GLP10-01-01

. Interi m Repor t 11 : Analysi s o fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) locate d i n Decatur

. A L i n Novembe r201 0
Stud yTitl e Analysi s o f Perfluorooctanoi cAci d (PFOA ) 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 f signin g Performin g Laborator y 3 M Environmenta l Healt h an d Safet yOperation s Environmenta l Laborator

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

5 3

Th e testin g reported herei n mee t th e requirement

s ofISO/IE C 17025-200 5 "Genera l Requirement

s fo rth e Competenc

e ofTestin g an d Calibratio n Laboratories" , I n accordanc e wit h th e A2L ACertificate #2052.01

. Testin g tha t complie s wit h thi s Intemationa l Standar d als o operat e i n accordanc

e wit h IS O 9001:2000

. Certificat e #2052.0 1GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

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

.

Pag e 2 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### GL P COMPLIANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 11

. Analysi s o

fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) at Decatur , A L i n Novembe r201 0 Study : Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program

. Thi s analytica l phas e wa s conducte d i n compliance wit h Toxi cSubstance s Contro l Ac t (TSCA ) Goo d Laborator yPractice (GLP ) Standards , 4 0 CF R 792 , wit h th e exception s liste d below :

• Thes e are environmenta l sample s where there i s n o specifi ctes t substance , n o specifi ctest syste m an d n o dosin g o f a 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 at th e test sit e hav e no t bee n determine d unde rGLPs

.

Gar yHqraenslein , Sponso rRepresentative Date



# ^' m

Jaisimh a Kesari , P.E. , DEE , Stud yDirecto rDate

Pag e 3 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### QUALIT YASSURANC E STATEMEN T Repor t Title : GLP10-01-01 , Interi m Repor t 11

. Analysi s o

fPFO Ai n Groundwate rSample s Collecte d a t th e Forme rSludg e Incorporatio n Are a (FSIA ) a t Decatur , A L i n Novembe r201 0 Study : Analysi s o fPerfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M Decatu rPhas e 3 Site-Relate d Monitorin g Program

. Thi s repor

t an d th e accompanyin g data were audite d b yth e 3 M Environmenta l Laborator yQualit y Assurance Uni t (QAU) , a s indicate d below

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

ymanagemen t an d stud ydirector

.

Inspectio n Date s 12/30/1 0 1/27/11-1/28/1 1 Phas e In-Phas e Data/Interi m Repor

t Dat e Reporte d t o

Testin g Facilit y Managemen t 2/4/1 1 2/4/1 1 Stud yDirecto r 2/4/1 1 2/4/1 1



### URepresealtati v 

# /•C-^eJ ^ 

# ;i'J'' f QA U Representative Date

Pag e 4 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

y9 3 Introductio n 1 0 4 Test s Contro l Substance s 1 1 5 Reference Substance s 1 1 6 Test Syste m 1 2 7 Metho d Summar

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

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

Pag e 5 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

9 Data Summar

yan d Discussio n 1 7 1 0 Conclusio n 3 0 1 1 Data/Sampl e Retentio n 3 0 1 2 Attachment s 3 0 1 3 Signature s 3 1 

### LIS TO F TABLE S Tabl e 1

. Summarize d PFO AResults (FSI AGroundwater , Decatur , AL , Novembe r2010 ) 1 0 Tabl e 2

. Instalmen t Parameters..

. 1 3 Tabl e 3

. Liqui d Chromatograph yCondition s 1 3 Tabl e 4

. Mas s Transition s 1 3 Tables

. Limi t of Quantitatio n (LOQ ) 1 4 Tabl e 6

. Laborator

yContro l Spik

e Recover

y1 5 Tabl e 7

. Analytica l Metho d Uncertaint y1 6 Tabl e 8

. Fiel d Matri xSpik e Level s 1 6 Tabl e 9

. DA L GW130 R 10110 5 1 8 Tabl e 10

. DA L GW130 S 10110 5 1 8 Tabl e 11

. DA L GW130 L 10110 5 1 8 Tabl e 12

. DA L GW131 R 10110 3 1 9 Tabl e 13

. DA L GW131 S 10110 3 1 9 Tabl e 14

. DA L GW131 L 10110 3 1 9 Tabl e 15

. DA L GW132 R 101102 2 0 Tabl e 16

. DA L GW132 S 101102 2 0 Tabl e 17

. DA L GW132 L 10110 3 2 0 Table18

. DALGW133R10110 2 2 1 Tabl e 19

. DA L GW133 S 10110 3 2 1 Tabl e 20

. DA L GW133 L 10110 3 2 1

Pag e 6 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 21

. DA L GW134 R 10110 5 2 2 Tabl e 22

. DA L GW134 S 10110 5 2 2 Tabl e 23

. DA L GW134 L 10110 5 2 2 Tabl e 24

. DA L GW135 R 10110 5 2 3 Tabl e 25

. DA L GW135 S 10110 5 2 3 Tabl e 26

. DA L GW135 L 10110 5 2 3 Table27

. DALGW136S10110 3 2 4 Table28

. DALGW136L10110 3 2 4 Table29

. DALGW137S10110 9 2 4 Table30

. DALGW137L10110 9 2 5 Table31.DALGW138S10111 0 2 5 Table32

. DALGW138L10111 0 2 5 Table33

. DALGWCW26R10111 0 2 6 Table34

. DALGWGVV26L10111 0 2 6 Table35

. DALGW140R10110 4 2 6 Table36

. DALGW141R10111 0 2 7 Table37

. DALGW142R10111 0 2 7 Table38

. DALGW144R10111 0 2 7 Tabl e 39

. Tri p Blan k

1 2 8 Table40

. TripBlank 2 2 8 Tabl e 41

. Tri p Blan k

3 2 8 Table42

. TripBlank 4 2 9 Tabl e 43

. Rinseat e Blank s 2 9

Pag e 7 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

. Westchester , P

A1938 0 Phone:(610)701-376 1 Fax:(610)701-740 1 j.kesari(@westonsolutions.co m Stud yLocatio n Testin g Facilit y 3 M EH S Operation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 Maplewood , M N 5510 6 Stud yPersonne l Willia m K

. Reagen , Ph.D. , 3 M Laborator yManage r Clesto n Lange , Ph.D. , Principa l Analytica l Investigator

. (clanqe(a).mmm.com) : phon e (651)-733-986 0 Susa n Wolf , 3 M Analys t Kevi n Eich ; Analys t Cheisi e Grochow , Analys t Jonatha n Steege ; Analys t Stud yDate s Stud yInitiation : Marc h 8 , 201 0 Interi m Repor

t 1 1 Experimenta l Tennination : Januar y8,201 1 Interi m Repor

t Completion : Dat e of Interi m Repor t Signin g Locatio n o f Archive s Al l origina l rawdat a an d th e analytica l repor t have bee n archive d a

t th e 3 M Environmenta l Laborator yaccordin g t o 4 0 CF R Par t 792

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

Pag e 8 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 2 Summar y Th e 3 M Environmenta l Laborator yreceive d groundwate rsample s fro m well s locate d a t th e Forme r Sludg e Incorporatio n Are a (FSIA) i n Decatur , AL , representin g thirt ydifferen t samplin g locations

. A tota l o f on e hundre d sixty-nin e sampl e bottle s were receive d a t th e 3 M Environmenta l Laborator yfo r perfluorooctanoat e (PFOA ) analysis , an d include d duplicat e groundwate rsample s fro m eac h samplin g location

. Sample s als o include d a t least two fiel d matri xspik e (FMS ) sample s fo reac h location , fou r tri p blan k sets containin g Milli-Q TM wate ran d appropriat e tri p blan k spikes , an d tw o equipmen t rinseates. I n addition , on e soi l equipmen t rinseate blan k fro m GLP10-01-01-1 2 wa s analyzed

. Th e equipmen t rinseate blank s di d no t have FM S sample s prepare d fo rdeterminatio n ofPFO Arecovery . Th e groundwate rsamples , tri p blank s an d two equipmen t rinseate blank s associate d wit h GLP10-01
- 01-1 0 were receive d fro m Westo n personne l o n Novembe r18 , 2010

. Th e equipmen t rinseate blan k associate d wit h GLP10-01-01-1 2 wa s receive d fro m Westo n personne l o n Octobe r15,2010

. Al l ofth e sample s were prepare d an d analyze d fo rPFO Afollowin g 3 M Environmenta l Laborator yMetho d ETS
8-044. 0 unde r3 M projec

t GLP-10-01-01-11

. Man yofth e groundwate rsample s require d dilutio n t o attai n PFO

Aconcentration s withi n th e rang e ofth e curve , i n som e instance s u p t o 100-fol d dilutio n were required

. Th e averag e measure d PFO Aconcentration s are summarize d i n Tabl e 1

. Th e equipmen t rinseates an d th e tri p blan k were belo

wth e lowe rlimi t ofquantitatio n (LLOQ ) of0.025 0 ng/mL , indicatin g adequat e contro l of sampl e contaminatio n durin g shippin g an d sampl e collections

. Th e PFO Aconcentratio n results fo ral l groundwater s range d ove rfou rorder

s ofmagnitud e fro m 0.27 1 ng/m L t o 291 0 ng/mL

. Th e analytica l uncertaint ywa s estimate d a

t 100 + 23%

.

Pag e 9 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO

Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 1

. Summarize d PFO AResult s (FSI AGroundwater , Decatur , AL , Novembe r2010 ) Sampl e I D DALGW130R10110 5 DALG W 130 8 1 0 110 5 DA L GW130 L 10110 5 DALG W 131 R 10110 3 DA L GW131 S 10110 3 DA L GW131 L 10110 3 DA L GW132 R 10110 2 DA L GW132 S 10110 2 DALGW132L10110 3 DA L GW133 R 10110 2 DALG W 133 8 10110 3 DA L GW133 L 10110 3 DA L GW134 R 10110 5 DALG W 134 8 1 0 110 5 DALGW134L10110 5 DA L GW135 R 10110 5 DALG W 135 8 10110 5 DALGW135L10110 5 DALG W 136 8 10110 3 DALGW136L10110 3 DALG W 137 8 10110 9 DALGW137L10110 9 DALG W 138 S 10111 0 DALG W 138 L 1 0 111 0 DA L GWCW26 R 10111 0 DA L GWCW26 L 10111 0 DA L GW140 R 10110 4 DALG W 141 R 10111 0 DALG W 142 R 10111 0 DALG W 144 R 10111 0 Tri p Blank s (Milli-Q TM Water ) GLP10-01-01-1 1 Equipmen t rinseate blanks : DA L G W 130 L an d DA L G W 144 R GLP10-01-01-1 2 Soi l Equipmen t rinseate blank : DA L 8 8 607 R Avg

. PFO A Concentratio n (ng/mL ) 79 3 17 4 70. 0 250 0 [a ] 24. 9 90. 7 25 1 96 2 40 4 10 2 38 5 25 2 1570[b l 5.4 9 52 0 291 0 [a l 13. 7 12 3 75. 4 75. 3 0.27 1 0.36 1 14 7 1.1 6 38 6 55 2 12 1 1.8 4 47. 6 57. 3 < 0.025 0
< 0.025 0

< 0.025 0 Relativ e

Percen t Differenc e 0.88 % 0.58 % 2.0 % 1.6 % 4.0 % 5.2 % 4.4 % 0.52 % 3.0 % 9.5 % 4.2 % 1.2 % 9.6 % 5.5 % 1.3 % 1.4 % 3.7 % 2.4 % 3.8 % 3.1 % 1.8 % 0.28 % 3.4 % 6.1 % 1.8 % 4.7 % 0.83 % 10 % 4.6 % 0.17 % N/ A N/ A N/ A N/A ; no t applicabl e Th e analytica l uncertaint yfo rPFO Awa s estimate d a t 10 0 + 23%

. [a ] Samplin g locatio n di d no t hav e a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . [b ] Th e analytica l uncertaint yha s bee n adjuste d fo rfiel d matri xspik e recoveryt o ±3 1 %

. 

