Tab 1 - Mass Calibration (Mass Spectrometer [MS] Instrument Resolution)

Peak Resolution for the Perfluorokerosene (PFK) Reference Ion resolution must be > 10,000 resolving power
(e.g. 10% Valley)
Resolving Power = A/(A-B)
where:

SDG
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-33
G578-33
G578-33
G578-33
G578-33
G578-33
G578-34
G578-34
G578-34
G578-34
G578-34

A = mass/charge (e.g. [m/z] ration signal {380.97604})

B = peak width of ion at 5% of maximum signal (e.g. 380.93795)

Experiment: Function: ppm Volts

File:
Date
EXP_DB5MS
1
200 0.0983 A30JUN09A_L 30-Jun-2009
EXP_DB5MS
2
200 0.0983 A30JUN09A_L 30-Jun-2009
EXP_DB5MS
3
200 0.0985 A30JUN09A_L 30-Jun-2009
EXP_DB5MS
1
200 0.0564 A30JUN09A
Res_Check
EXP_DB5MS
2
200 0.0627 A30JUN09A
Res_Check
EXP_DB5MS
3
200 0.0577 A30JUN09A
Res_Check
EXP_DB5MS
1
200 0.1150 A02JUL09A_L 2-Jul-2009
EXP_DB5MS
1
200 0.0801 A06JUL09C_L 6-Jul-2009
EXP_DB5MS
2
200 0.0800 A06JUL09C_L 6-Jul-2009
EXP_DB5MS
3
200 0.0748 A06JUL09C_L 6-Jul-2009
EXP_DB5MS
1
200 0.0352 Res_Check
7-Jul-2009
EXP_DB5MS
2
200 0.0448 Res_Check
7-Jul-2009
EXP_DB5MS
3
200 0.0440 Res_Check
7-Jul-2009
EXP_DB5MS
1
200 0.0630 A08JUL09B_L 8-Jul-2009
EXP_DB5MS
2
200 0.0756 A08JUL09B_L 8-Jul-2009
EXP_DB5MS
3
200 0.0764 A08JUL09B_L 8-Jul-2009
EXP_DB5MS
1
200 0.0702 A08JUL09B_L Res_Check
EXP_DB5MS
2
200 0.0733 A08JUL09B_L Res_Check
EXP_DB5MS
3
200 0.0698 A08JUL09B_L Res_Check
EXP_DB5MS
1
200 0.0419 A09JUL09A_3 10-Jul-2009
EXP_DB5MS
2
200 0.0493 Res_Check 10-Jul-2009
EXP_DB5MS
3
200 0.0455 Res_Check 10-Jul-2009
EXP_DB5MS
1
200 0.0301 Res_Check 11-Jul-2009
EXP_DB5MS
2
200 0.0410 Res_Check 11-Jul-2009

Ref.
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK

Time
16:42
16:42
16:42
4:48
4:49
4:50
13:17
15:49
15:49
15:49
3:57
3:58
3:59
15:44
15:44
15:44
3:51
3:52
3:53
22:01
22:02
22:03
9:22
9:23

A
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604

B
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795

Resolving
Power
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632

Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass

Tab 1 - Mass Calibration (Mass Spectrometer [MS] Instrument Resolution)

Peak Resolution for the Perfluorokerosene (PFK) Reference Ion resolution must be > 10,000 resolving power
(e.g. 10% Valley)
Resolving Power = A/(A-B)
where:

SDG
G578-34
G578-35
G578-35
G578-35
G578-35
G578-35
G578-35
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36

A = mass/charge (e.g. [m/z] ration signal {380.97604})

B = peak width of ion at 5% of maximum signal (e.g. 380.93795)

Experiment: Function: ppm Volts

File:
Date
EXP_DB5MS
3
200 0.0470 Res_Check 11-Jul-2009
EXP_DB5MS
1
200 0.0508 A09JUL09A_L 9-Jul-2009
EXP_DB5MS
2
200 0.0617 A09JUL09A_L 9-Jul-2009
EXP_DB5MS
3
200 0.0577 A09JUL09A_L 9-Jul-2009
EXP_DB5MS
1
200 0.0466 Res_Check 10-Jul-2009
EXP_DB5MS
2
200 0.0529 Res_Check 10-Jul-2009
EXP_DB5MS
3
200 0.2410 Res_Check 10-Jul-2009
EXP_DB5MS
1
200 0.0695 A28JUL09A_L 28-Jul-2009
EXP_DB5MS
2
200 0.0944 A28JUL09A_L 28-Jul-2009
EXP_DB5MS
3
200 0.1007 A28JUL09A_L 28-Jul-2009
EXP_DB5MS
1
200 0.0767 Res_Check 29-Jul-2009
EXP_DB5MS
2
200 0.0915 Res_Check 29-Jul-2009
EXP_DB5MS
3
200 0.0884 Res_Check 29-Jul-2009

Ref.
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK
PFK

Time
9:24
17:39
17:39
17:40
5:45
5:46
5:47
14:42
14:42
14:43
2:50
2:51
2:52

A
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604
380.97604

B
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795
380.93795

Resolving
Power
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632
10,001.99632

Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass

Tab 2 - Spot Check Calculations

1

Where:
2

Analyte conc. [ug/L]= [Qis x (An +An )]/[(Ais +Ais ) x RRFn x W]

SDG
G578-29-1B
G578-29-1B
G578-29-1B
G578-29-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-36-1B
G578-36-1B
G578-36-1B
G578-36-1B

Calibrated
using Lab Std
#
Analyte
20
1,2,3,7,8,9-HxCDD (#5)
21
1,2,3,4,6,7,8-HpCDD (#6)
22
OCDD (#7)
23
2,3,7,8-TCDF (#8)
20
1,2,3,7,8,9-HxCDD (#5)
21
1,2,3,4,6,7,8-HpCDD (#6)
22
OCDD (#7)
23
2,3,7,8-TCDF (#8)
20
1,2,3,7,8,9-HxCDD (#5)
21
1,2,3,4,6,7,8-HpCDD (#6)
22
OCDD (#7)
23
2,3,7,8-TCDF (#8)
20
1,2,3,7,8,9-HxCDD (#5)
21
1,2,3,4,6,7,8-HpCDD (#6)
22
OCDD (#7)
23
2,3,7,8-TCDF (#8)
20
1,2,3,7,8,9-HxCDD (#5)
21
1,2,3,4,6,7,8-HpCDD (#6)
22
OCDD (#7)
23
2,3,7,8-TCDF (#8)

Qis = internal std. added (pg)

An and An2 = area of primary and secondary analyte ions
1
2
13
Ais and Ais = area of primary and secondary standard ions ( C)
RRFn = Relative Response Factor of analyte
W = Dry weight of sample extracted (grams)
1

Qis

An1

An2

2000
2000
4000
2000
2000
2000
4000
2000
2000
2000
4000
2000
2000
2000
4000
2000
2000
2000
4000
2000

4.59E+05
9.65E+06
3.31E+08
2.37E+05
3.49E+05
8.07E+06
3.84E+08
1.76E+05
2.77E+05
8.10E+06
5.24E+08
1.09E+05
3.75E+05
8.92E+06
5.72E+08
2.24E+05
1.00E+05
1.49E+06
6.28E+07
1.75E+05

3.67E+05
9.25E+06
3.70E+08
2.64E+05
2.84E+05
7.86E+06
4.30E+08
2.52E+05
2.40E+05
7.84E+06
5.87E+08
1.39E+05
3.04E+05
8.46E+06
6.40E+08
2.75E+05
7.81E+04
1.46E+06
7.05E+07
2.31E+05

Wt.
before
drying
%
(g)
solids
11.48
11.48
11.48
11.48
10.54
10.54
10.54
10.54
11.66
11.66
11.66
11.66
11.72
11.72
11.72
11.72
10.14
10.14
10.14
10.14

81.2
81.2
81.2
81.2
85.1
85.1
85.1
85.1
83.8
83.8
83.8
83.8
88.4
88.4
88.4
88.4
67.6
67.6
67.6
67.6

