Do_4_upland_sed_fulldata_vol_2_of_5.pdf

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C:\Xcalibur\Data\Dioxin\07261 3\07261 302 7/26/2013 9:26:14 AM 52607-6703 WS+CP+CS3

RT: 25.49 26.50

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C:\Xcalibur\Data\Djoxin\07261 3\07261 302 7/26/2013 9:26:14 AM 52607-67-03 WS+CP+CS3

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2.38E4 m/z= 401.7560- 401 .9560

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1.82E4 mlz= 403.7530- 403.9530

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1.64E4 mlz= 407.6818- 407.8818

MS ICIS

07261302

1.57E4 mlz= 409.6789- 409.8789

MS ICIS

07261302

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2.71E4 mlz= 421.7190- 42 1.9190

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07261302

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2.68E1 m/z= 479.6165- 479.8165

MS ICIS

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9.23E3 mlz= 425.6740- 425.8740

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1.81E4 mlz= 435.7170- 435.9170

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1.69E4 mlz= 437.7140- 437.9140

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Vol. 2 of 5 p. 716

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48.0 48.5 49.0 49.5 50.0 50.5 51.0 51.5

Vol. 2 of 5 p. 717

RT: 47.73- 51.37 SM: 5G

NL:

158E4

LU

m/z=C)CO 457.6380- 457.8380

100 MS ICIS

07261302

60-

40-

0 NL:

1. 71 E4 mlz=CD

N- 459.6350- 459.8350

100 MS ICIS

H 07261302 80-

H 60-

40-

20-

0 NL:

CD 2.70E4

CD

co m/z=

469.6780- 469.8780

MS ICIS

I1 07261302 80-

60-

40-

20-

0 NL:

CD 3.06E4

CD

. m/zce ) 471 .6750- 471.8750

100 MS ICIS

A 07261302

48.0 48.5 49.0 49.5 50.0 50.5 51.0

Vol. 2 of 5 p. 718

C:\XcaIibur\Data\Doxin\07261 3\07261 302

RT: 2000 - 53.00

287 305 3961 00- 0.27.0.32 27.70

80-

60-

NL:

9.79E4 m/z= 304.48180- 305.48180

MS

07261302

7/26/2013 9:26:14 AM 52607-67-03 WS^CP+CS3

403 421 528 NL:

27 .97 28 37 fl 7A 670 748 806 2.24E5

. 33.88 35.61 3690 I -

0A7869- 80- 331 .47869

MS

60 07261302

40-

403 519 555 717 831 '''

3743 39.25 41.13 1110100- 27.97 30.54 31.33 34.92 42.12 ci)

Co ci)

NL:

1.30E5 mlz= 380.47550- 381.47550

MS

07261302

1171 130843.24 133745.59 46.09

NL:

7.41 E4

m/z= 392.47550- 393.47550

MS

07261302

1481 1574 1656 NL:

81 50.551402 48

52.09 8.01E4

47.33 m/z=

Af430.47231- 431.47231

MS

07261302

20 25 30 35 40 45 50

Vol. 2 of 5 p. 719

This page intentionally left blank.

Vol. 2 of 5 p. 720 b

N a m e

M a t c i x

S a m p l e

R e c e i p t

D a t e

E x t

D a t e

R n a l y s i s

D a t e

E x t r a c t

V o l u m e p L

I n j e c t i o n

V o l u m e p L

D i l u t i o n F a c t o r

C o n c e n t r a t i o n

U n i t s

A N A L Y T E

T C D D

P e C D D

H x C D D

H x C D D l H x C D D l H p C D D

O C D D

T C D F

P e C D F

P e C D F

H x C D F

H x C D F l H x C D F

H x C D F

-H p C

DF

H p C D F a l

T E Q

S e d i m e n t s

T i m e

D

1 1 p g g d r y

P C D D

P C D F

A N A L Y S I S

D A T A

S H E E T

L a b

S a m p l e

I D

S a m p l e

W t V o l

I n i t i a l

C a l i b r a t i o n

D a t e

I n s t r u m e n t

I D

G C

C o l u m n

I D

S a m p l e

D a t a

F i l e n a m e

B l a n k

D a t a

F i l e n a m e

C a l

V e r

D a t a

F i l e n a m e

C o n c e n t r a t i o n

U n i t s

C O N C

D E T E C T I O N

F O U N D

L I M I T

I O N

R A T I O N n d n d

T E Q

L A B E L E D

C O M P O U N D S n d l C T C D D

C l P e C D D l C N x C D D l C l H x C D D l C l H p C D D

C O C D D

C T C D F n d l C l P e C D F l C P e C D F l C l H x C D F

C l H x C D F l C l H x C D F

C H x C D F l C l N p C D F l C l H p C D F

C L E A N U P

S T A N D A R D

C T C D D l

M B u n i t s

D F S

D m

Z B S p g

S P I K E

C O N C . 1

C O N C

F O U N D

P a g e o f p m

H

I O N

R A T I O l j

Vol. 2 of 5 p. 721 g e o f

F i l e n a m e:

A c q u i r e d

P r o c e s s e d

A n a l y t e

N O

M A P P I N G

C a l

D I C A L

R e s u l t s

M B

S a m p l e t e x t

M B

S

C o m m e n t s

T y p

N a m e

Q M

A r e a

R M

A r e a

N A

N T

C o n c

T o x

D L

R e c

U n k

T C D F n n d n d

U n k l P e C D F y

U n k

P e C D F y

U n k l N x C D F y

LI

nk H x C D F y

U n k

H x C D F y

L

In k l H x C D F y

U n k l H p C D F y

U n k l H p C D F y

LI

nk

O C D F y

LI

nk

T C D D n n d n d

LI

nk

P e C D D y

LI

nk l H x C D D y

LI

nk l H x C D D y

LI

nk l H x C D D y

LI

nk l N p C D D y

LI

nk

O C D D y

I S N T

C T C D F y

I S

C P e C D F y

I S

C P e C D F y

I S l C M x C D F y

I S l C l H x C D F y

I S l C H x C D F y

I S l C l H x C D F y

I S l C l H p C D F y

I S l C l H p C D F y

I S l C T C D D y

I S l C l P e C D D y

I S l C l H x C D D y

I S

C H x C D D y

I S

C l M p C D D y

I S

C O C D D y

R S l C l T C D D y

P S N T l C l H x C D D y

C U p

C T C D D y

T o t

T o t a l

T e t r a F u r a n s y

T o t

T o ta l

T e tr a -D io x in s

T o t

T o t a l

P e n t a F u r a n s y

T o t

T o t a l

P e n t a D i o x i n s y

T o t

T o t a l

H e x a F u r a n s y

T o t

T o t a l

H e x a D i o x i n s y

T o t

T o t a l

H e p t a F u r a n s y

T o t

T o t a l

H e p t a D i o x i n s y

Vol. 2 of 5 p. 722

C:\Xcalibur\Data\Dioxin\07261 3\07261 303 7/26/2013 10:29:17 AM 53720-85-21 MB

RT: 18.95-28.27 SM: 5G

(7 NL:

3.56E1

LU 0)

m/z=

(0 p 304.0020

380 0726130

3.97E1 a, mlz= N-

IC) 305.7990-

305 9990

100 ' (0 .

07261303

3.17E3 mlz= 315.8420- 316.0420

I N -

3.89E3 N-mlz=

100 A MS ICIS

07261303

LU

NL:

2.22E1

IC) mlz= (\j

375.7364- 375.9364

072603

19 20 21 22 23 24 25 26 27 28

Vol. 2 of 5 p. 723

C:\Xcalibur\Data\Dioxin\07261 3\07261 303

Co ('4 lOO- VT

W2

7/26/2013 10:29:17AM 53720-85-21 MB

o Co LC) co

0 N L() C)

N L() Co

(N Co 0

21 22 23 24 25 Time (mm)

Co Lt) L()

Co LcILco O).

