GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# 3 M

GLP10-01-02 : Interi m Repor t 1 1 - Analysi s o fPFBS
. PFHS
. an d PFO S i n Groun d Wate r Sample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur
. A L i n Novembe r201 0 Stud yTitl e Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Progra m Dat a Requiremen t EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R Par t 79 2 Stud yDirecto r Jaisimh a Kesar i P.E. , DE E Westo n Solutions , Inc
. 140 0 Westo n Way Westchester , 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 , BId g 260-05-N-1 7 Maplewood , M N 55144 Projec t Identificatio n GLP10-01-02-1 1 Tota l Numbe ro fPage s

10 4

Th e testin g reporte d herei n mee t th e requirements o fISO/IE C 17025-200 5 "Genera l Requirement s forth e Competenc e o fTestin g an d Calibratio n L^tMiatories" , I n accordanc e wit h th e A2L ACertificat e #2052.01
. Testin g tha t compile s wit h thi s Intemationa l Standar d als o operat e i n accordanc e wit h IS O 9001:2000
. 

### Testin g Cer t #2052.0 1

Pag e 1 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

Page2of10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

t 1 1 Analysi s o

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

t th e Fonne rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n Novembe r201 0 Study : 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 Program
. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s where there i s n o specifi ctest substance , n o specifi ctest syste m an d n o dosin g o

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

t th e test sit e hav

e no t bee n detennine d unde rGLPs
. 

# t^( ( Gar yHol/enstein , Sponso rRepresentative Date

Jaisimhaf^esari , P.E. , DEE , Stud yDirecto rDate

Pag e 3 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

t 1 1 Analysi s ofPFBS , PFHS , an d PFO S i n Groun d Wate rSample s Collecte d a

t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n Novembe r201 0 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonate (PFHS ) an d Perfluorobutan e Sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program
. Thi s analytica l phas e wa s audite d b yth e 3 M Environmenta l Laborator yQualit yAssurance Uni t (QAU) , a s indicate d i n th e followin g table
. Th e findings were reporte d t o th e principa l investigato r(P.I.) , laborator ymanagemen t an d stud ydirector
.

Inspectio n Date s 3/24/11-3/25/1 1 Phas e Data / Repor t Dat e Reporte d t o

Testin g Facilit y Managemen t 4/25/1 1 Stud yDirecto r 4/25/1 1 

# ^-/O ' 

# u QA U Representative Date

Pag e 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - 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 ofTable s 6 1 Stud yInformatio n 8 2 Summar

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

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

s 1 6 8. 6 La b Contro l Spike s (LCSs ) 1 6 8. 7 Analytica l Metho d Uncertaint y2 1 8. 9 Fiel d Matri xSpike s (FMS ) 2 2

Pag e 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 9 Data Summar

yan d Discussio n 2 3 1 0 Conclusio n 4 3 1 1 Data/Sampl e Retentio n 4 3 1 2 /attachments 4 3 1 3 Signature s 4 4 

### LIS TO F TABLE S Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Results (FSI AGroundwater , Novembe r2010)
. .1 0 Tabl e 2
. Sampl e Descriptio n Ke yCod e 1 3 Tabl e 3
. Instalmen t Parameter s 1 4 Tabl e 4
. Liqui d Chromatograph yCondition s 1 4 Tabl e 5
. Mass Transition s 1 5 Tabl e 6
. Limi t ofQuantitatio n (LOQ ) 1 6 Tabl e 7
. Laborator

yContro l Spik

e Recover

y1 8 Tabl e 8
. Analytica l Uncertaint y2 2 Tabl e 9
. Fiel d Matri xSpik e Level s 2 2 Tabl e 10
. DA L GW130 R 10110 5 2 4 Tabl e 11
. DA L GW130 L 10110 5 2 4 Tabl e 12
. DA L GW130 S 10110 5 2 5 Tabl e 13
. DA L GW131 R 10110 3 2 5 Tabl e 14
. DA L GW131 L 10110 3 2 6 Tabl e 15
. DA L GW131 S 10110 3 2 6 Tabl e 16
. DA L GW132 R 101102 2 7 Tabl e 17
. DALGW132L10110 3 2 7 Tabl e 18
. DA L GW132 S 101102 2 8 Tabl e 19
. DA L G W133 R 101102 2 8 Tabl e 20
. DA L GW133 L 10110 3 2 9

Pag e 6 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 21
. DA L GW133 S 10110 3 2 9 Tabl e 22
. DA L GW134 R 10110 5 3 0 Tabl e 23
. DALGW134 L 10110 5 3 0 Tabl e 24
. DA L GW134 S 10110 5 3 1 Tabl e 25
. DA L G W135 R 10110 5 3 1 Tabl e 26
. DA L GW135 L 10110 5 3 2 Tabl e 27
. DA L GW135 S 10110 5 33 Tabl e 28
. DA L GW136 L 101103 33 Tabl e 29
. DA L GW136 S 10110 3 3 4 Tabl e 30
. DA L G W137 L 10110 9 34 Tabl e 31
. DA L GW137 S 10110 9 35 Tabl e 32
. DA L GW138 S 10111 0 3 6 Tabl e 33
. DA L GW138 L 10111 0 36 Table33
. DALGWCW26 R 10111 0 3 7 Table34
. DALGWCW26 L 10111 0 3 7 Table35
. DALG W140 R 101104 3 8 Table36
. DALG W141 R 10111 0 3 8 Table37
. DALG W142 R 10111 0 3 9 Table38
. DALG W144 R 10111 0 3 9 Tabl e 39
. Tri p Blan k

4 0 Tabl e 40
. Tri p Blan k

2 4 0 Tabl e 41
. Tri p Blan k

3 4 1 Table42
. TripBlank 4 4 1 Tabl e 43
. Rinseat e Blank s 4 2 Tabl e 44
. GLP10-01-02-1 2 Soi l Equipmen t Rinseat e Blan k 4 2

Pag e 7 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - 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 Investigator , (clange@mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Chelsi e Grochow , Analys t Stud yDate s Stud yInitiation : Marc h 8,201 0 Interi m 1 1 Experimenta l Termination : Februar y11,201 1 Interi m Repor

t Completion : Date ofInteri m Repor t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t 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 f104GLP10-01-02 : Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



## \2--'fsWmi^ary. : " 1 1 •Ml, ; 

### Th e 3 M Environmenta l Laborator yreceive d groun d wate rsample s fro m well s locate d a t th e Fonne r Sludg e Incorporatio n Are a (FSIA ) i n Decatur , AL , representin g thirt ydifferen t samplin g locations
. A tota l ofon e hundre d sixty-nin e sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo r perfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , an d include d duplicat e groun d wate rsample s fro m eac h samplin g location
. Sample s als o include d a

t least tw o fleld matri xspik e (FMS ) sample s fo reac h location , fou rtri p blan k sets containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseate blanks
. I n addition , on e soi l equipmen t rinseate blan k fro m GLP10-01-02-1 2 wa s analyzed
. Th e equipmen t rinseate blank s di d not have FM S sample s prepare d fo rdeterminatio n o fPFBS , PFHS , an d PFO S recovery . Th e groun d wate rsamples , tri p blank s an d two equipmen t rinseate blank s associate d wit h GLP10-01 - 02-1 1 were receive d fro m Westo n personne l o n Novembe r18 , 2010
. Th e soi l equipmen t rinseate blan k associate d wit h GLP10-01-02-1 2 wa s receive d fro m Westo n personne l o n Octobe r15,2010
. Al l ofth e sample s were prepare d an d analyze d fo rPFBS , PFHS , an d PFO S followin g 3 M Environmenta l Laborator yMetho d ETS-8-044. 0 an d conducte d unde r3 M projec t GLP-10-01-02-011
. Man yofth e groun d wate rsample s require d dilutio n t o attai n PFBS , PFHS , and/o rPOP S concentration s withi n th e rang e ofth e curve , i n som e instance s u p t o 100-fol d dilutio n were required
. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s are summarize d i n Tabl e 1
. Th e equipmen t rinseate an d th e tri p blan k sample s were belowth e lowe rlimi t ofquantitatio n (LLOQ) , indicatin g adequat e contro l of sampl e contaminatio n durin g shippin g an d sampl e collections
. Th e PFB S concentratio n results fo ral l groun d wate rsample s range d fro m 0.043 1 ng/m L t o 81. 2 ng/mL
. Th e PFH S concentratio n results fo ral l groun d wate rsample s range d fro m 0.091 4 ng/m L t o 83 9 ng/mL
. Th e PFO S concentratio n results fo ral l groun d wate rsample s range d fro m 0.31 5 ng/m L t o 151 0 ng/mL
. Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S + 20% , PFH S + 22 % an d PFO S + 33%
. Fo rsom e samples , th e metho d uncertaint ywa s expande d fo r PFH S o rPFOS
.

Pag e 9 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 1
. Summarize d PFBS , PFHS , an d PFO S Result s (FSI AGroundwater , Novembe r2010)
.
Samplin g Locatio n pALGW130R10110 5 pALGW130S10110 5 pALGW130L10110 5 DA L GW131 R 10110 3 DA L GW131 S 10110 3 DA L GW131 L 10110 3 DA L GW132 R 101102 DALG W132 8 101102 DALGW132L10110 3 DA L GW133 R 101102 DALG W133 8 10110 3 DALGW133L10110 3 DA L GW134 R 101105 DALGW134810110 5 DALGW134L10110 5 DA L GW135 R 101105 DALGW135S10110 5 DALGW135L10110 5 DALG W136 8 10110 3 DALGW136L10110 3 DALG W137 8 10110 9 DA L GW137 L 10110 9 DALG W138 8 10111 0 DALGW138L10111 0 DA L GWCW26 R 10111 0 DA L GWCW26 L 10111 0 DA L GW140 R 101104 DA L GW141 R 10111 0 DA L GW142 R 10111 0 DA L GW144 R 10111 0 Tri p Blank

s (Milli-Q TM Water

) GLP10-01-02-1 1 Equipmen t rinseate blank s GLP10-01-02-1 2 Soi l Equipmen t rinseate blan k PFB S Avg
. Cone
. (ng/mL ) ±RP D 16. 6 ±6.6 % 3.5 0 ±11 % 1.7 7 ±40 % 81. 2 ±4.2 % 0.785 ±3.2 % 3.35 ±4.5 % 8.0 3 ±3.5 % 25. 9 ±2.3 % 8.8 9 ±3.8 % 4.6 1 ±7.6 % 14. 0 ±0.0 % 7.65 ±1.7 % 56. 2 ±13 % 0.143 ±42 % 11. 9 ±3.4 % 81. 0 ±2.7 % 0.79 9 ±1.1 % 5.73 ±3.8 % 2.5 5 ±2.0 % 2,5 3 ±7,9 % 0,102 ±4.9 % 0,082 3 ±2,6 % 4,6 9 ±2,3 % 0.0473 ±5,3 % 8.2 7 ±3,1 % 12, 9 ±5,4 % 1,6 3 ±2.5 % 0.043 1 ±6,0 % 1.6 8 ±1.2 % 1.9 5 ±3.6 % <0.025 0 <0,025 0 <0,025 0 PFH S

Avg
. Cone
. (ng/mL ) ±RP D 12 8 ±0.0 % 31. 3 ±0.32 % 14, 4 ±3.5 % 41 3 ±0,73 % 4,6 3 ±6,3 % 20, 7 ±4,8 % 52. 8 ±5.9 % 20 5 ±1,5 % 77, 2 ±1,2 % 31. 1 ±6.4 % 91. 5 ±1.1 % 53. 4 ±2.4 % 50 3 ±9,4 % 1.7 1 ±6,5%'^ ' 11 2 ±0.0 % 83 9 ±1,9 % 6.2 5 ±3.2 % 35. 9 ±2.5 % 16. 5 ±5,5 % 16, 2 ±8,0 % 0.091 4 ±6.1 % 0.19 9 ±3.4 % 23. 5 ±4.7 % 0.144 ±0.70 % 63, 1 ±4.3 % 92, 9 ±5.8 % 17, 2 ±0,0 % 0.25 8 ±12 % 9,9 8 ±0.40 % 8,5 7 ±5.1 % <0.025 0 <0.025 0 <0.025 0 PFO S

Avg
. Cone
. (ng/mL ) ±RP D 58 3 ±2,4 % 11 7 ±3,4 % 82. 7 ±5.9 % 151 0 ±2.6 % 5.55 ±5.6 % 34, 3 ±5,0 % 29 5 ±1.7 % 63 3 ±12 % 29 3 ±5.5 % 60. 8 ±6,1 % 22 4 ±3,6 % 20 4 ±1,5 % 142 0 ±15 % 11. 4 ±1.8 % 57 9 ±2.6 % 89 2 ±2,6 % 4.8 8 ±5.3 % 22, 6 ±12 % 87. 1 ±3.7 % 79. 2 ±8.8 % 0,31 5 ±33%*^'^ ' 0.89 3 ±3,6 % 24 5 ±5,7 % 0.58 1 ±0.17 % 45 1 ±2.0 % 84 8 ±9.4 % 136 ±6.6 % 4.2 3 ±12 % 108 ±6.5 % NR<^ ' <0,25 0 <0.25 0 <0.25 0 Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results are : PFB S ±20% , PFH S ±22% , an d PFO S ±33%
. (1 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFH S base d o n FM S recover yfor : DA L G W134 S t o ±35%
. (2 ) Th e analytica l uncertaint yhas bee n adjuste d fo rPFO S base d o n FM S recover yfo rDA L G W137 S t o ±4 1 %
. Se e discussio n i n sectio n 9 ofth e report
. (3) Th e RP D di d no

t meet metho d acceptance criteri a ofS20%
. (4) N R = No

t Reported ; Matri xspik

e recover ywa s <50% , Se e sectio n 9 ofth e repor t fo radditiona l Infomnatlon ,

Pag e 1 0 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 3 Introductio n Thi s analytica l stud ywa s conducte d a s par t ofth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama
. Th e objective o fth e overal l progra m i s t o gai n infonnatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h a s groun d water , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility
. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d a t th e Forme rSludg e Incorporatio n Are a (FSAI ) i n Decatur , A L fo rPFBS , PFHS , an d PFO S i n a n effor t t o characteriz e on sit e groundwate rconditions
. Th e 3 M Environmenta l Laborator yprepare d sampl e container s (25 0 m L high-densit

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

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

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

e levels
. Th e aqueou s equipmen t rinseate sample s were collecte d i n plai n bottle s withou t mari<ings o r fortifications
. Sample s were prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 "Detemninatio n ofPerfiuorinate 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 sample s collected , th e tri p blanks , aqueou s equipmen t rinseate blanks , an d aqueou s soil-equipmen t rinseate blan k samples
. Table s 10-4 4 summariz e th e individua l sampl e results an d th e associate d field matri x spike recoveries
. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewhere i n thi s repor t
4 Ties f& Contro l Substance s There wa s not a test substance o rcontro l substance s i n th e classi csens e ofa GL P study
. Thi s stud y wa s purel yanalytica l i n nature
.

Pag e 1 1 o f104

## 5 Referenc e Substance s GLP10-01-02 ; Interi m Repor t 1 1 Analysi s ofPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - 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 PFB S (piredominantl ylinear ) Perfluorobutan e sulfonat e C4F9SO3 " Potassiu m Sal t 3 M 1/10/201 7 Froze n 41-2600-8442- 5 TCR-12 1 Whit e Powde r 96,7 % PFH S (linear ) Perfluorohexan e sulfonate C6F13SO3 " Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHX8AM08 TCR08-001 8 Crystallin e 98 %

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO S (linear ) Perfluorooctan e sulfonat e CgFiySO a 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 sulfonat e CsFiySOs ' Potassiu m Sal t CA S # 2795-39- 3 3 M 12/14/201 6 Froze n 17 1 TCR-69 6 Whit e Powde r 86.4 %

Pag e 1 2 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 6 Tes t Syste m Th e test syste m fo rthi s stud yare groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b y Westo n Solutions , Inc
. personnel
. Sample s fo rthi s stud yar e "rea l worid " samples , no t dose d wit h a specifi clo t oftest substance
. Tabl e 2
. Sampl e Descriptio n Ke yCode
. Strin g Numbe r Exampl e 1 2 3 4

5 Strin g Descripto r DA L GW135LD B 101105 Samplin g Locatio n Sampl e Typ e Samplin g Poin t Wel l Leve l Samplin g Dat e Sampl e Typ e Exampl e DA L = Decatur , A L GW = Groundwate r Example : 13 5 R = Residu m shallo wwater-bearin g zon e L = Bedroc k

water-bearin g zon e S = Epikars t middl e water-bearin g zon e 101105 = Novembe r5 , 201 1 0=primarysampl e DB=duplicat e sampl e L S = lo wspik e M S = mi d spik e H S = hig h spik e


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

## 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory
. Sampl e bottle s associate d wit h GLP10-01-02-1 1 were returne d t o th e laborator ya t ambien t condition s o n Novembe r18 , 2010
. Th e equipmen t rinseate blan k associate d wit h GLP10-0 1 -02-1 2 wa s returne d t o th e laborator ya t ambien t condition s o n Octobe r15,2010
. Sample s were store d refrigerate d a t th e laborator

yafte rreceipt
. Aset oflaborator yprepare d Tri p Blan k

an d Tri p Blan k field matri xspike s were sen t wit h eac h coole ro fsampl e collectio n bottles
. 

## 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis
. Sample s that require d dilutio n were prepare d b ydilution s ofIm L sampl e wit h 9 mL s o fMill i Q wate r (dilutio n 1:10)
. Most samplin g location s were dilute d 1:100 b yfurthe rdilutin g th e 1:1 0 dilutio n wit h additiona l Mill i Q water
.

Pag e 1 3 o f104GLP10-01-02 : Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



## 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 performance 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 cmas s transition s analyze d ar e describe d i n th e ra

wdat a har

d copie s place d i n th e final data packet , an d ar e briefl ydescribe d below
. Al l sample s were inifiall yprepare d o n 12/30/10
. Du e t o th e larg e numbe rofsample s requirin g analysis , alon g wit h networ k

communicatio n en'or

s that were experience d durin g th e analysis , th e sample s were broke n u p into thre e analytica l runs . Th e LC S sample s prepare d wit h th e sample s o n 12/30/1 0 were re analyze d wit h eac h analytica l batc h analyze d o n ETS Buste rfro m 1/7/1 1 -1/4/11
. Tabl e 3
. Instrumen t Parameters
. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r io n Sourc e Electrod e Polarit y Softwar e ETS Buste r ETS-8-044, 0 1/7/11,1/10/11 , an d 1/14/1 1 -PFBS , PFHS , an d PFO S Agilen t 1100 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 u

2or10n L Applie d Blosystem s AP

\ 400 0 Turtj o Spra

y Turtj o io n electrod e Negativ e /Analys t 1.4, 2 ETS Ginge r ETS-8-044. 0 2/11/11-PFBSan d PFO S Agilen t 110 0 Pris m R P (2. 1 m m X 5 0 mm) , 5 n Betasi l CI S (2. 1 rrir n X 100 mm) , 5 n

5or10^ L Applie d Blosystem s AP I 500 0 Turt) 0 Spra

y Turb o Io n electrod e Negative Analyst 1.4. 2 

### Tabl e 4
. Liqui d Chromatograph yConditions
. ste p Numbe r
0 1 2 3 4 5 Tota l Tim e

(min )
0 2. 0 14. 5 15. 5 16. 5 20. 0 Flo wRat e

(fdJmin ) Percen t A

( 2 m M ammoniu m acetate ) ETS-8-044. 0 Analyze d o n ETS Buste r 30 0 30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5, 0 5, 0 97. 0 97. 0 Percent B

(Methano O 3. 0 3. 0 95, 0 95. 0 3. 0 3. 0 ETS-8-044. 0 Analyze d o n ETS Ginge r 0 1 2 3 4 5 0

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

30 0 30 0 30 0 30 0 30 0 97. 0 97. 0 5, 0 5, 0 97. 0 97, 0 3. 0 3. 0 95, 0 95, 0 3. 0 3. 0

Pag e 1 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 5
. Mas s Transitions
.

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

Structur e Linea r Linea r
Linea r
Dwel l tim e wa s 5 0 mse cfo reac h transition
. Th e individua l transition s wer e summe d t o produce a "tota l io n chromatogram " (TIC) , whic h was

use d fo rquantitation
.