Ais1

Ais2

RRFn

SGS
Lab

9.32
9.32
9.32
9.32
8.97
8.97
8.97
8.97
9.77
9.77
9.77
9.77
10.36
10.36
10.36
10.36
6.85
6.85
6.85
6.85

4.12E+07
3.06E+07
4.67E+07
5.82E+07
4.90E+07
3.25E+07
5.19E+07
7.61E+07
5.67E+07
3.75E+07
6.02E+07
5.06E+07
5.50E+07
3.94E+07
6.42E+07
8.41E+07
4.95E+07
3.44E+07
4.41E+07
7.57E+07

3.30E+07
2.90E+07
5.23E+07
7.36E+07
3.88E+07
3.08E+07
5.79E+07
9.56E+07
4.50E+07
3.53E+07
6.71E+07
6.40E+07
4.37E+07
3.72E+07
7.13E+07
1.06E+08
3.93E+07
3.29E+07
4.91E+07
9.57E+07

0.9649
1.0612
1.0643
1.0368
0.9649
1.0612
1.0643
1.0368
0.9649
1.0612
1.0643
1.0368
0.9649
1.0612
1.0643
1.0368
0.9649
1.0612
1.0643
1.0368

2.48
64.1
2860
EMPC
1.67
52.9
3110
0.538
1.08
42.2
3360
0.428
1.38
41.2
3240
0.488
0.607
12
783
0.668

Tab 2 - Spot Check Calculations

1

Where:
2

Analyte conc. [ug/L]= [Qis x (An +An )]/[(Ais +Ais ) x RRFn x W]

SDG

Calibrated
using Lab Std
#
Analyte

Qis

An1

Qis = internal std. added (pg)

An and An2 = area of primary and secondary analyte ions
1
2
13
Ais and Ais = area of primary and secondary standard ions ( C)
RRFn = Relative Response Factor of analyte
W = Dry weight of sample extracted (grams)
1

An2

Wt.
before
drying
%
(g)
solids

Ais1

Ais2

RRFn

Note: per Method 8290, if a 2,3,7,8-TCDF isomer is detected on the DB-5

column, it must be confirmed using a DB-225 column; the result must be
reported from the DB-225 column (this relates to DB-5 isomer co-elution
issues)
G578-29-1B & G578-2C - the 2,3,7,8-TCDF isomer result was
flagged as EMPC with no second column confirmation
G578-30-1B and -2B / G578-33-1B and -2B / G578-34-1B and -2B /
G578-35-2B / G578-36-1B, -2B, -3B, -4B, -5B the 2,3,7,8-TCDF
isomer had positive hit results but there was no confirmation on the
DB-255 column reported.
Note: per SGS lab "DB-225 confirmation only used for
2,3,7,8-TCDF if the concentration or EMPC value is 1
pg/g for a 10 gram dry wt. sample"

SGS
Lab

Analyte
conc.
[ug/L]
Shaw
2.475
64.114
2855
0.787
1.666
52.878
3106
0.536
1.078
42.233
3357
0.427
1.376
41.274
3245
0.489
0.606
12.052
784
0.667

Analyte
conc.
[ug/L]
Shaw

Tab 3 - ION PAIR CHECK - Selected Ion Current Profile (SICP)

SDG
G578-29-1B
G578-29-1B
G578-29-1B
G578-30-1B
G578-30-1B
G578-30-1B
G578-30-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-33-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-34-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-35-1B
G578-36-1B
G578-36-1B
G578-36-1B
G578-36-1B
G578-36-1B
G578-36-1B

File
A07OCT08A
A07OCT08A
A07OCT08A
A06JUL09C
A06JUL09C
A06JUL09C
A06JUL09C
A09JUL09A
A09JUL09A
A09JUL09A
A09JUL09A
A09JUL09A
A09JUL09A
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A09JUL09A_5
A28JUL09A
A28JUL09A
A28JUL09A
A28JUL09A
A28JUL09A
A28JUL09A

Acq. Date
7-Oct-08
7-Oct-08
7-Oct-08
6-Jul-09
6-Jul-09
6-Jul-09
6-Jul-09
9-Oct-08
9-Oct-08
9-Oct-08
9-Oct-08
9-Oct-08
9-Oct-08
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
11-Jul-09
28-Jul-09
28-Jul-09
28-Jul-09
28-Jul-09
28-Jul-09
28-Jul-09

Time
17.23
17.23
17.23
16.41.32
16.41.32
16.41.32
16.41.32
17.59.38
17.59.38
17.59.38
17.59.38
17.59.38
17.59.38
10.15.38
10.15.38
10.15.38
10.15.38
10.15.38
10.15.38
10.15.38
10.15.38
11.52.17
11.52.17
11.52.17
11.52.17
11.52.17
11.52.17
11.52.17
11.52.17
17.58.11
17.58.11
17.58.11
17.58.11
17.58.11
17.58.11

Sample ID
3
3
3
2
2
2
2
10
10
10
10
10
10
2
2
2
2
2
2
2
2
4
4
4
4
4
4
4
4

Descriptor:
Analyte:
Ion ID:
Accurate Mass/Charge [m/z] Ratio:
Time (min/sec):

TCDD

TCDD

TCDD (S)

TCDD (S)

HxCDPE

PFK

PeCDD

PeCDD

PeCDD (S)

PeCDD (S)

M+2

M+2

M+2

319.8965

321.8936

331.9368

333.9338

327.8847

375.8364

31.39

31.39

31.37

31.37

29.41

29.41

29.40

29.40

28.54

28.54

28.53

28.53

29.39

29.39

LOCK
354.9792

M+2

M+4

M+2

M+4

355.8546

357.8516

367.8949

369.8919

34.25

34.25

34.24

34.24

32.03

32.02

33.17

33.17

33.20

33.20

33.16

33.16

33.17

33.17

33.16

33.16

29.41

26.09

26.11

32.18

32.18

26.09

26.11

32.40

32.40

26.28

26.28

32.50

32.50

33.17

33.18

29.40

26.12

26.12

32.04

32.02

26.28

26.27

32.19

32.19

29.41

29.40

32.42

32.42

30.42

30.41

32.52

32.52

33.22

33.21

33.36

33.36

26.11

26.11

32.02

32.02

26.28

26.27

32.17

32.17

26.50

26.50

32.34

32.34

27.32

27.32

32.39

32.39

29.40

29.39

32.50

32.49

33.18

33.18

32.01

32.01

32.16

32.16

32.39

32.39

32.49

32.49

33.17

33.17

33.31

33.31

26.08

26.11
28.52

28.52

29.37

29.37

29.39

HpCDPE

PFK

HxCDD

HxCDD

M+2
409.7974

LOCK
354.9792

HxCDD (S) HxCDD (5)

OCDPE

PFK

HpCDD

HpCDD

HpCDD (S)

M+2

M+4

M+2

M+4

M+4

LOCK

M+2

M+4

M+2

389.8156

391.8127

401.8559

403.8529

445.7555

430.9728

423.7767

425.7737

435.8169

???

???

37.03

37.03

40.34

40.35

40.33

37.10

37.10

37.09

37.09

37.25

37.25

37.24

37.24

35.42

35.42

35.41

35.41

38.48

38.48

38.47

???

???