-.. Co r

N- (0 (0 Co Co N -

C) C)

C) CO 00 Co Co N '1) - (0 Co ('4 Co

Co

(0 co N

D

•cr 'cr N N-Co

6272'8

Vol. 2 of 5 p. 724

7/26/2013 10:29:17AM 53720-85-21 MB

N-

LU/

(0 c)co N-

NL:

1.06E2

LU

mlz= 339.7600- 339.9600

A MS ICIS

07261303

C'4 N -o ci

U) 10 C-) C c8-o C

U)4

U)

N-c-'j

0) (0

N LU

0) C'J

I, 0)

(0 N-cs-i c, 0 C'4 c)

- 0)

U

NL:

6.07E3

LU

N- mlz=

351.8000- 352.0000

MS ICIS

07261303

LU

c) Cs-i 0) (-'I

(0 co 0) co

L:

3.71 E3

mlz= 353.7970- 353.9970

MS ICIS

07261303 c-)cO

LUN-

(0(0

NL:

2.22E1 mlz= 409.6974- 409.8974

07261 303

27 28 29 30 31 32 33 34 35 36

Vol. 2 of 5 p. 725

C:\Xcalibur\Data\Dioxin\07251 3\07261 303 7/26/2013 10:29:17 AM 53720-85-21 MB

RT: 2774 - 3750 SM: 5G

I LU

LU

C)

LU

CO

(_) ('1 co

100I

60 i I C1

20 /

100i

c) co LU r- co co

(N cULt) cU co -

LU

co

N- C) N-

LU

(N LU (0

CC. C'(.) N- vCO

C) (0 - LU (N LU (N

I - -

- '- C) (N t

LJ LL

(0 C) N- C (N

100-

80-

40 C)

LU

LU

LULU

- LU C) (N C) C N- (0 C) c) LU 0 N- CO 20-I - (N - (N (0 (0 (N N- (N (N

1L W 0 F_____ __ F F r_______ rfrr 1TfT Tir1T f

28 29 30 31 32 33 34 35 36 37

Vol. 2 of 5 p. 726

C:\Xcabur\Data\Dioxin\O7261 3\07261 303 7/26/2013 10:29:17 AM 53720-85-21 MB

RT: 37.02 - 42.45 SM: 5G

NL:

\ / 1.39E2 r- / co mIz co / . 373.7210-

I 373.9210

1.29E2co m/z= 375.7180-

375.9180

:j

! !100

2,21E1 mIz=If) 445.6555- 4458555

100-

I A I\A A A

< MS ICIS

<I\ 07261303

37.5 38.0 38.5 39.0 39.5 40.0 40.5 41.0 41.5 42.0

Vol. 2 of 5 p. 727

RT: 36.25 42.67 SM: 5G

I

N

6O I

H

Nco çj

- 0)

7/26/2013 10:29:17AM 53720-85-21 MB

(1/ cooco

CD

c) u

NL:

1.07E2 mlz= 389.7160- 389.9160

MS ICIS

07261303

c) q

CD

L() C) c)

C)

N t oco c)O co

NC'4

N-

(0 cc0 c.'J c•)

37 38 39 40 41 42 Time (mm)

NL:

9.55E1 mlz= 391.7130- 391.9130

MS ICIS

07261303

NL:

1.63E4 m/z= 401.7560- 401 .9560

MS ICIS

07261303

NL:

1.33E4 mlz= 403.7530- 403.9530

MS ICIS

07261303

Vol. 2 of 5 p. 728

C :\Xcalibur\Data\Dioxin\07261 3\07261 303

RT: 42.08 - 48.50 SM: 5G

100-:-: 3 0) Co

40- ('1

Co Cor-

100-

80 A60 Co

0 -

W i00 10 80-

C 60 A

I Co w 4O

LI) C'J

ci) 20 i L

LI)

c)

100-:

7/26/2013 10:29:17AM 53720-85-21 MB

NCo Co

A N- 0Co

'L

NL:

1.68E2

Co m/z= 409.6789- 409.8789 MS lOIS 07261303 cOO Co

CNC'4

NL:

10 i.03E4 Co m/z=

419.7220- 419.9220 MS lOISA 07261303

C,) ('4

C,)

H Cost -C') 0)Co CoD

H c 00 l b

0) '4 Co L Q)

C,)

C') c'i '4 CoN

A

43 44 45 46 47 48 Time (mm)

NL:

i.72E2 m/z= 407.6818- 407.8818 MS lOIS 07261303

967E3 mlz= 421.7190- 421 .91 90

MS ICIS

07261303

NL:

2. 39E 1 mlz= 479.6165- 479.8165 MS lOIS

Vol. 2 of 5 p. 729 ci)o8 C C', •0 C

C', ci)

(N (N (N

(N (N (N

Lf) CD co

C) co r -

(V)

N-

7/26/2013 10:29:17AM 53720-85-21 MB

N-co

LU

ctc000 LU cJLC)C) CDC cdo) c'

NL:

1.55E2 mlz= 423.6770- 423.8770 MS lOIS 07261303

NL:

1.47E2(1)

CD mlz=LU 425.6740- 425.8740

MSICIS

07261303

LU

NL:

8.34E3 mlz= 435.7170- 435.9170 MS lOIS 07261303

N- LU

v, (N c - c N- C)

CD Q CD (N (N Co N- C)

(N Co C)

LU

C)C) LU

Q N- (N C) LU COO) LU LU

N- LU LU I I LU CO

20 - o '- v- CD (N 'ct C) '- -

U 43 44 45 46 47

Time (mm)

NL:

7.91 E3

m/z= 437.7140- 437.9140

MS ICIS

Vol. 2 of 5 p. 730

C:\XcaIibur\Data\Doxn\0726l 3\07261 303

RT: 47.74-51.54 SM: 5G

N- C2 N C) C"j ct C)

7/26/2013 10:29:17AM 53720-85-21 MB

NL:

/ 2.81E2 mlz= 441 .6430- 441.8430

( MS ICIS

07261303 wo8 C

-D C

NL:

2.93E2 mlz= 443.6400- 443.8400

MS ICIS

Il 07261303

(0 (0 cv, NL:

9.36E3 mlz= 469.6780- 469.8780

MS ICIS

07261303

NL:

1.03E4 m/z= 471.6750- 471 .8750

MS ICIS

07261303

LU

48.0 48.5 49.0 49.5 50.0 50.5 51.0 51.5

Vol. 2 of 5 p. 731

C:\Xcalibur\Data\Dioxin\07261 3\07261 303 7/26/2013 10:29:17 AM 53720-85-21 MB

RI: 4773 - 5137 SM: 5G

NL:

242E2

C), mlz=

100- 457.8380

MS ICIS

07261303

80-

60-

40-

(N (N r w

-c C

(0 ci)

NL:

9.36E3 mlz= 469.6780- 469.8780

MS CIS

07261303

U

NL:C

1.03E4 mIz 471 .6750-

100 .- 471.8750

MS ICIS

I 07261303

NL:

2.77E2 mlz= 459.6350- 459.8350

MS ICIS

07261303

48.0 48.5 49.0 49.5 50.0 50.5 51.0

Vol. 2 of 5 p. 732

RT: 20.00 - 53.00

256 342 366100- 20.01 24.66 26.54 27.07

- 399 505 589 741

27.90 30.25 32.11 35.481 00

U

100 405 500 588

28.03 30.14 32 09

40-

20-

7/26/2013 10:29:17 AM 53720-85-21 MB

37.62 38,06 990

40.12 1008

40.42

, 42.37

NL:

8.44E4 m/z= 304.48180- 305.48180

MS

07261303

NL:

1.92E5 m/z= 330.47869- 331.47869

MS

07261303

NL:

1.17E5 mlz= 380.47550- 381.47550

MS

07261303

1310 1331 1370

1170 45.64 46.00 46.67

43.24 i

NL:

7.04E4 m/z= 392.47550- 393.47550

MS

07261303

1390 1466 1485 NL:

47.12 48.55 48.91 7.71E4 mIz 43047231- 431 .4723 1

MS

07261303

20 25 30 35 40 45 50

Vol. 2 of 5 p. 733

Vol. 2 of 5 p. 734 b

N a m e

M a t r i x

S a m p l e

R e c e i p t

D a t e

E x t

D a t e

A n a l y s i s

D a t e

E x t r a c t

V o l u m e p L

I n j e c t i o n

V o l u m e p L

D i l u t i o n F a c t o r

C o n c e n t r a t i o n

U n i t s

A N A L Y T E

T C D D l P e C D D

H x C D D l H x C D D l H x C D D

N p C D D

O C D D

T C D F l P e C D F

P e C D F l N x C D F l N x C D F

H x C D F

N x C D F l N p C D F

H p C D F a l

T E Q

S e d i m e n t s

T i m e

0 1 1 p g g d r y

P C D D

P C D F

A N A L Y S I S

D A T A

S H E E T

L a b

S a m p l e

I D

S a m p l e

W t V o l

I n i t i a l

C a l i b r a t i o n

D a t e

I n s t r u m e n t

I D

G C

C o l u m n

I D

S a m p l e

D a t a

F i l e n a m e

B l a n k

D a t a

F i l e n a m e

C a l

V e r

D a t a

F i l e n a m e

C o n c e n t r a t i o n

U n i t s

C O N C

D E T E C T I O N

F O U N D

L I M I T

I O N

R A T I O N

T E Q

L A B E L E D

C O M P O U N D S l C T C D D l C P e C D D l C H x C D D

C l N x C D D l C l N p C D D

C O C D D

C T C D F l C l P e C D F l C P e C D F l C l N x C D F l C N x C D F l C l N x C D F

C H x C D F l C l N p C D F l C l N p C D F

C L E A N U P

S T A N D A R D

C l T C D D

P a g e o f u n i t s gi n

D F S

G m

Z B p g

S P I K E

C O N C

C O N C

F O U N D

R

I O N

R A T I O

U f4

Vol. 2 of 5 p. 735 g e o f

F i l e n a m e:

