Appendix I Clam Tissue

Clam Tissue Collection Report

Wyckoff/Eagle Harbor Superfund Site

EPA ID: WAD009248295

Prepared for:

U.S. Environmental Protection Agency Region 10 1200 6th Avenue Seattle, Washington 98101

Prepared by:

U.S. Army Corps of Engineers Seattle District 4735 East Marginal Way South Seattle, WA 98134

16 January 2012

Contents 1.0 Background and Purpose ...... 3 2.0 Methods...... 3 2.1 Sampling Event ...... 3 2.2 Tissue Data...... 6 3.0 Results ...... 7 4.0 Discussion and Recommendations ...... 11 5.0 References ...... 11 Figures

Figure 1 Wyckoff Clam Survey Locations in 2003 and April and May 2011 ...... 5 Figure 2 Wyckoff Clam cPAH (0.5*RL) versus Lipid Fraction ...... 11

Tables

Table 1 Clam Tissue Total PAHs from all Locations ...... 9 Table 2 Clam Tissue cPAH from all Locations ...... 10

1.0 Background and Purpose The purpose of the collection and analysis of clam tissue is to gather additional information since the 2002 monitoring event, and to evaluate whether natural recovery has resulted in a decrease in chemical concentrations over time, and potentially evaluate whether clams from East Beach are safe for human consumption. The collection of clam tissue samples from East Beach and North Shoal sediments were first included in the 2002 OMMP Addendum and added the Intertidal Cap location for the 2011 sampling event. The previous clam tissue results (East Beach Clam Tissue Report, Wyckoff/Eagle Harbor Superfund Site East Harbor Operable Unit Bainbridge Island, Washington, 28 June 2004) reported polycyclic aromatic hydrocarbons (PAH) analysis from geoduck, horse, and littleneck clams. “On May 5, 2003 geoducks were collected on the North Shoal and horse clams and native littlenecks were collected along the East Beach and the clams were composited by species.” A review of the photographs, identified as geoduck clams (collected at North Shoal), are actually horse clams (Tresus capax). In addition, the composited horse clams collected at East Beach are most likely butter clams (Saxidomus gigantean) based on the photographs. Previously collected littleneck clams were correctly identified. T. capax spawns during February to May peaking in March and therefore, the tissue lipid content would be depleted during spawning. T. capax is a suspension/filter feeder eating diatoms, flagellates, dinoflagellates, and detritus. They are mature at three years with a shell length of approximately seven centimeters. The oldest clam recorded was 16 years old, however, the oldest clams found in Oregon are 10 to 12 years old (http://hmsc.oregonstate.edu/projects/msap/PS/masterlist/inverts/horseneckgaper.html ). Campbell et. al. (2009) found T. capax in British Columbia ranged in age from 4 to 29 years old. Even though horse clams are longer lived than littleneck clams, the data can be used to document current PAH trends as the size collected are between three to 10 years old. 2.0 Methods 2.1 Sampling Event A quality assurance project plan (QAPP) and work plan - specific to the clam tissue collection in 2011, were completed prior to the field event which took place within the same time window (April/May) used in the 2003 monitoring event. A reconnaissance survey was conducted on 19 April 2011 to determine if sufficient clams would be present for tissue collection and analysis. Based on that survey, horse clams were not found in sufficient numbers on the West Beach (aka EBS area) and were not collected from this location during the May collection event. Sediment at this are appeared to be predominantly fish mix gravels and was different from sediments found at the other sampling locations. Clams were collected on 18 and 19 May 2011 for PAH tissue analysis from three separate locations within the Intertidal Cap, North Shoal, and East Beach locations (Figure 1). Clams were not collected on a grid system as the objective was to collect enough clams for tissue analysis within the three delineated locations. Clams were collected from the locations adjacent to those previously sampled in 2003 to the extent practicable. The general collection sites were GPS located rather than at each specific hole from

3 which clams were collected. A new GPS reading was taken for all other sample locations on North Shoal, East Beach, and Intertidal Cap. All clams were placed in coolers with ice in accordance with the QAPP and were hand delivered to Manchester Laboratory under chain of custody at the end of each collection day.

