th e mi d an d hig h leve l LC S concentration s wer e mor e appropriat e a s compared t o th e sampl e concentration s reporte d fro m thi s run . Ametho d deviatio n i s include d i n th e ra wdata
. 12/15/1 0 Analysis : Tw o LC S level s wer e prepare d an d aniyze d i n triplicate
. Bot h LC S leve l o flinea r an d branche d PFO S me t metho d acceptanc e criteria
. Al l LC S result s wer e use d i n th e determinatio n o fmetho d analytica l uncertaint yi n sectio n 8.7
. Th e followin g calculation s wer e use d t o generat e dat a i n Tabl e 6 fo rlaboratorycontro l spikes :
1 ^or , . D Calculate d Concentratio n ..„„„ , LC S Percen t Recover

y= * 100 % Spike Concentratio n LCS % RS D = standard deviatio n LC S replicate s . ^QQ„/ ^ averag e LC S recover

y

Pag e 1 6 of6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 6
. Laborator yContro l Spil< e Recovery
. ETS-8-W4. 0 La b I D LCS-101115- 1 LCS-101115- 2 LCS-101115- 3 Averag e + %RS D LCS-101115- 4 LCS-101115- 5 LCS-101115- 6 Averag e ±%RS D "CrPFO S Spike d ConcerrtraOo n (ng/mL ) 0.094 8 0.094 8 0.094 8 Calculate d

Concentratio n (ng/mL ) 0.11 4 0.11 2 0.11 0 %Recover y 12 0 11 8 11 6 118 % ±1.7 % 0.94 0 0.94 0 0.94 0 0.99 0

1.03 1.0 2 10 5

10 9 10 9 108% + 2.1 % ETS-8-044. 0 Analyze d 11/23/1 0 La b I D LCS-101115- 1 LCS-101115- 2 LCS-101115- 3 Averag e ±%RS D LCS-101115- 4 LCS-101115- 5 LCS-101115- 6 Averag e ±%RS D LCS-101115- 7 LCS-101115- 8 LCS-101115- 9 Averag e ±%RS D Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 PFB S

Calculate d Concentratio n (ng/mL ) 0.16 8 0.20 5 0.21 2 %Recover y 84. 6 10 3 10 7 98.2 % ±12 % 1.9 6 1.9 6 1.9 6 1.85

2.1 3 2.0 4 94. 2

10 9 10 4 102 % ±7.4 % 9.9 4 9.9 4 9.9 4 9.1 0

10. 8 10. 5 91. 5

10 8 10 6 102 % ±8.8 % Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 PFH S

Calculate d Concentratio n (ng/mL j 0.18 9 0.21 9 0.22 9 VoRecover y 95. 5 11 1 11 6 108 % ±9.9 % 1.97 1.97 1.97 2.0 1

2.3 7 2.2 7 102

12 0 11 5 112% + 8.3% 9.9 5 9.9 5 9.9 5 10. 1

12. 0 11. 9 10 1

12 0 11 9 113 % ±9.4 % Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 PFOSOineai )

Calculate d Concentratio n (ng/mL ) <0.25 0 <0.25 0 <0.25 0 YcRecover y N/ A N/ A N/ A N/A'' ' 1.9 6 1.9 6 1.9 6 1.9 6

2.3 1 2.1 8 10 0

11 8 11 1 110 % ±8.3 % 9.9 4 9.9 4 9.9 4 10. 4

12. 0 12. 3 105

12 1 12 3 116 % ±8.5 % (1 ) N/ A= No t Applicable ; Arecover

ycoul d no

t b e calculate d as tti e detecte d valu e vira s belowth e limi t o fquantitation
. (2 ) Laborator

ycontro l sampl e di d no

t mee t metho d acceptance criteri a of100 % ±20%
.

Pag e 1 7 o f6 7GLP10-01-02 , Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 6 continued
. LaboratoryContro l Spik e Recovery
. ETS-8-044. 0 Analyzed 11/23/1 0 La b I D LCS-101115-1 0 LCS-101115-1 1 LCS-101115-1 2 Averag e ±%RS D LCS-101115-1 3 LCS-101115-1 4 LCS-101115-1 5 Averag e ±%RS D LCS-101115-1 6 LCS-101115-1 7 LCS-101115-1 8 Averag e ±%RS D PFO S (linear+branched ) Spike d Concentratio n (ng/mL ) 0.19 6 0.19 6 0.19 6 Calculate d

Concentratio n (ng/mL ) <0.25 0 <0.25 0 <0.25 0 %Recover y N/ A N/ A N/ A N/A" " 1.97 1.97 1.97 2.6 3

2.6 3 2.7 3 13 4

13 4 13 9 136 % ±2.1%' ' 9.9 0 9.9 0 9.9 0 12. 9

13. 3 13. 4 13 0

134 135 133 % ±2.2 % "

^ La b I D

LCS-101120- 1 LCS-101120- 2 LCS-101120- 3 Averag e ±%RS D LCS-101120- 4 LCS-101120- 5 LCS-101120- 6 Averag e ±%RS D LCS-101120- 7 LCS-101120- 8 LCS-101120- 9 Averag e ±%RS D PFO S (linear+branched ) Spike d Concentratio n (ng/mL ) 0.19 6 0.19 6 0.19 6 Calculate d

Concentratio n (ng/mL ) 0.29 8 <0.25 0 <0.25 0 %Recover y 15 2 N/ A N/ A N/A" ' 1.97 1.97 1.97 2.0 3

2.3 4 2.2 9 10 3

11 9 11 6 113 % ±7.5 % 9.9 0 9.9 0 9.9 0 10. 3

11. 7 11. 7 105

11 8 11 8 114 % ±6.6 % (1 ) N/ A= No t Applicable ; Arecover

ycoul d no

t b e calculate d a

s th e detecte d valu e wa s belowth e limi t o fquantitation
. (2 ) Laborator

ycontro l sampl e di d no

t meet metho d acceptance criteri a o f100 % ±20%
.

Pag e 1 8 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 6 continued
. LaboratoryContro l Spik e Recovery
. ETS-8-044. 0 Analyzed 12/15/1 0 La b I D LCS-101215- 1 LCS-101215- 2 LCS-101215- 3 Averag e ±%RS D LCS-101215- 4 LCS-101215- 5 LCS-101215- 6 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 0.19 8 0.19 8 0.19 8 Calculate d

Concentratio n (ng/mL ) 0.13 9 0.17 2 0.16 2 %Recover y 70. 3 86. 8 81. 9 79.7 % ±11 % 1.98 1.98 1.98 1.63

1.9 4 1.92 82. 5

97. 9 96. 7 92.4 % ±9.3 % La b I D LCS-101215- 7 LCS-101215- 8 LCS-101215- 9 Averag e ±%RS D LCS-101215-1 0 LCS-101215-1 1 LCS-101215-1 2 Averag e ±%RS D PFO S (linear+branched ) Spike d Concentratio n (ng/mL ) 0.19 6 0.19 6 0.19 6 Calculate d

Concentratio n (ng/mL ) 0.20 7 0.21 4 0.20 0 VoRecover y 10 6 10 9 102 106 % ±3.3 % 1.97 1.97 1.97 2.2 0

2.1 8 2.1 7 11 2

11 1 11 0 111 % ±0.90 % (1 ) N/ A= No t Applicable ; Arecover

ycoul d no

t b e calculate d a

s tti e detecte d valu e wa

s belowth e limi t ofquantitation
. (2 ) Laborator

ycontro l sampl e di d no

t mee t metho d acceptanc

e criteri a o f100 % ±20%
.

Pag e 1 9 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



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

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

yan d precision
. Th e metho d uncertaint yi s calculate d followin g ETS-12-012.2
. Th e standar d deviatio n i s calculate d fo rth e set ofaccurac yresults (i n %) obtaine d fo rth e QC samples
. Th e expande 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 of95%
. Tabl e 7
. Analytica l Uncertainty
. Analyt e PFB S PFH S PFO S Standar d Deviatio n

8.02 6.2 7 15. 2 Metho d

Uncertaint y ±16 % ±13 % ±30 % 

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

e sampl e wa s collecte d a t eac h samplin g poin t t o verif ytha t 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 of fiel d sampl e t o a containe rspike d b yth e laborator

ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o shippin g sampl e container s fo rsampl e collection
. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a o

f100±30 % 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 ofinterest
. Fiel d matri xspik e concentration s must b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike
. Fiel d matri xspike s are presente d i n sectio n 9 ofthi s report
. Tabl e 8
. Fiel d Matri xSpilt e Levels
. Samplin g Locatio n Al l samplin g location s - Lo wSpik e Al l samplin g location s - Hig h Spik e PFBS , ng/m L

0.97 0 9.72 PFHS , ng/m L

0.96 0 9.6 1 PFOS , ng/m L

0.98 0 9.78

FM S Recovery : (Sampl e Concentratio no f FM S - Averag e Concentratio n: Fiel dSampl e & Fiel dSampl e Dup. ) ^

Spilc e Concentrato n 100 %


## 9 Dat a Summaryan d 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 as th e Tri p Blank s an d rinseate blanks
. Results an d averag e value s ar e rounde d to thre e significan t figure s accordin g t o EP Aroundin g rules
. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspik

e recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e tha t th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G WMC L M W2 B 10111 0 - Th e H S recover yfo rPFO S wa s 135%
. Thi s wa s th e onl y appropriat e spike leve l fo rthi s samplin g location
. Th e analytica l uncertaintyha s bee n adjuste d fo r th e samplin g locatio n fo rPFO S t o ±35%
.

Pag e 2 0 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tables
. DA L GWMCLM WI B 10111 0

3 M LIM S I D GLP10-01-02-13-00 1 GLP10-01-02-13-00 2 GLP10-01-02-13-00 3 GLP10-01-02-13-00 4 Descriptio n DA L G WMC L M W1 B 0 10111 0 DALGWMCLMW1BD B 10111 0 DA L G WMC L M WI B LS 10111 0 DA L GWMC L M WI B H S 10111 0 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concentratio n (ng/mL ) 1.98 2.5 4 3.1 7 12. 8 YoRecover

y N A N A N C 10 8 2.2 6 ng/m L ±25%'^ ' PFH S Concentratio n (ng/mL ) 2.9 2 3.6 3 4.0 9 13. 9 YoRecover

y N A N A N C 11 1 3.2 8 ng/m L ±22 % <^

' PFO S Concentratio n (ng/mL ) 6.2 9 8.5 0 7.4 9 17. 6 YoRecover

y NA N A N C 104 7M ) ng/m L ±30Y

o 13C4-PFO S

XRecover y 98. 2 90. 2 99. 9 94. 7 95.7 % ±4.5 % NA= No t Applicabl e (1 ) Th e sample/sampl e duplicat e RP D wa s ^0%
. 

### Tabl e 10
. DA L GWMCLM W1110111 0

3MUIVISI D GLP10-01-02-13-00 5 GLP10-01-02-13-00 6 GLP10-01-02-13-00 7 GLP10-01-02-13-00 8 Descriptio n DA L GWMCLM W1 1 0 10111 0 DALGWMCLMW1ID B 10111 0 DA L G WMC L M W1 1 LS 10111 0 DA L G WMC L M W1 1 H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.52 0 0.46 6 1.7 2 11. 5 YoRecover

y N A N A 12 6 11 3 0.49 3 ng/m L ±11Y

o PFH S Concentratio n (ng/mL ) 1.0 1 0.92 2 2.1 6 12. 3 YoRecover

y N A N A 12 4 11 8 0.96 6 ng/m L ±9.1Y

o PFO S Concentratio n (ng/mL ) 1.56 1.3 7 2.6 1 12. 9 YoRecover

y N A N A 11 7 11 7 1.4 7 ng/m L ±13Y

o 13C4-PFO S

YoRecover

y 95. 6 96. 0 95. 6 10 1 97.1Yo±Z8Yo NA= No t Applicabl e

Pag e 2 1 o f6 7

### Tabl e 11
. DA L GWMCLM WI S 10111 0 GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

3 M LIM S I D GL P 10-01-02-13-00 9 GLP10-01-02-13-01 0 GLP10-01-02-13-01 1 GLP10-01-02-13-01 2 Descriptio n DA L GWMCLM WI S 0 10111 0 DA L GWMCLM WI S D B 10111 0 DA L G WMC L M WI S LS 10111 0 DA L GWMCLM WI S H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D rg A= No t Applicable PFB S Concentratio n (ng/mL ) 1.93 1.60 2.8 4 12. 8 YoRecover

y N A N A 11 1 11 4 1.7 7 ng/m L ±19Y

o PFH S Concentratio n (ng/mL ) 2.4 5 2.0 0 3.3 2 13. 7 YoRecover

y N A N A N C 11 9 2.2 3 ng/m L ±20Y

o PFO S

Concentratio n (ng/mL ) 7.0 5 5.7 8 7.2 1 17. 7 %Recover

y N A N A N C 11 5 6.42 ng/m L ±20Y

o 13C4-PFO S

%Recover

y 87. 7 98. 0 99. 1 97. 9 95.6 % ±5.6 %


### Tabl e 12
. DA L G WMC L MW2 B 10111 0

- 3 M LIM S I D GLP10-01-02-13-01 3 GLP10-01-02-13-01 4 GLP10-01-02-13-01 5 GLP10-01-02-13-01 6 Descriptio n DA L G WMC L M W2 B 0 10111 0 DA L G WMC L M W2 B D B 10111 0 DA L GWMCLM W2 8 LS 10111 0 DA L GWMCLM W2 8 H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 1.25 1.23 2.4 2 12. 1 %Recover

y N A N A 12 2 11 2 1.2 4 ng/m L ±I.6Y

0 PFH S Concentratio n (ng/mL ) 1.36 1.39 2.6 1 12. 7 YoRecover

y N A N A 12 9 11 8 1.3 8 ng/m L ±2.2Y

o PFO S

Concentratio n (ng/mL ) 14. 6 14. 9 16. 2 28. 0 YoRecover

y N A N A N C 13 5 <^ ' 14. 8 ng/m L ±2.0Yo' ^ 13C4-PFO S YoRecover

y 102 97. 1 10 0 99. 9 99.7Y o ±f.9 % NA = Not Applicabl e (1 ) Fiel d matrixspike recover ydi d no t mee t mettio d acceptance criteri a of100% ±30%
. (2 ) Th e analytica l uncertaint ytia s bee n adjuste d fo rFM S recover yt o 100 % ±35%
.