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

yspikin g know n amounts o fth e stoc k solutio n containin g th e targe t analyte s into prepare d i n Mill i Q water
. Atota l offifteen spike d standard s rangin g fro m 0.02 5 ng/m L t o 100 ng/m L (nominal ) were analyzed
. Lo

wo rhig h curve points ma yhave bee n disable d t o mee t metho d criteria
. Aquadratic , 1/ x weighted , calibratio n curve o fth e pea k are a counts wa s use d t o fit th e dat a fo reac h analyte
. Th e data were no t force d throug h zero durin g th e fitting process . Calculatin g th e standar d concentration s usin g th e pea k are a confinne d accurac

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

yrequirements of100±25 % (100±30 % fo rth e lowest curve point) were me t fo ral l analytes
. Th e con-elatio n coefficien t (r ) wa s greate rtha n 0.99 5 fo rPFBS , PFHS , an d PFOS
. 8. 2 Syste m Suitabilit y Acalibratio n standar

d wa s analyze d fou rtime s a t th e beginnin g ofeac h analytica l sequence t o demonstrat e overal l syste m suitability
. Th e acceptance criteri a ofles s tha n o requa l t o 5% relative standar d deviatio n (RSD ) fo rpea k are a an d retentio n tim e criteri a o fles s tha n o requa l t o 2 % RS D wa s met fo rPFBS , PFHS , an d PFOS
. 8. 3 Limi t o fQuantitatio n (LOQ ) Th e LO Q fo rthi s analysi s i s th e lowest non-zer o calibratio n standar

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

yrequirements an d fo rwhic h th e are a counts ar e a t leas t twic e thos e ofth e appropriat e blanks
. Th e LOQ fo ral l analyte s ca n b e foun d i n Tabl e 6
.

Pag e 1 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 6
. Limi t o fQuantitatio n (LOQ)
. Analysi s Dat e 1/7/1 1 an d 1/10/1 1 Analysi s

1/14/1 1 Analysi s 2/11/1 1 Analysi s
2/28/1 1 Analysi s Dilutio n 1 5 1 0 100 5 0 100 1 1 0 100 1 0 PFB S

LOQ , ng/m L 0,025 0 0.12 5 0,25 0 2,5 0 1.2 5 2.5 0 0,025 0 0,25 0 2,5 0 NA PFH S

LOQ , ng/m L 0.025 0 0.12 5 0.25 0 2.5 0 1.2 5 2.5 0 0.025 0 0.25 0 2,5 0 NA PFO S

LOQ , ng/m L 0.25 0 1.2 5 2.5 0 25. 0 12. 5 25. 0 0,030 0 0.30 0 3,0 0 0.25 0 N A= No t Applicabl e 

## 8. 4 Continuin g Calibratio n Durin g th e cours e ofeac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control
. Al l CCVs met metho d criteri a of100 % ±25 % fo rPFBS , PFHS , an d PFOS
. 

## 8. 5 Blank s Tw o type s o fblank

s were prepare d an d analyze d wit h th e samples : metho d blank s an d field/trip blanks
. Metho d blan k

results were reviewe d an d use d t o evaluat e metho d peri'onnance an d t o determin e th e LO Q fo reac h analyt e 

## 8. 6 La b Contro l Spike s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set
. LCS s were prepare d byspikin g know n amounts ofth e analyt e int o Mill i Q wate rt o produce th e desire d concentration
. Th e spike d wate rsample s were the n prepare d an d analyze d i n th e sam e manne ra s th e samples
. Th e metho d acceptance criteria , averag e ofLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D 520%AI I sample s were initiall yprepare d o n 12/30/10
. Du e t o th e larg e numbe ro fsample s requirin g analysis , alon g wit h networi < communicatio n error s that were experience d durin g th e analysis , th e sample s were broke n u p into thre e analytica l runs . Th e LC S sample s prepare d wit h th e sample s o n 12/30/1 0 were re-analyze d wit h eac h analytica l batc h analyze d o n ETS Buste rfi-om 1/7/1 1 -1/4/11
. 1/7/1 1 Analysis : Du e t o a n autosample rerror , th e third replicat e ofth e lo wset o fLC S sample s di d no t inject
. Th e averag e recover yfo rth e lo

wset ofLC S fo rPFB S wa s 122 % an d fo rPFH S 123%
. Al l othe r LC S analyze d i n thi s ru n me t metho d acceptance criteria
. 1/10/1 1 Analysis : Th e lo

wset ofLC S sample s fo rPFH S had a n averag e recover yof122%
. Al l othe r LC S analyze d i n thi s ru n me t metho d acceptacn e criteria
. 1/14/1 1 Analysis : Al l thre e set s ofLC S metho d acceptance criteri a fo rPFBS , PFHS , an d PFOS
. 2/11/1 1 Analysis : Al l thre e sets o fLC S metho d acceptance criteri a fo rPFBS , PFHS , an d PFOS
. A s th e reference materia l use d fo rquantitatio n o fPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s are comprise d ofbot h linea ran d branche d isomers , additiona l LC S sample s of

Pag e 1 6 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### PFO S (linea ran d branched ) were prepare d a t thre e concentration s i n triplicat e t o evaluat e th e potentia l fo ranalytica l bias
. 1/7/1 1 Analysis : Th e lo

wan d mi d sets oflinea ran d branche d PFO S LC S met metho d acceptance criteria , whil e th e averag e recover yofth e hig h set ofLC S sample s wa s 123%
. 1/10/1 1 Analysis : Th e lo wan d mi d sets oflinea ran d branche d PFO S LC S me t metho d acceptance criteri a whil e th e hig h set had a n averag e recover yof121%
. 1/14/1 1 Analysis : Al l thre e sets oflinea ran d branche d PFO S LC S met metho d acceptance criteria
. 2/11/1 1 Analysis : Th e lowan d mi d sets oflinea ran d branche d PFO S LC S met metho d acceptance criteri a whil e th e hig h se t ha d a n averag e recover yo f133%
. Th e recover

yo fth e hig h sets oflinea ran d branche d PFO S suggest possibl e analytica l bia s whe n sample s containtin g bot h linea ran d branche d isomer s o fPFO S are quantitate d against a calibratio n curve constnjcte d ofprimaril ylinea rPFOS
. Therefore , th e analytica l metho d uncertaint yfo rthi s stud y ha s bee n adjuste d base d o n th e highest averag e recover yofth e linea ran d branche d PFO S LC S sample s t o ±33%
. Th e followin g calculafion s were use d t o generat e dat a i n Tabl e 7 fo rlaborator ycontro l spikes
.

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

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

y

Pag e 1 7 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 7
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Analyze d 1/7/1 1
La b I D LCS-101230- 1 LCS-101230- 2 LCS-101230- 3 Averag e ±%RS D LCS-101230- 4 LCS-101230- 5 LC8-101230- 6 Averag e ±%RS D LC8-101230- 7 LC8-101230- 8 LC8-101230- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 NA'^ ' Calculate d

Concentratio n (ng/mL ) 0.63 1 0.58 0 NA<^ > '/oRecover y

12 7 11 7 NA<=^ ' 122±5.8%<^ ' 4.9 7 4.9 7 4.9 7 6,0 1

5,8 6 5,8 7 12 1

11 8 11 8 119 % ±1.5 % 29. 9 29. 9 29. 9 30, 6

29, 8 29, 9 10 2

99, 6 10 0 101 % ±1.3 % PFH S Spike d Concentratio n (ng/mL ) 0.49 8 0,49 8 NA<= ' Calculate d

Concentratio n (ng/mL ) 0,63 1 0,59 5 NA<^ ' %Recover y

12 7 11 9 NA'^ ' 123 % ±4.6%'^ ' 4.9 8 4.9 8 4.9 8 5.9 4

5.8 3 5.8 6 11 9

11 7 11 8 118 % ±0.85 % 29. 9 29. 9 29. 9 30. 7

29. 6 30. 5 10 3

99, 0 10 2 101 % ±2.1 %
ETS-8-044. 0 Analyze d 1/7/1 1
L a b I D LCS-101230- 1 LC8-101230- 2 LC8-101230- 3 Averag e ±%RS D LCS-101230- 4 LCS-101230- 5 LCS-101230- 6 Averag e ±%RS D LC8-101230- 7 LCS-101230- 8 LC8-101230- 9 Averag e ±%RS D PFO S (linear ) Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 NA<2 ' Calculate d

Concentratio n (ng/mL ) 0,52 4 0,50 7 NA<^ * %Recover y

10 5 10 2 NA<^ ' 104 % ±2.0 % 4.9 7 4,9 7 4,9 7 5.8 1

5.7 8 5.8 1 11 7

11 6 11 7 117 % ±0.49 % 29, 9 29. 9 29, 9 31. 2

31. 7 31, 3 10 4

10 6 10 5 105 % ±1.0 % La b I D LCS-101230-1 0 LCS-101230-1 1 LCS-101230-1 2 Averag e ±%RS D LCS-101230-1 3 LCS-101230-1 4 LCS-101230-1 5 Averag e ±%RS D LC8-101230-1 6 LCS-101230-1 7 LCS-101230-1 8 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 0,49 2 0,49 2 NA'^ ' Calculate d

Concentratio n (ng/mL ) 0,53 9 0,49 8 NA<^ ' XRecover y

11 0 10 1 NA<= ' 106 % ±6.0 % 4,9 3 4,9 3 4,9 3 6.1 0

5.8 7 5,7 7 12 4

11 9 11 7 120 % ±3.0 % 29. 6 29. 6 29. 6 36, 4

35, 7 37, 3 12 3

12 1 12 6 123 % ±2.0%'^ ' (1 ) Th e averag e recover ydi d no t meet metho d acceptance criteri a o f100 % ±20%
. (2 ) NA= No

t applicable : LC S wa s no

t injecte d du e t o a n autosample rerror .

Pag e 1 8 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate r Forme rSludg e Incorporatio n Area - Novembe r201 0



### Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. ETS-8-044. 0 Analyze d 1/10/1 1
La b I D LC8-101230- 1 LCS-101230- 2 LCS-101230- 3 Averag e ±%RS D LCS-101230- 4 LC8-101230- 5 LC8-101230- 6 Averag e ±%RS D LCS-101230- 7 LCS-101230- 8 LC8-101230- 9 Averag e ±%RS D PFB S

Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 0,49 7 Calculate d

Concentratio n (ng/mL ) 0.62 0 0.57 8 0.57 8 VoRecover

y 12 5 11 6 11 6 11 9 ±4.4 % 4,9 7 4,9 7 4,9 7 5.9 3

5.7 7 5.7 2 11 9

11 6 11 5 117 % ±1.8 % 29, 9 29. 9 29. 9 30. 4

29, 3 29, 2 102

98, 0 97, 8 99.3 % ±2.4 % PFH S Spike d Concentratio n (ng/mL ) 0,49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0.62 7 0,58 6 0,60 2 VoRecover y 12 6 11 8 12 1 122 % ±3.3%'^ ' 4,9 8 4,9 8 4,9 8 6,1 5

5,9 7 5.8 6 12 3

12 0 11 8 120 % ±2.1 % 29, 9 29. 9 29. 9 30. 8

30. 1 29. 8 10 3

10 1 99, 6 101 % ±1.7 % ETS-8-044, 0 Analyze d 1/10/1 1
La b I D LCS-101230- 1 LCS-101230- 2 LC8-101230- 3 Averag e ±%RS D LCS-101230- 4 LCS-101230- 5 LCS-101230- 6 Averag e ±%RS D LCS-101230- 7 LCS-101230- 8 LC8-101230- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 0.49 7 Calculate d

Concentratio n (ng/mL ) 0.53 6 0.53 2 0,51 2 '/oRecover

y 10 8 107 10 3 106 % ±2.5 % 4.9 7 4,9 7 4,9 7 5.9 2

5.8 4 5.8 7 11 9

11 8 11 8 118 % ±0.49 % 29. 9 29. 9 29. 9 30. 6

30. 7 30. 3 102

10 3 10 1 102 % ±0.98 % La b I D LCS-101230-1 0 LC8-101230-1 1 LCS-101230-1 2 Averag e ±%RS D LCS-101230-1 3 LC8-101230-1 4 LCS-101230-1 5 Averag e ±%RS D LCS-101230-1 6 LC8-101230-1 7 LC8-101230-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0,49 2 0,49 2 0,49 2 Calculate d

Concentratio n (ng/mL ) 0.55 9 0.50 9 0.55 1 VoRecover

y 11 4 10 3 11 2 110 % ±5.3 % 4.9 3 4.9 3 4.9 3 5.9 7

5.6 9 5,6 5 12 1

11 5 11 5 117 % ±3.0 % 29, 6 29, 6 29. 6 35, 2

36, 0 35. 9 11 9

12 2 12 1 121 % ±1.3%'^ ' (1 ) Tli e averag

e recover ydi d no t mee t mettio d acceptanc

e criteri a o f100 % ±20%
. (2 ) N A= No t applicable ; LC

S wa s no t Injecte d due t o an autosamplererror.

Pag e 1 9 o f10 4GLP10-01-02 : Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. ETS-8-044, 0 Analyze d 1/14/1 1
La b I D LC8-101230- 1 LCS-101230- 2 LC8-101230- 3 Averag e ±%RS D LC8-101230- 4 LC8-101230- 5 LCS-101230- 6 Averag e ±%RS D LCS-101230- 7 LC8-101230- 8 LCS-101230- 9 Averag e ±%RS D PFB S

Spike d Concentratio n (ng/mL ) 0.49 7 0,49 7 0,49 7 Calculate d

Concentratio n (ng/mL ) 0.61 2 0,58 9 0,59 0 VoRecover

y 12 3 11 9 11 9 12 0 ±1.9 % 4.9 7 4.9 7 4.9 7 5.9 9

5,7 3 5,7 8 12 1

11 5 11 6 117 % ±2.7 % 29. 9 29. 9 29. 9 30, 4

30, 1 29, 9 102

10 1 99, 9 101 % ±1.0 % PFH S Spike d Concentratio n (ng/mL ) 0,49 8 0,49 8 0,49 8 Calculate d

Concentratio n (ng/mL ) 0.60 2 0,58 9 0,58 9 VoRecover y 12 1 11 8 11 8 119 % ±1.5 % 4.9 8 4.9 8 4.9 8 6,0 3

5,8 2 5,8 1 12 1

11 7 11 7 118 % ±2.0 % 29. 9 29. 9 29. 9 31, 0

30, 5 30. 5 104

102 102 103 % ±1.1 % ETS-8-044. 0 Analyze d 1/14/1 1
La b I D LCS-101230- 1 LCS-101230- 2 LCS-101230- 3 Averag e ±%RS D LCS-101230- 4 LC8-101230- 5 LC8-101230- 6 Averag e ±%RS D LC8-101230- 7 LCS-101230- 8 LCS-101230- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0,49 7 0,49 7 0.49 7 Calculate d

Concentratio n (ng/mL ) 0.52 3 0.51 7 0.50 4 VoRecover

y 10 5 104 10 1 103 % ±2.0 % 4.9 7 4.9 7 4.9 7 5.8 7

5.6 6 5.7 2 11 8

11 4 11 5 116 % ±1.8 % 29. 9 29. 9 29. 9 31, 2

31, 6 30, 7 104

10 6 10 3 104 % ±1.5 % La b I D LCS-101230-1 0 LCS-101230-1 1 LC8-101230-1 2 Averag e ±%RS D LC8-101230-1 3 LCS-101230-1 4 LCS-101230-1 5 Averag e ±%RS D LCS-101230-1 6 LCS-101230-1 7 LCS-101230-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0.49 2 0.49 2 0.49 2 Calculate d

Concentratio n (ng/mL ) 0.52 2 0,47 2 0,52 7 VoRecover

y 106 96, 0 107 103 % ±5.9 % 4.9 3 4,9 3 4,9 3 6.0 3

5,6 9 5.6 5 12 2

11 5 11 5 117 % ±3.4 % 29, 6 29. 6 29. 6 34. 6

36. 0 36. 1 11 7

12 2 12 2 120 % ±2.4 % (1 ) Th e averag e recover ydi d no t meet metho d acceptance criteri a of100 % ±20%
. (2 ) N A= No

t applicable ; LC S wa s no t injecte d du e t o a n autosample rerror .

Pag e 2 0 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 7 continued
. Laborator yContro l Spik e Recovery
. ETS-8-044, 0 Analyze d 2/11/1 1
La b I D LCS-110210- 1 LCS-110210- 2 LCS-110210- 3 Averag e ±%RS D LCS-110210- 4 LC8-110210- 5 LCS-110210- 6 Averag e ±%RS D LCS-110210- 7 LCS-110210- 8 LCS-110210- 9 Averag e ±%RS D PFB S

Spike d Concentratio n (ng/mL ) 0,49 8 0,49 8 0,49 8 Calculate d

Concentratio n (ng/mL ) 0,56 3 0,54 2 0,58 1 VoRecover

y 11 3 10 9 11 7 11 3 ±3.5 % 4,9 8 4,9 8 4,9 8 5,3 7

5,5 2 5.5 8 10 8

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

31, 1 32, 0 10 0

104 10 7 104 % ±3.6 % PFH S Spike d Concentratio n (ng/mL ) 0,49 8 0,49 8 0,49 8 Calculate d

Concentratio n (ng/mL ) 0,60 3 0,59 4 0.59 9 VoRecover y 12 1 11 9 12 0 120 % ±0.83 % 4,9 8 4,9 8 4,9 8 5.6 1

5,3 6 5,9 6 11 3

10 8 12 0 114 % ±5.3 % 29, 9 29, 9 29, 9 30. 7

30, 8 32. 7 103

103 10 9 105 % ±3.3 % ETS-8-044, 0 Analyze d 2/11/1 1
La b I D LCS-110210- 1 LC8-110210- 2 LCS-110210- 3 Averag e ±%RS D LCS-110210- 4 LC8-110210- 5 LC8-110210- 6 Averag e ±%RS D LC8-110210- 7 LCS-110210- 8 LCS-110210- 9 Averag e ±%RS D PFO S (linear)

Spike d Concentratio n (ng/mL ) 0,49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0,65 0 0,58 7 0,54 0 VoRecover

y 13 0 11 8 10 8 119 % ±9.3 % 4.9 8 4.9 8 4,9 8 5,4 3

4.9 3 5,8 6 10 9

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

30. 7 32. 4 103

103 10 8 105 % ±2.8 % La b I D LCS-110210-1 0 LC8-110210-1 1 LC8-110210-1 2 Averag e ±%RS D LCS-110210-1 3 LCS-110210-1 4 LCS-110210-1 5 Averag e ±%RS D LCS-110210-1 6 LCS-110210-1 7 LC8-110210-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0.50 2 0.50 2 0.50 2 Calculate d

Concentratio n (ng/mL ) 0,53 9 0,58 5 0,54 1 VoRecover

y 10 7 11 7 10 8 111 % ±5.0 % 5.0 4 5.0 4 5,0 4 6,1 5

5,3 8 5,4 4 12 2

107 108 112 % ±7.5 % 30, 2 30, 2 30. 2 40. 7

40. 4 39. 6 135

134 13 1 133 % ±1.6

% <^ ' (1 ) Th e averag e recover ydi d no t meet metho d acceptance criteri a o f100 % ±20%
. (2 ) N A= No

t applicable ; LC S wa s no t injecte d du e t o a n autosample rerror .

Pag e 2 1 of104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

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

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

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h con-espond s t o a confidence leve l of95%
. Th e mos t recen t 5 0 dat a points were use d t o generat e th e metho d uncertaint

yvalue s liste d i n Tabl e 8
. Th e analytica l metho d uncertaint yfo rPFO S whe n calculate d followin g th e above describe d procedur e wa s foun d t o b e ±^8%
. However , du e t o potentia l analytica l bias that wa s observe d whe n quantitatin g LC S sample s containin g linea ran d branche d isomer s ofPFOS , th e analytica l fo rPFO S ha s bee n expande d t o ±33%
. Tabl e 8
. Analytica l Uncertainty
. Analyt e PFB S PFH S PFO S Standar d Deviatio n

10. 9 11. 0 9.07 Metho d Uncertaint y

±20 % ±22 % ±33%' " (1 ) Se e sectio n 8. 6 o fth e repor t fo ra discussio n ofth e assignin g ofth e analytica l metho d uncertaint yfo rPFOS , 

### 8. 8 Fiel d Matri xSpike s (FMS ) Low , mi d an d hig h fiel d matri xspike s (FMS ) were collecte d a t eac h samplin g poin t (lowan d hig h FM S onl ya t 131R , 134R , an d 135R) t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix
. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offield sampl e t o a containe rspike d b yth e laborator

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

e wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Fiel d matri xspik e concentration s must b e 50% ) ofth e sampl e concentratio n t o b e considere d a n appropriat e field spike
. Fiel d matri xspike s ar e presente d i n sectio n 9 o fthi s report
. Tabl e 9
. Fiel d IVIatri xSpik e Levels
. Samplin g Locatio n 136R , 137R , 137s , 137L , 138 L
130L , 131L , 132L , 133R , 134S , 134L , 136 S 130R , 130S , 131S , 132R , 132S , 133S , 133L , 135S , 135 L , 136L , 138 S , 138 R
131R , 134R , 135 R
Tri p Blan k Spik e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h PFBS , ng/m L

0.097 2 0.97 2 9.7 2 0.97 2 9,7 2 97, 2 9,7 2 97, 2 97 2 97. 2 97 2 0.97 2 9.7 2 97. 2 97 2 PFHS , ng/m L

0.096 1 0,96 1 9,6 1 0,96 1 9,6 1 96, 1 9.6 1 96. 1 96 1 96, 1 96 1 0,96 1 9,6 1 96. 1 96 1 PFOS , ng/m L

0.097 8 0.97 8 9.7 8 0,97 8 9,7 8 97, 8 9,7 8 97. 8 97 8 97. 8 97 8 0,97 8 9,7 8 97. 8 97 8

Pag e 2 2 o f104GLP10-01-02 : Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

(Sample Concentrationof

FM S - Average Concentration : Fiel dSampl e & FieldSampl

e Dup. ) ^ , „„„ , FM S Recover y = -^ ^ : - ^-^ * 100% Spik e Concentraton 

## 8. 9 Laborator yMatri xSpike s (LMS ) Th e mi d FM S sampl e fo rDA L G W144 R analyze d o n 1/10/1 1 di d no t meet metho d acceptance criteri a fo rPFO S wit h a recover

yof28.7%)
. Th e hig h FM S sampl e analyze d o n 1/10/1 1 exceede d th e instrumen t calibratio n range . Furthe rdilutio n ofth e hig h FM S sampl e wa s no t performe d since th e hig h FM S sampl e (spik

e leve l 97 8 ng/mL) wa s no t appropriat e a s compare d t o th e observe d sampl e concentration
. Th e sampl e se t wa s reanalyze d o n 2/28/1 1 alon g wit h a 5 0 ng/m L laborator ymatri x spike
. Laborator

ymatri xspike recoverie s withi n metho d acceptance criteri a of100±30 % confin n that "unknown " components i n th e sampl e matri xd o no t significantl yinterfer

e wit h th e extractio n an d analysi s ofth e analyte s ofinterest
. Se e sectio n 9 fo ra discussio n ofth e PFO S results
. 

