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

S i n Wate rSample

s fro m Decatur, AL June/July201 0 

# 3 M

GLP10-01-02 : Interi m Repor t 0 6 - Analysi s o fPFBS

. PFHS

. an d PFO S i n Groundwater/Surfac e Wate rSample s Collecte d a s Par t o fth e Avenu e AInvestigatio n Are a i n Decatur

. A L i n June/Jul y201 0

Stud yTitl e 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 Progra m

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

. 140 0 Westo n Way Westchester , PA1938 0 Phone : 610-701-376 1
Autho r Susa n Wol f 3 M Environmenta l Laborator y Interi m Repor t Completio n Dat e

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

y 3 M Center , BId g 260-05-N-1 7 Maplewood , M N 55144 Projec t Identificatio n GLP10-01-02-0 6
Tota l Numbe ro fPage s

6 7

Th e testin g reported herei n mee t th e requirements ofISO/iE C 17025-200 5 "Genera l Requirement

s fo rth e Competenc

e ofTestin g an d Calibratio n i.^boratories" , i n accordanc e wit h th e A2iA

. Certificate #2052.01

. Testin g tha

t compiies wit h thi s intematlona l Standar d als o operat

e i n accordanc

e wit h IS O 9001:2000

. Certificat e #2052.0 1GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Thi s pag e ha

s bee n reserve d fo rspecifi ccountr yrequirements

.

Pag e 2 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

t 0 6 Analysi s o

fPFBS , PFHS , an d PFO S i n Groundwater/Surface Wate r Sample s Collecte d as Par t ofth e Avenu e AInvestigatio n Are a i n Decatur , A L i n June/Jul y201 0 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site
Relate d Monitorin g Program

. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l 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 ofa test system

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

t th e test sit e have no

t bee n determine d unde rGLPs

.

Gar yHohenstein , Sponso rRepresentative Date ( ( % 

# OkkU i Jaisimh a Kesari , P.E. , DEE , Stud yDirecto r

Pag e 3 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

t 0 6 Analysi s ofPFBS , PFHS , an d PFO S i n Groundwater/Surface Wate r Sample s Collecte d a s Par t ofth e Avenu e AInvestigatio n Are a i n Decatur , A L i n June/Jul y201 0 Study : Analysi s ofPerfluorooctan e Sulfonat e (PFOS) , Perfluorohexan e Sulfonat e (PFHS ) an d Perfluorobutan e sulfonat e (PFBS ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site
Relate d Monitorin g Program

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

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

.

Inspectio n Date s 9/23 , 9/24 , 9/27 , an d 9/28/1 0 Phas e

Dat a an d Interi m Repor

t Dat e Reporte d t o Testin g Facilit y Managemen t 10/12/1 0 Stud yDirecto r 10/12/1 0 

# H^r^^ f /d-2^-/ 0 Date

Pag e 4 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 yInfomnatio n 8 2 Summar

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

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

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

yan d Discussio n 2 1

Pag e 5 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 1 0 Conclusio n 3 7 1 1 Data/Sampl e Retentio n 3 7 1 2 Attachment s 3 7 1 3 Signature s 3 8 LIS TO F TABLE S Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Results (Avenu e AInvestigation , June/Jul y2010)

. 1 0 Tabl e 2

. Sampl e Descriptio n Ke yCod e 1 4 Tabl e 3

. Instalmen t Parameters

. 1 5 Tabl e 4

. Liqui d Chromatograph yCondition s 1 5 Tabl e 5

. Mas s 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 0 Tabl e 9

. DALSWSW0 1 10062 3 2 2 Tabl e 10

. DA L SWSW0 2 10062 2 2 2 Tabl e 11

. DA L SWSW0 3 10062 2 2 3 Tabl e 12

. DA L SWSW0 4 10062 2 2 3 Tabl e 13

. DA L SWSW0 5 10062 2 2 4 Tabl e 14

. DA L SWSW0 6 10062 2 2 4 Tabl e 15

. DA L SWSW0 7 10062 2 2 5 Tabl e 16

. DA L SWSW0 8 10062 3 2 5 Tabl e 17

. DA L SWSW0 9 10062 3 2 6 Tabl e 18

. DA L SWSW1 0 10062 3 2 6 Tabl e 19

. DALSWSW1 1 10062 3 2 7 Tabl e 20

. DA L SWSW1 2 10062 3 2 8 Tabl e 21

. DALGWGP0 1 10070 9 2 8

Pag e 6 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 22

. DA L GWGP0 2 10070 9 2 9 Tabl e 23

. DA L G WGP0 3 10070 9 2 9 Tabl e 24

. DA L GWGP0 4 10070 9 3 0 Tabl e 25

. DA L G WGP0 5 10070 9 3 1 Tabl e 26

. DA L GWGP0 7 10070 9 3 1 Tabl e 27

. DA L GWGP0 8 10070 9 3 2 Tabl e 28

. DA L G WGP0 9 10070 9 3 2 Tabl e 29

. DA L GWGP1 0 10070 9 33 Tabl e 30

. DALGWGP1 1 10070 8 33 Tabl e 31

. DA L GWGP1 2 10070 8 34 Tabl e 32

. DA L GW216 R 10071 6 34 Tabl e 33

. Tri p Blan k

35 Tabl e 34

. Rinseat e Blank s 3 6

Pag e 7 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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(gwestonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laboratory

. Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator , (clanqe(a)mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analyst Jonatha n Steege ; analys t Stud yDate s Stud yInitiation : Marc h 8 , 201 0 Interi m Repor

t 0 6 Experimenta l Termination : Septembe r10 , 201 0 Interi m Repor

t Completion : Date o

fInteri m Repor

t Signin g Locatio n o fArchive s Al l origina l rawdat a an d th e analytica l repor t hav e bee n archive d 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 are archive d a t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 79 2

Pag e 8 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate ran d surface wate rsample s collecte d as par t ofth e Avenu e AInvestigatio n are a i n Decatur , AL , representin g twenty-fou rdifferen t samplin g locations

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

. Sample s als o include d a

t leas t two fiel d matri xspik

e (FMS ) sample s fo reac h location , thre e tri p blank s containin g Milli-Q'^" wate ran d appropriat e tri p blan k spikes , an d two equipmen t rinseates. Th e equipmen t rinseate blank s di d no t have FM S sample s prepare d fo rdeterminatio n o fPFBS , PFHS , an d PFO S recovery
. Th e surface wate rsamples , on e set o ftri p blank s an d equipmen t rinseate blank s were receive d fro m Westo n personne l o n Jun e 25,2010

. Th e groundwate rsample s an d on e set oftri p blank s were receive d o n Jul y13 , 2010

. Th e groundwate rsample s fro m locatio n 216 R an d on e set oftri p blank s were receive d o n Jul y22 , 2010

. Al l wate rsample s fo rthi s projec t were logge d unde rGLP10-0 1 -01-06

. I n addition , soil-equipmen t rinseate blank s fro m GLP10-01-02-0 3 (Wetland s Edg e Environmen t Cente r -WEE C Swamp) , GLP10-01-02-0 5 (Avenu e AInvestigatio n - Soils) , an d GLP10-01-02-0 8 (Phas e 3 Offsit e Soil ) ar

e als o reporte d herein

. 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-10-0 1 -02-06

. Mos t ofth e wate rsample s require d dilutio n t o attai n PFBS , PFHS , an d PFO S concentration s withi n th e rang e ofth e curve , i n som e instance s u p t o a 200-fol d dilutio n was required

. Th e averag e measure d PFBS , PFHS , an d PFO S concentration s ar e summarize d i n Tabl e 1 Th e equipmen t rinseates an d tri p blank s were belowth e lowe rlimi t ofquantitatio n (LLOQ ) collecte d wit h th e wate rsample s fo rGLP10
- 01-02-06 , indicatin g adequat e contro l o fsampl e contaminatio n durin g shippin g an d sampl e collections

. Th e soil-equipmen t rinseate blank s fro m GLP10-01-02-03 , GLP10-01-02-05 , an d GLP10-01-02-0 8 were belo wth e LLOQ wit h th e exceptio n o fon e soil-equipmen t rinseate blan k collecte d unde rGLP10
- 01-02-0 3 whic h had a detecte d concentratio n jus t above th e LLOQ

. Th e PFB S concentratio n results fo ral l groundwate ran d surface wate rsample s range d ove rthre e order s ofmagnitud e fro m 0.764 ng/m L t o 27 9 ng/mL

. Th e PFH S concentratio n results fo ral l groundwate ran d surface wate rsampl e range d ove rthre e order

s ofmagnitud e fro m 3.68 ng/m L t o 1130 ng/mL

. Th e PFO S concentratio n results fo ral l groundwate ran d surface wate rsample s range d ove rtw o order s ofmagnitud e fro m 17. 5 ng/m L t o 178 0 ng/m L

Pag e 9 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 1

. Summarize d PFBS , PFHS , an d PFO S Result s (Avenu e AInvestigation , June/Jul y 2010)

.

Samplin g Locatio n DALSWSW0 1 10062 3 DA L SWSW0 2 10062 2 DA L SWSW0 3 10062 2 DA L SWSW0 4 10062 2 DA L SWSW0 5 10062 2 DA L SWSW0 6 10062 2 DA L SWSW0 7 10062 2 DA L SWSW0 8 10062 3 DA L SWSW0 9 10062 3 DA L SWSW1010062 3 DALSWSW1 1 10062 3 DA L SWSW1 2 10062 3 DALGWGP0 1 10070 9 DA L GWGP0 2 10070 9 DA L GWGP0 3 10070 9 DA L GWGP0 4 10070 9 DA L GWGP0 5 10070 9 DA L GWGP0 7 10070 9 DA L GWGP0 8 10070 9 DA L GWGP0 9 10070 9 DA L GWGP1 0 10070 9 DALGWGP1 1 10070 8 DA L GWGP1 2 10070 8 DA L GW216 R 10071 2 PFB S Avg

. Cone

. (ng/mL ) ±RP D 15. 0 ±4.0 % 7.6 8 ±5.1 % 9.5 7 ±1.2 % 13. 7 ±5.8 % 20. 9 ±1.9 % 17. 4 ±4.6 % 10. 8 ±0.0 % 40. 7 ±4.2 % 27 9 ±2.5 % 22. 5 ±4.4 % 102 ±3.0 % 0,76 4 ±2.4 % 5.0 2 ±0.20 % 21. 1 ±13 % 66. 4 ±0.45 % 19. 1 ±0.0 % 30. 0 ±0.0 % 20. 7 ±3.9 % 6.3 6 ±1.1 % 20. 7 ±1.9 % 44 7 ±2.5 % 67. 0 ±3.1 % 2.5 9 ±58 % '^ ' 10. 6 ±1.9 % PFH S

Avg

. Cone

. (ng/mL ) ±RP D 12 0 ±1.7 % 52. 0 ±0.19 %

, 72. 2 ±2.1 % 86. 5 ±2.0 % 102 ±3.9 % 77. 5 ±0.77 % 47. 9 ±1.0 % 16 6 ±3.6 % 64 3 ±9.0 % 23 3 ±2.6 % 113 0 ±0.89 % 3,6 8 ±0,54 % 7,6 3 ±3,7 % 11, 2 ±13 % 41 3 ±0,24%'^ ' 85, 8 ±8,6 % 15 8 ±5,7 % 17 1 ±2,9 % 70, 2 ±7,8 % 36. 0 ±13 % 42 0 ±3,3 % 33 0 ±1,8 % 11,2±44%<^ ' 30, 5 ±3,0 % PFO S

Avg

. Cone

. (ng/mL ) ±RP D 24 8 ±4,0 % 21 3 ±7,7 % 19 7 ±1,1 % 192 ±2.2 % 39 2 ±3,6 % 22 8 ±1,1 % 12 9 ±2,2 % 26 6 ±1,9 % 38 2 ±2,1 % 38 9 ±1.0 % 85 0 ±3.2 % 104 ±2,0 % 26, 2 ±5,3 % 17, 5 ±20 % 37 3 ±17%'^ ' 152 ±30%'^ ' 38 2 ±18 % 178 0 ±4,5 % 142 0 ±4,9 % 95, 5 ±33 % '^ ' 12 7 ±31%*^ ' 66 0 ±6,1 % 48, 8 ±67 % '^ ' 11 9 ±9,2 %
Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results ar e a s follows : PFB S 100 % ±21% , PFH S 100 % an d PFO S 100 % ±41% , (1 ) Samplin g locatio n di d no t hav e a n appropriate FM S spik e leve l t o sufficientl yevaluate analyte recovery , (2 ) Th e RP D di d no

t meet metho d acceptance criteri a of£20% , (3) Sampl e GLP10-01-02-03-00 9 (DAL-SD-WESB4-RB ) PFO S resul t wa s 0,26 0 ng/ml

. ±23% ,

Pag e 1 0 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 1 continued

. Summarize d PFBS , PFHS , an d PFO S Result s (Avenu e AInvestigation , June/Jul y2010)

.

Samplin g Locatio n Tri p Blan k

an d (Milll-Q TM Water

) Equipmen t rinseate blank s GLP10-01-01-0 3 Soil-Equipmen t rinseate blank s GLP10-01-01-0 5 Soil-Equipmen t rinseat e blank s GLP10-01-01-0 8 Soil-Equipmen t rinseat e blank s PFB S

Avg

. Cone

. (ng/mL ) ±RP D <0.025 5 <0,025 5 <0,025 5 <0,025 5 <0,025 5 PFH S

Avg

. Cone

. (ng/mL ) ±RP D <0,10 3 <0,10 3 <0.10 3 <0.10 3 <0.10 3 PFO S

Avg

. Cone

. (ng/mL ) ±RP D <0,25 5 <0,25 5 <0,255'' ' <0.25 5 <0,25 5
Th e analytica l metho d uncertaintie s associate d wit h th e reporte d results ar e as follows : PFB S 100 % ±21% , PFH S 100 % ±25% , an d PFO S 100 % ±44% , (1 ) Th e RP D di d no

t mee t metho d acceptance criteri a of£20% , (2 ) Samplin g locatio n di d no t hav e a n appropriate FM S spik e leve l t o sufficientl yevaluate analyte recovery , (3) Sampl e GLP10-0 1 -02-03-00 9 (DAL-SD-WESB4-RB ) PFO S result wa s 0,26 0 ng/mL , 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 ofth e overal l progra m i s t o gai n informatio n regardin g concentration s ofperfluorooctan e sulfonat e (PFOS) , perfluorohexan e sulfonat e (PFHS ) an d perfluorobutan e sulfonat e (PFBS) , i n variou s environmenta l medi a suc h as groundwater , soil s an d sediments that are associate d wit h an d nea rth e Decatu rfacility

. Thi s analytica l studywa s conducte d t o analyz e groun d wate ran d surface wate rsample s collecte d a s par t o fth e Avenu e A Investigatio n 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

. I n addition , thre e aqueou s soil-equipmen t rinseate sample s fro m GLP10-01
- 01-0 3 (Wetland s Edg e Environmen t Center-WEE C Swamp) , si xsoil-equipmen t rinseate sample s fro m GLP10-01-01-0 5 (Avenu e AInvestigatio n - Soils) , an d on e soil-equipmen t rinseate sampl e fro m GLP10-01-01-0 8 (Phas e 3 Offsit e Soil ) are als o reporte d herein

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

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

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

. Eac h empt ycontaine rwa s mari<e

d wit h a "fil l t o here " lin e t o produce a fina l sampl e volum e of20 0 mL

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

e solutio n containin g PFB S (linear) , PFH S (linear) , an d PFO S (linear ) prio rt o bein g sen t t o th e fiel d fo rsampl e collection

. Al l sampl e bottle s include d th e additio n ofO2-PFBS , ^^Oa-PFHS , an d ^^Cs-PFOS (interna l standards ) at a nomina l concentratio n o f1 ng/mL

. However , du e t o th e level s of PFBS , PFHS , an d PFO S detecte d i n th e samples , th e us e o finterna l standard s was no t use d fo r quantitation

. 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 marking s o rfortifications

. 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 ofPerfluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injecfio n Analysis"

.