Pag e 2 2 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 13
. DA L GWMCLM W2110111 0

3 M LIM S I D GLP10-01-02-13-01 7 GLP10-01-02-13-01 8 GLP10-01-02-13-01 9 GLP10-01-02-13-02 0 Descriptio n DA L GWMC L MW2 I 0 10111 0 DA L GWMC L MW2 I D B 10111 0 DA L GWMC L MW2 I LS 10111 0 DA L G WMC L M W2 1 H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 2.0 9 2.0 2 3.1 6 12. 8 YoRecover

y N A N A N C 11 1 2.0 6 ng/m L ±3.4Y

o PFH S Concentratio n (ng/mL ) 1.39 1.36 2.5 4 12. 2 YoRecover

y N A N A 12 1 11 3 1.38ng/mL±2.2 % ' PFOS^ ^ Concentratio n (ng/mL ) 5.6 1 4.7 8 6.1 7 17. 0 %Recover

y N A N A N C 12 1 5.2 0 ng/m L ±16Y

o 13C4-PFO S

YoRecover

y 96. 3 96. 0 97. 7 10 3 98.3 % ±3.5 % NA = No t Applicabl e (1 ) Samples wer

e brackete d bya CCV tha t outsid e metho d acceptance criteri a wit h a recover yo f149%
. 

### Tabl e 14
. DA L G WMC L MW3 B 10111 0

3 M LIM S I D GLP10-01-02-13-02 1 GLP10-01-02-13-02 2 GLP10-01-02-13-02 3 GLP10-01-02-13-02 4 Descriptio n DA L G WMC L M W3 8 0 10111 0 DA L GWMC L MW3BD B 10111 0 DA L G WMC L M W3 8 LS 10111 0 DA L GWMC L MW38H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.040 3 0.035 9 1.22 11. 4 YoRecover

y N A N A 12 2 11 7 0.038 1 ng/m L ±12 % PFH S Concentratio n (ng/mL ) 0.033 2 0.032 0 1.2 1 11. 4 YoRecover

y N A N A 12 3 11 8 0.032 6 ng/m L ±3.7Y

o PFO S Concentratio n (ng/mL ) 0.29 3 0.27 2 1.2 2 NA<^ ' YoRecover

y N A N A 95. 7 NA<^' 0.28 3 ng/m L ±7.4Y

o 13C4-PFO S %Recover

y 10 1 98. 3 98. 2 99. 6 99.4Y o ±I.6Y 0 N A= No t Applicabl e (1 ) Sampl e set was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspik e sampl e v*a

s no t analyze d i n thi s mn .

Pag e 2 3 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 15
. DA L G WMC L M W3110111 0

3 M LIM S I D GLP10-01-02-13-02 5 GLP10-01-02-13-02 6 GLP10-01-02-13-02 7 GLP10-01-02-13-02 8 Descriptio n DA L GWMC L MW3 I 0 10111 0 DA L GWMC L MW3 I D B 10111 0 DALGWMCLMW3IL S 10111 0 DA L GWMC L MW3 I H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.027 8 0.028 0 1.1 9 11. 2 YoRecover

y N A N A 12 0 11 5 0.027 9 ng/m L ±0.72 % PFH S Concentratio n (ng/mL ) 0.031 1 0.033 7 1.2 6 11. 1 YoRecover

y N A N A 12 8 11 5 0.032 4 ng/m L ±8.0Y

o PFO S Concentratio n (ng/mL ) 0.26 1 0.26 2 1.2 4 NA'^ ' YoRecover

y N A N A 99. 8 NA'^ > 0.262 ng/m L ±0.38Y

o 13C4-PFO S %Recover

y 96. 5 98. 0 10 1 10 3 99.5 % ±2.9Y

o NA= No t Applicabl e (1 ) Sampl e set wa

s analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspik e sampl e wa s not analyze d i n thi s mn . 

### Tabl e 16
. DA L G WMC L MW3 S 10111 0

3 M LIM S I D GLP10-01-02-13-02 9 GLP10-01-02-13-03 0 GLP10-01-02-13-03 1 GLP10-01-02-13-03 2 Descriptio n DA L G WMC L M W3 S 0 10111 0 DA L G WMC L M W3 S D B 10111 0 DA L G WMC L M W3 S LS 10111 0 DA L G WMC L M W3 S H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.22 11. 3 XRecover y

N A N A 12 6 11 6 <0.025 0 ng/m L PFH S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.2 3 11. 2 YoRecover

y N A N A 12 8 11 7 <0.025 0 ng/m L PFO S Concentratio n (ng/mL ) 0.033 1 0.028 1 0.98 0 NA<^ ) YoRecover

y NA NA 96. 9 NA'^ > 0.0306 ng/m L ±16Y

o 13C4-PFO S YoRecover

y 94. 7 10 1 10 4 10 1 100Yo±4.0Y

o NA= No t Applicabl e (1 ) Sampl e se t was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspike sampl e wa s no t analyze d i n thi s run .

Pag e 2 4 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 17
. DA L G WMC L MW4 B 10111 0

3 M LIM S I D GLP10-01-02-13-03 3 GLP10-01-02-13-03 4 GLP10-01-02-13-03 5 GLP10-01-02-13-03 6 Descriptio n DA L G WMC L M W4 B 0 10111 0 DA L GWMC L MW4BD 8 10111 0 DA L G WMC L M W4 B LS 10111 0 DA L GWMC L MW4BH S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.1 9 11. 1 YoRecover

y NA NA 12 3 11 4 <0.025 0 ng/m L PFH S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.23 11. 4 YoRecover

y N A N A 12 8 11 9 <0.025 0 ng/m L PFO S Concentratio n (ng/mL ) 0.051 1 0.043 9 0.99 1 NA<^ ' YoRecover

y NA N A 96. 3 NA'^ ' 0.0475 ng/m L ±15Y

o 13C4-PFO S YoRecover

y 10 1 102 102 10 6 10r/o±2.2Y o NA= No t Applicabl e (1 ) Sampl e se

t was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspike sampl e wra s not analyze d i n thi s ain
. 

### Tabl e 18
. DA L G WMC L M W4110111 0

3 M LIM S I D GLP10-01-02-13-03 7 GLP10-01-02-13-03 8 GLP10-01-02-13-03 9 GLP10-01-02-13-04 0 Descriptio n DA L GWMC L MW4 I 0 10111 0 DA L G WMC L M W4 1 D B 10111 0 DA L GWMC L MW4IL S 10111 0 DA L GWMC L MW4IH S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.1 8 11. 7 YoRecover

y NA N A 122 12 0 <0.025 0 ng/m L PFH S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.20 11. 7 YoRecover

y N A N A 12 5 12 2 <0.02SO ng/m L PFO S Concentratio n (ng/mL ) 0.14 7 0.14 0 1.1 1 NA<^ ' YoRecover

y N A N A 98. 6 NA<^ ' 0.144 ng/m L ±4.9Y

o 13C4'PFO S

YoRecover

y 99. 9 98. 0 98. 1 102 99.5 % ±19 % NA= No t Applicabl e (1 ) Sampl e set was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspike sampl e was not analyze d i n thi s run .

Pag e 2 5 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 19
. DA L G WMC L MW4 S 10111 0

3 M LIM S I D GLP10-01-02-13-04 1 GLP10-01-02-13-04 2 GLP10-01-02-13-04 3 GLP10-01-02-13-04 4 Descriptio n DA L G WMC L MW4 S 0 10111 0 DALGWMCLMW4SD B 10111 0 DALGWMCLMW4SL S 10111 0 DA L G WMC L MW4 S H S 10111 0 Averag e Concentratio n (ng/mL ) ±%RPD/RS D PFB S Concerrtratio n (ng/mL ) <0.025 0 <0.025 0 1.2 1 11. 7 YoRecovery

^ N A N A 12 5 12 0 <0.025 0 ng/m L PFH S Concentratio n (ng/mL ) <0.025 0 <0.025 0 1.23 11. 7 YoRecover

y N A N A 12 8 12 2 <0.025 0 ng/m L PFO S Concentratio n (ng/mLj ^ 0.26 3 0.24 8 1.1 1 NA<^ ' YoRecover

y N A N A 87. 2 NA<^ > 0.25 6 ng/m L ±5.9Y

o 13C4-PFO S XRecover y 102 99. 3 10 6 104 103Y o ±2.8 % N A= No t Applicabl e (1 ) Sampl e set was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspik e sampl e wa s no

t analyze d i n thi s mn . 

### Tabl e 20
. DA L G WMC L M W13 B 10111 1

3 M LIM S I D GLP10-01-02-13-04 5 GLP10-01-02-13-04 6 GLP10-01-02-13-04 7 GLP10-01-02-13-04 8 Descriptio n DA L G WMC L M W13 8 0 10111 1 DA L GWMCLM W13 8 D 8 10111 1 DA L GWMCLM W13 8 L S 10111 1 DA L GWMCLM W13 8 H S 10111 1 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.096 4 0.10 1 1.3 1 10. 9 XRecover y

N A N A 12 5 11 1 0.098 7 ng/m L ±4.7 % PFH S Concentratio n (ng/mL ) 0.071 1 0.072 2 1.3 1 11. 2 YoRecover

y N A N A 12 9 11 6 0.071 7 ng/m L ±1.5 % PFO S Concentratio n (ng/mL ) <0.025 0 <0.025 0 0.98 7 NA<^ > YoRecover

y N A N A 10 1 NA<^ ' <0.025 0 ng/m L 13C4-PFO S YoRecover

y 10 4 99. 2 98. 9 99. 8 101 % ±2.6 % N A= No t Applicabl e (1 ) Sampl e set wa s analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspik e sampl e wa s no

t analyze d i n thi s mn .

Pag e 2 6 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o f PFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

Tabl e 21
. DA L G W MC L M W 13110111 1

3 M LIM S I D GLP10-01-02-13-04 9 GLP10-01-02-13-05 0 GLP10-01-02-13-05 1 GLP10-01-02-13-05 2 Descriptio n DA L GWMCLM W13 1 0 10111 1 DA L GWMC L M W13 1 D B 10111 1 DALGWMCLMW13IL S 10111 1 DA L G WMC L M W13 1 H S 10111 1 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.087 5 0.081 1 1.2 9 11. 3 YoRecover y

N A N A 12 4 11 5 0.084 3 ng/m L ±7.6 % PFH S Concentratio n (ng/mL ) 0.053 7 0.051 4 1.2 9 11. 7 YoRecover y

N A N A 12 9 12 1 0.052 6 ng/m L ±4.4 % PFO S Concentratio n (ng/mL ) <0.025 0 <0.025 0 0.95 5 NA'^ > XRecover y

N A N A 97. 4 NA<^ > <0.025 0 ng/m L 13C4-PFO S YoRecover y 99. 1 99. 9 10 0 10 0 99.9Yo±0.59 X NA= No t Applicabl e (1 ) Sampl e set was analyze d fo rPFO S o n 12/15/10
. Th e hig h field matri xspike sampl e wa s no t analyze d i n thi s mn . Tabl e 22
. DA L G W MC L M W 13 S 10111 1

3 M LIM S I D GLP10-01-02-13-05 3 GLP10-01-02-13-05 4 GLP10-01-02-13-05 5 GLP10-01-02-13-05 6 Descriptio n DA L GWMC L MW13 S 0 10111 1 DA L GWMC L MW13SD B 10111 1 DA L GWMC L MW13SL S 10111 1 DA L G WMC L M W13 S H S 10111 1 Averag e Concentratio n (ng/mL ) ±YoRPD/RS D PFB S Concentratio n (ng/mL ) 0.097 7 0.093 7 1.2 7 11. 6 YoRecover y

N A N A 12 1 11 8 0.095 7 ng/m L ±4.2 X PFH S Concentratio n (ng/mL ) 0.058 2 0.053 5 1.2 5 11. 5 YoRecover y

N A N A 12 4 11 9 0.055 9 ng/m L ±8.4 X PFO S Concentratio n (ng/mL ) <0.025 0 <0.025 0 0.94 3 NA'^ > YoRecover y

N A N A 96. 2 NA*^ ' <0.025 0 ng/m L 13C4-PFO S YoRecover y 10 4 10 5 98. 7 10 3 103X±2.r/ o NA= No t Applicabl e (1 ) Sampl e set was analyze d fo rPFO S o n 12/15/10
. Th e hig h fiel d matri xspike sampl e wa s no t analyze d i n thi s mn .

Pag e 2 7 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### Tabl e 23
. Tri p Blan k

3 M LIM S I D GLP10-01-01-13-05 8 GLP10-01-01-13-05 9 GLP10-01-01-13-05 9 GLP10-01-01-13-06 0 Descriptio n Tri p Blan k

Sampl e Tri p Blan k

Lo wSpik e Tri p Blan k

Lo wSpik e Tri p Blan k

Hig h Spik e PFB S Concentratio n (ng/mL ) <0.025 0 " ' 1.1 8 <^ > N A 11. 5 <^ > YoRecover y

N A 12 2 N A 11 8 PFH S

Concentratio n (ng/mL ) <0.025 0 *' > 1.2 3 <^ ' N A 11.6'^ ' YoRecover y

N A 12 8 N A 12 1 PFO S

Concentratio n (ng/mL ) <0.025 0 '^

> 0.93 6 <^ ' 1.12'^ ' 10. 9 <^ ' YoRecover y

N A 95. 5 11 4 11 1 N A= No t Applicabl e (1 ) Result

s reporte d fro m analytica l m n 11/23/10
. (2 ) Result

s reporte d ft-om analytica l m n fo rPFO S o n 12/15/10
. 

### Tabl e 24
. DA L G W602 S R B 10102 9

3 M LIM S I D GLP10-01-01-13-05 7 Descriptio n DA L GWMCLM W2 1 R B 10111 0 PFB S Concentratio n (ng/mL ) <0.025 0 '^ ' PFH S

Concentratio n (ng/mL ) <0.0250'' ' PFO S

Concentratio n (ng/mL ) <0.025 0 <^

' NA = No t Applicabl e (1 ) Result

s reporte d fro m analytica l m n 11/23/10
. (2 ) Result

s reporte d fi-om analytica l m n fo rPFO S o n 12/15/10
.