35.46

35.46

36.00

36.00

35.59

35.59

34.34

34.34

37.57

37.57

34.58

34.59

38.47

38.47

35.11

35.10

35.46

35.46

35.45

35.45

36.00

36.00

35.59

35.59

34.34

34.34

38.03

38.03

34.45

34.45

38.53

38.53

35.11

35.12

35.25

35.25

36.02

36.02

36.02

36.02

36.14

36.14

36.13

36.13

34.35

34.35

37.58

37.57

35.01

35.01

38.48

38.48

35.13

35.13
35.45

35.45

35.50

35.50

35.50

35.50

36.03

36.03

36.03

36.03

36.22

36.21

34.33

34.33

37.56

37.56

35.10

35.10

38.47

38.47

35.59

36.00

36.20

36.20

35.40

35.40

35.45

35.45

35.59

35.59

38.46

38.52

38.47

38.46

HpCDD (S)

NCDPE

PFK

OCDD

OCDD

DCDPE

PFK

TCDF

TCDF

M+4

M+4

LOCK

M+2

M+4

M+4

LOCK

M+2

437.8140

479.7165

430.9728

457.7377

459.7348

513.6775

442.9728

303.9016

305.8987

40.33

45.00

45.00

31.06

31.06

38.47

42.39

42.39

28.45

28.45

42.38

42.38

25.26

25.26

28.45

28.45

29.07

29.06

25.27

25.26

27.48

27.49

28.46

28.45

29.07

29.06

30.50

30.49

25.27

25.26

27.20

27.21

27.48

27.48

28.45

28.45

29.06

29.06

30.50

30.49

25.25

25.25

27.20

27.20

27.47

27.47

28.44

28.45

30.50

30.49

38.46

42.46

42.46

38.52

42.40

42.40

38.47

42.38
38.46

42.38

TCDF (S)

TCDF (S)

PeCDF

PeCDF

PeCDF (S)

PeCDF (S)

HxCDF

HxCDF

M+4

M+2

M+2

M+4

315.9419

317.9389

341.8567

339.8597

351.9000

353.8970

31.04

31.04

33.37

33.37

34.13

34.13

28.44

28.43

28.44

28.43

28.44

28.43

28.44

28.42

M+2

HxCDF (S) HxCDF (S)

4
HpCDF

M+4

M+2

M+2

373.8208

375.8178

383.8639

385.8610

407.7818

33.36

36.27

36.27

36.26

36.26

39.17

34.13

36.56

36.57

36.56

36.56

41.17

37.45

37.44

37.44

37.44

33.18

33.18

33.17

33.17

???

???

35.02

35.02

37.40

32.32

32.32

32.32

32.32

35.08

35.08

35.08

35.08

39.23

35.36

35.36

33.07

33.07

33.07

33.07

36.17

36.17

31.55

31.56

34.11

34.11

37.40

32.01

32.01

34.18

34.18

38.07

32.20

32.20

34.41

34.41

32.32

32.32

35.03

35.02

32.40

32.40

35.35

35.35

33.07

33.07

32.01

32.01

32.22

32.22

32.33

32.33

32.42

32.42

33.10

33.09

30.54

30.53

32.32

32.32

33.07

33.06

32.34

33.10

32.33

33.10

35.02

35.02

35.08

35.07

34.10

34.10

37.47

34.19

34.18

38.13

34.27

34.27

34.41

34.41

34.51

34.51

35.16

35.15

35.54

35.54

35.15

35.15

35.21

35.21

31.59

31.59

34.12

34.12

37.40

32.20

32.20

34.19

34.19

38.08

32.32

32.32

34.34

34.34

32.41

32.40

34.42

34.43

33.03

33.03

33.07

33.07

30.53

30.53

32.31

32.31

35.05
33.07

33.07
35.39

35.39

36.19

36.19

35.05

35.04

35.10

35.10

31.58

31.59

34.10

34.10

37.39

32.13

32.13

34.17

34.17

38.06

32.19

32.19

34.40

34.40

32.32

32.32

35.02

35.02

33.07

33.07

30.51

30.51

33.06

33.06
35.35

35.35

35.01

35.01

35.06

35.06

HpCDF

HpCDF (S)

HpCDF

OCDF

OCDF

OCDD (S) OCDD (S)

M+4

M+2

M+2

M+4

M+2

M+4

409.7788

417.8250

419.8220

441.7428

443.7399

469.7780

471.7750

39.17

39.16

39.16

44.59

44.59

41.17

41.17

41.17

45.19

45.18

44.59

44.59

37.40

37.39

37.39

42.54

42.54

42.38

42.38

39.23

39.22

39.22

42.38

42.38

37.40

37.39

37.39

42.37

42.37

39.22

39.22

42.37

42.37

37.46

37.46

42.45

42.45

42.47

42.47

42.45

42.45

39.27

39.27

43.01

43.01

37.39

37.39

42.41

42.41

42.39

42.39

42.54

42.54

42.39

42.39

42.37

42.37

38.06

37.46
38.13

37.40
38.08

39.22

37.39

37.38

42.38

42.40

42.53

42.53

39.22

37.38

38.06

42.36
42.53

39.22

39.21

42.53

Tab 4 - Estimated Detection Limit (EDL)

1
2
1
2
EDL [ug/L]= [(Hx +Hx ) x Qis x Df x 2.5]/[(His +His ) x RRFn x W]

Where:
Hx1 and Hx2 =
Qis =
Df =
Qrs =

Lab using a correction factor of 3 and not 2.5 - see SGS e-mail
Note: Shaw calc. correct for G578-30 1,2,3,7,8-PeCDD (#2) - see e-mail
Value of 3 used instead of 2.5 for consistency with SGS Lab Calculations

peak height of noise for primary and secondary analyte ions

internal std. added (pg)
Dilution factor
recovery std. added (pg)

His1 and His2 = peak height of noise for primary and secondary internal std. ions
RRFn = Relative Response Factor of analyte
W = Dry weight of sample extracted

SDG

Estimated Detection
Limit (EDL)

G578-29-1B
G578-30-1B
G578-30-1B
G578-33-1B
G578-33-1B
G578-34-1B
G578-34-1B
G578-35-1B
G578-35-1B
G578-36-1B
G578-36-1B

2,3,7,8-TCDD (#1)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
2,3,7,8-TCDD (#1)
1,2,3,7,8,9-HxCDF (#14)
2,3,7,8-TCDD (#1)
1,2,3,7,8,9-HxCDF (#14)
2,3,7,8-TCDD (#1)
1,2,3,7,8,9-HxCDF (#14)
2,3,7,8-TCDD (#1)
1,2,3,7,8,9-HxCDF (#14)

Hx1

Hx2

(see
note)

3.87E+03
4.38E+03
5.20E+03
3.70E+03
6.07E+03
4.86E+03
4.91E+03
5.13E+03
7.12E+03
4.28E+03
6.63E+03

4.93E+03
5.42E+03
5.54E+03
4.11E+03
4.64E+03
5.10E+03
5.24E+03
4.90E+03
7.00E+03
4.73E+03
6.51E+03

3
3
3
3
3
3
3
3
3
3
3

Qis Df
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000
2000

1
1
1
1
1
1
1
1
1
1
1

His1

His2

RRFn

7.66E+06
7.61E+06
1.90E+07
8.88E+06
1.47E+07
8.71E+06
1.30E+07
1.08E+07
1.60E+07
9.25E+06
1.32E+07

9.74E+06
9.57E+06
1.15E+07
1.13E+07
2.69E+07
1.10E+07
2.52E+07
1.38E+07
2.96E+07
1.18E+07
2.52E+07

1.0087
1.0087
1.0517
1.0087
0.9220
1.0087
0.9220
1.0087
0.9220
1.0087
0.9220

Wt.
before
drying
W (g)
(g)
% solids
9.32
9.90
9.90
8.97
8.97
9.77
9.77
10.36
10.36
6.85
6.85

11.48
11.50
11.50
10.54
10.54
11.66
11.66
11.72
11.72
10.14
10.14

81.2
86.1
86.1
85.1
85.1
83.8
83.8
88.4
88.4
67.6
67.6

SGS
Lab
0.323
0.342
0.505
0.257
0.558
0.316
0.512
0.235
0.482
0.372
0.729

SGS vs
Shaw %
Shaw (manual
diff
calculation) EDL Calc.
0.323
0.1
0.343
-0.2
0.203
59.8
0.257
0.1
0.187
66.5
0.308
2.7
0.177
65.4
0.234
0.4
0.194
59.6
0.371
0.2
0.325
55.4

Tab 5 - Estimated Maximum Possible Concentration (EMPC)

Where:
1
2
1
2
EMPC [ug/L]= [(Ax +Ax ) x Qis x Df]/[(Ais +Ais ) x RRFis x W]