Figure 1 Wyckoff Clam Survey Locations in 2003 and April and May 2011

Per discussion with Richard Brooks of the Suquamish Tribe (2/17/2011), it was anticipated that only shellfish of harvestable size would be collected (the State of Washington Statewide Harvest Rules has “no minimum size” for horse clams). The goal for the sampling effort was to represent as accurately as possible the types of shellfish that would actually be harvested and therefore it was determined that clams of four inches or larger would be collected. As described in the QAPP, five clams, larger than four inches of a single species, were collected at nine separate locations (3 each at Intertidal Cap, North Shoal, and East Beach). Both Tresus capax and T. nuttallii clam species were collected on the outgoing tide starting at North Shoal 1 (NS-1). Species identification was verified by Debbie Kay of the Suquamish Tribe. Five individual clams of each species were collected, rinsed with site seawater, placed in a labeled baggie, and placed on ice in the cooler in accordance with the QAPP. Five T. capax were collected at the second location (NS-2) and Debbie Kay recommended that the T. capax be sent for analysis as the dominant species found on the site. Based on the species found at the first two collection locations, the team determined that T. capax would be used for analysis due to its availability. Five T. capax were collected at the third location (NS-3). No clams were collected within the eelgrass bed. Several holes were dug to collect sufficient clams of one species at the targeted site. GPS locations were taken for the sampling area and not at each specific hole. A new GPS reading was taken for all subsequent sample area locations. Samples from the Intertidal Cap were collected on the incoming tide over both days (I-1, -2, and -3). Five individual T. capax were collected from each of three locations. Sediments at I-2 and -3 were more gravelly than found at the North Shoal locations. Sediment at I-1 was similar to the North Shoal sediments. All clams were placed in the coolers with ice in accordance with the QAPP and were hand delivered to Manchester Laboratory under chain of custody at the end of each collection day. Samples were collected on the East Beach area on an outgoing tide using rakes due to the large cobbles underneath the sand layer where the clams were located. Five T. capax were collected from each of three locations. Clams were collected within the eelgrass bed as it was not as dense as the bed at North Shoal and was located at a higher tidal elevation. Abundant Ulva sp. was present compared to the minimal Ulva sp. present at North Shoal. 2.2 Tissue Data There are no established tissue-based PAH protectiveness goals in the East Harbor Record of Decision (ROD). The ROD states a sediment-based human health objective of 1,200 ug/kg dry wt high-molecular weight polycyclic aromatic hydrocarbons (HPAH), which is based on the 90th percentile of background Puget Sound subtidal sediments. Tissue samples were collected in accordance with the Puget Sound Protocols and Guidelines, Recommended Guidelines for Sampling Marine Sediment, Water Column, and Tissue in Puget Sound (PSAT 1997). Nine composite samples were taken from the three separate beach areas and the data may be used to determine the 95 percent upper confidence limit, when a subsequent human health risk analysis is completed. Horse clams once removed from the sediment were rinsed in site seawater,

6 measured, and placed in baggies with a sample label. Whole clams were placed in a cooler with ice to cool them to 4oC and hand delivered to the laboratory where they were processed for archiving. A minimum of 100 g of clam tissue (whole body without shell) is required in each composite for analysis of PAH and lipids (gutball contents were removed and discarded prior to analysis). Since the clams are large, the liquid inside the shell was not retained similar to the process for cleaning geoducks and therefore, clams were not depurated prior to processing. The tissue sample preparation and homogenization procedure was modified from the WA Dept of Health February 4, 2011 Technical Assistance for preparing geoduck tissue samples. The laboratory process included resection of the entire clam tissue, remove the outer skin and hard tip from the neck, discard the contents of the gutball (empty the gutball and retain gutball tissue for analysis), homogenize the composite samples, and freeze the samples in glass jars at -18oC for later analysis. The laboratory reported the total weight for each homogenized sample. The Manchester Environmental Laboratory limit of quantitation (LOQ) for the seven carcinogenic PAHs is estimated to range from 1 to 2 ppb. This range of LOQs is calculated to resolve between 6.06 E-6 and 1.21 E-5 cancer risk for the child Tribal subsistence consumer. The tissue samples were extracted using EPA Method 3550-M modified (industrial blender), cleaned up using EPA Method 3660B, 3665A, and 3640A if needed, and analyzed for PAHs using EPA Method 8270D -SIM modified as necessary to achieve the required reporting limits. The Manchester Environmental Laboratory Standard Operating Proceedure was used for lipid content analysis (see attached memos).

3.0 Results The sum of the PAHs (nd=RL) ranged from a high of 86.41 ug/kg-w at North Shoal 2 to a low of 38.31 ug/kg-w at East Beach 1 (Table 1). Chemicals with the highest values were anthracene and pyrene at East Beach 1, and phenathrene and pyrene at North Shoal 2. Values at the North Shoal stations were greater (average ~73 ug/kg-w) than either the East Beach (average ~52 ug/kg-w) or Intertidal stations (average ~56 ug/kg-w). Lipid content ranged from a high of 0.71 percent at Intertidal Cap 3 to a low of 0.40 percent at East Beach 3. It should be noted that the 0.71 percent lipid is an outlier and may influence the interpretation of the data compared to locations where the lipid content was lower. Lipid normalized values ranged from 16.3 mg/kg-w at North Shoal 2 to a low of 7.09 mg/kg-w at East Beach 1. Total cPAH, 0.5*RL toxicity equivalency quotient (TEQ) ranged from a low of 2.98 ug-TEQ/kg-w at East Beach 1 to a high of 5.64 ug-TEQ/kg-w at North Shoal 1. The chemical with the highest value was benzo[g,h,i]perylene at all stations. All the North Shoal stations had higher values (all greater than 4.0 ug/kg-w) than either East Beach or the Intertidal stations (generally around 3.1 ug/kg-w). Numerous holes were found to have contamination present including free product at North Shoal 2. No sheen or free product was present in the sampled holes from the Intertidal Cap locations. The two locations towards the northern portion of East Beach had slight sheens (lesser degree than the sheens found at North Shoal) but no free product was present.