A c q u i r e d

P r o c e s s e d

A n a l y t e

N O

N A P P I N G

C a l:

D

IC

A L

R e s u l t s

S a m p l e t e x t

S

C o m m e n t s

T y p

N a m e

Q N

A r e a

R M

A r e a

R A

R T

C o n c

T o x

D L

R e c

U n k

T C D F y

U n k

P e C D F y

U n k

P e C D F y

U n k

N x C D F y

U n k l N x C D F y

U n k

N x C D F y

U n k l N x C D F y

U n k l N p C D F y

U n k

N p C D F y

U n k

O C D F y tj nk

T O D D y

U n k

P e C D D y

U nk l H x C D D y ti nk

H x C D D y

U n k

H x y tj nk

H p C D D y

U n k

O C D D y

I S R T l C T C D F y

I S l C P e C D F y

I S

C P e C D F y

I S

C H x C D F y

I S l C l H x C D F y

I S l C N x C D F y

I S

C l H x C D F y

I S

C H p C D F y

I S

C l H p C D F y

I S

T O D D y

I S

C l P e C D D y

I S

C N x C D D y

I S

C H x C D D y

I S

C N p C D D y

I S

C O C D D y

R S

T O D D y

R S R T

C N x C D D y

C U p

T O D D y

T o t

T o t a l

T e t r a F u r a n s y

T o t

T o t a l

T e t r a D i o x i n s y

T o t

T o t a l

P e n t a F u r a n s y

T o t

T o t a l

P e n t a D i o x i n s y

T o t

T o t a l

H e x a F u r a n s y

T o t

T o t a l

H e x a D i o x i n s y

T o t

T o t a l

N e p t a F u r a n s y

T o t

T o t a l

H e p t a D i o x i n s y

Vol. 2 of 5 p. 736

C:\Xcalibur\Data\Dioxin\07261 3\07261 304 7/26/2013 11:32:40 AM 53720-85-08 20130922

RT: 18.95 - 28.27 SM: 5G

I

Wi C) c (U

(U

(U (U f\ !.

Co C) N N- C) U) x- N- N- C) N- N co 'N- C) C)

C) 14) - U) N- C) N- C) (0 N- ' LU

0) N N N N - N- C) N U) f

C) C)

AU N C

Co C) C) N C)

201 -

N- CO

NL:

7.70E2 mlz= 303.8020- 304.0020

MS ICIS

07261304

NL:

8.98E2 mlz= 305.7990- 305.9990

MS ICIS

07261304

NL:

9.01 E3

mlz= 315.8420- 316.0420

MS ICIS

07261304

(0 NC) N -

N- rLflC) tU) N- -COCo U) CO t Co Co C) C) - C) N N Co CO C) C) N C) C) N N

NL:

Co 1.11E4 N m/z= 317 8390-.

318.0390

MS ICIS

07261304

'- N - C)

I NL

() C) N C) c) t N C)

- N - C) Co - - N -

NL:

2. 36E 1 m/z= 375.7364- 375.9364

Time (mm)

Co Co

Vol. 2 of 5 p. 737

C:\Xcalibur\Data\Dioxin\07261 3\07261 304 7/26/2013 11:32:40 AM 53720-85-08 20130922 lOOT

80-

60-

(0 C\J 10 - N - (0 C)

C) (0 C) r- t

2O[

(0co (0 ('4 0)

80-

2O r-co

80-

60-

40- C)

ON 10 ('4

20-

21 22 23 24 25 26 27 28

Time (mm)

NL:

1.31E3 m/z= 319.7970- 319.9970

MS ICIS

07261304

1.75E3 m/z= 321.7940- 321 .9940

MS ICIS

07261304 mlz= 331.8370- 332.0370

MS ICIS

07261304

NL:

1.86E4 mIz 333.8340- 334.0340

MS ICIS

07261304

Vol. 2 of 5 p. 738

Chromatogram

RT: 24.9226.92 SM: SC

1 00-

C.) -

C -

40-cl

° 20-a 25.23

25.10 25.23

25.0 25.2

Erty: 2378-tcd B: 2375-TCDD

Entry Parameters

RT: 25.95

26.24 26.45 26.63 26.83

1.75E3 mz 321.82-

321.81 MS

07281304

1.31 E3

mJz 319.8$-

319.91 MS

0728132$

26.19 26.48 26.80 J I I I I I I I I

25.4 25.6 25.8 26.0 26.2 26.4 26.6 26.8 Time (mm)

Compound Name 2378-TCDD Entry Identifier 2378-tcdd QM Retention Time 25.95 QMArea 10828 RM1 Area 8383 RM1 Ratio (A) 0.7742 Amount (pg/g dry) 91.22 Percent Recovery (A) Detection Limit (A) 0.1532 Status Overview passed

TEF 1.0000

TEQ(A) 91.2180

Vol. 2 of 5 p. 739

C:\Xcalibur\Data\Dioxin\07261 3\07261 304

N I0

100 A a 10 C-) C a)4 a)

0)

N

100-

7/26/2013 11:32:40 AM 53720-85-08 20130922

10 I C)

N-

AA cC C01() N

CD

- co

C) co

NL:

1.48E3 mlz= 339.7600- 339.9600

MS ICIS

07261304

NL:

C) 8.98E2 co co to m/z=co CD

341 7570-10 .

341 9570N

N-

MS ICIS0)

07261304H0 co N 3-

C) C)

C) 1.11E4

CD

co c') co m/z= C) N- 351.8000-

352.0000

MSICIS

07261304

N C) 10 01 c) -

0) 10

(0 0 C) 0 0

N- C) c) tO

(0

CD N -

t N

NL:

2. 39E 1 mlz= 409.6974- 409.8974 MS lOIS 07261304

27 28 29 30 31 32 33 34 35 36 Time (miri)

Vol. 2 of 5 p. 740 co ArC - co co N 1.0 N-

100.J

C cr)

Loco

40 .. N

L() 0

(CC

It)

() (DLO(D

(0 C)

7/26/2013 11:32:40 AM 53720-85-08 20130922

C) r-co Q N N-

N (•.J

C)

CO

c

N

N co - It) tC N

N cC -

N (0 CO

N- It)

N OC)

C) C '2- It) COC)

N CO N N CO C) N

- CO CO N- N N

N-

CO

It)

CO

N 0 CO COLt) C)

It) N C Lo C) N- N It)

0 CO (0 N N- 0 N C) - N C) CO

CO - CO N N - (0 N It)

28 29 30 31 32 33 34 35 36 37

Vol. 2 of 5 p. 741

RT: 33.53- 35.53 SM: SC

100-

CD

80-

33.86CD

130-

40- a

20-

0- 100-

33.88

RT: 34.54

34.88

35.01 35,3434.34

34.19

33.6 33.8 34.0 34.2

Enfry: 12378-p'Ecdd IS: 123Th-PECDD

Entry Parameters

Compound Name 12378-PeCDD Entry Identifier 12378-pecdd QM Retention Time 34.54 QMArea 368 RM1 Area 234 RMI Ratio (A) 0.6362 Amount (pglg dry) 3.59 Percent Recovery (A) Detection Limit (A) 0.1312 Status Overview passed

TEF 1.0000

TEQ (A) 3.5923

34.90

- 35.08 35.28

34.4 34.6 34.8 35.0 35.2 35.4 Time (mm)

8.1 TEl

ntz=

555.87 MS

5.82E1

27.S a.

357.87 MS

07251304

Vol. 2 of 5 p. 742

C :\Xcalibur\Data\Dioxin\07261 3\07261 304

RT: 37.02 - 42.45 SM: 5G

ce.)

(0 r

80-: 'a-

LU

100-

60-c'J

40, C-) C c8 D a)

N-

('4 (0

(0

(0 C)

c) (0 (0

('4 'a-

LU

LU

Co Co 'a-

LU

0)

LU

Co

1.23E4 m/z= 387.7580- 387.9580

MS CIS

07261304

NL:

2.32E1

0 Co m/z=

0)

.. - LU

0) 'a- 445.6555-

('4 ., 445.8555

37.5 38.0 38.5 39.0 39.5 40.0 40.5 41.0 41.5 42.0

Vol. 2 of 5 p. 743

RT: 39.45-41.45 SM: SC

39.55100:

G) -

80-

59. 0

20- 39.71

- 39.55 100-

80-

40.03

0- I I I I I I

39.8 39.8 40.0

Ently: 23478-hxcdf IS: 2347S-HxCDF

Entry Parameters

Compound Name 234678-HxCDF Entry Identifier 234678-hxcdf QM Retention Time 40.49 QMArea 994 RM1 Area 804 RM1 Ratio (A) 0.8081 Amount (pg/g dry) 8.15 Percent Recovery (A) Detection Limit (A) 0.4404 Status Overview passed

TEF 0.1000

TEQ (A) 0.8147

40.02

RT: 45.49

RT: 40.49

40.3.