## 9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blanks
. Results an d averag e value s are rounde d t o thre e significan t figures accordin g t o EP Aroundin g rules
. Becaus e ofrounding , value s ma yvar yslightl y fro m thos e liste d i n th e ra wdata
. Fiel d matri xspik

e recoverie s meetin g th e metho d acceptance criteri a of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G W134 S - Th e recover yofth e lo wFM S sampl e fo rPFH S wa s 135%)
. Th e mi d an d hig h FM S sample s me

t metho d acceptance criteria
. Since th e lo wspik e wa s th e most appropriat e spik e leve l as compare d t o th e sampl e concentration , th e analytica l uncertaint yhas bee n adjuste d fo rPFH S t o 100 % ±35%
. DA L G W137 S - Th e recover yo fth e mi d FM S sampl e fo rPFO S wa s 58.8%) , whil e th e recover yofth e hig h FM S wa s 59.4%i
. Since th e mi d spike was th e most appropriat e spik e leve l a s compare d t o th e sampl e concentration , th e analytica l uncertaint yha s bee n adjuste d fo rPFO S t o 100% ) ±41%
. DA L GW144R-Th e sampl e set wa s dilute d 1:1 0 an d analyze d o n 1/10/11
. Th e recover yofth e mi d FM S sampl e fo rPFO S wa s 28.7%)
. Th e hig h FM S sampl e exceede d th e instrumen t calibratio n range . Furthe rdilutio n o fth e hig h FM S sampl e wa s no t performe d sinc e th e hig h FM S sampl e (spik e leve l 97 8 ng/mL) wa s no

t appropriat e a s compare d t o th e sampl e concentration
. Th e sampl e set wa s re-dilute d an d analyze d o n 2/28/1 1 alon g wit h a 49. 8 ng/m L laborator ymatri xspike
. Th e recover yofth e mi d FM S sampl e wa s 33.4%) , an d th e recover yofth e LM S sampl e wa s 294%
. Since th e recover yo fbot h matri xspike sample s wa s <50%) , n o PFO S results wil l b e reporte d fo rDA L G W144R
.

Pag e 2 3 of104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 10
. DA L G W130 R 10110 5

3 M LIM S I D GLP10-01-02-11-00 1 GLP10-01-02-11-00 2 GLP10-01-02-11-00 3 GLP10-01-02-11-00 4 GLP10-01-02-11-00 5 Averag e Concen t Descriptio n

DA L GW130 R 0 10110 5 DALGW130RDB10110 5 DA L GW130RL S 10110 5 DA L GW130 R M S 10110 5 DA L GW130RH S 10110 5 ratio n (ng/mL ) + VoRP D PFB S Concentratio n (ng/mL ) 16. 0 17. 1 28. 0 12 2 99 8 VoRecover

y NA NA 11 8 108 10 1 16. 6 ng/m L ±6.6 % PFH S Concentratio n (ng/mL ) 12 8 12 8 14 0 23 2 112 0 VoRecover

y NA NA N C 10 8 103 12 8 ng/m L ±0.0 % PFO S Concentratio n (ng/mL ) 59 0 57 6 60 6 62 6 149 0 VoRecover

y N A N A N C N C 92. 7 58 3 ng/m L ±2.4 % N A= No t /Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spike level
. PFBS , PFHS , an d PFO S were analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. 

### Tabl e 11
. DA L G W1 SOL 10il0 5

3 M LIM S I D GLP10-01-02-11-01 1 GLP10-01-02-11-01 2 GLP10-01-02-11-01 3 GLP10-01-02-11-01 4 GLP10-01-02-11-01 5 Descriptio n DA L GW130 L 0 10110 5 DA L GW130LD B 10110 5 DALGW130LLS10110 5 DA L GW130 L M S 10110 5 DALGW130LHS10110 5 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 1.80 1.73 2.9 1 13. 0 10 7 VoRecover

y NA N A 11 8 11 6 108 1.77 ng/m L ±4.0 % PFH S Concentratio n (ng/mL ) 14. 1 14. 6 15. 9 25. 3 11 9 %Recover

y N A N A N C 11 4 10 9 14. 4 ng/m L ±3.5 % PFO S Concentratio n (ng/mL ) 85. 1 80. 2 82. 1 84. 5 18 2 VoRecover

y N A N A N C N C 10 2 82. 7 ng/m L ±5.9 % N A= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n I s greate rtha n 2 xtfi e spike level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/7/1 1 wit h a 1:1 0 dilution
.

Pag e 2 4 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 12
. DALG W1 SO S 10110 5

3 M LIM S I D GLP10-01-02-11-00 6 GLP10-01-02-11-00 7 GLP10-01-02-11-00 8 GLP10-01-02-11-00 9 GLP10-01-02-11-01 0 Descriptio n DALG W130 8 0 10110 5 DALG W130 8 D B 10110 5 DALG W130 8 LS 10110 5 DALG W130 8 M S 10110 5 DALG W130 8 H S 10110 5 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 3.3 0 3.7 0 13. 9 10 9 102 0 VoRecover

y N A N A 10 7 10 9 10 5 3.5 0 ng/m L ±11 % PFH S Concentratio n (ng/mL ) 31. 3 31. 2 41. 8 134 106 0 VoRecover

y N A N A N C 107 10 7 31. 3 ng/m L ±0.32 % PFO S Concentratio n (ng/mL ) 11 9 11 5 12 7 20 3 107 0 VoRecover

y N A N A N C 87. 9 97. 4 11 7 ng/m L ±3.4 % N A= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2xth e spik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:10 0 dilution
. 

### Tabl e IS
. DALG W131 R 10110 3

3 M LIM S I D GLP10-01-02-11-01 7 GLP10-01-02-11-01 8 GLP10-01-02-11-01 9 GLP10-01-02-11-02 0 Descriptio n DA L GW131 R 0 10110 3 DALGW131RD B 10110 3 DA L GW131RL S 10110 3 DA L GW131RH S 10110 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 82. 9 79. 5 18 4 112 0 VoRecover

y N A N A N C 10 7 81. 2 ng/m L ±4.2 % PFH S Concentratio n (ng/mL ) 41 1 41 4 51 2 144 0 VoRecover

y N A NA N C 107 41 3 ng/m L ±0.73 % PFO S Concentratio n (ng/mL ) 149 0 153 0 161 0 270 0 VoRecover

y N A N A N C 12 2 757 0 ng/m L ±Z6 % NA= No t /Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2 xth e spik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/14/1 1 wit h a 1:10 0 dilution
.

Pag e 2 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 14
. DA L G W131L10110 S

3 M LIM S I D GLP10-01-02-11-02 6 GLP10-01-02-11-02 7 GLP10-01-02-11-02 8 GL P 10-01-02-11-02 9 GLP10-01-02-11-03 0 Descriptio n DA L GW131 L 0 10110 3 DALGW131LD B 10110 3 DA L GW131LL 8 10110 3 DA L GW131 L M S 10110 3 DALGW131LH S 10110 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 3.4 2 3.2 7 4.5 7 14. 7 10 9 VoRecover

y N A N A N C 11 7 10 9 3.3 5 ng/m L ±4.5 % PFH S Concentratio n (ng/mL ) 20. 2 21. 2 21. 6 32. 8 12 7 VoRecover

y N A N A N C N C 11 1 20. 7 ng/m L ±4.8 % PFO S Concentratio n (ng/mL ) 33. 4 35. 1 33. 7 43. 0 12 8 VoRecover

y N A N A N C N C 95. 9 34. 3 ng/m L ±5.0 % tvI A= No t Applicabl e N C = No t Calculated ; th e endogenou s sampl e concentratio n i s greate rtha n 2 xth e spik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/7/1 1 wit h a 1:1 0 dilution
. 

### Tabl e 15
. DALG WISI S 10110 3

3 M LIM S I D GLP10-01-02-11-02 1 GLP10-01-02-11-02 2 GLP10-01-02-11-02 3 GLP10-01-02-11-02 4 GL P 10-01-02-11-02 5 Descriptio n DA L GW131 S 0 10110 3 DALGW131SD B 10110 3 DALGW131SL 8 10110 3 DALGW131 8 M S 10110 3 DALG W131 8 H S 10110 3 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 0.77 2 0.79 7 1.98 12. 6 11 2 VoRecover

y N A N A 12 3 12 2 11 4 0.78 5 ng/m L ±3.2 % PFH S Concentratio n (ng/mL ) 4.7 7 4.4 8 6.0 6 16. 3 11 2 VoRecover

y N A N A N C 12 1 11 2 4.6 3 ng/m L ±6.3 % PFO S Concentratio n (ng/mL ) 5.3 9 5.7 0 5.7 3 14. 5 10 1 VoRecover

y N A N A N C 91. 6 97. 6 5.5 5 ng/m L ±5.6 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/7/1 1 wit h a 1:1 0 dilution
.

Pag e 2 6 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 /\nalysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 16
. DA L G W1S2R10110 2

3MUMSI D GLP10-01-02-11-03 1 GLP10-01-02-11-03 2 GLP10-01-02-11-03 3 GLP10-01-02-11-03 4 GLP10-01-02-11-03 5 Averag e Concen t Descriptio n

DA L GW132 R 0 10110 2 DA L GW132RD B 10110 2 DALGW132RL 8 10110 2 DA L GW132 R M S 10110 2 DA L GW132RH S 10110 2 •atio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 8.1 7 7.8 9 19. 3 11 6 106 0 VoRecover

y N A N A 11 6 11 1 10 8 8.0 3 ng/m L ±3.5 % PFH S Concentratio n (ng/mL ) 54. 3 51. 2 65. 4 16 1 113 0 %Recover

y N A N A N C 11 3 11 2 5Z 8 ng/m L ±5.9 % PFO S Concentratio n (ng/mL ) 29 7 29 2 30 6 39 7 127 0 VoRecover

y N A N A N C N C 99. 7 29 5 ng/m L ±1.7 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/14/1 1 wit h a 1:10 0 dilution
. 

### Tabl e 17
. DALGW1S2L10110 3

3MUMSI D GLP10-01-02-11-04 1 GLP10-O1-O2-11-04

2 GLP10-01-02-11-043 GLP10-01-02-11-044 GLP10-01-02-11-045 Averag e Concen t Descriptio n

DA L GW132 L 010110 3 DA L GW132LD B 10110 3 DA L GW132LL 8 10110 3 DA L GW132 L M S 10110 3 DALGW132LHS10110 3 'atio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 9.0 6 8.72 19. 5 11 4 106 0 VoRecover

y NA NA 109 108 108 8.8 9 ng/m L ±3.8 % PFH S Concentratio n (ng/mL ) 76. 7 77. 6 85. 4 177 1140 VoRecover

y NA NA N C 10 4 11 1 77. 2 ng/m L ±1.2 % PFO S Concentratio n (ng/mL ) 28 5 30 1 36 7 48 9 1400 VoRecover

y N A NA N C N C 11 3 29 3 ng/m L ±5.5 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFOS wer e analyze d o n 1/7/1 1 wit h a 1:1 0 dilution
.

Pag e 2 7 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 18
. DA L GW132 S 10110 2

3 M LIM S I D GLP10-01-02-11-03 6 GLP10-01-O2-11-037 GLP10-01-02-11-03 8 GLP10-01-02-11-03 9 GLP10-01-02-11-04 0 Averag e Concen t Descriptio n

DALG W132 8 010110 2 DAL G W132 8 D B 101102 DALG W132 8 L

S 101102 DALG W132 8 M S 101102 DA L G W132 8 H S 101102 ratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 26. 2 25. 6 37. 3 12 9 1040 VoRecover

y NA NA N C 106 104 25. 9 ng/m L ±2.3 % PFH S Concentratio n (ng/mL ) 20 3 20 6 20 9 30 0 122 0 VoRecover

y N A N A N C N C 106 20 5 ng/m L ±1.5 % PFO S Concentratio n (ng/mL ) 59 3 67 2 58 4 61 2 157 0 VoRecover

y NA N A N C N C 95. 9 63 3 ng/m L ±12 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/14/1 1 wit h a 1:10 0 dilution
. 

### Tabl e 19
. DALG W133 R 10110 2

3MUMSI D GLP10-01-02-11-04 6 GLP10-01-02-11-04 7 GLP10-01-02-11-04 8 GLP10-01-02-11-04 9 GLP10-01-02-11-05 0 Averag e Concen t Descriptio n

DA L GW133 R 010110 2 DALGW133RDB10110 2 DAL GW133RL 8 101102 DALGW133RMS10110 2 DA L GW133RH S 101102 ratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 4.7 8 4.4 3 5.35 15. 3 106 VoRecover

y N A NA N C 11 0 10 4 4.6 7 ng/m L ±7.6 % PFH S Concentratio n (ng/mL ) 32. 1 30. 1 30. 4 41. 3 132 VoRecover

y N A NA N C N C 10 5 37. 7 ng/m L ±6.4 % PFO S Concentratio n (ng/mL ) 62. 6 58. 9 60. 5 68. 5 16 1 VoRecover

y N A N A N C N C 103 60. 8 ng/m L ±6.1 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
.

Pag e 2 8 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 20
. DA L G W1 SS L 10110 S

3 M LIM S I D GLP10-01-02-11-05 6 GLP10-01-02-11-05 7 GLP10-01-02-11-05 8 GLP10-01-02-11-05 9 GLP10-01-02-11-06 0 Averag e Concen t Descriptio n

DA L GW133 L 010110 3 DA L GW133LD B 10110 3 DALGW133LL810110 3 DA L GW133 L M S 10110 3 DAL GW133LH S 10110 3 •atio n (ng/mL ) ±VoRP D PFB S Concerttratio n (ng/mL ) 77 1 7.5 8 18. 3 11 4 98 4 VoRecover

y N A NA 11 0 109 100 7.6 5 ng/m L ±1.r/ o PFH S Concentratio n (ng/mL ) 54. 0 52. 7 63. 7 154 106 0 VoRecover

y N A N A N C 10 5 10 5 53. 4 ng/m L ±2.4 % PFO S Concentratio n (ng/mL ) 20 5 20 2 19 8 28 3 121 0 VoRecover

y NA N A N C N C 103 20 4 ng/m L ±1.5 % NA=NotApplicat)l e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. 

### Tabl e 21
. DA L GW1SS S 10110 3

3 M LIM S I D GLP10-01-02-11-05 1 GLP10-01-02-11-05 2 GLP10-01-02-11-05 3 GLP10-01-02-11-054 GLP10-01-02-11-05 5 Averag e Concen t Descriptio n

DALG W133 8 010110 3 DALG W133 8 D B 10110 3 DA L GW133SL S 10110 3 DALG W133 8 M S 10110 3 DALG W133 8 H S 10110 3 ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 14 0 14. 0 25. 1 11 7 96 6 VoRecover

y NA NA 11 4 106 97. 9 14. 0 ng/m L ±0.0 % PFH S Concentratio n (ng/mL ) 92. 0 91. 0 104 192 105 0 VoRecover

y NA NA N C 10 5 99. 7 91. 5 ng/m L ±1.1 % PFO S Concentratio n (ng/mL ) 22 8 22 0 23 5 33 0 1200 VoRecover

y N A N A N C N C 99. 8 22 4 ng/m L ±3.6 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
.

Pag e 2 9 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 22
. DA L G W134 R 10110 5

3 M LIM S I D GLP10-01-02-11-06 1 GLP10-01-02-11-062 GLP10-01-02-11-06 3 GLP10-01-02-11-064 Descriptio n DA L GW134 R 010110 5 DA L GW134RD B 101105 DA L GW134RL S 101105 DALGW134RHS10110 5 Averag e Concentratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 59. 9 52. 5 162 105 0 %Recovei y

NA NA 109 10 2 56. 2 ng/m L ±73 % PFH S Concentratio n (ng/mL ) 52 6 47 9 59 0 145 0 VoRecover

y NA NA N C 98. 6 50 3 ng/m L ±9.4 % PFO S Concentratio n (ng/mL ) 1530 131 0 1430 231 0 VoRecover

y N A N A N C 91. 0 142 0 ng/m L ±15 % N A= No t Applicatsl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/14/1 1 wit h a 1:100 dilution
. 

### Tabl e 23
. DALG W1S4 L 10110 5

3 M LIM S I D GLP10-01-02-11-07 0 GLP10-01-02-11-07 1 GLP10-01-02-11-072 GLP10-01-02-11-073 GLP10-01-02-11-074 Averag e Concen t Descriptio n

DA L GW134 L 010110 5 DA L GW134LD B 101105 DALGW134LL810110 5 DALGW134LMS10110 5 DA L GW134LH S 101105 ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 11. 7 12. 1 22. 3 11 0 NA<' ' %Recover

y NA NA 107 10 1 NA<^ ' 77. 9 na/m/. ±3.4 % PFH S Concentratio n (ng/mL ) 11 2 11 2 12 0 20 3 NA<^ ' %Recover

y N A NA N C 94. 7 NA'^ > 772 ng/m L ±0.0 % PFO S Concentratio n (ng/mL ) 57 1 58 6 61 7 64 6 1640 VoRecover

y N A N A N C N C 10 9 57 9 ng/m L ±2.6 % NA= No t Applicatil e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level
. PFB S an d PFH S wer

e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. PFO S wa s analyze d o n 1/14/1 1 wit h a 1:5 0 dilution
. (1 ) Adilutio n o

fth e sampl e wa s no

t prepare d as tti e spike leve l was no t appropriate a

s compare d t o th e sampl e concentrations
.

Pag e 3 0 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 24
. DALG W134 S 10110 5

3 M LIM S I D GLP10-01-02-11-06 5 GLP10^1-02-11-06 6 GLP10-01-02-11-06 7 GLP10-01-02-11-06 8 GLP10-01-02-11-06 9 Averag e Concen t Descriptio n

DALG W134 8 010110 5 DALGW134SDB10110 5 DALG W134 8 LS 101105 DALG W134 8 M S 101105 DALG W134 8 H S 101105 ratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 0.14 6 0.14 0 1.27 11. 6 102 VoRecover

y NA NA 11 6 11 8 10 5 0.14 3 ng/m L ±4.r/ o PFH S Concentratio n (ng/mL ) 1.7 6 1.6 5 3.0 0 13. 2 104 VoRecover

y NA NA 135'^ ' 12 0 106 7.7 7 ng/m L ±6.5%' ^ PFO S Concentratio n (ng/mL ) 11. 3 11. 5 10. 2 22. 4 11 9 VoRecover

y N A N A N C 11 2 11 0 77. 4 ng/m L ±1.8

% NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/7/1 1 wit h a 1: 5 dilution
. (1 ) Th e fiekJ matri xspik e di d no t meet metho d acceptance criteri a of10 0 ±30%
. (2 ) Th e analytica l uncertaint yhas bee n adjuste d t o ±35%
. 

### Tabl e 25
. DALG W135 R 10110 5

3 M LIM S I D GLP10-01-02-11-075 GLP10-01-02-11-07 6 GLP10-01-02-11-07 7 GLP10-01-02-11-07 8 Descriptio n DA L GW135 R 010110 5 DA L GW135RD B 101105 DA L GW135RL S 101105 DA L GW135RH 8 101105 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concerttratio n (ng/mL ) 82. 1 79. 9 195 1150 VoRecover

y NA NA 11 7 11 0 81. 0 ng/m L ±2.7 % PFH S Concentratio n (ng/mL ) 84 7 83 1 91 4 1900 VoRecover

y NA NA N C 11 0 83 9 ng/m L ±1.9 % PFO S Concentratio n (ng/mL ) 90 3 88 0 95 5 1890 VoRecover

y NA NA N C 10 2 89 2 ng/m L ±2.6 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentrato n greate rtha n 2xspike level
. PFBS , PFHS , an d PFO S wer e analyze d o n 1/14/1 1 wit h a 1:100 dilution
.

