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SEPTEMBER 2017 BERTH 5 OIL SPILL - Sampling Results and Interpretations JAMES R. PAYNE, PH.D. WILLIAM B. DRISKELL APRIL 2018 PWSRCAC Contract No. 951.18.08 The opinions expressed in this commissioned report are not necessarily those of PWSRCAC

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SEPTEMBER 2017 BERTH 5 OIL SPILL - Sampling Results and Interpretations

JAMES R. PAYNE, PH.D. WILLIAM B. DRISKELL APRIL 2018

PWSRCAC Contract No. 951.18.08

The opinions expressed in this commissioned report are not necessarily those of PWSRCAC

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Cover photo – Oil spill cleanup operations proceed near Berth 3 in the foreground with Berths 4 & 5 further west on 24 September 2017. Saw Island sampling site lies just beyond Berth 5; Jackson Point sampling site is below photo in foreground. Photograph courtesy of Alyeska Pipeline Service Company.

9-22-2017 Sheen under Berth 5. PWSRCAC Photo.

9-22-2017 Boom under Berth 5. PWSRCAC Photo.

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9-29-2017 Jackson Pt. Mussel Sampling. PWSRCAC Photo.

12-7-2017 Jackson Pt. Mussel Sampling. PWSRCAC Photo.

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2017 BERTH 5 OIL SPILL - SAMPLING RESULTS AND INTERPRETATIONS

James R. Payne, Ph.D. and William B. Driskell

Introduction On 21 September 2017, an estimated 150 gallons of Alaska North Slope (ANS) crude oil were accidentally released during crude oil loading arm leak testing at Berth 5 of the Alyeska Marine Terminal. As part of the post-spill monitoring efforts, mussels were collected from the same 3 Port Valdez stations annually sampled as part of the PWSRCAC Long Term Environmental Monitoring Program (LTEMP). Collections at Saw Island (SAW) adjacent to Berth 5, Jackson Point (JAC) east of Berth 3, and Gold Creek (GOC) across the port occurred on Sept 29-30 and again, as a follow up, 70 days later on Dec 7-9, 2017 (Figure 1). Two of the sampling sites, SAW and JAC, bracket the shoreline of the release location with the Saw Island site immediately adjacent (west) of Berth 5 (Figure 2). The GOC reference site is 6 km across the Port.

This report describes and illustrates the pre- and immediate post-spill hydrocarbon signatures plus the state of recovery in Port Valdez mussels 70 days after the spill.

Figure 1. Spill and sampling locations within Port Valdez (satellite image from Google Earth). Tankers are seen docked at both Berths 4 and 5.

Alyeska Marine Terminal

Valdez

Gold Creek

Saw Island Jackson Pt Berth 5

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Figure 2. Nautical chart of the offshore area immediately adjacent to the Valdez Marine Terminal detailing the Berth 5 incident site. Saw Island (the traditional LTEMP AMT sampling site) and Jackson Point (added to LTEMP in 2016) are denoted by a red X.

During the spill and subsequent cleanup efforts between 21 and 27 September 2017, oil and sheen were observed between Berths 4 and 5 and trending westward including some shoreline impacts between the berths and west and south of Saw Island. Berths 4 and 5 were entirely boomed to contain sheen and oil (Figure 3). Protective booms were also installed around the Solomon Gulch Fish Hatchery (to the east) and Duck Flats (to the northeast), although no oil or sheen was observed in those areas.

Figure 3. Sheen observed between Berths 4 and 5 during cleanup activities in September 2017. Photograph courtesy of Alyeska Pipeline Service Company.

