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SEDIMENT SAMPLING AND ANALYSIS PLAN

NPDES Permit WA0000124

Prepared for Nippon Dynawave Packaging Co. 3401 Industrial Way Longview, WA 98632

Prepared by

719 2nd Avenue Suite 700 Seattle, WA 98104

October 27, 2017

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

CONTENTS

LIST OF FIGURES ...... v LIST OF TABLES ...... vi ACRONYMS AND ABBREVIATIONS...... vii 1 INTRODUCTION AND BACKGROUND ...... 1-1 1.1 HISTORICAL AND CURRENT LAND USE ...... 1-1 1.2 REGULATORY FRAMEWORK ...... 1-2 1.3 PERMIT DISCHARGES ...... 1-3 1.4 PREVIOUS SEDIMENT INVESTIGATIONS ...... 1-4 1.4.1 NPDES Sediment Monitoring ...... 1-4 1.4.2 Dredged Material Characterizations, Mount Coffin Entrance Channel ...... 1-4 1.5 POTENTIAL CHEMICAL SOURCES ...... 1-6 2 OBJECTIVES AND DESIGN OF THE SEDIMENT INVESTIGATION ...... 2-1 2.1 SEDIMENT INVESTIGATION OBJECTIVES ...... 2-1 2.2 OUTFALL 001/002 PHYSICAL CHARACTERISTICS ...... 2-1 2.3 SAMPLING DESIGN ...... 2-1 2.4 PHYSICAL AND CHEMICAL CHARACTERIZATION ...... 2-2 2.5 BIOLOGICAL TESTING...... 2-2 3 FIELD METHODS ...... 3-1 3.1 SAMPLING VESSEL ...... 3-1 3.2 NAVIGATION AND POSITIONING ...... 3-1 3.3 SAMPLE COLLECTION TECHNIQUES ...... 3-1 3.4 DECONTAMINATION ...... 3-3 3.5 INVESTIGATION-DERIVED WASTE ...... 3-4 3.6 FIELD DOCUMENTATION ...... 3-4 4 SAMPLE HANDLING PROCEDURES ...... 4-1 4.1 SAMPLE LABELS AND STORAGE REQUIREMENTS...... 4-1 4.2 SAMPLE TRANSPORT AND CHAIN-OF-CUSTODY PROCEDURES ...... 4-1 5 LABORATORY ANALYTICAL METHODS ...... 5-1 5.1 CHEMICAL AND PHYSICAL ANALYSES ...... 5-1 5.1.1 Analytical Methods ...... 5-1 5.1.2 Chemical Limits of Detection ...... 5-3

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5.2 BIOLOGICAL ANALYSES AND TESTING ...... 5-3 5.2.1 Bioassay Reference Sediments ...... 5-4 5.2.2 Bioassay Laboratory Protocols ...... 5-4 5.2.3 General Biological Testing Procedures ...... 5-5 5.2.4 Bioassay-specific Procedures ...... 5-5 5.2.5 Bioassay Retest ...... 5-6 6 QUALITY ASSURANCE AND QUALITY CONTROL REQUIREMENTS ...... 6-1 6.1 QA/QC FOR CHEMICAL AND PHYSICAL ANALYSES ...... 6-1 6.1.1 Field QA/QC ...... 6-1 6.1.2 Laboratory QA/QC ...... 6-1 6.2 QA/QC FOR BIOLOGICAL TESTING ...... 6-2 6.3 TIMELINE FOR DATA REPORTING ...... 6-2 6.4 CHEMISTRY LABORATORY FINAL REPORT ...... 6-2 6.5 BIOASSAY LABORATORY FINAL REPORT ...... 6-3 6.6 DATA REVIEW, VERIFICATION, AND VALIDATION ...... 6-4 6.6.1 Physical and Chemical Data ...... 6-4 6.6.2 Biological Testing Results ...... 6-5 7 DATA ANALYSIS, RECORD KEEPING, AND REPORTING ...... 7-1 7.1 DATA ANALYSIS AND INTERPRETATION ...... 7-1 7.1.1 Sediment Chemistry and Physical Data ...... 7-1 7.1.2 Biological Testing Data ...... 7-1 7.2 RECORD KEEPING AND REPORTING PROCEDURES ...... 7-1 8 HEALTH AND SAFETY ...... 8-1 9 SCHEDULE ...... 9-1 9.1 FIELD SAMPLING ...... 9-1 9.2 ANALYTICAL AND QA RESULTS ...... 9-1 9.3 DATA REPORT ...... 9-1 10 REFERENCES ...... 10-1 Appendix A. Standard Operating Procedures Appendix B. Field Sampling Form Appendix C. Health and Safety Plan

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LIST OF FIGURES

Figure 1-1. Vicinity Site Map Figure 1-2. Permit WA0000124 Outfall Locations Figure 1-3. April 1990 NPDES Sampling Locations Figure 1-4. Ogden Beeman (1996) Sampling Locations Figure 1-5. NRC (2002) Sampling Locations Figure 1-6. Integral (2008) Sampling Locations, Mount Coffin Entrance Channel Figure 1-7. Integral (2015) Sampling Locations, Mount Coffin Entrance Channel and Salt Dock Figure 2-1. Proposed NPDES Sediment Monitoring Sampling Locations

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LIST OF TABLES

Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines Table 1-1b. April 1990 NPDES Permit Monitoring Sediment Bioassay Results: Hyalella azteca 10-day Mortality Table 1-1c. April 1990 NPDES Permit Monitoring Bioassay Results Evaluated Against Freshwater Biological Criteria Standards: Hyalella azteca 10-Day Mortality Table 1-2. 1996 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel Table 1-3. 2002 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel Table 1-4. 2008 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock Table 1-6. 2016–2017 Summary of Relevant Incident Information for the at Longview from Ecology Table 1-7 1999–2017 Spills to the Columbia River in the Vicinity of the NDP Property from National Response Center Database Table 2-1. Proposed Sampling Locations Table 4-1. Sample Storage Requirements Table 5-1. Chemical Parameters, Analytical Methods, and SMS Criteria Table 5-2. Performance Standards and Interpretive Criteria for Freshwater Bioassays Table 6-1. Laboratory QA/QC Requirements Table 6-2. Project Data Quality Objectives

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ACRONYMS AND ABBREVIATIONS

AKART all known, available, and reasonable methods of treatment ALS Analytical Laboratory Services ARI Analytical Resources Inc. ASTM American Society for Testing and Materials International bml below the mudline BMP best management plan CAS Columbia Analytical Services CDID Consolidated Diking Improvement District CFR Code of Federal Regulations COC chemical of concern CRD Columbia River Datum CSL cleanup screening level DMEF Lower Columbia River Dredged Material Evaluation Framework DMMU dredged material management unit Ecology State Department of Ecology EIM Environmental Information Management EPA U.S. Environmental Protection Agency GC/MS gas chromatography/mass spectrometry GIS geographic information system GPS global positioning system HASP health and safety plan Integral Integral Consulting Inc. MDL method detection limit NAD83 North American Datum 1983 NDP Nippon Dynawave Packaging NOAA National Oceanic and Atmospheric Administration NORPAC North Pacific Paper Co. NPDES National Pollutant Discharge Elimination System

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NRC Northern Resource Consulting PCB polychlorinated biphenyl PCDD/F polychlorinated dibenzo‐p‐dioxin and polychlorinated dibenzofuran PSEP Puget Sound Estuary Program QA/QC quality assurance and quality control RSET Regional Sediment Evaluation Team SAP sampling and analysis plan SCUM Sediment Source Control Standards User Manual SCUM II Sediment Cleanup Users Manual II SCO sediment cleanup objective SEF Sediment Evaluation Framework SMS Sediment Management Standards SOP standard operating procedure SQL sample quantitation limit SVOC semivolatile organic compound TEQ toxicity equivalent TMP thermo-mechanical pulp TOC total organic carbon TVS total volatile solids WET whole effluent toxicity

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1 INTRODUCTION AND BACKGROUND

This sampling and analysis plan (SAP) describes the sediment collection and testing procedures to be used to characterize sediments in the Columbia River adjacent to Outfalls 001/002 belonging to the Nippon Dynawave Packaging (NDP) property in Longview, Washington. This SAP has been prepared by Integral Consulting Inc. (Integral) in accordance with requirements of the NDP National Pollutant Discharge Elimination System (NPDES) permit WA0000124 Special Condition S15 following current Washington State Department of Ecology (Ecology) guidance. The permit states that the SAP must follow the guidance provided in the Sediment Source Control Standards User Manual (SCUM), Appendix B: Sediment Sampling and Analysis Plan (Ecology 2008); however, a note on Ecology’s web site dated April 2015 states that the document is no longer in use and has been replaced by Sediment Cleanup Users Manual II (SCUM II; Ecology 2015c). SCUM II Appendix A includes sampling guidance for NPDES permits under the State Sediment Management Standards (SMS). This sampling plan was prepared in accordance with SCUM (Ecology 2008) guidance and updated guidance from SCUM II (Ecology 2015c).

The NDP facility is located adjacent to Slaughters Channel, which is a relatively straight section of the Columbia River between approximately RM 63 and RM 66 (Figure 1-1). Information on current and historical land use, previous sediment investigations, and potential sources of chemicals to the Columbia River is described below.

1.1 HISTORICAL AND CURRENT LAND USE

The upland property included in the permit area comprises 700 acres and extends 3 miles along the Columbia River in Longview, Washington. Weyerhaeuser purchased the undeveloped property in the 1920s. The site has been used to manufacture a variety of forest products during its history. Products and production facilities have included sawmills, plywood production, log export, log debarking, a sulfite pulp mill, a batch kraft pulp mill, a Kamyr kraft pulp mill, a thermo-mechanical pulp (TMP) mill, a deink (recycle) pulp mill, wetlap pulp machine, newsprint, paperboard, corrugated medium, fine papers, and chlorine/caustic soda production.

Current site businesses operating under NPDES Permit 000012-4 include NDP’s bleached kraft pulp and liquid packaging plant; Weyerhaeuser’s log yard, truck shop, and sawmill and planer; and North Pacific Paper Co. (NORPAC) TMP and deink pulp mills and printing/publications paper machines. Until 2016, these businesses were owned and operated by Weyerhaeuser (NORPAC as a joint venture between Weyerhaeuser and Nippon Paper Industries). In 2016, the NDP facility was sold to Nippon Paper Industries, and NORPAC was sold to One Rock Capital Partners LLC.

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Other businesses currently active on the site include Axiall (a Westlake Company) producing chlorine and caustic; HASA Inc., producing consumer pool maintenance chemicals; and Specialty Minerals Inc., producing precipitated calcium carbonate. These other businesses are third party with land and services leased from NDP. NDP also provides services to several other third-party businesses adjacent to this site.

Annual production at the site includes roughly 370,000 tons of kraft pulp, 260,000 tons of paperboard, and 750,000 tons of NORPAC printing and publications papers. More than 350 million board feet of lumber is processed annually.

1.2 REGULATORY FRAMEWORK

NPDES permit WA0000124 was originally issued to Weyerhaeuser to discharge process wastewater, stormwater, and treated sanitary wastewater. Weyerhaeuser NR Company operated two separate wastewater treatment plants at its Longview facility that discharge to the Columbia River (Ecology 2014). The industrial wastewater treatment plant provides primary and secondary treatment for process wastewater and stormwater. The sanitary wastewater treatment plant provides anaerobic digestion, an overflow aeration lagoon, and disinfection for sanitary wastewater streams. The permit provides discharge limitations and monitoring requirements for process wastewater discharge through Outfalls 001/002 and stormwater through several other outfalls (Outfalls 006 through 011) associated with the site (Figure 1-2).

The NPDES permit was last renewed on October 15, 2014, and was modified on April 24, 2015 (Ecology 2015a). Compared to the previous permit, which had been issued by Ecology on May 11, 2004, the 2014 permit renewal included requirements for a stormwater pollution prevention plan; all known, available, and reasonable methods of treatment (AKART) analyses for water supply plant and certain outfalls; revised whole effluent toxicity (WET) testing requirements; and a cooling water intake report (Ecology 2014). It also revised or added certain effluent limits and established additional stormwater benchmarks. The 2015 modification replaced interim performance-based fecal coliform limits for Outfalls 003 and 004 (outfalls described in the following section) with a best management plan (BMP) approach, clarified monitoring requirements, corrected typographical errors, and improved the practicality of compliance reporting requirements (Ecology 2015d).