Pag e 3 1 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Table26
. DALG W1S5 L 10110 5

3 M LIM S I D GLP10-01-02-11-08 4 GLP10-01-02-11-08 5 GLP10-01-02-11-08 6 GLP10-01-02-11-08 7 GLP10-01-02-11-08 8 Averag e Concen t Descriptio n

DA L GW135 L 010110 5 DA L GW135LD B 101105 DALGW135LL 8 101105 DALGW135LM810110 5 DALGW135LH S 101105 ratfo n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 5.8 4 5.62 16. 5 12 0 1060 VoRecover

y NA N A 11 1 11 8 108 5.7 3 ng/m L ±3.8 % PFH S Concentratio n (ng/mL ) 35. 4 36. 3 48. 0 15 0 1090 VoRecover

y NA N A N C 11 9 11 0 35. 9 ng/m L ±2.5 % PFO S Concentratio n (ng/mL ) 23. 9 21. 3 39. 8 13 4 103 0 VoRecover

y N A N A N C 11 4 10 3 22.6nfi/mL±72 % NA=NotApplicat)l e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspike level
. PFB S an d PFH S wer

e analyze d o n 1/14/1 1 wit h a 1:10 0 dilution
. PFO S wa s analyze d o n 2/11/1 1 wit h a 1:1 0 dilution
.

Pag e 3 2 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 27
. DA L GW135 S 10110 5

3 M LIM S I D GLP10-01-02-11-07 9 GLP10-01-02-11-08 0 GLP10-01-02-11-08 1 GLP10-01-02-11-082 GLP10-01-02-11-08 3 Descriptio n DALG W135 8 010110 5 DALGW135SDB10110 5 DALGW1358L S 101105 DALG W135 8 M S 101105 DALGW135SH S 101105 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 0.79 4 0.80 3 1.9 4 11. 4 NA<^ ' VoRecover

y N A N A 11 7 10 9 NA'^ ' 0.79 9 ng/m L ±1.1 % PFH S Concentratio n (ng/mL ) 6.3 5 6.1 5 7.2 6 16. 8 NA TM VoRecover

y NA NA 10 5 11 0 NA TM 6.2 5 ng/m L ±3.r/ o PFO S Concentratio n (ng/mL ) 5.0 1 47 5 5.5 9 14 8 NA TM VoRecover

y N A N A N C 10 1 NA TM 4.8 8 ng/m L ±5.3 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/7/1 1 withou t dilution
. (1 ) Adilutio n ofth e sampl e was no t prepare d as th e spik

e leve l was no

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

### Tabl e 28
. DA L G W136 L 10110 S

3 M LIM S I D GLP10-01-02-11-09 4 GLP10-01-02-11-09 5 GLP10-01-02-11-09 6 GLP10-01-02-11-09 7 GLP10-01-02-11-09 8 Descriptio n DA L GW136 L 010110 3 DA L GW136LD B 101103 DA L GW136LL 8 101103 DALGW136LMS10110 3 DALGW136LH S 101103 Averag e Concerttratio n (ng/mL ) ±%RP D PFB S Concentratio n (n^mL ) 2.4 3 2.6 3 13. 5 103 97 6 VoRecover

y NA NA 11 3 10 3 100 2.5 3 ng/m L ±7.9 % PFH S Concentratio n (ng/mL ) 15. 5 16. 8 27. 2 11 7 102 0 VoRecover

y NA NA 11 5 10 5 10 4 16. 2 ng/m L ±8.0 % PFO S Concentratio n (ng/mL ) 75. 7 82. 7 91. 9 17 1 111 0 VoRecover

y N A N A N C 93. 9 105 79. 2 ng/m L ±8.8 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/10/1 1 with a 1:10dilution
.

Pag e 3 3 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 29
. DA L G W1S6 S 10110 3

3 M LIM S I D GLP10-01-02-11-08 9 GLP10-01-02-11-09 0 GLP10-01-02-11-09 1 GLP10-01-02-11-09 2 GLP10-01-02-11-09 3 Averag e Concen t Descriptio n

DALG W136 8 010110 3 DA L G W136 8 D B 10110 3 DALGW1368L S 10110 3 DALG W136 8 M S 101103 DALGW136SHS10110 3 ratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 2.5 2 2.5 7 3.6 6 13. 5 10 1 VoRecover

y N A N A N C 11 3 10 1 2.5 5 ng/m L ±2.0 % PFH S Concentratio n (ng/mL ) 16. 0 16. 9 17 7 27. 1 11 4 VoRecover

y N A N A N C 11 1 10 2 16. 5 ng/m L ±5.5 % PFO S Concentratio n (ng/mL ) 85. 5 88. 7 87. 2 94. 6 18 0 VoRecover

y N A N A N C N C 95. 0 87. 1 ng/m L ±3.7 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. 

### Tabl e 30
. DA L GW137 L 10110 9

3 M LIM S I D GLP10-01-02-11-104 GLP10-01-02-11-10 5 GLP10-01-02-11-10 6 GLP10-01-02-11-10 7 GLP10-01-02-11-10 8 Descriptio n DA L GW137 L 010110 9 DALGW137LDB10110 9 DA L GW137LL 8 10110 9 DA L GW137 L M S 10110 9 DALGW137LH 8 10110 9 Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 0.081 2 0.0833 0.19 0 1.2 2 10. 7 VoRecover

y N A N A 11 1 11 7 10 9 0.082 3 ng/m L ±2.6 % PFH S Concentratio n (ng/mL ) 0.11 7 0.12 1 0.24 0 1.2 5 10. 8 VoRecover

y N A NA 126 11 8 11 1 0.19 9 ng/m L ±3.4 % PFO S Concentratio n (ng/mL ) 0.87 7 0.90 9 0.94 8 1.7 9 10. 0 VoRecover

y N A N A N C 91. 7 93. 1 0.89 3 ng/m L ±3.6 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/7/1 1 withou t dilution
.

Pag e 3 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Table31
. DALG W1S7 S 10110 9

3 M LIM S I D GLP10-01-02-11-09 9 GLP10-01-02-11-10 0 GLP10-01-02-11-10 1 GLP10-01-02-11-102 GLP10-01-02-11-10 3 Descriptio n DA L GW137 S 010110 9 DALGW137SD B 10110 9 DALG W137 8 LS 10110 9 DALG W137 8 M S 10110 9 DALG W137 8 H S 10110 9 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 0.099 0 0.10 4 0.20 6 1.2 1 10. 6 VoRecover

y N A NA 108 11 4 108 0.10 2 ng/m L ±4.9 % PFH S Concentratio n (ng/mL ) 0.088 6 0.0942 0.20 1 1.1 5 10. 4 VoRecover

y NA NA 11 4 11 0 107 0.0974 ng/mL ±6.7 % PFOSf ^ Concentratio n (ng/mL ) 0.36 7 0.263 0.32 8 0.89 0 6.1 2 VoRecover

y N A N A N C 58.8 TM 59.4 TM 0.31 5 ng/m L ±33%'^^ ' NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/7/1 1 withou t dilution
. (1 ) Th e fiel d matri xspik e di d no t mee t metho d acceptance criteri a of10 0 ±30%
. (2 ) Th e analytica l uncertaint yfo rPFO S has bee n adjuste d fo rFM S recover yt o ±4 1 %
. (3) Th e RP D di d no

t mee t metho d acceptanc

e criteri a o fS20%
.

Pag e 3 5 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Table32
. DALG W138 S 10111 0

3 M LIM S I D GLP10-01-02-11-10 9 GLP10-01-02-11-11 0 GLP10-01-02-11-11 1 GLP10-01-O2-11-11 2 GLP10-01-02-11-11 3 Averag e Concen t Descriptio n

DALG W138 8 010111 0 DA L G W138 8 D B 10111 0 DA L G W138 8 LS 10111 0 DALG W138 8 M S 10111 0 DA L G W138 8 H S 10111 0 ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 4.7 4 4.6 3 16. 2 99. 8 94 9 VoRecover

y NA NA 11 8 97. 9 97. 2 4.6 9 ng/m L ±2.3 % PFH S Concentratio n (ng/mL ) 24. 0 22. 9 35. 4 11 9 99 1 VoRecover

y N A N A N C 99. 4 10 1 23. 5 ng/m L ±4.r/ o PFO S Concentratio n (ng/mL ) 25 2 23 8 25 6 30 7 121 0 VoRecover

y N A N A N C N C 98. 7 24 5 ng/m L ±5.7 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:5 0 dilution
. 

### Table33
. DALG W138 L 10111 0

3 M LIM S I D GLP10-01-02-11-11 4 GLP10-01-02-11-11 5 GLP10-01-02-11-11 6 GLP10-01-02-11-11 7 GLP10-01-02-11-11 8 Averag e Concen t Descriptio n

DA L GW138 L 010111 0 DA L GW138LD B 10111 0 DALGW138LL S 10111 0 DA L GW138 L M S 10111 0 DALGW138LH 8 10111 0 ratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 0.046 0 0.048 5 0.15 7 1.1 6 10. 8 VoRecover

y NA NA 11 3 11 4 11 1 0.047 3 ng/m L ±5.3 % PFH S Concentratio n (ng/mL ) 0.143 0.144 0.25 9 1.28 10. 9 VoRecover

y NA NA 12 0 11 8 11 2 0.144 ng/mL ±0.70 % PFO S Concerttratio n (ng/mL ) 0.58 1 0.58 0 0.684 1.29 8.42 VoRecover

y N A N A N C 72. 5 80. 2 0.58 1 ng/m L ±0.17% NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S were analyze d o n 1/7/1 1 withou t dilution
.

Pag e 3 6 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e S3
. DA L G WCW26 R 10111 0

3 M LIM S I D GLP10-01-02-11-11 9 GLP10-01-02-11-12 0 GLP10-01-02-11-12 1 GLP10-01-02-11-12 2 GLP10-01-02-11-12 3 Descriptio n

DA L GWCW26R 0 10111 0 DA L GWCW26RD B 10111 0 DA L G WCW26 R L

S 10111 0 DA L GWCW26 R M S 10111 0 DA L GWCW26RH 8 10111 0 Averag e Concentratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 8.1 4 8.4 0 19. 2 105 NA TM VoRecover

y NA NA 11 2 100 NA TM 8.2 7 ng/m L ±3.1 % PFH S Concentratio n (ng/mL ) 61. 7 64. 4 73. 9 155 NA TM VoRecover

y NA NA N C 95. 7 NA TM 63. 7 ng/mL ±4.3 % PFO S Concentratio n (ng/mL ) 45 5 44 6 43 9 52 6 1470 VoRecover

y N A N A N C N C 104 45 1 ng/m L ±2.0 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFB S an d PFH S wer

e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. PFO S were analyze d o n 1/14/1 1 wit h a 1:5 0 dilution
. (1 ) Adilutio n o fth e sampl e wa s no t prepare d a

s tfi e spik e leve l was no

t appropriate as compare d t o th e sampl e concentration
. 

### Tabl e 34
. DA L G WCW26 L 10111 0

3 M LIM S I D GLP10-01-02-11-12 4 GLP10-01-02-11-12 5 GLP10-01-02-11-12 6 GLP10-01-02-11-12 7 GLP10-01-02-11-12 8 Descriptio n

DA L GWCW26 L 010111 0 DALGWCW26LD B 10111 0 DA L GWCW26LL 8 10111 0 DA L G WCW26 L M S 10111 0 DA L GWCW26LH S 10111 0 Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 13. 2 12. 5 23. 3 107 NA TM VoRecover

y NA NA 10 8 96. 9 NA TM 12. 9 ng/m L ±5.4 % PFH S Concentratio n (ng/mL ) 95. 6 90. 2 10 2 183 NA TM VoRecover

y NA N A N C 93. 8 NA TM 92. 9 ng/mL ±5.8 % PFO S Concerttratio n (ng/mL ) 88 8 80 8 89 6 85 5 1840 VoRecover

y N A N A N C N C 10 1 84 8 ng/m L ±9ji % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level
. PFB S an d PFH S wer

e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. PFO S were analyze d o n 1/14/1 1 wit h a 1:5 0 dilution
. (1 ) Adilutio n o fth e sampl e wa s no t prepare d a

s th e spik e leve l was not appropriate as compare d t o tti e sampl e concentration
.

Pag e 3 7 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Ajrea - Novembe r201 0



### Tabl e 35
. DA L G W140R10110 4

3 M LIM S I D GLP10-01-02-11-12 9 GLP10-01-02-11-13 0 GLP10-01-02-11-13 1 GLP10-01-02-11-132 GLP10-01-02-11-13 3 Descriptio n

DA L GW140 R 010110 4 DALGW140RD B 101104 DALGW140RLS10110 4 DALGW140RMS10110 4 DA L GW140RH S 101104 Averag e Concentratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 1.6 5 1.6 1 11. 9 96. 4 NA TM VoRecover

y NA NA 106 97. 5 NA TM 1.6 3 ng/m L ±2.5 % PFH S

Concentratio n (ng/mL ) 17. 2 17. 2 27. 2 11 5 NA TM VoRecover

y NA NA 10 4 10 2 NA TM 17. 2 ng/mL ±0.0 % PFO S Concentratio n (ng/mL ) 140 13 1 139 22 9 NA TM VoRecover

y NA NA N C 95. 6 NA TM 13 6 ng/m L ±6.6 % N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level
. (1 ) Adilutio n o fth e sampl e was no t prepare d a

s th e spike leve l wa

s no t appropriate as compare d t o th e sampl e concentration
. 

### Tabl e 36
. DA L G W141 R 10111 0

3 M LIM S I D GLP10-01-02-11-134 GLP10-01-02-11-13 5 GLP10-01-02-11-13 6 GLP10-01-02-11-13 7 GLP10-01-02-11-13 8 Descriptio n DA L GW141R 0 10111 0 DA L GW141RD B 10111 0 DALG W14 1 RL S 10111 0 DA L GW141 R M S 10111 0 DA L GW141RH S 10111 0 Averag e Concentratio n (ng/mL ) ±VoRPD PFB S Concentratio n (ng/mL ) 0.044 4 0.041 8 10. 1 96. 7 97 7 VoRecover

y N A N A 10 3 99. 4 10 1 0.043 1 ng/m L ±6.0 % PFH S Concentratio n (ng/mL ) 0.273 0.243 10. 4 96. 2 NA TM VoRecover

y NA NA 10 6 99. 8 NA TM 0.25 8 ng»nL ±72 % PFO S Concentratio n (ng/ml ^ 4.4 8 3.9 7 11. 4 81. 2 NA TM VoRecover

y N A N A 73. 4 78. 7 NA TM 4.2 3 ng/m L ±ir/ o N A= No t Applicabl e PFH S an d PFO S wer

e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. PFB S wa s analyze d o n 2/11/11
. Th e sample , sampl e duplicat e an d L S were analyze d withou t a dilution , th e M S wit h a 1:1 0 dilution , an d th e H S wit h a 1:5 0 dilution
. (1 ) Adilutio n o fth e sampl e wa s not prepare d a s th e spike leve l was not appropriate a s compare d t o th e sampl e concentrations
.

Pag e 3 8 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 37
. DA L G W142 R 10111 0

3 M LIM S I D GLP10-01-02-11-13 9 GLP10-01-02-11-14 0 GLP10-01-02-11-14 1 GLP10-01-02-11-142 GLP10-01-02-11-14 3 Descriptio n DA L GW142 R 010111 0 DA L GW142RD B 10111 0 DA L GW142RL 8 10111 0 DA L GW142 R M S 10111 0 DA L GW142RH S 10111 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 1.6 9 1.6 7 11. 9 98. 0 NA TM VoRecover

y NA NA 10 5 99. 1 NA TM 7.6 8 ng'mL ±7.2 % PFH S Concentratio n (ng/mL ) 10. 0 9.9 6 19. 8 108 NA TM VoRecover

y NA NA 10 2 10 2 NA TM 9.9 8 ng/m L ±0.40 % PFO S Concentratio n (ng/mL ) 11 1 10 4 11 8 20 0 NA TM VoRecover

y NA NA N C 94. 6 NA TM 10 8 ng/m L ±6.5 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. (1 ) Adilutio n o fth e sampl e wa s not prepare d as tti e spik e leve l was no

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

### Tabl e 38
. DA L G W144 R 10111 0

3 M LIM S I D GLP10-01-02-11-144 GLP10-01-02-11-145 GLP10-01-02-11-14 6 GLP10-01-02-11-14 7 GLP10-01-02-11-14 8 Descriptio n DA L GW144 R 010111 0 DA L GW144RD B 10111 0 DALGW144RL S 10111 0 DA L GW144 R M S 10111 0 DALGW144RH 8 10111 0 Averag e Concentratio n (ng/mL ) ±VoRP D PFB S Concentratio n (ng/mL ) 1.9 8 1.9 1 11. 6 98. 5 NA TM VoRecover

y NA NA 99. 3 99. 3 NA TM 1.95 ng/m L ±3.6 % PFH S Concentratio n (ng/mL ) 8.7 9 8.35 17. 9 103 NA TM VoRecover

y NA NA 97. 1 98. 3 NA TM 8.5 7 ng/m L ±5.1 % PFO S Concentratio n (ng/mL ) VoRecover y

No t Reporte d

No t Reported' ^ NA= Not Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level
. PFBS , PFH S an d PFO S wer e analyze d o n 1/10/1 1 wit h a 1:1 0 dilution
. (1 ) Adilutio n o fth e sampl e was not prepare d as th e spik e leve l was not appropriate as compare d t o th e sampl e concentrations
. (2 ) No t Reported ; Th e matrixspik e sample s prepare d an d analyze d fo rthi s samplin g locatio n fo rPFO S had recoverie s <50%
.

Pag e 3 9 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 39
. Tri p Blan k

3 M LIM S I D GLP10-01-02-11-15 0 GLP10-01-02-11-15 1 GLP10-01-O2-11-152 GLP10-01-02-11-15 3 GLP10-01-02-11-15 4 Descriptio n TRI P BLAN K1 0 TRI P BLAN K1 LS TRI P BLAN K1 M S TRI P BLAN K1 MH S TRI P BLAN K1 H S PFB S Concentratio n (ng/mL ) <0.025 0 1.1 2 10. 6 98. 6 105 0 VoRecover

y NA 11 5 109 10 1 108 PFH S

Concentratio n (ng/mL ) <0.025 0 1.1 0 10. 5 10 1 105 0 VoRecover

y NA 11 4 109 10 5 109 PFO S

Concentratio n (ng/mL ) <0.25 0 1.0 4 10. 3 104 93 0 VoRecover

y N A 10 6 10 5 10 6 95. 1 NA= No t /Applicabl e 

### Tabl e 40
. Tri p Blan k

2

3 M LIM S I D GLP10-01-02-11-15 5 GLP10-01-02-11-15 6 GLP10^1-02-11-15 7 GLP10-01-02-11-15 8 GLP10-01-02-11-15 9 Descriptio n TRI P BLAN K2 0 TRI P BLAN K2 LS TRI P BLAN K2 M S TRI P BLAN K2 MH S TRI P BLAN K2 H S PFB S Concentratio n (ng/mL ) <0.025 0 1.1 2 10. 8 97. 1 1040 VoRecover

y N A 11 5 11 1 100 10 7 PFH S Concentratio n (ng/mL ) <0.025 0 1.0 9 10. 8 99. 3 1040 VoRecover

y NA 11 3 11 2 103 108 PFO S

Concentratio n (ng/mL ) <0.25 0 1.0 1 10. 7 10 5 95 2 VoRecover

y N A 103 10 9 107 97. 3 NA= No t Applicat)l e

Pag e 4 0 o f104GLP10-01-02 ; Interi m Repor t 1 1 /Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 41
. Tri p Blan k

3

3 M LIM S I D GLP10-01-02-11-16 0 GLP10-01-02-11-16 1 GLP10-01-02-11-162 GLP10-01-02-11-16 3 GLP10-01-02-11-164 Descriptio n TRI P BLAN K3 0 TRI P BLAN K3 LS TRI P BLAN K3 M S TRIPBU\NK3MH S TRI P BLAN K3 H S PFB S Concentratio n (ng/mL ) <0.025 0 1.1 1 10. 3 99. 2 1030 VoRecover

y NA 11 4 106 10 2 106 PFH S

Concentratio n (ng/mL ) <0.025 0 1.0 8 10. 4 10 1 1040 VoRecover

y NA 11 2 10 8 10 5 108 PFO S

Concentratio n (ng/mL ) <0.25 0 1.0 3 9.9 6 10 5 92 5 VoRecover

y N A 105 102 107 94. 6 N A= No t Applicabl e 

### Tabl e 42
. Tri p Blan k

4

3 M LIM S I D GLP10-01-02-11-16 5 GLP10-01-02-11-16 6 GLP10-01-02-11-16 7 GLP10-01-02-11-16 8 GLP10-01-02-11-16 9 Descriptio n TRI P BLAN K4 0 TRI P BLAN K4 LS TRI P BLAN K4 M S TRI P BLAN K4 MH S TRIPBL^NK4H 8 PFB S Concentratio n (ng/mL ) <0.025 0 1.1 0 10. 7 99. 5 102 0 %Recover

y N A 11 3 11 0 10 2 10 5 PFH S Concentratio n (ng/mL ) <0.025 0 1.0 9 10. 6 10 1 102 0 %Recover

y N A 11 3 11 0 10 5 106 PFO S

Concentratio n (ng/mL ) <0.25 0 0.98 3 10. 2 103 90 9 VoRecover

y N A 10 1 104 105 92. 9 NA= No t Applicabl e

Pag e 4 1 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Tabl e 43
. Rinseat e Blank s