Pag e 1 1 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o f PFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 1 summarize s th e averag e PFBS , PFHS , an d PFO S concentration s fo rth e duplicat e sample s collected , tri p blanks , groundwater-equipmen t rinseate samples , an d aqueou s soil-equipmen t rinseate samples

. Table s 9-3 4 summariz e th e individua l sampl e results an d th e associate d FM S recoveries

. Al l results fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s are reporte d an d discusse d elsewhere i n thi s repor t

.»r;« - 4 'i'Ces f & ContmliSubstanceS'V' '
There wa s no

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

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

.
5 • Reference'Substance s
.. .

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFB S (predominantl ylinear ) Perfluorobutan e sulfonate 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 CsFiaSO s Sodiu m Sal t Wellingto n 4/2/201 3 Froze n LPFHxSAMO

S TCR08-001 8 Crystallin e 98 %

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO S (linear ) Perfluorooctan e sulfonat e CsFiySO s Potassiu m Sal t CA S #2795-39- 3 Wellingto n 10/18/201 3 Froze n LPFOSKBM0 6 TCR08-000 1 Crystallin e 98 % PFO S (linea r+ branched ) Perfluorooctan e sulfonate C8F17SO 3 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 f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "O2-PFB S Labele d - Perfluorobutan e sulfonate C4F9S[^^02]0
- Ammoniu m Sal t RT I Internationa l 3/9/201 5 Froze n 11546-107-2 TCR-101 3 Liqui d 99 % "OrPFH S

Labele d - Perfluorohexan e sulfonate CeFiaSt^'Oal^'O " Sodiu m Sal t Wellingto n 7/24/201 1 Froze n MPFHXA0706 TCR-121 8 Liqui d 98 %

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

t Numbe r TC R Numbe r Physica l Descriptio n Purit y "Cg-PFO S Perfluorooctan e sulfonat e CsFi ySO 3 Sodiu m Sal t Wellingto n 6/17/201 2 Froze n M8PFOS060 9 TCR09-004 9 Liqui d 98 %

Pag e 1 3 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 6 Tes t Syste m
Th e test syste m fo rthi s stud yar e surface wate ran d groun d wate rsample s collecte d fro m well s locate d i n Decatur , A L b

yWesto n Solutions , Inc

. personnel

. Sample s fo rthi s stud yar e "rea l worid " samples , not dose d wit h a specifi clo t oftest substance

. Tabl e 2

. Sampl e Descriptio n Ke yCode

. strin g Numbie r Exampl e 1 2 4 Strin g Descripto r DA L SWSW0 7 010062 2 Sampl e Typ e Sampl e Locatio n Samplin g Dat e Sampl e Typ e Exampl e SW=Surfyc e Wate r Example : SVV0

7 100622-Jun e 22 , 201 0 0=piimarysampl 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 "Determinatio n ofPerfluorinate d Compound s I n Wate rb yHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

.

,T M , 

### 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene' TM (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory

. Sampl e bottle s were returne d t o th e laborator ya t ambien t condition s o n Jun e 25 , Jul y13 , an d Jul y22 , 2010

. Sample s were store d refrigerate d a t th e laborator

yafte rreceipt

. On e set o flaborator

yprepare d Tri p Blan k

an d Tri p Blan k

field matri xspike s were returne d wit h eac h batc h ofsampl e collectio n bottles

. 

### 7. 3 Sampl e Preparatio n Sample s were prepare d b yremovin g a n aliquot o

fth e wel l mixe d sampl e an d placin g it 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 ofMill i Q wate r (dilutio n 1:10)

. Afewsamplin g location s were dilute d 1:2 0 b ydilutin g 0.5m L ofsampl e wit h 9. 5 mL s o f H i Q water

. 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFBS , PFHS , an d PFO S usin g hig h perfomianc e liqui d chromatography/tande m mass spectrometr y(HPLC/MS/MS)

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

wdat a har

d copie s place d i n th e final data packet , an d ar e briefl ydescribe d below

.

Pag e 1 4 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

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 iVIas s Spectromete r io n Sourc e Electrod e Polarit y Softwar e ETSSta n ETS-8-044. 0 8/04/201 0 Agilen t 1100 Betasi l C1 8 (2, 1 m m X 100 mm) , 5 n Betasi l C1 8 (2, 1 m m X 100 mm) , 5) j

1 0 n L Applie d Biosystem s AP I 400 0 Turi wSpra

y Turt o io n electrod e Negativ e Analyst 1,4, 2 bIbMaryAn n ETS-8-044, 0 9/10/1 0 Agilen t 1100 Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n Betasi l C1 8 (2. 1 m m X 100 mm) , 5 n

2or10n L Applie d Biosystem s AP I 500 0 TurtD O Spra y TurtD o io n electrod e Negativ e Analyst 1,4, 2 Tabl e 4

. Liqui d Chromatograph yConditions

. ste p Numbe r Tota l Tim e

(min ) Flo wRat e

(fdJmin ) Percen t A

( 2 ir M ammoniu m acetate ) Percent B (Methanol ) 8/4/1 0 Analysi s 0 1 2 3 4 5 0

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

300 30 0 30 0 30 0 30 0 80, 0 80, 0 10, 0 10. 0 80, 0 80, 0 20, 0 20, 0 90, 0 90. 0 20, 0 20, 0 9/10/1 0 Analysi s 0 1 2 3 4 5 0

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

30 0 30 0 30 0 30 0 30 0 90, 0 90, 0 5, 0 5, 0 90, 0 90, 0 10, 0 10. 0 95, 0 95, 0 10, 0 10, 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 9 399/8 0 399/9 9 499/8 0 499/9 9 499/13 0 Dwel l tim e wa s 5 0 o r12 5 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 wa s use d fo rquantitation

.

Pag e 1 5 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



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

. Atota l offlfeen spike d standard s rangin g firam 0.02 5 ng/m L t o 100 ng/m L (nominal ) were analyzed

. Lo

wand/o rhig h curve points were disable d a s neede d t o mee t calibratio n acceptance criteria

. Aquadratic , 1/

xweighted , calibratio n curve ofth e pea k are a counts wa s use d t o fit th e data fo r eac h analyte

. Th e dat a were no t force d throug h zero durin g th e fitting process
. Calculatin g th e standar d concentration s usin g th e pea k are a confinne d accurac

yo feac h curve point

. PFOS : Th e calibratio n curve wa s constmcte d usin g th e linea risome rofPFO S only

. Since th e sample s were expecte d t o contai n bot h linea ran d branche d isomer s o fPFOS , LC S an d GLP10-01-02-0 6 sample s were quantitate d b yprocessin g th e PFO S linea ran d branche d isomer s separatel yan d summin g th e calculate d concentration s togethe rt o generat e th e final PFO S concentration

. Thi s wa s don e t o hel p minimiz e an ypotentia l analytica l bias du e t o quantitatin g linea ran d branche d isomer s of PFO S against a predominatel ylinea rreference standar d fo rPFOS

. 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

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

. 8. 2 Syste m Suitabilit y Acalibratio n standar

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

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

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

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

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

. Th e nomina l LOQ fo ral l analyte s ca n b e foun d i n Tabl e 6

. Tabl e 6

. Limi t o fQuantitatio n (LOQ)

. Analysi s Dat e 8/4/1 0

9/10/1 0 Dilutio n
1 1 0 2 0 1 20 0 PFB S

LOQ , ng/m L 0.025 5 0.25 5 0.51 0 0.030 6 NA PFH S

LOQ , ng/m L 0.10 3 1.0 3 2.0 6 0,103 NA PFO S

LOQ , ng/m L 0,25 5 2.5 5 5,1 0 N A 20, 4

Pag e 1 6 of6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

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 confin n that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control

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

. 

### 8. 5 Blank s Two type s ofblank

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

. Metho d blan k

results were reviewe d an d use d t o evaluat e metho d performance an d t o determin e th e LOQ 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 b yspikin g know n amounts o fth e analyt e into 4 0 m L ofMill i Q wate rt o produce th e desire d concentration

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

. Th e metho d acceptance criteri a state s that th e averag e ofLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D 220%

. 8/4/1 0 Analysis : Metho d acceptance criteri a wa s me t fo rth e PFBS , PFHS , an d th e mi d an d hig h set of linea rPFO S LC S samples

. Th e lo wset oflinea rPFO S LC S had a n averag e recover yo f12 1 %

. 9/10/1 0 Analysis : Metho d acceptance criteri a wa s met fo ral l thre e level s ofLC S fo rPFBS

. Th e mi d an d hig h LC S met metho d acceptance criteri a fo rPFH S an d PFOS

. Th e averag e recover yfo rth e lo

w set ofLC S fo rPFH S wa s 73.5 % an d no t calculate d fo rPFO S a s th e detecte d value s were <LOQ

. As th e reference material s use d fo rquantitatio n ofPFO S i s predominantl ylinear , an d th e PFO S presen t i n th e wate rsample s are comprise d o fbot h linea ran d branche d isomers , additiona l LC S sample s o f PFO S (linea ran d branched ) were prepare d a t thre e concentration s t o evaluat e th e potentia l fo r analytica l bias

. 8/4/1 0 Analysis : Th e low , mid , an d hig h set ofLC S (linea r+ branche d ) di d no t mee t metho d acceptance criteri a wit h a n averag e recover yo f166% , 128% , an d 14 1 % , respectively

. 9/10/1 0 Analysis : Th e mi d set o fLC S (linea r+ branched) , met metho d acceptance criteria , whil e th e lo w set (57.4% ) an d hig h set (123%) , di d no t mee t metho d acceptance criteria

. Base d o n th e recover

yo fth e linea ran d branche d PFO ALCS , i t i s th e opinio n ofth e laborator ythat th e recover ydiscrepenc

yofth e linea ran d branche d isomer s ofPFO Aindicate s a n analytica l bias

. Becaus e ofthi s bias , th e metho d uncertaint ywil l b e adjuste d t o 100 % ±4 1 % , base d o n th e highest recover yo f th e linea ran d branche d LCS , a t th e spik e leve l mos

t appropriat e a s compare d t o th e on-colum n concentration s ofPFO S detecte d i n th e samples

. I n thi s case , th e 3 0 pp b LC S (linea r+ branched ) analyze d o n 8/4/1 0 wit h a n averag e recover yof141%

. Ametho d deviatio n addressin g th e LC S recoverie s i s include d i n th e ra wdata package

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

.

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

y= * 100 % Spike Concentratio n LCS % RS D = ^'^"^^'•' ^

^^^'^''° " ^^ ^

^^P"^^^ ^

'100 % averag e LC S recover

y

Pag e 1 7 o f 6 7GLP10-01-02 ; interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 7

. Laborator yContro l Splic e Recovery

. ETS-8-044, 0 Analyze d 8/4/1 0

La b I D LCS-100726- 1 LCS-100726- 2 LCS-100726- 3 Averag e ±%RS D LCS-100726- 4 LCS-100726- 5 LCS-100726- 6 Averag e ±%RS D LCS-100726- 7 LCS-100726- 8 LCS-100726- 9 Averag e ±%RS D PFB S

Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 0.55 8 0.59 3 0.57 2 YoRecover

y 11 0 11 6 11 2 113 % ±2.7 % 5.1 0 5.1 0 5.1 0 4.5 9

5.6 4 5,6 4 90, 0

11 1 11 1 104 % ±12 % 30. 6 30. 6 30. 6 32. 1

32. 9 32, 4 10 5

10 7 10 6 106 % ±0.94 % PFH S Spike d Concentratio n (ng/mL ) 0,51 5 0,51 5 0,51 5 Calculate d

Concentratio n (ng/mL ) 0.51 3 0.61 3 0.53 1 YoRecover y 10 0 11 9 103 107 % ±9.7 % 5,1 5 5.1 5 5.1 5 4.7 0

5.6 3 5,8 4 91. 2

10 9 11 3 104 % ±11 % 30. 9 30. 9 30. 9 32, 6

33, 4 33. 4 10 6

10 8 10 8 107 % ±1.1 %

ETS-8-044. 0 Analyze d 8/4/1 0

La b I D LCS-100726- 1 LCS-100726- 2 LCS-100726- 3 Averag e ±%RS D LCS-100726^ LCS-100726- 5 LCS-100726- 6 Averag e ±%RS D LCS-100726- 7 LCS-100726- 8 LCS-100726- 9 Averag e ±%RS

D PFO S (linear ) Spike d Concentratio n (ng/mL ) 0,51 0 0,51 0 0,51 0 Calculate d

Concentratio n (ng/mL ) 0.59 0 0,65 2 0,61 3 YoRecover

y 11 6 12 8 12 0 121 % ±5.1%TM 5.1 0 5,1 0 5.1 0 4,6 7

5,7 0 5,8 1 91, 6

11 2 11 4 106 % ±12 % 30, 6 30, 6 30, 6 34. 5

34. 9 34, 9 11 3

11 4 11 4 114 % ±0.66 % La b I D LCS-100726-1 0 LCS-100726-1 1 LCS-100726-1 2 Averag e ±%RS D LCS-100726-1 3 LCS-100726-1 4 LCS-100726-1 5 Averag e ±%RS D LCS-100726-1 6 LCS-100726-1 7 LCS-100726-1 8 Averag e ±%RS D PFO S (linea r+ branched )

Spike d Concentratio n (ng/mL ) 0,50 0 0,50 0 0,50 0 Calculate d

Concentratio n (ng/mL ) 0.84 4 0,82 9 0,81 7 YoRecover

y 16 9 166 163 166 % ±1.6%TM 5,0 0 5.0 0 5,0 0 6,2 8

6,4 9 6,3 8 12 6

13 0 12 8 128 % ±1.6%TM 30, 0 30, 0 30, 0 42, 2

41, 9 43, 1 14 1

14 0 144 141 % ±1.5%

TM (1 ) Th e averag e recover ydi d not meet metho d acceptance criteri a o f100 % ±20% ,

Pag e 1 8 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 7 continued

. Laborator yContro l Spil< e Recovery

. ETS-8-044, 0 Analyze d 9/10/1 0

La b I D LCS-100910- 1 LCS-100910- 2 LCS-100910- 3 Averag e ±%RS D LCS-100910- 4 LCS-100910- 5 LCS-100910- 6 Averag e ±%RS D LCS-100910- 7 LCS-100910- 8 LCS-100910- 9 Averag e ±%RS D PFB S Spike d Concentratio n (ng/mL ) 0,20 4 0,20 4 0,20 4 Calculate d