On July 16, 2016, Weyerhaeuser notified Ecology that it had transferred the permit to Nippon Paper Industries Co., Ltd (Leuzzi 2016, pers. comm.), which now owns the wastewater treatment plants. NDP is a wholly owned subsidiary of Nippon Paper Industries Co., Ltd. However, Weyerhaeuser and NORPAC retain responsibility for compliance with activities and effluent discharges that are under their ownership and control.

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1.3 PERMIT DISCHARGES

The Longview facility discharges water through five primary outfalls: 001, 002, 003, 004, and 005 (Ecology 2014). Three of these are under NDP ownership and control, and two are under Weyerhaeuser ownership and control:

• Outfalls 001 and 002 (NDP) are located on the western portion of the site and discharge non-contact cooling water, filter bed backwash, and industrial and sanitary wastewater treatment facility effluent (Ecology 2014). Outfall discharge may be transported upstream during the flood tide. • Outfall 003 (Weyerhaeuser) is located along Industrial Way. Stormwater from the southeastern portion of the site, dust control water, truck/equipment wash water, and area wash-up water collect in a detention pond prior to discharge into Consolidated Diking Improvement District (CDID) Ditch #3 (Ecology 2014). • Outfall 004 (Weyerhaeuser) is located northwest of Outfall 003 along Industrial Way. Stormwater from the central portion of the site, process cooling/HVAC water, dust control water, car/truck wash water, area wash-up water, and equipment wash water discharge by a v-notch weir prior to conveyance to CDID Ditch #3 (Ecology 2014). • Outfall 005 (NDP) is an internal outfall that is located at the sanitary wastewater treatment facility along the shore of the Columbia River. Outfall 005 effluent is piped into Outfall 001 and discharges into the Columbia River (Ecology 2014).

Minor stormwater outfalls at the facility receive no treatment prior to discharge. These outfalls include (Ecology 2014):

• Outfall 006, 001/002 Ditch (NDP), which discharges into the Columbia River • Outfall 007, Adjacent to Export Dock (Weyerhaeuser), which discharges into the Columbia River • Outfall 008, Cargo Dock (NORPAC), which discharges into the Columbia River • Outfall 009, Export Dock (Weyerhaeuser), which discharges into the Columbia River • Outfall 010, Raw Water Ditch (NDP), which discharges into the Columbia River • Outfall 011, RW Office (NDP), which discharges into CDID Ditch #3.

Multiple third-party facilities operating on or adjacent to the site discharge process and sanitary wastewaters to NDP for treatment in NDP’s process and sanitary wastewater treatment facilities, prior to discharge of treated wastewaters via Outfalls 001, 002, and 005. Discharges from these third-party facilities to NDP are regulated by Ecology under individual State Waste Discharge Permits (Ecology 2014). Details of the physical characteristics of Outfalls 001 and 002 are provided in Section 2.

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1.4 PREVIOUS SEDIMENT INVESTIGATIONS

Previous sampling to characterize sediment in the vicinity of the Outfalls 001 and 002 include NPDES sediment sampling conducted in April 1990 and dredged material characterization sampling prior to maintenance dredging in the Mount Coffin Access Channel.

1.4.1 NPDES Sediment Monitoring

Sediment sampling for NPDES permit monitoring was performed in April 1990. Data for this study are available from Ecology’s Environmental Information Management (EIM) database under Study ID WEYLONG, Weyerhaeuser Co. - Class 2 Inspection. Samples were collected from three locations (Figure 1-3); note that the coordinates provided for one of these samples places it at an upland location, which may be erroneous. Sample depth intervals are not provided in the EIM data set.

The results of the chemical and grain size analyses for these three samples are provided in Table 1-1a, along with current freshwater criteria. None of the detected concentrations exceeded current criteria, although the reporting limits for phenol and di-n-octyl phthalate (150 U and 160 U µg/kg) exceed current SMS sediment cleanup objective (SCO) criteria.

Bioassay testing (Hyalella azteca 10-day mortality) was conducted on sediments from the three sample locations, as well as a negative control (Table 1-1b). These results, as compared to current freshwater biological criteria standards (Ecology 2015c; Table B), show that sediments passed the biological criteria (Table 1-1c). Current guidance (Ecology 2015c) calls for tests on at least two species and at least three endpoints (including a growth endpoint), but those requirements appear to post-date the 1990 testing, which used a single endpoint for a single species.

1.4.2 Dredged Material Characterizations, Mount Coffin Entrance Channel

Sediment in the vicinity of Outfalls 001 and 002 was analyzed as part of four dredged material characterization events in the Mount Coffin Access Channel, which are briefly summarized in this section:

• Ogden and Beeman 1996 • NRC 2002 • Integral 2009 and 2015

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1.4.2.1 1996 (Ogden Beeman 1996)

Ogden Beeman & Associates, Inc. collected seven surface sediment samples using a Ponar grab sampler from the Entrance Channel on July 27, 1996 (Figure 1-4). Sampling and handling methods followed Puget Sound Dredged Disposal Analysis and Puget Sound Estuary Program (PSEP) guidelines. Sediments were analyzed by Analytical Laboratory Services (ALS; formerly Columbia Analytical Services [CAS])1 for grain-size distribution, total volatile solids (TVS), and total organic carbon (TOC) (Table 1-2). No chemical analyses were performed. Surface sediment samples ranged from 95 to 99 percent sand, and TOC was not detected at 0.05 percent. TVS ranged from 0.32 to 0.63 percent. Sediments were characterized as medium to coarse sand.

1.4.2.2 2002 (NRC 2002)

Northern Resource Consulting (NRC) collected surface sediment samples from the Entrance Channel using a petite Ponar grab sampler on September 30, 2002. Three grabs were collected within each dredged material management unit (DMMU; Figure 1-5) and composited into one sample per DMMU. A total of three samples were submitted for analysis. Collection methods were consistent with Lower Columbia River Dredged Material Evaluation Framework (DMEF) guidance (DMEF 1998). ALS analyzed the three samples for DMEF conventional parameters (including grain size) and chemicals of concern (COCs). Surface sediment samples ranged from 60 to 98 percent sand, and TOC was detected at 0.04 percent in Composite 3. (Results were not available for Composites 1 and 2.) Metals and organics were either not detected or detected at concentrations well below DMEF screening levels (Integral 2015) and current SMS freshwater criteria (Table 1-3).

1.4.2.3 2008 (Integral 2009)

Integral collected surface sediment samples from the Entrance Channel using a van Veen sampler on September 2–4, 2008. Four grab samples were collected within DMMUs 8 and 10 and 5 grab samples were collected within DMMU 9 (Figure 1-6). Grab samples were composited into one sample per DMMU; a total of three samples were submitted for analysis. ALS analyzed the three samples according to DMMP guidance and the Regional Sediment Evaluation Team’s (RSET’s) freshwater chemical screening values. ALS analyzed the samples for conventional parameters (including grain size) and COCs (Table 1-4). Polychlorinated dibenzo‐p‐dioxins and polychlorinated dibenzofurans (PCDD/Fs, or dioxins/furans) were analyzed at ALS for DMMU-8 due to its proximity to potential upland sources of dioxin. Surface sediment samples ranged from 0 to 1.63 percent fines, and TOC was detected at 0.05 and 0.08 percent in DMMU 8 and DMMU 10, respectively. Metals and organic compounds were either not detected or detected at concentrations below regional Sediment Evaluation Framework (SEF) freshwater screening levels and DMMP marine screening levels, and are

1 ALS purchased CAS in November 2011.

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below current SMS freshwater criteria. Dioxin and furan toxicity equivalent in DMMU 8 sediment was approximately 0.0135 ng/kg, well below the range of background concentrations available at that time for freshwater samples in the lower Columbia River.

During the same sampling event, Integral collected three subsurface sediment cores from the Entrance Channel (C8-Z, C9-Z, and C10-Z) to characterize the anticipated post-dredging surface. ALS analyzed samples for conventional parameters (including grain size) and COCs. Subsurface sediment samples ranged from 0.9 to 81.7 percent fines, and TOC was detected at 0.07 percent at C8-Z(0-1), 0.47 percent at C8-Z(1-2), 0.06 percent at C9-Z(0-1), 0.08 percent at C9- Z(1-2), 0.74 percent at C10-Z(0-1), and 0.95 percent at C10-Z(1-2). PCDD/Fs were analyzed at ALS in the DMMU-8 z-samples. Toxicity equivalent (TEQ) concentrations were approximately 0.0131 ng/kg and 0.00834 ng/kg in the samples tested.

Only dimethyl phthalate exceeded the RSET Screening Level 1 value in one sample: C10-Z(1-2) at 350 μg/kg. No other chemical concentrations exceeded SEF or DMMP guidelines. To confirm the exceedance in Sample C10-Z(1-2), the archived sediment sample was provided to a second laboratory (Analytical Resources Inc. [ARI] in Tukwila, Washington) for dimethyl phthalate analysis. Dimethyl phthalate was not detected in either sample analyzed at ARI and it is possible laboratory contamination played a role in its original detection at ALS.

1.4.2.4 2015 (Integral 2015)

Sediment from the vicinity of Outfalls 001 and 002 were sampled and analyzed as composite samples from the Entrance Channel (DMMUs 8, 9, and 10) and nearby Salt Dock (DMMU 52) in 2015 (Figure 1-7). One core was also collected from each DMMU to characterize the post- dredge surface. The samples were analyzed for the DMMP COCs, organotins, and petroleum hydrocarbons (diesel range and residual range). Results showed no exceedances of DMMP screening levels, and all materials were deemed suitable for in-water disposal. No biological testing was required. The analytical results from DMMUs 5, 8, 9, and 10 are shown in Table 1-5, along with current SMS freshwater criteria. The results showed no exceedances.

1.5 POTENTIAL CHEMICAL SOURCES

Potential sources of contaminants existing in the immediate vicinity of the NDP outfalls include:

• Stormwater runoff from the Weyerhaeuser log yard • Stormwater discharge • Stormwater from CDID #1

2 The Salt Dock DMMU was also sampled in separate events in 2005 and 2010; the 2005 samples were not analyzed for chemical parameters, and all results for the 2010 DMMU samples were below SEF freshwater SLs (Integral 2015).

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• Hazardous material releases from industrial sites adjacent to and upstream of the project area (i.e., Kapstone Paper and Packaging Corporation, the ) • Spills and accidental discharges from vessels • Lower Columbia River bedload that might bring long-duration contaminants from upstream material release locations.

Summaries of Ecology spill records (Ecology 2015b; Table 1-6) and the National Response Center database (Table 1-7) provide an indication of the types and frequency of chemical releases from vessels.

No significant spills in the vicinity of the Outfalls 001/002 area have occurred since the last dredging characterization was performed. Ecology (2015b) records show four reported spill events on the Columbia River at Longview in 2017, including a spill of approximately 1 cubic yard of calcined coke, and three reports of releases of unknown amounts of oil from vessels (Table 1-7). National Response Center records list the most recent spill in the area as having occurred in January 2016, where “a few drops” of hydraulic oil was observed leaking from equipment; no visible sheen was observed for this event (Table 1-7).

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2 OBJECTIVES AND DESIGN OF THE SEDIMENT INVESTIGATION

The objectives and approach for the sediment monitoring program are discussed in this section.

2.1 SEDIMENT INVESTIGATION OBJECTIVES

The proposed sampling approach detailed in this SAP is designed to fulfill the purpose of the permit requirement to characterize the nature and extent of chemical contamination and biological toxicity of sediment in the vicinity of Outfall 001/002 at the Longview site.

2.2 OUTFALL 001/002 PHYSICAL CHARACTERISTICS

Outfalls 001 and 002 are described as parallel, pile-supported, wooden stave pipes extending into the Columbia River at an angle of approximately 35 degrees relative to the shoreline (Ecology 2014). The outfalls are located on aquatic parcels leased by Weyerhaeuser from Washington State Department of Natural Resources; the leasehold ownership is currently being renegotiated (Wood 2017, pers. comm.).

Outfall 001 is 840 ft long and 54 in. in diameter, with a 320-ft submerged diffuser section at its offshore end. The acute mixing zone for Outfall 001 extends 22.8 ft in any direction from the diffuser; the horizontal distance of the Outfall 001 chronic mixing zone is 228 ft.