40.87 40.80 41.04 41,29

5.04E2 mtz 373.88-

373.84 MS

072C1304

40.74 40.87 41.07 41.27

WL:

32:9E2 rniz 3?S 80- 3Th84 MS 87261304

I I I I I I I I I I I I

40.2 40.4 40.8 40.8 41.0 41.2 41.4

Vol. 2 of 5 p. 744

RT: 40.62-42,62 SM: SG

1 00- -w

80- -ci

40- -

40.87 41.07 41.27

20-

RT: 41,59

C 40.80 41.04 41.29

41.74

41.90 42.05 42.28 4a50

42.23 42.48

I .04E2 mJz 373.80-

373.24 MS

0F25I30-4

SCIEI

mIz 37520-

3754 MS

07251304

40.8 41,0 41.2 41,4 41.6 41.8 42.0 42.2 42.4 42,8 Time (mm)

Erifry: 123789-hxcdf IS: 123720-I-IxCDF

Entry Parameters

Compound Name 123789-HxCDF Entry Identifier 123789-hxcdf QM Retention Time 41.59 QMArea 172 RM1 Area 128 RM1 Ratio (A) 0.7417 Amount (pg/g dry) 1.37 Percent Recovery (A) Detection Limit (A) 0.4392 Status Overview passed

TEF 0.1000

TEQ(A) 0.1370

RI: $1.59

Vol. 2 of 5 p. 745

C:\Xcahbur\Data\Dioxjn\07261 3\07261 304

RT: 36.25 - 42.67 SM: 5G

a)o8 C

-o

:3

('3

a) !LJ

NL:

9.00E2 m/z= 389.7160- 389.9160

MS ICIS

07261304

(0

NL:

7.10E2 m/z= 391.7130- 391 .9130

MS ICIS

07261304

.0 c.-J

I

7/2612013 11:32:40 AM 53720-85-08 20130922

co co It)It) co(3) c)

[1 co 0)

N-co

c) (.C)

(0 N-)

(0 N- 0) C N-

(0

(0-

NL:

1.78E4 m/z= 401.7560- 401 .9560

MS ICIS

07261304

NL:

1.48E4 mlz= 403.7530- 403.9530 MS lOIS 07261304

37 38 39 40 41 42

Vol. 2 of 5 p. 746

RT: 3978-41.76 SM: 5G

39.83

1) -

80-

C 60-

40.8740-

RT:40.72R20-

40.07 $0.25

41.32

41.58

Entry: '12a47s.,hxdd IS: 12347S-HxCDD

Entry Parameters

Compound Name 123478-HxCDD Entry Identifier 123478-hxcdd QM Retention Time 40.72 QMArea 367 RM1 Area 266 RMI Ratio (A) 0.7236 Amount (pglg dry) 4.24 Percent Recovery (A) Detection Limit (A) 0.4954 Status Overview passed

TEF 0.1000

TEQ (A) 0.4245

\ 40,07 4025 I I I I I

39.8 40,0 40.2

40.87

RT:40.72

Ti iii

40.4 40.6 40.8

Time (mm)

41.32

I I I I I I I

41.0 41,2 41.4 41.8

9.00E2 rn/z

3aa24 MS O721 354

7.10 E2

miz a91,79-

391.83 MS

07291354

Vol. 2 of 5 p. 747

100-fl

(0 C) 10 -

C-) C

C

(t2 a)

7/26/2013 11:32:40 AM 53720-85-08 20130922

C)o f (0 (0 N

(0 A (0

LL E J

C) N- N

CO C)

J.

o N N- co C) N- CO aD

A '-'

- c)cO CO N r r r

NL:

C) N- 1.05E4 N

N- N- mlz= 421,7190- 421.9190

(\ 07261304

40 H Hco N Co

N-

1( ON-

20 J L I

NL:

1.66E2 m/z= 479.6165-

79 8165

100TI

4 .

MS ICIS

80 07261304

40 fl N

I_____________________ r

43 44 45 46 47 48 Time (mm)

NL:

5.63E3 m/z= 409.6789- 409.8789

MS ICIS

07261304

NL:

1.09E4 m/z= 419.7220- 419.9220

MS ICIS

07261304

NL:

5.95E3 mlz= 407.6818- 407.8818

MS 1015

Vol. 2 of 5 p. 748

C:\XcaHbur\Data\Dioxin\07261 3\07261 304

6O-

40-

7/26/2013 11:32:40 AM 53720-85-08 20130922

N- C r- cc (N C) (N cc

'- '- c) -w o8 C -c

(N

(N (N

43 44 cc (C (N

C

0) cc

- N-C0)

UI'

cc cc cc ce.)

IC)

N

It) N-

NL:

5.99E3 mlz= 423.6770- 423.8770

MS ICIS

07261304

5.95E3 mlz= 425.6740- 425.8740

MS ICIS

07261304 cc cc IC) (N It)

'- (N CO

It)

CO

C) It)

CO

CO

Time (mm)

NL:

8.81 E3

mlz= 435.7170- 435.9170

MS ICIS

07261304

NL:

8.15E3 m/z= 437.7140- 437.9140 MS lOIS

Vol. 2 of 5 p. 749

C:\Xcalibur\Data\Djoxin\07261 3\07261 304 7/26/2013 11:32:40 AM 53720-85-08 20130922

NL:

i 6.27E3 mlz= 441.6430-

441.8430100 A MS ICIS

ii 07261304 l N- Q C)

(N

N- . CD

0 NL:

(N

7.14E3 (NC', mlz=

443.6400-

100 MSICIS

I 07261304 80-

60-

40-t_ __________

(N P t C')

NL:

1.03E4 mlz= 469.6780- 469.8780

MS ICIS

07261304

C', cC (0 C)

1.13E4 mlz= 471.6750- 471 .8750

MS ICIS

07261304

IC) N -

IC) co C', '-

F F F F

48.0 48.5 49.0 49,5 50.0 50.5 51.0 51.5

Vol. 2 of 5 p. 750

C:\Xcalibur\Data\Djoxin\07261 3\07261 304 7/26/2013 11:32:40 AM 53720-85O8 20130922

RT: 47.73 - 51.37 SM: 5G / NL:

C) 3.24E4 mlz= 457.6380- 457.8380

100-i MS lOIS 07261304

6o

4o

-0 i

NL:

3.70E4 mlz= 459,6350- 459.8350

100 MS lOIS 07261304

80-c Co -c J

NL:

1.03E4

C) m/z=IC) 469.6780- 469.8780

100 MS lOIS 07261304

0 NL:

1,13E4 cC mlz=C) 471.6750- 471.8750

100 MS 1015

07261304

48.0 48.5 49.0 49.5 50.0 50.5 51.0

Vol. 2 of 5 p. 751

C:\XcaIibur\Data\Dioxn\07261 3\07261 304

52 117 289 368 ioo 21.63 25.38 27.11

NL:

8.10E4 mlz= 304.48180- 305.48180

MS

07261304

7/26/2013 11:32:40 AM 53720-85-08 20130922

402 42? ii öö4 787

1001 27.96 28.41 30.87 33.77 36.49 804 36.87

100 402 509 522 560 37.46 40.15 42.11 42.97

27.96 30.33 3062 31.46 a)

NL:

1.80E5 mlz= 330.47869- 331.47869

MS

07261304

NL:

1.15E5 mlz= 380.47550- 381 .47550

MS

07261304

1167 ii

43.19 44.46 46.58 46.95

2o1

NL:

6.98E4 m/z= 392.47550- 393.47550

MS

07261304

NL:1394 1412 1470 1647 7.61E4

47.19 47.53 48,62 51.94 m/z=

J430.4723 1- 31.47231

MS

07261304

25 30 35 40 45 50

Vol. 2 of 5 p. 752 b

N a m e

M a t r i x

S a m p l e

R e c e i p t

D a t e

E x t

D a t e

A n a l y s i s

D a t e

E x t r a c t

V o l u m e p L

I n j e c t i o n

V o l u m e p L

D i l u t i o n F a c t o r

C o n c e n t r a t i o n

U n i t s

A N A L Y T E

T C D D l P e C D D l H x C D D

H x C D D l H x C D D l H p C D D

D C D D

T C D F l P e C D F

P e C D F

H x C D F

H x C D F

H x C D F

H x C D F

H p C D F

H p C D F

D C D F

T o t a l

T E Q

S e d i m e n t s

T i m e

0 1 1 p g g d r y

P C D D

P C D F

A N A L Y S I S

D A T A

S H E E T

L a b

S a m p l e

I D

S a m p l e

W t V o l

I n i t i a l

C a l i b r a t i o n

D a t e

I n s t r u m e n t

I D

C C

C o l u m n

I D

S a m p l e

D a t a

F i l e n a m e

B l a n k

D a t a

F i l e n a m e

C a l

V e r

D a t a

F i l e n a m e

C o n c e n t r a t i o n

U n i t s

C O N C

D E T E C T I O N

F O U N D

L I M I T

I O N

R A T I O N

T E Q

L A B E L E D

C O N F O U N D S l C T C D D

C l P e C D D

C l H x C D D l C H x C D D l C l H p C D D

C O C D D l C T C D F

C l P e C D F l C P e C D F l C H x C D F

C l H x C D F

C H x C D F

C H x C D F

C l H p C D F l C l H p C D F

C L E A N U P

S T A N D A R D

C T C D D

P a g e o f u n i t s p m

D F S m

E B p g

S P I K E

C O N C

C O N C

F O U N D

R

I O N

R A T I O

Vol. 2 of 5 p. 753 g e o f

F i l e n a m e:

A c q u i r e d

P r o c e s s e d

A n a l y t e

N O

M A P P I N G

C a l

D I C A L

R e s u l t s

S a m p l e t e x t

C o m m e n t s

T y p

N a m e

Q M

A r e a

R M

A r e a

R A

R T

C o n c

T o x

D L

R e c

[i nk T C D F y

U n k l P e C D F y

U n k

P e C D F y

[i nk l H x C D F y

U n k l N x C D F y

U n k

N x C D F y

[i nk l H x C D F y

[i nk l H p C D F y tl nk l N p C D F y

[i nk

O C D F y

[i nk

T C D D y

[i nk l P e C D D y

[i nk

H x C D D y

[i nk l H x C D D y

[i nk l H x C D D y

[i nk l H p C D D y

[i nk

O C D D y

I S N T l C T C D F y

I S

C l P e C D F y

I S l C P e C D F y

I S l C l H x C D F y

I S l C l H x C D F y

I S l C x C J F y

I S l C l H x C D F y

I S l C l N p C D F y

I S l C l H p C D F y

I S l C T C D D y

I S l C l P e C D D y

I S l C l H x C D D y

I S l C l H x C D D y

I S l C N p C D D y

I S l C O C D D y

R S l C l T C D D y

R S R T

C l E x C D D y

C U p

C l T C D D y

T o t

T o t a l

T e t r a F u r a n s y

T o t

T o t a l

T e t r a D i o x i n s y

T o t

T o t a l

P e n t a F u r a n s y

T o t

T o t a l

P e n t a D i o x i n s y

T o t

T o t a l

H e x a F u r a n s y

T o t

T o t a l

H e x a D i o x i n s y

T o t

T o t a l

N e p t a F u r a n s y

T o t

T o t a l

N e p t a D i o x i n s y

Vol. 2 of 5 p. 754

C:\Xcahbur\Data\Doxjn\0726 1 3\07261 305 7/26/2013 12:36:01 PM 53720-85-09 20130923

RT: 18.95 -28.27 SM: 5G

NL:

/ 4.52E2 mlz= 303,8020-

1OO 304.0020

MS CIS

07261305 o 5.85E2 m/z= 305.7990-

-100 305.9990 r- r- MS ICIS 80 C" 07261305

U' W D II J LJL. ..

7.32E3co m/z= 315.8420- 316.0420

100- MS ICIS

80- 07261305

N-

' (0 N- N-

'2 N- N -r'- car- N ' N- CO 0 N- C) N- N- (C) 0) (0 0 C") ' C) N CO (C) C) CO 't N -

2o j ai ii iiiiii L\LIil_ _

NL:

9.17E3

N-mlz= 317.8390- 318.0390

100] MS ICIS

07261305

(0 It)(00) N- N

N- C) C') CO It) C") (0 N-N co co Co co N - N-

-C)(0 IC)

LC)I.t)N r

NL:

2. 34E 1 m/z= 375.7364- 375.9364

MS ICIS

07261305

19 20 21 22 23 24 25 26 27 28

Vol. 2 of 5 p. 755

C:\Xcalibur\Data\Dioxin\0726 1 3\07261 305

RT: 2078 - 28.43 SM: SG

I o8 C

C

-o

('3 a)

I

7/26/2013 12:36:01 PM 53720-85-09 20130923

(N '4-)

CN/

LI-)

C', llL J

I LX> /\. r

N- O N I I CO LC) Co LI) 0) CO 0) N- Q (0 N- N- (0 LI) Co

I N-N-N- I\1,c2r to

C', N

21 22 23 24 25 26 27 28

Vol. 2 of 5 p. 756

C:\Xcalibur\Data\Dioxin\07261 3\07261 305

(0 0)

(0 100-or' cl)l C) C

-o C ci) ci)

I

NL:

2.17E1

'ci- (0 mlz=

409.6974- 409.8974

MSICIS

20 /

F IJ I IrF1r1-fT L11 r

27 28 29 30 31 32 33 34 35 36 Time (mm)

N N- Cr)

7/26/2013 12:36:01 PM 53720-85-09 20130923

N co (0 (0

C', .ji

NL:

(0 co 4.49E3

Cr) Co

-Cr) m/z=

N 353.7970- 353.9970

MSICIS

A 07261305

NL:

8.83E2 m/z= 339.7600- 339.9600

MS ICIS

07261305

NL:

5.25E2 m/z 341.7570- 341.9570

MS ICIS

07261305

NL:

7.35E3 m/z= 351.8000- 352.0000

MS ICIS

07261305

Vol. 2 of 5 p. 757

C:\Xcalibur\Data\Dioxjn\07261 3\07261 305 7/26/2013 12:36:01 PM 53720-85-09 20130923

N- C.'4

N-.

(DN-

CoN-

1 00-

ci) C-) C Cxl -c

Co Cot- N - LC)Co L()

ci) 40 C_'4.. Co

Co's C) - C'J C.'J '- co

N-

CO

C)

Co

LC•)

CO

A c'N-r L cr 0 Coç.' C'4

1.06E2 m/z= 357.7520- 357.9520

MS ICIS

07261305

A. .1 L A

'- 0 C) c'4 CO C'4 C'4

IN-

IC)

C'J

L

C)

IC)

Co ("4

CO

N- '-N-c'4 C\J-

NL:

1.49E2 mlz= 355.7550- 355.9550

MS ICIS

07261305

NL:

5.13E3 mlz= 367.7950- 367.9950

MS ICIS

07261305

NL:

3. 34E3 mlz= 369.7920 369.9920

MS ICIS

07261305

IC)

'- Co cOC) N- 0 CC I 0 IC)'- t C) Co r r r

W _____________AL

rji ri I T1]1 1FT

28 29 30 31 32 33 34 35 36 37

Vol. 2 of 5 p. 758

RI: 33.49-35.49 SM: 50

1 00-

80- 33.84 Co /\ °' 40- ---------

CO

20-a- 100- 33.81

8U

3i!2.1 34.19

RT:

34.81

35.30

35.25

33.6 33.8 34.0 34,2 34.4 34.6 34.8 35.0 35.2 35.4 Time (mm)

Entry: i22J5pcdd iS: 1237S-PoCDC

Entry Parameters

Compound Name 12378-PeCDD Entry Identifier 12378-pecdd QM Retention Time 34.48 QMArea 186 RM1 Area 108 RM1 Ratio (A) 0.5808 Amount (pglg dry) 2.56 Percent Recovery (A) Detection Limit (A) 0.1409 Status Overview passed

TEF 1.0000

TEQ (A) 2.5633

34.08 34.21

RT: 34.4$

34.83 35.01

IlL:

§.SCEI

m/Z=

3.54-

355.57 MS

07261 30S

355 El m/z

357.37 MS

0726 130S

Vol. 2 of 5 p. 759

37.5 38.0 38.5 39.0 39.5 40.0 40.5 41.0 41.5 42.0

Vol. 2 of 5 p. 760

RT: 40.62- 42.62 SM: 5G

4x3 80-

60- RT:41.58/

403141

20-

709E1 mz= 373.80-

373.84 MS

07261306

42,08 42.40

40,86 4109

40.8 41.0 41.2

Entry: 1237S9-hxcdf IS: 123789-I4xCDF

Entry Parameters

Compound Name 123789-HxCDF Entry Identifier 123789-hxcdf QM Retention Time 41.58 QMArea 70 RM1 Area 55 RM1 Ratio (A) 0.7932 Amount (pg/g dry) 0.94 Percent Recovery (A) Detection Limit (A) 0.51 36 Status Overview passed

TEF 0.1000

TEQ (A) 0.0942

41.35

41.73

RT:41.59 I

41.59 /

41.4 41.6 41.8 Time (mm)

52SEI

miz 37680-

42.03

37584 MS

- 42.27 42A8 07261305

42.0 42.2 42.4 42.6

Vol. 2 of 5 p. 761

C:\Xcalibur\Data\Dioxin\07261 3\07261 305

RI: 3625 - 42.67 SM: 5G

40-wo8 C (0 -o C

(0 ci)

NL:

6.34E2 m/z=

389.7 1 60- 389.9160

MS ICIS

07261305

OD

C

(N

(N N- C (N

(N L() (N

U a) N- L•) L) co

LU

NL:

5.30E2 m/z= 391.7130- 391 .91 30

MS ICIS

07261305

I

(N

- LC)

(i.)