Concentratio n (ng/mL ) 0,18 5 0,23 1 0,24 5 YoRecover y

90. 7 11 3 12 0 108 % ±14 % 5,1 0 5,1 0 5,1 0 5,1 7

5,7 9 5,4 3 10 1

11 3 10 6 107 % ±5.7 % 15. 3 15. 3 15. 3 14, 8

17. 3 17. 1 96, 9

11 3 11 1 107 % ±8.2 % PFH S Spike d Concentratio n (ng/mL ) 0,20 6 0,20 6 0,20 6 Calculate d

Concentratio n (ng/mL ) <0,10 3 0.14 4 0,15 9 YoRecover y

N A 69, 8 77, 1 73.5 % ±7.0% TM 5.1 5 5,1 5 5,1 5 5,2 0

5,7 7 5.4 5 10 1

11 2 10 6 106 % ±5.2 % 15, 5 15, 5 15, 5 14. 9

16. 6 16. 7 96, 1

10 7 10 8 104 % ±6.4 %
ETS-8-044, 0 Analyze d 9/10/1 0

La b I D LCS-100910- 1 LCS-100910- 2 LCS-100910- 3 Averag e ±%RS D LCS-100910- 4 LCS-100910- 5 LCS-100910- 6 Averag e ±%RS D LCS-100910- 7 LCS-100910- 8 LCS-100910- 9 Averag e ±%RS D PFO S (linear )

Spike d Concentratio n (ng/mL ) 0,20 4 0,20 4 0,20 4 Calculate d

Concentratio n (ng/mL ) <0.10 2 <0.10 2 <0.10 2 YoRecover y

N A N A N A N A 5.1 0 5.1 0 5.1 0 4.4 4

4.9 7 4.6 5 87. 1

97, 5 91, 1 91.9 % ±5.7 % 15. 3 15. 3 15, 3 13. 7

15. 5 16. 2 89, 5

10 1 10 6 98.8 % ±8.6 % La b I D LCS-100910-1 0 LCS-100910-1 1 LCS-100910-1 2 Averag e ±%RS D LCS-100910-1 3 LCS-100910-1 4 LCS-100910-1 5 Averag e ±%RS D LCS-100910-1 6 LCS-100910-1 7 LCS-100910-1 8 Averag e ±%RS D PFO S (linea r+ branched ) Spike d Concentratio n (ng/mL ) 0,49 5 0.49 5 0,49 5 Calculate d

Concentratio n (ng/mL ) 0.30 2 0.27 8 0,27 3 YoRecover y

60, 9 56, 2 55, 2 57.4 % ±5.3 % '^

' 4.9 5 4,9 5 4,9 5 4,9 2

5,0 2 5,8 1 99, 3

10 1 11 7 106 % ±9.2 % 14, 8 14, 8 14, 8 17, 8

18, 3 18, 3 12 0

12 4 12 4 123 % ±1.9% TM (1 ) Th e averag e recover ydi d no t mee t metho d acceptance criteri a of100 % ±20% , 8. 7 Analytica l Metho d Uncertaint y Analytica l uncertaint

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

yan d precision

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

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

. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto ro

f2 , whic h con-espond s t o a confidence leve l o f95%

. Th e mos

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

yvalue s liste d i n Tabl e 7 fo rPFB S an d PFHS

. Fo rPFOS , th e analytica l uncertaint y

Pag e 1 9 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

wa s determine d base d o n th e qualit ycontro l data generate d wit h th e projec t sample s (Tabl e 6) an d wa s use d t o evaluat e metho d accurac yan d precision

. Du e t o th e analytica l hig h bias observe d durin g th e quantitatio n ofth e linea r+ branche d PFO S against a calibratio n curve constmcte d fro m th e analysi s ofcalibratio n standard s containin g linea rPFO S only , a n analytica l uncertaint yof4 1 % i s applie d t o al l PFO S sampl e results fo rthi s project

. Tabl e 8

. Analytica l Uncertainty

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

10. 6 11. 6 NA<^ > Metho d

Uncertaint y 100%±21 % 100%±23 % 100%±41 % (1 ) N A= No

t Applicable , Se e sectio n 8, 6 ofth e repor t fo ra discussio n o n th e assignin g o fth e 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 were collecte d a t eac h samplin g poin t t o verif ythat th e analytica l metho d i s applicabl e t o th e collecte d matrix

. Fiel d matri xspike s were generate d b yaddin g a measure d volum e offiel d sampl e t o a containe rspike d b yth e laborator

ywit h PFB S (linear) , PFH S (linear) , an d PFO S (linear

) prio rt o shippin g sampl e container s fo rsampl e collection

. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of100±30 % confim n that "unknown " components i n th e sampl e matri x d o no t significantl yinterfere wit h th e extractio n an d analysi s ofth e analyte s o finterest

. Fiel d matri xspik e concentration s must b e 50 % ofth e sampl e concentratio n t o b e considere d a n appropriat e fiel d spike

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

. Th e nomina l spike leve l fo rth e lo wfiel d matri xspik

e wa s 1. 0 ng/mL , th e mi d fiel d matri xspik e wa s 1 0 ng/mL , an d th e hig h fiel d mari xspik e wa s 100 ng/m L fo ral l samplin g locations

. Fo rsom e samplin g locations , th e hig h fiel d matri xspik e was no t appropriat e a s compare d t o th e sampl e concentration

. Fiel d matri xspik

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

.
(Sampl e Concentratio no f FM S - Averag e Concentratio n: Fiel dSampl e & Fiel dSampl e Dup ) „,„„„ , FM S Recover y = -^

^ 2 £ : : : £Li

. • i oo % Spik e Concentrato n
8. 9 Laborator yMatri xSpike s (LMS ) Sample s were analyze d unde rprojec t GLP10-01-01-0 6 fo rPFOA

. Results fro m that analysi s foun d that th e hig h FM S leve l wa s no t sufficien t fo rsevera l ofth e surface wate rsamplin g location s fo rPFOA

. Since i t wa s presume d that th e level s ofPFO S i n thes e sample s woul d b e simila rt o th e PFO Aresults , laborator ymatri xspike s were prepare d fo rGLP10-01-01-0 6 were analyze d instead ofth e FM S sample s prepare d wit h th e sampl e set

. Laborator ymatri xspik

e were prepare d an d analyze d fo rth e followin g sampl e locations : 200pp b LMS : DA L S WSW01 , DA L S WSW04 , DA L SWSW05 , an d DA L S WSW08 , 400pp b LMS ; DA L S WSW1 0 an d DA L S WSW11 , 500pp b LMS ; DA L SWSW09 , an d 1500pp b LMS ; DA L G WGP0 7 an d DA L G WGP0 8 Laborator ymatri xspike recoverie s withi n metho d acceptance criteri a of100±30 % confir m 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 analysis

.

Pag e 2 0 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

.„„ „ (LM S Sampl e Conc^entratio n - Averag e Concentration : Sampl e & Sampl e Pup,)«..pno / LM S Spik e Concentrato n 

### 9 Dat a SummaiyXanB'Disci^ ^
Th e table s belowsummariz e th e sampl e results an d fiel d matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blanks

. Results an d averag e value s ar e rounde d t o thre e significan t figure s accordin g t o EP Aroundin g rules

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

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

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

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

.

Pag e 2 1 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tables

. DALSWSW0 1 10062 3

3 M LIM S I D GLP10-01-02-06-03 5 GLP10-01-02-06-03 6 GLP10-01-02-06-03 7 GLP10-01-02-06-03 8 GLP10-01-02-06-03 9 GLP10-01-02-06-03 6 LM S Descriptio n DALSWSW0 1 0 10062 3 DALSWSW0 1 D B 10062 3 DALSWSW0 1 L S 10062 3 DA L S WSW0 1 M S 10062 3 DALSWSW0 1 H S 10062 3 DA L S WSW0 1 D B - 200pp b LM S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 15. 3 14. 7 NA' " NA' " NA' " 24 6 YoRecover

y N A N A NA' " NA' " NA' " 11 3 15. 0 ng/m L ±4.0Y

o PFH S Concentratio n (ng/mL ) 11 9 12 1 NA' " NA' " NA' " 34 5 YoRecover

y N A N A NA' " NA' " NA' " 10 9 12 0 ng/m L ±1.r/ o PFO S Concentratio n (ng/mL ) 24 3 25 3 NA' " NA' " NA' " 50 5 YoRecover

y N A N A NA' " NA' " NA' " 12 6 24 8 ng/m L ±4.0Y

o N A= No t Applicabl e (1 ) Tti e sampl e wa

s no t analyzed

. Tabl e 10

. DA L SWSW0 2 10062 2

3 M LIM S I D GLP10-01-02-06-03 0 GLP10-01-02-06-03 1 GLP10-01-02-06-03 2 GLP10-01-02-06-03 3 GLP10-01-02-06-03 4 Descriptio n DA L SWSW0 2 0 10062 2 DA L S WSW0 2 D B 10062 2 DA L SWSW02L S 10062 2 DA L S WSW0 2 LS 10062 2 DA L S WSW0 2 H S 10062 2 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 7.4 8 7.8 7 NA' " NA' " 11 9 YoRecover

y N A N A NA' " NA< " 10 9 7.6 8 ng/m L tS.IY o PFH S Concentratio n (ng/mL ) 51. 9 52. 0 NA< " NA< " 16 1 YoRecover

y N A N A NA< " NA< " 10 6 52. 0 ng/m L ±0.19Y

o PFO S Concentratio n (ng/mL ) 22 1 20 5 NA' " NA' " 30 7 YoRecover

y N A N A NA< " NA< " 92. 4 21 3 ng/m L ±7.7Y

o NA= No t Applicabl e (1 ) Tti e sampl e was no

t analyzed

.

Pag e 2 2 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 11

. DA L S WSW0 3 10062 2

3 M LIM S I D GLP10-01-02-06-02 1 GLP10-01-02-06-02 2 GLP10-01-02-06-02 3 GLP10-01-02-06-02 4 GLP10-01-02-06-02 5 Descriptio n DA L SWSW0 3 0 10062 2 DA L SWSW03D B 10062 2 DA L SWSW03L S 10062 2 DA L S WSW0 3 M S 10062 2 DA L SWSW03H S 10062 2 Averag e Concentratio n (ng/mL ) ±%RP D PFB S Concentratio n (ng/mL ) 9.5 1 9.6 2 NA' " NA' " 12 0 YoRecover

y N A N A NA' " NA' " 10 8 9.5 7 ng/m L ±1.2 % PFH S Concentratio n (ng/mL ) 71. 4 72. 9 NA' " NA< " 184 YoRecover

y N A N A NA< " NA< " 10 9 72. 2 ng/m L ±2.1Y

o PFO S Concentratio n (ng/mL ) 19 6 19 8 NA< " NA< " 27 8 YoRecover

y N A N A NA< " NA< " 80. 1 19 7 ng/m L ±1.1Y

o NA = No t Applicabl e (1 ) Tti e sampl e was no

t analyzed

. Tabl e 12

. DA L S WSW0 4 10062 2

3 M LIM S I D GLP10-01-02-06-01 6 GLP10-01-02-06-01 7 GLP10-01-02-06-01 8 GLP10-01-02-06-01 9 GLP10-01-02-06-02 0 GLP10-01-02-06-017 ; LM S

Averag e Conce n Descriptio n

DA L SWSW0 4 0 10062 2 DA L S WSW0 4 D B 10062 2 DA L S WSW0 4 LS 10062 2 DA L SWSW0 4 M S 10062 2 DA L SWSW04H S 10062 2 DA L S WSW0 4 D B - 200pp b LM S ti^on (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 14. 1 13. 3 NA' " NA' " NA' " 23 0 YoRecover

y N A N A NA' " NA' " NA' " 10 6 13. 7 ng/m L ±5.8Y

o PFH S Concentratio n (ng/mL ) 87. 3 85. 6 NA' " NA' " NA' " 32 0 YoRecover

y N A N A NA' " NA' " NA' " 11 3 86. 5 ng/m L ±2.0 % PFO S Concentratio n (ng/mL ) 19 0 19 4 NA' " NA' " NA' " 41 3 %Recover

y N A N A NA' " NA' " NA' " 10 8 19 2 ng/m L ±2.r/ o NA= No t Applicabl e (1 ) TTi e sampl e wa s no

t analyzed

.

Pag e 2 3 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 13

. DA L SWSW0 5 10062 2

3 M LIM S I D GLP10-01-02-06-01 1 GLP10-01-02-06-01 2 GLP10-01-02-06-01 3 GLP10-01-02-06-01 4 GL P 10-01-02-06-01 5 GLP10-01-02-06-012 ; LM S

Averag e Conce n Descriptio n

DA L SWSW0 5 0 10062 2 DA L S WSW0 5 D B 10062 2 DA L SWSW05L S 10062 2 DA L SWSW0 5 M S 10062 2 DA L S WSW0 5 H S 10062 2 DA L S WSW0 5 D B - 200pp b LM S tratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 21. 1 20. 7 NA' " NA' " NA' " 24 7 %Recover

y N A N A NA' " NA' " NA' " 11 1 20. 9 ng/m L ±1.9Y

o PFH S Concentratio n (ng/mL ) 104 100 NA' " NA' " NA' " 32 7 YoRecover

y N A N A NA' " NA' " NA' " 10 9 102 ng/m L ±3.9Y

o PFO S Concentratio n (ng/mL ) 39 9 38 5 NA< " NA< " NA< " 61 5 YoRecover

y N A N A NA' " NA' " NA' " 10 9 39 2 ng/m L ±3.6Y

o NA= No t Applicatil e (1 ) Th e sampl e was no

t analyzed

. Tabl e 14

. DA L S WSW0 6 10062 2

3MUMSI D GLP10-01-02-06-00 6 GLP10-01-02-06-00 7 GLP10-01-02-06-00 8 GL P 10-01-02-06-00 9 GL P 10-01-02-06-01 0 Averag e Concen t Descriptio n

DA L SWSW0 6 0 10062 2 DA L SWSW06D B 10062 2 DA L SWSW06L S 10062 2 DA L SWSW0 6 M S 10062 2 DA L S WSW0 6 H S 10062 2 ratio n (ng/mL ) ±YoRP D PFB S (ng/mL ) 17. 8 17. 0 NA' " NA' " 13 1 YoRecover

y N A N A NA< " NA< " 11 1 17. 4 ng/m L ±4.6Y

o PFH S Concentratio n (ng/mL ) 77. 8 77. 2 NA' " NA' " 19 0 YoRecover

y N A N A NA' " NA' " 10 9 77. 5 ng/m L ±0.77Y

o PFO S Concentiatio n (ng/mL ) 22 9 22 7 NA< " NA' " 32 5 YoRecover

y N A N A NA< " NA< " 95. 3 22 8 ng/m L ±1.1Y

o NA= No t Applicabl e (1 ) Th e sampl e was not analyzed

.