Data results of the clam tissue collected in 2003 found that “Nearly all PAHs were undetected in all samples, and the few detected values were less than the quantitation limit (the level at which an analyte is considered quantifiable). Phenanthrene, fluoranthene, and pyrene were detected in all samples but concentrations are estimated and below the quantiation limit.” The RL and QL for the 2003 clam tissue PAH analysis was 60 and 120 ug/kg wet wt respectively. The RL for the 2011 clan tissue PAH analysis was 0.93 ug/kg wet. Therefore, there can be no comparison of PAH levels from 2003 and 2011 sampling events.

Table 1 Clam Tissue Total PAHs from all Locations

Sample Location: EAST BEACH # 1 EAST BEACH # 2 EAST BEACH #3 INTERTIDAL #2 INTERTIDAL BEACH #3 INTERTIDAL CAP # 1 INTERTIDAL CAP # 3 NORTH SHOAL # 1 NORTH SHOAL # 2 NORTH SHOAL # 3 NORTH SHOAL REP lipid lipid lipid lipid lipid lipid lipid lipid lipid lipid lipid normal normal normal normal normal normal normal normal normal normal normal Result ized Result ized Result ized Result ized ized ized ized ized ized ized ized Compound ug/kg mg/kg Q ug/kg mg/kg Q ug/kg mg/kg Q ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q Result ug/kg mg/kg Q 2- 1.4 0.26 U 1.3 U 1.6 0.40 U 1.3 0.24 U 1.2 0.20 U 1.5 0.32 U 1.7 0.24 U 1 0.18 U 1 0.19 U 1.6 0.33 U 3.5 0.76 0.27 METHYLNAPHTHALENE ACENAPHTHENE 0.93 0.17 U 1.6 0.33 1 0.25 0.93 0.17 U 0.92 0.16 U 0.99 0.21 0.99 0.14 1.2 0.21 1.4 0.26 1.5 0.31 1.2 0.26 ACENAPHTHYLENE 0.93 0.17 U 0.93 0.19 U 0.95 0.24 U 1.1 0.20 1 0.17 1.2 0.26 1.6 0.23 1.4 0.25 1.2 0.23 1.3 0.27 0.95 0.21 U ANTHRACENE 4.5 0.83 4.3 0.88 5.2 1.30 10 1.82 10 1.69 9.6 2.04 17 2.39 10 1.79 9.9 1.87 11 2.29 5.3 1.15 Benz[a]anthracene 2.1 0.39 3 0.61 2.9 0.73 2.2 0.40 1.8 0.31 2.4 0.51 3.4 0.48 2.8 0.50 3.5 0.66 2.6 0.54 2 0.43 Benzo[a]pyrene 1.2 0.22 1.6 0.33 1.2 0.30 1.1 0.20 1.2 0.20 1.3 0.28 1.5 0.21 3.4 0.61 3 0.57 2.3 0.48 1.4 0.30 Benzo[b]fluoranthene 0.93 0.17 U 1.7 0.35 1.9 0.48 1.8 0.33 1.7 0.29 2.2 0.47 2.6 0.37 4.2 0.75 3.3 0.62 2.9 0.60 2 0.43 Benzo[g,h,i]perylene 5.7 1.06 5.1 1.04 6 1.50 6.8 1.24 6.3 1.07 5.1 1.09 6.2 0.87 5.8 1.04 5.2 0.98 4.3 0.90 4.3 0.93 Benzo[k]fluoranthene 0.93 0.17 U 0.93 0.19 U 0.95 0.24 U 0.93 0.17 U 0.92 0.16 U 0.92 0.20 U 0.95 0.13 U 1.2 0.21 1.1 0.21 1.4 0.29 0.95 0.21 U CHRYSENE 1.9 0.35 U 1.9 0.39 U 1.9 0.48 U 1.9 0.35 U 1.9 0.32 U 1.8 0.38 U 1.9 0.27 U 1.9 0.34 U 1.8 0.34 U 1.9 0.40 U 1.9 0.41 U Dibenz[a,h]anthracene 0.93 0.17 U 0.93 0.19 U 0.95 0.24 U 0.93 0.17 U 0.92 0.16 U 0.92 0.20 U 0.95 0.13 U 0.95 0.17 U 0.91 0.17 U 0.94 0.20 U 0.95 0.21 U DIBENZOFURAN 0.93 0.17 U 1.1 0.22 0.95 0.24 U 0.93 0.17 U 0.92 0.16 U 0.84 0.18 J 0.95 0.13 U 1.1 0.20 1 0.19 1.2 0.25 0.98 0.21 FLUORANTHENE 3.9 0.72 7.6 1.55 5.2 1.30 7.3 1.33 6.4 1.08 7.3 1.55 7.3 1.03 11 1.96 15 2.83 9 1.88 7.5 1.63 FLUORENE 0.93 0.17 U 1.6 0.33 1.1 0.28 1.2 0.22 1 0.17 1.2 0.26 1.4 0.20 1.7 0.30 1.5 0.28 1.9 0.40 1.6 0.35 Indeno[1,2,3-cd]pyrene 1.9 0.35 U 1.9 0.39 U 1.9 0.48 U 1.9 0.35 U 1.9 0.32 U 1.8 0.38 U 1.9 0.27 U 1.9 0.34 U 1.8 0.34 U 1.9 0.40 U 1.9 0.41 U NAPHTHALENE 1.1 0.20 U 1.4 0.29 U 1.5 0.38 U 0.93 0.17 U 1 0.17 U 1.1 0.23 U 1.3 0.18 U 1.8 0.32 U 2.1 0.40 U 2 0.42 U 1.4 0.30 U PHENANTHRENE 3.3 0.61 6.7 1.37 4.7 1.18 5.2 0.95 4.5 0.76 4.8 1.02 4.5 0.63 6.4 1.14 6.7 1.26 7 1.46 6 1.30 PYRENE 4.8 0.89 11 2.24 26 6.50 7.1 1.29 8.3 1.41 11 2.34 9.7 1.37 24 4.29 26 4.91 14 2.92 13 2.83