37 38 39 40 Time (mm)

NL:

CDa) 1.05E4 It)(N It) m/z=

401.7560- 401.9560

C MS lOIS c)

07261305 N- 0) coN

CD.

M

NL:

8.23E3

Co m/z 403.7530- 403.9530

C) MSICIS

C ! 07261305COC)

N-N 1/

41 42

Vol. 2 of 5 p. 762

RT: 39.73-41.73 SM: SC

39.80

ci) C) -

CD

C rJ

40-

CU

20- 40,07

39.80

I I

39.8 40.0

40.32 40.47

41.33

41.04 41.56

NL:

C.34E2 m/z

309.80-

389.24 MS

07281305

'NL:

5.3.0E2 rnk

391,73-

391.83 MS

07251305

40.86 RT:40.72f

40.30 40.54 I I I I I I I I

40.2 $0.4 40.6 40.8 Time (mm)

Entry: 123470-hxcdd IS: 123.4784-bcCDD

Entry Parameters

Compound Name 123478-HxCDD Entry Identifier 123478-hxcdd QM Retention Time 40.72 QMArea 201 RM1 Area 147 RM1 Ratio (A) 0.7295 Amount (pg/g dry) 3.49 Percent Recovery (A) Detection Limit (A) 0.5581 Status Overview passed

TEF 0.1000

TEQ (A) 0.3490

40.86

RT: 40.72

40.72

41.33

$1.12 $1.63 I I I I I

41.0 41.2 41,4 41.5

Vol. 2 of 5 p. 763

RT: 40.3342.33 SM: 5G

100-

(2* -

(L

40-

2:1 0,47

100-

40.72

41.04

RT: 41.33

41.56 41.78 41.90 42.05

Nt:

2.32E2 mz

389.54 MS

42.25 O7213O

40.72

40.54

40.4 40.6 40.8 41.0

Enfry: 123789-hxcdd IS: AvSTDI4xD

Entry Parameters

Compound Name 123789-HxCDD Entry Identifier 123789-hxcdd QM Retention Time 41.33 QM Area 639 RM1 Area 481 RM1 Ratio (A) 0.7531 Amount (pg/g dry) 10.80 Percent Recovery (A) Detection Limit (A) 0.5123 Status Overview passed

TEE 0,1000

TEQ (A) 1.0803

40.88

41.2 41.4 41.6 41.8 42.0 42.2

Vol. 2 of 5 p. 764

C:\Xcahbur\Data\Djoxin\07261 3\07261 305 7/26/2013 12:36:01 PM 53720-85-09 20130923

C / (0

100-a)1 C

C a)

Co a)

1\.

H Fi:; f\

LL L

C N- (0 Cv, Cv)

LC) C) r

NL:

3.50E3 m/z= 407.6818- 407.8818

MS ICIS

07261305

NL:

3.29E3 mlz= 409.6789- 409.8789

MS 1015

07261305

N- 2 L() (0 t ;

NL:

8.08E3 mfz= 419,7220- 419.9220

MS ICIS

I 07261305

N- CO (0 t 0

(0 C'J I I CO CO ('4 CO

C) L(JL IL

NL:

7.47E3 m/z= 421.7190- 421 .9190

MS ICIS

07261305

(0 0)0

NL:

1.05E2

C) I-mz-C)

479.6165- 479.8165

A MS ICIS

07261305

(N

Time (mm)

' N -coco

'-(N

I 1 1 1 T rjrrpmrmflrri

43 44

Vol. 2 of 5 p. 765

C :\Xcalibur\Data\Dioxin\07261 3\07261 305

RT: 4208 - 48.50 SM: 5G

100-i

a) o8 C

C

-o a)

D 0) L•) (q c (00 0) cr

LOT- IC)

43 44 ct co Cit coo

It) c'J c.'J

7/26/2013 12:36:01 PM 53720-85-09 20130923

I -.'- co

Lt)(0 t(0 It) '-C•'J N-(0 (N (0

It)

IC)

c) 0) colt) c•) r-Lt) C4

(oLt)cO c) 0)

('4

N- ('40 Ic)

It) It) (0 It) 0) r co - ('U) Q - co it) c) co 0)

45 46 Time (mm)

NL:

3.46E3 mlz= 423.6770- 423.8770

MS ICIS

07261305

NL:

3.32E3 m/z= 425.6740- 425.8740

MS ICIS

07261305

NL:

4.73E3 mlz= 435.7170- 435.9170

MS ICIS

07261305

NL:

4.30E3 m/z= 437,7140-

437. 9140

MS ICIS

07261305

(0

47 48

Vol. 2 of 5 p. 766

C:\XcaIibur\Data\Dioxn\0726 1 3\0726 1305 7/26/2013 12:36:01 PM 53720-85-09 20130923

NL:

2.51E3 mlz= 441.6430-

441.8430100 MS ICIS

07261305

NL:

2.79E3 mlz= 443.6400-

100 443.8400

MS 1015

07261305

L. _

NL:

5.36E3 mlz= 469.6780- 469.8780

MS ICIS

07261305

0) ce.)

NL:

5.86E3 co

('4 mlz= 471 .6750 471.8750

MS ICIS

07261305

H-

J 0)

20-

TIH 1E

48.0 48.5 49.0 49.5 50.0 50.5 51.0 51.5

Vol. 2 of 5 p. 767 o :\Xcalibur\Data\Dioxin\07261 3\07261 305 7/26/2013 12:36:01 PM 53720-85-09 20130923

RT: 47.73- 51.37 SM: 5G

NL:/ 1.37E4

LU mlz= 457.6380-

100 457.8380

MS ICIS

07261305

60 I40 L20-

NL:

1.48E4

(0 m/z= 459.6350-

MS ICIS

07261305 o 80 C H (0 H

-Q

40-

20-

NL:

5.36E3 m/z= 469.6780- 469.8780

MS 1015

07261305

NL:

0) (vU) 5.86E3 aDLU mlz=

471.6750- 471.8750

A MS CIS

07261305

48.0 48.5 49.0 49.5 50.0 50.5 51.0 Time (mn)

Vol. 2 of 5 p. 768

C:\Xcalibur\Data\ljioxin\0726 1 3\07261 305

21 08 107 282

21 41 25.23 358 fi 26.89 27.68

7/26/2013 12:36:01 PM 53720-85-09 20130923

NL:

427 622 634 1.65E529.18

32.84 33.11 m/z= 100- 28.52

- 399 781 330.47869- 80- 27.90 36.36 331 .47869

MS

60 07261305

40-

20-a

0j

456 NL:621

9.02E4427 2916 32.82 633 928 1120100 28.52 33.08 893 3908

42.30 1159 mlz

380.47550-38.49 80 381 .47550

42.95

MS

07261305 ci)

NL:

7.03E4 m/z= 304.48180- 305.48180

MS

07261305

NL:

4.96E4 mlz= 392.47550- 393.47550

MS

07261305

1174 43.55 45.82 1341 43.31

AI 46.18

1570 1677 NL:

1408 50 50 52.50 5.79E4.1391 47.46

47 14. 430.47231- 431.47231

MS

07261305

20 25 30 35 40 45 50

Vol. 2 of 5 p. 769

Vol. 2 of 5 p. 770 b

N a m e

N a t c i x

S a m p l e

R e c e i p t

D a t e

E x t

D a t e

A n a l y s i s

D a t e

E x t r a c t

V o l u m e p L

I n j e c t i o n

V o l u m e p L

D i l u t i o n F a c t o r

C o n c e n t r a t i o n

U n i t s

A N A L Y T E

T C D D

P e C D D l H x C D D

H x C D D l H x C D D l H p C D D

O C D D

T C D F

P e C D F

P e C D F l H x C D F l H x C D F

H x C D F

H x C D F

H p C

D R l H p C D F

O C D F

T o t a l

T E Q

S e d i m e n t s

T i m e

0 1 1 p g g d r y

P C D D

P C D F

A N A L Y S I S

D A T A

S H E E T

L a b

S a m p l e

I D

S a m p l e

W t V o l

I n i t i a l

C a l i b r a t i o n

D a t e

I n s t r u m e n t

I D

G C

C o l u m n

I D

S a m p l e

D a t a

F i l e n a m e

B l a n k

D a t a

F i l e n a m e

C a l

V e r

D a t a

F i l e n a m e

C o n c e n t r a t i o n

U n i t s

C O N C

D E T E C T I O N

F O U N D

L I M I T

I O N

N A T I O N n d

9.