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Saw Island

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Methods Following established LTEMP protocols, triplicate samples comprising approximately 30 adult mussels (Mytilus trossulus) were collected by Austin Love (PWSRCAC) along the shorelines at each location. Handling, processing and chemical analyses followed standard methods previously described in earlier LTEMP reports (Payne et al., 2010; and Payne and Driskell 2017b). Chemical analyses were conducted by PWSRCAC’s LTEMP contractor, Alpha Analytical Laboratory, in Mansfield, MA. Analyses comprised standard methods for polycyclic aromatic hydrocarbons (PAH) and sterane and triterpane biomarkers, using a modified 8270 EPA method on gas chromatography/mass spectrometry (GC/MS SIM) instruments, plus saturated hydrocarbons (SHC), using gas chromatography with flame-ionization detection (GC/FID). From these analyses, 63 PAH, 74 biomarkers and 37 SHC target compounds are reported. Note that the suite of 55 biomarkers normally reported for LTEMP was expanded to include additional mono- and tri-aromatic steranes. These components were recently added to Alpha Laboratory’s target analyte list, and it is believed that they will aid with oil fingerprinting in the future. PAH and biomarker analytes in tissues are reported on a µg/kg dry wt. (ppb) basis, while SHC in tissues are mg/kg (ppm), and all oil components are mg/kg (ppm). For forensic interpretations, an Excel application was assembled to review individual samples graphically overlaid by a source signature scaled to the sample. Comparative excesses or depletions in the patterns of individual analytes reveal the effects of weathering, mixing, or absence of spill oil. These methods are more fully described in Payne and Driskell, 2018; Driskell and Payne, 2018; Payne and Driskell 2017a,b; and Payne et al., 2008, 2010.

Source Oil Characterization During the response activities, a reference source sample was obtained by PWSRCAC from the spilled-oil collection barge on 29 September 2017. The source oil signature (Figure 4) show a slightly weathered ANS profile containing a full suite of PAH, partially evaporated but non-biodegraded SHC, and characteristic biomarkers that permit direct comparisons to the oiled and residual trace profiles observed in the mussel samples (discussed below).

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Figure 4. Analytic results of the source-oil sample comprise PAH (left plot), SHC (middle plot) and biomarkers (right plot; hopane highlighted). The red overlay line is the spilled source oil and thus exactly matches bar plot of the same source sample. This reference overlay method is used to compare the mussel samples to the source when reviewing each sample plot. Typically, the overlay is scaled to hopane for PAH and biomarkers and n-C27 for SHC.

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Pre-spill Conditions Routine LTEMP monitoring samples collected in early July 2017 showed expected trace background signatures both near the terminal and across the Port at the GOC reference site (Figure 5). These patterns do not appear to be from the degraded oil discharges of the Ballast Water Treatment Facility (BWTF) (Payne and Driskell, 2017; and 2018 in preparation). Instead, these are low-concentration background patterns, all similar, in which the PAH reflect primarily dissolved-phase (parent-dominated) naphthalenes (N), phenanthrene/anthracenes (P/A), fluoranthene/pyrenes (FP) and traces of particulate-phase combustion products.

Figure 5. Representative PAH and biomarker profiles from July 2017 mussel collections at Saw Island, Jackson Point, and Gold Creek (LTEMP stations: AMT, JAP and GOC, respectively). The dotted red line shows the expected scaled profiles from the fresh spill oil (Figure 4) normalized to hopane. Note that the triaromatic steranes and newly added biomarkers do not appear in tissue samples because they are removed during L/C chromatography to separate lipids.

As confirmed by the dissimilarity to fresh spill-oil patterns (indicated by the red dotted line), neither the PAH or biomarker patterns show any solid evidence of ANS crude oil. Instead, the background, dissolved-phase patterns and concentrations at AMT and JAP are essentially the same as those measured in July 2016 (Payne and Driskell 2017). During the July 2016 sampling at GOC there was evidence of a localized diesel spill (Payne and Driskell,

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2017), but that, too, had disappeared by July 2017 when the background pattern at GOC more closely matched those at the other two Port Valdez locations (Figure 5).

Post-Berth 5 Oil Spill Signatures Mussel samples collected at SAW and JAC just over a week after the Berth 5 spill show weathered PAH and biomarker patterns associated with the released ANS oil (Figure 6). At GOC, however, there was no evidence that the oil or sheen had migrated across the Port. Only traces of background PAH and biomarkers were observed (not matching any known source). Note that the newly added triaromatic steranes and extended biomarkers do not appear in tissue samples because they are removed during HPLC clean-up of the extracts to eliminate lipid interference. The additional components added by the lab are of primary interest for oil sample characterizations.

Figure 6. PAH and Biomarker patterns at SAW, JAC, and GOC collected on 29 September 2017, just over a week after the spill. The dotted red lines represent the anticipated profiles from the collected spill oil (Figure 4) normalized to hopane. Profiles from all three replicates at each site are shown in Appendix 1.