Pag e 2 4 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 15

. DA L SWSW0 7 10062 2

3 M LIM S I D GLP10-01-02-06-00 1 GLP10-01-02-06-00 2 GLP10-01-02-06-00 3 GLP10-01-02-06-00 4 GLP10-01-02-06-00 5 Averag e Concen t Descriptio n

DA L SWSW0 6 0 10062 2 DA L SWSW06D B 10062 2 DA L S WSW0 6 L S 10062 2 DA L SWSW0 6 M S 10062 2 DA L SWSW06H S 10062 2 ratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 10. 8 10. 8 NA< " NA< " 12 9 YoRecover y

N A N A NA' " NA' " 11 6 10. 8 ng/m L ±0.0Y o PFHSf^ ^ Concentratio n (ng/mL ) 47. 6 48. 1 NA' " NA' " 174 YoRecover y

N A N A NA< " NA< " 12 2 47. 9 ng/m L ±1.0Y o PFO S Concentratio n (ng/mL ) 12 8 13 1 NA' " NA' " 22 2 YoRecover y

N A N A NA' " NA' " 90. 8 129ng/mL±2.2y o N A= No t Applicabl e (1 ) Tti e sampl e was no

t analyzed

. Tabl e 16

. DA L S WSWO B 10062 3

3 M LIM S I D GLP10-01-02-06-04 5 GLP10-01-02-06-04 6 GLP10-01-02-06-04 7 GLP10-01-02-06-04 8 GLP10-01-02-06-04 9 GLP10-01-02-06-046 ; LM S Descriptio n DA L SWSW0 8 0 10062 3 DA L SWSW08D B 10062 3 DA L SWSW08L S 10062 3 DA L S WSW0 8 M S 10062 3 DA L SWSW08H S 10062 3 DA L S WSW0 8 D B - 200pp b LM S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 39. 8 41. 5 NA< " NA' " NA' " 26 4 YoRecover y

N A N A NA' " NA' " NA' " 10 9 40. 7 ng/m L ±4.2 % PFH S Concentratio n (ng/mL ) 16 9 16 3 NA' " NA' " NA' " 39 2 YoRecover y

N A N A NA' " NA' " NA' " 11 0 16 6 ng/m L ±3.6Y o PFO S Concentratio n (ng/mL ) 26 8 26 3 NA' " NA' " NA' " 50 4 YoRecover y

N A N A NA' " NA' " NA' " 11 7 26 6 ng/m L ±1.9Y o NA = No t Applicabl e (1 ) Th e sampl e wa s no

t analyzed

.

Pag e 2 5 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 17

. DA L SWSW0 9 10062 3

3 M LIM S I D GLP10-01-02-06-05 0 GLP10-01-02-06-05 1 GLP10-01-02-06-05 2 GLP10-01-02-06-05 3 GLP10-01-02-06-05 4 GLP10-01-02-06-051;LM S

Averag e Conce r Descriptio n

DA L SWSW0 9 0 10062 3 DA L SWSW09D B 10062 3 DA L SWSW09L S 10062 3 DA L S WSW0 9 M S 10062 3 DA L SWSW09H S 10062 3 DA L S WSW0 9 D B - 500pp b LM S rtration (ng/mL ) ±YoRPD PFB S Concentratio n (ng/mL ) 27 5 28 2 NA' " NA' " NA' " 80 8 YoRecover

y N A N A NA< " NA< " NA' " 104 27 9 ng/m L ±2.5Y

o PFH S Concentratio n (ng/mL ) 67 2 61 4 NA' " NA' " NA' " 120 0 YoRecover

y N A N A NA' " NA' " NA' " 10 8 64 3 ng/m L ±9.0 % PFO S Concentratio n (ng/mL ) 38 6 37 8 NA< " NA< " NA< " 96 0 %Recover

y N A N A NA' " NA' " NA' " 11 3 38 2 ng/m L ±2.1 % N A= No t Applicabl e (1 ) Th e sampl e was no

t analyzed

. Tabl e 18

. DA L SWSW1 0 10062 3

3 M LIM S I D GL P 10-01-02-06-06 0 GLP10-01-02-06-06 1 GLP10-01-02-06-06 2 GLP10-01-02-06-06 3 GLP10-01-02-06-06 4 GLP10-01-02-06-061;LM S

Averag e Conce r Descriptio n

DA L SWSW1 0 0 10062 3 DA L SWSW10D B 10062 3 DA L S WSW1 0 LS 10062 3 DA L SWSW1 0 M S 10062 3 DA L SWSW10H S 10062 3 DA L S WSW1 0 D B - 400pp b LM S rtration (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 23. 0 22. 0 NA' " NA' " NA' " 42 0 YoRecover

y N A N A NA' " NA' " NA' " 97. 4 22. 5 ng/m L ±4.4 % PFH S Concentratio n (ng/mL ) 23 6 23 0 NA' " NA' " NA' " 66 1 YoRecover

y N A N A NA' " NA' " NA' " 104 23 3 ng/m L ±2.6 % PFO S Concentratio n (ng/mL ) 38 7 39 1 NA' " NA< " NA' " 80 5 YoRecover

y N A N A NA' " NA' " NA< " 102 38 9 ng/m L ±1.0 % N A= No t Applicabl e (1 ) Th e sampl e was no

t analyzed

.

Pag e 2 6 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 19

. DA L SWSW1 1 10062 3

3 M LIM S I D GLP10-01-02-06-05 5 GLP10-01-02-06-05 6 GLP10-01-02-06-05 7 GLP10-01-02-06-05 8 GLP10-01-02-06-05 9 GLP10-01-02-06-056 ; LM S Descriptio n DALSWSW1 1 0 10062 3 DALSWSW1 1 D B 10062 3 DALSWSW1 1 LS 10062 3 DALSWSW1 1 M S 10062 3 DA L S WSW1 1 H S 10062 3 DALSWSW1 1 D B -500ppbLM S Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 10 3 10 0 NA' " NA' " NA' " 64 1 YoRecover

y N A N A NA' " NA' " NA' " 10 6 102 ng/m L ±3.0 % PFH S Concentratio n (ng/mL ) 112 0 113 0 NA< " NA' " NA< " 183 0 - YoRecover

y N A N A NA< " NA' " NA' " N O 1130ng/mL±0.89Yo^

^ PFO S Concentratio n (ng/mL ) 86 3 83 6 NA' " NA' " NA< " 140 0 YoRecover

y N A N A NA' " NA' " NA' " 10 8 85 0 ng/m L ±3.2 % NA = No t Applicabl e N C = No t Calculated ; Endogenou s concentratio n greate rtha n 2 xspik e level

. (1 ) Th e sampl e wa s no

t analyzed

. (2 ) Samplin g locatio n di d no t hav e a n appropriate fiel d matri xspik e level

.

Pag e 2 7 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 20

. DA L SWSW1 2 10062 3

3 M LIM S I D GLP10-01-02-06-04 0 GLP10-01-02-06-04 1 GLP10-01-02-06-04 2 GLP10-01-02-06-04 3 GLP10-01-02-06-04 4 Averag e Conceir t Descriptio n

DA L SWSW1 2 0 10062 3 DA L SWSW12D B 10062 3 DA L S WSW1 2 LS 10062 3 DA L SWSW1 2 M S 10062 3 DA L SWSW12H S 10062 3 ratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 0.77 3 0.75 5 NA< " 12. 4 11 4 YoRecover

y N A N A NA' " 11 4 11 1 0.764 ng/m L ±2.4 % PFH S Concentratio n (ng/mL ) 3.6 9 3,6 7 NA' " 15. 3 11 3 YoRecover

y N A N A NA< " 11 3 10 6 3.6 8 ng/m L ±0.54 % PFO S Concentratio n (ng/mL ) 10 3 10 5 NA' " 11 8 16 8 YoRecover

y N A N A NA< " N C 63.5'^ ' 10 4 ng/m L ±2.0Y

o N A= No t Applicabl e N C = No t Calculated ; Endogenou s concentratio n greate rtha n 2 xspike level

. (1 ) Th e sampl e wa s no

t analyzed

. (2 ) Fiel d matri xspik

e di d no t mee t metho d acceptance criteri a o f100 % ±30%

. Tabl e 21

. DA L GWGP0 1 10070 9

3 M LIM S I D GLP10-01-02-06-07 0 GLP10-01-02-06-07 1 GLP10-01-02-06-07 2 GLP10-01-02-06-07 3 GLP10-01-02-06-07 4 Averag e Concen t Descriptio n

DALGWGP0 1 0 100700 9 DALGWGP0 1 D B 10070 9 DALGWGP0 1 LS 10070 9 DALGWGP0 1 M S 10070 9 DALGWGP0 1 H S 10070 9 ratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 5.0 1 5.0 2 6.6 0 17. 1 12 3 5.02 ng/ m YoRecover

y NA NA N C 11 8 11 6 L±0.20Y o PFH S

Concentratio n (ng/mL ) 7.4 9 7.2 2 9.3 3 19. 5 12 1 YoRecover

y N A N A N C 11 8 11 0 7.36 ng/m L ±3.7Y

o PFO S Concentratio n (ng/mL ) 26. 9 25. 5 NA< " NA' " 11 5 YoRecover

y N A N A NA< " NA< " 87. 3 26. 2 ng/m L ±5.3 % NA = No t Applicabl e (1 ) Th e sampl e wa s no

t analyzed

.

Pag e 2 8 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 22

. DA L G WGP0 2 10070 9

3 M LIM S I D GLP10-01-02-06-07 5 GLP10-01-02-06-07 6 GLP10-01-02-06-07 7 GLP10-01-02-06-07 8 GLP10-01-02-06-07 9 Descriptio n DA L GWGP0 2 0 100700 9 DA L GWGP02D B 10070 9 DA L GWGP02L S 10070 9 DA L G WGP0 2 M S 10070 9 DA L GWGP02H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 19. 7 22. 4 NA< " NA< " 134 YoRecover

y N A N A NA' " NA' "

. Il l 21. 1 ng/m L ±13% , PFH S Concentratio n (ng/mL ) 10. 4 11. 9 NA' " NA' " 12 7 YoRecover

y N A N A NA' " NA< " 11 2 11. 2 ng/m L ±13 % PFO S Concentratio n (ng/mL ) 15. 7 19. 3 NA' " NA' " 87. 6 YoRecover

y N A N A NA' " NA< " 68.7'^ ' 17. 5 ng/m L ±20 % NA = Not Applicabl e (1 ) Th e sampl e wa s no

t analyzed

. (2 ) Fiel d matrixspik

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

. Tabl e 23

. DA L GWGP0 3 10070 9

3 M LIM S I D GLP10-01-02-06-08 0 GLP10-01-02-06-08 1 GLP10-01-02-06-08 2 GLP10-01-02-06-08 3 GL P 10-01-02-06-08 4 Descriptio n DA L GWGP0 3 0 100700 9 DA L GWGP03D B 10070 9 DA L G WGP0 3 L S 10070 9 DA L G WGP0 3 M S 10070 9 DALGWGP03H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 66. 2 66. 5 NA' " NA< " 18 0 YoRecover

y N A N A NA' " NA< " 11 1 66. 4 ng/m L ±0.45 % PFH S Concerrtratio n (ng/mL ) 41 3 41 2 NA' " NA' " 57 1 YoRecover

y NA NA NA' " NA' " N C 41 3 ng/m L ±0.24%' ^ PFO S Concerrtratio n (ng/mL ) 34 1 40 5 NA< " NA< " 67 8 YoRecover

y N A N A NA' " NA< " N C 37 3 ng/m L ±17%' ^ NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Th e sampl e was no

t analyzed

. (2 ) Samplin g locatio n di d no t hav e a n appropriate field matri xspike leve l fo rPFH S o rPFOS

.

Pag e 2 9 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s firo m Decatur , A L June/Jul y201 0

Tabl e 24

. DA L G WGP0 4 10070 9

3 M LIM S I D GLP10-01-02-06-08 5 GLP10-01-02-06-08 6 GLP10-01-02-06-08 7 GLP10-01-02-06-08 8 GLP10-01-02-06-08 9 Descriptio n DA L G WGP0 4 0 100700 9 DA L GWGP04D B 10070 9 DA L G WGP0 4 LS 10070 9 DA L GWGP0 4 M S 10070 9 DA L GWGP04H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concerrtratio n (ng/mL ) 19. 1 19. 1 NA' " NA' " 13 6 YoRecover

y N A N A NA< " NA< " 11 5 19. 1 ng/m L ±0.0 % PFH S Concentratio n (ng/mL ) 89. 5 82. 1 NA' " NA' " 23 2 %Recover

y N A N A NA' " NA< " 142(2 ) 85. 8 ng/m L ±8.6%'' ' PFO S Concentratio n (ng/mL ) 17 5 13 0 NA< " NA< " 29 6 YoRecover

y N A N A NA' " NA< " 14 1 '^ ' 152ng/mL±30Yo''- ^ NA = No t Applicabl e (1 ) Th e sampl e was no

t analyzed

. (2 ) Fiel d matri xspik

e di d no t mee t metho d acceptance criteri a o f100 % ±30%

. (3) Th e analytica l unceitaint yhas bee n adjuste d fo rfield matri xspik e recovet yt o 100 % ±42 % fo rPFH S an d 100 % ±4 1 % fo rPFOS

. (4 ) Th e sample/sampl e duplicate RP D di d no t meet metho d acceptance criteri a of<20%

.

Pag e 3 0 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 25

. DA L G WGP0 5 10070 9

3 M LIM S I D GLP10-01-02-06-09 0 GLP10-01-02-06-09 1 GLP10-01-02-06-09 2 GLP10-01-02-06-09 3 GLP10-01-02-06-09 4 Descriptio n DA L GWGP0 5 0 100700 9 DA L GWGP05D B 10070 9 DA L GWGP05L S 10070 9 DA L GWGP0 5 M S 10070 9 DA L GWGP05H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (rig/mL ) 30. 0 30. 0 NA' " NA' " 14 1 YoRecover

y N A N A NA' " NA' " 10 9 30. 0 ng/m L ±0.0 % PFH S Concentratio n (ng/mL ) 162 15 3 NA' " NA' " 28 0 YoRecover

y N A N A NA' " NA' " 11 9 15 8 ng/m L ±5.r/ o PFO S Concerrtratio n (ng/mL ) 41 6 34 7 NA< " NA< " 51 5 YoRecover

y N A N A NA< " NA< " N C 382ng/mL±18Yo' ^
NA = No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Th e sampl e wa s no

t analyzed

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

. Tabl e 26

. DA L G WGP0 7 10070 9

3MUMSI D GL P 10-01-02-06-09 5 GLP10-01-02-06-09 6 GLP10-01-02-06-09 7 GLP10-01-02-06-09 8 GLP10-01-02-06-09 9 GLP10-01-02-06-09 5 LM S

Averag e Concen t Descriptio n

DA L GWGP0 7 0 100700 9 DALGWGP07D B 10070 9 DA L GWGP07L S 10070 9 DA L GWGP0 7 M S 10070 9 DA L G WGP0 7 H S 10070 9 DA L GWGP0 7 0 ; 1500pp b LM S 'ratio n (ng/mL ) ±YoRPD PFB S Concentratio n (ng/mL ) 20. 3 21. 1 NA' " NA' " 137 NA' " YoRecover

y N A N A NA< " NA' " 11 4 NA' " 20. 7 ng/m L ±3.9 % PFH S Concentratio n (ng/mL ) 17 3 16 8 NA< " NA< " 29 8 NA< " YoRecover

y N A N A NA' " NA' " 12 4 NA' " 17 1 ng/m L ±2.9 % PFO S Concentratio n (ng/mL ) MA O 182 0 NA' " NA' " NA' " 366 0 YoRecover

y N A N A NA' " NA' " NA' " 12 3 178 0 ng/m L ±4.5 %
N A= No t Applicabl e (1 ) Th e sampl e wa s no

t analyzed

.