Pag e 2 8 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### 1 0 Conclusio n Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytic^al metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS
. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein
. 1 1 Data/Sampl e Retentio n Al l remainin g sample s an d associate d projec t data (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures
. 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 1 3 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d Attachmen t D : Metho d Deviatio n

Pag e 2 9 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



## 1 3 Signature s

Date 

# ^-^Iz^i ] Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r 

# 3 / x^c^/ / Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yManage r Date



# :7-
. i { Gar yHohemstein/yJ M Sponso rRepresentative 

# (MA / Date



# M Jaisimh a Kesari , stud yDirecto r Date

Pag e 3 0 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t AMorga n Count y^^%%^,f^ff^^fa'cW'^M°01-0 2



### Amendmen t 1 3



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

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

Amendmen t Date : Novembe r9 , 201 0 Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 55144-100 0
Laborator yProjec t Identificatio n GLP10-01-02-1 3
Samplin g Even t Morga n CountyLandfil l - Groundwate rSamplin g



# Exa d Cop yo fOrigina l Inltia i DM

© Pag e 1 o f6 Pag e 3 1 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o f PFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t AMorga n Count y^^')^j\»^i^%ff^^tO%f'&^Mh-0 2



### Amendmen t 1 3 Thi s amendmen t modifie s tli e followin g portio n o f protocol : "Analysi s o f PFOS , PFH S an d PFB S i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

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

PROTOCO L READS : 

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

AMBNDTOREAD : 

### N o change s t o th e wordin g o f th e protoco l ar e required
. Thi s amendmen t orll yaddresse s an d document s th e additio n o fth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o f groundwate rsample s fro m Decatur , AL , an d conducte d a s par t o fth e 3 M Decatu rPhas e 3 Progra m fo rPFOS , PFH S an d PFB S (GLP10-01-02)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e tirhefram e o f Novembe r10-11 , 2010
. Th e groundwate rsample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s project GLP10-01-02-1 3 an d reporte d a s interi m repor t GLP10-01-02-13 , (reflectin g stud yGLP10-01-0 2 an d amendment-13)
.
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 thre e page s i n lengt h an d include d as attache d t o thi s amendmen t fomn
.

Pag e 2 o f 6 Pag e 32 o f 6 7Attactimen t A GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morgan Count

y^^mim^Ymtb'^Wm^-h-0 2



### Amendmen t 1 3 

## Amendmen t Approva l 

# U u WPnmn

i i i O t J Gar yHoheiTistein , Sponso rRepresentative Date 

# yf/2^/^ Clesto n C
. Lange , Principa l Analytica l Investigato r Date 

# ///fA^ / VWIIia m Reagen , EH S Opn s Environmenta l La b Managemen t 

# MX(
. Date 

# i//i<h m Jaisimh a Kesar i P.E. , DEE , Stud yDirecto r Dat e

Pag e 3 o f6 Pag e 3 3 o f6 7Attachmen t A GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morgan Count

y^^mim'f'F^^(oW^f=m}1-0 2



### Amendmen t 1 3 

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

Genera ! 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 : WiM m Reagen , 3 M EHS&Opns ; Environmente l La b

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

Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu r Phas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 13-Morga n CountyLandfil l Groundwate r 

## 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numlje r Projec t Schedufe/Tes t Date s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 flahotiensteIn@miT!m,,:«>'r! 3 M Environmenta l Laborator yManagemen t Willia m K
. Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 w k reaaen<S)mmm
. co m Principa l Analytica l Investigato r Clesto n Lang e 3IW 1 EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 (Jdange^mmrp.com , Samplin g Coordinato r Timoth yFrinal < Westo n Solution s Timothv.frinakSjwestonsolutlons.co m Phone ; (334).332-912 3 GLP10-01^2-1 3 Dep t #530711
. Project #002267444 9 Samplin g schedule d fo rNovembe r10-11 , 201 0 

### Al l verba l an d writte n correspondenc e wil l b e directe d t o GaryHohenstein
. Pag e 4 o f6 Pag e 3 4 o f6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t AMorga n CountyLarj^fil^/Dgc|tyr^L^^No,^e^e^0J_0^^_^ 2 

### Amendmen t 1 3 

## 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 five monitorin g stations
. Eac h monitorin g statio n a t th e facilit yi s constructe d wit h tw o t o thre e wells , monitorin g th e residuum , th e intermediat e zon e (epikarst ) an d bedrock
. Base d o n revie wo fth e wel l location s an d groundwate rflo wpattern s fo rth e site , th e followin g well s hav e bee n selecte d fo rsamplin g an d th e rational e i s provide d fo reac h selecte d location : MW- 1 (S , I , B) ; MW- 2 (I , B) ; MW- 3 (S , I , B) ; an d MW- 4 (S , I , B ) - Thes e eleve n well s represen t downgradien t complianc e well s fo rth e facilitywhich , base d o n groundwate rcontours , monito rflo wfro m mos t o fth e activ e landfil l area . Wel l designation s are : S-shallo wwell , I - Interfac e well , an d B ~ Bedroc k well
. MW-1 3 (S , I , B) - Thi s wel l cluste rrepresent s a n upgradien t monitorin g poin t t o th e landfil l an d serve s a s a backgroun d monitorin g point
. Samplin g location s wil l b e analyze d fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfiuorooctanesulfonat e (PFOS ) a s par t o fth e Morga n CountyLandfil l groundwate r sampling
. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC AGoo d Laborator y Practic e Standard s 4 0 CF R 792
. Groundwate rsample s fro m Decatur , A L wil l b e collecte d byWesto n Solution s personne l Novembe r10-11 , 2010 , Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensure tha t result s fo rPFBS , PFHS , an d PFO S ar e ofa know n precisio n an d accuracy . Th e final repor t wil l b e submitte d t o Gar

yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m report GLP10-01-02-13
. 

## 3 Projec t Schedul e Sampl e collectio n bottle s vwl ! b e prepare d b y3 M Envinanmenta l Laborator yforsamplin g Novembe r10-11 , 2010
. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo ranriva l o n Wednesday , Novembe r 10 , 2010
. Sampl e bottle s shoul d b e store d refrigerate d on-sit e unti l sampl e collection
. Marti n Smit h \

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

## 4 Tes t Parameter s Th e targete d limi t o fquantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFBS , PFHS , an d PFOS
. Atota l o ffourtee n samplin g location s have bee n specified
. Fo reac h samplin g location , a tota l o ffou rsampl e bottle s wil l b e collecte d (sample , sampl e duplicate , low-leve l field matri xspike , an d high-leve l field matri x spike).Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e txJttl e wil l b e 20 0 mL
. On e se t o ftri p blank s consistin g of reagent-grad e water , a low-leve l tri p blan k spike , an d a high-leve l tri p blan k spike wil l b e prepare d a

t th e 3 M Environmenta l Laborator

yan d sen t t o th e samplin g locatio n wit h th e othe rtwttles
. Th e lowfield matri xspike wil l fcie prepare d a t 1 ng/m L an d th e hig h field matri xspik e a t 1 0 ng/mL
. Tw o additiona l bottle s wil l be prepare d t o b e use d fo rth e preparatio n o fth e equipmen t rinseate blanks
. I n additio n t o frie sampl e bottles , a 1-L containe ro fMill i Q wate rwil l b e include d t o b e use d fo rth e preparatio n ofth e rinseate blanks
. Al l sampl e bottle s wil l includ e frie additio n of'®Oz-PFBS , ^^Oz-PFHS , an d ^^Cn-PFOS
. 1802-PFB S (interna l standards ) at a nomina l concenfi^tio n of1 ng/mL
. Al l sampl e bottle s wil l als o includ e th e additio n of"C4-PFO S (surrogat e spike ) a

t a nomina l concentratio n o f0. 1 ng/mL
. Atota l o f6 1 sampl e bottle s wil l b e prepared
.

Pag e 5 o f6 Pag e 3 5 of6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t AMorga n Count y^^M^i^m)^l^o^ll^tPfd^dl-0 2



### Amendmen t 1 3 5 Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 0 "Detenninatio n ofPerfluorinate d Compound s I n Wate rb

yHig h Perfbmianc e Liqui d Chromatography/Mas s Spectromefr yDirec t Injectio n Analysis"
. Alternately , sample s ma yb e analyze d b

yETS 8-154. 3 "Determinatio n o fPerfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry
. Where applicable , sample s wil l b e analyze d against a n interna l standar d calibratio n curve . Eac h curve poin t wil l contai n isotopically-labele d PFBS , PFHS
. an d PFO S a t a nomina l ojncentratio n o f1 ng/mL
. Th e calibratio n curve wil l b e generate d b ytakin g tti e rati o ofth e standar d pea k are a counts ove rth e interna l standar d pea k are a counts t o fit th e dat a foreac h analyte
. Laborator ycontro l sample s prepare d wit h th e sample s must have a n averag e recover ywithi n 100±20 % an d a RS D 520%
. Th e dat a qualit yobjective fo rthi s stud yi s quantitative results forth e targe t analyte s wit h a n analytica l accurac

yo f100±30%
. Fiel d matri xspike s not yieldin g recoverie s wthi n 100+30 % wil l b e addresse d i n Bi e repor

t an d th e final accurac

ystatemen t ma

yb e adjuste d accordingly
. 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e results forth e sample , sampl e duplicate , an d th e two field matri xspikes
. Tri p blan k an d tri p blan k

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

s ofreagen t wate rprepare d a t ttie tim e ofsampl e extractio 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 where th e field matri xspike leve l wa s not appropriate , du e to highe rtha n expecte d analyt e concentrations , a laborator ymatri xspii<e ma

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

Pag e 6 o f6 Pag e 3 6 of6 7•ETS-Mar yAn n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^is^SiP f^i.? fnS9??f359?di P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# •

( 0 

### <

ro < B ">
. a s m101123a.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -0.0080 8 x'' 2 + 1.2 9 x+ 0.017 3 ( r= 0.9993 )
46 - 44 - 42 - 40 - 38 - 36 - 34 - 32 - 30 - 28 - 26 - 24 - 22 - 20 - 18 - 16 - 14 - 12 - 10 - 8 - 6 - 4 - 2 0 - 

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

y y y y y 

# y / /

0 2 4 6 8 1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 3 0 Analyt e Cone
. /

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. ^ • ^



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.

5 0 Dat a worke d up byST W Printin g Time : 11:10:2 0 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 3 7 of 6 7••ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^^^g^f f^^^FHJSgP^falJPPdi P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# •

ra ( D 

### <

< D a > 

### < B 

### *> * 0 ! C 

### < mIO l 123a.rd b (PFHS) : "Quadratic " Regressio n (" 1 /x " weighting) ; y= 48- 1 46 - 44 - 4 2 40 - 38 - 36 - 34 - 32 - 30 - 28 - 26 - 24 - 22 - 20 - 18 - 16 - 14 - 12 - 10 - 8 - 6 - 4 - 2 0 - y y y

y '

y y y 

# y ' 

# y 0 5 1 0 1 5 -0.0059 1 x'^ 2 -H.1 9 x-

H 0.015 2 ( r= 0.9996 )



### " ^

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## ,/-" • X y ' y y y y 

### y

2 0 2 5 3 0

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. /

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. 

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yST W Printin g Time : 11:10:3 4 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 3 8 of 6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi mRepor t 1 3 Analy^elf f^^? fHlSe^^lfs^Pai P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# •

TO 0 ) 

### < C O 2 < O J > * TO c < mIO l 123a.rd b (PFOS) ; "Quadratic " Regressio n (" 1 / x " weighting) : y= -0.0097 3 x'' 2 + 1. 5 x- H 0.25 1 ( r= 0.9992 ) 5 4 5 2 50 - 48 - 46 - 44 - 42 - 40 - 38 - 36 - 34 - 32 - 30 - 28 - 26 - 24 - 22 - 20 - 18 - 16 - 14 - 12 - 10 - 8 - 6 - 4 - 2 0 - ^'' '

X ' y ^ y' k X ' y ' ^ X X y ^ y ^ 

## y ' y y ' y ' 

# y ' y y 

# y y 

# y

/ 0 5 1 0 1 5 2 0 2 5 3 0 Analyt e Cone
. /

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p b yST W Printin g Time : 11:10:5 0 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 3 9 o f 6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy§iS3g^f f^^5F^^g55lf3|9g^^5 , Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 mIO l 123a.rd b (13C4-PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -0.0 2 x* 2 + 0.99 2 x+ 0.026 1 ( r= 0.9998 )
8.0 - 7.5 - 7.0 - 6.5 - 6.0 - 5.5 - 5.0 - 4.5 - 4.0 - 3.5 - 3.0 - 2.5 - 2.0 - 1.5 - 1.0 ^ 0.5 - 0.0 : 

### • ^ / • ' / / /

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

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

p byST W Printin g Time : 11:11:1 2 A M Printin g Date ; Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 4 0 of 6 7"ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^is^gl ff^^PF^1S95t^f350g^i5 l Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

SampteName;-m101123a019 - SarT^t e rO : "10007-6-8 - PeakName:-13C4-PF0S - Pttess^es):-503.0/80. 0 amu " I Cor>wnent-1.0n9AnLFC«tdin95%Synth.V*ter/5%ACN Fte;-m101123a.wi r Annotation;" "
Concentration : C»Unl3i:« dCone : Acq . VAZb-
. Acq . Ti.T.e : H=Ji£ied : Proc . Alqorichn : Mil.
. Pta k

Hfiioh t Hin

- Pea k

Vlidth : ?noot!iin qWidth : S T WinJ^jw : Expecte dKT : O.sS i n g ii.SO O n q 11/2J/201 0 •:<6:? 3 P

H Ko Int^lliCua n- : 0.0 0 cf.-E 0.0 0 sa c 0 pui n 30. 0 .•^ec 15. ? mil , O

L n.l
.