Outfall 002 is 1,490 ft long and 48 in. in diameter. It terminates with a 300-ft, submerged diffuser section. The acute mixing zone for Outfall 002 extends 22.1 ft in any direction. The horizontal distance of the chronic mixing zone is 221 ft. The end of east diffuser section (Outfall 001) and the beginning of the west diffuser section (Outfall 002) are separated by 300 ft.

Non-contact cooling water, filter bed backwash, and industrial wastewater streams combine at a junction box prior to discharge through Outfalls 001 and 002. Treated sanitary wastewater combines with the Outfall 001 effluent after the junction box (Ecology 2014). Total effluent discharge from Outfalls 001 and 002 averages 50 million gallons per day (Ecology 2014).

2.3 SAMPLING DESIGN

The proposed NPDES sediment monitoring sampling design includes 24 locations in the vicinity of Outfalls 001/002 (six upstream and six downstream of each diffuser) consistent with SCUM II guidance for multiport diffusers in a bidirectional flow environment (Figure 2-1). The samples closest to the outfalls are placed to be located at least 50 ft away from the outfall pipes to avoid potentially damaging the pipes during sampling. Samples of surface sediment from

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0-10 cm below the mudline (bml) will be collected for chemical analyses at each location. Adequate volumes of sediment for potential bioassay testing will also be collected at all locations. The coordinates, water depths, and sampling intervals for the proposed sampling locations are provided in Table 2-1.

Analyses of sediment samples will be based on a tiered approach. Initially, only the 12 stations closest to the outfall diffusers (“x” in Figure 2-1) will be submitted for chemical analyses per Table 8-1 of SCUM II; the bioassay samples and all other chemistry samples will be archived pending the results of the initial 12 chemistry samples. If any of the initial 12 chemistry samples analyzed contains concentrations exceeding the SMS freshwater SCOs, a bioassay sample associated with that side of the outfall will be submitted for toxicity testing.

Sampling must take place between August 15 and September 15, 2018 as stated in the NPDES permit.

2.4 PHYSICAL AND CHEMICAL CHARACTERIZATION

To characterize the nature and extent of chemical contamination and biological toxicity of sediment in the vicinity of Outfall 001/002, the samples selected for analysis will be analyzed for chemicals per the freshwater criteria shown in Table 8-1 of the SCUM II (Ecology 2015c). Additional analyses will include TOC, which will allow for comparison of sediment results to organic-carbon-normalized chemical criteria, and grain size. Details of the chemical and physical analytical methods are provided in Section 5.1.

Previous testing in the entrance channel near Outfalls 001 and 002 in 2008 showed polychlorinated biphenyl (PCB) Aroclors were not detected, and dioxin/furan TEQ concentrations were very low. In the 2015 dredged material characterization, PCB Aroclors were not detected in samples from the entrance channel near the outfalls, and were detected at only 3 µg/kg (estimated) near the Salt Dock about 0.3 mile upstream of the outfalls (Table 1-5). Dioxin/furan testing was not required by the DMMP agencies in sediment from the Entrance Channel or Salt Dock in 2015 because these compounds do not appear to be an issue in this area based on previous sampling results (Table 1-4). For these reasons, analysis of dioxins/furans and PCB congeners is not recommended for this monitoring event. PCB Aroclors will be analyzed.

2.5 BIOLOGICAL TESTING

As discussed in Section 2.3, if the results of the chemical analyses in sediment nearest the outfalls exceeds SCOs, indicating potential biological toxicity, a bioassay sample associated with that side of the outfall will be submitted for toxicity testing. Biological toxicity tests will be

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3 FIELD METHODS

This section describes the methods to be used during field sampling.

3.1 SAMPLING VESSEL

Surface sediment samples will be collected using a stainless-steel power grab deployed from a subcontracted sampling vessel. The vessel will be equipped with suitable deployment gear to properly collect acceptable sediment samples per the standard operating procedure (SOP) described in SOP SD-04 Surface Sediment Sampling (Appendix A). The vessel operator will be thoroughly familiar with accurate deployment and retrieval of the sampling gear. The subcontracted vessel and operator have yet to be determined.

3.2 NAVIGATION AND POSITIONING

Station positioning will be accomplished using the sampling vessel’s global positioning system (GPS). The GPS receiver will be situated over the sampling gear to achieve the most accurate position for each station. A positional fix will be recorded when the sampler impacts the seafloor. The positional accuracy of the GPS will be ± 2 m. Accuracy of the GPS will be verified at a horizontal control or navigation check point daily before sampling activities begin. Horizontal coordinates will be recorded as latitude and longitude, North American Datum 1983 (NAD 83) in decimal degrees to six decimal places (e.g., 46.127182°, -122.985601°).

Water levels will be periodically recorded from the National Oceanic and Atmospheric Administration (NOAA) tide station #9440422 located approximately 2.3 nautical miles upstream at a Port of Longview facility. Preliminary water level data referencing Columbia River Datum (CRD) are uploaded to the station’s web site every 6 minutes.3 The web site will be accessed via smartphone each time a station is occupied. Water depths at sampling locations will be measured by lead-line when samples are collected and will be converted to approximate mudline elevations referenced to CRD based on water level readings from the NOAA tide station.

3.3 SAMPLE COLLECTION TECHNIQUES

Sediment grab samples will be collected using a stainless-steel, 0.3 m3 power grab sampler. The grab sampler will be attached to a winch and cable and deployed from the research vessel. It will be lowered through the water column at a steady rate to prevent disturbance of the sediment surface on impact. Once the sampler is retrieved, overlying water will be siphoned off

3 http://tidesandcurrents.noaa.gov/waterlevels.html?id=9440422

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017 and sample acceptability assessed. A sample will be determined to be acceptable if the following conditions (PSEP 1986) are met:

• Sediment does not extrude from the upper surface of the sampler. • No water is leaking from the sampler (overlying water is present, indicating minimal leakage). • The overlying water is clear or not excessively turbid. • The sediment-water interface is intact and relatively flat, with no sign of channeling or sample washout. • The following penetration depths are achieved: Medium to coarse sand 4 to 5 cm Fine sand 6 to 7 cm Silt/clay 10 cm. • There is no evidence of sediment loss (incomplete closure of sampler, penetration at an angle, or tilting upon retrieval).

If the grab sample is unacceptable, the location will be slightly shifted and another attempt will be made to collect a new grab sample. After multiple attempts with no success, a decision will be made to abandon or move the location to obtain an acceptable grab sample.

If the sample is acceptable, the penetration depth and physical characteristics of the sediment sample (e.g., color, texture, odor) will be recorded on the sampling form (Appendix B). Descriptions will include the following information:

• Grab sampler penetration • Physical soil description (i.e., soil classification, density/consistency, color) • Odor (e.g., hydrogen sulfide, petroleum) • Visual stratification and lenses • Vegetation • Debris • Evidence of biological activity (e.g., detritus, shells, tubes, bioturbation, live or dead organisms) • Presence of oil sheen • Other distinguishing characteristics or features.

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Following description, sediments from the 0–10 cm bml sample interval will be placed in a decontaminated, stainless-steel bowl, with care taken to avoid collecting sediment touching the sides of the sampler. When all suitable sample material is in the bowl, it will be thoroughly mixed to a uniform color and texture prior to being placed in sample containers. For sulfide analysis, 2–44 mL of 2N zinc acetate will be placed in a 2-oz sampling jar. The sample sediment (approximately 5 g) will be placed in the jar and covered. The jar will be shaken vigorously to properly preserve the sample. The sulfide sample jar labels will indicate that zinc acetate has been added as a preservative.

Multiple grabs may be required to collect sufficient sample material for all analyses at a given station (Table 2-1). If so, sample material from all grabs at a station will be individually described before being composited and homogenized. A minimum of 6 L of homogenized sample will be prepared to provide adequate volume for all chemical analyses and potential bioassay testing (Table 2-1). All sample material will be taken from the same homogenate at a given location and placed into appropriate sample containers.

3.4 DECONTAMINATION

All sampling equipment that contacts sediment samples (i.e., stainless-steel bowls, utensils) will be decontaminated prior to use and between sampling locations. The decontamination procedure will consist of the following sequential rinses:

• Rinse with tap water or water supplied by the sampling vessel • Scrub with laboratory-grade detergent (i.e., Alconox) solution • Rinse with tap water • Rinse with distilled water.

The above procedure follows the general procedure outlined in SOP SD-01 Decontamination of Sediment Sampling Equipment (Appendix A), with the exception that nitric acid and solvent rinses will not be used. A solvent wipe will only be used in the unlikely event that evidence of contamination (e.g., sheen) remains on the sampling equipment following washing. If obvious residual contamination remains on the sampling equipment or is difficult to remove using the standard decontaminations procedures, an additional wipe with a small amount of hexane and a paper towel may be added, followed by a repeated wash and water rinse as above.

All decontaminated equipment will be wrapped in aluminum foil to prevent contamination when not in use. Any excess water or sediment remaining after processing will be returned to the river in the vicinity of the collection site. Any water or sediment spilled on the deck of the sampling vessel will be washed into the surface waters at the collection site before proceeding to the next station.

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The sampling crew will wear disposable nitrile gloves during sample processing (i.e., classification, subsampling, compositing, and filling sample containers). The gloves will be replaced or decontaminated between each sample station to prevent sample contamination.

The sampling area is an area of extreme concern for the invasive New Zealand mud snail. To aid in controlling the spread of this invasive species, final demobilization decontamination procedures will include drying, as specified in Standard Operating Procedures to Minimize the Spread of Invasive Species (see Summary of Field Gear Cleaning and Decontamination Procedure) provided in Attachment 7 of the health and safety plan (HASP; Appendix C).

3.5 INVESTIGATION-DERIVED WASTE

Any excess water or sediment remaining after processing will be returned to the river in the vicinity of the collection site. Any water or sediment spilled on the deck of the sampling vessel will be washed into the surface waters at the collection site before proceeding to the next station.

All disposable materials used in sample collection and processing, such as paper towels and disposable coveralls and gloves, will be placed in heavyweight garbage bags or other appropriate containers. Disposable supplies will be removed from the site by sampling personnel and placed in a normal refuse container for disposal at a solid waste landfill. Phosphate-free detergent-bearing liquid wastes from decontamination of the sampling equipment will be washed overboard or disposed into the sanitary sewer system as will rinsate from the decontamination process.

3.6 FIELD DOCUMENTATION

Field documentation will include a field log, sample photographs, sample collection logs, and chain-of-custody forms.

A field log will be maintained during all field sampling activities. Included in this log will be the following:

• Names of field supervisor and person(s) collecting and logging in the sample • Weather conditions • Date and time of collection of each sediment grab sample • The sample station number • Any observations relevant to sample collection or condition • Any deviations from the approved SAP.

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4 SAMPLE HANDLING PROCEDURES

This section discusses sample handling in the field following collection and homogenization.

4.1 SAMPLE LABELS AND STORAGE REQUIREMENTS

Pre-labeled jars for chemical, toxicity, and conventional parameter analyses will be filled with the homogenized sediment. Portions of each composite sample will be placed in appropriate containers obtained from the laboratory.

Each sample container will be clearly labeled with the project name, sample identification, type of analysis to be performed, date and time, and initials of person(s) preparing the sample. Samples will be stored on ice or refrigerated at approximately 4°C until delivered to the laboratory. The storage and holding time requirements for each type of analysis are outlined in Table 4-1.

4.2 SAMPLE TRANSPORT AND CHAIN-OF-CUSTODY PROCEDURES

When sampling is completed, sediment sample containers will be transported to the analytical laboratory. Specific sample shipping/delivery and chain-of-custody procedures will be as follows:

• Individual sample containers will be placed in sealed plastic bags, packed to prevent breakage, and transported on ice in a sealed cooler or other suitable container. • Ice will be placed in separate, sealed plastic bags in the cooler. • The shipping containers will be clearly labeled with sufficient information (name of project, time and date container was sealed, person sealing the container and consultant’s office name and address) to enable positive identification. • Information tracked in the chain-of-custody records will include sample identification, date and time of sample collection and receipt, analyses and analytical methods required, and signatures of each person in custody of the samples. • The coolers will be clearly labeled with sufficient information (name of project, time and date container was sealed, person sealing the cooler, and company name and address) to enable positive identification. • A sealed envelope containing signed and dated chain-of-custody forms will be enclosed in a plastic bag and taped to the inside lid of the cooler prior to shipping. • Each cooler containing sediment samples for analysis will be delivered to the laboratory within 24 hours of being sealed.