In agreement with observations and photographic evidence obtained during the spill response, the PAH and biomarker concentrations also confirm that most of the released oil migrated to the west, impacting the adjacent

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Saw Island site, as the TPAH concentrations were significantly higher at SAW compared to JAC (see further discussion below).

Spill Recovery Signatures By December (70 days post), hydrocarbon levels in the mussel samples at all three locations were reduced to near-background concentrations with patterns nearly identical to pre-spill conditions (Figure 7). Total PAH (TPAH) concentrations (Figure 8) also reflect the spilled-oil uptake and rapid depuration after the spill. Other studies have suggested that mussels can purge themselves fairly rapidly following short episodic oil exposures with the decreases in the hydrocarbon concentrations following an exponential curve. Early work reported a depuration half-life of less than a week (Lee, 1977 and Mason, 1988). Later work following the Prestige oil spill suggested more complex processes with two phases of depuration (Neito et al., 2006). A number of factors may affect depuration rates; oil composition, exposure period, water temperature, mussel size, maturity, body lipid content, stress, etc. The Berth 5 spill data are too limited to establish depuration rates but suffice to say, 70 days after the episodic event, the mussels were effectively clean.

Figure 7. PAH and Biomarker patterns at SAW, JAC, and GOC collected on 12 December 2017, just over 10 weeks (71 days) after the spill. The dotted red lines represent the anticipated profiles from the collected spill oil (Figure 4) normalized to hopane. Profiles from all three replicates at each site are shown in Appendix 1.

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MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1712-1

0

1

2

3

4

5

6

7

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0

N1

N2

N3

N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

ug/k

g

GOC-1712-1

TPAH4 Hopane0.83

0

1

2

3

4

5

6

7

8

9

10

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1712-1

11

Figure 8. Average total PAH (TPAH) concentrations measured at the three collection sites between July 2017 and December 2017.

Table 1. TPAH values, means and std error of means for all samples.

Means SE of Means Date Saw Island Jackson Pt Gold Creek Saw Island Jackson Pt Gold Creek Saw Island Jackson Pt Gold Creek 7/8/2017 6.7 5.7 7.5 6.3 8.4 8.0 0.23 2.58 0.44 7/8/2017 6.0 5.9 7.7 7/8/2017 6.1 13.6 8.9 9/29/2017 157.7 21 5.5 150.2 26.2 5.1 21.86 2.64 0.38 9/29/2017 109.2 28.2 4.3 9/29/2017 183.8 29.5 5.4 12/7/2017 10.4 4.1 4.1 9.0 3.3 2.7 0.70 0.8 0.68 12/7/2017 8.2 4.1 2.1 12/7/2017 8.4 1.7 2 ng/g dry wt

These data also show the relative impacts based on the TPAH loadings in the western (Saw Island) versus eastern (Jackson Point) collection sites adjacent to the terminal. As noted above, these data support the prevailing surface oil/sheen transport to the west observed during the spill event.

Quality Control All sample results were validated by Alpha Laboratory QC personnel as meeting lab performance standards. Noted artifacts include the T26 biomarker interferant and below-MDL trace-level n-C23-n-C34 “haystack” patterns in the method blanks. That haystack pattern also appeared in all of the mussel samples collected in September and December 2017 (Figure 9) where the concentrations were all well above the sample-specific MDLs.

Table 2. Summary of surrogate analyte recoveries for field and QC samples (acceptable range 40-120%).

QC Recovery (%) Average Max Min Count

Naphthalene-d8 61.0 111 44 25

Phenanthrene-d10 76.0 105 60 25

Benzo[a]pyrene-d12 75.4 116 54 25

o-terphenyl 96.7 97 96 3

d50-Tetracosane 95.3 111 78 25

5B(H)Cholane 106.8 123 96 25

0

20

40

60

80

100

120

140

160

180

200

Jul-17 Aug-17 Sep-17 Oct-17 Nov-17 Dec-17

ng/g

dry

wt

Mussel Tissue TPAH

Saw Island avg

Jackson Pt avg

Gold Creek avg

SE of means

12

Mussel Tissue SHC – September 2017 Mussel Tissue SHC – December 2017

QC Method Blanks – September 2017 Samples QC Method Blanks – December 2017 Samples

Figure 9. SHC patterns in September and December 2017 mussel-tissue samples at all three sites with the red line denoting the sample-specific MDL (upper plots) and the laboratory method blanks (note at order-of-magnitude lower concentrations) analyzed with the September and December sample batches (lower plots). The n-C15, n-C17, and pristane observed in the tissues represent input from phytoplankton and zooplankton (Short, 2005) while the C23-C34 “haystack” likely derives from marine bacteria (Davis, 1968; Han and Calvin 1969; and NAS 1975).