I'. '
3 2.10 5

2.0. 5 1.9e 5 ,.8. 5 ,.7. 5 1.6e 5 1.5e 5 1.4 ^ 1.3e 5 1.2o 5 l.le S 1.0- 5 9.06 4 8.0 ^ 7.0» 4 6.0e 4 5.0e 4 4.0m A 3.0a 4 2.06 4 1.0e 4 1 5 2 7



## 1 L I Sampl e Name:'m101l233034 ' Sampt o 10 ; PeakNama;-13C4-PFOS ' Mass(«s):-S03. ' I Comnwnt'2ppbLCS/1ppbsun'ogatBLCS " •LCS-101115-4 - File;"m101123a.wi r .0/80. 0 amu " Annotation : " Sampl * Type : <:*lcuUt« d <

. 0,94 0 nq/n L

0.9S 0 nq/m L 11/23/201 0 9:00:1 8 P

M

PH«> ; H^igtit : Pea k Width : .ihini j Width : it-lliQu ; O.D O 0.0 0 B T Ki ; Expflf.pr i R

T Us e R«lativ
. Int
. Typfl : nr.i o H«iql v Vslle y 15. : e:7&e i =

< 212000 . < 15. 1 lb. 7 2. 1 e S ZOft S 1.9e 5 1.8. 5 1.7« 5 1.66 5 1.Se 5 1.4« 5 1.3e 5 1.2B 5 1.le 5 1.06 5 9.0e 4 e.0« 4 7.06 4 6.0e 4 5.06 4 4.06 4 3.0* 4 2.06 4 1.0* 4 15.2 4

L 1 4 1 6 1 8 

# I Sampl e Name : "ml01123a048 - Sampl e ID ; "LCS-101115-15 " FBe;-fn101123a.wi r Pea k Name : -13C4-PF0S - Mass(e5) : -503.0^0. 0 amu " Commen t '2pp b LC S EC P Annotalion;" " 

# I Sampl e Name : "m10ll23a060 - Sampl e ID ; Pea k Name : -13C4-PF0S ' Mass(as) : "503. ' Commen t 'OA L GWMC L M WI B 0 101110 " ampl e Index : £ 1 ampl e Type : Vnfcnow n oiicon t ration : H/ A alculatf dCone : 0.097 4 nq/m L 11/24/201 0 6:04:i 5 A

M AC4
. • Mod1i , [l o •GL P 10-01-01-13001 " Fito;"m101123a.*Mf r .0/80. 0 amu ' Annotation ; ~
Z56 4 2.464 - Z36 4 2.26 4 Min
. r«a k

Widt h Sn.oothin yWidt h R TKiiidov : E.-.pact« d RT : Bas e T 3 Bas e 15. ^ mi n 9517 1 count s 253O0 . cp s 15. 1 mi n 15. 5 mi n 2. 1 e 4 2.06 4 1.96 4 1.86 4 1.7e 4 1.66 4 l.Se 4 1.46 4 1.3e 4 1.264 - 1.1e 4 1.0* 4 9000. 0 BOOa. D 7O0O.0 - 6000. 0 5000. 0 4000. 0 3000.0 - 2000. 0 1000, 0 0. 0 16.6 4 1 2 1 4 1 6 Dat a worke d u

p b yST W Printin g Time : 11:13:2 0 AM Printin g Date : Wednesday , Januar y2 6 , Pag e 1 o f 9 Pag e 4 1 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^is^g^f f^^^Fh^g5i5!f3^0g, p Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

•Sampl e Name : •'ml01123a083 " San ^ ID : "Metho d Blank " Fde:'ml01123a.<M r I Pea k

Name:-13C4-PF0S - Ma»s<es):-503.0/80. 0 amu * I Comment : "1 0 005-229 " Annotation;" " .^anpl t Index : 9 4 Simpl fTypo : "nkno-v n Concentration : N/A Calculate d Cone : flr^. D*t« : Acq
. Time : M^Jiri«J : Proc
. Algorithm : Min
. P«af cH.;igh t Min
. Faa k

Hidth : Smoothin g Width : R TVJinduw : Expecte d f<T : Us e Relativ e RT : Inc
. Type : Retentio n Tin.e : Area : Haiqht : Star t Tirae : En d Time : • ; 0 11/2J/ 2 2:06:2 4 N o Incoll i 1 0.0 0 0.0 0 0 .iO. O N o bas p T o 15. 2 iI15 5 soil)
. 15. 1 15. 4 1 0

P M
\ i a

B a

- P 0.95 0 ng/m L ti/ A 11/23/2L'1 C J:46:2 J P

M 2.3*5 1 2.2* 5 2.16 5 2.0* 5 1.9* 5 1.8* 5 1.7* 5 1.6* 5 1.5* 5 1.4e 5 1.3* 5 1.2* 5 1.1* 5 1.0* 5 9.0* 4 8.0* 4 7.0* 4 6.0* 4 5.0* 4 4.0* 4 3.0* 4 2.0*4 - 1.0* 4 15.2 7



# i T 

# I SampI * Name : -m101123a034 - Sampl e ID ; "LCS-IOI115-4 ' Fll* : -m101123a.w( r Pea k Name : "MBPFOSflS) - Mass{e») ; "507.0/80. 0 amu " Commen t •2pp b LCS/ 1 pp b sunngat * LCS - Annotation; ' Sampl e Index : i ^ Sampl e Nam*;-mIO l 1238048 - San^ID : •LCS-101115-15 - Fi«e:"m101123a.iM r Paa k Nam* : -M8PF0S(IS rMass(es) : -507.0ffi0. 0 amu " Commen t •'2pp b LC S ECF " Annotation;" "
tion : 0.54 4 Calculate dCone : N/ A Arq . Ddt« : \l/2:/2i
. Ac'.j
. Tine : S:CO:l a M-'difit-d : ¥e j Proc . Algorithm : Intelli t Hin
. Peak : Height : 0.0 0 Min
. real : Hi^tii : 0.0 0 .'!^rt>othi.^ g Vlidth : 0 R T Wi:idrji.- : 30. 0 Etf.act5 dRT : 15. 3 I's e Relativ e BT : N o ny/ r

6e-00 5 cp s 15. 1 mil l 15. 0 n,i n Sampl e Type : Calculatn d Cone : Acq
. [Mte : AC'j
. Tima : M.jdlfibd : Proc
. Alocrithr.. : Hin
. Pea k

Heigfi t Hin
. Pea k

Widtli : Sn.oC'thin a Width : R TKindu-v : E-nacta U RT : Us e Relativ e RT : Int
. Type : R.ttntio n Tir,* : Area : 7 H«iqhr : o c 0.95 5 H / A n/24/21M 0 1:53:2 7 AM Y « S lnt«!!iQ'J a 0.0 0 0.0 0 0 P 1-0
. n 15. 3 N o Valle \ 15. 2 75S 2 co u .S43'00 5 1.9* 5 1.8* 5 1.7* 5 1.6* 5 1.5* 5 1.4* 5 1.3* 5 1.2* 5 1.1* 5 1.0* 5 9.0* 4 6.0* 4 7.0* 4 6.0* 4 5.0* 4 4.0* 4 3.0* 4 2.0* 4 1.0* 4 15.2 3

L1 Dat aworke du p b y ST W Printin g Time : 11:13:2 0 A M Printin g Date : Wednesday , Januar y 26 , 201 1 Pag e 2 o f Pag e 4 2 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^|?38if f^^P fK|ag5,5lf3l|Op^i p Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

Proc
. Min
. Kmu^j t R TV I i Expa ^ Algorithm : ^eal : Hpi(3ht : l-sa KHidth : •.iii g Width : te d RT : Inte l lit '

0.0 0 O.QO 0 .^O. C 15. 3 .i n -

c p =

m m 

# I Sampl e Nam* ; "011011233060 - Sampl e )0 : "GLP10-01-01-13-001 ' File ; "m101123o.mif r Pea k Name : -M8PF0S(!S) " Mass(es) : "507.0/80. 0 amu " Commen t "DA L G WMC L M W1 B 0 101110 ' Annotation : " " £in[>l e Typp : Mnkno'^ n ,1.56 0 ng/ri, L - _ N/A^-^ ^ 11/24/201 0 6:04:i 5 A

M 1 •8« 5 YG3 1.7e 5 1.6* 5 1.5* 5 1.4* 5 1.3* 5 1.2* 5 1.1* 5
^ l.Oe S a I 9.0* 4 8.0* 4 7.0* 4 6.0* 4 5.0e 4 4.0* 4 3.0» 4 2.0* 4 1.0e 4 Hfii.jht : St^c t Ti t En d Time :

0. 0 1 2 1 4 1 6 

# I Sampl B Name ; "mlO l 123a083 " Sampl e ID ; "Metho d Blantc " Fite ; -m101123a.wi r Pea k Name : "M8PF0S<IS) " Mas5(*s) ; "507.0/80. 0 amu " Commen t "10.005-229 " Annotation;" " iarafjl* ^ Index : 84 iampl e Type : Unkncv n :oncenrtitiori : 0
. 95 0 ng/m L ;alculat6 d Cone : H/A

•«3i : Hiiqh t 'ea k Widrh : dn< j Width :

•er i RT : 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0e 5 1.8* 5 1.6* 5 1.4*5 - 1.2* 5 1.0*5 - 8.0* 4 6.0* 4 4.0* 4 Z0e 4 152 3



### » 1 2 1 4 1 6 

# I Sampl e N3me:-m101123a019 " Sanpl * 10 : "10007-6-8 " Pea k Name ; "MPFBS{IS) - Mas&(es) : "303.0/84. 0 amu " Commen t "1. 0 ng/m L F C sl d i n 95 % Synth
. Wat*r/S%ACN " Cilcrjlater i Acq
. D,,t« ; Acq
. Tims : FBe:-m101123a. » Annotatiofi:" " 

# I Sampl e Name ; "ml01123a034 - Sampt e ID : •LCS-101115-4 " File ; "m101l23a.wi«fr ' Pea k Name ; "MPFBS{[S) " Mass(*s) ; -303.a«4. 0 amu " Comnwn t "2pp b LCS/lpp b tuffogat e LCS " Annotation:" "

0 . 7 5 N / A 11/ 2 3: 4 6 / 2

' ¥« s Int e 0 1 0 P H UOua n 0 0 c ?n,oothin q Hi R TWindow : Exp^cts d RT : 4.0* 5 3.6* 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 2.0* 5 1.8* 5 1.6*5 - 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0*4 - 4.0* 4 2.0* 4 12.6 1

L ^ p i e Type : culate dC

. Date :

. Tirae : ified : c . Al^cr i

. Pe.3 k H e

. Pea k W i orhin y W

i Window : «Cts J BT : Relativ e

. Type : entio nT i J : Qhr : r t Tim« : Time : n c

hr a g h ti l T h

R T



### . , Q C 0.95 5 H/ A 

### , . n g 11/23/201 0 S:0O:i e P

H Y s 3 IntelliQ i : 0.0 0 I'O. O 12. 6 N o Valle y 12. 6 171257 4 C

O 3.S4.3-00 5 12. 4 13. 3 a n-

c p s pcjin t m i n

. . n lint s c p s rain rain raL

l O A 

### ^

t 3.6* 5

3.4*5
- 3.2* 5 3.0*5
- Z8e 5 2.6*5
- 2.4e 5 2.2* 5 2.0* 5

1.4e S 1.2*5 - 1.0* 5 8.0* 4 6.0* 4 4.0e 4 2.0* 4 1 6 1 8 0.0 - 1 2 1 4 Dat a worke d up b

yST W Printin g Time : 11:13:2 1 AM Printin g Date ; Wednesday , Januar y26 , 201 1 Pag e 3 o f 9 Pag e 4 3 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analym8l? f^Ya? fnag^'JfslOaf fGroundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

Pro= . Algorithm : Miti

- pMa k

Height : Min
. Paa V WiJtti : Smoothin g Wirtth : R T VJinduw ; Expecte dRT : Vs aRelativ e BT : Int . Tipe : Retantio nTlrae : Atoa : 1S 7 H«i^tit : i IntflliQua n 0.0 0 c 0.0 0 s 0 y. a 30. 0 3 1?. S m N o Valle y 1 i
. S n . 717 acou n .S6«-00 5 C

F •Sampl e Name ; •m101123a048 " Sampl e ID:'LCS-101115-15 " FH*;-m101123a.wi r I Pea k Name ; -MPFBS(IS) - Mass(*s} : -303.0«4. 0 amu ' I Comnn*nt : "2pp b LC S EOF " Annotation:" - .-ampl t Indar : 4 5 aispl fTypn ; v c C-~n'-entracion : O.ST O ng/r. L Caic.i!ar« d Cone : N/A^•^' ' Af^ . D-tt^ : 11/24/201 0 Acq
. Time : 1:53:: ' AM 3.4* 5 3.2* 5 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 &
. 2.0* 5

» 1.8* 5

- 1.6* 5 1.4* 5 1.2* 5 1.0* 5
6.0* 4 4.0* 4 2.0* 4 0. 0 

# I Sampl e Nam* ; 'mIO l 123a060 - Sampt e ID : -GLP10^1-01-13-001 - FOa ; "mlO l 123a.wi r P*a k Nam* : 'MPFBSdS) - M3Ss{*s} ; "303.0/84, 0 amu Comm*n t "DA L GWMC L M WI B 0 lOIHO ' Annototkin : - SatTf-l e lr,de}i : G l Concentration : 0.97 5 n'j/n i x-Lj
. LMte :

jmoothin qWidt h K T Window : Eipec-e d ftT: it^Uiptjai i - IQ A 0.0 0 cp s 0. 0 0 s« c 3.2* 5 3.0* 5 2.8* 5 ^6* 5 2.4* 5 2.2* 5 2.0* 5 1.6* 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0*4 - 4.0* 4 Z0* 4 0. 0 1 6 1 8 

# I Sampl e Name : 'm1011233083 ' Ssm; ^ ID : 'Metho d Blank " Fie : "m101123a.wi r Pea k Name ; -MPFBS(IS) - Masses) : '303.0/84. 0 amu ' Comnwnt : "1 0 005-229 " Annotalion;" "
Cili:ul.--tn d Cone : N/A flc^. D-.t« : 11/24/201 0 AC-J
. Ti!l,s : 2:06:: 4 P H Proc
. Algorithm : Intelliiua n - I^ A Min
. pea k

Height : 0.0 0 cp s Hin
. Tdak
. Hidth : 0.0 0 se c ."imoothin q Width : 0 point s R TKiiid.ju : 20. 0 E« C V'5 e R-iativ e FIT : N o Int
. Tipe : Valle y Retentio n Time : 12. 8 mil
. Area : 154564 3 count s Hoiqht : i.70n'00 5 cp s En d Tiae : 13. 2 n,i n 

### & £ • 3.6* 5 3.4* 5

3.0* 5 2.8* 5 Z6* 5 2.4* 5 2.2* 5 2.0* 5 1.8* 5 1.6* 5 1.4*5 - 1 A 5 1.0o5 - 8.0* 4 6.0* 4 

# I SampI * Nam*;-m10n23a019 ' Sampt o ID ; "10007-6-8 " Paa k Name : "MPFHSdS rMas*(*») ; '403.0B4. 0 amu " Comm*n t "1. 0 ngftn L F C st d i n 95 % Synth
. V\bter/5%ACN " sampl e Type : Standar d 0.9 4 5 ri'j/ra L ite d ; N/ A Acq
. Dac^ : Acq
. Time : tloditied : Proc
. Alv^t-cithm : Min
. Pea k

Height : Min
. Pfca t Widrh : Sraoothin q Width : R TKindo-* : E-p£Ct5 d RT : L's e Relativ e RT : Int
. Type : R-tentio n Time : H3ig.-,t : 1 En d Time : 1/23/201 0 : 46:2 3 P