Pag e 3 1 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 27

. DA L G WGP0 8 10070 9

3 M LIM S I D GLP10-01-02-06-10 0 GLP10-01-02-06-10 1 GLP10-01-02-06-10 2 GLP10-01-02-06-10 3 GLP10-01-02-06-10 4 GLP10-01-02-06-100LM S

Averag e Concen t Descriptio n

DA L G WGP0 8 0 100700 9 DA L GWGP08D B 10070 9 DA L GWGP08L S 10070 9 DA L GWGP0 8 M S 10070 9 DA L GWGP08H S 10070 9 DA L GWGP0 8 0 ; ISOOpp b LM S tatio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 6.3 9 6.3 2 NA' " NA' " 11 8 NA< " YoRecover

y NA NA NA< " NA' " 10 9 NA' " 6.36 ng/m L ±1.1 % PFH S Concerrtratio n (ng/mL ) 67. 4 72. 9 NA' " NA' " 17 3 NA< " YoRecover

y NA N A NA' " NA' " 99. 9 NA' " 70. 2 ng/m L ±7.8 % PFO S Concentratio n (ng/mL ) 138 0 145 0 NA' " NA' " NA' " 321 0 YoRecover

y N A N A NA' " NA' " NA< " 11 7 142 0 ng/m L ±4.9 %
N A= No t Applicabl e (1 ) Th e sampl e was not analyzed

. Tabl e 28

. DA L G WGP0 9 10070 9

3 M LIM S I D GLP10-01-02-06-10 5 GLP10-01-02-06-10 6 GLP10-01-02-06-10 7 GLP10-01-02-06-10 8 GLP10-01-02-06-10 9 Descriptio n DA L GWGP0 9 0 100700 9 DA L GWGP09D B 10070 9 DA L GWGP0 9 L S 10070 9 DA L G WGP0 9 M S 10070 9 DA L GWGP09H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 20. 9 20. 5 NA< " NA' " 12 8 YoRecover

y N A N A NA< " NA< " 105 20. 7 ng/m L ±1.9 % PFH S Concentratio n (ng/mL ) 33. 7 38. 3 NA' " NA< " 14 7 YoRecover

y N A N A NA' " NA' " 10 8 36. 0 ng/m L ±13Y

o PFO S Concentratio n (ng/mL ) 79. 9 11 1 NA' " NA< " 18 8 YoRecover

y N A N A NA' " NA' " 90. 6 95. 5 ng/m L ±33%' ^
N A= No t Applicabl e (1 ) Th e sampl e wa

s not analyzed

. (2 ) Th e sample/sampl e duplicate RP D di d no t mee t metho d acceptance criteri a o f<20%

.

Pag e 3 2 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 29

. DA L G WGP1 0 10070 9

3 M LIM S I D GLP10-01-02-06-11 0 GLP10-01-02-06-11 1 GLP10-01-02-06-11 2 GLP10-01-02-06-11 3 GLP10-01-02-06-11 4 Descriptio n DA L GWGP1 0 0100700 9 DA L GWGP10D B 10070 9 DA L GWGP10L S 10070 9 DA L GWGP1 0 M S 10070 9 DA L GWGP10H S 10070 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concerrtratio n (ng/mL ) 44 1 45 2 NA' " NA' " 54 1 YoRecover

y N A N A NA' " NA' " N C 44 7 ng/m L ±2.5Yo' ^ PFH S Concerrtratio n (ng/mL ) A l l 41 3 NA< " NA< " 53 2 YoRecover

y N A N A NA' " NA' " N C 420ng/mL±3.3Yo ^ PFO S Concentratio n (ng/mL ) 14 6 107 NA' " NA< " 20 0 YoRecover

y N A N A NA' " NA' " 72. 1 12 7 ng/m L ±31%'' '
N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. (1 ) Th e sampl e wa

s no t analyzed

. (2 ) Samplin g locatio n di d not hav e a n appropriate field matri xspik e leve l fo rPF S o rPFHS

. (3 ) Th e sample/sampl e duplicat e RP D di d not mee t metho d acceptance criteri a of<20%

. Tabl e 30

. DA L GWGP1 1 10070 8

3 M LIM S I D GLP10-01-02-06-11 5 GLP10-01-02-06-11 6 GLP10-01-02-06-11 7 GLP10-01-02-06-11 8 GLP10-01-02-06-11 9 Descriptio n DALGWGP1 1 0 100700 8 DALGWGP1 1 D B 10070 8 DALGWGP1 1 LS 10070 8 DALGWGP1 1 M S 10070 8 DALGWGP1 1 H S 10070 8 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 65. 9 68. 0 NA< " NA< " 18 1 YoRecover

y N A N A NA' " NA' " 11 2 67. 0 ng/m L ±3.1 % PFH S Concentratio n (ng/mL ) 32 7 33 3 NA' " NA< " 48 6 YoRecover

y N A N A NA' " NA' " N C 33 0 ng/m L ±1.8

% ( ^ PFO S Concentratio n (ng/mL ) 64 0 68 0 NA' " NA' " 107 6 YoRecover

y N A N A NA' " NA' " N C 66 0 ng/m L ±6.1%' ^ N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspike level

. (1 ) Th e sampl e was no

t analyzed

. (2 ) Samplin g locatio n di d not hav e a n appropriate field matri xspik e leve l fo rPF S o rPFHS

.

Pag e 3 3 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 31

. DA L GWGP1 2 10070 8

3 M LIM S I D GLP10-01-02-06-12 0 GLP10-01-02-06-12 1 GLP10-01-02-06-12 2 GLP10-01-02-06-12 3 GLP10-01-02-06-12 4 Descriptio n DA L GWGP1 2 0 100700 8 DALGWGP12D B 10070 8 DALGWGP12L S 10070 8 DA L G WGP1 2 M S 10070 8 DALGWGP12H S 10070 8 Averag e Concentratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 1.8 4 3.3 3 3.9 2 14. 4 11 7 YoRecover

y N A N A N C 11 6 11 2 2.5 9 ng/m L ±58%' ^ PFH S Concentratio n (ng/mL ) 8.7 8 13. 7 13. 8 24. 4 12 6 YoRecover

y N A NA N C 12 8 11 1 11. 2 ng/m L ±44%' ^ PFO S Concentratio n (ng/mL ) 32. 4 65. 1 NA' " NA' " 148 YoRecover

y N A N A NA' " NA' " 96. 9 48.8ng/mL±67Yo' ^ N A= Not Applicabl e (1 ) Th e sampl e was no

t analyzed

. (2 ) Th e sample/sampl e duplicat e RP D di d no t meet metho d acceptance criteri a ofs20%

. Tabl e 32

. DA L G W216 R 10071 6

3 M LIM S I D GLP10-01-02-06-13 0 GLP10-01-02-06-13 1 GLP10-01-02-06-13 2 GLP10-01-02-06-13 3 GLP10-01-02-06-13 4

Averag e Concen t Descriptio n

DA L GW216 R 0 100701 6 DALGW216RD B 10071 6 DA L GW216RL S 10071 6 DA L GW216 R M S 10071 6 DALGW216RH S 10071 6 "ratio n (ng/mL ) ±YoRP D PFB S Concentratio n (ng/mL ) 10. 5 10. 7 NA< " NA< " 11 8 YoRecover

y N A N A NA< " NA< " 10 5 10.6ng/mL±1.9 % PFH S Concentratio n (ng/mL ) 30. 9 30. 0 NA' " NA' " 14 1 YoRecover

y N A NA NA' " NA' " 107 30. 5 ng/m L ±3.0 % PFO S Concentratio n (ng/mL ) 11 4 12 5 NA' " NA' " 192 YoRecover

y N A N A NA' " NA' " 71. 6 11 9 ng/m L ±9.Z'/

o NA= Not Applicabl e (1 ) Th e sampl e was no

t analyzed

.

Pag e 3 4 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 33

. Tri p Blan k

3 M LIM S I D GLP10-01-02-06-02 6 GLP10-01-02-06-02 7 GLP10-01-02-06^2 8 GLP10-01-02-06-02 9 GLP10-01-02-06-06 6 GLP10-01-02-06-06 7 GLP10-01-02-06-06 8 GLP10^1-02-06-06 9 GLP10-01-02-06-12 5 GLP10-01-02-06-12 6 GLP10-01-02-06-12 7 GLP1(W)1-02-06-128 ( Descriptio n DA L SWTRIP 1 010062 2 DA L SWTRIP1L S 10062 2 DALSWTRIP 1 M S 10062 2 DA L SWTRIP1H S 10062 2 DALGWTRIP 1 010070 8 DALGWTR1P1L S 10070 8 DALGWTRIP 1 M S 10070 8 DA L GWTRIP1H S 10070 8 DA L GWTRIP 2 010071 6 DA L GWTRIP2LS10071 6 DA L GWTRIP 2 M S 10071 6 DA L GWTRIP2HS10071 6 PFB S Concentratio n (ng/mL ) <0.025 5 1.2 1 11. 4 12 0 <0.10 2 1.2 1 11. 9 12 1 <0.10 2 1.1 6 11. 4 11 2 YoRecover y

N A 11 9 11 2 11 8 N A 11 9 11 7 11 9 N A 11 4 11 2 11 0 PFH S

Concentratio n (ng/mL ) <0.10 3 1.1 9 11. 6 11 9 <0.25 8 1.1 5 11. 6 11 9 <0.25 8 1.1 2 11. 7 11 5 YoRecover y

N A 11 6 11 3 11 6 N A 11 2 11 3 11 6 N A 10 9 114 11 2 PFO S

Concerrtratio n (ng/mL ) <0.25 5 1.2 2 10. 9 10 1 <0.25 5 1.1 3 10. 6 10 2 <0.25 5 1.2 2 10. 9 10 2 YoRecover y

N A 12 0 10 7 99. 0 N A 11 1 10 4 10 0 N A 12 0 10 7 10 0 NA= Not Applicabl e

Pag e 3 5 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Tabl e 34

. Rinseat e Blank s

3 M LIM S I D GLP10-01-01-06-06 5 GLP10-01-01-06-12 9 GLP10-01-01-03-00 9 GLP10-01-01-03-01 5 GLP10-01-01-03-02 1 GLP10^1-01-05-00 8 GLP10-01-01-05-02 0 GLP1001-01-05-05 3 GLP10-01-01-05O8 6 GLP10-01-01-05-10 0 GLP10-01-01-05-11 0 GLP10-01-01-08O1 0 Descriptio n DAL SWSW 1 OR B 10062 3 DALGW216RR B 10071 6 DAL-SD-WESB4-R&O00 0 DAL-SD-WESC4-RB-000 0 DAL-SS-WEU01-RB-000 0 DA L SDSD03R B 10062 5 DAL SDSD08RB10062 5 DAL SSSS0 6 RB I 0070 7 DAL SSGP06R B 10070 9 DAL SSGP09R B 100708 DAL SSGP1 1 RB I 0070 8 DAL-SS-OSS08-RB-001 0 PFB S Concentratio n (ng/mL ) <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 <0.025 5 YoRecover y

N A N A N A N A N A N A N A N A N A N A N A N A PFH S

Concentratio n (ng/mL ) <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 <0.10 3 YoRecover y

N A N A N A N A N A N A N A N A N A N A N A N A PFO S

Concentratio n (ng/mL ) <0.25 5 <0.25 5 0.26 0 <0.25 5 <0.25 5 <0.25 5 <0.25 5 <0.25 5 <0.25 5 <0.25 5 <0.25 5 <0.25 5 YoRecover y

N A N A N A N A N A N A N A N A N A N A N A N A
NA= Not Applicabl e

Pag e 3 6 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 1 0 Conclusio n Laborator ycontro l spike s an d fiel d matri xspike s were use d t o determin e th e analytica l metho d accurac yan d precisio n fo rPFBS , PFHS , an d PFOS

. Analysi s wa s successfull ycomplete d followin g 3 M Environmenta l Laborator ymetho d ETS-8-044. 0 describe d herein

. 1 1 Data/Sampl e Retentio n Al l remainin g sample s an d associate d projec t data (hardcopyan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures

. 

### 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 0 6 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d Attachmen t D : Metho d Deviatio n

Pag e 3 7 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 1 3 Signature s 

# I^jzq-Itd/ O Clesto n Lange , Ph.D. , 3 M Principa l Analytica l Investigato r Date 

## 2 f a>/s>^/o Willia m K

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

# fl^H^ i ( I / O Gar yHohenstein , Sponso rRepresentative 

# l^A^

. Date

I ' Date Jaisimh a Kesari , Stud yDirecto r

Pag e 3 8 of 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s of PFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 ^^^^^^^ ^ ^^^^^^^ ^

GLP10-01.0 2 Amendmen t 0 6



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

Decatu rPhas e 3 Site-Relate d Monitorin g Progran n

PROTOCO L AMENDMEN TNO

. 0 6

Amendmen t Date : Jun e 16 , 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 Avenu e AInvestigatio n - Surfac e Wate ran d Groundwate r

Pag e 1 of 6 Pag e 3 9 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

. . . . . ^

. ^ , ^^ ^

^ ^ „ „ Analytica l Protocol : GLP10-01-0 2

^ Amendmen t 0 7 

### 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 : Sectio n 9.2.1 : Astabl e isotope-labele d surrogat e [(1,2.3,4-"C4)-PFOS ] wil l als o b e adde d a t a fixe d leve l t o eac h sample , LMS , LCS , procedura l blank , an d a t variabl e kncsvn concentration s i n calibratio n standards , an d quantifie d t o evaluat e surrc^at e recoveries

.
Asteibl e isotope-labele d iritema l standard , [(1,2,3,4,5,6,7,8-^^C8)-PFOS ] wil l b e adde d at a fixe d concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n o fPFO S an d th e sunnogate

. Astabl e isotope-labele d interna l standard , [(^^OzH'FHS ] wil l b e adde d at a fixe d concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n ofPFHS

.
Astabl e isotope-labele d interna l standard , [(^®02)-PFBS] wil l b e adde d a t a fixed (X)ncentratip n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standard fo raidin g quantitatio n o fPFB S

AMEN D T

O READ : Astabl e isotope-labele d surrogat e t(1,2,3,4-''^C4)-PFOS ] ma yals o b e adde d at a fixe d leve l t o eac h sample , LMS , LCS , procedura l blank , an d at variabl e know n concentration s i n calibratio n standards , an d quantifie d t o evaluat e surrogat e recoveries

.
Astabl e isotope-labele d interna l standard , [(1,2.3,4,5,6,7,8-"C8)-PFOS ] ma yb e adde d at a fixed concentratio n t o eac h sample , LMS , LCS