Ax1 and Ax2 =

Qis =
1
Ais and Ais2 =
RRFis =
Qis =
W=

Note: SGS Lab incorrectly calculated EMPC for 1,2,3,7,8-PeCDF (see e-mail)

SDG
G578-29-1B
G578-30-1B
G578-33-1B
G578-33-1B
G578-34-1B
G578-34-1B
G578-35-1B
G578-35-1B
G578-36-1B
G578-36-1B

Analyte
1,2,3,7,8-PeCDD (#2)
1,2,3,4,6,7,8-HpCDF (#15)
1,2,3,7,8-PeCDF (#9)
2,3,4,6,7,8-HxCDF (#13)
1,2,3,7,8-PeCDF (#9)
2,3,4,6,7,8-HxCDF (#13)
1,2,3,7,8-PeCDF (#9)
1,2,3,7,8,9-HxCDF (#14)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)

Ax

2.66E+05
5.74E+04
7.71E+04
1.18E+05
5.01E+04
7.34E+04
9.52E+04
4.12E+04
3.52E+04
9.08E+04

Ax

1.39E+05
4.42E+04
6.20E+04
1.12E+05
4.57E+04
4.79E+04
6.09E+04
2.86E+04
3.03E+04
7.42E+04

Qis (pg) Df
2000
1
2000
1
2000
1
2000
1
2000
1
2000
1
2000
1
2000
1
2000
1
2000
1

Ais

Ais

RRFn

4.73E+07
2.06E+07
9.12E+07
3.90E+07
8.93E+07
3.96E+07
1.10E+08
4.37E+07
8.34E+07
8.34E+07

2.97E+07
4.67E+07
5.75E+07
7.38E+07
5.62E+07
7.54E+07
6.99E+07
8.22E+07
5.21E+07
5.21E+07

1.0517
1.3752
0.9873
1.0650
0.9873
1.0650
0.9873
0.9220
0.9873
1.0154

area of primary and secondary internal standard ions

recovery std. added (pg)
area of primary and secondary recovery standard ions
Relative Response Factor of Internal Std.
internal std. added (pg)
Dry weight of sample extracted
SGS vs

Wt. before
drying (g) % solids W (g)
11.48
11.50
10.54
10.54
11.66
11.66
11.72
11.72
10.14
10.14

81.20
86.10
85.10
85.10
83.8
83.8
88.4
88.4
67.6
67.6

9.32
9.90
8.97
8.97
9.77
9.77
10.36
10.36
6.85
6.85

SGS
Lab
1.080
0.222
0.212
0.426
0.137
0.203
0.596
0.116
0.143
0.350

Shaw %
diff
Calc.
EMPC [ug/L]
1.073
-0.7
0.222
-0.1
0.211
-0.3
0.427
0.2
0.137
-0.4
0.203
-0.1
0.170
-251.3
0.116
0.1
0.143
-0.1
0.350
0.0

Tab 6 - Internal Standard % Recoveries

Internal Std. % Recovery (%Ris)= [(Ais +AiS ) x Qrs x 100]/[(Aris +Ars ) x RRFis x Qis]
1
2
Ais and Ais =
Where:
Qrs =
1
Ars and Ars2 =
RRFis =
Qis =

SDG

Ais (Ion 1)

Ais (Ion 2)

G578-29-1B

13

4.19E+07

5.30E+07

2000

G578-29-1B

13

4.73E+07

2.97E+07

2000

G578-29-1B

13

4.12E+07

3.39E+07

G578-29-1B
G578-29-1B

13

C 1,2,3,4,6,7,8-HpCDD (#21)
13
C OCDD (#22)

3.06E+07
4.67E+07

2.90E+07
5.23E+07

G578-30-1B

13

4.09E+07

G578-30-1B

13

4.87E+07

G578-30-1B

13

G578-30-1B
G578-30-1B

13

C 1,2,3,4,6,7,8-HpCDD (#21)
13
C OCDD (#22)

G578-33-1B

SGS (lab
Qis(pg) calculation)

% Ris (Shaw
manual calc.)

Ars (Ion 2)

RRFis

4.53E+07

5.72E+07

1.1153

2000

83.0

83.0

4.53E+07

5.72E+07

0.8155

2000

92.1

92.1

2000

4.76E+07

3.79E+07

1.0442

2000

83.1

84.1

2000
2000

4.76E+07
4.76E+07

3.79E+07
3.79E+07

0.7878
0.6269

2000
4000

88.5
92.2

88.5
92.4

5.19E+07

2000

4.66E+07

5.92E+07

1.1153

2000

78.6

78.6

3.01E+07

2000

4.66E+07

5.92E+07

0.8155

2000

91.3

91.3

4.59E+07

3.65E+07

2000

4.93E+07

3.97E+07

1.0442

2000

88.7

88.7

3.06E+07
4.43E+07

2.92E+07
4.96E+07

2000
2000

4.93E+07
4.93E+07

3.97E+07
3.97E+07

0.7878
0.6269

2000
4000

85.4
84.1

85.3
84.1

13

4.65E+07

5.90E+07

2000

5.39E+07

6.80E+07

1.1153

2000

76.6

77.6

G578-33-1B

13

5.50E+07

3.48E+07

2000

5.39E+07

6.80E+07

0.8155

2000

90.4

90.3

G578-33-1B

13

4.90E+07

3.88E+07

2000

5.20E+07

4.14E+07

1.0442

2000

90.1

90.0

G578-33-1B
G578-33-1B

13

C 1,2,3,4,6,7,8-HpCDD (#21)
13
C OCDD (#22)

3.25E+07
5.19E+07

3.08E+07
5.79E+07

2000
2000

5.20E+07
5.20E+07

4.14E+07
4.14E+07

0.7878
0.6269

2000
4000

86.1
93.7

86.0
93.8

G578-34-1B

13

5.02E+07

6.38E+07

2000

6.51E+07

8.21E+07

1.1153

2000

69.5

69.4

G578-34-1B

13

5.12E+07

3.24E+07

2000

6.51E+07

8.21E+07

0.8155

2000

69.6

69.6

G578-34-1B

13

5.67E+07

4.50E+07

2000

6.04E+07

4.82E+07

1.0442

2000

89.6

89.7

G578-34-1B
G578-34-1B

13

3.75E+07
6.02E+07

3.53E+07
6.71E+07

2000
2000

6.04E+07
6.04E+07

4.82E+07
4.82E+07

0.7878
0.6269

2000
4000

85.1
93.4

85.1
93.5

G578-35-1B

13

5.95E+07

7.58E+07

2000

6.31E+07

7.96E+07

1.1153

2000

85.0

85.0

G578-35-1B

13

6.78E+07

4.28E+07

2000

6.31E+07

7.96E+07

0.8155

2000

95.0

95.0

G578-35-1B

13

5.50E+07

4.37E+07

2000

5.93E+07

4.73E+07

1.0442

2000

88.6

88.7

G578-35-1B
G578-35-1B

13

3.94E+07
6.42E+07

3.72E+07
7.13E+07

2000
2000

5.93E+07
5.93E+07

4.73E+07
4.73E+07

0.7878
0.6269

2000
4000

91.2
101.0

91.2
101.4

G578-36-1B

13

4.58E+07

5.79E+07

2000

4.48E+07

5.65E+07

1.1153

2000

91.8

91.8

Analyte
C 2,3,7,8-TCDD (#18)
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)

C 2,3,7,8-TCDD (#18)
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)

C 2,3,7,8-TCDD (#18)
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)

C 2,3,7,8-TCDD (#18)
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)
C 1,2,3,4,6,7,8-HpCDD (#21)
C OCDD (#22)

13

C 2,3,7,8-TCDD (#18)
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)
C 1,2,3,4,6,7,8-HpCDD (#21)
C OCDD (#22)

13

C 2,3,7,8-TCDD (#18)

Qrs(pg) Ars (Ion 1)

area of primary and secondary internal standard ions

recovery std. added (pg)
area of primary and secondary recovery standard ions
Relative Response Factor of Internal Std.
internal std. added (pg)