### 3 Introductio n Thi s analytica l stud ywa s conducte d a s par t o fth e Phas e 3 Environmenta l Monitorin g an d Assessmen t Progra m fo rth e 3 M facilit ylocate d i n Decatur , Alabama

. Th e objectiv e o f th e overal l progra m i s t o gai n informatio n regardin g concentration s o fperfluorooctanoat e (PFOA ) i n variou s environmenta l medi a

Pag e 1 0 o

f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a • Novembe r201 0

suc h a s groundwater , soil s an d sediment s tha t ar e associate d wit h an d nea rth e Decatu rfacility

. Thi s analytica l stud ywa s conducte d t o analyz e groun d wate rsample s collecte d fro m variou s well s locate d a t th e Forme rSludg e incorporatio n Are a (F8AI ) i n Decatur , A L fo rPFO Ai n a n effort t o characteriz e regiona l groundwate rconditions

. Th e 3 M Environmenta l Laboratoryprepare d sampl e bottle s (25 0 m L high-densit ypolyethylene ) whic h wer e shippe d t o Decatur , A L Westo n personne l prio rt o fiel d sampling

. Sampl e bottl e set s fo reac h groundwate rsamplin g locatio n include d a fiel d sample , fiel d sampl e duplicate , an d a minimu m o f tw o fiel d spik e samples

. Eac h empt ycontaine rfo rgroundwate rsampling s wa s mari<e d wit h a "fil l t o here " lin e t o produc e a fina l sampl e volum e o f 20 0 mL

. Container s designate d fo rfiel d matri xsample s wer e fortifie d wit h a n appropriat e matri xspik e solutio n containin g PFO Aprio rt o bein g sen t t o th e fiel d fo r sampl e collection

. Se e sectio n 8. 8 o fth e report fo rfiel d matri xspik e levels

. Sample s wer e prepare d an d analyze d accordin g t o th e procedur e define d i n 3 M Environmenta l Laboratorymetho d ETS-8-044. 0 "Determinatio n o f Perfluorinate d Compound s i n Wate rb yHig h Performanc e Liqui d Chromatography/Mas s SpectrometryDirect Injectio n Analysis"

. Tabl e 1 summarize s th e averag e PFO Aconcentration s fo rth e duplicat e groundwate rsample s collected , th e tri p blank , an d equipmen t rinseate samples

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

. Al l result s fo rth e qualit ycontro l sample s prepare d an d analyze d wit h th e sample s ar e reporte d an d discusse d elsewher e i n thi s report

. 

### 4 Tes t & Contro l Substance s Ther e wa s no t a tes t substanc e o rcontro l substance s i n th e classi csens e o f a GL P study

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

. 

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

.

1 Referenc e Substanc e Chemica l Nam e Chemica l Formul a Identifie r Sourc e Expiratio n Dat e Storag e Condition s Chemica l Lo t Numbe r TC R Numbe r Physica l Descriptio n Purit y PFO A Perfluorooctanoat e C7F15COO H CA S # 335-67- 1 Oakwoo d Product s 09/29/201 2 Froze n 344 0 TCR07-004 1 Powde r 99.5 % PFO A Perfluorooctanoat e C7F15COO
Ammoniu m Sal t CA S # 335-67- 1 3 M 02/27/201 7 Froze n 33 2 TCR-12 3 Whit e Powde r 95 %

Pag e 1 1 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

6 Tes t Syste m There wa s no

t a tes t syste m fo rthi s stud yi n th e classi csens e o fa GL P study

. Thi s stud ywas conducte d fo ranalysi s of 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 " environmenta l samples

. Sampl e Descriptio n Ke yCode

. strin g Numbe r Exampl e 1 2 3

4 5 strin g Descripto r DA L 132 R 010110 2 Sampi e Locatio n Wei l I D Wei l Leve l
Samplin g Dat e Sampi e Typ e Exampl e DAL = Decatur , Alaliam a Example : 132 R = Residu m shallo wwater-bearin g zon e L = Bedroc k

water-bearin g zin e S = Epikars t middl e water-bearin g zon e 101102
- Novembe r2,201 0 0=primarysampl e 1=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 o f Perfluorinate d Compound s I n Wate rb yHig h Perfonnance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

.

-T M , 7. 2 Sampl e Collectio n Sample s were collecte d i n 25 0 m L Nalgene" " (high-densit ypolyethylene ) bottle s prepare d a t th e 3 M Environmenta l Laboratory

. Sampl e bottle s associate d wit h GLP10-01-01-1 1 were retume d t o th e laborator ya t ambien t condition s o n Novembe r18 , 2010

. Th e equipmen t rinseate blan k associate d wit h GLP10-0 1 -0 1 -1 2 wa s returne d t o th e laborator ya t ambien t condition s o n Octobe r15,2010

. Sample s were store d refrigerate d at th e laborator yafte rreceipt

. Aset o flaborator yprepare d Tri p Blan k

an d Tri p Blan k fiel d matri xspike s were sen t wit h eac h coole rofsampl e collectio n bottles

. 7. 3 Sampl e Preparatio n Sample s were prepare d byremovin g a n aliquot ofth e wel l mixe d sampl e an d placin g i t i n a n autovia l fo r analysis

. Sample s that require d dilutio n were prepare d b ydilution s Im L sampl e wit h 9 mLs o fMilli- Q wate r (dilutio n 1:10)

. Som e samplin g location s were dilute d 1:100 b ydilutin g th e 1:1 0 an d additona l wit h Milli
Q water

. 7. 4 Analysi s Al l stud ysample s an d qualit ycontro l sample s were analyze d fo rPFO Ausin g hig h perfonnance liqui d chromatography/tande m mas s spectrometr y(HPLC/MS/MS)

. Detaile d instrumen t parameters , th e

Pag e 1 2 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a • Novembe r201 0

liqui d chromatograph ygradien t program , an d th e specifi cmass transition s analyze d ar e describe d i n th e ra wdat a har

d copie s place d i n th e fina l data packet , an d ar e briefl ydescribe d belowi n Tabl e 2 , Tabl e 3 an d Tabl e 4

. Tabl e 2

. Instrumen t Parameters

. Instrumen t Nam e Analytica l Metho d Followe d Analysi s Dat e Liqui d Chromatograp h Guar d colum n Analytica l colum n Injectio n Volum e Mas s Spectromete r Io n Sourc e Electrod e Polarit y Softwar e ETS Buste r ETS-8-044. 0 1/3/11-1/8/1 1 Agilen t 1100 Pris m R P (2. 1 m m X 5 0 mm) , 5 n Betasi l C1 8 (2. 1 m m X 100 mm) , 5 u

2or10n L /Applied Biosystem s AP I 400 0 Turb o Spra

y Turb o io n electrod e Negativ e Analyst 1.4. 2 Tabl e 3

. Liqui d Chromatograph yConditions

. ste p Numbe r 0 1 2 3 4 5 Tota l Tim e

(min ) 0 2. 0 11. 5 13. 5 13. 6 17. 0 Flo wRat e

(nUmin ) 30 0 30 0 30 0 30 0 30 0 30 0 Percen t A

( 2 m M ammoniu m acetate )

. 97. 0 97. 0 5. 0 5. 0 97. 0 97. 0 Percen t B

(Methanol ) 3. 0 3. 0 95. 0 95. 0 3. 0 3. 0 Tabl e 4

. Mas s Transitions

.

Analyt e
PFO A Mas s Transitio n

Q1/Q 3 413/36 9 413/21 9 413/16 9 Dwel l tim e wa s 10 0 mse cfo reac h transition

. Th e individua l transition s w/er e summe d t o produce a "tota l io n chromatogram " (TIC) , whic h wa s use d fo rquantitation

.
8 Analytica l Result s 8. 1 Calibratio n Sample s were analyze d against a n extema 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 a laboratory
Mill i Q water

. Atota l o f fiftee n spike d standard s rangin g fro m 0.02 5 ng/m L t o 10 0 ng/m L (nominal ) were

Pag e 1 3 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

prepared

. Th e tw o highest curve points were disable d t o meet linearit ycriteria

. Aquadratic , 1/

x weighted , calibratio n curve of th e pea k are a counts wa s use d t o fi t th e dat a fo rPFOA

. Th e data were not force d throug h zero durin g th e fittin g process . Calculatin g th e standar d concentration s usin g th e pea k are a confinne d accurac

yo f eac h curve point

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

yrequirements of 100±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 rPFOA

. 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 was met fo rPFOA

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

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

yrequirements an d fo rwhic h th e are a counts are a t least twic e 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 5

. Tabl e 5

. Limi t o f Quantitatio n (LOQ)

. Analysi s Dat e 1/3/1 1 PFOA

LOQ , ng/m L 0.025 0 

### 8. 4 Continuin g Calibratio n Durin g th e cours e o f eac h analytica l sequence , continuin g calibratio n verificatio n sample s (CCVs ) were analyze d t o confir m that th e instrumen t respons e an d th e initia l calibratio n curve were stil l i n control

. Al l CCV s met metho d criteri a o f 100 % ±25 % fo rPFOA

. 

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

s were prepare d an d analyze d wit h th e samples : solven t blanks , tri p blank s an d equipmen t rinseate blanks

. Solven t blan k results were reviewe d an d use d t o evaluat e metho d performance t o determin e th e LO Q fo rPFOA

. Tri p blank s reflec t th e shippin g an d sampl e collectio n conditon s th e sampl e bottle s an d sample s experience

. Equipmen t rinseate blank s are aqueou s sample s that reflec

t th e efficienc

yof equipmen t cleanin g i n th e fiel d betwee n differen t sampl e collection s an d ar e proof o f n o cros s contaminatio n ofsample s fro m th e equipment

. 

### 8. 6 La b Contro l Spilte s (LCSs ) Low , mid , an d high-leve l la b contro l spike s were prepare d an d analyze d i n triplicat e wit h eac h preparatio n set

. LCS s were prepare d b yspikin g know n amounts ofth e analyt e into 4 0 m L oflaborator y Mill i Q water , t o produce th e desire d concentration

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

. Th e metho d acceptance criteria , averag e ofLC S a t eac h leve l shoul d b e withi n 100 % ±20 % wit h a n RS D <2i3/o , were met fo rth e linea rPFO ALC S samples

. As th e reference material s use d fo rquantitatio n ofPFO Ai s predominantl ylinear , an d th e PFO Apresen t i n th e wate rsample s are comprise d of linea ran d branche d isomers , additiona l LC S sample s o flinea r an d branche d PFO

Awere prepare d a

t thre e concentration s t o evaluat e th e potentia l fo ranalytica l bias

. Th e averag e recover

yof th e linea ran d branche d LC S a t th e lo wan d hig h level s met metho d acceptance criteria

. Th e mid-leve l linea ran d branche d LC S had a n averag e recover yof123%

. Ai l LC S sample s were use d i n th e determinatio n ofmetho d uncertaint yi n sectio n 8.7

.