. procedura l blan k an d calibratio n standarc l fo raidin g quantitatio n o fPFO S an d th e surrogate

.
Astabl e isotope-labele d intema l standard , [('®02)-PFHS ] ma yb e adde d at a fixe d concentratio n t o eac ^ sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n o fPFHS

.
Astabl e isotope-labele d intema l standard , [{^®02)-PFBS] mayb e adde d a t a fixe d concentratio n t o eac h sample , LMS , LCS , procedura l blan k an d calibratio n standar

d fo raidin g quantitatio n o fPFBS

.
Th e us e ofintema l standard s an d sun-cjgat e are onl yappropriat e fo rthos e samplin g location s wit h PFBA , PFHS

. an d PFO S concentration s i n th e lo wpp b range. Prio rt o eac h samplin g event , i fpreviousl yobtaine d PFBS , PFHS , an d PFO S dat a i s availabl e fo rtiie samplin g points o finterest , th e dat a wil l b e reviewe d t o determin e i ftiie us e o fintema l standard s an d surrogat e i s appropriat e fo rth e cunan t samplin g even t

Pag e 2 o f9 Pag e 4 0 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 ^^^^^.^^ ^ p^^^^^^^_

. Q^^Q^^.^ ^ Amendmen t 0 6 

## Amendmen t Approva l


# ^fd^jWPui ^ Gar yHohenstein , sponso rRepresentative 

### Dat e


## I •7-/2^^ ^ Clesto n C

. Lange , Principa l Analytica l investigato r Dat e 

# /yJ^^^-^/o Willia m Reagen , EHSipjpn s Environrtiehta l La b Managemen t



# [QMM / Dat e



# mk
Jaisimh a Kesar i P.E. , DEE , Stud yDirecto r Datf e

Pag e 3 o f6 Pag e 4 1 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Julv201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 6


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

Genera l Projec t Outlin e To : Gar

yHohenstein , 3 M EHS&Opn s From : Susa n Wotf

. 3 M EHS&Opns ; Environmenta l La b cc : Willia m Reagen , 3 M EHS&Opns ; Environmenta l La b

Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charie s Young , Westo n Solution s Ti m Frinak

. Westo n Solution s Date : Jun e 16,201 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 0 6 - Avenu e AInvestigatio n 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r Si xDigi t Departmen t Numbe r Projec t SchedulefTes 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 SainfPaul.M N 55144-100 0 Phone:(651)737-357 0 flahPtiepstein@mfTim.cpiH 3 M Environmenta l Laborator yManagemen t Willia m K

. Reage n 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-973 9 wi<reaaen(a>mmm.co m Principa l Analytica l Investigato r Clesto n Lang e 3 M EH S Opns , Environmenta l Laborator y 260-5N-1 7 65 1 733-986 0 cclanaeffimmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinakSiwestonsolutions.co m Phone : (334)-332-912 3 GLP10-01-02^ 6 Dep t #530711 , Project #002267444 9 Samplin g schedule d fo rth e wee k o fJun e 21,201 0
Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein

.

Pag e 4 o f6 Pag e 4 2 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 6 

### 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 surfac e wate ran d groundwate rsample s collecte d fro m twenty-fiv e samplin g location s fo rPerfluorobutanesulfonat e (PFBS) , Perfluorohexanesulfonat e (PFHS) , an d Perfluorooctanesulfdnat e (PFOS ) a s part o fth e Avenu e A Investigation

. Analyse s wil l b e conducte d unde rth e GL P requirement s o fEP ATSC AGoo d Laborator y Practic e Standard s 4 0 CF R 792

. Groundwate rsample s fro m Decatur , A L wil l b e collecte d b yWesto n Solution s personne l th e wee k o fJun e 21,2010

. 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 e fo rPFBS , PFHS , an d PFO S ar e o fa know n precisio n an d accuracy
. Th e fina l repor t wil l b e submitte d t o Gar yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m report GLP10-01-02
- 06

. 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d by3 M Environmenta l Laborator yfo rsamplin g th e wee k

ofJun e 21 , 2010

. Sampl e botUe

s wil l b e shippe d i n cooler s overnigh t t o 3 M Decaturfo rarriva l o n Friday , Jun e 18,2010

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

. Marti n Smit h \

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

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

. Atota l o ftwenty-five samplin g location s have bee n specified

. Samplin g locatio n description s were not availabl e at th e time o fsampl e botU e preparation

. Fo reac h samplin g location , a total o ffive sampl e botfle s wil l b e collecte d (sample , sampl e duplicate , low-leve l field matri xspike , mid-leve l field matii xspike , an d high-leve l field matri xspike).Th e "fil l t o here " lin e o n eac h 2K ] m L Nalgen e botU e wil l b e 20 0 m L Thre e set s 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 , an d a high-leve l ti-ip blan k spike wil l b e prepare d at tiie 3 M Environmenta l Laborator yan d seri t t o tiie samplin g locatio n witi i th e othe r botOes

. Th e lowfield matii xspike wil l b e prepare d at 1 hg/mL , th e mi d field matii xspike a t 1 0 ng/mL , an d tiie hig h field matii xspike a t 10 0 ng/mL

. Five additiona l botUe s wil l b e prepare d t o b e use d fo rtiie preparatio n o f th e equipmen t rinseate blanks

. Atota l o f142 sampl e bottie s wil l b e prepared

.

Pag e 5 o f6 Pag e 4 3 o f6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 Analytica l Protocol : GLP10-01-0 2 Amendmen t 0 6
Tes t Method s Sample s vwl l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 0 "Determinatio n o fPerfluorinate d Compound s I n Wate rb yHig h Perfbrmance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

. Th e dat a qualit yobjective s fo rtiiese studie s are quantitative result s fo rtiie targe t analyte s witi i a n analytica l accurac

yo f100±30%

. Fiel d matii xspike s not yieldin g recoverie s withi n 100±30 % wil l b e addresse d i n tiie repor

t an d tiie final accurac

ystatemen t ma

yb e adjuste d accordingly

. Alternately , sample s mayb e analyze d b yETS 8-154. 3 "Detenninatio n o fPerfluorinate d Acids , Alcohols , AmkJes , an d Sulfonate s I n Wate rBySoli d Phas e Extractio n an d Hig h Perfoimanc e Liqui d Chromatography/Mas s Spedrometiy"

. Metiio d ETS-8-15 4 has bee n validate d fo rPFOAan d PFO S only ; however , specifi cqualitycontro l sample s analyze d witi i th e sample s wil l b e use d t o detennineoveral l metho d precisio n an d accuracy
. 6 Reportin g Requiremen t Fo reac h samplin g location , tiie report wil l contai n ttie results fo rth e sample , sampl e duplicate , an d th e tiiree field matri xspikes

. Tri p blan k an d tri p blan k

spike s wil l b e reporte d fo rtiie samplin g even t a s wil l an y equipment/rinseat e blank s prepare d i n tiie field. Laborator yconti-o l spike s o freagent wate rprepare d a t ttie time o fsampl e extractio n wil l als o b e reported an d use d t o evaluat e tiie overal l metho d accurac yan d precision

. Metiio d blank

s o freagent wate rprepare d at th e time ofsampl e extinctio n wil l b e use d t o detennin e tiie metho d detectio n limit

. Fo rttiose samplin g kacation s where ttie field matri xspike leve l wa s no t appropriate , du e to highe rtiian expecte d analyt e concenti^ations , a laborator ymatri xspike rtiayb e prepare d an d wil l b e include d i n tiie final report.

Pag e 6 o f6 Pag e 4 4 o f 6 7•Sca n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

s100804a.rd b (PFBS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -2.22e+00 3 x'^ 2 + 5.52e+00 5 x+ 2.94e+00 3 ( r= 0.9999 )
3.6e 7 3.4e 7
3.2e 7
3.0e 7
2.8e7 H
2.6e 7
2.4e7
- 2.2e7
- 2.0e7
- /
1.8e 7 ( 0 2 1.6e 7 

### < 1.4e 7 1.2e 7 1.0e 7 8.0e 6 6.0e 6 4.0e 6 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 6 0 Concentration , ng/m L 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0
*Dat a work-u p performe d b yST W Pag e 1 o f 1 Printin g Time : 1:16:0 2 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 4 5 o

f 6 7»Sta n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

• s100804a.rd b (PFHS) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -1.49e+00 3 x'^ 2 + 3.98e+00 5 x+ 2.74e+00 4 ( r= 0.9998 )

2.6e7
- 2.5e7
- 2.4e7
- 2.3e7
- 2.2e7
- 2.1e7
- 2.0e7
- 1.9e7
- 1.8e7
- 1.7e 7 1.6e7
- 1.5e7
-
« 1.4e 7 - 8 •'•3e7
- S 1.2e7
- ^ 1.1e7
- 1.0e7
- 9.0e6
- 8.0e6
- 7.0e 6 6.0e6
- 5.0e6
- 4.0e6
- 3.0e6
- 2.0e6
- 1.0e6
- 0.0
- 

### ^^'"" " ^^" " ^ ^" ^ 

### /-^ ' ^ y ^ 

## y ' y i

y ^

• / / 

### / / 

## p ' / __.J»
- ^
- ' "

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 7 0 7 5 8 0 8 5 9 0 9 5 100 Concentration , ng/m L *Dat a work-u p performe d b yST W Pag e 1 o f 1 Printin g Time : 1:16:2 2 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 4 6 o

f 6 7•Sta n flPI4000 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

s100804 a PFO S linear.rd b (pfos) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -47 9 x* 2 + 1.63e+00 5 x+ -1.06e+00 4 ( r= 0.9997 )

2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 6 0 Concentration , ng/m L 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 •Dat awork-u p performe db y ST W Pag e 1 o f

1 Printin g Time : 1:18:3 8 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 4 7 o f6 7***Sta nAPI400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# I Sampl e Narrw : ••100804a026 " Sampl « ID : "0 8 00&-147-09
- Fito : "«1008(Ma.wi r Pea k Name : "PFBS " Uass(es) : -298.9/79. 8 amu.298.9/99. 0 amu ' Comment : -2. 5 pp b curv e poin t i n Mill i 0 Water ' Annotation : Sampl e Index : 2 5 nrj/is L Sampl e Type : Concentrati o Calculate d C acq
. r^te : Acq

. Tiino : McdiEied i R TWindo« : Experta d RT : Us e ftdUtiv« R

T Standar d 2-5. S 2.5 3 e/J/201 0 e:l«:3 J Ye s 3P. 0 IP. l NL-

. 

# I Sampl a Name : -a10O8O4a043 " Sampl e ID : "LCS-100726-6 " File : "•100804a.wi r Pea k Name : -PFBS
- Maw(e«) : "298.9/79. 8 Commen t "Spp b LCS ' Annotation : * " ampl e Index : 4 3 ampl e Typa : O C 'jncBnttation : 5

. 1 0 n-j/m L Calc u «cq . ncq . Mod i R T K i Exp« r l a P a T i i e n d c «

H-iqht : Star t Ti

. En dTim «

*Dat a work-u p performe d b yST W Pag e 1 o f 4 Printin g Time : Printin g Date : 1:15:1 6 P M

Friday , Oc t obe r 22 , 201 0 Pag e 4 8 o f 6 7^**Sta nAPI400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS

. an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

I SarrvleNama;-s100804a06 r Sampl e ID:'Solven t blanl T I Pea k Name : 'PFBS ' Ma»(e9) i *298.9/79. 8 amu, : I Comment"MiIIiQWilBrTNlCW27 r Annotafion : Sampl e InJez : 6 1 San,p U Type : UriKnov n Ccnc«nirdtion : N/ A Calculate dCone : 0.0011 1 ng/m L Acq

. m« : e/5/201 C Acq

. Time : f : J3:3 6 A M

Hin

. Pea t

wi d Jno.!thin g Wi d R T Window : Exparta dRT : 

# I Sampl e Name : "s100804a07 rSampt e ID : "GLP10-01-01-06-021 " File : 's i 00804a.wif T Pea k Name : "PFBS " Ma««(ea) : "298.9/79. 8 a m u ,298.9/99. 0 amu ' Commen t "DA L SWSV« 3 0 10062 2 (1;1 0 DU.) "

• Type : Calc i H/ A 9.5 1 q/fu L Acq

. rate : 8/5/201 0 Acq

. Tim*; : 2:Z4:< J Modified : re s R T Window : 30. 0 Experts dRT : 10. 1 US B Relativ e BT : Ni ; Int

. Type : Manua l Retentio nTime : 10. 1 Area : 5257J 5 c 9.?iqht : •).07^-00 4 Star t Tine : 9.57 1 En dTimft : 10.30 0 ^ P M

s e c mi n

c p s mi n B.8e 4

S.6e 4 e.4e4 S.2e4 ' 8.0e 4 7.8* 4 7.6e4

. 7.4* 4 • 7.2* 4 7.0e 4 6.8* 4

*Dat awork-u p performe db y ST W Pag e 2 o f

4 Printin g Time : 1:15:1 6 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 4 9 o f 6 7*^**Sta n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o f PFBS

. PFHS , an d PFO S i n Wate rSample s fro m Decatur

. A L June/Jul y201 0

• Samp h Name : ''s10D804a026 ' Sampl e ID : ' C I Pea k Name:'PFHS " Mass(es):'399.0/79. 8 an ; I Commen t "2. 5 pp b curv e poin t i n Mil l O Water " Sampl e Index : 2 5 Sampl e Type : Standar d Concentration : i.L S n-j/m L Calculate d Cone : 2.5 3 ntj/m L 008-147-09
- Rta : •«1008O4a.wi r I.399.W99. 0 amu ' Annotation:" "

Acq

. rate : Acq

. Time : Modified : PrDC

. Algor i Nois e Parre l Base

. Sub

. K Psak-Split

. Repor t Larg e Min

. Pea k

H e Min

. Peak

w i aracwthin g W

i B T Window : Expecte dRT : Us e Rdlativ a Int

. Type : Retentio n T

i Area : Height : Star t Time : EndTirao : :hm :

:a'je : Tact o S t P e ight : dth : dth :
RT : 9/1/201 0 e;l?:3 J P

M Ye s :ntBlliOu a 9 5 l.O C r : i ak ; N

o 0.0 0 0.0 0 3C. 0 12. 7 N o Bas e T o Ba 12. 7 102572 1 ec u i .OJe-OC S 12.59 0 12.92' ! 2.0e S
2.0* 5 1.9e 5 1.9e S 1.8* 5

^ 1.8*5

. 1.7* 5 1.7* 5 1.6* 5 1.6* 5 1.5* 5 1.5* 5 1.4* 5
1.4* 5 1.3* 5 1.3* 5 1JZe 5 1.2* 5 1.1* 5 I 1.1* 5

" 1.0* 5 I 9.5e 4 9.0e 4
8.5e 4 8.0e 4 7.5*4
- 7.0e4
- 6.Se4
- 6.0e4

- S.Se4
- S.0e4
- 4.5e4

- 4.0e4

- 3.5*4

- 3.0*4 ; 2.5*4
- 2.0*4 : 1.5*4
- 1.0*4

- 5000.0 : 0.0 ; 