M N o ntelli'J.ia n - 0.0 0 cp s 0.0 0 se c 0 poin t :-0. 0 s« c 14. 3 mi n H o Valle y 14. 3 rain 44 2 count s 57.S.00 5 cp s 15. 0 mi n I D A 

### '
& 

## f 3.4* 5 3.2* 5 3.0* 5 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0* 5 1.8* 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0* 4 4.0* 4 2.0* 4
1 6 1 6 Dat a worke d u p b yST W Printin g Time : 11:13:2 1 A M Printin g Date : Wednesday , Januar y 26 , 201 1 Pag e 4 o f9 Pag e 4 4 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^^s^g^f f^^^Fh^g5i^f3|9P^i5 , Groundwate rSample s Morga n CountyLandfill
. Decatur
. A L - Novembe r201 0 

# r Sampl a Name ; "ml01123aO34 ' SampI * ID ; "LCS-101115-4 " File ; "m101123a.wif r Pea k Name ; -MPFHS<IS) " Ma»s<*s) ; '403.0/84. 0 ami / Commen t '2pp b LCS/ 1 pp b eurrogal a LCS " /Annotation : Sampl e Indoy : 3 5 S^!T.f>l e Type : yc ^ Concenitition : .1.92 5 nq/oi L Cal-;'i;at.e d Cone : N/A Af4
. DrfC« : l]/2;-/201 0 Acq
. Time : 9:00:l e P M Proc . Algoritli:r. : IntPlli'Ju
. Min
. Pwa k

H.>iij|-]t : 0.0 0 Min
. Peal : Ui-ith : 0.0 0 Smuijthin qWidth ; 0 [ R T Wind.)v : iO. C Expecte dRT : 14. i Us e Relativ e RT : H o Int . T\pe ; Valle y Betentio.- i Time : 1 4 . i Area : 13 7 i97 5 co i Height : J.27«.&C 5 Jtsr t Tine ; 14. 1 En dTim3 : 14. 9 Sampl e Nam* ; "ml01123a048 " Sampl e ID:'LCS-IOIIIS-IS ' File:'m101123a.wjf r Paa k Nam* : *MPFHS{IS rMaM(*») : "403.0ffl4. 0 amu " Commen t "2pp b LC S ECF " Annotation ; ~ Sampl e Typo : C.K T calculate d Cone : Il/ A3.3, 5 Acq . L'-ta : 11/24/201 0 Acj . TimB : 1:52:2 7 A M 3.0* 5

" ^ 2.6*5 .

2.6*5
- Z4* 5 2.2* 5 Z0* 5
a . 1.8* 5 I 1.6*5
- 

### I 1.4* 5 1,2* 5 1.0* 5 8.0* 4 6.0*4 ' 4.0* 4 2.0* 4 Pcou . Alqcrith m Hin
. P«3 k

Heigl i Hin
. P«a k

Widr n Smootninr j wijc h R T Kjnd!;-J : Expecte dRT : Us e Relativ e S T Int . Tvpo : Ratsntior , Time : Acaa : 1 H-.iqt,t : Star t Tin,* : iritelU Q

: 0.0 0 0.0 0 C ;-o. o I J . 3 H o 7a[le i 14. 3 6063 3 =

C 3..'l.i»0C 5 11. l

0. 0 

# I Sampt e Name ; "m101123a060 ' Sampt a ID;'GLP10-01-01-13<»1 " Fil* ; •m101123a.vi(i r Pea k Name ; -MPFHS(IS) - Mass(*s) ; "403.0/84. 0 amu CommenL"D/y.GWMCLMW1 B 0101110 " Annotation : ~ Sampl e Index : 6 1 Concen t

ra t i-in : 0.S 4 5 ny/n-. L Calculater i Cone : N/ A Ac-q . Dat.: : 11/24/201 0 Ac^ . Tir^£ : 6:04:3 5 A H

Area : 1225S5 2 count s Height : 2.95e»00 5 cp s Star t Tima : 14. 1 mi n En J Time : 14. 9 n.i n s 2.8* 5 2.6* 5 2.4* 5 2.2* 5 2.0* 5 1.8* 5 1.8* 5 1.4* 5 1,2* 5 l.Oe S 8.0* 4 6.0* 4 4.0* 4 2.0* 4 1 4 2 5

L 

# I SampI * Name ; -m101123a083 - SampI * ID ; "M*tho d BlanK " Fil* ; 'm101123a.wif r P*s k Name : "MPFHSflS rMas«(*a) ; •403.0fi4. 0 amu " Comm*n t "1 0 005-229 " Annotation ; " " Sampl e Inrtex : 9 4 Sampl e Type ; Vnknowt i Concentra rion : 0.94 S n^/m L Calculate d Cone : rl/ A Acq . Vit-. : ll/24/2in O 3.8* 5 Acq . Time : 2:06:2 4 P H 3.6* 5 I1-.3dilie.l : H o Proc . AlocritMiT, : intelliOJ^ n- IQA34^5 . Mill , pea k

Height : 0.0 0 t-p s Min
. P*. k

Widr.^ : 0.0 0 ,e c ^^^^ ^ Stficjothin o Hidrn : 0 point s R T Kitidu-v : :T.. 0 S^ C E.-f.«cte dBT : 14. 3 mi n3.0*&- i li* e Relaci-/ s RT : M o 2.8* 5 Int . Type : /alU i R-tontio nTi=e : 14. 3 mi nZ6* 5 2.4* 5 I 2.2*5 -

' \ ZOeS - ; 1.8* 5 1.6* 5 1.4* 5 1.2* 5 1.0*5 - 8.0* 4 6.0* 4 4.0*4
- 2.0* 4 IS5274 5 co(int s 3.ESe-O0 5 cp s 14. 1 mi n

0. 0 1 2 1 4 Dat a worke d u p b yST W Printin g Time : 11:13:2 2 A M Printin g Date : Wednesday , Januar y 26 , 201 1 Pag e 5 o f9 Pag e 4 5 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Anafy^^^g^f f^^|FHtag?<ilf350p^i5 i Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# ( Sampl e Name : •m101123a019 " Sarrvl e ID ; -10007-6-8 " File : "mlO l 123a.wi r Pea k Hume : "PFBS " Ma5«(*s) ; "299.0ffi0. 0 amu,299.Qf99. 0 amu ' Comment ; "1. 0 ng/m L F C st d i n 95 % Synth
. \ftfat*r/5%ACN ' Annotation ; " " FampL e Indt./. : 2 0 Sampl e Typ» : itandar d Concentration : ?.S9 5 ng/m L Cal'jiilate dCone : 1.0 7 ncj/m l 5 : Ar-ij
. Dat*, : ll/2;"/201 0

Rela--iv e R

T Tlpe : ntio nTime : : 2. . lir : 4 .

5 5 N o lanua l 12. 6 2« 1 4000 .

8

- 3.0* 5 

# I Sampl e Nanfie:"ml01123a034 " SampI * ID : "LCS-101115^1 " Fito ; "m101123a.iM r Pea k Name ; "PFBS " Mass(es) : "239.0/80. 0 amu,299.0/99. 0 amu " Comn^n t "2pp b LCS/lpp b sun-ogat e LCS * Annotalion ; 1.5 Gnq/ra L 1.B 5 ng/m L 1/23/201 0 • : 00:1 8 P

M



# I Sampl e Name : "m10n23aO48 " Samp h ID:'LCS-IO I 115-15 ' FBe:'m101123a.wi r Pea k Nam* : "PFBS * Ma5s{*s) ; "299.0/80. 0 amu,299.0/99. 0 amu " Commen t "2pp b LC S EC P Annotation;' " S.'impl e Type : Q C Concentration : 0.0 0 ng/m L Calculate dCone: : 0.016 0 ng/m L Ac-,? . Date : 11/24/201 0 1,5* 4 Ac-j
. Ti=is : 1:53:2 7 AM N o Intellig i : 0.0 0 0.0 0

12. S 6J4S 2 c c 1S200 . ; 12. 5 12. B 1.3* 4 1.2* 4

^ 8000.0
-

- 7000. 0 6000.0
- 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 

# L [ Sampl e Name : -m101123aD60 ' Sampl e ID : 'GLP10-01-01-13-001 ' File ; 'm101123a.vKf r Paa k Name : "PFBS " Mass(*s) : "299.0/80. 0 amu.299.0/99. 0 Commen t 'DM
. GWMC L M WI B 0 101110 " Annotation ; Cancentratlon : N/ A Calculate dCone : 1.S B i Acq . L-ato : ll/24/2i^l O ACfj
. Time : 6:0 4 : i hA H H-:;dified : Ye s R T Windo-J : 30. 0 s i Expecte dRT : 12. 6 m Us e Relativ aBT : N o

Dat a worke d u

p b yST W Printin g Time : 11:13:2 2 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 6 o f 9 Pag e 4 6 o f6 7••ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analyas38i§ f^^^ fH|a955'f3l??di P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0



### • Sampl e Name ; •m101123a083 " SarT^I * ID ; •M*tho d Blank " File ; 'm101123a.wi r Pea k Name ; "PFBS " Massjes) ; -299.0/80. 0 am i Comment : '1 0 005-229 " Annotation : • " -''arapl o lndu>: : 3 4 Sampl e Type : Unkno-w n Con'-entration : N/ A Calculate d Cone : • ; 0 Ar-.] . Dat« : Acq . Time : HcJitiud : Proc . Algorithm : Hin
. P«al ; Heigh t Min
. Pea k

Hidth : Smoothin g Hidth : R T Window- ; Expecte dRT : U3 B R«lativ e RT : Int . Type : Retentio nTime : Area : H«ight : Ctar t Time : En dTime : 11/24/ 2 2:06:2 4 N o Intell i : 0.1) ( O.O i 30. 0 12. i N o Valle \ 12. 1 LOSl ! 250D . 12. 5 12. 7 Oil ) P M

poin t mi n

coiint. f t p s mi n :o A 

# I SampI * Nam* ; "mlO l 1233019 " Samf ^ ID ; "10007-6-8 " File : "m101123a.w4i r Pea k Name ; 'PFHS ' Mass(es) : '399.0/80. 0 amu.399.0/99. 0 amu " Comm*n t '1. 0 ng/m L F C st d i n 95 % Synth , Water/SWACN " Annotation ; " S.impl e Typ- : calculate dCon e Ac;j
. Catu : Acq . Time : H-jd i fifed : Proc . Algcrith n Koia e Percentag e Ba?e . Sob
. Mind o Standar d 1.0 0 1.0 7 11/23/201 0 3:46:2 3 P

M N o Intellipua n : S O w : l.O I P-ijV.-Spllt
. Factor : i Repor t Litr:) « = t

1 I'^in
. Pea k

Heigh : Min
. P«a k

Widt h Sniootliinv i Widt h R T Window : E.".pect« dRT : Us e Relativ e R

T int
. Typ* : Retentio nTime : eak : W o : 0.0 0

0.0 0 0 30. 0 E 14. 3 n N o Bas e T 3 Ba s 14. 3 m Ataa : 202475 4 -c^- m Height : 454000 . cp s nq/m L ng/m L

- My mi n c p j s u e p c n

n 3



# I Sampl e Nam* ; "m101123a034 ' San^jl * ID ; •LCS-101115-4 - File ; "m101123a.wif r P*a k Name : "PFHS ' Mass(*s) ; "399
. Comm*nt ; "2pp b LCS/ 1 pp b surrogat e LCS " Annotation :
Calculate d ! Acq
. Date : 

# I SampI * Nam* ; "ml01123a04 rSamfrf * ID ; 'LCS.101115-15 " F8e ; "m101123a.wif r P*a k Nam* : 'PFHS " Mass(es) ; '399.0/80. 0 amu,399.0/99. 0 amu " Comm*n t '2pp b LC S ECF * Annotation: " Sampl e Index : 4 9 Q C n-j/m L Sampl e Type : C(jncontration : Calculate d Con e Acq
. Date : AC)
. Time : M-iditied : R TWindo-j : Expecte d RT : Q C 0.0 0 0.12 4 11/24/201 0 1:53:2 7 A H Ys s •0. 0 14. 3

Dat aworke du p b y ST W Printin g Time : 11:13:2 2 A M Printin g Date : Wednesday , Januar y 26 , 201 1 Pag e 7 o f 9 Pag e 4 7 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy§is^8lf f^^^lf^iS9?^f3l9?di5 ' Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# I SampI * Name;-ml01123aO60 " Sampl e ID ; "GLP10O1-01-13-001 " File:"m101123a.wrf r Pea k Name : 'PFHS " Mass(e6) : "399.0/80. 0 amu.399.0/99. 0 amu " Comment ; "DA L GWMC L MW1 B 0 101110 " Annotation ; " " ampl « In . ion : N/A Concen t

ra t CaKiilate d Ac:) . Date : 11/24/20 ! Acq . Tin,6 : £:04:.' S ; MjJified : Ye s R T Window : 30. 0 Expjict^ dRT i 14. ? Us e Relativ e RT : H o I:jt
. Type : Manua l !ketentio nTime : 14. 3 Area : 4(4393 2 c t Hfei-jht : B59000 . . Star t Time : I'-. t 8.5e 5 8.0* 5 7.5* 5 7.0* 5 6.5* 5 e.Oe S 5.5* 5 S.Oe S 4.5* 5 4.0* 5 3.5* 5 3.0e 5 Z5e 5 2.0e 5 1.5* 5 1.0* 5 5.0* 4 14.2 5 1

14.1 1

1 , 1 , , 1 1 1 •1 ••^ ^ 1 4 1 6 1 8 SampI * Nam* : "m101123a083 ' SampI * ID ; "Metho d Blank "



## I Paa k Nam* : 'PFHS ' Mass(*s) : "399.0/80. 0 amu.399.0/99. 0 Commant'1 0 005-229 " Annotation; TM Sampl e Indo;< : B i Sampl e Type : I'nknow n Concentration : H/ A Calculate dCone : ^ 0 Ac;] . [.Mtu : 11/24/201 0 Acq . Tima : 2:06:2 4 P M 600 0 H-jd i Pro c Ba^ e P..a K R'fpc ; Mi.-i
. Hin
. SltiO O K TK liod : Alge r EutJ -iJpl i r t L a Pea k Pea k rhin o ndo- v tlim :

taqe : Fact u g«= t Pe Height : W 1 4 dth : dUi : 550 0

1475 9 jaunr : 4 900 . CP 5 IJ. 2 mi r

1 6 1 8 

# I Sampl e Name ; "ml01123a019 " Sanpl e ID : "10007-6-6 ' File : 'ml01123a.wif r Pea k Name : "PFOS ' Mac£(es} : "499.0/99. 0 amu.499.0/80. 0 amu,499.0/130. 0 amu " Comment ; '1. 0 ng/m L F C st d i n 95 % Synth
. VUatmy5%ACN ' Annotation : Sampl e Index : 2 0 Sanpl e T-.-pe : Standar d Concentration : 0.39 5 ng/m L Calculate d Cone : 1.0 5 ng/m L Acq
. D;.t.) : Il/2;/2;31 C