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• Samples will be packaged and shipped in accordance with U.S. Department of Transportation regulations, as specified in 49 Code of Federal Regulations (CFR) 173.6 and 49 CFR 173.24.

Upon receipt of samples at the laboratories, the shipping container seal will be broken and the receiver will record the condition of the samples. The laboratories will maintain chain-of- custody internally to track handling and final disposition of all samples.

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5 LABORATORY ANALYTICAL METHODS

This section describes the project requirements for the analytical laboratories for chemical and biological analyses, chemical target detection limits, and corrective actions.

5.1 CHEMICAL AND PHYSICAL ANALYSES

The sediment samples will be analyzed for the chemicals for which there are established SMS freshwater criteria as listed in Table 8-1 of the SCUM II guidance.

5.1.1 Analytical Methods

Laboratory testing procedures are discussed below and are listed in Table 5-1.

5.1.1.1 Conventional Parameters

Conventional parameters to be analyzed include ammonia, grain size, TOC, total solids, total sulfides, and TVS.

Ammonia will be analyzed by U.S. Environmental Protection Agency (EPA) Method 350.1. The method, originally developed for use in water samples, will be modified for sediment samples. Colorimetry will be used to determine ammonia concentrations.

Particle grain-size distribution for each composite sample will be determined in accordance with American Society for Testing and Materials International (ASTM) Method D-422 (modified). Wet sieve analysis will be used for the sieve sizes U.S. No. 4, 10, 20, 40, 60, 140, and 200. Hydrogen peroxide will not be used in preparations for grain size analysis. Hydrogen peroxide breaks down organic aggregates, and its use may provide an overestimation of the percent fines found in undisturbed sediment. The pipette procedure will be used for particle sizes finer than the 200 mesh to subdivide the silt-clay fraction.

TOC will be analyzed using a carbonaceous analyzer according to EPA Method 9060 (modified for sediments) protocols.

Total solids will be determined according to SM 2540G (APHA 2006) protocols. These results will be used to calculate analyte concentrations on a dry-weight basis and will also be reported in the database.

Total sulfide analysis will include distillation of the sulfide into a sodium hydroxide trap and analysis by colorimetry according to SM 4500-S2D (APHA 2011) protocols.

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TVS will be determined according to SM 2540G (APHA 2006). Samples will be heated to 550°C ± 10°C to measure the amount of organic matter present.

5.1.1.2 Metals

Strong acid digestion with nitric acid and hydrogen peroxide will be used to prepare samples for the analysis of metals other than mercury. Analysis will be completed by inductively coupled plasma/mass spectrometry, according to EPA Method 200.8.

Mercury samples will be extracted with aqua regia and oxidized using potassium permanganate. Analysis will be completed by cold vapor atomic absorption spectrometry, according to EPA Method 7471B.

5.1.1.3 Organometallic Compounds

Sample extractions for organometallic compounds (butyltins) will be completed using ALS SOP SOC-Butyl which uses an automated Soxhlet extraction followed by a Grignard reaction. Samples will be analyzed by gas chromatography/flame photometric detector. Extraction, derivatization, and analysis are based on techniques described in various papers (Unger et al. 1986; Krone et al. 1988)

5.1.1.4 Semivolatile Organic Compounds 4

Sample extractions for semivolatile organic compounds (SVOCs) will be completed using automated Soxhlet extraction (EPA Method 3541) and 10–40 g of sample (wet weight). Gel permeation chromatography cleanup (EPA Method 3640A) will be performed on the sample extract. SVOCs will be analyzed by gas chromatography/mass spectrometry (GC/MS), according to EPA Method 8270D.

5.1.1.5 Organochlorine Pesticides

Organochlorine pesticides will be extracted from samples using automated Soxhlet extraction procedures (EPA Method 3541). Florisil column cleanup (EPA Method 3620C) will be performed on the sample extract followed by sulfur removal by tetrabutylammonium sulfite procedures (EPA Method 3660B). Samples will be analyzed by gas chromatography/electron capture detection according to EPA Method 8081B.

4 Includes polycyclic aromatic hydrocarbons (PAHs), chlorinated hydrocarbons, phthalate esters, phenols, and miscellaneous extractables; detailed in Table 5-1.

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5.1.1.6 PCB Aroclors

PCB Aroclors will be extracted from samples using automated Soxhlet extraction procedures (EPA Method 3541). Acid cleanup (EPA Method 3665A) will be performed on the sample extract followed by Florisil (EPA Method 3620C) and finally sulfur removal by tetrabutylammonium sulfite procedures (EPA Method 3660B). Samples will be analyzed by GC/MS according to EPA Method 8082A.

5.1.1.7 Total Petroleum Hydrocarbons

Diesel- and residual-range petroleum hydrocarbons will be extracted from samples using methylene chloride and analyzed by a gas chromatograph equipped with a flame ionization detector, according to NWTPH-Dx (DEQ 2015) protocols.

5.1.2 Chemical Limits of Detection

The samples identified for analysis in Section 2.3 and Table 2-1 will be analyzed for all the analytes listed in Table 5-1, as discussed above. The preparation procedures, test methods, and sample quantitation limits (SQLs) to be achieved by the analytical laboratory in addition to the SMS Freshwater SCO and cleanup screening level (CSL) values are identified in Table 5-1. SQLs, also known as reporting limits, are established by the low standard of the initial calibration curve or low-level calibration check. SQLs are typically three to five times the method detection limits (MDLs). The MDL is a minimum concentration that can be measured and reported with 99 percent confidence that the chemical concentration is greater than zero. Detected analyte concentrations will be reported to the MDL, and both the MDL and the sample SQL will be reported for non-detects. SQLs of all COCs must be below SCO values. Failure to achieve detection limits at or below SCO values may result in a requirement to reanalyze or perform bioassays.

The testing laboratory will be specifically cautioned by NDP’s sediment monitoring contractor to make certain that it complies with the detection limit requirements. All reasonable means, including additional cleanup steps and method modifications, will be used to bring detection limits below SCO values. In addition, an aliquot (16 oz) of each sediment sample for analysis will be archived and preserved at -20°C for possible additional analysis.

5.2 BIOLOGICAL ANALYSES AND TESTING

Bioassay testing may be necessary if SMS chemical criteria are exceeded for any one station and biological confirmation is needed (Ecology 2015c). Results from the chemical testing will be obtained prior to the decision to conduct biological testing. If bioassay testing is required, the standard suite of bioassays will be conducted following SCUM II (Ecology 2015c) guidelines for freshwater bioassays.

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The hold time for bioassay samples is 8 weeks (56 days). To the maximum extent practicable, chemical results will be provided for biological testing decisions within 21 days of first sample collection. The remaining 35-day period will allow time for bioassay test preparation and execution, as well as time for retests, if necessary. The Ecology project manager will be kept informed of analytical progress to support biological testing decisions. The following sections address procedures associated with bioassay testing should they be required.

5.2.1 Bioassay Reference Sediments

Freshwater bioassay testing are based on a comparison to control treatments due to the lack of established reference sites in Washington State and the highly variable responses observed in reference sediment (Ecology 2015c). Therefore, no reference sediment will be collected.

5.2.2 Bioassay Laboratory Protocols

All sediment samples for bioassays will be stored at 4°C with no headspace, pending completion of chemical analyses and initiation of any required bioassay testing. All bioassay analyses, including retests, will commence within 56 days after collection of the first sediment sample to be analyzed. Chain-of-custody procedures will be maintained by the laboratory throughout biological testing.

Bioassay testing will be planned such that appropriate testing will be initiated as soon as possible after the first chemical results become available and the decision is made to conduct bioassays. This includes obtaining test organisms and control sediments in a timely manner. This approach will support the opportunity for any additional biological testing within the allowable 56-day holding period if such need arises. As initial chemistry data become available, the project manager and the bioassay laboratory representative will maintain close coordination with Ecology to expedite biological testing decisions.

The guidance (Ecology 2015c) requires the use of three toxicity tests that 1) use at least two species, 2) evaluate both acute and chronic endpoints, and 3) involve at least one sublethal endpoint (e.g., growth). The following freshwater bioassays will be conducted, if necessary, on the test sediment:

• Amphipod—Hyalella azteca 10-day mortality test • Midge—Chironomus dilutus 20-day mortality and growth test.

All biological testing will be in strict compliance with standard protocols established by ASTM (2010) and USEPA (2000). General biological testing procedures and specific procedures for each sediment bioassay are summarized in the following sections.

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5.2.3 General Biological Testing Procedures

The sections below discuss aspects of biological testing procedures.

5.2.3.1 Negative Controls

Negative control sediments are used in bioassays to check laboratory performance. Negative control sediments are clean sediments in which the test organism normally lives and which are expected to produce low mortality. The source of negative control sediments for any necessary bioassay tests will be Yaquina Bay, Oregon (Irissarri 2017, pers. comm.). All sediments proposed for negative controls for this project will be approved by Ecology before bioassay testing is initiated.

Performance standards for negative controls in all tests are identified in Section 6.2.

5.2.3.2 Replication

Eight laboratory replicates of test sediments and negative controls will be run for each freshwater bioassay (per ASTM and EPA guidance).

5.2.3.3 Positive Controls

A positive control will be run for each bioassay. Positive controls are chemicals known to be toxic to the test organism and provide an indication of the sensitivity of the particular organisms used in a bioassay.

5.2.3.4 Water Quality Monitoring

Water quality monitoring will be conducted for the amphipod and midge bioassays in accordance with the ASTM (2010) and USEPA (2000) protocols. Water quality monitoring in the 10-day amphipod test consists of daily measurements of temperature and dissolved oxygen; pH is measured on days 0 and 10. Water quality monitoring in the 20-day midge test consists of temperature measurements daily, dissolved oxygen and pH measurements three times per week, and conductivity measurements weekly. Hardness, alkalinity, ammonia N, conductivity, pH, dissolved oxygen, and temperature will be measured at the beginning and end of all tests. Monitoring will be conducted for all test sediments and negative controls. Parameter measurements must be within the limits specified for each bioassay. Measurements for each treatment will be made on a separate chemistry beaker set up to be identical to the other replicates within the treatment group, including the addition of test organisms.

5.2.4 Bioassay-specific Procedures

The sections below discuss bioassay-specific procedures.

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5.2.4.1 Amphipod 10-Day Survival Bioassay

This test measures the survival of amphipod Hyalella azteca after a 10-day exposure to the test sediment. Daily emergence data and the number of amphipods failing to rebury at the end of the test will be recorded, as well. Test performance standards are given in Table 5-2.

5.2.4.2 Midge 20-Day Survival/Growth Bioassay

This test measures the survival and growth of the midge Chironomus dilutus after a 20-day exposure to the test sediment. Test performance standards are given in Table 5-2.

5.2.5 Bioassay Retest

Any bioassay retests will be fully coordinated with, and approved by, Ecology.

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6 QUALITY ASSURANCE AND QUALITY CONTROL REQUIREMENTS

This section discusses the quality assurance/quality control (QA/QC) requirements for the project for physical, chemical, and bioassay data.

6.1 QA/QC FOR CHEMICAL AND PHYSICAL ANALYSES

Quality control samples will be prepared in the field and at the laboratories to monitor the bias and precision of the sample collection and analysis procedures.

6.1.1 Field QA/QC

Two field duplicate sediment samples and equipment wipe samples will be collected to fulfill field QA/QC requirements (a frequency of 1 in 20 samples collected). One of the two field duplicate samples will be analyzed in the initial round of chemical analyses; the second field duplicate and the equipment wipe samples will be archived for potential subsequent analyses if needed.

6.1.2 Laboratory QA/QC

Laboratory quality control procedures, where applicable, include initial and continuing instrument calibrations, standard reference materials, laboratory control samples, matrix replicates, matrix spikes, surrogate spikes (for organic analyses), and method blanks. Table 6-1 lists the type and frequency for laboratory QA/QC samples, and Table 6-2 summarizes the data quality objectives for precision, bias, and completeness for all analyses.

For the analysis of SVOCs, pesticides, PCBs, metals, and most conventional parameters, initial instrument calibrations are required before any samples are analyzed after each major disruption of equipment, and when ongoing calibration fails the acceptance criteria. Ongoing calibration is required before and after every 10 to 12 samples or every 12 hours (whichever is more frequent).