Sums nd = RL 38.31 7.09 54.59 11.14 65.90 16.48 53.55 9.74 51.88 8.79 55.97 11.91 65.84 9.27 81.75 14.60 86.41 16.30 68.74 14.32 56.83 12.35 nd = 0*RL 25.50 4.72 41.00 9.24 55.20 13.80 43.80 7.96 42.20 7.15 47.93 10.02 56.19 7.91 74.20 13.25 78.80 14.87 60.40 12.58 47.18 10.60 nd = 0.5*RL 31.91 5.91 45.65 10.37 60.55 15.26 48.68 8.85 47.04 7.97 51.95 10.87 61.02 8.59 77.98 13.92 82.61 15.59 64.57 13.45 51.21 12.49

Table 2 Clam Tissue cPAH from all Locations

Benzo(a)p yrene Relative Response Sample Location: Factor EAST BEACH # 1 EAST BEACH # 2 EAST BEACH #3 INTERTIDAL #2 INTERTIDAL BEACH #3 INTERTIDAL CAP # 1 INTERTIDAL CAP # 3 NORTH SHOAL # 1 NORTH SHOAL # 2 NORTH SHOAL # 3 NORTH SHOAL REP Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid Res lipid ult normali ult normali ult normali ult normali ult normali ult normali ult normali ult normali ult normali ult normali ult normali ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed ug/k zed Compound g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ g-w mg/kg Q TEQ BENZ(A)ANTHRA 2.1 0.39 3 2.9 0.73 2.2 0.40 1.8 0.31 2.4 0.51 3.4 0.48 2.8 0.50 3.5 0.66 2.6 0.54 2 0.43 0.61 CENE 0.1 0.21 0.3 0.29 0.22 0.18 0.24 0.34 0.28 0.35 0.26 0.2 BENZO(A)PYREN 1.2 0.22 1.6 1.2 0.30 1.1 0.20 1.2 0.20 1.3 0.28 1.5 0.21 3.4 0.61 3 0.57 2.3 0.48 1.4 0.30 0.33 E 1 1.2 1.6 1.2 1.1 1.2 1.3 1.5 3.4 3 2.3 1.4 BENZO(B)FLUOR 0.9 0.17 U 0.04 1.7 1.9 0.48 1.8 0.33 1.7 0.29 2.2 0.47 2.6 0.37 4.2 0.75 3.3 0.62 2.9 0.60 2 0.43 0.35 ANTHENE 0.1 3 65 0.17 0.19 0.18 0.17 0.22 0.26 0.42 0.33 0.29 0.2 BENZO(K)FLUOR 0.9 0.17 U 0.00 0.9 U 0.00 0.9 0.24 U 0.00 0.9 0.17 U 0.00 0.9 0.16 U 0.00 0.9 0.20 U 0.00 0.9 0.13 U 0.00 1.2 0.21 0.01 1.1 0.21 0.01 1.4 0.29 0.01 0.9 0.21 U 0.00 0.19 ANTHENE 0.01 3 465 3 465 5 475 3 465 2 46 2 46 5 475 2 1 4 5 475 BENZO[g,h,i]PERY 5.7 1.06 0.00 5.1 0.00 6 1.50 0.00 6.8 1.24 0.00 6.3 1.07 0.00 5.1 1.09 0.00 6.2 0.87 0.00 5.8 1.04 0.00 5.2 0.98 0.00 4.3 0.90 0.00 4.3 0.93 0.00 1.04 LENE 0.001 57 51 6 68 63 51 62 58 52 43 43 CHRYSENE 1 1.9 0.35 U 0.95 1.9 0.39 U 0.95 1.9 0.48 U 0.95 1.9 0.35 U 0.95 1.9 0.32 U 0.95 1.8 0.38 U 0.9 1.9 0.27 U 0.95 1.9 0.34 U 0.95 1.8 0.34 U 0.9 1.9 0.40 U 0.95 1.9 0.41 U 0.95 DIBENZ(A,H)ANT 1 0.9 0.17 U 0.46 0.9 U 0.46 0.9 0.24 U 0.47 0.9 0.17 U 0.46 0.9 0.16 U 0.9 0.20 U 0.9 0.13 U 0.47 0.9 0.17 U 0.47 0.9 0.17 U 0.45 0.9 0.20 U 0.9 0.21 U 0.47 0.19 HRACENE 3 5 3 5 5 5 3 5 2 0.46 2 0.46 5 5 5 5 1 5 4 0.47 5 5 INDENO(1,2,3- 0.1 1.9 0.35 U 0.09 1.9 U 0.09 1.9 0.48 U 0.09 1.9 0.35 U 0.09 1.9 0.32 U 0.09 1.8 0.38 U 1.9 0.27 U 0.09 1.9 0.34 U 0.09 1.8 0.34 U 1.9 0.40 U 0.09 1.9 0.41 U 0.09 0.39 CD)PYRENE 5 5 5 5 5 0.09 5 5 0.09 5 5