Pag e 1 4 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Th e followin g calculation s were use d t o generat e dat a i n Tabl e 6 fo rlaborator ycontro l spikes :
LC S Percen t Recover

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

y Tabl e 6

. Laborator yContro l Spik e Recovery

. ETS-8-044. 0 Analyze d 1/3/201 1

La b I D LCS-101230- 1 LCS-101230- 2 LCS-101230- 3 Averag e ±%RS D LCS-101230- 4 LCS-101230- 5 LCS-101230- 6 Averag e ±%RS D LCS-101230- 7 LCS-101230- 8 LCS-101230- 9 Averag e ±%RS D Linea rPFO A Spike d Concentratio n (ng/mL ) 0.49 7 0.49 7 0.49 7 Calculate d

Concentratio n (ng/mL ) 0.58 0 0.55 7 0.59 0 VoRecover y

11 7 11 2 11 9 116 % ±3.1 % 4.9 7 4.9 7 4.9 7 5.8 3

5.6 9 5.6 9 11 7

11 5 114 115 % ±1.3 % 29. 9 29. 9 29. 9 25. 6

25. 8 25. 7 85. 6

86. 3 85. 9 85.9 % ±0.41 % ETS-8-044. 0 Analyze d 1/3/201 1

La b I D LCS-101230-1 0 EC F LCS-101230-1 1 EC F LCS-101230-1 2 EC F Averag e ±%RS D LCS-101230-1 3 EC F LCS-101230-1 4 EC F LCS-101230-1 5 EC F Averag e ±%RS D LCS-101230-1 6 EC F LCS-101230-1 7 EC F LCS-101230-1 8 EC F Averag e ±%RS D Linea r+ Branche d PFO A Spike d Concentratio n (ng/mL ) 0.49 8 0.49 8 0.49 8 Calculate d

Concentratio n (ng/mL ) 0.54 6 0.55 3 0.54 1 YoRecover y

11 0 11 1 10 9 110 % ±0.91 % 4.9 9 4.9 9 4.9 9 6.2 9

6.0 3 61 2 12 6

12 1 12 3 123 % ±2.0%' " 29. 9 29. 9 29. 9 31. 3

30. 8 30. 6 10 5

10 3 10 2 103 % ±1.5 % (1 ) Laborator

ycontro l sampl e averag e recover ydi d no t mee t metho d acceptance criteri a o f100 % ±20%

.

Pag e 1 5 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



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

yi s base d o n historica l Q C 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 Q C samples

. Th e expande d uncertaint

yi s calculate d b

ymultiplyin g th e standar

d deviatio n b

ya facto rof2 , whic h con-espond s t o a confidence leve l of 95%

. Tabl e 7

. Analytica l IVIetho d Uncertainty

. Analyt e PFO A Metho d

ETS-8-044. 0 Standar d Deviatio n 11. 3 Metho d

Uncertaint y ±23 % 8. 8 Fiel d Matri xSpike s (FMS ) Aminiu m of two 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 of fiel d sampl e t o a containe rspike d b yth e laborator

ywit h th e targe t analyte s prio rt o shippin g sampl e container

s fo rsampl e collection

. Fiel d matri xspik e recoverie s withi n metho d acceptance criteri a of 100±30 % 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 analysi s of th e analyte s o finterest

. Fiel d matri xspike concentration s must b e 50 % of th 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 o f thi s report

. Tabl e 8

. Fiel d Matri xSpik e Levels

. Samplin g Locatio n 136R , 137R , 137s , 137L , 138 L
130L , 131L , 131S , 133R , 134S , 135S , 136 S 130R , 130S , 132R , 132L , 132S , 133S , 133L , 134L , 135L , 136L , 138S , 138R , CW26R , CW26L , 140R , 141R , 142R , 143R , 144 R 131R , 134R , 135 R
Tri p Blan k Spik e Leve l Lo w Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h PFOA , ng/m L

0.099 1 0.99 1 9.9 1 0.99 1 9.9 1 99. 1 9.9 1 99. 1 99 1 99. 1 99 1 0.99 1 9.9 1 99. 1 99 1

^
. ,„ „ (SarapleConcentratio no f FMS-Averag e Concentration: Fiel dSampl e & FieldSampl

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

Pag e 1 6 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 9 Dat a Summar yan d Discussio n Th e table s belowsummariz e th e sampl e results an d field matri xspik e recoverie s fo rth e samplin g location s a s wel l a s th e Tri p Blank s an d rinseate blanks

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

. Becaus e o frounding , 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 of±30% , demonstrat e that th e metho d wa s appropriat e fo rth e give n matri xan d thei rrespective quantitative ranges . DA L G W 134R10110 4 - Th e high-leve l FM S di d meet metho d acceptance criteri a wit h a recover yof 69.1%

. Th e low-leve l FM S wa s no t appropriat e a s compare d t o th e sampl e concentration

. Th e analytica l uncertaint

yhas bee n adjuste d fo rPFO At o ±3 1 %

. DA L G W 1 SI R 10110 3 - Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no

t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery . DA L G W 135R10110 5 - Du e t o th e hig h concentratio n ofPFO Adetecte d i n th e sample , thi s samplin g locatio n di d no

t have a n appropriat e FM S spik e leve l t o sufficientl yevaluat e PFO Arecovery .

Pag e 1 7 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tables

. DALG W 130 R 10110 5

3MUIVISI D GLP10-01-01-11-00 1 GLP10-01-01-11-00 2 GLP10^1-01-11-00 3 GLP10-01-01-11-00 4 GLP10-01-01-11-00 5 Descriptio n DA L GW130 R 010110 5 DALGW130RDB10110 5 DALGW130RLS10110 5 DALGW130RMS10110 5 DALGW130RHS10110 5 Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 78 9 79 6 80 5 89 5 1680 YoRecovery

^ N A N A N C N C 89. 6 79 3 ng/m L ±0.88 % NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 10

. DALG W 130 3 10110 5

3 M LIM S I D GLP10-01-01-11-00 6 GLP10-01-01-11-00 7 GLP10-01-01-11-00 8 GLP10-01-01-11-00 9 GLP10-01-01-11-01 0 Descriptio n DA L GW130 S 010110 5 DA L GW130SD B 101105 DALGW130SLS10110 5 DALGW130SMS10110 5 DA L GW130SH S 101105 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 17 4 17 3 183 27 0 115 0 YoRecover

y N A N A N C 97. 4 98. 5 174 ng/m L ±0.58Y

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

. Tabl e 11

. DALG W 1 SOL 10110 5

3 M LIM S I D GLP10-01-01-11-01 1 GLP10-01-01-11-01 2 GLP10-01-01-11-01 3 GLP10-01-01-11-01 4 GLP10-01-01-11-01 5 Descriptio n DA L GW130 L 0 101105 DALGW130LDB10110 5 DALGW130LLS10110 5 DALGW130LMS10110 5 DALGW130 L H S 101105 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 69. 3 70. 7 71. 0 73. 3 16 2 YoRecover

y NA NA N C N C 92. 8 70. 0 ng/m L 12.0Y

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

.

Pag e 1 8 of 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 12

. DA L G W 131R10110 3

3 M LIM S I D GLP10-01-01-11-01 7 GLP10-01-01-11-01 8 GLP10-01-01-11-01 9 GLP10^1-01-11-02 0 Descriptio n DA L GW131R 0 101103 DA L GW131RD B 101103 DA L GW131RL S 101103 DA L GW131RH S 101103 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 252 0 248 0 2b/ U 324 0 YoRecovery

^ NA NA N C N C 250 0 ng/m L ±1.6Yo'^

^ N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Samplin g locatio n di d no t hav e a n appropriate spike leve l t o evaluate PFO Arecoveiy

. Tabl e 1S

. DA L G W1 S I S 10110 S

3 M LIM S I D GLP10-01-01-11-02 1 GLP10-01-01-11-02 2 GLP10-01-01-11-02 3 GLP10-01-01-11-02 4 GLP10-01-01-11-02 5 Descriptio n DA L GW131 S 010110 3 DALGW131SD B 101103 DALGW131SL S 101103 DALGW131 S M S 101103 DALGW131SH S 101103 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 25. 4 24. 4 25. 3 34. 6 12 7 YoRecover

y N A N A N C N C 103 24. 9 ng/m L ±4.0Y

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

. Tabl e 14

. DA L G W 131 L 10110 S

3 M LIM S I D GLP10-01-01-11-02 6 GLP10-01-01-11-02 7 GLP10-01-01-11-02 8 GLP10-01-01-11-02 9 GLP10-01-01-11-03 0 Descriptio n DA L G W 131 L 010110 3 DA L GW131LD B 101103 DA L GW131LL S 101103 DA L G W 131 L M S 101103 DA L GW131LH S 101103 Averag e Concentratio n (ng/mL ) ±YoRPD PFOA Concentratio n (ng/mL ) 88. 3 93. 0 87. 7 96. 9 179 YoRecover

y NA NA N C N C 89. 2 90. 7 ng/m L ±5.2Y

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

.

Pag e 1 9 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 15

. DALG W 1S2R10110 2

3 M LIM S I D GLP10-01-01-11-03 1 GLP10-01-01-11-032 GLP10-01-01-11-03 3 GLP10-01-01-11-034 GLP10-01-01-11-03 5 Descriptio n DA L GW132 R 010110 2 DALGW132RDB10110 2 DALGW132RLS10110 2 DALGW132RMS10110 2 DA L GW132RH S 101102 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 25 6 24 5 26 7 35 6 116 0 YoRecover

y N A N A N C N C 91. 8 25 1 ng/m L ±4.4Y

o NA= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 16

. DALG W132 8 10110 2

3 M LIM S I D GLP10-01-01-11-03 6 GLP10-01-01-11-03 7 GLP10-01-01-11-03 8 GLP10-01-01-11-03 9 GLP10-01-01-11-04 0 Descriptio n DA L GW132 S 010110 2 DALGW132SD B 101102 DALGW132SL S 101102 DALGW132SMS10110 2 DALGW132SHS10110 2 Averag e Concentratio n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 95 9 96 4 92 6 102 0 181 0 YoRecover

y NA NA N C N C 85. 6 96 2 ng/m L ±0.52Y

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

. Tabl e 17

. DALG W1S2L10110 3

3 M LIM S I D GLP10-01-01-11-04 1 GLP10-01-01-11-042 GLP10-01-01-11-04 3 GLP10-01-01-11-044 GLP10-01-01-11-04 5

Averag e Con e Descriptio n

DA L GW132 L 010110 3 DALGW132LDB10110 3 DALGW132LLS10110 3 DALGW132LMS10110 3 DA L GW132LH S 101103 entratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 39 8 41 0 45 1 48 2 129 0 YoRecover

y NA NA N C N C 89. 4 40 4 ng/m L ±3.0Y

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

.

Pag e 2 0 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 18

. DA L G W 1SS R 10110 2

3 M LIM S I D GLP10-01-01-11-04 6 GLP10-01-01-11-04 7 GLP10-01-01-11-04 8 GLP10-01-01-11-04 9 GLP10-01-01-11-05 0 Descriptio n DA L GW133 R 010110 2 DA L GW133RD B 101102 DALGW133RLS10110 2 DALGW133RMS10110 2 DALGW133RHS10110 2 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 107 97, 3 10 2 108 193 YoRecover

y NA NA N C N C 91. 7 102 ng/m L ±9.5Y

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

. Tabl e 19

. DALG W 1SSS 10110 3

3 M LIM S I D GLP10-01-01-11-05 1 GLP10-01-01-11-05 2 GLP10-01-01-11-05 3 GLP10-01-01-11-05 4 GLP10-01-01-11-05 5 Descriptio n DA L GW133 S 010110 3 DALGW133SDB10110 3 DALGW133SLS10110 3 DALGW133SMS10110 3 DALGW133SHS10110 3 Averag e Concentratio n (ng/mL ) ±YoRPD PFOA Concentratio n (ng/mL ) 39 3 37 7 40 7 48 5 126 0 YoRecover

y NA NA N C N C 88. 3 38 5 ng/m L ±4.2Y

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

. Tabl e 20

. DALG W1 SS L 10110 3

3 M LIM S I D GLP10-01-01-11-05 6 GLP10-01-01-11-05 7 GLP10-01-01-11-05 8 GLP10-01-01-11-05 9 GLP10-01-01-11-06 0 Descriptio n DA L GW133 L 010110 3 DALGW133LDB10110 3 DALGW133LLS10110 3 DA L GW133 L M S 101103 DALGW133LHS10110 3 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 25 3 25 0 26 5 35 5 119 0 25 2 ng/m L YoRecover

y N A N A N C N C 94. 7 ±7.2 % N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

.