Surrogates are required for all organic analyses, for every sample, including matrix spike samples, blanks, laboratory control samples, and standard reference materials. Matrix spike and matrix spike duplicates are required for SVOCs, pesticides, and PCBs for every 20 samples received. Matrix spikes and laboratory duplicates are required for metals analyses and selected conventional parameters. Matrix triplicates are analyzed for grain size.

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All samples are diluted and reanalyzed if target compounds are detected at levels that exceed their respective established calibration ranges. Reanalyses are performed if surrogate, internal standard, or spike recoveries are out of control to demonstrate matrix effects.

6.2 QA/QC FOR BIOLOGICAL TESTING

Bioassay tests will be conducted by Northwestern Aquatic Sciences, which is accredited by Ecology for the bioassay tests that may be conducted for this project. Bioassay test QA/QC requirements are provided in the ASTM (2010) protocol and address facilities and equipment, test chambers and conditions, test organisms, water quality monitoring, food quality, test performance evaluation, etc. Ecology (2015c) guidance notes that particular attention should be paid to the following:

• Water quality conditions. The laboratory needs to ensure that water quality conditions remain within acceptable limits during the test procedure. Otherwise, it can contribute to observed toxicity and confound the actual toxicity results. In particular, temperature, dissolved oxygen, and pH need to stay within the specified control limits. • Negative and positive controls. Bioassays must be conducted using negative and positive controls. The SMS performance standards for control sediment are summarized in Table 5-2.

6.3 TIMELINE FOR DATA REPORTING

To the maximum extent practicable, all chemical results will be provided within 21 days of sampling to allow a timely decision for tiered chemical and biological testing.

Sediment samples reserved for potential bioassays or archived for possible future chemical analysis will be stored under chain-of-custody at temperatures shown in Table 4-1. All samples for physical, chemical, and biological testing will be maintained at the testing laboratory at appropriate temperatures and analyzed prior to the expiration times specified in Table 4-1.

6.4 CHEMISTRY LABORATORY FINAL REPORT

The chemistry laboratories will provide a data package for each sample delivery group or analysis batch that is comparable in content to a full Contract Laboratory Program package. It will contain all information required for a complete quality assurance review, including the following:

• A cover letter discussing analytical procedures and any difficulties that were encountered

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• A case narrative referencing or describing the procedures used and discussing any analytical problems and deviations from referenced methods and this SAP • Chain-of-custody and cooler receipt forms • A summary of analyte concentrations (to two significant figures, unless otherwise justified), method reporting limits, and MDLs • Laboratory data qualifier codes appended to analyte concentrations, as appropriate, and a summary of code definitions • Sample preparation, extraction, dilution, and cleanup logs • Instrument tuning data • Initial and continuing calibration data, including instrument printouts and quantification summaries, for all analytes • Results for method and calibration blanks • Results for all QA/QC checks, including surrogate spikes, internal standards, laboratory control samples, matrix spike samples, matrix spike duplicate samples, and laboratory duplicate or triplicate samples • Original data quantification reports for all analyses and samples • All laboratory worksheets and standards preparation logs • EIM-ready data • Comprehensive data package for Ecology (electronic submittal).

6.5 BIOASSAY LABORATORY FINAL REPORT

A written report will be prepared by the biological laboratory documenting all the activities associated with sample analyses. As a minimum, the following will be included in the report:

• Results of the laboratory bioassay analyses and QA/QC results. Raw data (including bench sheets) will be legible or typed. • All protocols used during analyses, including explanation of any deviation from standard protocols (ASTM 2010; USEPA 2000) and the approved SAP. • Chain-of-custody procedures, including explanation of any deviation from the identified protocols. • Location and availability of data, laboratory notebooks, and chain-of-custody forms. • Locations of bioassay test organism acquisition, and negative control sediment and water acquisition.

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As appropriate, this SAP may be referenced in describing protocols.

6.6 DATA REVIEW, VERIFICATION, AND VALIDATION

Procedures for data review, verification, and validation are discussed in the sections below.

6.6.1 Physical and Chemical Data

Field and laboratory data for this project will undergo a formal verification and validation process. All entries into the database will be verified. All errors found during the verification of field data, laboratory data, and the database will be corrected prior to release of the final data.

Data verification and validation will be conducted in accordance with Guidance on Environmental Data Verification and Data Validation (USEPA 2002). Data verification and validation for organic and inorganic compounds will be completed according to methods described in the EPA guidance for data review (USEPA 2017a,b) and Ecology QA1 guidance (PTI 1989). Control limits provided in Table 6-2 will be used during data validation to assess laboratory control samples, matrix spike samples, and matrix spike or laboratory duplicates. Data may be qualified as estimated if control limits for any other quality control sample or procedure do not meet laboratory control limits.

Results for field splits and replicates will be evaluated using a target control limit of 50 relative percent difference (RPD). Data will not be qualified as estimated if the target control limit is exceeded, but RPD results will be tabulated, and any exceedances will be discussed in the data report. Equipment blanks will be evaluated and data qualifiers will be applied in the same manner as method blanks, as described in the functional guidelines for data review (USEPA 2017a,b) and/or Ecology QA1 guidance (PTI 1989). Sample preparation blanks will be reviewed and qualified in accordance with the functional guidelines for data review (USEPA 2017a,b) and/or Ecology QA1 guidance (PTI 1989).

The lead contractor will complete data verification and validation as described above. All analyses will undergo a QA1 (PTI 1989) review, which comprises evaluation of field collection and handling, completeness, data presentation, and detection limits, and the acceptability of test results for method blanks, certified reference materials, analytical replicates, matrix spikes, and surrogate recoveries.

All data generated from the Puget Sound standard reference material (for PCB Aroclors) will be validated, equivalent to a Stage 2B validation.

The accuracy and completion of laboratory entries to the database will be verified at the laboratory when the electronic data deliverables (EDDs) are prepared and again as part of data validation. Ten percent of entries to the database from laboratory EDDs will be checked against

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laboratory data report packages. In addition to verification of field and laboratory data and information, data qualifier entries into the database will be verified. Any discrepancies will be resolved before the final database is released for use.

6.6.2 Biological Testing Results

The lead contractor’s bioassay QA/QC manager will ensure that the bioassay laboratory is using the proper test protocol, materials, and methods. The QA/QC manager will also confirm that the bioassay testing includes all proper control samples (negative and positive), and that the samples are handled, transported, and stored under the specified conditions. All testing will be done in a “blind” fashion, and all test containers will be randomized in the test system. The QA/QC manager will maintain contact with the laboratory during testing to ensure that water quality and testing conditions remain within acceptable limits. Any deviations noted at the end of the test will be evaluated to determine if successful tests have been conducted. If the testing conditions are deemed unacceptable for any reason, retesting will be initiated immediately.

Once the test laboratory finalizes the test data, the QA/QC manager will review all raw data, testing conditions, and water quality data to determine the quality and validity of the test results. A 100 percent check of data transcriptions from raw data sheets to electronic formats will be made. The laboratory will correct any errors or emissions.

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7 DATA ANALYSIS, RECORD KEEPING, AND REPORTING

This section discusses procedures for data analysis, record keeping, and reporting.

7.1 DATA ANALYSIS AND INTERPRETATION

Procedures for data analysis and interpretation for sediment chemistry and physical data, as well as biological testing data, are discussed below.

7.1.1 Sediment Chemistry and Physical Data

Results for the chemical and physical analyses of the surface sediment samples will be tabulated along with the SMS freshwater SCO and CSL criteria shown in Table 8-1 of the SCUM II guidance (Ecology 2015c). Organic carbon-normalized chemical data will also be tabulated against associated organic-carbon-normalized SCUM II chemical criteria (Ecology 2015c).

7.1.2 Biological Testing Data

Bioassay control and test sample results will be tabulated. The results for the control samples will be compared to the performance standards, while the test sample results will be evaluated against the interpretive criteria (Table 5-2).

7.2 RECORD KEEPING AND REPORTING PROCEDURES

Records will be maintained documenting all activities and data related to sample collection and laboratory analyses, as well as data verification and validation activities.

The lead contractor will prepare a written report documenting all activities associated with the collection, compositing, transportation, and chemical and biological analyses of samples. The laboratory reports will be included as appendices. The data report will be submitted in both hard copy and electronic format, and will include:

• A brief statement of the purpose of sampling. • A brief summary of the field sampling and laboratory analytical procedures, with any deviations from the SAP noted. • A general vicinity map showing the location of the site, sampling stations, and outfall/storm drain location(s). • Coordinate values (i.e., latitude and longitude) and their datum reported in an accompanying table for all stations, including the outfall diffuser beginning and end

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points. An electronic geographic information system (GIS) shapefile with projection details will be provided. • Tables summarizing the data results, as well as pertinent QA/QC data, including: – Station numbers – Sample numbers (corresponding to laboratory data sheets) – Sampling station water column depth – Sample collection date – Sampling interval (upper and lower sediment sampling depth in centimeters) – Sample replicates – Chemistry results converted to the same units as the criteria (e.g., mg/kg dry weight for metals, mg/kg TOC for nonionizable organics; parts per million) – Chemistry data for organic compounds should also be reported as dry weight concentrations (µg/kg dry weight; parts per billion) – Practical quantitation limits with appropriate qualifiers.

• A discussion of the interpretation of the results including any exceedances of the benthic criteria. • A map indicating area(s) exceeding the SMS freshwater SCO and CSL criteria.

Following approval of the data report, the project data will be uploaded to Ecology’s EIM database (electronic submittal only).

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8 HEALTH AND SAFETY

Fieldwork will be conducted in accordance with a site-specific HASP (Appendix C). The HASP identifies safety-related elements for the proposed fieldwork including key personnel roles, chemical and physical hazards, personal protective gear and safety protocols to be used, and emergency response procedures.

Project personnel, if Integral is selected as the lead contractor to perform the field sampling and data reporting, are listed in the following table:

Title Name Email Office Phone Cell Phone Project Manager Susan FitzGerald sfitzgerald@integral- (206) 957-0355 (206) 257-9002 corp.com

Site Safety Officer, Stefan Wodzicki swodzicki@integral- (360) 303-2708 (360) 303-2708 Field Lead corp.com

Corporate Health Matthew Behum mbehum@integral- (410) 573-1982 (443) 454-1615 and Safety Manager corp.com

Project Chemist Glenn Esler gesler@integral- (503) 943-3617 (503) 358-0157 corp.com

Project Ecologist Shannon Ashurst sashurst@integral- (206) 957-0373 (206) 878-2557 corp.com

Data Manager Gerald Palushock gpalushock@integral- (206) 957-0331 (206) 960-1884 corp.com

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

9 SCHEDULE

This section details the proposed schedule for sampling, data analyses, and reporting.

9.1 FIELD SAMPLING

It is anticipated that field sampling will be conducted between August 15 and September 15, 2018, as stated in the NPDES permit. Surface grab sample collection and processing are expected to be completed in 2 sampling days.

9.2 ANALYTICAL AND QA RESULTS

The proposed sampling and analytical program discussed in Sections 2 and 4 is summarized per location in Table 2-1. Samples will be submitted for chemical analysis based on a standard turnaround time of 3 weeks. Results of these analyses will be evaluated and shared with Ecology for decisions regarding potential analyses of archived samples.

All laboratory data for the initial round of analyses is expected to be received within 1 month following the collection of the last sample. Data validation and verification will be completed within 1 month following receipt of the final data from the laboratories. The analytical results will be tabulated and incorporated into the data report. All data comparison to SMS criteria will follow Ecology (2015c) guidance.

As soon as possible following receipt of the chemistry results, data will be reviewed to determine whether bioassay results are necessary. The bioassay laboratory needs 2 to 3 weeks’ notice prior to test initiation in order to obtain test organisms at the proper stage of development. Consequently, the decision regarding the need for bioassay testing will likely be made on unvalidated chemistry results. Upon receipt of the final report from the bioassay laboratory, Integral will perform a QA review of the test results (see Section 6.2). Should any retests be required (Section 5.2.5), they will be initiated as quickly as possible in order to stay within the sample holding times.