Total cPAH, 0.5*RL 2.98 3.59 3.21 3.02 3.07 3.22 3.63 5.64 5.14 4.38 3.33 Total cPAH, KM 1.52 1.89 1.68 1.96 2.36 4.41 3.98 3.11 1.97 Sum 8 2.28 6 8 1.72 8 8 6 4 2 6 Total cPAH, lipid mg/kg 2.89 3.48 4.43 3.19 2.82 3.50 2.73 3.96 3.89 3.80 3.35

4.0 Discussion and Recommendations As stated previously, there are no established tissue-based PAH protectiveness goals in the East Harbor Record of Decision. Non-urban Puget Sound background PAH values are approximately 0.6 ug/kg-w as B(a)P TEF. For comparison in terms of clam concentration at the UCL95, background is 1.09 ug TEQ/kg-w compared with the Wyckoff site-related 4.24 ug TEQ/kg-w (both calculated using the 0.5*RL method of summation). The background values are about four times less than the tissue samples from Wyckoff. To account for how compounds vary in toxicity, EPA calculates weighted values called toxic equivalents (TEQs) from the individual mass quantity data reported by facilities and the associated Toxic Equivalency Factors (TEFs). The TEQs from this sampling can be used to facilitate a risk assessment. A risk calculation at this time would only show current risk and not be able to show any time trend of increasing or decreasing exposure to PAHs at the Wyckoff site. A comparison of the cPAH (0.5*RL) to the lipid fraction found no correlation (p-value = 0.3774) (Figure 2). If clams had been collected when they were at their maximum lipid content, data results may have shown a correlation. Figure 2 Wyckoff Clam cPAH (0.5*RL) versus Lipid Fraction

Since most of the 2011 tissue data values are detected, compared to all of the 2003 tissue data values are undetected, it is recommended that an additional clam collection event be conducted to help with a time-trend evaluation as to the effectiveness of the natural recovery for East Beach.

5.0 References Campbell, B.N., J.B. Groot, and S.M. Mahannah. 2009. An investigation into ageing methods for horse clams (Tresus nuttallii and T. capax). Can. Tech. Rep. Fish. Aquat. Sci. 2765:iii+25p 11

PSAT. 1997. Puget Sound Water Quality Action Team (PSAT). Recommended Guidelines for Sampling Marine Sediment, Water Column, and Tissue, in Puget Sound. April 1997. Washington Department of Health. February 4, 2011. Technical Assistance Geoduck Tissue Sample Preparation and Homogenization: Standard Operating Procedure.