3 M LIM S I D GLP10-01-02-11-01 6 GLP10-01-02-11-14 9 Descriptio n DA L GW130LR B 101105 DA L GW144RR B 10111 0 PFB S Concentratio n (ng/mL ) <0.025 0 <0.025 0 VoRecover y NA NA PFH S

Concentratio n (ng/mL ) <0.025 0 <0.025 0 VoRecover y NA NA PFO S

Concentratio n (ng/mL ) <0.25 0 <0.25 0 VoRecover y N A N A NA = Not/Applicabl e 

### Tabl e 44
. GLP10-01-02-1 2 Soi l Equipmen t Rinseat e Blan k

3 M LIM S I D GLP10-01-02-12-00 9 Descriptio n DA L S S 607 R R B 004 0 PFB S Concentratio n (ng/mL ) <0.025 0 VoRecover y NA PFH S

Concentratio n (ng/mL ) <0.025 0 VoRecover y N A PFO S Concerttratio n (ng/mL ) <0.25 0 VoRecover y N A NA= No t /Applicabl e

Pag e 4 2 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



## 1 0 Conclusion;
. ••• . Laborator ycontro l spike s an d fiel d matri xspilces were use d t o determin e th e analytic^al metlio d acxurac yan d precisio n fo rPFBS , PFHS , an d PFOS
. Analysi s wa s successfull ycomplete d followin g 3I\/I 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 SM Environmenta l Laborator ystandar d operatin g procedures
. 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 1 1 (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 4 3 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



## 1 3 Signature s 

# ^/io/2ai ) Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date 

# /^A^ y^/ / Willia m K
. Reagen , Ph.D. , 3 M Environmenta l Laborator yDepartmen t Manage rDate 

# ra 9 : If Gar yHohenstain , Sponso rRepresentative 

# Olhd , Date

' Date Jaisimh a Kesari , Stud yDirecto r

Pag e 4 4 o f104GLP10-01-02 ; interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### ATTACHMEN TA : PROTOCO L AMENDMEN T

Pag e 4 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e incorporatio n Are a - Novembe r201 0



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

Amendmen t 1 1



## Stud yTitl e Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) I n Groundwater , 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 1

Amendmen t Date : Octobe r20 , 201 0 Performin g Laborator y 3 M Environmental , Health , an d SafetyOperation s

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

Laborator yProjec t Identificatio n

GLP10-01-0 2
Samplin g Even t Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r

Pag e 1 o f7 Pag e 4 6 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S I n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

### Analytica i Protocol : GLP10-01-0 2

Amendmen t 1 1 

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

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

PROTOCO L READS : 

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

AMEN D TO READ : 

### N o change s t o th e wordin g o fth e protoco l ar e required
. Thi s amendmen t onl yaddresse s an d document s th e additio n ofth e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s fro m Decatur , AL , an d conducte d a s par t ofth e 3 M Decatu rPhas e 3 Progra m fo rPFOS , PFH S an d PFB S (GLP10-01-02)
. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e ofOctobe r25 , 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 y LIM S a s project GLP10-01-02-1 1 an d reporte d a s interi m repor t GLP10-01-02-11 , (reflectin g stud y GLP10-01-0 2 an d amendment-11)
.

Reason : 

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

Pag e 2 of7 Pag e 4 7 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

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

Amendmen t 1 1 

## Amendmen t Approva l

/ 

# ^ % ljW%m^

k i O L , 

# i d Gar yHohenstein , Sponso rRepresentative Date

I D6te Clesto n C
. Lange , Principa l Analytica i Investigato r 

# o / cjcr'^o/ o Willia m Reagec

d EH S Opn s Environmenta l La b Managemen t Date

Jaisimh a Kesar i P.E. , DEE , Stud yDirecto r

Pag e 3 o f7 Pag e 4 8 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

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

Amendmen t 1 1
Environmenta l Healt h & Safet yOperations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gar

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

Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charle s Young , Westo n Solution s Ti m Frinak , Westo n Solution s Date : Octobe r20,201 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 1 1 - Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r 

## 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r Projec t Schedule/Tes t Date s 3 M Sponso rRepresentativ e Gar 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 aahohenstein(a)mmm.co m 3 M Environmenta l Laborator yManagemen t Willia m K
. Reage n SIV I EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wkreaqenOmmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanqeOmmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinakOwestonsolutions.co m Phone : (334)-332-912 3 GLP10-01-02-1 1 Dep t #530711 , Project #002267444 9 Samplin g schedule d fo rth e wee k ofOctobe r25 , 201 0 

### Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein
. Pag e 4 of7 Pag e 4 9 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

Amendmen t 1 1 

## 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m twenty-seve n groundwate rwell s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfonat e (PFOS ) fro m th e Forme rSludg e Incorporatio n Are a (FSIA)
. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792
. Groundwate rsample s fro m Decatur , A L wil l b e collecte d byWesto n Solution s personne l th e wee k o f Octobe r25 , 2010
. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFBS , PFHS , an d PFO S ar e ofa know n precisio n an d accuracy . Th e fina l report wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10 - 01-02-11
. 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b y3 M Environmenta l Laborator yfo rsamplin g th e wee k

o fJun e 21 , 2010
. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l o n Friday , Jun e 18,2010
. 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 ofthirty-fou rsamplin g location s hav e bee n specified
. Fo reac h samplin g location , a sample , sampl e duplicat e an d a minimu m oftwo fiel d matri xspike s wil l b e collected
. Tabl e 1 indicate s th e wel l I D an d con-espondin g fiel d spike levels
. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL
. Fou rsets o ftri p blank

s consistin g o freagent-grad e water , a low-leve l tri p blan k spike , mid-leve l field spike , mid-hig h fiel d spike , an d a high-leve l tri p blan k spik e wil l b e prepare d a

t th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles
. Tw o additiona l bottle s wil l b e prepare d t o b e use d fo rth e preparatio n o fth e equipmen t rinseat e blanks
. Atota l of18 9 sampl e bottle s wil l b e prepared
.

Pag e 5 o f7 Pag e 5 0 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

Amendmen t 1 1 Tabl e 1
. Samplin g Location s an d Fiel d Matri xSpik e levels
.

Wel l No
.
136R , 137R,137S,137L , 138 L 130L , 131L , 131S , 133R , 134S , 1358,136 8 130R,130S,132R , 132L , 132S , 133S , 133L , 134L , 135L , 136L , 138S , 138R , CW26R , CW26L , 140R , 141R , 142R , 143 , an d 144 R 131R , 134R , 135 R Tri p Blan k

Se t 1,2 , 3 , an d 4 Sampl e Leve l Low Mi d Hig h Low Mi d Hig h Low Mi d Hig h Low Hig h Low Mi d Mid-Hig h 

### Hig h Spik e Cone
. (ng/mL ) 0. 1 1. 0 1 0 1 1 0 10 0 1 0 10 0 100 0 10 0 100 0 1 1 0 10 0 100 0


### 5 Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S follov\fln g ETS-8-044. 0 "Detenninatio n ofPerfiuorinate d Compound s I n Wate rb

yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"
. Th e dat a qualit yobjective s fo rthes e studie s ar e quantitative result s fo rth 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 withi n 100±30 % wil l b e addresse d i n th e repor

t an d th e fina l accurac

ystatemen t ma

yb e adjuste d accordingly
. Base d o n th e results fro m previousl ycollecte d sample s fro m th e FSI A(GLP10-01-02-07) , most samplin g location s wil l require dilutio n wit h laborator yreagen t wate rprio rt o sampl e analysi s b yETS-8-044.0
. Altemately , sample s ma

yb e analyze d b

yETS 8-154. 3 "Determinatio n ofPerfiuorinate 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"
. 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e results fo rth e sample , sampl e duplicate , an d fiel d matri x spikes
. Tri p blan k

an d tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an yequipment/rinseat e blank s prepare d i n th e field. Laborator ycontro l spike s ofreagen t wate rprepare d at th e tim e o fsampl e preparatio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d precision
. Metho d blank s ofreagen t wate rprepare d at th e tim e ofsampl e preparatio n wil l b e use d t o determin e th e metho d detectio n limit
. Fo rthos e samplin g location s where ttie fiel d matri xspike leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspik

e ma yb e prepare d an d wil l b e include d i n th e final report
. 7 Emai l Correspondenc e Attachmen t A : Samplin g Bottl e Request

Pag e 6 o f7 Pag e 5 1 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

Amendmen t 1 1
Attachmen t A 

# Bottl e Reques t Decatu r Groundwate r

Samplin g On-sit e FSI AWell s 02181.129.145.000 4 DAT EREQUESTED : 1 8 Octobe r 201 0 DAT EREQUIRED : 2 5 Octobe r 201 0 Thi s reques t

addresse s th e bottl e requirement s for th e followin g wells : 130R 130 S 130L 131 R 131 S 131 L 132 R 132 S 132L

133 R 133 S 133 L 134R 134 S 134L 135 R 135 S

135 L 136 R 136 S 136L 137 R 137 S 137 L 138 R

138 S 138 L CW26 R CW26 L NO R 141 R 142 R 143 R

144R

Tota l Wells : 3 4 Sampl e Summar y No
. of Sample s 3 4 2 4 Sampl e Typ e

Groundwater Rinseate Sampl e Tri p Blank s Commen t Will nee dHPL C water Anticipate 1 per

cooler Note : Som

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

# SHIPPIN GINFORMATIO N Pleas e ship to the followin g address : Marti nSmith\Westo nFiel dOffic e 3 M Decatu r

Plan t 1400 Stat e Dock s Roa d Decatur , A L3560 1 256-552-618 9

Pag e 7 o f7 Pag e 5 2 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0


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

Pag e 5 3 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bll0107a.da b


## •

m c 8 C O 

### < b110107a.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weigliting) : y= -7.8e+00 3 x' 2 + 1.03e+00 6 x+ 5.1e+00 3 ( r= 0.9997 ) 4.8e7 - 4.6e7 - 4.4e7 - 4.2e7 - 4.0e7 - 3.8e7 - 3.6e7 - 3.4e7 - 3.2e7 - 3.0e7 - 2.8e7 - 2.6e 7 2.4e7 - 2.2e 7 2.0e7 - 1.8e7 - 1.6e7 - 1.4e7 - 1.2e7 - 1.0e7 - 8.0e 6 6.0e6 - 4.0e6 - 2.0e6 - 0.0 ^ 

### / ' '


### / 

# A / /

/ / / / / / / • / / / 0 5 1 0 1 5 2 0 2 5 3 0 3 5 4 0 

### ^.. ^ 

### ' " "

4 5 5 0 5 5 6 0 6 5 Concentration , ng/m L 

### -.- .

7 0 O



### —-__ _

7 5 8 0 "•''•--, „

8 5 ^^•^ ^

9 0 9 5 

### ^

X

10 0 Printin g Time : 3:12:0 3 P M Printin g Date : Tuesday , Februar y01 , 201 1 Pag e 1 o f 1

Pag e 5 4 o f 10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bll0107a.da b
b110107a.rd b (PFHS) : "Quadratic " Regressio n {" 1 / x " weighting) : y= -7.09e+00 3 x" 2 + 9.06e+00 5 x+ 4.64e+00 3 ( r= 0.9997 )
4.16 / 4.0e 7 - 3.8e7 - 3.6e7 - 3.4e7 - 3.2e7 - 3.0e 7 - 2.8e7 - 2.6e7 - 2.4e7 - 2.2e7 - 2.0e7 - 1.8e7 - 1.6e7 - 1.4e7 - 1.2e 7 1.0e7 - 8.0e6 - 6.0e6 - 4.0e 6 - 2.0e6 - 0.0 - 

### P / / / / 

### / / / / / , / X '

y 

### / ,--'' ' ^^••"' ^ 

### ^ '^ ' O



### -—.,^,
.

""•"--- ^ 

### \
_ ^^-.

^ v_ /



### ' ^

-v .

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 85 9 0 9 5 100 Printin g Time : 3:12:2 5 ? K Printin g Date : Tuesday , Februar y01 , 201 1 Pag e 1 o f 1
Pag e 5 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bll01073.da b
b110107a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -6.1e+00 3 x'' 2 + 8.64e+00 5 x+ 2.98e+00 4 ( r= 0.9999 ) 4.2e 7 4.0e 7 3.8e 7 3.6e 7 3.4e 7 3.2e7

- 3.0e 7 2.8e 7 2.6e 7 2.4e 7 2.2e 7 2.0e 7 1.8e 7 1.6e 7 1.4e 7 1.2e 7 1.0e7

- 8.0e6

- 6.0e6

- 4.0e6

- 2.0e 6 0. 0 

### / O



### /

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 Prin t in qTim e : 3 : 1. ? : 5 1 ? K Printin g Date : Tuesday , Februar y01 , 201 1 Pag e 1 o f 1
Pag e 5 6 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS
. PFHS
. an d PFO S i n Groundwate r Fonne rSludg e Incorporatio n Are a - Novembe r201 0 Bliste r J293C20 3 

# I Sampto Name : -i)11O1O7a0l6 ' Sampl B ID rtlB00«-194^ * Pvn k Name : "PFBS - Messfas} : •299.0/99. 0 aTM.299J3('80. 0 a CofimBnl ; '1. 0 nglni
. F C »I d i t M S Q Watai ' Aniotalion ' -

2.4e 5 2AB S 2JB 5 2J« S Z2e S 2.2e S 2.ie S 2.1« 5 2J0t& - 2.0e S 1.9eS 1.9»S 1.8«5 - 1.8»i5- 1.roS 1.7oS 1.6«S 1. &

1.4e S 1.46 S 1.34 S 1-3e S 1^« S 1.2e S 1.1«S I.Io S 1.0«5 9.5e 4 ^.O M a.te 4 8-0e 4 7.Se 4

&.S M 5.0 M 4.SM ' 4.0e 4 3.5* 1 • 3.0e4 2.& M 2.ae4 ' 1.5 ^ 1.0e4 - 500 0 J > 0. 0 A<J&£ ^ 

# I SampteNafn«:-b1tOia7a0a8 ' Sauipt e 10:'Solver: ! Kan k (AAiO^ O Element) ' Fie : tj-llOIOZal. w Pea k Name : "PFBS * Ma*s(es} : •299.a'9S. 0 «niu.299.a'80. 0 amu " Commen t tm-
. Q Wate rTN11JXKJB " Anno-ation : -

Ki.-i
. r#» k

HDight :

Printin g Titne : 2:56:4 1 P M Printin g Date : Tuesday , Marc h Pag e 1 o f 4 1 0 1 2 Ttrnq
. mi n 2 9 , Pag e 5 7 O f10 4Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I Sampte Name : T>nO1O7«034 ' Sampl e ID : 1.05-101230-4 " PM k Name : TFBS " Maa*(es) : •2M.0«9. 0 amu,299.0iB0, a a j Cotrment : "Spf * LCS * Armotaltor ' ~ Conctri.-at i 1.20* 6 I.I89 6 I.i6e 6 I.14e 6 1.12e6 1.10o« - V0S« 6 t.06e e I.04e 6 1.D2e 6 1-00c6 - 9.B0« 5 3.60B 5 9.<0e 5 9.20e 5 9.00e 5 g.eoe 5 8.60e 5 B.40e 5 8.20e5

- B.00e 5 7.806 5 7.60e 5 7.40e 5 7.20e 5 VOOeS

6.S0a 5 6.eaeS ' 6.40e 5 ; t20BS ' 6.00«5 - 5.fiOe5 5.60e&- 5.40«5 - 5,20e S S.MteS 4.80«5 ' 4.e0e S 4.40eS 4.20e a 4.00e 5 3,60o 5 3.60e 5 3.40o 5 3.30B 5 3-00e 5 2.S0e 6 2.G0a S 2.40e 5 2.20 ^ 2.00« 5 I.BOe S VSOe S V40« S 1.20eS l.OCteS ' S.OOM e.00e 4 4.00* 1 2.00e 4 O.tX) ' t-Spllt
. Faozo r 

## ( Sampl e Name : " b •1O107aO92- Sampto ID : ••GLPIiMli-02- ! Pea k Nanw : TFBS ' MaM[es) : '299.&-9S. 0 Bniu.299.!V80. 0 a r Comment : "DA L GW 134 S 0 lO l ^05 " Annotation : " Sansl c Type : Ur.V.-.ow n Ccncer. i ra t ioi : !i.'. « 640 0

«3rtiii(ic : N o 800 0

760 0 C
- .-r. j ^po-r.: : '''X W J.i n 720 0
i;. = '00 0 i^'-t' ! 680 0
^ i n 660 0 $40 0
620 0
600 0
580 0 sec o
S40 0
520 0
SOO O
460 0
•(600

-

. 4«0 .

- 400 0 330 0 360 0 3400

- 320 0
KX»
- 2S0Q ' 2fi0 0 2400

- 2200

- 2000

-

MO O 120 0 100 0

li.llU4..Jt4^.i ; Printin g Time : 2:56:4 1 P M Princin g Date : Tuesday , Marc h 29 , Pag e 2 o f 4 Pag e 5 8 o f 104Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS
. PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I SampteName:T>11O1O7a016 " Sampte ID-"08008-194-8 ' File:-b110107a1.wit r P«a k Naire : -PFHS ' Massfea) : -39S.Q'-99. 0 amu.3S9.0,'80. 0 ama ' Con-jnent : "1. 0 ng/m L F C st d i n MM i Q Wstai ' Annotaso r~ 

# I Sampl e Name : "b l 10107a008 ' Sampl e ff): 'Stdven t Blan k (tM Q eiemeni) - Fla : "b l I01Q7a1.wi r Pea k Name : -PFMS " Mas8(es) : -SSS.O'-Sg.O amy.399.0m0. 0 amu " Comment : tm-
. Q Wate rTN I 1-OOOS " Annotation : * •
2.3e S 2.3e5 :

2. 1 e S 2.1e 5 2.0e 5

1.7e5 - I.Se S

I.ift 5 l.ie S 1.0e 5 9.5e4 ' &.0e 4 B.5e4

7.0* 4 6.5o 4 fi.0o4- 5.Se 4 S.OoA

4.5*4

- 4.0e4

- 3.5B4

- 3.0e 4 2.5e4

- 2.0e4

- 1.5e4

- 1.0e4

- 5000.0

- 0.0

- • 

### ..-A.
. 1 JlJIi i 1 6 1 8 2 0 Printin g Time : 2:56:4 1 P M Printin g Date : Tuesday , Marc h Pag e 3 o f 4 Pag e 5 9 o f 10 4Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

tor.t i •.tjt-: 5 1

36P7 : 1. 1 & • 

## [ Sampl e Name:-b110iO7aO34 - Sampto ID : T-CS-lOIZStM - Fie:1)noi07a1.wt( r Peakt(ama:TFHS - MaM(e»):-399.0^. 0 amu,3e9.(V80^ attw * Cotrmenl : "Sppt i LCS ' AnnoCalkxi- "

1.14e 6 1.l2e 6 1.IDe 6 1.0ee 6 1.06e 6 I.04a 6 1.02a 6 1.00e 6 9.60e S 3.60e 5 9.40e 5 9.20e 5 9.00e 5 e.80e 5 e.60e 5 e.40e 5 a.2ae 5 a.00e 5 7.60e 5 7.60e5

- 7.40e5

- 7.!0e 5 r.OOe S &B0ft 5 S.60e 5 S.40e S 5.20a 5

. S.0Oe S

• S.eOe 5 5.60e 5 S.40eS ' SJOe S 5.00e5

- 4.S0« 5 4,60e 5 4.40eS ' 4.20e5 ' 4.00e5 ' 3.80c4

- 3.60e5 ' 3.4ae S 3.2005

- 3.00* 5 3.80 ^ 2.60e 5 2.40e 5 2.20e 5 2.00e5

- 1.80e5 ' I.60e5

- 1.40«S

LlOeS 1.00e5

- e.oo»4 - 6.00e4

- 4.006 4 • 2.00e4

- 0.00

- 

# I SamplaName:'bilO107aO9 rSampteffl:-GLPlfrOl-02-i1-065 - F9et)I10107ai.wi( P Pea k Name : "PFHS - MaMfes) : •399.0-^. 0 amu.399.0/80. 0 amo * CommenfDALG\V;34S0101l05 - AmtOaSon: -

6.5e 4 6.4e 4 6.3e 4 6.2fr 4 6.1 M 6.0e 4 5.9* 4 5.86 4 5.7* 4 5.6» 4 5.5» 4 5,4e 4 5.3* 4 5.2* 4 5.ie 4 5,0e 4 4.9* 4 4.Be 4 4.7e 4 4.Se « 4.5* 4 4.4e 4 4Jfl 4 4.2 M 4.le i 4.Ce 4 3.9* 4 3.ae 4 3,7e 4 3.6* 4 3.5e 4 3.4* 4 3.3* 4 3.2* 4 3.1* 4 3.0* 4 2.9e 4 2.9* 4 2.7* 4 2.6* 4 2.5* 4 2.4e 4 2.3* 4 2.2e * 2. 1 e 4 2.0* 4 i.9e 4 i.8e 4 i.7* a 1.S* 4 t.5e 4 t.4e 4 1JJ* 4 1.2* 4 1.1* 4 1J}» 4 9000. 0 8000. 0 70OC. 0 6000. 0 5000. 0 4000. 0 3000. 0 2000. 0 1000. 0 0. 0 1 4 I B