9.3 DATA REPORT

Per the permit requirements, the Sediment Data Report containing the results of the sediment sampling and analysis must be submitted to Ecology no later than November 1, 2018. Specifically, Special Condition S15.B requires that:

The Permittee must submit two paper copies and an electronic copy (preferably as a PDF)….In addition to a Sediment Data Report, the sediment chemical and

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

biological data must be submitted to Ecology’s EIM database (http://www.ecy.wa.gov/eim/). Ecology’s MyEIM tools must be used to confirm the accuracy of the submitted data (http://www.ecy.wa.gov/eim/MyEIM.htm).

The electronic copy of the Sediment Data Report will be prepared as a PDF file, which NDP will upload, certify, and submit to Ecology electronically via Secure Access Washington as a Scheduled Submittal on Ecology’s WQWebSubmittal web portal.

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10 REFERENCES

APHA. 2006. Standard Method 2540G. Total, fixed, and volatile solids in solid and semisolid samples. Standard Methods for the Examination of Water & Wastewater. American Public Health Association.

APHA. 2011. Standard Method 4500-S2—. Sulfide. Standard Methods for the Examination of Water & Wastewater. American Public Health Association.

ASTM. 2010. Standard. E1706-05: Standard test method for measuring the toxicity of sediment-associated contaminants with freshwater invertebrates. American Society for Testing and Materials International, West Conshohocken, PA.

DEQ. 2015. NWTPH-Dx. Semi-volatile petroleum products method for soil and water. Available at: http://www.deq.state.or.us/lab/techrpts/docs/nwtphDx.pdf. Oregon Department of Environmental Quality, Portland, OR.

DMEF. 1998. Dredged material evaluation framework guidance for the lower Columbia River management area. Draft. Cooperatively published by U.S. Army Corps of Engineers, Seattle District, Portland District, Northwestern Division; U.S. Environmental Protection Agency, Region 10; Washington State Department of Ecology; Oregon Department of Environmental Quality; and Washington State Department of Natural Resources, Seattle, WA.

Ecology. 2008. Sediment source control standards user manual (SCUM), Appendix B: Sediment sampling and analysis plan. Washington State Department of Ecology.

Ecology. 2014. Fact Sheet for NPDES Permit WA0000124. Weyerhaeuser Longview. Washington State Department of Ecology. October 15, 2014.

Ecology. 2015a. National Pollutant Discharge Elimination System Waste Discharge Permit No. WA0000124. Modified April 24, 2015. Available at: https://fortress.wa.gov/ecy/industrial/UIPermit/ViewDocument.aspx?DocumentId=215. Washington State Department of Ecology, Industrial Section. Olympia, WA.

Ecology. 2015b. Past spills and incidents database. http://www.ecy.wa.gov/programs/spills/incidents/main.html. Accessed July 21, 2015. State of Washington Department of Ecology, Olympia, WA.

Ecology. 2015c. Sediment cleanup users manual II: Guidance for implementing the cleanup provisions of the Sediment Management Standards, Chapter 173-204 WAC. Publication No. 12- 09-057. Available at: https://fortress.wa.gov/ecy/publications/documents/1209057.pdf. Washington State Department of Ecology. March.

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Ecology. 2015d. Weyerhaeuser Longview NPDES Permit WA0000124 Supplemental Fact Sheet. Washington State Department of Ecology. March 20.

Integral. 2009. Sediment characterization report. Prepared for Weyerhaeuser Company, Longview, WA. Integral Consulting Inc., Portland, OR. January 14.

Integral. 2015. Sediment characterization report. Prepared for Weyerhaeuser Company, Longview, WA. Integral Consulting Inc., Portland, OR. November 12.

Irissarri, G. 2017. Personal communication (e-mail to S. Ashurst, Integral Consulting Inc., Seattle, WA, dated September 28, 2017, regarding source of negative control bioassay test sediment). Northwestern Aquatic Sciences, Newport, OR.

Krone, C.A., D.W. Brown, D.G Burrows, R.G Bogar, S. Chan, and U. Varanasi. 1988. A Method for analysis of butyltin species and measurement of butyltins in sediment and English sole livers form Puget Sound. Marine Environmental Research 27:1–18.

Leuzzi, P. 2016. Personal communication (letter to P. Franke, Nippon Paper Industries Co., LTD, Seattle, WA, and K. Wigfield, Washington State Department of Ecology, Olympia, WA, dated July 21, 2016, regarding transfer of Weyerhaeuser NR Company NPDES permit.) Weyerhaeuser Law Department, Federal Way, WA.

NRC. 2002. Mt. Coffin shipping channel sediment characterization. Prepared for Weyerhaeuser Company, Longview, WA. Northern Resource Consulting, Inc., Longview, WA.

Ogden Beeman. 1996. Dredged material sediment characterization data report. Mt. Coffin Ship Access Channel in Columbia River. Prepared for Weyerhaeuser Company, Longview, WA. Ogden Beeman & Associates, Inc., Portland, OR.

PSEP. 1986. Recommended guidelines for measuring conventional sediment variables in Puget Sound. Prepared for EPA, Region 10, Seattle, Washington. Tetra Tech, Inc., Bellevue, WA.

PTI. 1989. Puget Sound dredged disposal analysis guidance manual: data quality evaluation for the Washington Department of Ecology, Olympia, WA. PTI Environmental Services, Bellevue, WA.

Unger, M.A, W.G. MacIntyre, J. Greaves, and R.J. Huggett. 1986. GC determination of butyltins in natural waters by flame photometric detection of hexane derivatives with mass spectrometric confirmation. Chemosphere 16(4):461–470.

USEPA. 2000. Methods for measuring the toxicity and bioaccumulation of sediment associated contaminants with freshwater invertebrates, Second Edition. EPA-600-R-99-064. U.S. Environmental Protection Agency, Washington, D.C.

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Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

USEPA. 2002. Guidance on environmental data verification and data validation. USEPA/240/R-02/004. U.S. Environmental Protection Agency, Office of Environmental Information, Washington, DC. November.

USEPA. 2017a. USEPA Contract Laboratory Program national functional guidelines for inorganic Superfund methods data review. USEPA-540-R-2017-001. U.S. Environmental Protection Agency, Office of Superfund Remediation and Technology Innovation, Washington, DC. January.

USEPA. 2017b. USEPA Contract Laboratory Program national functional guidelines for organic Superfund methods data review. USEPA-540-R-2017-002. U.S. Environmental Protection Agency, Office of Superfund Remediation and Technology Innovation, Washington, DC. January.

Wood, B. 2017. Personal communication (telephone conversation with S. FitzGerald, Integral Consulting Inc., Seattle, WA, on September 18, 2017, regarding site information). Nippon Dynawave Packaging Company, Longview, WA.

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FIGURES

2 6

M R

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Mount Coffin Ship Access Channel 4 M 6 P M 4 R 1 : C 1

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Figure 1-1. Vicinity Site Map L O N G V I E W

RW Office (Outfall 011) (!

Outfall 004 (!

Outfall 003 001/002 Ditch (Outfall 006) (! M (! P

0 Raw Water Ditch (Outfall 010) 3 :

1 Outfall 001 2 : Outfall 002 (!

1 (! Cargo Dock (Outfall 008) (! 7

1 (! 0 2 / 3 2 / 0 1 d x m . s l l a f t u o _ 2 _ 1 _ e r u Adjacent to Export Dock (Outfall 007) g i F \

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Figure 1-2. Permit WA0000124 Outfall Locations Outfall 002 !( S-2 !( Outfall 001 001/002 Ditch (Outfall 006) !( S-1

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Figure 1-3. April 1990 NPDES Sampling Locations Figure 1-4. Ogden Beeman (1996) Sampling Locations Figure 1-5. NRC (2002) Sampling Locations !(

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N DMMU Boundary _ 9 0 7 1 Aerial Source: Esri, NAIP (2016) C \ s t c e 0 100 200 j o r P \ Feet S I ¯ G \ : N

Figure 1-6. Integral (2008) Sampling Locations, Mount Coffin Entrance Channel !( 001/002 Ditch (Outfall 006)

!( 2015 Sample Location !( Outfall (approximate) DMMU Boundary 2015 Bathymetry Depth (ft) 51.08

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Figure 2-1. Proposed NPDES Sediment Monitoring Sampling Locations

TABLES

Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier Conventionals Particle/Grain Size, Gravel % ------2 6 1 Particle/Grain Size, Sand % ------98 94 99 Total organic carbon % ------0.14 0.13 0.05 Total solids % ------76 75 75 Total volatile solids % ------0.3 0.5 0.3 Metals Antimony mg/kg ------0.1 U 0.1 U 0.1 U Arsenic mg/kg 14 120 0.48 J 1.2 0.58 Beryllium mg/kg ------0.2 U 0.2 U 0.2 U Cadmium mg/kg 2.1 5.4 0.052 0.186 0.053 Chromium mg/kg 72 88 4.8 J 3.8 J 4.2 J Copper mg/kg 400 1,200 8.5 10.9 9.5 Lead mg/kg 360 >1,300 0.77 2.28 0.62 Mercury mg/kg 0.66 0.8 0.0083 0.013 0.006 J Nickel mg/kg 26 110 10.9 5.3 J 4 U Selenium mg/kg 11 >20 0.2 U 0.2 U 0.2 U Silver mg/kg 0.57 1.7 0.3 U 0.3 U 0.3 U Thallium mg/kg ------0.25 U 0.56 J 0.25 U Zinc mg/kg 3,200 >4,200 17.7 24.4 14.8 Organochlorine Pesticides .alpha.-Endosulfan µg/kg ------10 U 10 U 10 U .beta.-Endosulfan µg/kg ------10 U 10 U 10 U 4,4'-DDD µg/kg 310 860 10 U 10 U 10 U 4,4'-DDE µg/kg 21 33 10 U 10 U 10 U 4,4'-DDT µg/kg 100 8,100 10 U 10 U 10 U Aldrin µg/kg ------10 U 10 U 10 U alpha-BHC µg/kg ------10 U 10 U 10 U

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Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier beta-BHC µg/kg ------10 U 10 U 10 U Chlordane µg/kg ------10 U 10 U 10 U delta-BHC µg/kg ------10 U 10 U 10 U Dieldrin µg/kg 4.9 9.3 10 U 10 U 10 U Endosulfan Sulfate µg/kg ------10 U 10 U 10 U Endrin µg/kg ------10 U 10 U 10 U Endrin Aldehyde µg/kg ------10 U 10 U 10 U Heptachlor µg/kg ------50 U 50 U 50 U Heptachlor Epoxide µg/kg ------10 U 10 U 10 U Lindane (beta-Hexachlorocyclohexane) µg/kg 7.2 11 10 U 10 U 10 U Methoxychlor µg/kg ------10 U 10 U 10 U Toxaphene µg/kg ------500 U 500 U 500 U Volatile Organic Compounds 1,1,1-Trichloroethane µg/kg ------2 U 2 U 2 U 1,1,2,2-Tetrachloroethane µg/kg ------2 U 2 U 2 U 1,1,2-Trichloroethane µg/kg ------2 U 2 U 2 U 1,1-Dichloroethane µg/kg ------2 U 2 U 2 U 1,1-Dichloroethene µg/kg ------2 U 2 U 2 U 1,2,4-Trichlorobenzene µg/kg ------150 U 160 U 150 U 1,2-Dichlorobenzene µg/kg ------150 U 160 U 150 U 1,2-Dichloroethane µg/kg ------2 U 2 U 2 U 1,2-Dichloroethene µg/kg ------2 U 2 U 2 U 1,2-Dichloropropane µg/kg ------2 U 2 U 2 U 1,3-Dichlorobenzene µg/kg ------150 U 160 U 150 U 1,4-Dichlorobenzene µg/kg ------150 U 160 U 150 U 2,4-Dinitrotoluene µg/kg ------150 U 160 U 150 U 2,6-Dinitrotoluene µg/kg ------150 U 160 U 150 U 2-Hexanone µg/kg ------2 U 2 U 2 U