QC Method Blanks – September 2017 Samples QC Method Blanks – December 2017 Samples

Figure 9. SHC patterns in September and December 2017 mussel-tissue samples at all three sites with the red line denoting the sample-specific MDL (upper plots) and the laboratory method blanks (note at order-of-magnitude lower concentrations) analyzed with the September and December sample batches (lower plots). The n-C15, n-C17, and pristane observed in the tissues represent input from phytoplankton and zooplankton (Short, 2005) while the C23-C34 “haystack” likely derives from marine bacteria (Davis, 1968; Han and Calvin 1969; and NAS 1975).

0

0.002

0.004

0.006

0.008

0.01

0.012

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1059598-1-BLANK

TSHC0

0

0.005

0.01

0.015

0.02

0.025

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1078906-1-BLANK

TSHC0

0

0.002

0.004

0.006

0.008

0.01

0.012

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1059598-1-BLANK

TSHC0

0

0.005

0.01

0.015

0.02

0.025

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1078906-1-BLANK

TSHC0

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1709-1

TSHC2

0

0.05

0.1

0.15

0.2

0.25

0.3

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1709-2

TSHC2

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1709-3

TSHC2

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-1

TSHC4

0

0.05

0.1

0.15

0.2

0.25

0.3

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-2

TSHC2

0

0.05

0.1

0.15

0.2

0.25

0.3

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-3

TSHC2

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-1

TSHC2

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-2

TSHC2

0

0.05

0.1

0.15

0.2

0.25

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-3

TSHC2

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-1

TSHC1

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-2

TSHC1

0

0.05

0.1

0.15

0.2

0.25

0.3

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-3

TSHC1

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-1

TSHC1

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-2

TSHC1

0

0.05

0.1

0.15

0.2

0.25

0.3

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-3

TSHC2

0

0.02

0.04

0.06

0.08

0.1

0.12

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-1

TSHC1

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-2

TSHC1

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-3

TSHC1

13

SHC Artifacts

One intriguing aspect of the data analysis regarded the ubiquitous n-C23 to n-C34 “haystack” pattern observed in the SHC distributions for all the mussel samples reviewed (Figure 9 and Appendix 1). It was thought at first that they might be associated with the spill event because the pattern neatly fit beneath the spilled-oil, SHC fingerprint normalized to n-C27. But that couldn’t be because the pattern (based on m/z 85 ion data) also appeared in one of three AMT samples, two of three GOC samples, and at varying concentrations in two of three JAC samples from the July 2017 LTEMP collections before the Berth 5 spill (Payne and Driskell, 2018 in preparation). Note that SHC were not quantified in the mussel samples for 2016 LTEMP. The next potential source could possibly be laboratory or field contamination, but the lab blanks (while showing a similar pattern, but at an order-of-magnitude lower concentration – see Figure 9) seemed to rule that out. Field contamination was also unlikely because the July 2017 samples were collected by Payne and Janka as part of the LTEMP effort on the Auklet, while the September and December 2017 samples were collected by Austin Love using a water taxi out of Valdez. It seems highly unlikely that three separate field efforts completed by different personnel from different vessels over a six-month time frame would encounter the same contamination.

Review of pre-2017 LTEMP data generated by the NOAA Auke Bay Laboratory also showed the occasional presence of this n-C23 to n-C35 haystack (Payne et al., 2010). After further literature review, we believe that the haystack pattern can be traced to bacterial sources. NAS (1975, p 29) reports that an odd-to-even n-alkanes ratio of one in the C25-C33 range may not always be due to oil as some bacteria can generate alkanes with this distribution (Davis, 1968; Han and Calvin, 1969). For additional details on biogenic and petrogenic sources, see the LTEMP Oil Primer in Appendix A of our Final 2006-2008 LTEMP report (Payne, Driskell, Short, and Larsen, 2010).