Tab 6 - Internal Standard % Recoveries

Internal Std. % Recovery (%Ris)= [(Ais +AiS ) x Qrs x 100]/[(Aris +Ars ) x RRFis x Qis]
1
2
Ais and Ais =
Where:
Qrs =
1
Ars and Ars2 =
RRFis =
Qis =

SDG

Ais (Ion 1)

Ais (Ion 2)

G578-36-1B

13

5.12E+07

3.25E+07

2000

G578-36-1B

13

4.95E+07

3.93E+07

2000

G578-36-1B

13

3.44E+07

3.29E+07

G578-36-1B

13

4.41E+07

4.91E+07

G578-36-1B

13

7.57E+07

9.57E+07

Analyte
C 1,2,3,7,8-PeCDD (#19)
C 1,2,3,6,7,8-HxCDD (#20)
C 1,2,3,4,6,7,8-HpCDD (#21)
C OCDD (#22)
C 2,3,7,8-TCDF (#23)

Qrs(pg) Ars (Ion 1)

area of primary and secondary internal standard ions

recovery std. added (pg)
area of primary and secondary recovery standard ions
Relative Response Factor of Internal Std.
internal std. added (pg)
SGS (lab
Qis(pg) calculation)

% Ris (Shaw
manual calc.)

Ars (Ion 2)

RRFis

4.48E+07

5.65E+07

0.8155

2000

101.0

101.3

4.91E+07

3.91E+07

1.0442

2000

96.4

96.4

2000

4.91E+07

3.91E+07

0.7878

2000

96.8

96.9

2000

4.91E+07

3.91E+07

0.6269

4000

84.3

84.3

2000

4.48E+07

5.65E+07

1.6529

2000

102.0

102.4

Tab 7 - First & Last Eluters (Spot Check)

First & Last Isomer Eluters for each homologue of PCDD and PCDF
SDG

Lab Sample ID

Comment

G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29

RETCON S30-144H

Ical

RETCON S32-184L

RETCON S32-184L

RETCON S32-184L

Instrument ID File Name

WG17173

a07oct08a

a30jun09a

a30jun09a

a02jul09

Sample
Date
Time
Date
Time
No.
Acquired Acquired Processed Processed Name
1

15

7-Oct-08

15.46.35

30-Jun-08 16.43.56

1-Jul-09

2-Jul-09

04.00.27

13.24.00

8-Oct-08

1-Jul-09

1-Jul-09

3-Jul-09

08.19.56 TCDD
PeCDD
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
HpCDF
OCDF
07.02.23 TCDD
PeCDD
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
HpCDF
OCDF
07.02.30 TCDD
PeCDD
HxCDD
HpCDD
OCDD
TCDF
PeCDF
HxCDF
HpCDF
OCDF
09.30.03 TCDD
PeCDD
HxCDD
HpCDD
OCDD

First Eluter Last Eluter

(RT)
RT
28.35
33.02
35.48
39.37
44.60
26.52
32.11
35.22
39.16
45.19
26.12
32.02
34.34
37.57
42.39
24.30
30.51
34.11
37.40
42.53
26.11
32.01
34.34
37.57
42.38
24.30
30.51
34.11
37.39
42.53
26.13
32.02
34.35
37.59
42.41

32.08
34.40
37.24
40.35
32.12
34.52
37.45
41.17
30.43
33.32
35.60
38.48
30.50
33.41
36.17
39.23
30.43
33.32
35.59
38.47
30.50
33.41
36.17
39.22
30.44
33.32
36.01
38.49

Tab 7 - First & Last Eluters (Spot Check)

First & Last Isomer Eluters for each homologue of PCDD and PCDF
SDG
G578-29
G578-29
G578-29
G578-29
G578-29

Lab Sample ID

Comment

Instrument ID File Name

Sample
Date
Time
Date
Time
No.
Acquired Acquired Processed Processed Name
TCDF
PeCDF
HxCDF
HpCDF
OCDF

First Eluter Last Eluter

(RT)
RT
24.31
30.52
34.12
37.41
42.55

30.51
33.42
36.18
39.24

Tab 8 - Total Dioxin/Furan Calculations

SDG

Note: see attached e-mail from SGS Laboratory regarding Totals Calculations
Status
Peaks
Kept
EDL (SDG (SDG
(SDG Shaw
Name (Totals) (Y/N) RT
Conc.
Lab)
Lab)
SDG Lab Lab) (manual)

G578-29-1B

Tetra-Dioxins

26.12
26.28
26.51
27.31
27.46
28.00
28.10
28.34
28.57
29.42
30.01
30.43

0.344
0.213
0.139
0.090
0.291
0.143
0.181
0.318
0.161
0.106
0.118
0.089

0.344 0.1361
0.213 0.1361
0.139 0.1361
0.1361
0.291 0.1361
0.1361
0.181 0.1361
0.318 0.1361
0.161 0.1361
0.1504
0.118 0.1361
0.1361

ok
ok
ok
S2N
ok
S2N
ok
ok
ok
S2N
ok
S2N

2378-TCDD
S2N (Manual Correction)
0.1504
1.7650
1.7650

G578-29-1B

Hepta-Furans

37.42
37.58
38.07
39.24

4.653
0.185
7.056
0.254

0.0994
0.1116
0.1116
0.1274

Tetra-Furans

y
y
y
n
y
n
y
n

24.30
24.55
25.27
25.46
26.06
26.30
26.43
27.12

0.192
0.145
0.586
0.280
0.261
0.303
0.091
0.168

0.192 0.1498
0.145 0.1498
0.586 0.1498
0.1498
0.261 0.1498
0.1498
0.1498
0.1498

8
8

1.7650

ok
ok
ok
ok

ok
ok
ok
EMPC
ok
EMPC
S2N
EMPC

EDL (2378-TCDD)
Total EMPC Tetra-Dioxins
Total Tetra-Dioxins
123678-HpCDF
1234789-HpCDF

0.1274
12.1480
12.1480
G578-29-1B

Comment

4
4

0.1274
12.1480
12.1480

EDL (123478-HpCDF)
Total EMPC Hepta-Furans
Total Hepta-Furans

Tab 8 - Total Dioxin/Furan Calculations

SDG

Note: see attached e-mail from SGS Laboratory regarding Totals Calculations
Status
Peaks
Kept
EDL (SDG (SDG
(SDG Shaw
Name (Totals) (Y/N) RT
Conc.
Lab)
Lab)
SDG Lab Lab) (manual)

2378-TCDF

y
y
n
n
n
n
n
y
n

27.22
27.49
28.04
28.16
28.31
28.39
28.46
29.07
30.52

0.417 0.417 0.1498

0.268 0.268 0.1498
0.091
0.1498
0.105
0.1498
0.187
0.1498
0.169
0.1498
0.366
0.1498
0.359 0.359 0.1498
0.198
0.1498

Comment

ok
ok
S2N
S2N
EMPC
EMPC
EMPC
ok
EMPC
0.1498
2.2280
3.8990

7
14

2.2280

EDL (2378-TCDF)
Total Tetra-Furans
Total EMPC Tetra-Furans

Tab 9 - Matrix Spike/Matrix Spike Duplicate %Recovery Recalculation

(e.g. Ongoing Precision Results [OGP] / Ongoing Precision Duplicate Results [OGPD])
Where: %R = percent recovery
MS/MSD %R = (Spike Recovered - Sample original conc.) x 100 / Spike Added

Spk rec. = Spike concentration recovered

Spk add = Spike concentration added
Orig. conc. = Original sample concentration

% RPD = ABS(MS-MSD) x 100 / Average % recovery

SDG
G578-29
G578-29
G578-29
G578-29
G578-30
G578-30
G578-30
G578-30
G578-33
G578-33
G578-33
G578-33
G578-34
G578-34
G578-34
G578-34
G578-35
G578-35
G578-35
G578-35
G578-36
G578-36
G578-36
G578-36

Analyte
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)