Expecte dRT : Us e Relativ e RT : Int . T^p« : Retentio nTime : Area : 164 5 Hfeight : 3 = 1 5 N o Va! l i ; 45 7 Jco o 

# I SampI * Nam* ; •ml0n23a034 - SampJelD : •LCS-101115-4 " Fil* ; 'ml01123a.wi r Pea k Nam* ; "PFOS " Mas*<*6) : •499.0ffi9. 0 emu,499.QreO. O amu.499.0 n 30. 0 amu " Commen t '2pp b LCS/lpp b sutTogat o LCS " Annotation: " Sampl e Inden : 3 5 Sampl e Type : Concentration : 1.5 6 irj/m L i.c- e nq/m L Acq . Dat» : Acc) . Tima : 14,>di£ied : R T Kindo-v : Expecte dRT : Us e Relativ a Int . Typ^ : Retentio nT

J Area : Height : R

T ll/?5/2l?1 0 5:00:i e PH Ye a 30. 0 15. 3 ti o Manua l IS. 2 263125 5 -o u 613000 . r. p 

### &

i 

### 1 6.0* 5 5.5* 5 5.0* 5 4.5* 5 4.0e 5 3.5* 5 3.0* 5 2.5* 5 Z0* 5 1.5* 5 1.0* 5 5.0* 4 1 5 2 5



# i y \ ^ . . 1 4 1 6 I

B Dat aworke du p b y ST W Printin g Time : 11:13:2 3 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 8 o f 9 Pag e 4 8 o f6 7*ETS-Mar y An n Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 AnalymSie f^..^ fha9?5'f3|Oai P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# r San^eName:"m101123aO48 * Sampl e ID: " Pea k Name : "PFOS ' Mas*(ee) : '499.0/99. 0 a i Commen t "2pp b LC S ECF " Annotation: " 1.9 T

R T Window : Exp^cf dRT : U.v e Relativ e fiT: nq/ r 5.0* 5 4.6* 5 4.6* 5 4.4*5
- 4.2* 5 4.0* 5 3.8* 5 3.6* 5 3.4* 5 3.2* 5 3.0a 5 2.8* 5 2.6* 5 2.4* 5 2.2*5
- 2.0* 5 1.8* 5 1.6* 5 1.4* 5 1.2* 5 1.0* 5 8.0* 4 6.0e 4 4.0e 4 2.0* 4 0. 0 

# 1

-£t
_ 

# I SampI * Name : "mlO l 123a083 " Sampl e ID: " Pea k Name : "PFOS ' M*s«(*«) : "499.0/99. 0 a i Commen t "1 0 005-22? " Annotation : ~ Sampl e I n 

# I Sampl e Name : "ml011233060 - Sampl e ID : "GLPIOOl-OI-lS-OO rFile:-m101123a.v«f r Pea k Nam* : "PFOS " Mass(*s) : "499.0/99. 0 amu.499.0ffi0. 0 amu,499.0/130. 0 amu " Commen t "DA L G WMC L M W1 B 0101110 " Anrwtatkin;" " impl e Type ; oncGiT
. id t i ( alculate d ' L'nkncw n N/ A 6.2 9 t 11/24/201 0

Kelativ e BT :

. Type : a : 1 2 qht : r t Time : Time : H o

Hrfnua l 15. : 4704 7 05^-0 0 0 . 14. 7 15. e 9.5* 5 • ) 9.0* 5 8.5* 5 8.0* 5 7.5*5
- 7.0* 5 6.5* 5 6.0* 5 5.5* 5 S.Oe S 4.5* 5 4.0* 5 3.5* 5 3.0*5
- 2.5* 5 2.0* 5 1.5* 5 1.0* 5 5.0* 4 0. 0

T-.-pe : ,tn dCO I
H.-.Ji£ied : R T Windfjw : Expecte dR

Us e Relati ' N/ A 0.13 1 ng/m L 11/24/701 0

15. 2 nooo . I 1.10* 5 1.05*5
- 1.00e 5 9.50* 4 9.00* 4 8.S0e 4 8.00e4 - 7.50e 4 7.00e 4 6.50* 4 J 6.00* 4 

### = • ^ 5.50* 4 S
= 5.00* 4 4.50*4 : 4.00* 4 3.50* 4 3.00* 4 2.50* 4 Z00e 4 1.50* 4 1.00* 4 5000.0 0

•0.0 0 

# Jj L

1 0 1 2 1 4 1 6 1 8 Dat aworke du p b y ST W Printin g Time : 11:13:2 3 A M Printin g Date : Wednesday , Januar y26 , Pag e 9 o f 9 201 1 Pag e 4 9 o f6 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 AnalymSlf f^*? fH^S^^illPPdi P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 g101215a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) ; y= -0.051 2 x'^ 2 + 1.7 4 x-

^ 0.01 9 ( r= 0.9995 ) /. a 7.5 - 7.0 - 6.5 - 6.0 - 5.5 - 5.0 - 4.5 - 4.0 - 3.5 - 3.0 - 2.5 - 2.0 - 1.5 - 1.0 - 0.5 - 0.0 - 

### ^ * ' 

### 0 . > X ^ y' '



### , • " y

y 

### ,^

' ./ ' 

### ,.. / / '

^ y y



# X y 

# y y y y ' 

# X ' X ^/-"" ' ,- 

## y y ^ X ' ' 

### '-' ^ ^ X , y ^^.-• 4 

### -^'" ^

0. 0 0. 5 1. 0 1. 5 2. 0 2. 5 3. 0 Analyt e Cone
. /

I S Cone
. 3. 5 4. 0 4. 5 5. 0 Dat a worke d up byST W Printin g Time : 11:14:3 3 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 5 0 of 6 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 AnalyiEStf f^^PlfH^gp^fs^Op^ij i Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

Dat a worke d u

p b yST W Printin g Time : 11:14:5 6 AM Printin g Date : Wednesday , Januar y26 , 201 1 Pag e 1 o f 1 Pag e 5 1 o f6 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^iA^g^f f^^^FH^gy^fj^pgjj p Groundwate rSample s Morga n Count

yLandfill , Decatur , A L - Novembe r201 0

•Sampl e Name ; "gl0l2l53019 - Sampl e ID; ' I PeakName;"l3C4-PFOS - M3ss(es) : 10007* ^ Fil.:-s101215>.» r •503.0/80. 0 amu " •Commen t "1. 0 ng/m L F C st d i n Synlti
. Watet " ?air.pl e Inde/ : 1 9 Sampl e Typ- : standar d Cancantration : 0.0 0 n y Calculate d Cone : < 0 Acq
. Uatij : 12/15/20U > Acq
. Time : 1:12:3 0 P M rr.JC
. Algr,irlthm ; Inte l !:'^i:a n - Min
. pHa k

H«i(jht : O.& O cp = Min
. Pea k

kiidth : 0.0 0 sa c FmtJ'jtlunc j (lidth : 0 pui n R TWindow : JO. O se c Us * Relativ e RT : N o Int
. Typ*. : Valle y Retentio n Time : 12. J mi n Area : 5B6 0 count s Star t Time : 12. 2 mi n En d Tim-. : 12. 5 mi n m L

ICJ A
3 A/fnotat»n:" "

&

- ^ 140 0

120 0

100 0 90 0

iiiL.iiLl
. ,1^
. 

# m i|..i,u.4t.tJ i 1 2 1 3 1 4 1 5 1 6 1 7 

### • Sampl e Name ; 'glOIZlSaOS rSarr ^ ID ; 'LCS-101215-2 ' File : -g10121Sa.wi r Pea k Name : -13C4-PFOS " Masstles) : '503.0/80. 0 amu ~ Comm*n t '0.2pp b LCS ' Anrwtation;" " Samfil e Indiit : 64 Sajipl - Typ- : V 0 nq/7ii L

1.49e-00 i 12.
- i;. 5



# I SampI * Name ; 'gl01215a0e6 ' Sampl e ID ; 'LCS-101215-6 " File ; "g101215a.wff ' P*a k Nam* ; '13C4-PFOS " Mass(**) : '503.0/80. 0 amu * Comment'"0.2pp b LC S EC P Annotation : " 0.0 0 ny/ni L 12/lf/201 C 135 0 130 0 125 0 120 0 1150 - 110 0 105 0 100 0

60 0 550
-

350 ; 30 0 

# k jJUJiiJii i 6.5 0 7 

# I SampI * Nam* ; "g101215a02 rSampl e ID:"GLP1(W)l-02 - P*a k Name : •13C4-PFOS " Mass{*s) ; "503.0/80. 0 Comm*nt-D/U.GWMCLMW3B0101110 - Annotation : ampl e Index : 2 6 Acq
. Pat e Ac^
. Tima : It/ A 0.004 6 12/lb/ Z J:^4 : 2 3 II o 1 0 P M IntclliOu a 0.0 0 Saoo t R T W i E-pe c I's e P Int . R?te i Heig h En dT hin u ,tia:
. t a d Typ e tio n Tin

ine : W ; T I V 1



# 'illiiiliiii i ilAitiihiiiri i
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. Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

# I Sampl e Name : "g10121SaO39 - Samfrf e ID : "1 0 01O-39 ' Fite ; •g101215a.wi r Pea k Nam e -13C4-PFOS " Mass{es) : "503.0/80. 0 amu ' Comment : "Mettw d blank " Annotation : " " ."^arnpl aIndex : " 3 9 C:^ncenrtJriQn : U/ A c:alculat* dcone : - ; 0 ^ ^ Ac;) . Djtn : 12/15/201 0 Acq . Time : 7:12:3 J P M 150 0 Proc . Algorithm : InteiliCua n- K] A Min
. Ppa k

Height : 0.0 0 cp s 1400 - Min
. Pea K

Width : O.O O st c Smcothiii qWidth : 0 f-'ii-t s ^-^QQ . Ejjpacte nRT : 12.-
- rain Us e Relativ e RT : ti o 120 0

100 0 57& 5 c 1 . s;.a+&0. ' 12. 3 90 0 

# I Sampt e Name ; •gl01215a019 " Sampl e ID : "10007-6-8 ' File : "gl01215a.vw r Pea k Name ; "MSPFOSflS) ' Mass(es) : '507.0/80. 0 amu " Commen t "1. 0 ng/m L F C st d i n Synth
. Wate rAnnotation : " "

9.0e 4 8.5* 4 8.0*4 : 7.5* 4 7.0*4
- 6.5* 4 6.0*4
- 5.5* 4 5.0* 4 4.5* 4 4.0* 4 3.5*4
- 3.0e 4 2.5e 4 2.0* 4 1.5* 4 1.0* 4 5000. 0 H.<Lght : Stat t 1 En dTi r

0. 0 -.^^^ ^ '•]3-7 A 1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 

# ( Sampl e Name ; "g101215aD83 " Sampt e lD;"LCS-101215- rFile ; "g101215a.wi r Pea k Name : "M8PF0S(IS) " Mass(«s) ; "507.0«0. 0 amu " Commen t "0.2pp b LCS " Annotation : ~ SampI e Type : y C Cfncantra t Cal.tulate d AcL]
. Dat« : Acq
. Time : Mr.Jified : R TWindow : Exoectcr j Ik cCn
. 0
. 95. ' N/ A 12/lf/201 C 5:57:0 5 PL

' 30. 0 13.1 ' n y

, . c m l 7.5* 4

7.0* 4 6.5e 4 

# I Sampt e Name : "g101215a086 " Sampt e ID ; 'LCS-1D1215-e " Fite : 'gl01215a.iM r Pea k Nam* ; "M8PFOS(IS rMass(*s) : '507.0/80. 0 amu * Commen t "0.2pp b LC S EC P Annotation : " * Sampl e Inoex : 9 7 Sampl e Type :

Height : 5t.st t Ti r En H Time : 0.95 3 N/A 12/15/201 C S:51:1 2 P

M

Manua l
• : i:. e 3T2e0 7 - • 12. 7 ng/ i 7.5* 4 7.0* 4 6.5* 4 8.0* 4 5.5* 4 5.0* 4 4.5* 4 4.0* 4 3.5* 4 3.0* 4 2.5* 4 Z0* 4 1.5* 4 1.0* 4 5000. 0 0,0 - Dat a worke d up b

ySTW Printin g Time : 11:16:5 2 AM Printin g Date : Wednesday , Januar y2 6 , 201 1 Pag e 2 o f 4 Pag e 5 3 o f6 7Ginge r AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analy^i^SiP f^ta^lfH^gP^iPslOai ? Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

•Sampl e Nam*;'g101215a02e - Sampl e ID ; •GLP1&O1-02-13O21 " Fite;'g101215a.wi r I Pea k Nam* : "M8PF0S(IS) - Mass(es):'SOT.OffiO. O amu " •Comm*nt;'DALGWMCLMW3B0101110 " Annotation;" " ."lampl e Indez : 2 9 Sanpl e Type : Unlctiow n Concentration : 0.56 0 nq/n. L 8.5* 4 Calculate d Cont: : N'/ A Acq
. Dat« : 12/15/2CU ' Acq
. TiEia : 3:54:: ' P H "-" ^ Mcdilied : Hi
. 7.Se 4 Proc
. Algorichw : Intellifus n - lO A Hin
. P«a k

H-iqtit ; 0.0 0 cp s Hin
. Peat : Width : 0.0 0 s^ c'•°* * Smoothin g Width : o point s R TWind.jw : .10. C s^< - 65e 4 Expecte d RT : 12. i itii n Us e Relativ e BT : N u 6.0e 4 Int
. Type : Valle y fistention Tin.e : li. J n,i n 55 ^ Area : 30011 5 count s Star t Time : 12. 2 r.i n 5,De 4 En d Time : 12. 5 mi n . "
. 4.5* 4 1 4.0* 4 3.5* 4 3.0* 4 2.5* 4 2.0* 4 1.5* 4 1.0* 4 5000. 0
1 2 3 4 5