Summary Pre-spill samples showed traces of hydrocarbons whose signatures could not be attributed to the degraded oil discharges of the Ballast Water Treatment Facility. In the week after the Berth 5 spill event, crude oil was present in the tissues from the adjacent Saw Island site and from Jackson Point. The reference site across the Port was unaffected. By December, all three locations had returned to near-background concentrations and to patterns, nearly identical to pre-spill patterns.

References Davis, J.B. 1968. Paraffin hydrocarbons in the sulfate-reducing bacterium Desulfovibrio desulfuricans. Chem. Geol. 155-160.

Driskell, W. B., and J.R. Payne. 2018. Development and application of phase-specific methods in oiled-water forensic studies. Chapter 14 in (S. Stout and Z. Wang, eds). Oil Spill Environmental Forensics Case Studies. Butterworth-Heinemann/Elsevier Publishers, Oxford, United Kingdom and Cambridge, Massachusetts. 2018: 289-323.

Han, J. and M. Calvin. 1969. Hydrocarbon distribution of algae and bacteria, and microbiological activity of sediments. Proc. Natl. Acad. Sci. 64: 436-455.

Lee, R.F. 1977. Accumulation and turnover of petroleum hydrocarbons in marine organisms. In: Fates and effects of petroleum hydrocarbons in the marine environment. Wolfe, DA (ed). New York: Pergammon Press.

Mason, R.P. 1988. Accumulation and depuration of petroleum hydrocarbons by black mussels. 1. Laboratory exposure trials, South African Journal of Marine Science, 6:1, 143-153, DOI: 10.2989/025776188784480582

14

National Academy of Sciences (NAS). 1975. Petroleum in the Marine Environment. Workshop on inputs, fates, and the effects of petroleum in the marine environment. May 21-25, 1973. Airlie House, Airlie, Virginia. 107 pp.

Neito, O., J. Aboigor, R. Buján, M. N’Diaye, J. Graña, L. Saco-Álvarez, Á. Franco, J.A. Soriano, R. Beiras. 2006. Temporal variation in the levels of polycyclic aromatic hydrocarbons (PAHs) off the Galician Coast after the Prestige oil spill. Marine Ecology Progress Series 328:41-49, DOI10.3354/meps328041

Payne, J.R. and W.B. Driskell. 2018. Macondo oil in northern Gulf of Mexico waters – Part 1: Assessments and forensic methods for Deepwater Horizon offshore water samples. Marine Pollution Bulletin 129(1): 399-411.

Payne, J.R. and Driskell, W.B. 2017a. Water-column measurements and observations from the Deepwater Horizon oil spill Natural Resource Damage Assessment. Proceedings of the 2017 Oil Spill Conference. American Petroleum Institute, Washington, DC. Paper No. 2017-167.

Payne, J.R. and W.B. Driskell. 2017b. Long-term environmental monitoring program: 2016 sampling results and interpretations. Report for PWSRCAC Contract No. 951.1.01. August 2017. 69 pp.

Payne, J.R., W.B. Driskell, J.W. Short, and M.L. Larsen. 2010. Long-Term Environmental Monitoring Program: Final 2006-2008 LTEMP Monitoring Report. PWSRCAC Contract Nos. 951.07.01 and 951.08.01. February 2010. 198 pp.

Payne, J.R., W.B. Driskell, J.W. Short, M.L. Larsen. 2008. Long term monitoring for oil in the Exxon Valdez spill region. Marine Pollution Bulletin 56: 2067-2081.

Short, J.W. 2005. Seasonal variability of pristane in mussels (Mytilus Trossulus) in Prince William Sound, Alaska. Ph.D. Thesis. University of Alaska, Fairbanks. 204 pp.

15

Appendix 1 – All analytic results

Source oil from spill collection barge. Here, the red overlay is also the source oil; highlighted biomarker is hopane.