# I Sampl e Name:'s100804a043 ' Sampl e ID:-LCS-10072e-«
- Pea k Name : "PFHS " Mas«(es) : "399.0/79. 8 smu.399.a99. 0 Commen t '5pp b LCS " Annotation : — Sampl e Index : 4 3 s c c A A M P N

. B mpl e Type : Q C ML-KntratioTi : 5,1 5 n' j iculata dCone : 5.5 4 n q q . Pate : 8/5/20l a q . Time : 2:20:0 7 A H dified : Ye s o c . Al()orithn, : IntelliQua n- i s e P-.rcentag« : 5 5 3 8

. Jub

. Window : 1.0 0 m ml

. rt. L

H Q

Expec-ttt dBT : Us e Relativ e Int

. Type : Retentio nT i Area : H-.igl.t : Star t Tir,e : En dTime : 12. 7

RT : N o Bas e T o , e : 12. 7 2:'0080 0 c 4.6ee*00 S 12.56 0 12.93 9

•^Datawork-u p performe db y ST W Pag e 3 o f

4 Pr i Pr i ntin g Time : 1:15:1 6 P M ntin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 0 o f 6 7^*Sta n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

• Sarr^il e Name : "s100804a061 * Sanipl e ID : "Solven t blank " File : "si00804a.wiii r I Pea k Name : "PFHS " Mass(es} : "399.0/79. 8 armi,399.0/99. 0 amu " I Commen t "Mill i Q Wate rTN I 0-0272 " Annotation : ~ ,n,pl e Type ; Unk i Calculate d Cone : Acq

. Pate ; 6 / Acq

. Time : Mod i tied : Proc

. Alcforithm : I n Nuis e Pecceiitage : Base

. Sub

. Window : P-ak-Split

. Factor : Repor t Larges t Pea k Min

. Pea k

Heit|lit : Min

. Pea k

Width : 3m<...;thin g Width : R THindo-rf : Exp«cta d RT : Ui e Relativ e RT : Int

. Type : 7 Retentio n Time : Area : 10 5 Height : 2. 0 V 0 /201 0 3:3 6 A H N o elUQu a ;, o 1.0 0 4 N o 0.0 0 0.0 0 0. 0 12- 7 N o alle y 12. 7 5e-00: < 480 0 470 0 460 0 450 0 440 0 430 0 420 0 410 0 400 0 390 0 360 0 3700

- 360 0 350 0 340 0 330 0 320 0 310 0 300 0 290 0

2500

- 240 0 230 0 220 0 210 0 200 0 190 0 160 0 1701

- 160 0 1500

- 140 0 130 0 120 0 1100

-

• * "-V- ' ^ 

# I Sampl e Name : "«100804a077 " Sampl e ID ; •GLPl{W)1-01-0&02 rFile : " s 100804a.(Mt T Pea k Name : "PFHS " Mass(es) : -399,0/79. 8 amu,399.ora9. 0 amu " Commen t 'DA L SWSWD3 0 10062 2 (1:1 0 Oil.) " Annotation :

Percentage : :plit

. Fact o Larges t P e 'ea k Height : 'ea k Width : lin g Width :

• e dRT : elliQua i S O 1,0 0

*Dat a work-u p performe d b yST W Pag e 4 o f 4 Printin g Time : 1:15:1 6 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 1 o f 6 7"**Sta nAPI400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur

. A L June/Jul y201 0 

# r SaiTvi h Name : -s10D804a02 rSampl e ID : Pea k Name : 'pfos * Mass(es) ; "498.9/99. 2 Comment : "2. 5 pp b curv e poin t i n MiR i Q Water " Annotation : Sampl e InJey. : 2 6 Sampl e Typa : .standar d 008-147-09 " Fita : "sl00804a.»ri r ,438.9/130. 0 amu,498.9/80. 0 amu "

Calculate d Cone : Acq

. Pate : Acq

. Time : Mcditied : R TWindow : Expecte d RT : Us e Relativ e Int

. Type : Retentio n T i Area : Height : Star t Time : En d Time : RT :

e : 2.5 ?

2.3 9 B/J/201 0
Ye s 30. 0 lA. b

Manua l 14. 3 7&ai 2 c e.OTatOO J iJ.19 8 1J.50 1 ng/ra L

PH

se c m m

mi n
ffiin 8.0* 4

7.8e 4
7.6 M
7.4e 4 7.2e 4
7.0e 4
6.e<» 4

6,2e 4
6.0e 4
5.8e 4
5.6e 4
5.4e 4
5.2* 4
5.0e 4
4.8e 4
4.6 M
4.4e 4

. 4.2* 4
4.0* 4
3.8* 4
3.6* 4
3.4* 4
3.2* 4
3.0* 4
2.8* 4
Z6* 4
2.4*4

- 2.2*4

- 2.0* 4
1.6* 4
1.6*4

- 1.4*4

- 1.2*4

- 1.0*4

- 8000.0

- 6000.0

- 4000.0

- 3000.0

- 0.0

- 

### :yU:i s C'jncontration : Calcutata d Con e Acq

. rate : Acq

. Time : Modified : R TWindow : ExpoctH d RT : Us s Relativ e Inc

. Type : Retentio n T i Area : Height : B T

e , 5

5 e/5 / 2:2 0

3 0 1

1 2234 3 l.SS e e l ng/n, L 01 0 0 7 A H

. 5

a l

. : 00 5 : "

cp s 

## ( Sampl e Nam* : "8100804*043 " Sampl e ID : tCS- l 00726-6 * File : "s i 00804a

. wif T Pea k Name : 'pfos " Ma««(*») : '498.9«9. 2 amu,498.9 n 30. 0 a m Comment " ^p b L C S ' Annotation:" "

1.9* 5
1.9* 5
1.8* 5
1.8e 5
1.7* 5
1.7* 5
1.6* 5
1.6* 5
1.5* 5
1.5* 5
1.4* 5
1.4* 5
1.3* 5
1.3*5
- 1.2* 5
1.2* 5
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
- 3.Se 4
3-0* 4
2.5* 4
Z0e4
- 1.5* 4
1.0* 4
5000. 0

0. 0 *Dat a work-u p performe d byST W Pag e 1 o f 3 Printin g Time : 1:18:1 5 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 2 o f6 7"Sta n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

• Sampt a Nanne : •»100804a055 ' Sampl e ID : 'LCS-100726-15 " Fil* : -«100804a.iM r I P«a k Name : "pfos ' Ma$s<»s) : "498.9/99. 2 amu.498.9/130. 0 amu,498.9/80. 0 amt /

• Commen t "5pp b LC S ECF " Annotation : " Sampl e Indez ; b t Sampl e Type : Q C Concentratiuri : 5.0 0 nrj/ia l Calculate dCone : J.1 5 ng/m L Acq

. P^te : e/S/201 0 1.3e 5 Acq . Time : Modified : R T Win-do-,j : Expecte d R

- ;:35:4 4 A M

RT : Int

. Type : Manua l Retentio n Time ; 14. 3 mi n Area : 65991 7 count s Height : 1.35e+00 5 cp s En dTi l IJ.19 S 11.53 2

c 6.5* 4 Sampl e Nam* : "s100e04a061 " SamF^ a ID : ~Solv*n t btank " Fit* : "•100804a.>M r P*a k Name : "pfos ' Mass(«s] : '498.9/99. 2 annu,498.9/130. 0 amu.498.9/80. 0 amu ' Commen t 'Mill i Q Wate rTN10^)272 " Annotation : Sampl e lnde.\ : 6 1 Sampl e TiT e : Unknow n Onc^ntcation : N/ A Calculate d Cone : 0.07 6 Acq

. Pate : 5/b/2 Q Acq

. Tipe : 1:43:3 ' Hoditied : Ye s R TWindow : 30. 0 Expecte d RT : 14

. : U3 « Relativ e RT : tfi

.

3.38e*0P 2 cp s

*Dat a work-u p performe d b yST W Pag e 2 o f

3 intin g Time : 1:18:1 5 P M intin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 3 o f6 7•Sta n API400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS

. an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# I San^t e Name : •s1O08O4a07 rSampl e ID : "GLP1(M1-01-06-021 " File:*»100804a,wif r Pea k Nam* : 'pfos ' Mass(es) : '498.9/99. 2 amu,49e.9/130. 0 amu,4S8.9A0. 0 amu Corrmon t "DA L SWSVW 3 0 10062 2 (1:1 0 Dl fAnnotation : - Sampl e Tvpe : Calculate dC Acq

. Pate ; A^q

. Time : Modified : R T Window : Exp«rte dRT : Us e Relativ e Int

. Type ; Retentio nT i Area : Height : Star t Time : En dTime : >n c

R T

.. , 1 101

. ng/m L 6/5/201 0 2:2J:< 4 P

M Ye s 30. 0 sa c 14. 5 mi n

Manua l H . 3 mi n 523J 3 count s 3.2?e'O0 5 cp s IJ.ie S (Si n 1J.50 7 mi n 3.2* 5
3.1* 5
3.0* 5
2.9*5

- 2.8* 5

*Dat awork-u p performe db y ST W Pag e 3 o f

3 Printin g Time : 1:18:1 5 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 4 o f 6 7***Sta nAPI400 0 V166030 5 GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0 

# I SampI * Name : -«100804a055 " Sampl e ID : "LCS-100726-15 " Fife : "s100e04a.wi r Pea k Name : 'pfos ' Mass(es) : '498.9/99. 2 amu.498.9/130. 0 amu.498.9/80. 0 amu " Commen t "5pp b LC S ECF " Annotation : " " Sampl e IndeK : 5 5 San.plf l Type : C^ ~ Calculate dCone ; 2.2 3 ng/m L Acq

. P»ca : 8/5/201 0 Acq

. Ti l 4 1 A M Modified : R T Window : Exp«rte dRT : Us e Rslativt , Int

. Type : Retentio nT i Heigfit : Star t Tine : En dTime : RT :

n e : y

3 0 1 K M.in I .iO e 1 3

- I J

. 1.3* 5

1.3* 5

1.2* 5

1.2* 5

1.1* 5

1.1* 5

1.0* 5

9.5* 4

9.0* 4

6.5* 4

8.0* 4

7.5* 4

7.0e 4

6.5* 4

6.0* 4

5.5* 4

5.0* 4

4.5* 4

4.0e 4

3.5* 4

3.0* 4

Z5* 4

2.0* 4

1.5* 4

1.0* 4

5000. 0 1 4

14.07.

. 3 0 

# I SampI * Nam* : "sl00e04aa77
- SampI * ID : "GLP1&O1-01-06-021
- Fil0:'s1OO8O4a.wif r Pea k Nanv : "pfos " Mass(es) : "498.9/99. 2 amu,438.9/130. 0 amu,498.9/80. 0 Comman t "DA L SWSVW 3 0 10062 2 {1:1 0 DB.) " Annotation : Sanip L Sampl e Typ e Unhnow ; N/ A ^cq

. rsta : Acq

. Tiwe : ModiEiert : R TWindow : ExpertHr i RT : 9/5/201 0 2:2<:4 4 P H
YP S 30. 0 1^. 5

H-iqht : Star t 1 ^n dTi r

*Dat awork-u p performe db y ST W Pag e 1 o f 1 Printin g Time : 1:21:5 1 P M Printin g Date : Friday , Octobe r 22 , 201 0 Pag e 5 5 o f 6 7

### DocQm'Brtiro3ai|it& & iMj56«!Q6 f current , fo r1 4 days fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



# 3 M Eiffidronmenfa l laixNBlor y

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

b yLC/MS/MS ; Direc t Injectio n Analysi s Metho d Number : ETS-8-044. 0 Adoptio n Date : Upo n Signin g Effectiv e Date : Q U I n [ o " 1

Approve d By :

^ 

### ^//^/ o • > Willia m K

. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Page t of1 1 Methiod o fAnalysi s fo rtti e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 5 6 o f 6 7DocQ(:Ra=iiitrai|it<'m8: i s«lsBft]oe fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

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

. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n alternat e metho d suc h a s ETS-8-15 4 "Detenninatio n of Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Perfonnanc e 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 IVIetho d Summar y Clea n aqueou s sample s are analyze d b ydirec t injectio n usin g LC/MS/MS

. Sample s containin g heav y particulat e ma

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

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

. Thi s i s a perfonnance-base d method

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

t multipl e concentrations

. Thi s metho d als o require s that th e precisio n an d accurac yfo reac h sampl e b e 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 o f70 % t o 130% , ma

yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l no

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

. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t 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 t o detennin e th e statemen t of accurac yfo ranalytica l results

. 

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

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

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

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

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

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

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

. 3. 3 Fiel d Blan k

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

. Th e purpos e o fth e F B i s t o detennin e i ftest substance s o r othe rinterference s ar

e presen t i n th e fiel d environment

. Thi s sampl e i s als o referre d t o a s a Tri p Blank

.

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

t Injectio n Analysi s Pag e 5 7 o f 6 7DocGmf!*rtifei^ijitteiK€patsloe fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

3. 4 Fiel d Duplicat e Sampl e (FDS , Fiel d Dup ) Asampl e collecte d i n duplicat e a t th e sam e tim e fro m th e sam e locatio n as th e sample

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

. Analysi s o

fth e FD S compare d t o that o fth e firs t sampl e give s a measur e ofth e precisio n associate d wit h sampl e collection , preservatio n an d storage , 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 o fth e targe t analyte s ar

e adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n o faqueou s samples

. Aknown , specifi cvolum e o f sampl e mus

t b e adde d t o th e sampl e containe rwithou t rinsing

. Thi s ma yb e accomplishe d b

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

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

. I fth e expecte d rang e 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 o fth e sampl e analysis

. 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot ofAST M Typ e I , HPLC grad e water , o rothe rsuitabl e water , t o whic h know n quantitie s ofth e targe t analyte s are adde d i n th e laborator yprio rt o th e shipmen t ofth e collectio n bottles

. Th e FSC S i s extracte d an d analyze d exactl ylik e a stud ysampl e t o hel p detennin 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 are no t know n o rma

yvary
. At least on e separate , un-spike d sampl e must b e take n a t th e sam e tim e an d place as eac h FMS

. 3. 7 Laborator yContro l Sampl e (LCS ) A n aliquot o

fcontro l matri xt o whic h know n quantitie s ofth e 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 detennin e whethe rth e metho d i s i n control

. LCS s shoul d b e prepare d eac h da ysample s are extracted

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

ymatri xspik

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

. Th e LM S i s analyze d exactl ylik e a laborator

ysampl e t o detemnin e whethe rth e sampl e matri xcontribute s bias t o th e analytica l results

. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e determine d i n a separat e aliquot an d th e measure d value s i n th e LM S correcte d fo rthes e concentrations

. LMS s are optiona l fo ranalysi s ofaqueou s samples

. 

### 3. 9 Laborator ySampl e Aportio n o raliquot ofa sampl e receive d fro m th e fiel d fo rtesting

. 3.1 0 Limi t o fQuantitatio n (LOQ ) Th e lowe rlimi t ofquantitatio n (LLOQ ) fo ra dataset i s th e lowest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits 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 as th e lowest non-zer o standar d i n th e calibratio n curve that meets metho d criteria

. Sampl e LLOQ s are matrix-dependent

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

. Th e highest standar

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

.