•SampI * Nam* : "g101215a0i rSampt e ID;'10007-6-8 " Fite ; "gl01215a.wi r 1 P*a k Name;'PFOS - Mass(es):'499.0/S9.0amu.49g.ara0.0amu,439.0/130. 0 ami / •Comment;'1. 0 ng/m L F C st d i n Synth
. Water - Annotation : " Sampl e In-iex : 1 " Sampl e Type : atanrtard " Cot,cantration : 0.59 0 ng/:T, L Calculit«r fcone : O.^' ? ng/n L Acq
. D.,ta : 12/1?/20U ' ,.5^5
. Acq
. Time : 1:12:3 0 Pi « Hc,di£jo(3 : N o 1.4e5 - R TWindow : 30. 0 se c EKpecce d FiT : 12. 3 mi: i Us e Relativ e RT : N n 1-3*5 - Je^enll^rTi^e : ""'iT ] .i n Area : 56343 7 count
. Star t Tine : 12. 2 mi n En d Tim- : 12. 5 mi n l.Oe S

« 9-0« 4 

### & ^ 8.0e4 - S

- 7.0e4 - 6.0e4 - S.0e4 - 4.0e4 - 3.0e4 - 2.0* 4 1.0* 4 0. 0 •;•••••-••••• ,6 7 8 9 1 C Tim* , mi n

7 8 9 1 0 1 2 3 1



### L 1 1 1 2 1 3 1 4 1 5 1 6 1 7

123 1

1 1 1 2 1 3 1 4 1 5 1 6 1 7 •Sampl e Nam*:-g10121SaO39 " Sanpt e ID ; "10010-39 " FH* ; "g101215a.<M r 1 P*a k Nam*:-M8PFOS(tS} ' ' Masses);'507.0/80. 0 amu ' 1 Commen t 'Metho d blanl T/^notation ; ~ .Sampl e Indes : 3 5 Sampl e Type : (•nki-.cw n Concen t ta t ion : 0.9-J O n-j/m L Calculate d 'Jonc : H/ A Acq
. DJt^ : 12/15/201. 1 g_o* 4 Acq
. Tima : 7:12:J 3 P M 85* 4 H-idified : N o ""^ ^ Ptoc
. Algcritnrs : Inteilipua n - lO A Min - Pea k

H-iiht : 0.0 0 cp s ^-O* * Min
. Pea k

Mid-.T : 0.0 0 se c Jmoothin- j Width : 0 point s 7.5* 4 R TKindu-.v : -O. O =s r Expecte.- i hT : i:. i mi n 70 ^ Us e Relativ e RT : N c Int
. Type : Valle y^-^ ^ Retentio n Tin-e : la. i mi n Area : iiilS' b co-int s 6.0* 4 H-iiaht : 0.45d-C0 4 '•f.. a Stat t Time : 12. 2 mi n 5.5* 4 En d Time : i:. 5 mi n » ^ 5.0* 4 t 1 4.5*4 4.0* 4 3.5* 4 3.0* 4 2.5* 4 2.0* 4 1.5* 4 1.0* 4 5000. 0 1

1 2 3 4 5

•SamfrieName:-g101215aO83 " Sampt e ID ; "LCS-101215- rFde : "gl01215a.»vt r 1 Pea k Name ; "PFOS " Mas*(es);"499.Qre9.0amu.499.oraO.Oamu,499.0/130.0amu - •Commen t "0.2pp b LCS " Annotation ; " Sampl e Index ; 54 Sampl e Type : Q C Concentration : 0.1S 8 ng/m L Calculat-. d Cone : 0.17 2 ng/m L 27e4 - Acq
. l:at*! : 12/1S/2P1 C Acq
. Tims : 5:^7:0 9 P M 2.6*4 - „„di»., , ,. , ^ ^ R TKindo-j ; 30. 0 se c2.4*4 - Expecte d RT ; 12. ? r.i n Us e Relativ e RT : H o ^•*" ' Z2* 4 j".jr^r„„ : ""i n .i „ ^rea : seSl O count s 2.0*4 - Haight : 2.7£e-00. ) cp a Star t Time : i:. 9 mi n '-S^ ' En n Time : 13. 0 mi n 18*4 - 1.7* 4 1.6* 4 1 1.5* 4 ^ 1.4* 4 1 1.3* 4

~ 1.2* 4 1.1* 4 1.0* 4 gooo.o8000. 0 7000.0 - 6000. 0 5000,0 - 4000.0 - 3000, 0 2000.0 - 1000. 0 0 0 J - •.• ^

~t— ^ -„—^. , .—y—, —

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Tim* , mi n

1
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. 1 , . .,. . 6 7 6 9 1 0 128 5

1 , „ ^ 1 

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AG0133050 9 Attachmen t B GLP10-01-02 ; Interi m Repor t 1 3 Analyfi?s8if f^Y»? fH^S?^f5l9?di P Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0

[ Sampl e Name ; -g101215a088 " Sampl e ID:"LCS-101215* " Fil* ; 'gl01215a,wi r I Pea k Name : "PFOS " Mas$(es} : '499.0J99. 0 a . I Comment ; "0.2pp b LC S ECF " /\nnotabon ; " Sampl e Indaz : 8 7 Simpl e Type : y C Concentration : 0
. 19 5 nq/m L Calciilata d Cone : 0.21f l nq/m L Ar-.)
. Date : 12/lf/20U ' u,499.0/130. 0 amu '

1.9e 4 1.8* 4 1.7* 4 1.6*4
- 1.5* 4 1.4* 4 l,3e 4 1,2* 4 1.1* 4 l,0e4
- 9000. 0 8000. 0 7000.0
- 6000. 0 5000. 0 4000. 0 3000. 0 2000.0
- 1000.0
- 0. 0 i - ^ 1 0 I I 1 2 1 3 1 4 1 5 1 6 1 7 I Sampl e Name : "91012153028 " Sampl e ID:"GLP1(M31-02-13<J21 " Fil* ; "gl01215a.V ( Pea k Name : "PFOS " Masses) : "499,0«9. 0 amu,499.0ffiO. D amu.499.0/130. 0 amu " I Comnwn fOALGWMCLMW3B0101110 - Annotation ; " Sampl e Index : 2 5 Sampl e Type : Unknow n Acq
. fatn ; Acq
. Time : Hodilibd ; R TKindo-j : Expec l riv e R

T Int
. Type : Height : Star t T i En d Tim e Manu :

16371 6 26*4- 1 25*4 - 24*4 - 23*4 - 22*4 - 2.1*4 - 20*4 - 1.9e4 - 1.8e 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 - 8000.0 - 7000.0 - 6000. 0 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 -MW*V , • .IfiL
. , -i.. ^ , I,,I. , l,*.„t..f. M 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 

# I SampI * Name ; "gl01215a039 ' Sampt e ID ; '1001&<39 ' File : 's10l215a.wi r P*a k Nam* : "PFOS * Msss(es) ; '498.0/99. 0 amu.439.0/80. 0 amu.493.0^30. 0 amu " Commen t *M*ttK> d blank * Annotation : ~ Sampl e Index : J 9 Sampl e Type : Unkno-v n IJ/ A Calculate d Acq
. D.iti ; Acq
. Tima : M.->Jl(iad : Proc
. Aiq o fJjia e P^r c Ea.-e
. Sue
. Cone :

i W hra : ig e 0.0020 3 nq/m L 12/15/2011 ' 7:12:I 3 PI 1 Mt , Intelliyua n - MOI l 1 0 ndow : l.,-^ 0 ::a n 850 0 800 0

700 0

5500 5000 4500 400 0 3500 3000 2500
- 2000
- 1500
|l.itljfkU.j.t|tlp.i|ill|ti,»i^l l 12.9 0

1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 Dat a worke d u

p b yST W Printin g Time : 11:16:5 3 AM Printin g Date : Wednesday , Januar y 26 , Pag e 4 o f 4 201 1 Pag e 5 5 o f6 7

## Documen t ntafifeei«ft6T^ri}viB,e|ji5reT* , fo r1 4 days fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S I n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0



# 3 M Environmenta l Laborafm y

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

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8'044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q ^

1( 1 [ o " 1
Approve d By : 

# ^

y •g- > Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 of11
. Mettio d ofAnalysi s fortti e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 5 6 o f6 7

### Documen t nmnfmrnmifit^kr^swcimt , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PRO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


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

yrequir e preparatio n b

ya n alternat e metho d suc h as ETS-8-15 4 "Determinatio n o f Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"
. Thi s metho d i s considere d a performance-base d method
. Data i s considere d acceptabl e as lon g as th e define d Q C elements ar

e satisfied
. Sampl e collectio n i s no

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

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

t multipl e concentrations
. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e determine d usin g fiel d matri xspike s t o verif ythat th e metho d i s applicabl e t o eac h sampl e matrix
. Sampl e results fo rspike s outsid e of70 % t o 130% , ma yb e flagge d as suc h (wit h expande d accurac

ystatements) , o rwil l no

t be reporte d du e to non-complian t qualit ycontro l samples
. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t least 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o determin e th e statemen t of accurac yfo ranalytica l results
. 3 Definition s 3. 1 Calibratio n Standar d Asolutio n prepare d b

yspikin g a know n volum e ofth e Workin g Standar d (WS ) into a predetermine d amoun t o fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , an d analyze d accordin g t o thi s method
. Calibratio n standard s are use d t o calibrat e th e instrumen t respons e wit h respec t t o analyt e concentration
. 

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

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

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

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d as a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures
. Th e purpos e ofth e F B i s t o determin e i ftest substance s o r othe rinterference s ar

e presen t i n th e fiel d environment
. Thi s sampl e i s als o referre d t o as a Tri p Blank
.

ETS-8-044. 0 Pag e 2 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 7 o f6 7

### Documen t ns:».filK-ai«g^arij!erilli36pr8f;S , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0 

## 3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n as th e sample
. Th e FD S i s handle d unde ridentica l circumstance s an d treate d exactl yth e sam e throughou t fiel d an d laborator y procedures
. Analysi s o

fth e FD S compare d t o that o fth e firs t sampl e give s a measur e ofth e precisio n associate d wit h sampl e collection , preservatio n an d storage , as wel l as wit h laborator yprocedures
. 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s ofth e target analyte s ar e adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n o faqueou s samples
. Aknown , specifi cvolum e of sampl e mus

t b e adde d t o th e sampl e containe rwithou t rinsing
. Thi s ma yb e accomplishe d b

ymakin g a "fil l t o thi s level " lin e o n th e outsid e ofth e sampl e container
. Th e FM S shoul d b e spike d betwee n approximatel y50 % an d 1 0 time s th e expecte d analyt e concentratio n i n th e sample
. I fth e expecte d rang e o fanalyt e concentration s i s unknown , multipl e spike s a t varyin g level s ma

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

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

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

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot o

fAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e target analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p detemnin e i fth e metho d i s i n contro l an d whethe ra los s ofanalyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues
. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s ar e no t know n o rma

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

t th e sam e tim e an d place as eac h FMS
. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot o

fcontro l matri xt o whic h know n quantitie s ofth e target analyte s ar e adde d i n th e laborator

ya t th e tim e o

fsampl e extraction
. At leas t two level s 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 t o uppe rrang e o fth e curve . Th e LCS s ar e extracte d an d analyze d exactl ylik e a laborator

ysampl e t o determin e whethe rth e metho d i s i n control
. LCS s shoul d be prepare d eac h da ysample s ar

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

ymatri xspik

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

ysampl e t o detennin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results
. Th e endogenou s concentration s o fth e analyte s i n th e sampl e matri xmust b e detennine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations
. LMS s are optiona l fo ranalysi s o faqueou s samples
. 3. 9 Laborator ySampl e Aportio n o raliquot ofa sampl e receive d fro m th e fiel d fo rtesting
. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e lowes t concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac

ydurin g routin e operatin g conditions
. To simplif ydat a reporting , th e LLO Q i s generall yselecte d as th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria
. Sampl e LLOQs are matrix-dependent
. Th e uppe rlimi t o

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

ydurin g routin e operatin g conditions
. Th e highest standar

d i n th e calibratio n curve that meets metho d criteri a i s define d as th e ULOQ
. ETS-8-044. 0 Pag e 3 of1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 8 of6 7

### Documen t ntayiban^SieriferiifiSijjrorert , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


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

ysampl e includin g exposure t o al l glassware , equipment , solvents , an d reagents that are use d wit h othe rlaborator ysamples
. Th e metho d blan k i s use d t o detennin e i ftest substance s o rothe rinterference s ar e presen t i n th e laborator y environment , th e reagents , o rth e apparatus
. 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yofmateria l intende d t o represen t th e origina l source material
. 3.1 3 Stoc k

Standar d Solutio n (SSS ) Aconcentrate d solutio n ofa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound
. 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e target analyte(s) , bu t i s no t nonnall y foun d i n th e sample(s)
. Asurrogat e compoun d i s typicall ya target analyt e wit h a t leas t on e ato m containin g a n isotopically-labele d substitution
. I fused , sun'ogate(s ) are adde d t o al l sample s an d qualit y contro l samples
. Sun-ogate(s) are adde d t o quantitativel yevaluat e th e entire analytica l procedur e includin g sampl e collection , preparation , an d analysis
. Inclusio n o fa sun'ogate analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired
. 3.1 5 Workin g Standar d (WS ) Asolutio n ofsevera l analyte s prepare d i n th e laborator yfro m SSS s an d dilute d as neede d t o prepar e calibratio n standard s an d othe rrequire d analyt e solutions
. 4 Warning s an d Caution s 4. 1 Healt h an d Safet y Th e acute an d chroni ctoxicit yo fth e standard s fo rthi s metho d hav e no t bee n precisel ydetermined ; however , eac h shoul d b e treate d as a potentia l healt h hazard
. Th e analyst shoul d wea rgloves , a la b coat , an d safet

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

yi s responsibl e fo rmaintainin g a saf e wor k environmen t an d a curren t awarenes s o floca l regulation s regardin g th e handlin g o fth e chemical s use d i n thi s method
. Areference fil e o fmateria l safet

y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 4. 2 Caution s Th e analyst mus

t 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 use ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedur e o roperato rmanua l fo radditiona l informatio n an d cautions
. 

## 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s ar e reagents an d glassware
. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s ofanalysi s b

yrunnin g metho d blanks
.

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

t Injectio n Analysi s Pag e 5 9 o f6 7Attachmen t C 

### Documen t n©,aiyii>8i«i9rtkiifiS6pr8f3t , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0


### Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yo f interference and/o rcontamination
. Thes e ma yinclude , bu t ar

e no t limite d to : was h bottles , Teflon ® line d caps , autovia l caps , HPLC parts , etc
. Th e us e ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes
. 