Appendix A Field Trip Report and Memos from EPA Region 10 Laboratory

CENWS-EN-GB-ET

MEMORANDUM FOR: Karl Kunas, Project Manager, CENWS-PM-EM

Subject: Field Report for Wyckoff Superfund Site Clam Tissue Sampling 18 to 19 May 2011 1. On 18 May 2011, the Corps sampling team of Deborah Johnston, Karah Haskins, John Killeagle, and Maleena Scarsella traveled to the Wyckoff Superfund site to collect horse clams (Tresus capax and/or T. nuttallii) for an analysis study of tissue contaminant levels. As described in the QAPP, five clams, larger than four inches of a single species, were to be collected at eight separate locations (Intertidal Cap, North Shoal, and East Beach – see map for locations). The Seattle District, U.S. Army Corps of Engineers (Corps) under contract to the U.S. Environmental Protection Agency (EPA) is performing long-term monitoring activities at the Wyckoff/Eagle Harbor Superfund site located in Bainbridge Island, Washington. The monitoring activities are being conducted pursuant to CERCLA, Superfund Amendment and Reauthorization Act (SARA), the requirements of the 1994 Wyckoff/Eagle Harbor Superfund Site East Harbor Operable Unit (EHOU) Record of Decision (ROD), and regulatory requirements of the National Oil and Hazardous Substances Pollution Contingency Plan (NCP). The purpose of the clam tissue collection and analysis is to determine the polynuclear aromatic hydrocarbon (PAH) body burdens of clams on the beaches adjacent to the Wyckoff site. The tissue chemistry data may be used in a future human health risk assessment, future trends analysis, and for assessment of natural recovery. 2. The Corps team traveled on the Seattle to Bainbridge ferry and arrived on-site at 1015. The weather was sunny and clear. A Site-specific Safety and Health Plan (SSHP) review was conducted on the ferry by Deborah Johnston. All participants reviewed the SSHP and signed the signature page. An additional review was conducted for Debbie Kay (Suquamish Tribe) and Howard Orlean (EPA) on-site where they joined the sampling team. Sample equipment and coolers were prepared according to the QAPP. 3. Due to the current tide level (descending) and the site topography (generally flat), it was determined to start the sample collection in the west end of the North Shoal area as the steep beach in the Intertidal Cap area was not low enough to collect horse clams. a. Both Tresus capax and T. nuttallii clam species were collected at the first location (photo 1). The identification of the clam species was verified by Debbie Kay of the Suquamish Tribe. Five individual clams of each species were collected, rinsed with site seawater, placed in a labeled baggie, and placed on ice in the cooler in accordance with the QAPP. Five T. capax were collected at the second location and Debbie Kay of the Tribe made a decision that the T. capax would be sent for analysis as the dominant species of the site. Five T. capax were collected at the third location. No clams were collected within the eelgrass bed.

Since several holes were dug to collect sufficient clams of one species, numerous holes were found to have contamination present (photo 2) including free product. Mr. Orlean took photos of the collection process. All collection sites were GPS located (sample location map) for the general area and not at each specific hole within the site. The sample of T. nuttallii was placed in a separate location of the freezer by Manchester Laboratory staff and not analyzed because no other stations had enough T. nuttallii tissue mass for analysis. b. The sampling team moved to the Intertidal Cap location to continue collecting horse clams. Only one location was completed due to the incoming tide. Five T. capax were collected (photo 3). One clam from a second Intertidal Cap location was collected but the remaining four clams (for the full sample size) were collected on the second day due to time constraints. No sheen or free product was present in the sampled holes. Sampling ended for the day (~1500 hrs) and all collected clams were hand delivered to Manchester Laboratory under chain of custody in accordance with the QAPP. The sampling team returned to the Seattle District via the Southworth - Fauntleroy ferry at approximately 1900. 4. The sampling team returned to the site on 19 May 2011 at 0945 to finish collecting at the remaining locations. Neither Debbie Kay nor Howard Orlean was able to join the sampling team on this date. The weather was sunny and clear. a. Sampling began on the East Beach area using rakes due to the large cobbles underneath the sand layer where the clams were located. Five T. capax were collected from each of three locations (photo 4). The two locations towards the northern portion of East Beach had slight sheens (lesser degree than the sheens found at North Shoal) but no free product was present. Clams were collected within the eelgrass bed as it was not as dense as the bed at North Shoal and was located at a higher tidal location. Abundant Ulva sp. was present as can be seen in Photo 4. There was minimal Ulva sp. present at North Shoal. b. The sampling team then proceeded to the Intertidal Cap to finish collecting the necessary horse clams for a full sample (ended on 18 May due to the incoming tide). Five T. capax were collected from the third location and four T. capax were collected from the second location which was combined with the individual clam collected on the previous day. No sheen or product was observed at any of the locations in the Intertidal Cap area. The Intertidal Cap sediment was primarily composed of pea gravel (see photo 3). All clams were placed in the coolers with ice in accordance with the QAPP. 5. Sampling ended for the day (~1500 hrs) and all collected clams were hand delivered to Manchester Laboratory under chain of custody in accordance with the QAPP. The sampling team returned to the Seattle District via the Southworth - Fauntleroy ferry at approximately 1900.