.0 n d

T E Q

L A B E L E D

C O M P O U N D S l C T C D D l C P e C D D n d l C l N x C D D l C l H x C D D l C l N p C D D l C O C D D l C T C D F l C l P e C D F l C P e C D F l C l H x C D F l C l N x C D F l C l N x C D F n d l C N x C D F l C l N p C D F l C l N p C D F

C L E A N U P

S T A N D A R D

C T C D D

P a g e o f l u n i t s g m

D F S m

Z B p g

S P I K E

C O N C

C O N C

F O U N D

R

I O N

R A T I O

Vol. 2 of 5 p. 771 g e o f

F i l e n a m e

A c q u i r e d

P r o c e s s e d

A n a l y t e

N O

N A P P I N G

C a l

D I C A L

R e s u l t s

S a m p l e t e x t

C o m m e n t s

T y p

N a m e

Q M

A r e a

R M

A r e a

R A

R T

C o n c

T O x

D L

R e c

U n k

T C D F y

U n k

P e C D F y

U n k

P e C D F y

U n k

N x C D F y

D n k

N x C D F y

U n k

N x C D F y

U n k l N x C D F n n d n d

U n k

N p C D F y

U n k

N p C D F y

D n k

O C D F y

U n k

T O D D y

U n k

P e y

U n k

N x C D D n n d n d

U n k

N x C D D y

U n k

H x C D D y

U n k l H p C D D y

U n k y

I S R I

C T C D F y

I S l C P e C D F y

I S

C P e C D F y

I S

C N x C D F y

I S

C l H x C D F y

C N x C D F y

C H x C D F y

I S

C N p C D F y

I S

C l N p C D F y

I S

T O D D y

I S

C P e C D D y

I S

C H x C D D y

I S

C H x C D D y

I S

C N p C D D y

[5 C O C D D y

R S

T O D D y

R S R T

C N x C D D y

C/ ti p

T O D D y

T o t

T o t a l

T e t r a F u r a n s y

T o t

T o t a l

T e t r a D i o x i n s y

T o t

T o t a l

P e n t a F u r a n s y

T o t

T o t a l

P e n t a D i o x i n s y

T o t

T o t a l

N e x a F u r a n s y

T o t

T o t a l

H e x a D i o x i n s y

T o t

T o t a l

H e p t a F u r a n s y

T o t

T o t a l

H e p t a D i o x i n s y

Vol. 2 of 5 p. 772

C:\XcaIbur\Data\Dioxin\O7261 3\07261 306 7/26/2013 139:19 PM 53720-85-10 20130924

RT: 18.95-28.27 SM: 50

4.bbt m/z= 303.8020-

0100 304.002

07261306

5.60E2 mlz= 305.7990-

1oo- 305.9990 LU . MS lOIS

80- 07261306 o . _______________________________ NL:

8.28E3 m/z= 315.8420- 316 0 20

W 100 A . 4

MS lOIS 80 07261306

NL:

1.03E4 mlz=

100 MS lOIS

61306 v 2.73E1 m/z= 375.7364- 375.9364

100 A MS lOIS

8OT . . .. .. .. . A J 07261306

19 20 21 22 23 24 25 26 27 28

Vol. 2 of 5 p. 773

C:\Xcahbur\Data\Dioxin\07261 3\07261 306

LC)

(0

a) C (0 -o C

0)

(0 0)

7/26/2013 1:39:19 PM 53720-85-10 20130924

(0 1

('1

I - (N 0 Ce) - co r- - -

(0 (N (0 Ce)

(0 C)

Time (mm)

NL:

1.45E4 mlz= 333.8340- 334.0340 MS lOIS 07261306

Vol. 2 of 5 p. 774

C:\Xcalibur\Data\Dioxin\07261 3\07261 306 7/26/2013 1:39:19 PM 53720-85-10 20130924

RT : 26.65 - 36.79 SM: 5G

NL:

6.03E2 m/z= 339.7600-

100- / 339.9600

07261306

3.73E2 mlz= 341.7570- 341.9570

100- MS ICIS

80 .. 07261306 f\ IL.

4.44E3 (N (N m/z= 353.7970- 353.9970

2,26E1

- mIz= ci 'i- 409.6974-r 409.8974

F F - F J 1T I fT FTI

27 28 29 30 31 32 33 34 35 36

Vol. 2 of 5 p. 775

RT: 30.82-32.82 SM: SC

31.10

100- Cu

80- Cu

1:

40-

31,08 100 A

31.0 31.2

Entrj: '122.Th-pEcdf S: i238-PeCOF

Entry Parameters

RT: 31.81

32.01

I I I I I I I

31.4 31.6 31.8 32.0 Time (mm)

Compound Name 12378-PeCDF Entry Identifier 12378-pecdf QM Retention Time 31.83 QMArea 521 RM1 Area 338 RM1 Ratio (A) 0.6487 Amount (pglg dry) 5.19 Percent Recovery (A) Detection Limit (A) 0.3776 Status Overview passed

TEF 0.0300

TEQ (A) 0.1556

31.65

/'- RT:31.83

31.45

32.54

32.21

32.54

32.23 ae8E2 rmz 33as4-aass MS 072e12.Oe

2.32E2 mz 341.84-

341.87 MS

O7231 3O

32.2 32.4 32.6 32.8

Vol. 2 of 5 p. 776

C:\Xcalibur\Data\Dioxin\07261 3\07261 306 7/26/2013 1:39:19 PM 53720-85-10 20130924

RT: 2665 - 36.79 SM: 5G

NL:

6.03E2

0) m/z= 339.7600-

I / 339.9600

. / / 07261306

Li iu i 3.73E2

0) m/z= c' 341.7570-

00) . 341.957

100 MS ICIS

80 / 07261306 cj 100 MS ICIS 80- 07261306

H I 4.44E3 m/z=

C) .. 353.7970-

353.9970

100: MS ICIS

80 0726130611.

NL:

2.26E1 m/z= 409.6974- 409.8974

27 28 29 30 31 32 33 34 35 36

Vol. 2 of 5 p. 777

C:\Xcalibur\Data\Dioxjn\07261 3\07261 306

RT: 27.74 37.50 SM: 5G

-Q -(C

40- c

20- ('.-

a) C

60 ()Q

40-

201!1

7/26/2013 1:39:19 PM 53720-85-10 20130924

NL:

1.18E2 m/z= 355.7550- 355.9550

) MS ICIS

07261306 cC (C C)C) R

T N r r - N

!\ ; A1 A

N N C) cC 0 Nco 0 LU2 co

0 - CC.. 0

C) d co (C)

A I\ <I A A

N

(0 o (0 N

It) N-

-0 N It) 00 r r Cfl r

NL:

8.38E1 m/z= 357.7520- 357.9520

MS ICIS

07261306

NL:

5.92E3 mlz= 367.7950- 367.9950

MS ICIS

07261306

NL:

3.78E3 m/z= 369.7920-

- 369.9920100 H MS lOIS 07261306

40 H (0 N I co Ho NNJ

LOcO(0 C) - C)20 - -

0 1 1 1 1 r I I

28 29 30 31 32 33 34 35 36 37 Time (mm)

N-

(C)

N C) N c) t (0

Vol. 2 of 5 p. 778

RI: 33.60-35.50 SM: SC

100- 33.35

a) -

80-

I so- ° 33.65

40-

20-

34.11

RI: 34.49

- 35.29

NL:

4, 42E I

355.54-

355.57 MS

a: 34.09 34.27

RT: 34.51 NL

2..-4E 1 rn 357.23-

/ 35.35 357 31 MS

33.6 33,8 34.0 34.2

Eaty: 1 2372-pcdd IS: 12372-PCDD

Entry Parameters

Compound Name 12378-PeCDD Entry Identifier 12378-pecdd QM Retention Time 34.49 QMArea 137 RM1 Area 83 RMI Ratio (A) 0.6043 Amount (pglg dry) 1.91 Percent Recovery (A) Detection Limit (A) 0.1104 Status Overview passed

IEF 1.0000

IEQ(A) 1.9105

34.4 34.6 34.8 35.0 35.2 35.4 Time (mirI)

Vol. 2 of 5 p. 779

C:\Xcalibur\Data\Dioxin\07261 3\07261 306

RT: 37.02 42.45 SM: 5G

80 0 c) L()60

A

0) N-

10011 80 A 60- (N

(N

Wi C (t3

C

W

W

(0

It) 0)

100- (N A

(N

53720-85-10 20130924

N-co

0co0 (0

N- It)

Co C,)

(0co

C,)

NL:

1.03E3 mlz= 373.7210- 373.9210 MS lOIS 07261306

NL:

7.99E2 m/z= 375.7180- 375.9180

MS ICIS

07261306

NL:

7.85E3 mlz= 385.7610-

385.96 10

MS ICIS

07261306

JL JL

6.30E3 mlz= 387.7580-

(N .. (N 387 9580.