Sample
(pg/uL)
0.106
0.501
0.426
1.259
0.342
0.505
0.505
0.505
0.369
0.563
0.563
0.563
0.316
0.285
0.516
1.110
0.235
0.521
0.828
1.070
0.372
0.729
0.292
0.493

Spiked (amt.
added)
pg/uL

MS Recovery
(SGS Calc.)
pg/uL

10
50
50
50
10
50
50
50
10
50
50
50
10
50
50
50
10
50
50
50
10
50
50
50

10.2
48.8
50.7
48.0
9.9
46.1
45.7
44.3
11.0
49.0
50.4
48.6
10.3
48.7
48.2
49.7
10.3
48.7
48.2
49.7
10.4
47.7
45.5
49.7

MS %
Recovery MSD Recovery
(SGS
(SGS Calc.)
Calc.)
pg/uL
102
97.6
101
95.9
99.4
92.2
91.4
88.6
110
98
101
97.3
103
97.3
96.5
99.4
103
97.3
96.5
99.4
104
95.4
91
99.4

10.6
48.2
50.3
46.9
10.1
46.0
45.3
43.2
10.4
48.5
48.9
48.9
10.5
48.4
49.1
49.3
10.5
48.4
49.1
49.3
10.7
48.6
49.0
48.9

MSD %
Recovery MS % Recovery
(SGS Calc.) (Shaw manual)
106.0
96.4
101.0
93.8
101.0
92.0
90.5
86.5
104.0
97.0
97.8
97.8
105.0
96.8
98.2
98.6
105.0
98.6
98.2
98.6
107.0
97.2
98.0
97.8

100.8
96.6
100.6
93.4
96.0
91.2
90.4
87.6
106.3
96.9
99.7
96.1
99.8
96.8
95.4
97.2
100.7
96.4
94.7
97.3
100.3
93.9
90.4
98.4

MSD %
Recovery
(Shaw
manual)

% RPD
(Shaw
manual)

104.5
95.4
99.7
91.3
97.6
91.0
89.6
85.4
100.3
95.9
96.7
96.7
101.8
96.2
97.2
96.4
102.7
95.8
96.5
96.5
103.3
95.7
97.4
96.8

3.61
1.15
0.89
2.21
1.55
0.25
0.84
2.53
5.61
1.03
3.02
0.62
1.92
0.62
1.85
0.81
1.92
0.62
1.85
0.81
2.84
1.87
7.41
1.62

Tab 10 - Spot Check Relative Response Factor Calculations & Ion Ratios
(RRF Calculation for unlabeled PCDDs/PCDFs &
1

13

C-labeled Recovery Standard)

Response Factor (RRFn)= [(An +An ) x Qis]/[(Ais +Ais ) x Qn]

1
2
1
2
Ion Ratio (RRFis) = [(Ais +Ais ) x Qrs]/[(Ars +Ars ) x Qis]
1

Where: An and An = areas of the primary and secondary ions of interest

Ais1 and Ais2 = area of primary and secondary internal standard ions
Ars1 and Ars2 = area of primary and secondary recovery standard ions
13
rs = C 1,2,3,4-TCDD (#27)
is=
13
rs = C 1,2,3,7,8,9-HxCDD (#28)
is=
Qn = quantity of unlabeled PCDD/PCDF analyte injected (pg)
Qis = quantity of internal standard injected (pg)
Qn = quantity of recovery (e.g Injection) standard injected (pg)
SDG
G578-29-1B

Name
2,3,7,8-TCDD (#1)

1,2,3,7,8-PeCDD (#2)

13

C 1,2,3,7,8,9-PeCDD
13
C 1,2,3,6,7,8-HxCDD

RRFn#
RRFn (SDG Lab)
1
1.06
2
0.99
3
0.99
4
1.01
5
1.00
Mean
1.0087
%RSD
2.99
1
2
3
4
5
Mean
%RSD

RRFn (Shaw - manual)

1.0612
0.9902
0.9870
1.0052
1.0013
1.0090

1.06
1.04
1.06
1.05
1.06
1.0517
6.26

1.0595
1.0421
1.0544
1.0481
1.0558
1.0520

RRFis (SDG Lab)

0.7882
1.0656

RRFis (Shaw - manual)

0.7879
1.0665

13
13

C 1,2,3,7,8-PeCDD
C 1,2,3,6,7,8-HxCDD

An1
1.76E+05
1.26E+06
6.26E+06
2.68E+07
1.38E+08

An2
2.40E+05
1.58E+06
8.22E+06
3.46E+07
1.79E+08

Qis
100
100
100
100
100

Ais1
6.93E+07
6.37E+07
6.53E+07
6.81E+07
7.05E+07

Ais2
8.75E+07
7.97E+07
8.14E+07
8.46E+07
8.78E+07

An1
8.52E+05
6.65E+06
3.44E+07
1.45E+08
7.85E+08

An2
5.73E+05
4.25E+06
2.18E+07
9.25E+07
5.02E+08

Qis
100
100
100
100
100

Ais1
6.61E+07
6.41E+07
6.52E+07
6.95E+07
7.46E+07

Ais2
Qn
4.15E+07
1.25
4.05E+07
10.00
4.14E+07
50.00
4.38E+07 200.00
4.73E+07 1000.00

Qrs
100
100

Ars
Ars
5.99E+07 7.54E+07
5.79E+07 4.59E+07

Ais
6.52E+07
6.18E+07

Ais
4.14E+07
4.89E+07

Qn
0.25
2.00
10.00
40.00
200.00

Qis
100.00
100.00

Tab 11 - Initial Calibration Mean and %RSD Recalculation

RRFavg = average response factor
Where:
RRFaverage =

(RRF1 + RRF2 + RRF3 + RRFn)/ n

RRFn = response factor for n calibration std of initial calibration

n = number of standards used for initial calibration
%RSD = percent relative std deviation
SD = Std deviation of the RF's for a compound

% RSD = SD x 100 / RRFavg

* Note: per SGS Lab if [2,3,7,8-TCDF] < 1 pg/g DB225 2nd column confirmation not used (see e-mail)

SDG
G578-29
G578-29

Column
DB225
DB5

G578-29
G578-29
G578-29
G578-30
G578-33
G578-34
G578-35
G578-36

DB5
DB5
DB5
used ICAL
used ICAL
used ICAL
used ICAL
used ICAL

ANALYTE NAME
RRF1 RRF2 RRF3
* Not Used by SDG Laboratory
2,3,7,8-TCDD (#1)
1.06 0.99 0.99
13
C 2,3,7,8-TCDF (#23)
1.62 1.69 1.61
1,2,3,7,8-PeCDD (#2)
1.06 1.04 1.06
37
C14 2,3,7,8-TCDD (#29)
1.24 1.18 1.13
from G578-29
from G578-29
from G578-29
from G578-29
from G578-29

RRF4

RRF5

Shaw (manual
SDG (Lab)
calculation)
MEAN %RSD MEAN %RSD
SD

1.01

1.00

1.0087

2.99 1.0100 2.89

0.0292

1.63
1.05
1.16

1.70
1.06
1.24

1.6529
1.0517
1.1889

2.59 1.6500 2.54

0.73 1.0540 0.85
4.22 1.1900 4.12

0.0418
0.0089
0.0490

Tab 12 - Continuing Calibration Recalculation for Concentration of Unlabeled Compound

Where:
1
2
1
2
Cc = [(An +An ) x Qis]/[(Ais +Ais ) x RRFICAL]
%D= [(RRFICAL-RRFCCAL) x 100]/RRFICAL

An1 and An2 = areas of the primary and secondary ions of interest
Qis = the concentration of the internal standard
Ais1 and Ais2 = area of primary and secondary internal standard ions
RRFCCAL = the response of the analyte from Continuing Calibration
RRFICAL = the response of the analyte from Initial Calibration
Cc = concentration of the unlabeled compound in the extract
Ct = concentration of the actual spiked compound
%D = % Difference between RRFICAL & RRFCCAL