ETS-8-044. 0 Pag e 3 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 8 o f 6 7Docamsgpliwtawtf e sc-aftloi fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

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

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

. Th e metho d blan k i s use d t o detennin e i ftest substance s o rothe rinterference s 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 ofa single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound

. 

### 3.1 4 Surrogat e Acompoun d simila ri n chemica l compositio n an d behavio rt o th e targe t analyte(s) , bu t i s no t nomrially foun d i n th e sample(s)

. Asurrogat e compoun d i s typicall ya target analyt e wit h a t leas t on e ato m containin g a n isotopically-labele d substitution

. I fused , surrogate(s ) ar e adde d t o al l sample s an d qualit y contro l samples

. Surrogate(s ) are adde d t o quantitativel yevaluat e th e entire analytica l procedur e includin g sampl e collection , preparation , an d analysis

. Inclusio n ofa sun'ogate analyt e i s a n optiona l qualit ycontro l measur

e an d i s NO

Trequired

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

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

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

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

. Th e laborator

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

. Areference fil e o fmateria l safet y dat a sheets (MSDS ) shoul d b e availabl e t o al l personne l involve d i n thes e analyses

. 4. 2 Caution s Th e analyst mus

t b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e ofsolvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems

. Refe rt o th e appropriat e equipmen t procedur e o roperato rmanua l fo radditiona l infomnatio 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 interf'erence s unde r condition s o fanalysi s b

yrunnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 5 9 o f 6 7DocGica«SRlif0»|itfee«|3seloe fcurrent , fo r1 4 day s fro m 10/26/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Parts an d supplie s that contai n Teflon® shoul d b e avoide d o rminimize d du e t o th e possibilit yof interference and/o rcontamination

. Thes e ma yinclude , bu t are no

t limite d to : was h bottles

. Teflon ® line d caps , autovia l caps , HPLC parts , etc

. Th e us e ofdisposabl e micropipette s o rpipette s t o aliquot standar d solution s i s recommende d t o mak e calibratio n standard s an d matri xspikes

. 

### 6 Instrumentation , Supplies , an d Equipmen t 6. 1 Instrumentatio n an d Equipmen t Ahig h perfomianc 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 balance capabl e ofreadin g t o 0.000 1 g Adevice t o collec

t ra wdat a fo rpea k

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

. Gas tigh t syringes , 25pL , 50pL , lOOpL , 250pL , 500pL , 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 C18,4. 6 m m x100 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

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

Are a - quadrati ccurve fit , 1/ xweighted

. RunTime : ~ 17minutes

. 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 that dat a qualityobjective s are met

.

ETS-8-044. 0 Pag e 5 of1 1 Metho d ofAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 0 o f 6 7DocQmsKli«eai|itlf » gipsaloe fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 313- > 11 9 36 3 ^ 319 , 36 3 ^

16 9 an d 36 3 ^

11 9 41 3 ^ 369 , 41 3 - > 21 9 an d 41 3 - * 16 9 46 3 - > 419 , 46 3 ^

16 9 an d 46 3 ^

21 9 51 3 ^ 469 , 51 3 ^

21 9 an d 51 3 - > 26 9 56 3 ^ 519 , 56 3 - ^

26 9 an d 56 3 -^21 9 61 3 ^ 569 , 61 3 - » 16 9 an d 61 3 - > 31 9 29 9 - ^ 8 0 an d 29 9 - » 9 9 39 9 - ^ 8 0 an d 39 9 - ^

9 9 49 9 - ^ 80 , 49 9 - ^

9 9 an d 49 9 ^

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

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

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

. 7 Reagent s an d Standard s
7. 1 Chemical s 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 a s NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHp A- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFO A- 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 (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Perfluorododecanoi cAci d (PFDoA-C1 2 acid) ; Oakwoo d Products , In c Perfluorobutanesulfonat e (PFB S - C4 sulfonate) ; 3 M Perfluorohexanesulfonat e (PFH S - C 6 sulfonate) ; 3 M Perfluorooctanesulfonat e (PFO S - C 8 sulfonate) ; 3 M ETS-8-044. 0 Pag e 6 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 1 of6 7DocGtcRCOFdiKraatfitt e H6i»i»]o6

fcurrent , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 : Alternative volume s ma yb e prepare d a s lon g a s th e ratio s ofth e solven t t o solut e ratio s ar e maintained

. 7. 4 Stoc k

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

d preparatio n procedur

e serve s a s a n example

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

. Fo rexample , p L volume s ma yb e spike d into volumetri cflask s whe n dilutin g stoc k

solution s t o appropriat e levels

. 10 0 Mg/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 con-ectio n i s give n belo wfo rPFOS

.

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

49 9 PFO S (K^ ^ )sal t correctio n facto r= ^3f i = 0.927 5 53 8 1 0 m g CgFiySOs'K

* wit h purit

y90 % = 8.35m g CsFuSOs " (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 lOOpg/m L SSS s t o a lOm 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 worltin g standard—Ad d 1.25m L o fth e 5 pg/m L -mixe d worthin g standar d solutio n t o a 25m L volumetri cflas k

an d brin g u p t o volum e wit h solvent

. 12 5 ng/m L mixe d standard—Ad d 625p L ofth e 5 pg/mL-mixe d 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 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 2 o f 6 7Doc'3OT<JXKlittBaijiteteigiia«!G«.f'tioe fcurrent , fo r1 4 day s fro m 10/26/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0



### 7. 5 Calibratio n Standard s Usin g th e wori<in 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 o fwate ran d wori<in g standard s ma y b e adjuste d t o meet th e dat a qualit yobjective s addresse d i n th e genera l projec t outline

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

.

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

.

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 i 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 o

fglas s autovials , t o preven t th e possibl yoffluorochemica l stickin g t o th e glass

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

. Prepar e metho d QC sample s an d multipl e metho d blank s an d aliquot into labele d plasti cautovials

. Prepar e a t least fiv e metho d blanks

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

d curve prio rt o eac h set ofsamples

. Th e standar d curve ma

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

xo runweighted , o rb

yquadrati cfi l (

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

xo runweighted , usin g suitabl e software

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

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

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

. Hig h and/o rlo

wpoints ma

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

. Low-leve l curve points shoul d als o b e exclude d i f thei rare a counts ar e no t a t least twic e that ofth e metho d and/o rsolven t blanks

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

. Eac h poin t i n th e curve must b e withi n ±25 % ofth e theoretica l concentratio n wit h th e exceptio n ofth e LLOQ , whic h ma y ETS-8-044. 0 Pag e 8 o f1 1 Metho d o fAnalysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direct Injectio n Analysi s Pag e 6 3 o f 6 7DocQmffi^iiiK^i|it&f t g^^olpe f current , fo r1 4 day s fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

b e withi n ±30%

. Justificatio n fo rexclusio n ofcalibratio n curve points wil l b e note d i n th e ra wdata

. Aminimu m of6 points wil l b e use d t o constmc t th e calibratio n curve
. I fth e calibratio n curve doe s no t meet acceptance criteria , perfon n routin e maintenance o rprepare a ne wstandar d curve (i fnecessary) an d reanalyze

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

yofth e calibratio n curve
. Analyz e a mid-rang e calibratio n standard , on e ofth e sam e standard s use d t o constnjc 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 data accurat e t o ±30 % wit h a targete d LO Q of0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belo wwil l b e documente d i n th e ra wdata an d footnote d i n th e fina l report

. 10. 2 Metho d Blank s Metho d blank

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

. At least fiv e metho d blank s mus t 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 mn
. Th e mea n are a coun t fo reac h analyt e i n th e metho d blank s mus t b e les s tha n 50 % o

fth e are a coun t ofth e LOQ standard

. Th e standar

d deviatio n ofth 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 o fth e metho d blank s excee d 50 % o

fth e LOQ standard , the n th e LOQ must b e raise d t o th e 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 detennin e outliers , o rtechnica l justificatio n t o eliminat e on e o rmor e results shoul d b e made

. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field

. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagge d i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo r replicate s exclude s fiel d blanks

. 

### 10. 4 Surrogat e Spike s Sunnogat 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 oftwo 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 ofth e curve
. Th e relative standar

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

. I fth 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 Determinatio n o fPerfluorinate d Compound s i n Wate rb yLC/MS/MS ; Direc

t Injectio n Analysi s Pag e 6 4 o f 6 7DocQicR®?di-Rffiaijit&8i8ffp«.i5i0e fcurrent , fo r1 4 day s fro m 10/26/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 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 % o fth e fortifie d levels

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

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

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

. Th e averag e 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 softwar

e program : A, ^ rJ / , , V (Pea k

Are a - Intercept ) ^..^ Analyt e foun d (ng/mL ) = -^ ^ ^-^

xD F Slop e D F = facto rb

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

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

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

t achieve d mus

t b e considere d i n th e evaluatio n o fth e data

. Nonconfomnanc

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 perfonnance sectio n are no t met , maintenance ma

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

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

. I fdat a ar e t o b e reporte d whe n perfonnance criteri a hav e no t bee n met , th e data mus t 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 m n prio rt o th e calibratio n curve
. Typicall ythes e sample s are at a concentratio n nea rth e mi d leve l ofth e calibratio n curve an d are repeate d injection s fro m on e autosample rvial

. Th e syste m suitabilit yinjection s 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 ofdetenninatio n (r^ ) valu e fo rth e calibratio n curve mus t b e greate rtha n o r equa l t o 0.990

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

yb e withi n ±30%

. CCV Performance : Th e calibratio n standard s that are intersperse d throughou t th e analytica l sequence are evaluate d a s continuin g calibratio n verification s i n additio n t o bein g par t ofth e calibratio n curve
. Th e accurac yo f 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 byCCVs no

t meetin g thes e criteri a must b e reanalyzed

.

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

t Injectio n Analysi s Pag e 6 5 o f 6 7

### DocQi:R'aRtiwi«Mte!i » ia«^Mloe fcurrent , fo r1 4 days fro m 10/25/201 0 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0

Demonstratio n o fSpecificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % of standard ) an d th e mass 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 ar

e designe d t o generat e data that are accurat e t o +/-30%

. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d accurac yo flaborator

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

ymatri xspikes

. 

### 12. 5 Precisio n Sample s shoul d b e collecte d i n duplicat e i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

. RP D results greate rtha n 20 % wil l b e flagged i n th e report , bu t wil l no t b e exclude d fro m reporting

. Th e requiremen t fo rreplicate s exclude s field blank s o rrinse blanks

. Sectio n 1 0 contain s additiona l infonnatio n regardin g th e require d precisio n oflaborator ycontro l spikes

. 

### 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfomnin g thi s metho d wil l b e dispose d ofappropriately

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

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

. 1 4 Record s Eac h dat a packag e generate d fo ra stud ymust includ e al l supportin g informatio n fo rreconstructio n ofth e data

. Informatio n fo rth e dat a packag e must include , bu t i s no t limite d t o th e followin g items : stud yo rprojec t number , sampl e an d standar

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

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

. 

### 1 5 Affecte d Document s None

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

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

t Injectio n Analysi s Pag e 6 6 o f 6 7GLP10-01-02 ; Interi m Repor t 0 6 Analysi s o fPFBS , PFHS , an d PFO S i n Wate rSample s fro m Decatur , A L June/Jul y201 0


### /

. Identificatio n Stud y/ Projec t No

. GLP10-01-02-0 6 Deviatio n typ e (Ctiecl < one ) 

## a

D Date(s ) o fOccurrence : s100804aan d miq0910 a
_ SO P D Equipmen t Procedur e Protoco l 0 GP O Documen t Number : ETS-8-044. 0 0 D Metho d Other : //

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

### Metho d Requirements : T

. LC S averag e recover yo f100 % ±20% / 2

. Sample/Sampl e Duplicat e RP D s20%

. 3

. LMS/FM S recover

yof100 % ±30%

. 

### Actua l procedure/process : (1 ) LC S averag e recover yfo rlinea ran d branche d PFO S wa s >120 % (s100804a)

. LC S averag e recover y fo rth e lowse t o fLC S fo rPFHS , an d th e lowan d hig h se t o flinea ran d branche d PFO S wa s outsid e acceptanc e criteri a (mIOOQIOa)

. (2 ) Th e RP D fo rPFO S fo rsamplin g locatio n GP0 4 wa s 30% , GP0 9 PFO S RP D wa s 33% , GP1 0 PFO S RP D wa s 31% , GP1 2 RP D fo rPFBS , PFHS , an d PFO S wa s >50%

. (3 ) Th e recover

yo fth e hig h FM S sampl e fo rSW1 2 fo rPFO S wa s 63.5%

. Th e recover yofth e hig h FM S sampl e fo rGP0 2 fo rPFO S wa s 68.7%

. Th e recover yofth e hig h FM S sampl e fo rGP0 4 fo rPFO S wa s 141%

. 

### /// , Action s Take n

(sue! ) a s amendmen t issued , SO P revision , etc. ) 

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

) Reference : Acceptabilit yo fth e nonconformin g work : 1 ) Th e linea r+ branche d PFO S LC S whe n quantitate d agains t a calibratio n curv e prepare d fro m linea r PFO S have bee n quantitatin g aroun d 15-30 % higher

. B yquantitatin g th e linea ran d branche d isomers o fPFO S separately , agains t a linea rPFO S curve , an d summin g th e resultin g concentrations , appears t o hel p reduc e th e recover

yofth e linea r+ branche d PFO S hig h LC S at 30pp b 8%

. Asligh t increas e wa s see n i n th e recover

yofth e lowan d mi d linea r+ branche d PFO S LCS , an d a n 18 % decreas e i n th e recover yo flowse t oflinea rPFO S LCS

. Th e metho d analytica l uncertaintywa s assigne d base d o n th e averag e recover

yo fth e hig h se t oflinea r+ branche d PFO S LC S (141%) , sinc e th e sampl e on-colum n concentration s mos t closel ymatche d th e 3 0 pp b LCS

. LC S averag e recoverie s outsid e metho d acceptanc e criteri a wil l b e footnote d i n th e fina l report

. 2 ) Th e RP D valu e fo rsamplin g location s wit h RP D value s >20 % wil l b e footnote d i n th e dat a tables

. 3) Sinc e th e metho d analytica l uncertaintyfo rPFO S i s 100 % ±41% , n o adjustmen t wa s mad e t o th e analytica l uncertaintyfo rPFO S o n SW12 , GP02 , an d GP04

.

Actions : D Haltin g o fWor k D Clien t Notificatio n n Wor k Recal l D Withholdin g o fRepor t 0 Other : Deviation s wil l b e note d i n final repor t 

### Project Lead/PA I Approval : S/Jsa n Wol f Stud yDirecto r(i fGLP ) Sponso rApprova l (fo rGL ^ protoco l deviations) : N

A Technica l Reviewe r(optional) : N A Laborator yDepartmen t Manage rApproval : /^/a</ /

Date : N A Date : IV

. Authorizatio n t o Resum e Wor k Where iialtin g o fworl < occurred , resumptio n o fworl < mus t firs t b e approve d b yLaborator yManagemen t 

### Laborator yDepartmen t Manage rApproval : N ADate : N A Deviatio n No

. (assigne d b yStud yDirecto ro rTea m Leade ra t th e en d o fstud yo rproject ) Pag e 6 7 o f 6 7