Feel free to contact me with questions or comments.

Deborah Johnston CENWS-EN-GB-ET

Photo 1. T capax on white board and T. nuttallii (at upper left of photo) collected at North Shoal

Photo 2. Clam hole at North Shoal showing free product

Photo 3. T. capax collected at Intertidal Cap

Photo 4. T. capax collected at East Beach

QUALITY ASSURANCE MEMORANDUM FOR ORGANIC CHEMICAL ANALYSES

Date: September 13, 2011

To: Howard Orlean, EPS Office of Environmental Cleanup, USEPA Region 10

From: Chris Pace, Chemist Office of Environmental Assessment, USEPA Region 10 Laboratory

Subject: Quality Assurance Review for the Polycyclic Aromatic Hydrocarbon Analysis of Samples from the Wyckoff/ Eagle Harbor SF Site Clam Tissue Sampling, Bainbridge Island, WA Project

Project Code: WEH-021A Account Code: 2011T10P302DD2C10S1LA00

CC: Catherine Martin, USACE

The following is a quality assurance review of the data for polycyclic aromatic hydrocarbon analysis of samples from the above referenced site. The analyses were performed by the EPA Region 10 Laboratory utilizing method SW-846 8270D.

This review was conducted for the following samples:

11204400 11204401 11204402 11204403 11204404 11204406

11204407 11204408 11204409 11204410 11204411

1. Data Qualifications

Comments below refer to the quality control specifications outlined in the Laboratory‟s current Quality Assurance Manual, Standard Operating Procedures (SOPs) and the Quality Assurance Project Plan (QAPP). No excursions were required from the method Standard Operating Procedure.

The quality control measures which did not meet Laboratory/QAPP criteria are annotated in the title of each affected subsection with “Laboratory/QAPP Criteria Not Met”.

For those tests for which the EPA Region 10 Laboratory has been accredited by the National Environmental Laboratory Accreditation Conference (NELAC), all requirements of the current NELAC Standard have been met. Data Review Wyckoff clam/ WEH-021A Page 2 of 4

2. Sample Transport and Receipt

Upon sample receipt, no conditions were noted that would impact data quality.

3. Sample Holding Times

The concentration of an analyte in a sample or extract of a sample may increase or decrease over time depending on the nature of the analyte. The holding time maximum criteria applied for the extraction of tissue samples is one year from the time of collection. Extracts have a holding time maximum of 40 days from the time of preparation. All samples were extracted and analyzed within these criteria.

4. Sample Preparation

Samples were prepared according to the method/SOP.

5. Initial Calibration/Continuing Calibration Verification (CCV)

Initial calibration was performed on 08/10/11. Percent relative standard deviations (RSDs) of the calibration factors met the criteria of ≤15% or correlation coefficients met the criteria of ≥0.99.

The CCV for samples met the criteria for frequency of analysis and relative retention time (RRT) windows for all target and surrogate analytes. The relative response factors were ≥0.05 and the percent accuracies were 80- 120% of the true value.

6. LCS/LCSD

Laboratory Control Samples/Laboratory Control Sample Duplicates (LCS/LCSD) are generated to provide information on the accuracy and precision of the analytical method and the laboratory performance. The LCS/LCSD recoveries were within the criteria of 70-130% with a RPD of ≤30.

7. Blank Analysis

Method blanks were analyzed with each sample batch to evaluate the potential for laboratory contamination and effects on the sample results. Target analytes detected in samples were reported without qualification if the results were five times that of the blank(s). Detected sample results were qualified „U‟ if the results were below these criteria. The sample concentration or the sample quantification limit, whichever is greater, was reported as the qualified result.

8. Surrogate Spikes

Surrogate recoveries are used to help in the evaluation of laboratory performance on individual samples. All surrogate recoveries were within the criteria of 70-130%.

9. Matrix Spike/Matrix Spike Duplicate Analysis (MS/MSD) - “Laboratory/QAPP Criteria Not Met”

MS/MSD analyses are performed to provide information on the effects of sample matrices toward the analytical method. An MS/MSD analysis was performed using sample 11204400. The recoveries met the criteria of 70-130% with a relative percent difference (RPD) of ≤30 with the following exception.

The matrix spike of sample 11204400 resulted with >130% recovery for chrysene. The non-detected chrysene result in the native sample did not require qualification on this basis.