Analyte

G578-29
G578-29
G578-29
G578-30
G578-30
G578-30
G578-33
G578-33
G578-33
G578-34
G578-34
G578-34
G578-35
G578-35
G578-35
G578-36
G578-36
G578-36

2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF
2,3,7,8-TCDD
1,2,3,7,8-PeCDF

2,3,7,8-TCDF

An1 (Ion 1) An2 (Ion 1) Qis Ais1 (Ion 1) Ais2 (Ion 2) RRFCCAL RRFICAL
9.12E+06
5.79E+07
1.27E+07
1.05E+07
9.39E+07
1.61E+07
2.30E+07
1.97E+08
3.41E+07
1.69E+07
1.47E+08
2.46E+07
1.69E+07
1.47E+08
2.46E+07
3.75E+06
2.95E+07
5.64E+06

1.16E+07
3.74E+07
1.64E+07
1.33E+07
6.03E+07
2.04E+07
2.93E+07
1.25E+08
4.29E+07
2.18E+07
9.47E+07
3.15E+07
2.18E+07
9.47E+07
3.15E+07
4.73E+06
1.89E+07
7.18E+06

100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100

8.90E+07
1.14E+08
1.36E+08
9.59E+07
1.96E+08
1.56E+08
2.23E+08
4.02E+08
3.33E+08
1.70E+08
3.10E+08
2.50E+08
1.70E+08
3.10E+08
2.50E+08
3.57E+07
6.24E+07
5.75E+07

1.13E+08
7.25E+07
1.73E+08
1.21E+08
1.25E+08
1.94E+08
2.83E+08
2.52E+08
4.19E+08
2.16E+08
1.98E+08
3.13E+08
2.16E+08
1.98E+08
3.13E+08
4.52E+07
3.96E+07
7.12E+07

1.0289
1.021
0.9418
1.0989
0.9622
1.0425
1.0341
0.9834
1.0241
1.0042
0.9508
0.997
1.0042
0.9508
0.997
1.0485
0.9487
0.9959

1.0087
1.0517
1.0368
1.0087
1.0517
1.0368
1.0087
1.0517
1.0368
1.0087
1.0517
1.0368
1.0087
1.0517
1.0368
1.0087
1.0517
1.0368

Cc (SDG Ct (SDG
Lab)
Lab)

10.200
48.540
9.084
10.890
48.730
10.060
10.250
49.800
9.878
9.955
48.150
9.161
9.955
48.150
9.616
10.390
48.040
9.606

%D
(SDG
Lab)

10

2.00

50
10

-2.90
-9.20
-0.03
-6.20
-7.60
2.50
-0.40
-1.20
-0.40
-3.70
-3.80
-0.40
-3.70
-3.80
3.90
-3.90
-3.90

10

50
10
10

50
10
10

50
10
10

50
10
10

50
10

Cc
Cc (Shaw (Shaw
%D
manual) manual)
(Shaw
w/
w/
manual) RRFCCAL RRFICAL

2.0
-3.0
-10.1
8.2
-9.3
0.5
2.5
-6.9
-1.2
-0.4
-10.6
-4.0
-0.4
-10.6
-4.0
3.8
-10.9
-4.1

9.97
50.05
10.00
9.99
49.92
10.00
10.00
50.07
10.00
9.98
50.04
9.99
9.98
50.04
9.99
10.00
50.02
10.00

10.17
48.59
9.08
10.88
45.68
10.06
10.25
46.82
9.88
9.94
45.24
9.61
9.94
45.24
9.61
10.39
45.12
9.61

Tab 13 - Spot Check Continuing Calibration Recalculation for Concentration of Labeled Compound
Where: Cc = concentration of the unlabeled compound in the extract
Ct = True Concentration
1

An and An = areas of the primary and secondary ions of interest

Qis = the concentration of the internal standard
Ais1 and Ais2 = area of primary and secondary internal standard ions

Cc = [(An +An ) x Qis]/[(Ais +Ais ) x RRFIs]

%D= [(RRFICAL-RRFCCAL) x 100]/RRFICAL

RRFIs = the response from the internal standard

RRFICAL = the response of the analyte from Initial Calibration
RRFCCAL = the response of the analyte from Continuing Calibration
%D = % Difference between RRFICAL & RRFCCAL

SDG

CCAL Analyte

G578-29
G578-29

Initial
Final

37

G578-30
G578-30

Initial
Final

37

G578-33
G578-33

Initial
Final

37

G578-34
G578-34

Initial
Final

37

G578-35
G578-35

Initial
Final

37

G578-36
G578-36

Initial
Final

37

37

37

37

37

37

37

An1

An2

Qis

Ais1

Ais2

RRFIS

RRFICAL RRFCCAL

Cc (Shaw
manual)
Cc (SGS Ct (SGS
w/
Lab)
Lab)
RRFCCAL

%D
(SGS
Lab)

%D
(Shaw
manual)

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

2.10E+07
2.60E+07

100 8.90E+07 1.13E+08

100 1.09E+08 1.39E+08

1.1097
1.1036

1.1889 1.1592
1.1889 1.1406

9.750
9.594

10
10

9.37
9.50

-2.5
-4.1

2.5
4.1

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

2.20E+07
2.30E+07

100 9.41E+07 1.19E+08

100 9.59E+07 1.21E+08

1.1296
1.1253

1.1889 1.1801
1.1889 1.2077

9.926
10.160

10
10

9.14
9.42

-3.1
-2.1

0.7
-1.6

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

2.90E+07
5.20E+07

100 1.23E+08 1.56E+08

100 2.23E+08 2.83E+08

1.1154
1.1193

1.1889 1.1652
1.1889 1.1516

9.801
9.724

10
10

9.32
9.18

-1.1
-0.1

2.0
3.1

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

2.80E+07
3.90E+07

100 1.19E+08 1.51E+08

100 1.70E+08 2.16E+08

1.1231
1.1434

1.1889 1.1623
1.1889 1.1713

9.777
9.852

10
10

9.23
8.84

0.9
1.9

2.2
1.5

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

2.80E+07
3.90E+07

100 1.19E+08 1.51E+08

100 1.70E+08 2.16E+08

1.1231
1.1434

1.1889 1.1623
1.1889 1.1713

9.777
9.852

10
10

9.23
8.84

2.9
3.9

2.2
1.5

CL 2,3,7,8-TCDD
CL 2,3,7,8-TCDD

8.20E+06
8.30E+06

100 3.46E+07 4.37E+07

100 3.57E+07 4.52E+07

1.0771
1.0767

1.1889 1.1317
1.1889 1.1058

9.519
9.301

10
10

9.72
9.53

4.9
5.9

4.8
7.0

Tab 14 - Recalculation of Percent Difference for the RRFs for the Continuing Calibration Values:
% Difference (%D) = (RRFCCAL - RRFICAL) x 100 / RRFCCAL
Where:

RRFICAL = Relative Response factor from the initial calibration

RRFCCAL = Relative Response factor from the continuing calibration

SDG

G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-29
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-30
G578-33
G578-33
G578-33
G578-33

Analyte

RRFCCAL

RRFICAL

(SDG lab)
%D

2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)

1.0058
1.0349
0.9240
0.9427

1.0087
1.0517
0.9489
0.9916
0.9649
1.0612
1.0643
1.0368
0.9873
1.0154
1.0087
1.0517
0.9489
0.9916
0.9649
1.0612
1.0643
1.0368
0.9873
1.0154
1.0087
1.0517
0.9489
0.9916

-0.3
-1.6
-2.6
-4.9
-2.3
-5.2
-3.6
-7.6
-6.2
-6.3
0.1
-3.9
-1.3
-4.6
-2.7
-1.7
-1.9
-7.4
-4.9
-1.1
2.5
-0.3
-1.7
-3.4

0.9430
1.0057
1.0255
0.9577
0.9262
0.9515
1.0093
1.0110
0.9361
0.9457
0.9386
1.0428
1.0437
0.9600
0.9391
1.0044
1.0341
1.0488
0.9328
0.9577