Pag e 2 1 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 21

. DA L G W 1S4 R 10110 5

3 M LIM S I D GLP10-01-01-11-06 1 GLP10-01-01-11-06 2 GLP10-01-01-11-06 3 GLPiaO1-01-11-06 4 Descriptio n DA L GW134 R 010110 5 DALGW134RDB10110 5 DALGW134RLS10110 5 DALGW134RHS10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 164 0 149 0 162 0 225 0 YoRecover y

N A N A N C 69. 1 <^ ' 157 0 ng/m L ±9.6Y o N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Fiel d matri xspike di d not meet metho d acceptance criteri a of 100 % ±30%

. Tabl e 22

. DA L G W 1S4 S 10110 5

3 M LIM S I D GLP10-01-01-11-06 5 GLP10-01-01-11-06 6 GLP10-01-01-11-06 7 GLP10-01-01-11-06 8 GLP10-01-01-11-06 9 Descriptio n DA L GW134 S 010110 5 DALGW134SDB10110 5 DALGW134SLS10110 5 DALGW134SMS10110 5 DALGW134SHS10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 5.6 4 5.3 4 6.9 5 16. 6 10 2 YoRecover y

N A N A N C 11 2 97. 4 5.4 9 ng/m L ±5.5Y o N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. Tabl e 23

. DALG W 1S4 L 10110 5

3 M LIM S I D GLP10-01-01-11-07 0 GLP10-01-01-11-07 1 GLP10-01-01-11-07 2 GLP10-01-01-11-07 3 GLP10-01-01-11-07 4 Descriptio n DA L GW134 L 010110 5 DALGW134LDB10110 5 DALGW134LLS10110 5 DALGW134LMS10110 5 DALGW134LHS10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 52 3 51 6 53 0 59 9 139 0 YoRecover y

N A N A N C N C 87. 8 52 0 ng/m L ±1.3Y o N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

.

Pag e 2 2 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 24

. DA L G W 1 SS R 10110 5

3 M LIM S I D GLP10-01-01-11-07 5 GLP10-01-01-11-07 6 GLP10-01-01-11-07 7 GLP10-01-01-11-07 8 Descriptio n DA L GW135 R 010110 5 DA L GW135RD B 10110 5 DA L GW135RL S 10110 5 DALGW135RHS10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 293 0 289 0 293 0 384 0 YoRecover y

N A N A N C N C 291 0 ng/m L ±1.4Yo'^ ' N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

. (1 ) Samplin g locatio n di d no t have a n appropriate spik e leve l t o evaluate PFO

Arecovery . Tabl e 25

. DA L G W 135 3 10110 5

3 M LIM S I DCJ)O•<-CNCOt^00COCOCO22222IIIII99999mila.a.a.a.a._i_i_i_i_iCDCDCDCDCD Descriptio n

DA L GW135 S 010110 5 DA L GW135SD B 10110 5 DA L GW135SL S 10110 5 DALG W 135 8 M S 10110 5 DALGW135SHS10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 13. 9 13. 4 14. 5 24. 2 110 YoRecover y

N A N A N C 10 6 97. 2 13. 7 ng/m L ±3.7Y o N A= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. Tabl e 26

. DA L G W 1S5 L 10110 5

3 M LIM S I D GLP10-01-01-11-08 4 GLP10-01-01-11-08 5 GLP10-01-01-11-08 6 GLP10-01-01-11-08 7 GLP10-01-01-11-08 8 Descriptio n DA L GW135 L 010110 5 DALGW135LDB10110 5 DA L GW135LL S 10110 5 DALGW135LMS10110 5 DA L GW135LH S 10110 5 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 12 4 12 1 12 9 22 6 107 0 YoRecover y

N A N A N C 10 4 95. 6 12 3 ng/m L ±2.4Y o N A= No t /Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

.

Pag e 2 3 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 27

. DA L G W 1S6 S 10110 3

3 M LIM S I D GLP10-01-01-11-08 9 GLP10-01-01-11-09 0 GLP10-01-01-11-09 1 GLP10-01-01-11-09 2 GLP10-01-01-11-09 3 Descriptio n DA L GW136 S 010110 3 DALGW136SDB10110 3 DALGW136SLS10110 3 DALGW136SMS10110 3 DALGW136SHS10110 3 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 73. 9 76. 8 77. 6 86. 1 166 YoRecover

y N A N A N C N C 91. 5 75. 4 ng/m L ±3.8Y

o NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2 xspik e level

. Tabl e 28

. DA L G W 1S6 L 10110 3

3 M LIM S I D GLP10-01-01-11-09 4 GLP10-01-01-11-09 5 GLP10-01-01-11-09 6 GLP10-01-01-11-09 7 GLP10-01-01-11-09 8 Descriptio n DA L GW136 L 010110 3 DALGW136LDB10110 3 DA L GW136LL S 101103 DALGW136LMS10110 3 DA L GW136LH S 101103 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 74. 1 76. 4 86. 2 16 9 1030 YoRecover

y NA NA N C 94. 6 96. 3 75. 3 ng/m L ±3.1Y

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

. Tabl e 29

. DA L G W1S7 S 10110 9

3 M LIM S I D GLP10-01-01-11-09 9 GLP10-01-01-11-10 0 GLP10-01-01-11-10 1 GLP10-01-01-11-10 2 GLP10-01-01-11-10 3 Descriptio n DA L GW137 S 010110 9 DA L GW137SD B 10110 9 DALGW137SLS10110 9 DA L GW137 S M S 10110 9 DA L GW137SH S 10110 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 0.27 3 0.26 8 0.35 0 1.3 2 10. 9 YoRecover

y NA NA N C 106 107 0.27 1 ng/m L ±I.8Y

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

.

Pag e 2 4 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e SO

. DA L G W 137 L 10110 9

3 M LIM S I D GLP10-01-01-11-10 4 GLP10-01-01-11-10 5 GLP10-01-01-11-10 6 GLP10-01-01-11-10 7 GLP10-01-01-11-10 8 Descriptio n DA L GW137 L 010110 9 DALGW137LDB10110 9 DALGW137LLS10110 9 DALGW137LMS10110 9 DALGW137LHS10110 9 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 0.36 0 0.36 1 0.45 8 1.4 0 10. 7 YoRecover

y N A N A N C 10 5 10 4 0.36 1 ng/m L ±0.28Y

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

. Tabl e 31

. DA L G W 138 3 10111 0

3 M LIM S I D GLP10-01-01-11-10 9 GLP10-01-01-11-11 0 GLP10-01-01-11-11 1 GLP10-01-01-11-11 2 GLP10-01-01-11-11 3 Descriptio n DA L GW138 S 010111 0 DALGW138SD B 10111 0 DALGW138SL S 10111 0 DALGW138SMS10111 0 DALGW138SHS10111 0 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 149 14 4 162 23 0 102 0 YoRecover

y NA NA N C 84. 3 88. 1 14 7 ng/m L ±3.4Y

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

. Tabl e S2

. DA L G W 1 SS L 10111 0

3 M LIM S I D GLP10-01-01-11-11 4 GLP10-01-01-11-11 5 GLP10-01-01-11-11 6 GLP10-01-01-11-11 7 GLP10-01-01-11-11 8 Descriptio n DA L GW138 L 010111 0 DA L GW138LD B 10111 0 DA L GW138LL S 10111 0 DA L GW138 L M S 10111 0 DA L GW138LH S 10111 0 Averag e Concentrati'o n (ng/mL ) ±%RP D PFOA Concentratio n (ng/mL ) 1.1 9 1.1 2 1.2 4 2.1 8 11. 2 YoRecover

y NA N A N C 103 10 1 1.1 6 ng/m L ±6.1Y

o NA= No t Applicabl e N C = No t Calculated ; Endogenou s sampl e concentratio n greate rtha n 2xspik e level

.

Pag e 2 5 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e SS

. DA L G W CW26 R 10111 0

3 M LIM S I D GLP10-01-01-11-11 9 GLP10-01-01-11-12 0 GLP10-01-01-11-12 1 GLP10-01-01-11-12 2 GLP10-01-01-11-12 3 Descriptio n DA L GWCW26 R 010111 0 DA L GWCW26RD B 10111 0 DA L G W CW26 R L S 10111 0 DA L GWCW26 R M S 10111 0 DA L GWCW26RH S 10111 0 Averag e Concentrati'o n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 38 2 38 9 39 5 45 0 129 0 YoRecover y

N A N A N C N C 91. 3 38 6 ng/m L ±1. 8 Y

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

. Tabl e 34

. DA L G W CW26 L 10111 0

3 M LIM S I D GLP10-01-01-11-12 4 GLP10-01-01-11-12 5 GLP10-01-01-11-12 6 GLP10-01-01-11-12 7 GLP10-01-01-11-12 8 Descriptio n DA L GWCW26 L 010111 0 DA L GWCW26 L D B 10111 0 DA L G W CW26 L L S 10111 0 DA L G W CW26 L M S 10111 0 DA L G W CW26 L H S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 56 5 53 9 55 2 62 3 148 0 YoRecover y

N A N A N C N C 93. 6 55 2 ng/m L ±4. 7 Y

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

. Tabl e 35

. DA L G W 140 R 10110 4

3 M LIM S I D GLP10-01-01-11-12 9 GLP10-01-01-11-13 0 GLP10-01-01-11-13 1 GLP10-01-01-11-13 2 GLP10<31-01-11-13 3 Descriptio n DA L GW140 R 010110 4 DALGW140RDB10110 4 DALGW140RLS10110 4 DALGW140RMS10110 4 DALGW140RHS10110 4 Averag e Concentratio n (ng/mL ) ±YoRP D PFO A Concentratio n (ng/mL ) 12 1 12 0 12 8 21 7 97 3 YoRecover y

N A N A N C 97. 4 86. 0 12 1 ng/m L ±0.8 3 Y

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

.