### 1 

# 1 1 

# J
i*i.ii^r— • i | 

# i 

# A
1*1—J.— , 1 6 1 8 2 0 Printin g Tine : 2:56:4 1 P M Printin g Date : Tuesday , Marc h 2 9 , Pag e 4 o f 4 Pag e 6 0 o f10 45te r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

• Sampl e Nam*:'b t 10107<t0l6 - Sampi * ID : XS0Ofl-l94-8 - FBe : -b1101U7a1.wrf r I Peakrtamo:-PFOS - Massieil:-':e9.C«9.0amu.499,0«OJ)aTXj.499.0.'I30.0ami r I ComTienl:'1.0n9fniLFCs;iJ>--)MAQWate[ ' An:>olat>on- ' Sjr-pl e In^CK - 1 l i

Printin g Time ; 2:53:1 5 P M Printin g Date : Tuesday , Marc h Pag e 1 o f 3 Pag e 6 1 o f10 4Buste r J293020 3 GLP10-01-02 ; interi m Repor t 1 1 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

I Sampl e Name ; •bl10IO7a034

- Sampl e 10 : XCS-10123IM

- Fae:-b1iO107a1. w I Pea k Naire ; -PFOS

- Massiet) : "JSa.OraS. O amu.499.0«0. 0 amu.499.3.'130. 0 am i I Corrmeni : •5pp b LCS ' AnnotaUon ' "
1.14e6

- 1.12e6

- 1.10e« ' 1.060 6 i.oeo6 ' 1.04« 6 1.02e 6 1.00* 6 

# I Sampl e Name : •b110107a04 r Sampl e ff):T.CS-!0i23O-i3- Fde
. •b110107al.*i r Pea k Name : TFOS ' MassCes) : '499IV99. 0 amu,499.0)80. 0 aim;.499.0/130. 0 amu ' Comment : 'Spp b LC S ECF " Annotation." "

Enpect'^ c RT :
9.60e S 9.40e 5 9.20e5

- 9.00e 5 e.80a S B.e0e 5 8.40* 5 a.20c 5 aooo s 7.80e 5 r.COe S 7.40* 5 7.20e 5 7.00* 5 3.B0e 5 6.60*5 ' 5,40eS • 6.20*5 ' S 6.00*5

- ^ S.80e5

- I 5.G0eS ' S.40e5

- 5.20c5

- S.OOr.6

- 4,80eS

- <.60e5 ' 4.40* 5 4.20e5 ' 4,00e5

- 3.80* 5 3.60eS

3.40*5 ' 3.20e5 ' 3.00e5 '

3.40e S 2.20r 6 2.00* 5 I.80e 5 I.60e 5 V40e 5 1.20* 5 1.00* 5 a.00e * 6.00* 4 4.00 M 2.00* 4 0.0 0 

### '!!=] L Printin g Time : 2:58:1 5 P M Printin g Date : Tuesday , Marc h Pag e 2 o f 3 Pag e 6 2 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS
. an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Buste r J293020 3 

# I Sampl e Name : *bll0107a092 ' Sampl e ID : •GW'0-OA.Ql- i Pea k Name : *PFOS * Mass(e£) : '^lES.CJSSi } amu.499.0/80. 0 a i Cofrmeot:XA l G W13^ 5 0101105 ' Annoaflon; "

.k-ipU t I
. ?«a h• 2.2* 5 2.2e 5 2.1* 5 2.1e 5 2.0* 5 2.0e 5 i.9e 5 1.9e 5 1-8e 5 13e 5 1-7e5 1.7* 5 1-6* 5 1.6* 5 1.5* 5 l.Se S 1,46 5 1.4e 5 13e 5 13* 5 1J?e 5 1.20 5 1.1* 5 1.1* 5 1.0* 5 9.5* 4 9,0* 4 aie 4 EOe A 7.5* 4 7.0* 4 65* 4 6.0e 4 5.5* 4 5.0* 4 45* 4 4.0* 4 3.5e 4 3.0* 4 2.5e 4 2.0* 4 1.5* 4 1.0* 4 5000, 0
n n 15.1 6

15,0 K

V-*-

- . . Printin g Time : 2:53:1 5 P M Printin g Date : Tuesday , Marc h Pag e 5 o f Pag e 6 3 O f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fomrie rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bllOllOa.da b
b110 1 lOa.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) ; y= -7.03e-^00 3 x'^ 2 + 9.02e•^005 x•

^ 6e-^003 ( r= 0.9995 )



### < 4.0e7 - 3,8e7 - 3.6e 7 - 3,4e7 - 3,2e7 - 3,0e7 - 2,8e7 ' 2.6e7 - 2,4e 7 - 2.2e7 - 2.0e7 - 1.8e7 - 1.6e7 - 1.4e7 - 1,2e7 - 1.0e7 - 8.0e6 - 6,0e 6 - 4,0e6 - 2.0e6 - 0,0 - 

### / / 

### P / / j d 

### / / 

### / / / / ^ / / / 

### , „ ,-'' ' y ' 

### y / • ,^' ' ^y' ' 

### .-•' — 

### o

_ ^

"'•'"-\. , v_ /



### \ ^

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 Printin qTime : 3:32:1 7 P M Printin g D-3te : Tuesday , Februar y01 , 201 1 Pag e 1 o f 1
Pag e 6 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc hName : bHOHOa,da b
b l 10110a,rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -8.15e-^00 3 x* 2 - ^ 1.05e+00 6 x+ 4,4e•^003 ( r= 0.9996 )
4.8e7

- 4.6e7

- 4.4e 7 - 4.2e7

- 4.0e7

- 3.8e7

- 3.6e7

- 3.4e7

- 3,2e7

- 3.0e7

- 2.8e7

- 2,6e7

- 2.4e7

- 2.2e 7 - 2,0e7

- 1.8e7

- 1.6e7

- 1,4e7

- 1.2e7

- 1.0e7

- 8,0e6

- 6,0e 6 - 4.0e 6 - 2,0e 6 - 0,0

- 

### /
• - / / /

/ 

### / / / / / y ' y ' y y 

### / ,y'' '
y ^ 

### ^,^' .••-— " 

### o

•—•-—. - ~'-

^ 

### ^'

- ^-v

^

""^ N v. ^



### \ ^

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 100 Pri n Pri n :in g Time : 3:31:5 6 P M ling Date : Tuesday , Februar y01 , 201 1 Pag e 1 o f 1
Pag e 6 5 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fonne rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bllOllOa.da b b110110a,rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -6,12e-^00 3 x'^ 2 - f8.81e-^005 x+ 1.98e•^00 4 ( r= 0,9999 )
4,je / 4.2e7 - 4.0e7 - 3.8e7 - 3.6e7 - 3.4e7 - 3.2e7 - 3.0e7 - 2,8e7 - 2,6e7 - 2,4e 7 - 2.2e7 - 2.0e7 - 1.8e7 - 1,6e7 - 1,487 - 1.2e7 - 1.0e7 - 8.0e6 - 6.0e6 - 4,0e6 - 2.0e6 - 0.0 - 

### / • / / / /

/ / / / y y y ^ y '

, x '

y 

### ,.,-•••'' ' o

"'~~---.„ ^ K j

""•^•^ ^ 

### "--,

0 5 1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration
. ng/m L 6 0 6 5 7 0 7 5 8 0 85 9 0 9 5 10 0 printin g Time : 3;32:'! 5 ? K Printin g Date : Tuesday . Februar y01 , 201 1 Pag e 1 o f 1
Pag e 6 6 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 i',iste r J293020 3 

# I SampteName:1,110il0aOi6 ' Satr^ e 10--OSOOS-IS WF««:-b1t0110a-*« r PM k Nflir*:-PFBS

- Massjes) : •299,tM93. 0 arrw.2a9.0«0. 0 ajwj

CommanI : *1. 0 ngm i FC s! dnU S O Wala,

- Annotatio n"

q . Dlti :

L
. ?vp.- : b /IJ.' /


### "'"" :

js.: ' 

### "Ir - ^ 4

•jua. T-

:t ;


### '"'
. :', :

Mwl l 2.5* 5

2.5* 5 2.4* 5 2.4* 5 2J* S 2.3* 5 2Ji* 5 2.2* 5 2.1* 5 2.1* 5 2-0* 5 2.0* 6 1.9* 5 1.9* 5 1.3*5 - 1.8* 5 1.7* 5

Print i Print : n g Time : 3:C3:2 1 n g Date : Tuesday , t-Jarc h2 3 Sampl e Name : •bllOllOaOO r Sampl e tD : "Solxer- t

Blani i JfAIlO Elemeni)

- F»e:-b110110a.*n r Pea k Name : 'PFeS ' M3s*(es L•299.a'99. 0 amu.299.0iW). 0 amu " Commen t

'MS t Q Wate r TN I 1-O308 " Annotation: "

Pag e ] o f Pag e 6 7 O f10 4Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

w F * - Pea l hin < rr!<- h :nr i c^ej L H•ig ^ w^d-. ^ B T t ?.; « 

# I Sampl e Nam*:-bllonOaO W Sampl e ID : TCS-101230-4 ' FBa : •bllOHOa.w r Pea k Name : Tf=BS - Mass(es) : '299.0n%.l 3 amu,295.0*80. 0 amu ' CofT-menl : "SpplJ LCS ' AnnoCalion- "

1.24*6 - i.22« 6 1.20* 6 1.18e 6 1.1C* 6 1.14*6 - 1.12B 6 i.iOeS i.oacfl 1.06* 6 1.04*6

- 1.02o6

- 1.00*6

- 9.e0e 5 9.60* 5 9.4De5 ' 9.20*5

- 9.00* 5 6.80*5

- 8.60c5 ' S.40« 5 8.20*5

- 9.00* 5 7.80*5

- 7.6Qe5

- 7,40e 5 7.20* 5 7.00* 6 3.80* 5 6.60e 5 ; e.40o S o.20e 5 e.OOeS 5.60* 5 S.eOa S 5.40* 5 5,20e 5 5.00* 5 4.e0o 5 4.60* 5 4.40* 5 4.20*5 ' 4.00e 6 3.60* 5 3.60* 5 3.40*5

- 3.20*5

- 3.00* 5 2.60*5

- 2-60c6

- 2.40* 5 2.20e5 ' 2.00* 6 1.80*5

- 1.60e 5 1.40* 5 • 1.20o5

- 1.00*5

- a.00* 4 6.00* 4 4.00* 4 2.00*4

- 0.00

- [ Sampl*ltome:t)110110a05 rSampl e ID:'GLP1O^)1-02-;i-O46 ' FSe-bllOilOa.wW r Pea k Name ; *PFeS ' MaM(es) : •299.0.'9S. O amu.299.0'80. 0 I CommenL'DAl
. GW133R 0 101102(di l 1:10) * Annotation: "

:xpic',« aF.T.

-

l 6 1 8 2 0 Printin g Time : 3:03:2 1 P M Printin g Date : Tuesday , Marc h 2 9 , 2 01 1 Pag e 2 o f Pag e 6 8 o f 104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Bliste r J293020 3 Sampl e Name:-b l 101108016 - Sampl e ID'-08008-194-6 ' Fie : ti1iai10a.wi( r 

### I Pea k Name : -pFHS " Mass{o») ; •399.Q'9g. 0 a-no.3S9.(y80i l amu ' Con-.inenl:'1.0r.9'mLFC«Id<--iM:SQkr;ala rAnnolatior- ~

2.4e 5 2.3« 5 2.3a 6 2Je 5 2.2* 5 2.1* 5 2.1* 5 2.0* 5 2.0* 5 Heigl; ; : 1.9*5 - 1.ea5 - 1.8e5 1.7e5 - i.7e 5 1.6eS 1.So5 - 13e5 - 15* 5

I.Oe S 9.5* 4 9,0* 4 8.5* 4 8.0* 4 7.5* 4 7,0* 4 6.5* 4 6,0* 4 5.5* 4 5^4 - 4.5*4 - 4,0* 4 3.5* 4 3.0*4 ' 2.5* 4 • 2.0* 4 13* 4 1.0* 4 5000 X 0.0 - ,>A
. 

# I Sampl e Nam*:-b l 10 1 lOaOO rSampl e IO:'Sotrar t Blan k (MiniOEterrent) ' Fle:*b11011i : Pea k Name : 'PFHS ' htessfei) : •339.0''S9. 0 amo,399.0/80i ) amu Commen r-Pts

a Q Wrte rTN11-0008 " Annotation : -

iK-Jpat
. Fac : 

### /

% I/I3,',-:JI

-
N
-
:.5 C =-.!.-

,
O.C G .ip

s o"' ^ "H i
I.. : .i. , ^'\^ i .-

n z s

1

S 265 0 250 0 255 0 250 0 245 0 240 0 235 0 230 0 225 0 220 0 215 0 210 0 205 0 20G 0 195 0 190 0 185 0 1800

- 175 0 170 0 165 0 1SO 0 1550

- 150 0 146 0 1400

- 135 0 13C 0 1250

- 1200

- 1150

- 1100

- 1050

- 100 0

Printin g Time : 3:03:2 1 P M Printin g Date : Tuesday , Marc h Pag e 3 o f 4 Pag e 6 9 o f 10 4GLP10-01-02 : Interi m Repor t 1 1 Analysi s o f PFBS
. PFHS
. an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Suste r J29302C 3 

# I Sampl e Name : "bilO l 10JI034 ' Sampl e ID : XCS-10i23(M ' FSe : "bllOHOa.Wif r Pea k Name : -pFHS " tWass!**) : "399.(^99. 0 a?wi,3S9.a'80. 0 amu " Corrmeni : "Spp b LCS " AnnoCalion

- - Jjcpi e In-ifx : 3 4 ier-F'l e !•,•?- : v ^ :aici::iM«' i Co-c : H. M nrj'n L \=q
. D.-it,t : 1/11,'?01 1 1,16* 6 1.14* 6

= r^r'"AliOtitV.r. : In.9Lii::ua n - Hul l ^-'^ ^ PEsk-JFllt
. ?tc--ot : - 1,08o6 - ^in
. Pea k

i!«i=h; : C-.C C :p i 1.06e6

- li.i
. i.*i>
. Via-..-. : j.C C S4C 3xot.;hit. ^ •-i.jLh : • ) pyii-; s 1.04«6 '
J! * S(lal.lv * ?.? t

:ir
. ^^^ ^ i:iTi
. t-ypc : ''^^t'' ; 9.e0e5

- '.c^^.-
. 5^64'-i ; t-oi-ni J 9.60* 5 Star-.
. lixf : l':- l J.i. i 9.40*5

- 9.20* 5 • g.OOeS S.S0* 5 8.60e 5 8.40e5 - 8.20* 5 8.00*5

- 7.80e 5 7.60e5

- 7.40e5

- ?.20c 5 /.00e5 - 6.80* 5 3.60* 5 6.40* 5
« 6.20e 5 > . 6.00* 5 S S.80e 5

~ 5.60* 5 5.40e 5 5.20* 5 5.00* 5 4.80* 5 4.60* 5 4.40e S 4.20* 5 4.00e 5 3-80e 5 3.60* 5 3.40e 5 3.20* 5 3.00e 5 2.80* 5 2.60* 5 2.40* 5 2.20* 5 2.00* 5 i.eoe s 1.60* 5 i.40eS 1.20* 5 I.OOe S 8.00* 4 5.00e 4 4.00* 4 2.00* 4 0.00 - FHe:"b110110».w!( r I Commwrt:"OALewi33K010l102(dal:10 r Annotation:" '

5.7* 5 5.6* 5 5-Se 5 5.4* 5 5.3* 5 6.2* 5 5.1* 5 S.Ce 5 4,9e 5 4,8* 5 4.7* 5 4,6* 5 4.5* 5 4.4* 5 4.3* 6 4.2* 5 4.1* 5 4,G«S 3.9* 5 3.6* 5 3.7* 5 3.6* 5 3.5e 5 3.4* 5 3.3* 5 3.29 5 3.1* 5 3.0* 5 2.8* 5 2.ee 5 2.7* 5 2.6* 5 2.5* 5 2.4e b 2.3* 5 2.2* 5 2-1* 5 2.0* 5 1.9* 5 1.Be 5 1.7e5 1.6e5 1.Sc 5 1.4* 5 1.3« 5 1Je 5 1.1* 5 1.Ce 5 9,Ct> 4 8,0* 4 -.0* * 6.0* 4 5.0* 4 4,0e 4 3.Ce4 2.0e 4 1.0* 4 0. 0 1 4

14.03.. , 1 8



# 1 

# 1



# _-.

_

# _L
.

_ 1 2 1 4 1 6 1 8 2 0 Printin g Tine : 3:03:2 1 P M Printin g Date : Tuesday , Marc h 29 , 2 0 Pag e 4 c f 4 Pag e 7 0 o f 104Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I Sampl e Name : "S I lOIIOaOie " SampI * ID ' *D80O8-i94-8

- P«a k Kama : -pFOS ' Masses) : "'99.IV99J ) 3mu.499.0/80J ) a ' Cofrm*nl:-1.0nflPiH
. FCsaJiaMJIiQWalBf

- An--vaallor--" "
2.2e 5 2.2e 6 2.1e 5 2-1* 5 2.0a 5 2.0* 5 1.9* 5 1.9* 6 1-8«5 ' 1.ae 5

1.7* 5 1.6e5 ' 1-6e 5 1.5* 5 13*5 ' 1-4e 5 1.4e 5

9.5*4

- 9.0* 4 65* 4 8.0e 4 7.5* 4 T.O M 6.5*4

- 6-0*4

- 5.5* 4 5.0* 4 4.5*4

- 4 0fi4 3.5* 4 3.0*4

- 2.5*4

- ZXteA

1.5*4

- 1.0*4

- 5000.0

- 0. 0 J&fV * 

# I Sampl e Nam* : "b l 10 1 lOaOOa " Sampl e 10 : 'SolW M BUn< [MiH ^ EiorP*nt)

- Fie : ti l 10110a.*i r Pea k Nam* : •PFOS " Mas»(*S) : •499JJ.'99, 0 amu.49S.aB0. 0 amo.499.0/130. 0 am*. " Comment : "MS : Q Water TN I 1-<KI08

- Anno!3lkxi: "

Exoftc'.e a F.T :
PetB.-.iio nria-

-

Printin g Time : 3:04:1 7 P M Printin g Date : Tuesday , Marc h 1.9* 4 1.6* 4 1.8* 4 1.7* 4 1.7e 4 1.6* 4 1.5* 4 l - ^ 1.5*4 1.4*4 1.4e 4 1.3* 1 1.3*4 1^* 4 l,2n 4 1.1*4 1.1*4 1.0*4 § ? 9500, 0 

### » ^ 9000. 0
asoc o 80O0. O 7500. 0 7000. 0 6S0C. 0 6000. 0 5500. 0 5OOC. 0 4500. 0 4000. 0 3500. 0 300C. 0 250C. O 2000. 0 1500 0 100C. 0 500. 0 0. 0 i 1
. : i i , . 1 , , __^^ i

. , .1 ^ 1-1.-1^ ^ i...-1-.
. *tj yI ; * ^ ,- , , . Lj
. . 1 J_
. Jl i •. . < V I JJfci^^,itn*> , .^IIM M 

# , 1

.-i^MiivJi t 1 

# k^ • "nrf^ii.u u , 1 0 1 2 1 6 1 6 2 0 Pag e 1 o f 3 Pag e 7 1 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS
. PFHS
. an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

[Sampt e Name : "b l 10110a034 - Sampl e ID : TCS-10123fr4 " Pea k Kama : -PFOS " Masstesl : "499.0/991 ) amo,49 3 OfflO. 0 a i t Cw"nen!:-Spp b LCS " Annotation-• "

1.16*6 ' 1.14*6

- 1.12* 6 1.10* 6 i.0Se6 ' 1.06*6

- 1.<>**6 1.02* 6 1,00* 6 9.80e5 ' 3.60* 5 9.40* 5 9.20*5

- 9.00e5

- 8.80* 5 8.60* 5 8.40*5

- 8.20*5

- 8.00* 5 7.80e S 7,60*5

- 7.40e5

- 7.20*5

- 7.00* 5 6.60*5

- 6.60*5

- 6.40*5

- I 6.20e 5
^ 6.00*5

- I 5.60*5

- 5.60c5

- 5.40* 5 5.20*6

- 5.00*5

- 4,80e5

- 4.60*5

- 4.40*5

- 4.20e5

- 4,00*5

- 3,80*5

- 160* 5 3.40*5

- 3.20*5

- 3.00*5

- 2.SOe5 ' 2.60e5

- 2.40*5

- 2.20e5

- 2.00e 5 1.80c*

- 1.60e5

- I.40e5

- I.20e5

- 1.00c6

- 8.00*4

- 6.00*4

- 4.00M

2.00* 4 • 0.00

- 

# I SampleName:"b'!l0110a04 rSampl e !D : 105-101230-13 - Fil*:-b110110a.wi( r Pea k Name : "PFOS - M3U(*3) : "499.0.'S9. 0 amu.49S.Q(SO. O amu.499.0/130. ' Comm*ni : *5pp b LC S FC P Anooiatioo: "