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Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier Acetone µg/kg ------10 UJ 2 U 11 UJ Benzene µg/kg ------2 U 2 U 2 U Bromoform µg/kg ------2 U 2 U 2 U Bromomethane µg/kg ------2 U 1 UJ 0.5 UJ Carbon Disulfide µg/kg ------0.4 J 0.5 J 0.4 J Carbon Tetrachloride µg/kg ------2 U 2 U 2 U Chlorobenzene µg/kg ------2 U 2 U 2 U Chlorodibromomethane µg/kg ------2 U 2 U 2 U Chloroethane µg/kg ------2 U 2 U 2 U Chloroform µg/kg ------2 U 1 J 2 U Chloromethane µg/kg ------2 U 0.2 UJ 0.2 UJ Cis-1,2-Dichloroethene µg/kg ------2 U 2 U 2 U Cis-1,3-Dichloropropene µg/kg ------2 U 2 U 2 U Dichlorobromomethane µg/kg ------2 U 2 U 2 U Ethylbenzene µg/kg ------2 U 2 U 2 U Methyl ethyl ketone µg/kg ------2 U 2 U 4 U Methyl isobutyl ketone µg/kg ------2 U 2 U 2 U Methylene Chloride µg/kg ------6 UJ 5 UJ 6 UJ Styrene µg/kg ------2 U 2 U 2 U Tetrachloroethene µg/kg ------2 U 2 U 2 U Toluene µg/kg ------2 U 2 U 2 U Total Xylenes µg/kg ------0.8 U 2 U 2 U Trans-1,3-Dichloropropene µg/kg ------2 U 2 U 2 U Trichloroethene µg/kg ------2 U 2 U 2 U Vinyl Acetate µg/kg ------2 U 2 U 2 U Vinyl Chloride µg/kg ------2 U 2 U 2 U

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Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier Semivolatile Organic Compounds PAHs 2-Methylnaphthalene µg/kg ------150 U 160 U 150 U Acenaphthene µg/kg ------150 U 160 U 150 U Acenaphthylene µg/kg ------150 U 160 U 150 U Anthracene µg/kg ------150 U 160 U 150 U Benz[a]anthracene µg/kg ------150 U 160 U 150 U Benzo(a)pyrene µg/kg ------150 U 160 U 150 U Benzo(ghi)perylene µg/kg ------150 U 160 U 150 U Chrysene µg/kg ------150 U 160 U 150 U Dibenzo(a,h)anthracene µg/kg ------150 U 160 U 150 U Fluoranthene µg/kg ------150 U 160 U 150 U Fluorene µg/kg ------150 U 160 U 150 U Indeno(1,2,3-cd)pyrene µg/kg ------150 U 160 U 150 U Naphthalene µg/kg ------150 U 160 U 150 U Phenanthrene µg/kg ------150 U 160 U 150 U Pyrene µg/kg ------150 U 160 U 150 U Total PAHs µg/kg 17,000 30,000 Phthalate esters Diethyl phthalate µg/kg ------150 U 160 U 150 U Di(2-ethylhexyl) phthalate µg/kg 500 22,000 150 U 160 U 150 U Dibutyl phthalate µg/kg 380 1,000 150 U 160 U 150 U Di-N-Octyl Phthalate µg/kg 39 >1,100 150 U 160 U 150 U Dimethyl phthalate µg/kg ------150 U 160 U 150 U Butyl benzyl phthalate µg/kg ------150 U 160 U NA Phenols 2,4,5-Trichlorophenol µg/kg ------750 U 760 U 740 U 2,4,6-Trichlorophenol µg/kg ------150 U 160 U 150 U

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Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier 2,4-Dichlorophenol µg/kg ------150 U 160 U 150 U 2,4-Dimethylphenol µg/kg ------150 U 160 U 150 U 2,4-Dinitrophenol µg/kg ------750 U 760 U 740 U 2-Chlorophenol µg/kg ------150 U 160 U 150 U 2-Nitrophenol µg/kg ------150 U 160 U 150 U 4,6-Dinitro-2-Methylphenol µg/kg ------750 U 760 U 740 U 4-Chloro-3-Methylphenol µg/kg ------150 U 160 U 150 U o-Cresol µg/kg ------150 U 160 U 150 U p-Cresol µg/kg 260 2,000 150 U 160 U 150 U Pentachlorophenol µg/kg 1,200 >1,200 750 U 760 U 740 U Phenol µg/kg 120 210 150 U 160 U 150 U Miscellaneous extractables 2-Nitroaniline µg/kg ------750 U 760 U 740 U 3,3'-Dichlorobenzidine µg/kg ------NA NA 150 U 4-Chloroaniline µg/kg ------150 U 160 U 150 U 4-Chlorophenyl-Phenylether µg/kg ------150 U 160 U 150 U 4-Nitroaniline µg/kg ------750 U 760 U 740 U Benzoic Acid µg/kg 2,900 3,800 750 U 760 U 740 U Bis(2-Chloroethoxy)Methane µg/kg ------150 U 160 U 150 U Bis(2-Chloroethyl)Ether µg/kg ------150 U 160 U 150 U Bis(2-chloroisopropyl) ether µg/kg ------150 U 160 U 150 U Dibenzofuran µg/kg 200 680 150 U 160 U 150 U Hexachlorobenzene µg/kg ------150 U 160 U 150 U Hexachlorobutadiene µg/kg ------150 U 160 U 150 U Hexachlorocyclopentadiene µg/kg ------310 U 320 U 310 U Hexachloroethane µg/kg ------150 U 160 U 150 U Isophorone µg/kg ------150 U 5 J 3 J m-Nitroaniline µg/kg ------750 U 760 U 740 U

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Table 1-1a. April 1990 NPDES Permit Monitoring Sediment Chemistry Analytical Results Compared to DMMP Freshwater Guidelines

Location ID: WEYLONGS-1 WEYLONGS-2 WEYLONGS-3 SMS Freshwater a 15-8035 15-8037 15-8039 Analyte Units SCO CSL Result Qualifier Result Qualifier Result Qualifier Nitrobenzene µg/kg ------150 U 160 U 150 U N-Nitrosodi-n-propylamine µg/kg ------150 U 160 U 150 U N-Nitrosodiphenylamine µg/kg ------150 U 160 U 150 U PCN-002 µg/kg ------150 U 160 U 150 U PBDE-015 µg/kg ------150 U 160 U 150 U PCBs Aroclor 1016 µg/kg ------50 U 50 U 50 U Aroclor 1221 µg/kg ------50 U 50 U 50 U Aroclor 1232 µg/kg ------50 U 50 U 50 U Aroclor 1242 µg/kg ------50 U 50 U 50 U Aroclor 1248 µg/kg ------50 U 50 U 50 U Aroclor 1254 µg/kg ------50 U 50 U 50 U Aroclor 1260 µg/kg ------50 U 50 U 50 U Aroclor 1262 µg/kg ------50 U 50 U 50 U Aroclor 1268 µg/kg ------50 U 50 U 50 U Total PCB Aroclors µg/kg 110 2,500 50 U 50 U 50 U Notes: a SMS Freshwater screening levels from Table 8-1 (SCUM II 2015/2017). Shaded cells indicate concentrations above the freshwater SCO. --- = no criteria CSL = cleanup screening level DMMP = Dredged Material Management Program NPDES = National Pollutant Discharge Elimination System PAH = polycyclic aromatic hydrocarbon PCB = polychlorinated biphenyl SCO = sediment cleanup objective SMS = Sediment Management Standards (Washington State Guidelines) J = estimated concentration U = indicates the target analyte was not detected at the reported concentration UJ = indicates the target analyte is considered not detected at the reported value, and the associated numerical value is an estimated value.

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Table 1-1b. April 1990 NPDES Permit Monitoring Sediment Bioassay Results: Hyalella azteca 10-day Mortality

Lab Initial Survived Mortality Location ID Sample ID Replicate (# Individuals) (# Individuals) (# Individuals) % Survival % Mortality — Negative Control 1 15 15 0 100 0 — Negative Control 2 15 13 2 87 13 — Negative Control 3 15 15 0 100 0 — Negative Control 4 15 13 2 87 13 — Negative Control 5 15 12 3 80 20 Mean 15 14 1 91 9 S-1 15-8035 1 15 14 1 93 7 S-1 15-8035 2 15 12 3 80 20 S-1 15-8035 3 15 14 1 93 7 S-1 15-8035 4 15 13 2 87 13 S-1 15-8035 5 15 15 0 100 0 Mean 15 14 1 91 9 S-2 15-8037 1 15 14 1 93 7 S-2 15-8037 2 15 13 2 87 13 S-2 15-8037 3 15 13 2 87 13 S-2 15-8037 4 15 14 1 93 7 S-2 15-8037 5 15 13 2 87 13 Mean 15 13 2 89 11 S-3 15-8039 1 15 14 1 93 7 S-3 15-8039 2 15 13 2 87 13 S-3 15-8039 3 15 13 2 87 13 S-3 15-8039 4 15 15 0 100 0 S-3 15-8039 5 15 14 1 93 7 Mean 15 14 1 92 8 Source: Ecology's EIM database (Study ID WEYLONG, Weyerhaeuser Co. - Class 2 Inspection).

Notes: Ecology = Washington State Department of Ecology EIM = Environmental Information Management NPDES = National Pollutant Discharge Elimination System

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Table 1-1c. April 1990 NPDES Permit Monitoring Bioassay Results Evaluated Against Freshwater Biological Criteria Standards: Hyalella azteca 10-Day Mortality

Biological Test Performance Standard Endpoint / a b c c Sample ID Control Reference SCO CSL Freshwater Biological Criteria Standards H. azteca M < 20% M < 25% M – M > 15% M – M > 25% 10-day Mortality C R T C T C

April 1990 NPDES Bioassay Results M = 9% Negative Control C Not Applicable Not Applicable Not Applicable (Pass)

MT – MC = MT – MC = S-1 Not Applicable Not Applicable 9% – 9% = 0% 9% – 9% = 0% (Pass) (Pass)

MT – MC = MT – MC = S-2 Not Applicable Not Applicable 11% – 9% = 2% 11% – 9% = 2% (Pass) (Pass)

MT – MC = MT – MC = S-3 Not Applicable Not Applicable 8% – 9% = -1% 8% – 9% = -1% (Pass) (Pass)

Source (Standards): Ecology. 2015. Sediment Cleanup Users Manual II. Publication No. 12-09-057. March. Source (Data): Ecology's EIM database (Study ID WEYLONG, Weyerhaeuser Co. - Class 2 Inspection).

Notes: Mean results (5 replicates) used for this evaluation, by location or negative control. Refer to Table 1-1b. M = Mortality; C = Control; R = Reference; T = Test CSL = cleanup screening level Ecology = Washington State Department of Ecology EIM = Environmental Information Management NPDES = National Pollutant Discharge Elimination System SCO = sediment cleanup objective

a These tests and parameters were developed based on the most updated American Society for Testing and Materials (ASTM International) protocols.

b Reference performance standards are provided for sites where Ecology has approved a freshwater reference sediment site(s) and reference results will be substituted for control in comparing test sediment to criteria.

c An exceedance of the sediment cleanup objective and cleanup screening level requires statistical significance at p = 0.05.

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Table 1-2. 1996 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

Analyte Unit MRL 1c 2c 3c 4c 5c 6c 7c Conventionals Total solids percent NA NA NA NA NA NA NA Total volatile solids percent 0.44 0.38 0.42 0.34 0.32 0.39 0.63 Preserved total solids percent NA NA NA NA NA NA NA Total organic carbon percent ND ND ND ND ND ND ND Total sulfides mg/kg 0.05 NA NA NA NA NA NA NA N-ammonia mg/kg NA NA NA NA NA NA NA Gravel percent 3.78 0.35 0.12 0.15 0.91 1.26 2.48 Very coarse sand percent 4.94 2.23 0.99 1 3.8 1.55 4.27 Coarse sand percent 25.6 20.9 8.9 10.5 15.6 7.96 25.8 Medium sand percent 59.8 73.5 83.4 77.6 74.5 77.6 63 Fine sand percent 5.79 6.28 10.3 11.3 8.18 13.9 6.95 Very fine sand percent 0.08 0.05 0.16 0.12 0.07 0.32 0.12 Silt (4 to 8 phi) percent 0.03 0.01 0.05 0 -0.01 0.03 -0.1 Clay (>8 phi) percent 0.16 0.17 0.15 0.18 0.21 0.22 0.19

Notes: Grain size data represents percent of total weight recovered.