Pag e 2 6 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

Tabl e 36

. DA L G W 141 R 10111 0

3 M LIM S I D GLP10-01-01-11-134 GLP10-01-01-11-13 5 GLP10-01-01-11-13 6 GLP10-01-01-11-13 7 GLP10-01-01-11-13 8 Descriptio n DA L GW141R 0 10111 0 DALG W 14 1 RD B 10111 0 DALG W 14 1 RL S 10111 0 DALG W 14 1 RM S 10111 0 DALG W 14 1 RH S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 2.1 3 1.5 5 11. 4 95. 5 90 8 YoRecover

y NA NA 96. 5 94. 5 91. 4 1.8 4 ng/m L ±1 0 Y

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

. Tabl e 37

. DA L G W 142 R 10111 0

3 M LIM S I D GLP10-01-01-11-13 9 GLP10-01-01-11-14 0 GLP10-01-01-11-14 1 GLP10-01-01-11-142 GLP10-01-01-11-14 3 Descriptio n DA L GW142R 0 10111 0 DALGW142RDB10111 0 DA L GW142RL S 10111 0 DA L GW142 R M S 10111 0 DA L GW142RH S 10111 0 Averag e Concentratio n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 46 5 48. 7 55. 3 143 92 5 YoRecover

y NA NA N C 96. 3 88. 5 47. 6 ng/m L ±4. 6 Y

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

. Tabl e 38

. DA L G W144 R 10111 0

3 M LIM S I D GLP10-01-01-11-144 GLP10-01-01-11-14 5 GLP10-01-01-11-14 6 GLP10-01-01-11-14 7 GLP10-01-01-11-14 8 Descriptio n DA L GW144 R 010111 0 DALGW144RDB10111 0 DALGW144RLS10111 0 DALGW144RMS10111 0 DALGW144RHS10111 0 Averag e Concentrati'o n (ng/mL ) ±YoRP D PFOA Concentratio n (ng/mL ) 57. 2 57. 3 67. 6 14 2 96 6 YoRecover

y N A NA N C 85. 5 91. 7 57. 3 ng/m L ±0.1 7 Y

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

.

Pag e 2 7 o f 5 3Tabl e 39

. Tri p Blan k 1

N A= No t Applicabl e Tabl e 40

. Tri p Blan k

2

N A= No t Applicabl e Table41

. Tri p Blank s GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

3 M LIM S I D GLP10-01-01-11-15 0 GLP10-01-01-11-15 1 GLP10-01-01-11-15 2 GLP10-01-01-11-15 3 GLP10-01-01-11-15 4 Descriptio n TRI P BLAN K1 0 TRI P BLAN K1 LS TRI P BLAN K1 M S TRI P BLAN K1 MH S TRI P BLAN K1 H S PFOA Concentratio n (ng/mL ) <0.025 0 1.0 8 10. 6 99. 1 1040 %Recovery

NA 109 107 100 10 5

3 M LIM S I D GLP10-01-01-11-15 5 GLP10-01-01-11-15 6 GLP10-01-01-11-15 7 GLP10-01-01-11-15 8 GLP10-01-01-11-15 9 Descriptio n TRI P BLAN K2 0 TRI P BLAN K2 L

S TRI P BLAN K2 M S TRI P BLAN K2 MH S TRI P BLAN K2 H S PFOA Concentratio n (ng/mL ) <0.025 0 1.0 8 10. 9 96. 9 102 0 %Recovery

NA 109 11 0 97. 8 103

3 M LIM S I D GLP10-01-01-11-16 0 GLP10-01-01-11-16 1 GLP10-01-01-11-16 2 GLP10-01-01-11-16 3 GLP10-01-01-11-16 4 Descriptio n TRI P BLAN K3 0 TRI P BLAN K3 L

S TRI P BLAN K3 M S TRI P BLAN K3 MH S TRI P BLAN K3 H S PFOA Concentratio n (ng/mL ) <0.025 0 1.0 7 10. 4 10 1 105 0 YoRecover

y NA 108 10 5 10 2 106 N A= No t Applicabl e

Pag e 2 8 o f5 3Tabl e 42

. Tri p Blan k 4

N A= No t Applicabl e Tabl e 43

. Rinseat e Blank s GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

3 M LIM S I D GLP10-01-01-11-16 5 GLP10-01-01-11-16 6 GLP10-01-01-11-16 7 GLP10-01-01-11-16 8 GLP10-01-01-11-16 9 Descriptio n TRI P BLAN K4 0 TRI P BLAN K4 L

S TRI P BLAN K4 M S TRI P BLAN K4 MH S TRI P BLAN K4 H S PFOA Concentratio n (ng/mL ) <0.025 0 1.0 6 10. 4 95. 4 98 5 YoRecover

y NA 107 10 5 96. 3 99. 4

3 M LIM S I D GLP10-01-01-11-01 6 GLP10-01-01-11-14 9 GLP10-01-01-12-00 9 Descriptio n DALGW130LRB10110 5 DA L GW144RR B 10111 0 DA L S S 607 R R B 004 0 PFOA Concentratio n (ng/mL ) <0.025 0 <0.025 0 <0.025 0 YoRecover y NA NA NA N A= No t Applicabl e

Pag e 2 9 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

1 0 Conclusio n Laborator ycx)ntro l spike s an d fiel d matri xspike s were use d t o determin e th e analytic^a l metho d accurac yan d precisio n fo rPFOA

. Analysi s was 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 (hardcop

yan d electronic) wil l b e archive d accordin g t o 3 M Environmenta l Laborator ystandar d operatin g procedures

. 1 2 Attachment s Attachmen t A : Protoco l Amendmen t 1 1 (Genera l Projec t Outline ) Attachmen t B : Representative Chromatogram s an d Calibratio n Curve s Attachmen t C : Analytica l Metho d - ETS-8-044. 0 Attachmen t D : Metho d Deviatio n

Pag e 3 0 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 1 3 Signature s

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

### 5^/6^;gf ^o/ / Willia m K

. Reagen , Ph.D. , 3 M Environmenta l Laborator yManage r 

# 1

. Date

Gar yHohenstein , 3 M Sponso rRepresentative 

# OM/i l 2



# m _ Date 

# 2M l Jaisimh a Kesaffi , Stud yDirecto r 

### Jate

Pag e 3 1 o f 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Attachmen t AForme rSludg e Incorporatio n Are a - Novembe r201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 1



### Stud yTitl e Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

3 M Decatu rPlias e 3 Site-Relate d Monitorin g Progra m

PROTOCO L AMENDMEN TNO

. 1 1

Amendmen t Date : Octobe r20 , 201 0
Performin g Laborator y SIV I Environmental , Health , an d SafetyOperation s 3 M Environmenta l Laborator y Buildin g 260-5N-1 7 IVIaplewood , IVI N 55144-100 0

Laborator yProjec t Identificatio n

GLP10-01-0 1
Samplin g Even t Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r

Pag e 1 o f7 Pag e 32 of 5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Attachment A'Trf^Fy>tl^ W P?S&!''b'tm'^8n r^°' °

Amendmen t 1 1 

### Thi s amendnnen t modifie s th e followin g portio n o fprotocol : "Analysi s of Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e

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

PROTOCO L READS : N o change s t o th e wordin g o f th e protoco l ar e required

.

AMEN D T

O READ : N o change s t o th e wordin g o f th e protoco l ar e required

. Thi s amendmen t onl yaddresse s an d document s th e additio n o f th e Genera l Project Outlin e (GPO ) fo rth e collectio n an d analysi s o fgroundwate rsample s a t Decatur , AL , an d conducte d a s par t ofth e 3 M Decatu rPhas e 3 Progra m fo rPFOA(GLP10-01-01)

. Th e anticipate d sampl e collectio n wil l occu raroun d th e timefram e o fOctobe r25 , 2010

. Th e groundwate r sample s fo rthi s samplin g even t wil l b e entere d int o th e 3 M Environmenta l Laborator yLIM S a s projec

t GLP10-01-01-1 1 an d reporte d a s interi m repor t GLP10-01-01-11 , (reflectin g stud yGLP10-01-0 1 an d amendment-11)

.

Reason : Th e reaso n fo rthi s amendmen t i s t o documen t th e Genera l Project Outlin e (GPO ) whic h describe s th e anticipat e groundwate rsampl e collectio n even t t o b e conducte d fo rth e 3 M Decatur , A L facility

. Th e GP O i s fou rpage s i n lengt h an d include d as attache d t o thi s amendmen t form

.

Pag e 2 o f7 Pag e 3 3 o f 5 3Attachmen t A GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r 

# '%%imi^r8i^csmm^sn^'''°' °

Amendmen t 1 1 

### Amendmen t Approva l 

# %i-

. '1 0 Gar yHohenstein , Sponso rRepresentative Dat e

Date Clesto n C

. Lange , Principa l Analytica l Investigato r


## ? / OC / 

# i^o / 0 Willia m Reagen , EH S Opn s Environmenta l La b Managemen t

Jaisimh a Kesatf P.E. , DEE , Stud yDirecto r Dat e

#

Pag e 3 o f7

Pag e 3 4 o f 5 3Attachmen t A GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r

Amendmen t 1 1

ovember201 0



### wIV I Environmenta l Healt h & SafetyOperations , Environmenta l Laborator y Genera l Projec t Outlin e To : Gar

yHohenstein , 3 M EHS&Opn s From : Susa n Wolf , 3 M EHS&Opns ; Environmenta l La b cc : Willia m Reagen , 3 M EHS&Opns ; Environmenta l La b Cliffto n Jacoby , 3 M EHS&Opns ; Environmenta l La b Ja i Kesari , Westo n Solution s Charle s Young , Westo n Solution s Ti m Frinak , Westo n Solution s Octobe r20 , 201 0 Date : Subject : Analysi s o f Perfluorooctanoi cAci d (PFOA ) i n Groundwater , Soi l an d Sedimen t fo rth e 3 M

Decatu rPhas e 3 Site-Relate d Monitorin g Program ; GL P Interi m Repor t 1 1 - Forme rSludg e Incorporatio n Are a (FSIA ) Groundwate r 

### 1 Genera l Projec t Informatio n

Contact s

La b Reques t Numbe r SixDigi t Departmen t Numbe r Projec t Schedule/Tes t Date s 3 M Sponso rRepresentativ e Gar yHohenstei n 3 M EH S Operation s 3 M Buildin g 224-5W-0 3 Sain t Paul , M N 55144-100 0 Phone:(651)737-357 0 aahohensteinSJmmm.co m 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 wkreaaen@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 cclanae(5)mmm.co m Samplin g Coordinato r Timoth yFrina k Westo n Solution s Timothv.frinak(a)westonsolutions.co m Phone : (334)-332-912 3 GLP10-01-01-1 1 Dept #530711 , Projec

t #002267444 9 Samplin g schedule d fo rth e wee k o fOctobe r25 , 201 0
Al l verba l an d writte n correspondenc e wil l b e directe d t o Gar yHohenstein

. Pag e 4 o f7 Pag e 3 5 o f5 3Attachmen t A GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Former.Sludg e Incorporatio n Are a - Novembe r201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 1 

### 2 Backgroun d Informatio n an d Projec t Objective(s ) Th e 3 M EH S Operation s Laborator y(3 M Environmenta l Lab ) wil l receiv e an d analyz e groundwate r sample s collecte d fro m twenty-seve n groundwate rwell s fo rPerfluorooctanoi cAci d (PFOA ) fro m th e Forme rSludg e Incorporatio n Are a (FSIA)

. Analyse s wil l b e conducte d unde rth e GL P requirement s o f EPATSC AGoo d Laborator yPractic e Standard s 4 0 CF R 792

. Groundwate rsample s fro m Decatur , A L wil l b e collecte d byWesto n Solution s personne l th e wee k of Octobe r25 , 2010

. Th e 3 M Environmenta l Laborator ywil l prepar e th e sampl e bottle s wit h al l require d spike s t o ensur e tha t result s fo rPFOAare o fa know n precisio n an d accuracy . Th e fina l repor t wil l b e submitte d t o Gar

yHohenstei n an d Ja i Kesar i upo n completio n unde rinteri m repor t GLP10-01-01-11

. 