1 2 1 4 1 6 1 6 2 0 Printin g Time : 3:04:1 7 P M Printin g Date : Tuesday , Marc h 29 , Pag e 2 o f3 Pag e 7 2 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fonne rSludg e Incorporatio n Are a - Novembe r201 0 Buste r J29302C 3

Princin qTime : 3:04:1 7 P M Printin g Date : Tuesday , t-jarc h 29 , Pag e 3 o f 3 Pag e 7 3 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bllOll'i a .da b
bllO l 14a,rd b (PFHS) ; "Quadratic " Regressio n (" 1 /x " weighting) : y= -6,64e-^00 3 x'^ 2 -i - 8.6e-t-005 x+ 3.29e-^003 ( r= 0.9997 )

i 2 c 3 

### 8 a 

### < 4.0e7 - 3.8e7 - 3.6e7 - 3.4e7 - 3.2e7 - 3.0e7 - 2.8e7 - 2.6e7 - 2,4e7 - 2.2e 7 - 2,0e 7 - 1,8e7 - 1.6e7 - 1.4e7 - 1.2e7 - 1.0e7 - a.OeS 6.0e6 - 4.0e6 - 2.0e6 - 0.0 - 

### / / P / / / / / / / / ^y" ^ ^ y '

y ' y y ^ y 

### ..---' " -•--" " '"\.
. O



### ^ 

### ^\., ^ ' \ \

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 Printin g Time : 9:06:1 3 A M Printin g Date : Wednesday , Februar y02 , 201 1 Pag e 1 o f 1
Pag e 7 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fonne rSludg e Incorporatio n Are a - Novembe r201 0

Buste r J293020 3 Batc h Name : bllOll'Sa.da b
b110114a.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -7,54e-^00 3 x'^ 2 + 9,96e•^005 x+ 5.76e-^003 ( r= 0.9996 ) t,/e / 4,6e 7 - 4.4e7

- 4.2e7

- 4.0e7

- 3.8e7

- 3.6e 7 - 3.48 7 - 3.2e7

- 3,0e7

- 2,8e7

- 2.6e7

- 2.4e7

- 2.2e7

- 2.0e7

- 1.8e7

- 1.6e7

- 1.4e7

- 1.2e7

- 1.0e7

- 8.0e6

- 6.0e6

- 4.0e 6 • 2.0e6

- 0.0

- 

### / / / / 

## • / / / / / y

/ / / y'' '

^ y 

## / /

. * -• ' ' .,---'' ' o

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### o



### ""^^ ^

X

1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 85 9 0 9 5 10 0 '.-rin

- ?ri n lin g Time : 9:05:5 1 A M .in g Date : Wednesday , Februar y 02 , 201 1 Pag e 1 o f 1
Pag e 7 5 O f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fornie rSludg e Incorporatio n Are a - Novembe r201 0
Buste r J293020 3 Batc hNaine : bllOll'Sa.da b
b l 10114a.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -5.57e-^00 3 x* 2 + 8.19e-^005 x+ 5.51e-^004 ( r= 1,0000)

* 2 

### 8 C O 

### < 4.0e 7 3.8e 7 3,6e 7 3.4e7 - 3,2e7 - 3.0e7 - 2.8e7 ~ 2.6e7 - 2.4e7 - 2.2e7 - 2.0e 7 - 1.867 - 1.6e7 - 1.4e7 - 1.2e7 - 1.0e7 - 8.0e 6 - e.OeS4.0e6 - 2.0e6 - 0.0 - 

### /

9 

### / / / / 

### / / / 

### / / „. - X

y y y 

### ,,-«'' '

.,.^' ' ,.'"' ' o

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1 0 1 5 2 0 2 5 3 0 35 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 Printin g Time : 9:06:3 3 A K Printin g Date : Wednesday , Februar y02 , 201 1 Pag e 1 o f 1
Pag e 7 6 o f10 4Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I Sampl e Nam* : ti l 10114a016 - Sampl e ID : "08008-194-6 ' Pea k Narr^e : "P fBS - Mass(Bsl : -299.0/99. 0 amu,299.0/SO, 0 Corrment : -1. 0 og/m L F C st d i- i M S Q WaWr" Annotation-" "
23t S 23* 5 2.2* 5 2.2* 5 2.1* 5 2.1* 5 2.0e 5 2.0* 5 1.9e5

? 1 " 1.7* 5 1.7* 5 1.6* 5 1.6e S 1.5* 5 1.5* 5 1.4* 5 1/4* 5 1.3e5 1.3e S 1J!e 5 1.2* 5

1.0* 5 9.5*4

- 9.0* 4 8.5e 4 e.0e 4 7.5*4

- 7.0*4

- 6.5*4

- 6.0e4 ' 5.5*4

- 5i>e 4 4.5*4

- 4J}e4 - 3.5* 4 3.0* 4 2.5*4 - 2.0* 4 13* 4 IJM - 5000.0 - 0.0 - U i ^ 

# I SamptaNaina:liliai14a0a8 - Sampl e ID.'Sotver^tBlam t {MdlK D E)e[r.*nt} ' Fl*:-b110114a.<w r Pea k Name : "PFBS " Masses) : •299.0.'9S. O aniii.299-0W. 0 amu ' Commen t "M3t : Q Wa!e ' TN I 1-0008 " Annoialion :

Printin g Tine : 3:Cb:C 3 P M Pri.ntin g Date : Tuesday , Marc h Pag e 1 o f 25 , Pag e 7 7 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fonne rSludg e Incorporatio n Are a - Novembe r201 0 ii.-5te r J293020 3 SampteName:-bll0114a05 rSampl e iO;-Gt.PHWll.02- : Pea k Nanw:-PFBS - Maaa(es):-299.a'9e. 0 ainu.299.0'SO. O « r Comfnenl:-DALGW-.34L010110S{(tlT10 rAreiolallon' -

Printin g Time : Printin g Date : 3:06:0 3 P M

Tuesday , Marc h .... . .- : ..^IfSu^.^.j^^l'^i.fi^.^.^.^jM ^ Vii,rt,iftii Pag e 2 o f

4 Pag e 7 8 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS , PFHS , an d PFO S i n Groundwate r Fornie rSludg e incorporatio n Are a - Novembe r201 0 Buste r J293020 3 

# I T Sampl e Name : "blIOIMBOIS " Sampl e ID : -0800«-194.« " Pea k hame : "PFHS ' Mass;«») : •399.a'99, 0 a.'nu,3fi9.C«0.0
. ConTnanl : *1. 0 ngfir L F C el d i n M: S Q Watar " An-iotallon - 

# I Sampl e Name : "b l 10 1 MaOOS ' Sampl e ID : 'Solver t Blani^ {MUS^ Q Elerr«nt) ' Fie : "b110114a.Mf r Pea k Name : "PFHS " MaM(*s] : -399.o;99. 0 amu.399.0/80. 0 amu * Comn>*ni:"Min:QWBt*rTN11-0008 ' Annotation: "

y.od.ii^t : Fro:
. Aioarithn : .V=is e Ferc-nr.,g B

Ki^

- r« k

UBign- , ill^.t't ' xtd^

V R l i>i.r.do.f

f-ap^c'.*.•'
. r:T :

Peten-aor : rln-a : K*i(ihL : Fr dTint ; 11:^ 1 N O inuf i 

### :; :

3 D
. N o 6ds «

1 < : ; 5 *; i

9 0

o.c-cc.c- e J
. = rtC m i

. 2 pii n

. 2 Bi n .•n L 

### ^ ll'.r
. J 330 0

325 0 320 0 315 0 310 0 305 0 300 0 295 0 290 0 285 0 2B0 0 275 0 270 0 2S5 0 260 0 255 0 250 0 245 0 240 0 235 0 230 0 22S 0 220 0 215 0 210 0 205 0 200 0 195 0 190 0 165 0 180 0 175 0 170 0 iia o

Printin g Time : 3:06:0 3 P M Printin g Date : Tuesday , Marc: n Pag e 3 o f 4 29 , 201 1 Pag e 7 9 o f 10 4Buste r J293020 3 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I Sampl e Name : "bllO ! 14a034 ' Sampl e ID ' T.CS-1012JO^ - Fte : "bllOIUa.w r Pea k Name : "P fHS " M3s»(e») : "399.0.'99. 0 3.110,399,0/80. 0 amu " Cofrnient : "Spp b LCS " Annotation- "

i:2» : > S ^ M 1.14e6

1.12* 6 1.10* 6 1.08e 6 1.06e 6 1.04* 6 1.02e« ' i.00e € 9.80* 5 g.GOeS 9.40* 5 9.20* 5 9.00* 5 e.80e 5 B.60e5 ' e.40e 5 8.20* 5 6.00* 5 7.60* 5 7.60* 6 7.40* 5 f.20* 5 7.00* 5 S.80a 5 3.60* 5 • 5.40e 5 6.20e 5

• d.oOeS

-

- S.80eS

5.60* 5 5.-<0e5

- 5.20e 5 5.00* 5 4.S0eS ' 4.60e 5 4.40* 5 4.20* 5 4.00* 5 3.80e 5 3.60* 5 3,40*5

- 3.20* 5 3.00*5

- 2.S0e5 ' 2.60*5

- 2.40*5

- 2.20*5

- 2.00* 5 1.80* 5 i.eoe s 1.40*5 - 1.20*5 - 1.00*5 - 8.00*4 - 6.00*4- 4.00*» - 2.00*4 - 0.00 - 

## [ Sampl e Name ; "b l I0ll4a0s rSampl e !D : "GLPI0-01-02- 1 Pea k Name : "PFHS " Mais{e») : "399.0''S9. 0 amu.399.0/8D. O CWnmenI : "DAI
. GW134 L 0 10110 5 (d a I -lO fAnnotallor - ^

^ne :

- c : .^i c = rlt.ho : .'iiiti
. ••.-ind o p-it
. Fac

- «sk
. fl»iri.i ' '.r. qHldch : is'.iv e RT :

ri.Tie : <:3J:,; ? A 4 V,. , IiisL^lliWua,-

- -

'J O a^ ; [ly O-CC 0 i«. Z.,r . ajs e T o Bif. s K . ZBi n .S7t-i5 5 cp ^ 13. i .ni o • 3

'o--

- 3.8e 5

3.7* 5 3.6* 5 3.5e S 3.4* 5 3.3* 5 3.2a S 3.ie 5 a.Oe S 2.9e 5 2Je 5 2.7e 5 2.6e 5 2.5e 5

Printin g Time : 3:06:0 3 P M Printin g Date : Tuesday , Marc h 29 , Pag e 4 o fA Pag e 8 0 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Ete r J293020 3 

# I Sampl e Name : ^110114a0l6 " Sampl e 10 : -08008-194-8 - Pea k Name : -PFOS ' MasM**) ; '469.0/99. 0 amu.499.0/80. 0 w Conmenl : "1. 0 ng/ml
. F C sl d i n Mff i Q Water ' AmotaUoP ' "
2.2*5 - 2.1* 5 2.1e5 - 2.0*5 - 2.0* 5 1.9* 5 1.9e S 1.8* 5 1.8* 5 1.7* 5 1.7* 5 1.6* 5 1.6e S 1.5e5 15e 5 1.4* 5 1.4*5 - 1Je 5 1.3*5 - 1.2e5 - 1.2e5 1.1*5 - 1.1*5 - 1.0* 5 9.5*4 - 9.0*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 - 35*4 - 3.0*4 - 23* 4 2.0* 4 1.5*4 1.0*4 5000. 0
0.0 - Printin qTime ; 3:06:5 8 P M Printin g Date : Tuesday , Marc h 

## ( Sampl e Name : "bllO ! 14a00a ' Sampl e 10 : "Solven t man^ t {Milti O Elerr.enl) ' FUe : "b l I0114a.>vrf r Pea k Kama : "PFOS " Mass(e3j : "499i>''g9. 0 amu.49S.0iS0. 0 amu.499.0/130. 0 amu " Comment : "MJ l Q Wate rTN1 1 -0008 " Annotation : ~ 3J© 4 32e 4 3.2* 4 3.ie 4 3.1* 4 3.0* 4 3.0* 4 2.9* 4 2-9* 4 2-ee4 2.8* 4 2.7* 4 2,7e 4 2.6* 4 2.5* 4 2.Se4 2i6 4 2.4* 4 2.4* « 2.3* 4 2.3* 4 2i* 4 2.2* 4 2.1* 4 2.1* 4 2.0* 4 2.0* 4 1.9* 4 1.9* 4 1.6*4 1.8*4 !.7* 4 I.7e 4 t.6* 4 1.6* 4 1.5* 4 i.Se 4 1.4*4 1.4* 4 1.30 4 13* 4 1.2* 4 1Je 4 1.1* 4 1.1*4 1.0*4 950C. 0 9000. 0 8500. 0 8000. 0 7500. 0 7000. 0 6S0C. 0 600C. O 550C. 0 500C. 0 4500. 0 4000. 0 35O0. O 3000, 0 :soc. o 2000. 0 1500. 0 lOOC O 50C. 0 0. 0 ...^.....U
. ^

, ^.^.....^.^^ ^ ....^L,U,t»I.^^M" * 1 5 2 4

j j 

# 4 , T * **fty*t*>t*i<d*i....
. 1 6 1 8 2 0 Pag e 1 o f

J Pag e 8 1 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o f PFBS
. PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 3ii5te r J293020 3 

# I Sampl e Name : "b l 10114a034 " Sampl e ID : •LCS-101230-* " Pea k Kame ; TTOS " Massies) , "499,W99. 0 amu.493,0«0. 0 a i Comment : "Spp b LCS " Annoialion- "
Conctr.^iaticr. ; *
. 5 " .-1.,,'nl , 1.12* 6 1.10* 6 1.08* 6 1.06* e 1,04* 6 I.02e 6 1.00* 6

•• * 9.80* 5 9.60* 5 9.40* 5 9.20* 5 9.00* 5 • 8.80* 5 • B,60e 5 S.40« 5 8.20* 5 BOOcS 7.60e 5 7.60* 5 7.40e 5 7.20* 5 7.00* 5 G.C0e5 6.60e S 3.40* 5 6.20* 5 6.00* 5 §

- 5.80* 5 I " 5,60e 5 £5,40*5

- 5.20e5

- 5.00e 5 4.80* 5 4.80*5 ' 4.40*5

- 4,?0e 5 4.00e 5 3.eOe5

- 3.60* 5 3.40« S 3.20e 5 3.00* 5 2.eae 5 2.60* 5 2.40* 5 2.20* 5 2.00* 5 1.80* 5 1.60B5 ' 1.40* 6 1.20* 5 1,00* 5 8.00e 4 8.00* 4 4.00 ^ 2.00* 4 0.0 0 I SamBteName:'bl10114aO4 r Sampl e ID : "LCS-10i230-i r Fil*:"b1I0n4a.w« r

15.0&. ^
Printin g Time : Printin a Date : :0t;:5 8 P M uesday , Marc h Pag e 2 o f 3 Pag e 8 2 o f 10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundw/ate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Buste r J293020 3

Printin g Tine : Printin a Date : 3:06:5 8 P M Tuesday , Marc: n29 , 201 1 Pag e 3 c f 3 Pag e 8 3 o f10 4Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b g1102 1 la.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -3.35e-*-003 x'*2 + 6.88e-^005 x+ 3.41e•^003 ( r= 0.9997 )
2.7e7 - 2.6e7 - 2.5e7 - 2.4e7 - 2.3e7 - 2.2e7 - 2.1e7 - 2.0e 7 1.9e 7 1.8e7 - 1.7e7 - 1.6e7 - 1.5e7 - 1.4e7 - 1.3e7 - 1.2e7 n 1.1e 7 1.0e7 - 9.0e6 - 8.0e6 - 7.0e6 - 6.0e6 - 5.0e6 - 4.0e6 - 3.0e6 - 2.0e6 - i.oee 0.0 - ^ • ^ y



### 9 ^ / y

y y y y y y y y y

, y / y '

y y ' " y

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## y d y ' ^ 

# X ,.'- ' .,.''' ' y ' ,..--' " . ^ ...--'-"' " ....-' ' ^-" " _..• •

1 0 1 2 1 4 1 6 1 8 2 0 2 2 2 4 2 6 2 8 Concentration , ng/m U 3 0 32 3 4 3 6 3 8 4 0 4 2 4 4 4 6 4 8 5 0 Pri r Pri r tin g Tine : 3:16:3 3 P M tin g Date : Tuesday , Marc: n 29 , 2 0 Pag e 1 o f 1 Pag e 8 4 o f10 4Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundw/ate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b

• g1102 1 la.rd b (PFOS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -1.24e•^004 x'^ 2 + 1.76e-t-00

6 x+ 8.61e-f00 3 ( r= 0.9998 ) 5.9e 7 i 5.8e7 - 5.6e7 - 5.4e7 - 5.2e 7 - 5.0e7 - 4.8e7 - 4.6e 7 - 4.4e7 - 4.2e 7 - 4.0e7 - 3.8e 7 3.6e7 - 3.4e 7 - 3.2e7 - 1 3.0e7 - 8 CO - 2.8e 7 < 2.6e 7 2.4e7 - 2.2e 7 2.0e7 - 1.8e7 1.6e7 - 1.4e7 1.2e7 - 1.0e7 - 8.0e 6 e.OeS4.0e6 - 2.0e6 - 0.0 - ..-' ' .,-'' ' ,^ ' y ' ^ ,•' ' 

## y

y y y 

### y' ^
y y y y y / < 

### y y y / / /
m ' 

# • 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 32 Concentration , ng/m L 3 4 3 6 ,y' '

3 8 .^--"" '

4 0 .,-- "

4 2 „...- '

4 4 ,..--'' "

4 6 4 8 _^. m

5 0 Printin g Time : 3:16:5 8 P M Printin g Date : Tuesday , t-Iarc: n 29 , 2 0 Pag e 1 o f 1 Pag e 8 5 o f10 4Ginge r AG0i33050 9 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b 

# I Sampl e Name:'gllO211a0i9 - SampI * ID : •10007-27-e ' Fll«:"g1102t1a.wit r Pea k Name : T fBS " Massfes) : •299.0«9. 0 amu,29S.QfB0, 0 amu " Cofnm*nt : 1J 3 ng/ml
. F C sl d i n hl:l fQ water " Annotation - ' :Ur.p; e Ir.fjer. -



### % 1.6* 5 1.6* 5 1.5* 5 1.Se 5 1.4* 5
1.4e5 1.3* 5 1,3e5 U « 5 1.2* 5 l.le S
1.1* 5 1.0e S 95* 4
9.0e 4 8.5» 4 8.0* 4 7.5* 4 7.0* 4 65* 4 6-0* 4 5.5* 4 5.0* 4 4.5* 4 4.0* 4 3.5* 4 3.0* 4 2.5* 4 2.0* 4 1.5* 4 1.0* 4

SDOO. O
0. 0 1 0



### - I t
. - ,-. . 

### - -.- . 

### .-.. - ^-
. 59

k
. ,--, _ Pri.nting Time : 3:14:5 5 P M Printin g Date : T-jesday , Marc h 29 , 201 1 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 ^ rBn*.ipfn ^
_II I I Sampl o Name:-91102113011 ' Sampl e ID:"Solver t Blani< " Fiki:"g110211a.*if r Pea k Name : "PFBS ' Hassles) : •299.0«9.0amu.299.0i80.0amu I Comment'Ml^QWEdeiTNII-OOS rAnnotation: -

i«« k HBigh ;

Pag e 1 o f 2 Pag e 8 6 o f10 4Ginge r AGOi33050 9 GLP10-01-02 ; Interi m Reportl l Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b
I SampleName:-Bl10211a032 ' SamptelD:1.CS-110210-4 " FUe:'g l 102 1 la.wif T Pea k Name : T>FBS - Mas4<as) ; "299.0/99. 0 Bmu.299.0i80. 0 amu " I Conrnenl : "Spp b LCS ' Annotation- " SampI * Name ; "gnoaiialOS * SaniplolO:"GLP1<W)l-02- ! 1-134 ' Fte--g110211a.w!fr Pea k Name : TrBS ' Mass(«t} : '299.a-9S. 0 aniu.299.a'80. 0 amu " Comm*n fDAl,CW'!41R 0 101110 " AnnolaUon: -

5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 ^/it L

Li.- .