Data Review Wyckoff clam/ WEH-021A Page 3 of 4

10. Internal Standard Performance

Internal standards performance criteria ensure that GC/MS sensitivity and response are stable during every analytical run. The retention time variations of all internal standards were within 30 seconds of the continuing calibration standard. The percent areas of all the internal standards were within the specified 50% to 200% of the continuing calibration standard for all reported results.

11. Compound Quantitation

The initial calibration functions were used for calculations. Reported quantitation limits were based on the initial calibration standards and sample size used for the analysis. Detected analyte concentrations below the sample quantitation limits were qualified as estimated, “J”.

The quantitation limit for chrysene and indeno(1,2,3-cd)pyrene was increased by a factor of two due to matrix interference.

All manual integrations have been reviewed and found to comply with acceptable integration practices.

12. Identification

All of the compounds detected in the analyses were within the RRT windows, met the USEPA spectral matching criteria and/or were judged to be acceptable.

13. Data Qualifiers

All requirements for data qualifiers from the preceding sections were accumulated. Each sample data summary sheet and each compound was checked for positive or negative results. From this, the overall need for data qualifiers for each analysis was determined. In cases where more than one of the preceding sections required data qualifiers, the most restrictive qualifier has been added to the data.

The usefulness of qualified data should be treated according to the severity of the qualifier in light of the project‟s data quality objectives. Should questions arise regarding the data, contact Chris Pace at the Region 10 Laboratory, phone number (360) 871 - 8703.

Data Review Wyckoff clam/ WEH-021A Page 4 of 4

Qualifier Definition

U The analyte was not detected at or above the reported value.

J The identification of the analyte is acceptable; the reported value is an estimate.

UJ The analyte was not detected at or above the reported value. The reported value is an estimate.

R The presence or absence of the analyte can not be determined from the data due to severe quality control problems. The data are rejected and considered unusable. No value is reported with this qualification.

NA Not Applicable, the parameter was not analyzed for, or there is no analytical result for this parameter. No value is reported with this qualification.

QUALITY ASSURANCE MEMORANDUM FOR ORGANIC CHEMICAL ANALYSES

Date: September 14, 2011

To: Howard Orlean, EPS Office of Environmental Cleanup, USEPA Region 10

From: Chris Pace, Chemist Office of Environmental Assessment, USEPA Region 10 Laboratory

Subject: Quality Assurance Review for the Percent Lipids Analysis of Samples from the Wyckoff/ Eagle Harbor SF Site Clam Tissue Sampling, Bainbridge Island, WA Project

Project Code: WEH-021A Account Code: 2011T10P302DD2C10S1LA00

CC: Catherine Martin, USACE

The following is a quality assurance review of the data for percent lipids analysis of samples from the above referenced site. The analyses were performed by the EPA Region 10 Laboratory utilizing method SW-846 3541/ SOP Or_P009A.

This review was conducted for the following samples:

11204400 11204401 11204402 11204403 11204404 11204406

11204407 11204408 11204409 11204410 11204411

1. Data Qualifications

Comments below refer to the quality control specifications outlined in the Laboratory’s current Quality Assurance Manual, Standard Operating Procedures (SOPs) and the Quality Assurance Project Plan (QAPP). No excursions were required from the method Standard Operating Procedure.

The quality control measures which did not meet Laboratory/QAPP criteria are annotated in the title of each affected subsection with “Laboratory/QAPP Criteria Not Met”.

2. Sample Transport and Receipt

Upon sample receipt, no conditions were noted that would impact data quality.

3. Sample Holding Times

The concentration of an analyte in a sample or extract of a sample may increase or decrease over time depending on the nature of the analyte. The holding time maximum criteria applied for the extraction of frozen tissue samples is one year from the time of collection. Extracts have a holding time maximum of 40 days from the time of preparation. All samples were extracted and analyzed within these criteria.

4. Sample Preparation

Samples were prepared according to the method/SOP.

5. Blank Analysis

Procedural blanks were prepared with the samples to show potential contamination from the analytical procedure. The results from the blank analysis are required to be less than the minimum reporting limit (MRL). The procedural blanks did not contain a detectable percentage of lipids.

6. Duplicates

Duplicate sample analyses are performed to provide information on the precision, in the matrix of interest, of the analytical method. All percent lipids results which were above 5 times the MRL were within the 20% relative percent difference criteria.

7. Data Qualifiers

All sample results that fall below the MRL are assigned the value of the MRL and the “U” qualifier is attached.

The usefulness of qualified data should be treated according to the severity of the qualifier in light of the project’s data quality objectives. Should questions arise regarding the data, contact Chris Pace at the Region 10 Laboratory, phone number (360) 871 - 8703.