### 3 Projec t Schedul e Sampl e collectio n bottle s wil l b e prepare d b y3 M Environmenta l Laborator yfo rsamplin g th e wee k ofOctobe r 25 , 2010

. Sampl e bottle s wil l b e shippe d i n cooler s overnigh t t o 3 M Decatu rfo rarriva l o n Friday , Octobe r22 , 2010

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

. Marti n Smit h \

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

### 4 Tes t Parameter s Th e targete d limi t o f quantitatio n wil l b e 0.02 5 ng/m L (ppb ) fo rPFOA

. Atota l of thirty-fou rsamplin g location s hav e bee n specified

. Fo reac h samplin g location , a sample , sampl e duplicat e an d a minimu m of two fiel d matri xspike s wil l b e collected

. Tabl e 1 indicate s th e wel l I D an d con-espondin g fiel d spike levels

. Th e "fil l t o here " lin e o n eac h 25 0 m L Nalgen e bottl e wil l b e 20 0 mL

. Fou rsets of tri p blank

s consistin g of reagent-grad e water , a low-leve l tri p blan k spike , mid-leve l fiel d spike , mid-hig h fiel d spike , an d a high-leve l tri p blan k spike wil l b e prepare d a t th e 3 M Environmenta l Laborator yan d sen t t o th e samplin g locatio n wit h th e othe rbottles

. Tw o additiona l bottle s wil l b e prepare d t o b e use d fo rth e preparatio n ofth e equipmen t rinseat e blanks

. Atota l of18 9 sampl e bottle s wil l b e prepared

. Tabl e 1

. Samplin g Location s an d Fiel d Matri xSpil< e levels

.

Wel l No

. 136R,137R,137S,137L , 138 L 130L

. 131L , 131S , 133R , 134S , 135S.136 S 130R , 130S,132R,132L , 132S , 133S , 133L , 134L , 135L , 136L , 138S

. 138R , CW26R , CW26L , 140R , 141R , 142R , 143 , an d 144 R 131R , 134R , 135 R TripBlankSet1,2 , 3 , and 4 Sampl e Leve l Low Mi d Hig h Lo w Mi d Hig h Lo w Mi d Hig h Lo w Hig h Lo w Mi d Mid-Hig h Hig h Spik e Cone

. (ng/mL ) 0. 1 1. 0 1 0 1 1 0 10 0 1 0 10 0 100 0 10 0 100 0 1 1 0 10 0 100 0
Pag e 5 of7 Pag e 3 6 o f5 3GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o fPFO Ai n Groundwate r

, „ . , . Forme rSludg e Incorporatio n Area-Novembe r201 0 Attachment

AAnalytica l Protocol : GLP10-01-0 1 Amendmen t 1 1



### 5 Tes t Method s Sample s wil l b e prepare d an d analyze d b yLC/MS/M S followin g ETS-8-044. 0 "Determinatio n ofPerfluorinate d Compound s I n Wate rbyHig h Performance Liqui d Chromatography/Mas s Spectrometr yDirec t Injectio n Analysis"

. Th e dat a qualityobjective s fo rthes e studie s are quantitative result s fo rth e targe t analyte s wit h a n analytica l accurac

yo f 100±30%

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

t an d th e fina l accurac

ystatemen t ma

ybe adjuste d accordingly

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

. Alternately , sample s ma yb e analyze d b

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

. 

### 6 Reportin g Requirement s Fo reac h samplin g location , th e repor t wil l contai n th e results fo rth e sample , sampl e duplicate , an d field matri x spikes

. Tri p blan k

an d tri p blan k

spike s wil l b e reporte d fo rth e samplin g even t a s wil l an yequipment/rinseat e blank s prepare d i n th e field

. Laborator ycontro l spike s ofreagen t wate rprepare d a t th e tim e ofsampl e preparatio n wil l als o b e reporte d an d use d t o evaluat e th e overal l metho d accurac yan d precision

. Method blank s o f reagen t wate rprepare d a t th e tim e o fsampl e preparatio n wil l b e use d t o determin e th e metho d detectio n limit

. Fo rthos e samplin g location s wher e th e fiel d matri xspike leve l wa s not appropriate , du e t o highe rtha n expecte d analyt e concentrations , a laborator ymatri xspike ma

yb e prepare d an d include d i n th e fina l report

. 

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

Pag e 6 o f7 Pag e 3 7 o f5 3Attachmen t A

Attachmen t A GLP10-01-01 ; Interi m Repor t 1 1 Analysi s o f PFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 Analytica l Protocol : GLP10-01-0 1

Amendmen t 1 1 

# Bottl e Reques t Decatu r Groundwate r

Samplin g On-sit e FSI AWell s 0218L129.145.000 4 DAT EREQUESTED : 1 8 Octobe r 201 0 DAT EREQUIRED : 2 5 Octobe r 201 0 Thi s reques t

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

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

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

138 S 138 L CW26 R CW26 L 140 R 141 R 142 R 143 R

144 R

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

### Groundwater

Rinseate Sampl e Trip Blank s Will nee dHPL C water Anticipate 1 pe r

cooler Note : Some ofth e well s hav e limite dvolume s o th e smaller th e volum e requirement s th e better

. 

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

Plan t 140 0 Stat e Dock s Roa d Decatur , A L3560 1 256-552-618 9

Pag e 7 of7 Pag e 3 8 of5 3Buste r

J293020 3 Attachmen t B GLP10-01-01 ; Interi m Repor t 1 1 Forme rSludg e Incorporatio n Are a - Novembe r201 0
b110103a.rd b (PFOA) : "Quadratic " Regressio n (" 1 / x " weighting) : y= -1.02e+00 4 x'^ 2 + 1.32e+00 6 x+ 7.38e+00 3 ( r= 0.9996 )
6.2e 7 6.0e 7

5.5e 7

5.0e 7

4.5e 7

4.0e 7

3.5e 7

" 3.0e 7 o f 

### <
2.5e7
-
2.0e 7

1.5e7
-
1.0e 7 5.0e 6

0. 0 

### / O



### o

/ / / /

0 5 1 0 1 5 2 0 2 5 3 0 3 5 4 0 4 5 5 0 5 5 Concentration , ng/m L 6 0 6 5 7 0 7 5 8 0 8 5 9 0 9 5 10 0 Dat aworke du p b y ST W Printin g Time : 12:41:0 2 P M Printin g Date : Tuesday , Februar y 08 , 201 1 Pag e 1 o f 1 Pag e 3 9 o f 5 3"* * Buste r

J293020 3 Attachmen t B GLP10-01-01 ; Interi m Repor t 1 1 Forme rSludg e Incorporatio n Are a - Novembe r201 0 

# I Sampl a Name : -b110103a021 " Sampl e ID : -08008-194-8
- File : -bllOIOSa.tM T Pea k Name : 'PFOA ' Mass(ee) : '413.0/369. 0 •rTHj,413.0/219. 0 arT)u,413.CV169. 0 amu Commen t *2. 5 nghn L F C el d i n Mil l Q V\btBr * Anrwtation : Sampl e Type : Standar d Cancsntration : 2.5 0 ny/m L Calculate d Cone : 2.6 5 nq/m L ftcq. Data : 1/3/201 1 Acq

. Tin<e : 5:28:0? ! P M Modified : B T Wind'jw : Expacta dRT : I's e Ralativ e Int
. Type : Retentior

. T i Area : Height : ?tar t Time : Er. dTima : RT :

H 2 S Va s 30. 0 1 4
. e N o Manua l i^. e °B5 6 C

O 349*00 5 U . 7 15. 0 m

i

c p mi mi m Sampl e Name:-b1101O3aO37
- Sampl e ID:-LCS-1D123C>6 ' I Pea k Name : 'PFOA ' hAass(ea) : "413.0/369. 0 amu,413.(V21 9
• Commen t "Spp b LCS " Annotation : • " Sampl e Inde_l : 3 7 Sampl e Type ; Q C Concentration : 4.9 7 nq/m L Calcul:ste dCone : 5.6 9 ng/m L1.6e 6 Acq
. Date : 1/3/201 1 Acq
. Time : 11:05:1' ' P M 1.5e 6 File:-bllOl03a.wi r D amu.413.(V169. 0 amu *

Modified : H o Ptoc

. Al^';rithrii : Int^lliQua n - Ba^e

. Sub

. Window : 1.0 0 ra Peak-Split

. Factor : 2 Rapor t Larges t PaaK : N o nul l

Hln

. Pea k

Width : 0.0 0 Smoottiin g Width : 0 R TWindow : 30. 0 sa c I's e Relativ e RT : N o Int

. Type : Valle y R.itei.tio n Tirr-e : 1J. & mi n Area : 718173 1 coMnt s Haiglit : l.eje.OO e cp 3 Star t Time : 1J. 7 mi n e c poi n s ^ f F 1.4e 6
1.3e 6

1.1e 6 I.Oe S
9.0e 5

7.0* 5
6.0e 5
5.0e 5
4.0e 5
3.0e 5
2.0e S l.Oe S

1 6 1 8 I SamplaName:-b110103a049 ' Sampl e ID;-LCS-10123D-13
- FBe : tllDloaa.wif r Pea k Name : 'PFOA ' Mass(es) : "413.0 /
• Commen t 'Spp b LC S ECF * Anrwtation : * " Sampl e Index : 4 9 Sampi e Type : O C Concentration : 4.& 5 ng/» L Calculate dCore : 6.3 9 ng/m L Acq
. DatB : 1/4/201 1 Acq
. Tima : 3:19:2 9 A H iu.413.0/169.0ami f 

# I Sampl e Name:-b110103a069
- Sampt o ID : 'Solven t Blan k (Milli Q Elemerrt) ' File : -b110103a.wtf r Pea k Name : "PFOA " Mass(ea) : "413.0/369. 0 amu,413.a/219.Damu,413.0/169. 0 amu " Commen t "Mil E Q Wtate rTNlO-0475 " /^notation : "

R T Windov : Expecte dRT : Us e Relativ e RT : l;it

. Tvp« : Retentio nTime : Area : 76 ? Heigtit : ! Star t Time : En dTim? : 30. 0 H . 8 N o Manua l H . 8 678 3 c .626+00 5 14. 5 15. 0 1.6e 6
1.5e 6
1.4e 6
1.3a E
1.2e 6
1.1e 6
I.Oe e 9.0e S
a.Oe S
7.0e 5
e.0e 5
5.0e 5
4.0e 5
3.De 5
ZOeS

1.0e5

- 1 4

14.66...
. 