1 740 0

720 0

700 0

6BO 0

650 0

640 0

620 0

500 0

580 0

560 0

540 0

520 0

500 0

480 0

460 0

440 0

420 0

400 0

380 0

360 0

340 0 3» 0 300 0 2S0 0 260 0 34O 0 220 0 200 0 190 0 160 0 140 0 120 0 100 0

BOO 60 0 40 0 20 0 0 i \ 

# k
. *.4

- •i..L,
. -,-iJ

- 

## u. ^ J ^ 

### ^•^ ^ j t



# h 

# 'J^y' ' ^»^>%,^^m^ \

1 5 1 6 1 7 Printin g Tine : 3:14:5 5 P M Printin g Date : Tuesday , Marc h 29 , Pag e 2 o f 2 Pag e 8 7 o f10 4Ginge r AG O GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b 

## ( SamploNanwg 0211aO 9 Sampl e ID:-10007-27-8 " RIe;-g110211a.vnt r PaakNan- e PFO S Masses ) a99C/990amu.499.0/80.0amu.499.0/13D.Oam t Con-„ie n C ng,T U F s d MIS Q wale, - AnnotatJor ' ~ 4.2* 5 4.1e S 4i)6 5 3.96 5 3.ae 5 3.7e 5 3.6* 5 3.5e 5 3.4* 6 3.3* 5 3.2* 5 3.1* 5 3.0* 5 2.9* 5 2.6* 5 2.7* 5 2.6* 5 2.5* 5 2.4* 5 2.3* 5 2.2* 5 2.1e 5 2.0* 5 1.9* 5 1.6* 5 1.7* 5 1.6e 5 1.Se 5 1.4* 5 1.3* 5 U e S 1.1*5

- 1.0*5

- SJ>s 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

- n o 1 2



### , 3 9

L^>- V : 1 2 1 3 1 4 1 5 

## ( Sampl e Name : "g l 102 1 laOII " Sampl e ID:'Solven t Kank " File : "01102 1 la.wir T Pea k Name ; "PFOS ' Mass{esj : •499.0<'99. 0 amo.49S.Q/e0. 0 amo.499.0/130. 0 amL " Comment ; "Mifl : Q Wate rTN I l-005 rAnnotation : " •

Eziiio'.e dRI :

54O0 520 0 500 0 48D D 460 0 440 0 420 0 400 0 380 0 380 0 34O0 3200

- 300 0 280 0 260 0

1200 1C0 0 

### i



# I t

^.4ik4 i ii^...,aijXtfi4-*U>,.ifl^,>^ji.uiti^Jta^JvJi ^ 

# i /

2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 1 6 1 7 Printin g Time : 3:15:5 7 P M Printin g Date : Tuesday , t-5arc. h 29 , 201 1 Pag e 1 o f 3 Pag e 8 8 o f104Ginge r AG0133050 9 GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b 

# I Sampt * Name : "9110211*032 " Sa*npl * ID : \CS-110210-4 " Pea k N«re : "PFOS ' Ua»»(*»» : '-isg.twgj j 8rw.499.0«O. D a ^ CoRvnenI : *Sf>pt

> LCS " Anniatation : " *ir.i.i e iRripx : 3 2 ar'E.l e T-,-?- ; : U C oncc-r.v:»tic.:i : *
. 9 6 n^/nl , 2.2e 6 aiculotB' i Co-c : 5.4 3 aj/aL -q . Dit.!.

- 2/l?.'iO: i „^ , .:.!
. TiiiE ; *:l<:i?

- ».! 1 edified : N o 2.1e 6 f=c
. Aliciir..^.n : Inv«iii5iia n - Mu i I o n e .i-ei-.-^.-itrtSe : 5 u 2.1e 6 •,is.j
. Sub
. Wir.dow : i-e P ni.- i

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. ?«ak:ieich; : O.C C -p a ;in
. p»i» L Widtf-. ; O.C C sa c 2.0* 6 .ROoit-.ir> g siidTL^, : J poii-z s •xp.it'^o'RT : 1?. 4 sVS i '^'^ ^ 13 * Ruiatlv e ?.T : M o 1.9* 6 !it.
. Type ; Villii y -lar.tlar
. Tlne^ ^ i:.4^^^s.ir , , g ^ eigfi; : i:CO-30-3
. cc » i-ar v Ti.T* : i:. ? ii: i 1-8*6 1.7*6

- 1.7o e 1.6*6

- 1.6e 6

1.4* 6 1.4* 6 lJe 6 1J* 6 1.2*6

- 1.2* 6 1.1* 6 1.1* 6 1.0* 6 9.5*5

- 9.0e 5 6.5* 5

6.5* 5 6.0* 5 55e 5 S.OeS 45e5

- 4.0* 5 33* 5 3.0* 5 2,5* 5 2.0* 5 15* 5 1.0* 5 S.0e 4
1 0 1 1 1 2 1 3 I SampleName:"gn0211»04 rSamplelD:XCS-110210-i3 ' FS*:-fll102l1a.ynf r

Printin g Tine : 3:15:5 7 P M Printin g Date : Tuesday , t-Jarc h 25 , 201 1 Pag e 2 c f 3 Pag e 8 9 o f10 4GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Result s Name : gll0211a.rd b

Pag e 3 o f

3 Pag e 9 0 o f10 4 Ginge r AG0i33050 9
I SampleNam«;-gH0211a096 - SarM " ID:-GLPiO4)1-02-11-0 WFlte;-g1102!la.w« -

5.1* 5 5.0* 5 4.9* 5 4.SeS 4.7* 5 4£e 5 45e 5 4.4e 5 4.3e 5 4.2* 5 4.1* 5 4.0* 5 3.9* 5 3.8* 5 3.7* 5 3.6* 5 .1.5* 5 3.4* 5 3.3e S 3.2* 5 3.1* 5 3.0e 5 2.9e 5 2.8* 5 2.7* 5 2.6* 5 2.5* 5 2.4* 5 2.3* 5 2.3* 5 2.1* 5 2.0* 5 1.9e5 1.6* 5 1.7e5 1.6eS 1.5e S 1.4e5 1.3e5 1.2a 5 1.1o 5 lOe S 9.0e 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 12.17.
.

Printin g Time : 3:15:5 8 P M Printin g Date : Tuesday , Marc h29 , 201 1GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0


### ATTACHMEN TC : ANALYTICA L METHO D

Pag e 9 1 o f104GLP10-01-02;Jnteri m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0


# 3 M Enviranmenta l Laboraloi y

Metho d Metho d o fAnalysi s fo rth e Determinatio n o fPerfiuorinate 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 : 

# ^//j/ a y Willia m K
. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 of1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfiuorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 9 2 o f10 4GLP10-01-02 : Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 Perfluorooctanesulfonat e (PFOS ) b yHig h Perfonnance Liqui d Chromatograph ycouple d t o a tande m Mas s Spectrometri cDetecto r(LC/MS/MS ) i n clea n wate rsamples
. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

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

t covere d unde rthi s analytica l procedure
. 2 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 perfomnance-base d method
. Metho d accurac yi s detennine 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 detennine 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 a s suc h (wit h expande d accurac

ystatements) , o rwil l no

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

yspikin g a know n volum e ofth e Workin g Standar d (WS ) int o a predetermine d amoun t 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 ofth e precisio n associate d wit h laborator yprocedures , bu t no

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

(FB)/Tri p Blan k AST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , place d i n a sampl e containe ri n th e laborator y an d treate d a s a sampl e i n al l respects , includin g exposure t o samplin g sit e conditions , storage , preservatio n an d al l analytica l procedures
. Th e purpos e o fth e F B i s t o detemnin e i ftest substance s o r othe rinterference s are presen t i n th e fiel d environment
. Thi s sampl e i s als o refen-ed t o as a Tri p Blank
. ETS-8-044. 0 Pag e 2 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfiuorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 9 3 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 ofth e FD S compare d t o that ofth e firs t sampl e give s a measur e o fth e precisio n associate d wit h sampl e collection , preservatio n an d storage , a s wel l a s wit h laborator yprocedures
. 

## 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s ofth e targe t analyte s 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 must b e adde d t o th e sampl e containe rwithou t rinsing. Thi s ma yb e accomplishe d b

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

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

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

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

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s o fth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles
. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p detemiin 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 must b e take n at th e sam e tim e an d place a s eac h FMS
. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot o

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

ya t th e tim e o

fsampl e extraction
. A

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

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

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

ysampl e t o detemnin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results
. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri 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 ofaqueou s samples
. 3. 9 Laborator ySampl e Aportio n o raliquot ofa sampl e receive d fro m th e fiel d fo rtesting
. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits ofprecisio n an d accurac ydurin g routin e operatin g conditions
. To simplif ydat a reporting , th e LLO Q i s generall yselecte d a s th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria
. Sampl e LLOQ s are matrix-dependent
. Th e uppe rlimi t 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 a s th e ULOQ
.
ETS-8-044. 0 Pag e 3 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfiuorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 9 4 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 ar e use d wit h othe rlaborator ysamples
. Th e metho d blan k i s use d t o detemiin e i ftest substance s o rothe rinterference s are presen t i n th e laborator y environment , th e reagents , o rth e apparatus
. 3.1 2 Sampl e Asampl e i s a n aliquot remove d fro m a large rquantit yofmateria l intende d t o represen t th e origina l source material
. 

## 3.1 3 Stoc k

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

## 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t nomiall y foun d i n th e sample(s)
. Asurrogat e compoun d i s typicall ya targe t analyt e wit h a t 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 ofa sun-ogat e analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired
. 

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

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

yi s responsibl e fo rmaintainin g a saf e wori < environmen t an d a curren t awarenes s ofloca l regulation s regardin g th e handlin g ofth e chemical s use d i n thi s method
. Areference fil e ofmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses
. 

## 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems
. Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l infonnatio n an d cautions
. 

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

yrunnin g metho d blanks
.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfiuorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 5 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 are no

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

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

t ra wdat a fo rpea k

integratio n an d quantitatio n 15-m L an d 50-m L disposabl e polypropylen e centrifug e tubes
. Gas tigh t syringes , 25pL , 50pL , lOOpL , 250pL , 500|JL , 

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

## 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C I 8 , 4. 6 m m x10 0 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

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

t Injectio n Analysi s Pag e 9 6 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Fornie rSludg e Incorporatio n Are a - 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 PFHp A PFOA PFN A PFD A PFUn A PFDoA PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263^21 9 31 3 ^26 9 an d 31 3 ^11 9 36 3 - ^ 319 , 36 3 - > 16 9 an d 36 3 ^ 11 9 41 3 - ^ 369 , 41 3 ^

21 9 an d 41 3 ^

16 9 46 3 - ^ 419 , 46 3 ^

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

21 9 an d 51 3 ^

26 9 56 3 - ^ 519 , 56 3 - ^

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

16 9 an d 61 3 ^

31 9 29 9 - > 8 0 an d 29 9 - > 9 9 39 9 - ^ 8 0 an d 39 9 - > 9 9 49 9 - » 80 , 49 9 - ^

9 9 an d 49 9 - > 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n 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 ofon e daughte rio n i s acceptabl e i fmetho d sensitivityi s achieved , provide d tha t retentio n tim e criteri a ar e me t t o assur e adequat e specificity
. Th e previou s infonnatio n i s intende d a s a guide , alternat e instalment s an d equipmen t ma yb e used
. 

## 7 Reagent s an d Standard s 7. 1 Chemical s Wate r- Milli-Q , HPLC grade , o rothe rsuitabl yappropriat e source s Methano l - HPLC grad e Ammoniu m Acetat e -A.C.S
. Reagen t Grad e 7. 2 Standard s Perfluorobutanoi cAci d (PFBA- C4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFHA - C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFNA - C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUn A- C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C I 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfiuorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 7 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### Th e previou s informatio n i s intende d a s a guide
. Reagent s an d standard s fro m alternat e source s ma yb e used
. 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t water
. Note : Alternativ e volume s ma yb e prepare d a s lon g a s th e ratio s ofth e solven t t o solut e 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 procedure serve s a s a n example
. Weighe d amounts an d fina l volume s ma yb e change d t o sui t th e need s ofa particula rstudy
. Fo rexample , p L volume s ma yb e spike d into volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels
. 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 t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask
. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container
. Prepar e a separat e solutio n fo reac h analyte
. Expiratio n date s an d storag e condition s ofstoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure
. A n exampl e ofpurit yan d sal t correctio n i s give n belowfo rPFOS
.

, . , , molecula rweigh t o fanio n sal t correctio n facto r= moclecula rweigh t ofsal t 49 9 PFO S (K-')sal t correctio n facto r= - ^ = 0.927 5 53 8 1 0 m g CaFiySOa'K

* wit h purit

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

an d brin g u p t o volum e wit h solvent
. 12 5 ng/m L mixe d standard—Ad d 625p L o fth e 5 pg/mL-mixe d worthin 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 ofpreparation
.

ETS-8-044. 0 Pag e 7 of1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfiuorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 9 8 of104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0


## 7. 5 Calibratio n Standard s Usin g th e worthin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline
. Note : Volume s ofwate ran d worthin g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline
. Calibratio n level s othe r tha n thos e liste d belowca n b e prepare d a s needed
.
Concentratio n o fWS , ng/m L 12 5 12 5 12 5 12 5 25 0 25 0 25 0 25 0 500 0 500 0 500 0 Volum e o fWS,ft L

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

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

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

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

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

yno t b e suitabl e fo r analysi s b

ythi s method
. Sample s containin g suspende d particulat e shoul d b e 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 int o labele d plasti cautovials
. Prepar e a t least fiv e metho d blanks
. 9 Sampl e Analysi s - LC/MS/M S Analyz e th e standar

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

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

xo runweighted , o rb

yquadrati cfi l (

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

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

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

wpoints ma

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

fth e metho d and/o rsolven t blanks
. Th e coefficien t ofdetenninatio n (f ) valu e fo rth e calibratio n curve mus t b e greate rtha n o requa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfiuorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 9 9 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 of6 points wil l b e use d t o constmc l th e calibratio n curve . I fth e calibratio n curve doe s no t meet acceptance criteria , perfor m routin e maintenance o rprepar e a ne wstandar d curve (i fnecessary) an d reanalyze
. Continuin g calibratio n verification s (CCV) are analyze d t o verif yth e accurac

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

t a minimu m afte rever ytent h sample , no

t includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set
. Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable
. Th e calibratio n curve an d th e last passin g CCV wil l the n bracket acceptabl e samples
. Multipl e CCV level s ma yb e used
. Sample s containin g analyte s that ar e quantitate d above th e concentratio n ofth 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 wdat a an d footnote d i n th e fina l report
. 10. 2 Metho d Blank s Metho d blank

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

s ma yb e injecte d multipl e times , bu t n o mor e tha n 3 injection s shoul d b e remove d fro m a singl e metho d blank
. At a minimum , metho d blank s ar e analyze d prio rt o 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 njn
. Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s must b e les s tha n 50 % o fth e are a coun t o

fth e LOQ standard
. Th e standar

d deviatio n 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 firs t standar

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

## 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field
. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l not b e exclude d fro m reporting
. Th e requiremen t fo r replicate s exclude s fiel d blanks
. 

## 10. 4 Surrogat e Spike s Surrogat e spike s are no

t require d bu t ma

yb e use d o n projec

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

ftwo differen t concentration s are t o b e prepare d wit h eac h preparatio n batch
. Lo wla b contro l spike s shoul d b e prepare d a t concentration s i n th e rang e o ffiv e 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 les s tha n o requa l t o 20 % an d th e averag e recover ymust b e 80-120%
. I f th e above criteri a are no t met , th e entire set ofsample s shoul d b e re-injecte d o rre-prepare d a s appropriate
.

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

t Injectio n Analysi s Pag e 10 0 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0


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

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

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

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

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

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

xD F Slop e D F = facto rb

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

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

## 1 2 Metho d Performanc e An ymetho d perfonnanc e parameter s that are no

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

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

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

ystandard s are no

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

yth e technica l manager , a minimu m ofthre e syste m suitabilit ysample s ar

e injecte d a

t th e beginnin g ofeac h analytica l ru 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 count s wit h a n RS D of^5 % an d a retentio n tim e RS D ofS2 % t o b e compliant
. 12. 2 Quantitatio n Calibratio n Curve : Th e coefficien t ofdetemninatio n (r^ ) valu e fo rth e calibratio n curve must b e greate rtha n o r equa l t o 0.990
. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n of th e LLOQ , whic h ma

yb e withi n ±30%
. CCV Performance : Th e calibratio n standard s that ar e intersperse d throughou t th e analytica l sequence are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve . Th e accurac yof eac h curve poin t mus

t b e withi n 25 % ofth e theoretica l valu e (withi n 30 % fo rlowest curve point)
. Sample s that 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 o f1 1 Metho d ofAnalysi s fo rth e Determinatio n ofPerfiuorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 10 1 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - 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 mas s spectra l respons e ofuniqu e ions
. 12. 3 Sensitivit y Th e targete d limi t ofquantitatio n fo ral l analyte s i s 0.02 5 ng/mL
. Th e LOQ fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluatio n o fappropriat e blank

s an d th e accurac

yofth e low-leve l calibratio n curve points
. Refe r t o Sectio n 1 0 fo radditiona l details
. 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s are designe d t o generat e dat a that are accurat e t o +/-30%
. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d accurac yoflaborator

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

ymatri xspikes
. 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field
. Th e relative percen t difference , RPD , shoul d b e reported
. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting
. Th e requiremen t fo rreplicate s exclude s 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 perfomiin 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 dat a packag e generate d fo ra stud ymus t includ e al l supportin g infonnatio n fo rreconstructio n o fth e data
. Infonnatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

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

## 1 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 o fAnalysi s fo rth e Determinatio n o fPerfiuorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 102 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , an d PFO S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

## i'. H ATTACHMEN TD : DEVIATIO N

Pag e 103 o f104GLP10-01-02 ; Interi m Repor t 1 1 Analysi s o fPFBS , PFHS , and PFO

S i n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/
. Identificatio n stud y/ Projec t No
. GLP10-01-02-1 1 Date(s ) o fOccurrence : 1/7/1 1 -2/11/1 1 Documen t Number : ETS-8-044. 0 Deviatio n typ e 0 SO P D Equipmen t Procedur e 0 Metho d (Chec k one ) D Protoco l D GP O D Other :

//
. Descriptio n (attac h extr a page s a s needed ) lyiethq d Requirernen^^^ ^ (1 ) LC S averag e recover yof100 % ±20%
. (2 ) Sample/Sampl e Duplicat e RP D <20%
. (3 ) Fiel d matri xspik e recover yo f100 % ±30%
. 

### Actua l procedure/proces^^ ^ (1 ) 1/7/11 ; th e averag e recover yfo rth e lowse t o fLC S fo rPFB S wa s 123 % an d fo rPFH S 123%
. Th e averag e recover

yofth e hig h se t ofEC F LC S sample s fo rPFO S wa s 123%
. 1/10/11 ; th e lowse t ofLC S sample s fo rPFH S ha d a n averag e recover yof122%
. Th e averag e recover yofth e hig h se t o fEC F LC S sample s fo rPFO S wa s 121%
. 2/11/11 ; th e hig h se t o fEC F LC S fo rPFO S ha d a n averag e recover yof133%
. (2 ) PFO S RP D valu e fo rDA L G W137 S wa s 33%
. (3 ) PFO S FM S recovery ; DA L G W137 S (59.4% ) an d DA L G W144 R (28.7%)
. PFH S FM S recovery ; DA L GW134S(135%)
. 

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

### Correctiv e Actio n ( D Ye s 0 No) Reference : Acceptabilit yo fth e nonconformin g work : 1 ) I n general , th e EC F LCS s fo rPFO S hav e bee n runnin g 15-20 % highe rwhe n quantitate d usin g linea r PFOS
. Al l LC S wer e use d i n th e determinatio n o fmetho d uncertainty
. Th e detenninatio n ofth e metho d uncertaintybyETS-12-012. 2 wa s ±18%
. However , du e t o potentia l analytica l bia s tha t wa s observe d whe n quantitatin g LC S sample s containin g linea ran d branche d isomers ofPFOS , th e analytica l fo rPFO S fo rthi s stud yhas bee n expande d t o ±33%
. 2 ) Samplin g location s wit h RP D value s S20 % wil l b e footnote d i n th e dat a tables
. 3 ) Analytica l uncertaintie s fo rDA L G W137 S an d DA L G W134 S wil l b e adjuste d accordingly
. Samplin g locatio n DA L G W144 R - PFO S result s wil l not b e reported
. Sample s wer e re-dllute d an d a LM S sample s wa s prepared
. Recoverie s fo rth e LM S sampl e fo rPFO S were stil l ~30 % fo rth e re-analysis
. Actions : D Haltin g o fWor k D Clien t Notificatio n D Wor k Recal l D Withholdin g o fRepor t 0 Other : Deviation s wil l b e note d i n finaPreport. Projec t Lead/PA I Approval : Susar i Wol f( 

### Stud yDirecto r(i fGLP) : Sponso rApprova l (fo rGL P protoco l deviations) : N A Technica l Reviewe r(optional) : N Ai Date : N A Laborator yDepartmen t Manage rApproval : Date :

IV
. Authorizatio n t o Resum e Wor k Wlier e haltin g ofworl < occurred , resumptio n ofworl < mus t firs t b e approve d b yLaborator yManagemen t 

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

yStud yDirecto ro rTea

m Leade ra

t tli e en d ofstudyo rproject ) ETS-4-008. 7 Pag e 1 o f1 Documentatio n o fDeviation s an d Contro l o fNonconfomiin g Testin g ^^^ ^ ^ ^ ° ^ ^°' *