0

200

400

600

800

1000

1200

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0

N1

N2

N3

N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

mg/

kg

BAR-1709-1

TPAH7,291 Hopane138

0

500

1000

1500

2000

2500

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

BAR-1709-1

TSHC31,252

0

50

100

150

200

250

300

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

mg/

kg

BAR-1709-1

16

Gold Creek Reference site, Sept 2017, with hopane- or C-27-scaled source oil overlay.

0

0.5

1

1.5

2

2.5

3

3.5

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0

N1

N2

N3

N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

ug/k

g

GOC-1709-1

TPAH5 Hopane0.46

0

0.2

0.4

0.6

0.8

1

1.2

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

GOC-1709-1

TSHC2

0

1

2

3

4

5

6

7

8

9

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1709-1

0

0.5

1

1.5

2

2.5

3

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

GOC-1709-2

TPAH4 Hopane0.355

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1709-2

TSHC2

0

1

2

3

4

5

6

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1709-2

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

GOC-1709-3

TPAH5 Hopane0.256

0

0.2

0.4

0.6

0.8

1

1.2

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1709-3

TSHC2

0

1

2

3

4

5

6

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1709-3

17

Jackson Point impact site, Sept 2017, with hopane- or C-27-scaled source oil overlay.

0

2

4

6

8

10

12

14

16

18

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1709-1

TPAH21 Hopane2.26

0

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

1.8

2

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-1

TSHC4

0

1

2

3

4

5

6

7

8

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1709-1

0

2

4

6

8

10

12

14

16

18

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1709-2

TPAH28 Hopane2.33

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-2

TSHC2

0

1

2

3

4

5

6

7

8

9

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1709-2

0

2

4

6

8

10

12

14

16

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1709-3

TPAH29 Hopane2.13

0

0.2

0.4

0.6

0.8

1

1.2

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1709-3

TSHC2

0

1

2

3

4

5

6

7

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1709-3

18

Saw Island impact site, Sept 2017, with hopane- or C-27-scaled source oil overlay.

0

5

10

15

20

25

30

35

40

45

50

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1709-1

TPAH158 Hopane6.17

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-1

TSHC2

0

1

2

3

4

5

6

7

8

9

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1709-1

0

10

20

30

40

50

60

70

80

90

100

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1709-2

TPAH109 Hopane12.7

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-2

TSHC2

0

2

4

6

8

10

12

14

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1709-2

0

10

20

30

40

50

60

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1709-3

TPAH184 Hopane7.29

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1709-3

TSHC2

0

2

4

6

8

10

12

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1709-3

19

Gold Creek Reference Site, Dec 2017, with hopane- or C-27-scaled source oil overlay.

0

1

2

3

4

5

6

7

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

GOC-1712-1

TPAH4 Hopane0.83

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-1

TSHC1

0

1

2

3

4

5

6

7

8

9

10

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1712-1

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

GOC-1712-2

TPAH2 Hopane0.604

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-2

TSHC1

0

1

2

3

4

5

6

7

8

9

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1712-2

0

1

2

3

4

5

6

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

GOC-1712-3

TPAH2 Hopane0.756

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

GOC-1712-3

TSHC1

0

1

2

3

4

5

6

7

8

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

GOC-1712-3

20

Jackson Point Impact Site, Dec 2017, with hopane- or C-27-scaled source oil overlay.

0

1

2

3

4

5

6

7

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1712-1

TPAH4 Hopane0.924

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-1

TSHC1

0

1

2

3

4

5

6

7

8

9

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1712-1

0

1

2

3

4

5

6

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1712-2

TPAH4 Hopane0.738

0

0.1

0.2

0.3

0.4

0.5

0.6

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-2

TSHC1

0

1

2

3

4

5

6

7

8

9

10

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1712-2

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

JAC-1712-3

TPAH2 Hopane0.581

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

JAC-1712-3

TSHC1

0

1

2

3

4

5

6

7

8

9

10

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

JAC-1712-3

21

Saw Island Impact Site, Dec 2017, with hopane- or C-27-scaled source oil overlay.