# 1 7 9

M
. _4^

- ^ sampl e Type : I'nk r i : H/ A )nc : 0.0033 2 ate : ime : e d : Algcrithm : Percentag e Sub

. Wind o 1/4/201 1

10:20:3 4 N o IntalliQ' j : 9 0 u : 1.0 0

Smoothin g Wi d Expecte d RT : 5.2e 4 5.0e 4 4.ae 4 4.6e4 ' 4.4e 4 4.2e 4 4.0e 4 3.8o 4 3.6e 4 3.4« 4 3.2e 4 3.0« 4 2.8e 4 Z6e 4 2.4e 4 2.2e 4 2.0e 4

1.4e 4 1.2e 4 1.0e 4 8000. 0 6000.0
- 4000. 0 2000.0
- 0. 0 nwlll i MK^ff***^"' ' 1 0 1 2 1 4 1 8 1 8 Timg

. mi n Dat aworke dup b y ST W Printin g Time : 12:43:0 2 P M Printin g Date : Tuesday , Februar y 08 , 201 1 Pag e 1 o f 2 Pag e 4 0 of 5 3** * Buste r

J293020 3 Attactimen t B GLP10-01-01 ; Interi m Repor t 1 1 B a t AP^?i l :° fffi9fbi?a9SJ'i"«*'"a'er Forme rSludg e Incorporatio n Are a - Novembe r201 0

Dat a worke d u p b

yST W Printin g Time : 12:43:0 2 P M Printin g Date : Tuesday , Februar y08 , 201 1 Pag e 2 o f 2 Pag e 4 1 o f 5 3

### Documen t ma ybeGLF*'o-oi-ui mter.mfieFw-11 4 days fro m 02/08/20 " Analysi s o f PFO Ai n Groundwate r Attactimen t 0 Fomie rSludg e Incorporatio n Are a - Novembe r201 0



# 3 M Environmenfa l LaixxrafDi y

Metho d Metho d o f Analysi s fo rth e Determinatio n o f Perfluorinate 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 i^^f^^^ j

Approve d By : 

# ^yyjy o • > Willia m K

. Reagen , Laborator yManage rDat e

ETS-8-044. 0 Pag e 1 o f1 1 Metho d of Analysi s fo rth e Determinatio n ofPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 2 o f 5 3Documen t ma ybeGUBtoM,i-:6i;:irit€-nrnHefKv-ri1 4 day s fro m 02/08/20 ' Analysi s o fPFO Ai n Groundwate r Attactimen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

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

. Wate rsample s containin g heav y particulat e ma

yrequire preparatio n b

ya n altemat e metho d suc h a s ETS-8-15 4 "Determinatio n of Perfluorinate d Acids , Alcohols , Amides , an d Sulfonate s I n Wate rB ySoli d Phas e Extractio n an d Hig h Performance Liqui d Chromatography/Mas s Spectrometry"

. Thi s metho d i s considere d a performance-base d method

. Data i s considere d acceptabl e a s lon g as th e define d Q C elements are satisfied

. Sampl e collectio n i s not 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 of70 % t o 130% , ma yb e flagge d a s suc h (wit h expande d accurac

ystatements) , o rwil l no

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

. Fortificatio n level s fo rfiel d matri xspike s an d fo rlaborator ymatri xspike s shoul d b e a t least 50 % ofth e endogenou s leve l an d les s tha n 1 0 time s th e endogenou s leve l t o b e use d t o detemnin e th e statemen t of accurac yfo ranalytica l results

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

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

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

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

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

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

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

. 

### 3. 3 Fiel d Blan k

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

. Th e purpos e ofth e F B i s t o determin e i ftes t substance s o r othe rinterference s are presen t i n th e fiel d environment

. Thi s sampl e i s als o refen-ed t o as a Tri p Blank

. ETS-8-044. 0 Pag e 2 o f1 1 Metho d of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 3 o f5 3Documen t ma ybewh'!0^o^^^cimmr!\ke^m•^i 4 day s fro m 02/08/201 1 Analysi s o fPFO Ai n Groundwate r Attachmen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

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

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

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

. 3. 5 Fiel d Matri xSpik e (FMS ) Asampl e t o whic h know n quantitie s ofth e targe t analyte s are adde d t o th e sampl e bottl e i n th e laborator y befor e th e bottle s are sen t t o th e fiel d fo rcollectio n o faqueou s samples

. Aknown , specifi cvolum e of sampl e must b e adde d t o th e sampl e containe rwithou t rinsing

. Thi s ma yb e accomplishe d b

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

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

. I fth e expecte d rang e of analyt e concentration s i s unknown , multipl e spike s a t varyin g level s ma

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

t a n appropriat e leve l i s made

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

ycomplicat e th e interpretatio n ofth e sampl e analysis

. 

### 3. 6 Tri p Blan k

Spik e (Fiel d Spik e Contro l Sample , FSCS ) A n aliquot of AST 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 of analyt e coul d b e attribute d t o holdin g time , sampl e storag e and/o rshipmen t issues

. A lo wan d hig h FSC S are appropriat e whe n expecte d sampl e concentration s ar e no t know n o rma

yvary . At least on e separate , un-spike d sampl e must b e take n 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 of contro 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 of sampl e extraction

. At 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 o fth e curve . Th e LCS s are extracte d an d analyze d exactl ylike a laborator

ysampl e t o determin e whethe rth e metho d i s i n control

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

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

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

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

ysampl e t o determin e whethe rth e sampl e matri xcontribute s bia s t o th e analytica l results

. Th e endogenou s concentration s ofth e analyte s i n th e sampl e matri xmust b e detennine d i n a separat e aliquot an d th e measure d value s i n th e LM S con^ecte 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 of a sampl e receive d fro m th e fiel d fo rtesting

. 3.1 0 Limi t o f Quantitatio n (LOQ ) Th e lowe rlimi t of quantitatio 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 of quantitatio n (ULOQ ) fo ra dataset i s th e highest concentratio n that ca n b e reliabl y quantitate d withi n th e specifie d limits o fprecisio n an d accurac ydurin g routin e operatin g conditions

. Th e highest standard 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 f Analysi 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 4 4 o f 5 3Documen t ma ybmm^m0^cmermte^m^^ 4 day s fro m 02/08/20 ' Analysi s o f PFO Ai n Groundwate r Attactimen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

3.1 1 Metho d Blan k A n aliquot o f contro 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 determin e i f test 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 yofmateriai 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 of a single-analyt e prepare d i n th e laborator ywit h a n assaye d reference compound

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

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

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

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

. Inclusio n o fa sun-ogate analyt e i s a n optiona l qualit ycontro l measure an d i s NO Trequired

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

. 4 Warning s an d Caution s
4. 1 Healt h an d Safet y Th e acut e an d chroni ctoxicit yof th e standard s fo rthi s metho d have not bee n precisel ydetennined ; however , eac h shoul d b e treate d a s a potentia l healt h hazard

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

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

. Th e laborator

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

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

. 4. 2 Caution s Th e analyst must b e familia rwit h th e laborator yequipmen t an d potentia l hazard s including , bu t no t limite d to , th e us e of solvents , pressurize d gas an d solven t lines , hig h voltage , an d vacuu m systems

. Refe rt o th e appropriat e equipmen t procedure o roperato rmanua l fo radditiona l infonnatio n an d cautions

. 5 Interference s Durin g sampl e preparatio n an d analysis , majo rpotentia l contaminan t source s are reagents an d glassware

. Al l material s use d i n th e analyse s shal l b e demonstrate d t o b e fre e fro m interference s unde r condition s o f analysi s b

yrunnin g metho d blanks

.

ETS-8-044. 0 Pag e 4 o f1 1 Metho d o f Analysi 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 4 5 o f5 3Attactimen t C )ocumen t ma ybeGmAm\iS\ommffAepm-6 4 day s fro m 02/08/201 1 Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0

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

. Thes e ma yinclude , bu t ar

e no t limite d to : was h bottles , Teflon ® line d caps , autovia l caps , HPLC parts , etc

. Th e us e of disposabl 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 performance liqui d chromatograp h capabl e ofpumpin g u p t o two solvent s an d equippe d wit h a variabl e volum e injecto rcapabl e of injectin g 5-10 0 p L connecte d t o a tande m Mas s Spectromete r (LC/MS/MS)

. I Analytica l balance capabl e o f readin 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 , 25|JL , 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 o f spinnin g 15-m L an d 50-m L polypropylen e tube s a t 300 0 rpm . 6. 2 Chromatographi cSyste m Guar d Column : Pris m RP , 4. 6 m m x5 0 mm , 5 p m Analytica l Column : Betasi l C I 8,4. 6 m m x10 0 mm , 5 p m Temperature : 10° C Mobil e Phas e (A) : 2 m M Ammoniu m Acetat e i n Wate r Mobil e Phas e (B) : Methano l Gradien t Program :

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

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

3 3 9 5 9 5 3 3 FlowRat e

(mUmin ) 1. 0 1. 0 1. 0 1. 0 1. 0 1. 0 Injectio n Volume : 10 0 pL

. Quantitation : Pea k

Are a - quadrati ccurve fit , 1/ xweighted

. 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 tha t dat a qualityobjective s are met

.
ETS-8-044. 0 Pag e 5 o f1 1 Metho d o f Analysi 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 4 6 o f 5 3Attachmen t C 

### Documen t ma ybeGUBWEfeiiicwiwrriiiefferi1 4 days fro m 02/08/20 " Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0



### 6. 3 MS/M S Syste m 6.3. 1 Mode : Electrospna yNegativ e ion , MR M mode , monitorin g th e followin g transitions : Analyt e PFB A PFPe A PFH A PFHp A PFOA PFN A PFD A PFUn A PFDo A PFB S PFH S PFO S Transitio n Monitore d 213^16 9 263- > 21 9 313- > 26 9 an d 31 3 ^11 9 36 3 ^ 319 , 36 3 - > 16 9 an d 36 3 - > 11 9 41 3 - ^ 369 , 41 3 ^

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

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

21 9 an d 51 3 - ^

26 9 56 3 ^ 519 , 56 3 ^

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

16 9 an d 61 3 - ^

31 9 29 9 ^ 8 0 an d 29 9 - » 9 9 39 9 - > 8 0 an d 39 9 - > 9 9 49 9 - ^ 80 , 49 9 - > 9 9 an d 49 9 ^ 13 0 Multipl e transition s fo rmonitorin g th e analyte s i s a n option , a s summin g multipl e transition s ma yprovid e quantitatio n o f isomers tha t mor e closel ymatche s NM R dat a an d ma yhav e th e adde d benefi t o f increase d sensitivity

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

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

. 

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

. Reagen t Grad e 

### 7. 2 Standard s Perfluorobutanoi cAci d (PFBA-C 4 acid) ; Oakwoo d Products , In c Perfluoropentanoi cAci d (PFPeA- C 5 acid , als o know n as NFPA , nonafluoropentanoi cacid) ; Alf a Aesa r Perfluorohexanoi cAci d (PFHA-C 6 acid) ; Oakwoo d Products , In c Perfluoroheptanoi cAci d (PFHpA- C 7 acid , als o know n a s TDHA , tridecafluoroheptanoi cacid) ; Oakwoo d Products , In c Perfluorooctanoi cAci d (PFOA- C 8 acid) ; 3 M Perfluorononanoi cAci d (PFNA-C 9 acid) ; Oakwoo d Products , In c Perfluorodecanoi cAci d (PFDA- CI O acid) ; Oakwoo d Products , In c Perfluoroundecanoi cAci d (PFUnA-C1 1 acid) ; Oakwoo d Products , In c Periluorododecanoi cAci d (PFDoA-CI 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 of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Pag e 4 7 o f5 3 Analysi sDocumen t ma ybeGLir'to-ai-iiir^nfei-irrmefftKi' M day s fro m 02/08/2 C Analysi s o f PFO Ai n Groundwate r Attachmen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

Th e previou s informatio n i s intende d a s a guide

. Reagent s an d standard s fro m alternat e source s ma yb e used

. 7. 3 Reagen t Preparatio n 2 m M Ammoniu m acetat e solutio n (Analysis)—^Weig h 0. 3 g ofAmmoniu m acetat e an d dissolve i n 2. 0 L o freagen t water

. Note : Alternativ e volume s ma yb e prepare d a s lon g as th e ratio s ofth e solven t t o solut e ratio s ar e maintained

. 7. 4 Stoc k

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

d preparatio n procedur

e serve s a s a n example

. Weighe d amounts an d final volume s ma yb e change d t o sui t th e need s of a particula rstudy

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

solution s t o appropriat e levels

. 10 0 |jg/m L targe t analyt e SSSs—Weig h ou t 1 0 m g ofanalytica l standar d (correcte d fo rpercen t sal t an d purity\ an d dilut e t o 10Om L wit h methano l o rothe rsuitabl e solvent , i n a 10Om L volumetri cflask. Transfe rt o a 125m L LDP E bottl e o rothe rsuitabl e container

. Prepar e a separat e solutio n fo reac h analyte

. Expiratio n date s an d storag e condition s of stoc k solution s shoul d b e assigne d i n accordance wit h laborator ystandar d operatin g procedure

. A n exampl e of purit yan d sal t con-ectio n i s give n belowfo rPFOS

.