Shaw (manual)
%D
-0.3
-1.6
-2.6
-4.9
-2.3
-5.2
-3.6
-7.6
-6.2
-6.3
0.1
-3.9
-1.3
-4.6
-2.7
-1.7
-1.9
-7.4
-4.9
-1.1
2.5
-0.3
-1.7
-3.4

Tab 14 - Recalculation of Percent Difference for the RRFs for the Continuing Calibration Values:
% Difference (%D) = (RRFCCAL - RRFICAL) x 100 / RRFCCAL
Where:

RRFICAL = Relative Response factor from the initial calibration

RRFCCAL = Relative Response factor from the continuing calibration

SDG

G578-33
G578-33
G578-33
G578-33
G578-33
G578-33
G578-34
G578-34
G578-34
G578-34
G578-34
G578-34
G578-34
G578-34
G578-34
G578-34
G578-35
G578-35
G578-35
G578-35
G578-35
G578-35
G578-35
G578-35

Analyte

RRFCCAL

RRFICAL

(SDG lab)
%D

1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)

0.9282
1.0534
1.0593
1.0241
0.9834
0.9766
1.0195
1.0445
0.9430
1.0022
0.9935
1.0519
1.0563
1.0030
0.9689
1.0235
1.0195
1.0445
0.9430
1.0022
0.9935
1.0519
1.0563
1.0030

0.9649
1.0612
1.0643
1.0368
0.9873
1.0154
1.0087
1.0517
0.9489
0.9916
0.9649
1.0612
1.0643
1.0368
0.9873
1.0154
1.0087
1.0517
0.9489
0.9916
0.9649
1.0612
1.0643
1.0368

-3.8
-0.7
-0.5
-1.2
-0.4
-3.8
1.1
-0.7
-0.6
1.1
3.0
-0.9
-0.7
-3.3
-1.9
0.8
1.1
-0.7
-0.6
1.1
3.0
-0.9
-0.7
-3.3

Shaw (manual)
%D
-3.8
-0.7
-0.5
-1.2
-0.4
-3.8
1.1
-0.7
-0.6
1.1
3.0
-0.9
-0.8
-3.3
-1.9
0.8
1.1
-0.7
-0.6
1.1
3.0
-0.9
-0.8
-3.3

Tab 14 - Recalculation of Percent Difference for the RRFs for the Continuing Calibration Values:
% Difference (%D) = (RRFCCAL - RRFICAL) x 100 / RRFCCAL
Where:

RRFICAL = Relative Response factor from the initial calibration

RRFCCAL = Relative Response factor from the continuing calibration

SDG

G578-35
G578-35
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36
G578-36

Analyte

RRFCCAL

RRFICAL

(SDG lab)
%D

1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)
2,3,7,8-TCDD (#1)
1,2,3,7,8-PeCDD (#2)
1,2,3,4,7,8-HxCDD (#3)
1,2,3,6,7,8-HxCDD (#4)
1,2,3,7,8,9-HxCDD (#5)
1,2,3,4,6,7,8-HpCDD (#6)
OCDD (#7)
2,3,7,8-TCDF (#8)
1,2,3,7,8-PeCDF (#9)
2,3,4,7,8-PeCDF (#10)

0.9689
1.0235
1.0181
1.0174
0.9225
0.9465
0.9111
1.0211
1.0300
0.9769
0.9419
0.9780

0.9873
1.0154
1.0087
1.0517
0.9489
0.9916
0.9649
1.0612
1.0643
1.0368
0.9873
1.0154

-1.9
0.8
0.9
-3.3
-2.8
-4.5
-5.6
-3.8
-3.2
-5.8
-4.6
-3.7

Shaw (manual)
%D
-1.9
0.8
0.9
-3.3
-2.8
-4.5
-5.6
-3.8
-3.2
-5.8
-4.6
-3.7

Tab 15 - Toxic Equivalency Factors (TEF) "Spot Check"

SDG

SEM

Lab ID

Sampled

Extracted

Analyzed

G578-29-1B
G578-30-1B
G578-30-2B
G578-33-1B
G578-33-2B
G578-33-3B
G578-33-4B
G578-34-1B
G578-34-2B
G578-35-1B
G578-35-2C
G578-36-1B
G578-36-2B
G578-36-3B
G578-36-4B
G578-36-5B

SEM-015
SEM-017
SEM-017
SEM-029
SEM-029
SEM-029
SEM-029
SEM-035
SEM-035
SEM-031
SEM-031
SEM-034
SEM-034
SEM-034
SEM-034
SEM-034

9794676006
9794971005
9794971005
9796518001
9796518003
9796518004
9796518005
9797431001
9797431002
9796885001
9796885002
9797191001
9797191004
9797191005
9797191006
9797191007

6/15/2009
6/16/2009
6/16/2009
6/25/2009
6/25/2009
6/25/2009
6/25/2009
7/1/2009
7/1/2009
6/29/2009
6/29/2009
6/30/2009
6/30/2009
6/30/2009
6/30/2009
6/30/2009

6/29/2009
7/5/2009
7/5/2009
7/7/2009
7/7/2009
7/7/2009
7/7/2009
7/8/2009
7/8/2009
7/8/2009
7/8/2009
7/23/2009
7/23/2009
7/23/2009
7/23/2009
7/23/2009

7/2/2009
7/7/2009
7/7/2009
7/10/2009
7/10/2009
7/10/2009
7/10/2009
7/11/2009
7/11/2009
7/11/2009
7/11/2009
7/28/2009
7/28/2009
7/28/2009
7/28/2009
7/28/2009

Spot Check: G578-29-1B

Where: if [conc] = ND, then for ND=0.5 TEF WHO 2005 use [EDL] or [EMPCs] at for the ND=

2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD

TEF WHO 2005

Value
1
1
0.1
0.1
0.1
0.01
0.0003

2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF

0.1
0.03
0.3
0.1
0.1
0.1
0.1

ND = 0.5 (for
EDL or EMPC [Sample Conc.] x
values)
WHO 2005 TEF
0.162
0.1615
0.269
0.2685
0.914
0.0914
2.7
0.27
2.48
0.248
64.1
0.641
2860
0.858
0.161
0.352
1.05
1.26
0.646
0.951
0.269

0.0161
0.01056
0.315
0.126
0.0646
0.0951
0.02685

ND = 0 (for
EDL or
EMPC
EDL or EMPC
values)
0.323
0
0.537
0
0.914
2.7
2.48
64.1
2860
0.322

0.537

0
0.352
1.05
1.26
0.646
0.951
0

1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF

0.01
0.01
0.0003

9.99
0.545
21.4

0.0999
0.00545
0.00642
3.30

9.99
0.545
21.4
TEQ [pg/g]
where ND=0.5

EMPC [WHO WHO 2005

2005 TEQ
TEQ
WHO 2005 (ND=0) (ND=0)]
(ND=1/2)
[pg/g]
[pg/g]
[pg/g]
2.83
4.01
3.30
0.0895
0.0918
0.7530
0.0568
0.0606
0.9180
2.67
2.72
2.87
2.86
2.86
3.24
3.50
3.58
4.23
0.0979
0.1660
0.8340
2.15
2.20
2.39
0.1730
0.2980
0.7390
2.53
3.14
2.68
0.0167
0.0487
0.7900
0.5770
0.6870
1.40
1.19
1.43
1.59
1.16
1.43
1.64
0.2190
0.2190
0.7780
0.0478
0.0478
0.6790

[EDL] or [EMPCs] at for the ND= value

[Sample Conc.] x
WHO 2005 TEF
0
0
0.0914
0.2700
0.2480
0.6410
0.8580
0
0.0106
0.3150
0.1260
0.0646
0.0951
0

EMPC [WHO 2005

TEQ (ND=1/2)]
[pg/g]
4.17
0.7530
0.9180
2.88
3.24
4.27
0.8030
2.39
0.6190
3.14
0.8140
1.39
1.58
1.64
0.7780
0.6790

0.0999
0.0055
0.0064
2.83 TEQ [pg/g]
where ND=0