MSICIS

07261306

It) 2.14E1

C,) It) N- mlz= cj

':j- 445.6555- 445.8555

A A A A 07261306

37.5 38.0 38,5 39.0 39.5 40.0 40.5 41,0 41.5 42.0

Vol. 2 of 5 p. 780

RT: 38.55 40.55 SM: SC

1 00 U) - 0 - C (U

-U) C -

. 38.59

38.69

/ \, 38.92 39,10 I I I I I

38.6 38.8 39.0 39.2

Ertry: 123e7&.hxcdj IS: 12aS7S-4xCDF

Entry Parameters

Compound Name 123678-HxCDF Entry Identifier 1 23678hxcdf QM Retention Time 39.54 QMArea 1402 RM1 Area 1125 RM1 Ratio (A) 0.8024 Amount (pglg dry) 20.18 Percent Recovery (A) Detection Limit (A) 0.5020 Status Overview passed

TEE 0.1000

TEQ(A) 2.0184

39.36

RT: 39.54

40.46 :g.ss 40.01 40.20

I .03E3 nifz 373.e3

37324 MS

oaei ace

RT: 39.52

39.81 4001 40.46

39.4 39.6 39.8 40.0 40.2 40.4 Time (mm)

7.99E2 rn/zr

37504 MS

07201305

Vol. 2 of 5 p. 781

RI: 36.25 - 42.67 SM: 5G

lOOT c00)

NL:

3.40E2 m/z= 389.7160- 3899160

MS ICIS

07261306

C) (0

C) co (N r a)o8 C

C

Co ci) o co N- (N

N- (0 (N

Li

(0 N-

1.0(0 (N () (N 0

37 38 39 40 Time (mm)

C) C)

Ah

NL:

2.71E2 m/z= 391.7130- 391 .9130

MS ICIS

07261306

Cc

NL:

1.03E4 mlz= 401.7560- 401 .9560 MS lOtS 07261306

NL:

8.23E3 mlz= 403.7530- 403.9530 MS lOIS

Vol. 2 of 5 p. 782

C :\Xcalibur\Data\D ioxin\07261 3\07261 306 7/26/2013 1:39:19 PM 53720-85-10 20130924

RT: 4208 - 48.50 SM: 5G

NL:

354E3 co/ mlz= / 407.6818-

407.8818

100 MS ICIS

80 07261306

20I

NL:

3.28E3 m/z= 409,6789-

09 789

4 .8

07261306

20- J

NL:

6.72E3 mlz= 41 9 7220-.

419 9220 w 100

MS ICIS

80- 07261306

20-

NL:

6.24E3

LU LU

mlz= 421 7190-.

421 9190

MS ICIS

80: 07261306

1.36E2 mlz= 479.6165- 479.8165

1 07606 i20

Vol. 2 of 5 p. 783

RI: 42.08-4850 SM: 5G

CD

0) co a)

Co

C n

Co a) co

(N

C N-

(-)c'4 (N 10 C) tOLO

0) 0)

IC)

CD

CD

N.

0)

(N N-

7/26/2013 1:39:19 PM 53720-85-10 20130924

0) N-

(v)

IC)

IC)

N- 'flo)

N

(DCD (N

- C) IC) CD CO

CD cO '- C'J

CD

CD

CD

'-CD

C., (() '-CD (N

0)10 f lIC.)

jC)

- crCOr CN

45 46 47 Time (mm)

NL:

1.96E3 mlz= 423.6770- 423.8770 MS tCIS 07261306

NL:

189E3 m/z= 425.6740- 425.8740 MS lOIS 07261306

NL:

3.77E3 mlz= 435.7170- 435.9170

MS ICIS

07261306

NL:

3.53E3 mlz= 437.7140- 437.9140 MS lOIS

Vol. 2 of 5 p. 784

C:\XcaIibur\Data\Dioxn\07261 3\07261 306 ci)o8 C

C cti ci)

0cv.)

N Co Lt) N

7/26/2013 1:39:19 PM

0) 1)

53720-85-10 20130924

NL:

3.57E3 m/z= 441.6430- 441 .8430

MS ICIS

07261306

NL:

5.77E3 mlz= 469.6780- 469.8780

MS ICIS

07261306

(0 I Co

(V.)

Co N

C

6.38E3 mIz 471.6750- 471 .8750 MS lOIS 07261306

48.0 48.5 49.0 49.5 50.0 50.5 51.0 51.5

Vol. 2 of 5 p. 785

C :\Xcalibur\Data\Dioxin\07261 3\07261 306 7/26/2013 1:39:19 PM 53720-85-10 20130924

RT: 47.73 - 51.37 SM: 5G

NL:

1.18E4 mlz= 457.6380-

1oo- 457 8380

MS ICIS

07261306

80-i

60-

20-1

NL:

1.34E4

L() mlz= 459.6350-

459.835

MS ICISH 07261306

o 80

60-n

CL) 40.2

0 NL:

5.77E3 aD LU m/z=(N

469.6780- 69 8780

100- 4 .

MS ICIS

07261306

80-

-1

20-

0 NL:

6.38E3 co mlz=(N 471,6750- 471.8750 lOOj f' MS CIS\ 07261306

48.0 48.5 49.0 49.5 50.0 50.5 51.0

Vol. 2 of 5 p. 786

C:\Xcalibur\Data\Dioxjn\0726 1 3\07261 306

RT: 20.00 - 53,00

51 28724.81 25.33 368100 2017 . ,. , 27.10

- 459 529 625

419 29.22 30.77 32.89 63733.16 80128.33 A 36.79 a)

C ci)

7/26/2013 1:39:19 PM 53720-85-10 20130924

NL:

7.17E4 mlz=

304.48 1 80- 305.48180

MS

07261306

NL:

1.74E5 m/z= 330.47869- 331 .47869

MS

07261306

458 623 635 403 29.19 32.85 33.12 810 f

37.09 829

27.98 37.41 1054 1088 \J 41.76

NL:

9.36E4 m/z= 380.47550- 381 .47550

MS

07261306

1192 1384

43.61 46.90

43.13 / 1M.Y\ I

NL:

4.83E4 m/z= 392.47550- 393.47550

MS

07261306

1598 NL:

1400 ?2642 51.01 5.88E4

47.30 '

1392 t/1430.47231- 431 .4723 1

47.15 MS

07261306

20 25 30 35 40 45 50

Vol. 2 of 5 p. 787

Vol. 2 of 5 p. 788 b

N a m e

E a t r i x

S a m p l e

R e c e i p t

D a t e

E x t

D a t e

A n a l y s i s

D a t e

E x t r a c t

V o l u m e p L

I n j e c t i o n

V o l u m e p L

D i l u t i o n F a c t o r

C o n c e n t r a t i o n

U n i t s

T C D D l P e C D D l H x C D D

H x C D D

H x C D D l H p C D D

O C D D

T C D F l P e C D F

P e C D F

N x C D F l N x C D F

H x C D F

N x C D F

N p C D F l N p C D F

OC

D F

T o t a l

T E Q

S e d i m e n t s

T i m e

1 1 p g g d r y

P C D D

P C D F

A N A L Y S I S

D A T A

S H E E T

L a b

S a m p l e

I D

S a m p l e

W t V o l

I n i t i a l

C a l i b r a t i o n

D a t e

I n s t r u m e n t

I D

G C

C o l u m n

I D

S a m p l e

D a t a

F i l e n a m e

B l a n k

D a t a

F i l e n a m e

C a l

V e r

D a t a

F i l e n a m e

C o n c e n t r a t i o n

U n i t s

C O N C

D E T E C T I O N

F O U N D

L I M I T

I O N

R A T I O N n d u n i t s gi n

D F S m

Z B p g

P a g e o f

S P I K E

C O N C

T E Q

L A B E L E D

C O M P O U N D S

C O N C

F O U N D

R

I O N

R A T I O l C T C D D l C l P e C D D

C l N x C D D l C l N x C D D l C l N p C D D l C O C D D l C T C D F

C l P e C D F l C P e C D F l C l N x C D F l C l N x C D F

C l N x C D F n d

C N x C D F l C l N p C D F l C l H p C D F

C L E A N U P

S T A N D A R D

C T C D D

Vol. 2 of 5 p. 789 g e o f

F i l e n a m e:

A c q u i r e d

P r o c e s s e d

A n a l y t e

N O

M A P P I N G

C a l

D I C A L

R e s u l t s

S a m p l e t e x t l l

C o m m e n t s

T y p

N a m e

Q M

A r e a

R M

A r e a

P A

R T

C o n c

T o x

D L

N e c ri nk T C D F y ri nk P e C D F y ri nk P e C D F y ri nk l H x C D F y ri nk l H x C D F y ri nk H x C D F y ri nk l H x C D F n n d n d ri nk l H p C D F y ri nk l H p C D F y ri nk

O C D F y ri nk

T C D D y ri nk l P e C D D y ri nk

H x C D D y ri nk l H x C D D y ri nk l N x C D D y ri nk l N p C D D y ri nk

O C D D y

I S R T l C T C D F y

I S l C P e C D F y

I S l C P e C D F y

I S

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