, . X
- r1 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= -^ ^ = 0.927 5 53 8 1 0 m g CsFiySOs'K

" wit h purit

y90 % = 8.35m g CsFiySOa" (1 0 mg*0.90*0.9275=8.3 5 mg ) 5 Mg/m L (500 0 ng/mL ) mixe d workin g standard—Ad d 0.5m L eac h ofth e lOOpg/m L SSS s t o a 10m L volumetri c flask an d brin g u p t o volum e wit h solvent

. 25 0 ng/m L mixe d workin g standard—Ad d 1.25m L ofth e 5 pg/m L -mixe d wori<in g standar d solutio n t o a 25m L volumetri cflask

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

. 12 5 ng/m L mixe d standard—^Ad d 625p L ofth e 5 pg/mL-mixe d wori<in g standar d solutio n t o a 25m L volumetri c flask 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 procedure o ri n a refrigerato ra t 4°±2° C fo ra maximu m perio d of6 month s fro m th e dat e ofpreparation

.

ETS-8-044. 0 Pag e 7 o f1 1 Metho d o f Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 8 o f5 3Attachmen t C )ocumen t ma ybeGuotsiaiJlicwierffrrte^i M d a Analysi s o fPFO Ai n Groundwate r Forme rSludg e Incorporatio n Are a - Novembe r201 0 

### ro m 02/08/201 1

7. 5 Calibratio n Standard s Usin g th e worthin g standard s describe d above , prepare calibratio n solution s i n AST M Typ e I water , HPLC water , o r othe rsuitabl e water , usin g th e followin g tabl e as a guideline

. Note : Volume s ofwate ran d 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 f WS , 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./d

.

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

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

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

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

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

. Sample s containin g heav yparticulat e ma

yno t b e suitabl e fo r analysi s b

ythi s method

. Sample s containin g suspende d particulat e shoul d b e centrifug e prio rt o removin g a sampl e aliquot , o rfiltered. Thoroughl ymi xsampl e before 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 of glas s autovials , t o preven t th e possibl yoffluorochemical stickin g t o th e glass

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

. Prepare metho d Q C sample s an d multipl e metho d blank s an d aliquot int o labele d plasti cautovials

. Prepare at least five metho d blanks

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

» Analyz e th e standar

d curve prio rt o eac h set ofsamples

. Th e standar d curve ma

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

xo runweighted , o rb

yquadrati cfil (

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

xo runweighted , usin g suitabl e software

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

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

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

. Hig h and/o rlo

wpoints ma

yb e exclude d fro m th e calibratio n curve s t o provid e a bette rfit ove rth e rang e appropriat e t o th e dat a o rbecaus e theydi d no t meet th e pre-detemnine d acceptanc e 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 o f detemninatio n {f ) 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 curv e 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 of Analysi s fo rth e Determinatio n o fPerfluorinate d Compound s i n Wate rbyLC/MS/MS ; Direc t Injectio n Analysi s Pag e 4 9 o f 5 3Documen t ma ybeGmmm0^cm&mte^mx^l 4 day s fro m 02/08/20 1 • Analysi s o fPFO Ai n Groundwate r Attachmen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

b e withi n ±30%

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

. Aminimu m o f6 points wil l b e use d t o constmc t th e calibratio n curve . I f th e calibratio n curve doe s no t meet acceptance criteria , perfor m routin e maintenance o rprepare a ne wstandar d curve (i f necessary) an d reanalyze

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

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

t a minimu m afte rever ytent h sample , no

t includin g solven t blanks , wit h a minimu m ofon e pe rsampl e set

. Calibratio n verificatio n injection s must b e withi n ±25 % t o b e considere d acceptable

. Th e calibratio n curve an d th e las t passin g CCV wil l the n bracket acceptabl e samples

. Multipl e CCV level s ma yb e used

. Sample s containin g analyte s that ar e quantitate d above th e concentratio n ofth e highest standar d i n th e curve shoul d b e furthe rdilute d an d reanalyzed

. 1 0 Qualit yContro l
10. 1 Dat a Qualit yObjective s Thi s metho d an d require d qualit ycontro l sample s i s designe d t o generat e dat a accurat e t o ±30 % wit h a targete d LO Q of 0.02 5 ng/mL

. An ydeviation s fro m th e qualit ycontro l measure s spelle d ou t belowwil l b e documente d i n th e ra wdat a an d footnote d i n th e final 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 five 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 of CC V 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 must b e les s tha n 50 % ofth e are a coun t ofth e LOQ standard

. Th e standar

d deviatio n ofth e are a counts o fthes e metho d blank s shoul d b e calculate d an d reported

. I f th e mea n are a count s ofth e metho d blank s excee d 50 % ofth e LOQ standard , the n th e LOQ must b e raise d t o th e first standar

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

. 

### 10. 3 Sampl e Replicate s Sample s duplicate s are collecte d i n th e field. Th e relative percen t difference , RPD , shoul d b e reported

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

. Th e requiremen t fo r replicate s exclude s field blanks

. 10. 4 Surrogat e Spike s Sun-ogat e spike s are not 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 offive t o te n time s highe rtha n th e targete d LOQ an d hig h la b contro l spike s shoul d b e prepare d a t concentration s nea rth e mid-poin t ofth e curve . Th e relative standar

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

. I f th e above criteri a are no t met , th e entire set of sample 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 f Analysi 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 0 o f5 3Documen t ma ybe<Mimm^%Mmmne^m-0i 4 day s fro m 02/08/201 1 Analysi s o fPFO Ai n Groundwate r Attachmen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

10. 6 Fiel d Matri xSpike s / La b Matri xSpike s Recoverie s of field 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 flagged 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

. 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 o faccurac yfo ranalytica l results

. Th e averag e of th e sampl e an d th e field duplicat e shoul d b e use d t o calculat e th e recovery . 1 1 Dat a Analysi s an d Calculation s Us e th e followin g equatio n t o calculat e th e amoun t ofanalyt e foun d (i n ng/mL , base d o n pea k area) usin g th e standar d curve (linea rregressio n parameters ) generate d b ya n appropriat e software program : Analyt e foun d (ng/mL ) = (Pea k Are a - Intercept ) ^

^ ^ 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 ofth e data

. Nonconfonnanc 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 f criteri a liste d i n thi s metho d performance sectio n are no t met , maintenance ma

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

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

. I f dat a are t o b e reporte d whe n perfonnance criteri a have no t bee n met , th e dat a 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 of thre e syste m suitabilit ysample s are injecte d a

t th e beginnin g o

feac h analytica l ru n prio rt o th e calibrafio n curve . Typicall ythes e sample s ar e a t 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 must have are a count s wit h a n RS D of S5 % 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 of determinatio n (r^ ) valu e fo rth e calibrafio n curve must b e greate rtha n o r equa l t o 0.990

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

yb e withi n ±30%

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

. Sample s that are brackete d b

yCCVs no

t meetin g thes e criteri a must b e reanalyzed

.

ETS-8-044. 0 Pag e 1 0 o f1 1 Metho d o f Analysi 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 1 o f5 3Documen t ma ybm\mwm^tmemrAe:^mri 4 day s fro m 02/08/201 1 Analysi s o fPFO Ai n Groundwate r Attachmen t C Forme rSludg e Incorporatio n Are a - Novembe r201 0

Demonstratio n o f Specificity : Specificit yi s demonstrate d b

ychromatographi cretentio n tim e (withi n 4 % of standard ) an d th e mas s spectra l respons e ofuniqu e ions

. 12. 3 Sensitivit y Th e targete d limi t of quantitatio n fo ral l analyte s i s 0.02 5 ng/mL

. Th e LO Q fo ran yspecifi canalyt e ma yvar y dependin g o n th e evaluafio n of appropriat 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 raddifiona l details

. 12. 4 Accurac y Thi s metho d an d require d qualit ycontro l sample s are designe d t o generat e 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 yoflaborator

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 not 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 informatio n regardin g th e require d precisio n o flaborator ycontro l spikes

. 1 3 Pollutio n Preventio n an d Wast e Managemen t Wast e generate d whe n perfonnin g thi s metho d wil l b e dispose d o fappropriately

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

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

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

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

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

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

. 1 5 Affecte d Document s None

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

ETS-8-044. 0 Pag e 1 1 of1 1 Metho d o f Analysi 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 2 of 5 3GLP10-01-01 ; Interi m Repor t 1 1 3 M Confidentia l Analysi s o fPFO Ai n Groundwate r Attachmen t D

__. _ _.. . Forme rSludg e Incorporatio n Area-Novembe r201 0 

## RECOR D O F DEVIATION/NONCONFORMANC E

/ , Identificatio n Stud y/ Projec t No

. Date(s ) o f Occurrence : Documen t Number : GLP10-01-01-1 1 1-3-1 1 ETS-8-044. 0 Deviatio n typ e 0 SO P D Equipmen t Procedur e D Metho d (Chec k one ) D Protoco l O GP O D Other :



### //

. Descriptio n (attac h extr a pages as needed ) Metho d Requirements : 1

. LC S averag e recoverie s withi n ±20 % (sectio n 10.5)

. 2

. FM S recoverie s withi n ±30 % (sectio n 10.6 )


### Actua l procedure/process : 1

. Th e averag e PFOArecover yfo rth e 5 pp b EC F LC S wa s 123%

. 2

. Th e hig h FM S recover yfo rsampl e DA L G W134 R wa s 69.1%

.



### ///

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

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

) Reference : Acceptabilit yo f tfi e nonconformin g work : 1

. Low , mid , an d hig h set s of linear , an d linea r+ branche d (ECF ) LC S sample s wer e prepare d an d analyze d wit h th e samples

. Al l set s me t rrietho d acceptanc e criteri a wit h th e exceptio n o f th e mi d leve l EC F LCS

. Th e linea r+ branche d PFOALCS , whe n quantitate d agains t calibratio n curv e poin t prepare d fro m linea r PFOA , hav e bee n quantitatin g aroun d 5-15 % higher

. Th e recover yfo rth e 5 pp b EC F LC S (123% ) wil l b e flagge d i n th e fina l report

. Al l LC S wer e use d i n th e determinatio n o f metho d analytica l uncertainty

. 2 , Th e FM S recover

yfo rth e sampl e outsid e th e acceptanc e criteri a wil l b e flagge d i n th e fina l report

. Th e metho d uncertaint yfo rPFO Awil l b e adjuste d according

.
Actions : D Haltin g o f Wor k D Clien t Notificatio n D Wor k Recal l D Withholdin g o f Repor t 0 Other : Deviation s wil l b e note d i n fina l report

. 

### Project Lead/PA I Approval : / } ^ ^ Date: , , 

# ^l^/ l 

# '^ 0 Stud yDirecto r(i f GLP) : M Vj.J>^^'{K/vC> ^ Date?
- Sponso rAppfova i (fo rGL P protoco l deviations) : N ADate : N A Technica l Reviewe r(optional) : N ADate : N A Laborator yDepartmen t Manage rApproval : Date :

IV

. Authorizatio n t o Resum e Wor k Wher e haltin g o f wor k

occurred , resumptio n o f wor k mustfirs t b e approve d b yLaboratoryManagemen t 

### Laborator yDepartmen t Manage rApproval ; - . Date : A

.

Deviatio n No

. (assigne d b yStud yDirecto ro rTea m Leade ratth e en d o fstud yo rproject )

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

Documentatio n o f Deviation s an d Contro l o fNonconformin g Testin g Pag e 5 3 o f 5 3