## 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h perfonnance liqui d chromatograp h capabl e ofpumpin g u p t o two solvents an d equippe d wit h a variabl e volum e injecto rcapabl e ofinjectin g 5-10 0 p L connecte d t o a tande m Mass Spectromete r (LC/MS/MS)
. I Analytica l balance capabl e ofreadin g t o 0.000 1 g Adevice t o collec

t ra wdata fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25pL , 50pL , 100pL , 250^JL, 500pL , lOOOpL
. 1 m L plasti cHPLC autovial
. Disposabl e pipettes , polypropylen e o rglas s as appropriat e Centrifug e capabl e o

fspinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C18,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

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

t Injectio n Analysi s Pag e 6 0 o f6 7Attachmen t C 

### Documen t niaf'ib>ai«s;QrftWiffie:!3preT3t , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0


## 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospra yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e PFBA PFPeA PFH A PFHpA PFOA PFN A PFDA PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213-^16 9 263^21 9 313-^26 9 an d 313-^11 9 36 3 - > 319 , 36 3 - * 16 9 an d 36 3 ^ 11 9 413- » 369 , 41 3 ^

21 9 an d 41 3 ^

16 9 46 3 ^ 419 , 46 3 ^

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

16 9 an d 61 3 - > 31 9 29 9 - > 8 0 an d 29 9 ^

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

9 9 49 9 - ^ 80 , 49 9 - » 9 9 an d 49 9 ^ 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , as summin g multipl e transition s ma yprovid e quantitatio n ofisomers tha t more closel ymatche s NM R dat a an d ma yhave th e adde d benefi t of increase d sensitivity
. Th e us e o fon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a are met t o assure adequat e specificity
. Th e previou s informatio n i s intende d as a guide , alternat e instalment s an d equipmen t ma yb e used
. 

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

## 7. 2 Standard s Perfluorobutanoi cAci d (PFBA - C4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPe A- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alfa Aesa r Perfluorohexanoi cAci d (PFH A- C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHp A- C 7 acid , als o know n as TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PF0A-C 8 acid) ; 3 M Perfluorononanoi cAci d (PFN A- C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- C1 0 acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUn A- C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C1 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfiuorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 1 o f6 7

### Documen t mm}^b•m^2>^^ikr^BmrG^ , fo r1 4 day s fro m 01/26/201 ' Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


### Th e previou s informatio n i s intende d as a guide
. Reagent s an d standard s fro m alternat e source s ma yb e used
. 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t water
. Note : Alternative volume s ma yb e prepare d as lon g as th e ratio s ofth e solven t t o solut e ratio s ar e maintained
. 

## 7. 4 Stoc k

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

d preparatio n procedur

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

solution s t o appropriat e levels
. 10 0 pg/m L targe t analyt e SSSs—^Weig h ou t 1 0 m g ofanalytica l standar d (correcte d fo rpercen t sal t an d purity ) an d dilut e to 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask
. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container
. Prepar e a separat e solutio n fo reac h analyte
. Expiratio n date s an d storag e condition s o

fstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. An'exampl e ofpurit yan d sal t correctio n i s give n belowfo rPFOS
.

„ X - rX molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t ofsal t PFO S (K * )sal t correctio n facto r= -^ ^ = 0.927 5 53 8 1 0 m g CsFiySOs'K

* wit h purit

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

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m L mixe d standard—Ad d 625p L ofth e 5 pg/mL-mixe d workin g standar d solutio n t o a 25m L volumetri c flas k an d brin g u p t o volum e wit h solvent
. Storag e Conditions—Stor e al l SSS s an d workin g standard s i n accordance wit h laborator ystandar d operatin g procedur e o ri n a refrigerato ra

t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e o fpreparation
.

ETS-8-044. 0 Pag e 7 of1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 2 o f6 7Attachmen t C 

### Documen t ncRfift-aiffls^iBfcrimB&i^meTrt , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Morga n CountyLandfill , Decatur , A L - Novembe r201 0


## 7. 5 Calibratio n Standard s Usin g th e workin g standard s describe d above , prepar e calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline
. Note : Volume s o fwate ran d workin g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline
. Calibratio n level s othe r tha n thos e liste d belo

wca n b e prepare d as needed
. Concentratio n o fWS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS , /j L

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

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

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

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

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

yno t b e suitabl e fo r analysi s b

ythi s method
. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered
. Thoroughl ymi xsampl e befor e removin g a n aliquot an d placin g i n a labele d plasti cautovial
. Plasti ci s preferre d ove rth e us e ofglas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass
. Dilut e sample , i fnecessary , wit h AST M Typ e I , HPLC water , o rothe rsuitabl e water
. Prepar e metho d QC sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials
. Prepar e a t least five metho d blanks
. 

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

d curve prio rt o eac h set ofsamples
. Th e standar d curve ma

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

xo runweighted , o rb

yquadrati cfi l (

y= ax ^ •< •b x+ c) , weighte d 1/

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

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

wpoints ma

yb e exclude d fro m th e calibratio n curve s to provid e a bette rfi t ove rth e rang e appropriat e t o th e data o rbecaus e theydi d no t mee t th e pre-detennine d acceptance criteria
. Low-leve l curve points shoul d als o b e exclude d i fthei rare a counts are no t a t least twic e that o

fth e metho d and/o rsolven t blanks
. Th e coefficien t o

fdeterminatio n (r^

) valu e fo rth e calibratio n curve mus t b e greate rtha n o requa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 of1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 3 o f6 7

### Documen t maijiMi-meh'tWi m B&jireTst , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


### b e withi n ±30%
. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata
. Aminimu m o

f6 points wil l b e use d t o constmc t th e calibratio n curve . I fth e calibratio n curve doe s no t meet acceptance criteria , perfon n routin e maintenance o rprepare a newstandar d curve (i fnecessary

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

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

t a minimu m afte rever ytent h sample , no

t includin g solven t blanks , wit h a minimu m 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 CC V level s ma

yb e used
. Sample s containin g analyte s that ar e quantitate d above th e concentratio n o fth e highest standar

d i n th e curve shoul d b e furthe rdilute d an d reanalyzed
. 

## 1 0 Qualit yContro l 10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LOQ o f0.02 5 ng/mL
. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belo wwil l b e documente d i n th e ra wdata an d footnote d i n th e fina l report
. 10. 2 Metho d Blank s Metho d blank

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

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

t th e en d ofth e analytica l run . Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s mus t b e less tha n 50 % o

fth e are a coun t o

fth e LOQ standard
. Th e standar

d deviatio n o

fth e are a counts ofthes e metho d blank s shoul d b e calculate d an d reported
. I f th e mea n are a counts ofth e metho d blank s excee d 50 % o

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

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

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

t require d bu t ma

yb e use d o n projec

t specifi crequirements
. 10. 5 La b Contro l Sampl e Triplicat e la b contro l spike s a t a minimu m o

ftwo differen t concentration s ar e t o b e prepare d wit h eac h preparatio n batch
. Lo wla b contro l spike s shoul d b e prepare d at concentration s i n th e rang e offive t o te n time s highe rtha n th e targete d LOQ an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t o fth e curve . Th e relative standar

d deviatio n ofth e contro l spike s evaluate d independentl ya t eac h concentratio n leve l mus t b e less tha n o requa l t o 20 % an d th e averag e recover ymust b e 80-120%
. I fth e above criteri a are no t met , th e entir

e set ofsample s shoul d b e re-injecte d o rre-prepare d as appropriate
.

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

t Injectio n Analysi s Pag e 6 4 o f6 7

### Documen t n(S:ftfil)>ei««;6rJierimge^c«r8T:* , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


## 10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s offield matri xspike s an d laborator ymatri xspike s ar

e anticipate d t o b e betwee n 70 % an d 130 % o fth e fortifie d levels
. Sampl e results fo rspike s outsid e o f70 % t o 130% , ma

yb e flagged as suc h (wit h expande d accurac ystatements) , o rwil l no

t b e reporte d du e t o non-complian t qualit ycontro l samples
. Th e targete d fortificatio n level s shoul d b e a t leas t 50 % o fth e endogenou s leve l an d less tha n 1 0 time s th e endogenou s leve l t o b e use d withou t justificatio n t o determin e th e statemen t ofaccurac yfo ranalytica l results
. Th e averag e ofth e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 

## 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t ofanalyt e foun d (i n ng/mL , base d o n pea k area ) usin g th e standar d curve (linea rregressio n parameters ) generate d b ya n appropriat e software program : A, xrJ /

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

xD F Slop e D F = facto rb

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

_Tota l analyt e foun d (ng/mL ) - Averag e analyt e foun d i n sampl e (ng/mL ) Analyt e adde d (ng/mL ) 

## 1 2 Metho d Performanc e An ymetho d performance parameter s tha t ar e no t achieve d must b e considere d i n th e evaluatio n o fth e data
. Nonconformance to an yspecifie d parameter s mus t b e describe d an d discusse d i fth e Technica l Manage r(non GL P study) o rStudyDirecto r(GL P study) choose s t o repor t th e data
. I fcriteri a liste d i n thi s metho d perfonnance sectio n are no t met , maintenance ma

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

t ofth e report
. 

## 12. 1 Syste m Suitabilit y Syste m Suitabilit

ystandard s are no

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

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

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

t have are a counts wit h a n RS D ofS5% an d a retentio n tim e RS D of^2 % t o b e compliant
. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t ofdeterminafio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o r equa l t o 0.990
. Eac h poin t i n th e curve mus t b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

ybe 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 as continuin g calibratio n verification s i n additio n t o bein g par t o fth e calibratio n curve . Th e accurac yof eac h curve poin t mus

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

t Injectio n Analysi s Pag e 6 5 of6 7

### Documen t nmj^tbmismt^rmsm^eTA , fo r1 4 day s fro m 01/26/201 1 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s Attachmen t C Morga n CountyLandfill , Decatur , A L - Novembe r201 0


### Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % o f standard ) an d th e mass spectra l respons e o funiqu e ions
. 

## 12. 3 Sensitivit y Th e targete d limi t ofquantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n o fappropriat e blank

s an d th e accurac

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

e designe d to generat e data tha t are accurat e t o +1-30%
. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d accurac yo flaborator

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

ymatri xspikes
. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks
. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d precisio n oflaborator ycontro l spikes
. 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfonnin g thi s metho d wil l b e dispose d o fappropriately
. Th e origina l sample s wil l b e archive d a

t th e 3 M Environmenta l Laborator yi n accordance wit h interna l procedures
. 1 4 Record s Eac h data packag e generate d fo ra stud ymus t includ e al l supportin g infonnatio n fo rreconstructio n ofth e data
. Infonnatio n fo rth e data packag e mus t include , bu t i s no

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

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

ypages) , instrumen t results files, chromatograms , calibratio n curves , an d dat a calculations
. 1 5 Affecte d Document s None
. 1 6 Revision s Revisio n Numbe rSummar yo fChange s

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

t Injectio n Analysi s Pag e 6 6 of6 7GLP10-01-02 ; Interi m Repor t 1 3 Analysi s o fPFBS , PFH S an d PFO S i n Groundwate rSample s AMcWfl&^l^"^'^ ' Morga n CountyLandfill , Decatur , A L - Novembe r201 0



## RECOR D O F DEVIATION/NONCONFORMANC E

/
. Identificatio n Stud y/ Projec t No
. GLP10-01-02-1 3 Date(s ) o fOccurrence : m101123aandg101215 a Documen t Number : ETS-8-044. 0 Deviatio n typ e D SO P D Equipmen t Procedur e IZ I Metho d (Chec k one ) D Protoco l E l GP O D Other :

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

### Metho d Requirements : (1 ) LC S averag e recover yof100 % ±20%
. (2 ) Sample/Sampl e Duplicat e RP D <20%
. (3 ) Fiel d matri xspik e recover yof100 % ±30%
. 

### Actua l procedure/process : (1 ) LC S averag e recover yfo rbot h set s oflinea ran d branche d PFO S were outsid e metho d acceptanc e criteri a wit h averag e recoverie s of136 % an d 133%
. (2 ) Th e RP D value s fo rPFBS , PFHS , an d PFO S fo ron e samplin g locatio n were >20%
. (3 ) Th e recover

yofth e hig h FM S sampl e fo rDA L G WMC L MW2 B 10111 0 wa s 135%
.



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

### Correctiv e Actio n ( D Ye s 0 No) Reference : Acceptabilityo fth e nonconformin g work : (1 ) I t wa s suspecte d tha t th e EC F stoc k standard use d t o prepare th e linear+branche d LCs ma yhave becom e contaminated
. Anewlinea ran d branche d stoc k standard wa s prepared , wit h newLC S prepare d at th e sam e thre e concentratio n levels
. Two ofth e lowleve l linea ran d branche d LC S coul d not b e calculate d a s th e detecte d concentratio n wa s belo wth e limi t ofquantitation
. On e replicat e at th e lowleve l ha d a recover

yof152% , whil e bot h th e newmi d an d hig h leve l linea ran d branche d LC S me t metho d acceptanc e criteri a wit h averag e recoverie s of114%
. Th e mi d an d hig h leve l LC S concentration s were more appropriat e as compare d t o th e sampl e concentration s reporte d fro m thi s run . Al l LC S were use d i n th e determinatio n ofmetho d uncertainty
. (2 ) Samplin g locatio n DA L GWMC L M E I B 10111 0 ha d RP D value s >20 % fo ral l thre e analytes
. Th e result s wil l b e footnote d i n th e dat a tables
. (3 ) Th e hig h FM S sampl e wa s th e onl yappropriat e spike leve l fo rPFO S fo rthi s samplin g location
. Th e analytica l uncertaintywil l b e adjuste d t o ±35%
. IZ I Other : Deviation s wil l b e note d i n final report
. 

### Project Lead/PA I Approval : Sijsa n Wol f<-_5i,^fV^>H
_ stud yDirecto r(i fGLP) : Sponso rApprova l (fo rGL P protoco l deviations) : N A Technica l Reviewe r(optional) : NA Laborator yDepartmen t Manage rApproval : Date : NA Date : IV
. Authorizatio n t o Resum e Wor k Where haltin g o fwor k

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

### Laborator yDepartmen t Manage rApproval : N AI Date : N A Deviatio n No
. (assigne d b yStud yDirecto ro rTea m Leade ra t th e en d o fstud yo rproject )

Attachmen t AETS-4-008. 7 Pag e 1 o f1

Documentatio n o fDeviation s an d Contro l o fNonconformin g Testin g ^^^ ^ ^ ^ ° ' ^ ^