0

1

2

3

4

5

6

7

8

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1712-1

TPAH10 Hopane1.03

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-1

TSHC1

0

2

4

6

8

10

12

14

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1712-1

0

0.5

1

1.5

2

2.5

3

3.5

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1712-2

TPAH8 Hopane0.459

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-2

TSHC1

0

1

2

3

4

5

6

7

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1712-2

0

1

2

3

4

5

6

7

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4 N0 N1 N2 N3 N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4NB

TNB

T1NB

T2NB

T3NB

T4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HABG

HIP

ug/k

g

SAW-1712-3

TPAH8 Hopane0.902

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npris C17

Pris

C18

Phy

C19

C20

C21

C22

C23

C24

C25

C26

C27

C28

C29

C30

C31

C32

C33

C34

C35

C36

C37

C38

C39

C40

mg/

kg

SAW-1712-3

TSHC2

0

2

4

6

8

10

12

14

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

SAW-1712-3

22

PAH and SHC Method Blanks, Sept 2017

Note dramatically lower (more sensitive) SHC concentration scale (0.00 – 0.012 mg/kg) for WG1059598 1-BLANK vs. September field samples (0.00 – 2 mg/kg).

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7DE

CDE

C1DE

C2DE

C3DE

C4 BT0

BT1

BT2

BT3

BT4

N0

N1

N2

N3

N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

ug/k

g

WG1057108-1-BLANK

TPAH4 Hopane#N/A

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

#N/A

WG1057108-1-BLANK

TSHC#N/A

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

#N/A

WG1057108-1-BLANK

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4N

0N

1N

2N

3N

4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

#N/A

WG1059598-1-BLANK

TPAH#N/AHopane0

0

0.002

0.004

0.006

0.008

0.01

0.012

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1059598-1-BLANK

TSHC0

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

WG1059598-1-BLANK

23

PAH and SHC Method Blanks, Dec 2017

Note lower SHC (more sensitive) concentration scale (0.00 – 0.025 mg/kg) for WG1078906-1-BLANK vs. December field samples (0.00 – 0.7 mg/kg).

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9DE

CDE

C1DE

C2DE

C3DE

C4 BT0

BT1

BT2

BT3

BT4

N0

N1

N2

N3

N4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

ug/k

g

WG1077170-1-BLANK

TPAH3 Hopane#N/A

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

#N/A

WG1077170-1-BLANK

TSHC#N/A

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

#N/A

WG1077170-1-BLANK

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

DEC

DEC1

DEC2

DEC3

DEC4 BT

0BT

1BT

2BT

3BT

4N

0N

1N

2N

3N

4 BP DBF

ACY

ACN F F1 F2 F3

ANT

PHN

PA1

PA2

PA3

PA4

RET

DBT0

DBT1

DBT2

DBT3

DBT4

CARB FL

ABB

FPY

RFP

1FP

2FP

3FP

4N

BTN

BT1

NBT

2N

BT3

NBT

4BA

A C0 C1 C2 C3 C4 BBF

BJKF BA

FBE

PBA

PPE

R IPDA

HA

BGH

IP

#N/A

WG1078906-1-BLANK

TPAH#N/AHopane0

0

0.005

0.01

0.015

0.02

0.025

C9 C10

C11

C12

C13

1380 C1

414

70 C15

C16

Npr

isC1

7Pr

isC1

8Ph

yC1

9C2

0C2

1C2

2C2

3C2

4C2

5C2

6C2

7C2

8C2

9C3

0C3

1C3

2C3

3C3

4C3

5C3

6C3

7C3

8C3

9C4

0

mg/

kg

WG1078906-1-BLANK

TSHC0

0

0.02

0.04

0.06

0.08

0.1

0.12

0.14

T4 T5 T6 T6a

T6b

T6c T7 T8 T9 T10 Ts

TR30

aTR

30b

Tm 14a

14b

T15

T16

T17

T18 OL

T19

T20

T21

T22

Gam

mT2

6T2

7T3

0T3

1T3

2T3

3T3

4T3

5 S4 S5 S8DI

A29S

DIA2

9R S18

S19

S20

S24

S25

S28

S14

S15

S22

S23

S26

S27

Preg

MPr

egEP

regA

EPre

gBTA

S0TA

S1TA

S2TA

S3TA

S4TA

S5TA

S6M

AS1

MAS

2M

AS3

MAS

4M

AS5

MAS

6M

AS7

MAS

8M

AS9

MAS

10M

AS11

MAS

12

ug/k

g

WG1078906-1-BLANK