MRL = method reporting limit from data package NA = not analyzed ND = not detected at or above MRL TOC = total organic carbon TVS = total volatile solids

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Table 1-3. 2002 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater DMMU 1 DMMU 2 DMMU 3 Analyte Unit SCO CSL MRL MDL 1a,1b,1c MRL MDL 2a,2b,2c MRL MDL 3a,3b,3c Conventionals Total solids percent ------NA NA NA Total volatile solids percent ------0.1 0.1 1.2 0.1 0.1 0.4 0.1 0.1 0.4 Preserved total solids percent ------NA NA NA Total organic carbon percent ------0.05 NA 0.05 NA 0.05 NA Total sulfides mg/kg 39 61 0.8 0.2 0.5 J 0.8 0.2 0.2 U 0.8 0.2 0.2 U N-ammonia mg/kg 230 300 0.4 0.2 11.2 0.4 0.2 0.2 U 0.4 0.2 0.4 Gravel percent ------100 97.8 99.2 Very coarse sand percent ------99.7 90 95.6 Coarse sand percent ------98.4 67.2 80.9 Medium sand percent ------87.7 19.7 21.2 Fine sand percent ------54 2.4 2.7 Very fine sand percent ------40.2 2 2.5 0.074 mm percent ------43.4 1.5 4.7 0.005 mm percent ------5 0 0 0.001 mm percent ------0 0 0 Metals Antimony mg/kg ------0.05 0.05 0.06 0.06 0.06 0.06 U 0.07 0.07 0.07 U Arsenic mg/kg 14 120 0.50 0.10 1.1 0.6 0.1 0.8 0.7 0.1 0.9 Cadmium mg/kg 2.1 5.4 0.05 0.02 0.14 0.06 0.02 0.06 0.07 0.03 0.06 B Chromium mg/kg 72 88 0.52 0.30 6.38 0.59 0.04 4.47 0.7 0.04 3.9 Copper mg/kg 400 1200 0.10 0.04 13.4 0.12 0.05 9.87 0.14 0.06 9.92 Lead mg/kg 360 >1,300 0.05 0.03 2.55 0.06 0.04 0.94 0.07 0.04 0.88 Mercury mg/kg 0.66 0.8 0.007 0.004 0.027 0.017 0.009 0.009 U 0.018 0.009 0.009 U Nickel mg/kg 26 110 0.52 0.02 6.85 0.59 0.02 7.85 0.7 0.03 7.21 Selenium mg/kg 11 >20 NA NA NA Silver mg/kg 0.57 1.7 0.02 0.01 0.05 0.02 0.01 0.03 0.03 0.01 0.04 Zinc mg/kg 3200 >4,200 0.50 0.10 30.6 0.6 0.1 21.2 0.7 0.1 39.6 Polycyclic Aromatic Hydrocarbons (PAHs) 1-Methylnaphthalene μg/kg ------Naphthalene μg/kg ------13 1.7 2.4 J 15 1.9 ND U 14 1.9 ND U Acenaphthylene μg/kg ------13 1.8 ND U 15 2.1 ND U 14 2 ND U Acenaphthene μg/kg ------13 1.3 ND U 15 1.5 ND U 14 1.4 ND U Fluorene μg/kg ------13 2.2 ND U 15 2.5 ND U 14 2.4 ND U Phenanthrene μg/kg ------13 1.7 8 J 15 1.9 ND U 14 1.9 ND U Anthracene μg/kg ------13 1.8 3.4 J 15 2.1 ND U 14 2 ND U 2-Methylnaphthalene μg/kg ------13 1.5 ND U 15 1.8 ND U 14 1.7 ND U Low Molecular Weight PAH μg/kg ------NA NA NA Fluoranthene μg/kg ------13 2.8 14 15 3.2 ND U 14 3.1 ND U Pyrene μg/kg ------13 1.7 14 15 1.9 ND U 14 1.9 ND U Benzo(a)anthracene μg/kg ------13 1.8 6.5 J 15 2.1 ND U 14 2 ND U Chrysene μg/kg ------13 1.8 10 J 15 2.1 ND U 14 2 ND U Benzo(b)fluoranthene μg/kg ------13 3.2 11 J 15 3.6 ND U 14 3.5 ND U Benzo(k)fluoranthene μg/kg ------13 3.2 ND U 15 3.6 ND U 14 3.5 ND U Benzo(b+k)fluoranthene μg/kg ------NA NA NA Benzo(a)pyrene μg/kg ------13 2.0 7 J 15 2.3 ND U 14 2.3 ND U

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Table 1-3. 2002 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater DMMU 1 DMMU 2 DMMU 3 Analyte Unit SCO CSL MRL MDL 1a,1b,1c MRL MDL 2a,2b,2c MRL MDL 3a,3b,3c Indeno(1,2,3-cd)pyrene μg/kg ------13 2.4 5.9 J 15 2.8 ND U 14 2.7 ND U Dibenzo(a,h)anthracene μg/kg ------13 2.8 ND U 15 3.2 ND U 14 3.1 ND U Benzo(g,h,i)perylene μg/kg ------13 2.9 6 J 15 3.3 ND U 14 3.3 ND U High Molecular Weight PAH μg/kg ------NA NA NA Total PAHs 17000 30000 Chlorinated Hydrocarbons 1,3-Dichlorobenzene μg/kg 6.2 0.89 ND U 7 1.1 ND U 6.7 0.99 ND U 1,4-Dichlorobenzene μg/kg ------6.2 1.1 ND U 7 1.2 ND U 6.7 1.2 ND U 1,2-Dichlorobenzene μg/kg ------6.1 0.82 ND U 7 0.94 ND U 6.7 0.91 ND U 1,2,4-Trichlorobenzene μg/kg ------25 0.97 ND U 28 1.2 ND U 27 1.1 ND U Hexachlorobenzene μg/kg ------25 0.94 ND U 28 1.1 ND U 27 1.1 ND U Phthalates ------Dimethyl phthalate μg/kg 13 2.3 ND U 15 2.6 ND U 14 2.6 ND U Diethyl phthalate μg/kg ------13 4.4 ND U 15 5.1 ND U 14 4.9 ND U Di-n-butly phthalate μg/kg 380 1000 13 3.3 ND U 15 3.8 ND U 14 3.7 ND U Butylbenzyl phthalate μg/kg ------13 1.9 ND U 15 2.2 ND U 14 2.1 ND U Bis(2-ethylhexyl) phthalate μg/kg 500 22000 250 2.2 190 J 290 2.5 8.6 J 280 2.4 21 J Di-n-octyl phthalate μg/kg 39 >1,100 13 1.5 ND U 15 1.8 ND U 14 1.7 ND U Phenols Phenol μg/kg 120 210 38 2.4 ND U 43 2.8 4.4 J 42 2.7 3.9 J 2-Methylphenol μg/kg ------13 4.3 ND U 15 4.9 ND U 14 4.8 ND U 4-Methylphenol μg/kg 260 2000 13 3.7 ND U 15 4.2 ND U 14 4.1 ND U 2,4-Dimethylphenol μg/kg ------63 6.9 ND U 72 7.9 ND U 70 7.7 ND U Pentachlorophenol μg/kg 1200 >1,200 63 11.0 ND U 72 13 ND U 70 12 ND U Miscellaneous Organic Compounds Benzyl alcohol μg/kg ------13 4.7 ND U 15 5.3 ND U 14 5.2 ND U Benzoic acid μg/kg 2900 3800 250 120 ND U 290 140 ND U 280 140 ND U Dibenzofuran μg/kg 200 680 13 2 ND U 15 1.9 ND U 14 1.9 ND U Hexachloroethane μg/kg ------13 3 ND U 15 3.2 ND U 14 3.1 ND U Hexachlorobutadiene μg/kg ------13 1.8 ND U 15 2.1 ND U 14 2 ND U N-Nitrosodiphenylamine μg/kg ------13 2.8 ND U 15 3.2 ND U 14 3.1 ND U Pesticides Total of 4,4'-DDD, -DDE, -DDT μg/kg ------NA NA NA 4,4'-DDD μg/kg 21 33 1.3 0.2 NA 1.5 0.22 ND U 1.4 0.22 NA 4,4'-DDE μg/kg 310 860 1.3 0.31 NA 1.5 0.36 ND U 1.4 0.35 NA 4,4'-DDT μg/kg 100 8100 1.3 0.22 NA 1.5 0.25 ND U 1.4 0.24 NA Aldrin μg/kg ------1.3 0.63 NA 1.5 0.34 ND U 1.4 0.33 NA alpha-Chlordanes μg/kg ------1.3 1.3 NA 1.5 0.16 ND U 1.4 0.15 NA Total Chlordanes μg/kg ------NA NA NA cis-Chlordane μg/kg ------NA NA NA trans-Chlordane μg/kg ------NA NA NA cis-Nonachlor μg/kg ------NA NA NA trans-Nonachlor μg/kg ------NA NA NA Oxychlordane μg/kg ------NA NA NA Dieldrin μg/kg ------2.5 0.39 NA 1.5 0.44 ND U 1.4 0.43 NA Heptachlor μg/kg ------1.3 0.17 NA 1.5 0.2 ND U 1.4 0.19 NA

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Table 1-3. 2002 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater DMMU 1 DMMU 2 DMMU 3 Analyte Unit SCO CSL MRL MDL 1a,1b,1c MRL MDL 2a,2b,2c MRL MDL 3a,3b,3c gamma-Hexachlorocyclohexane μg/kg ------NA NA NA gamma-BHC (Lindane) μg/kg ------2.5 NA 1.5 1.5 ND Ui 1.4 0.34 NA Heptachlor epoxide μg/kg ------NA NA NA PCB Aroclors Aroclor 1016 μg/kg ------13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclor 1221 μg/kg ------25 1.1 ND U 29 1.2 ND U 28 1.2 ND U Aroclor 1232 μg/kg ------13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclor 1242 μg/kg ------13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclor 1248 μg/kg ------13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclor 1254 μg/kg ------13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclor 1260 μg/kg 13 1.1 ND U 15 1.2 ND U 14 1.2 ND U Aroclors μg/kg 110 2500 Aroclors mg/kg, OC ------Volatile Organic Compounds Trichloroethene (TCE) ------6.2 0.35 ND U 7 0.41 ND U 6.7 0.39 ND U Tetrachloroethene (PCE) ------6.2 0.39 ND U 7 0.45 ND U 6.7 0.44 ND U Ethylbenzene ------6.2 0.72 ND U 7 0.82 ND U 6.7 0.8 ND U m,p-Xylenes ------6.2 1.90 ND U 7 2.2 ND U 6.7 2.1 ND U Dioxin/furan TCDD toxicity ng/kg ------Notes: Silt and clay percent passing determined using hydrometer analysis. -- = no criteria CSL = cleanup screening level DMMU = dredged material management unit MDL = method detection limit ML = maximum level MRL = method reporting limit NA = not analyzed ND = not detected at or above MRL OC = normalized to the organic carbon content of the sample PCB = polychlorinated biphenyl SCO = sediment cleanup objective SMS = Sediment Management Standards

Qualifiers: B = value detected below calibration range J = estimated concentration U = the analyte was not detected at the quantitation limit shown

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Table 1-4. 2008 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater Parameter SCO CSL DMMU-8-C8 DMMU-9-C9 DMMU-10-C10 C8-Z(0-1) C8-Z(1-2) C9-Z(0-1) C9-Z(1-2) C10-Z(0-1) C10-Z(1-2) Conventionals Ammonia (mg/kg) 230 300 0.006 U 1.6 0.006 U ------23.8 123 Grain size (% fines) ------1.15 0 1.63 0.9 27 1.95 1.39 9.27 81.7 Total organic carbon (%) ------0.05 0.02 U 0.08 0.07 0.47 0.06 0.08 0.74 0.95 Total solids (%) ------75.5 67.6 67.9 73.3 73.5 80.3 77.3 76.0 69.8 Total volatile solids (%) ------0.5 0.5 0.56 Total sulfides (mg/kg) 39 61 0.8 U 0.9 U 0.9 U ------Metals (mg/kg dw) Antimony ------0.04 U 0.05 U 0.05 U 0.05 U 0.04 U 0.04 U 0.04 U 0.04 UJ 0.1 Arsenic 14 120 0.54 B 0.61 B 0.59 B 0.49 B 1.09 0.51 B 0.45 B 0.63 2.12 Cadmium 2.1 5.4 0.022 B 0.028 0.033 0.024 0.06 0.02 B 0.025 0.041 0.173 Chromium 72 88 1.89 2.59 2.33 2.24 5.8 2 2.42 3.06 12.6 Copper 400 1200 6.35 7.74 7.04 6.97 11.2 6.93 6.87 8.21 16.2 Lead 360 >1,300 0.74 0.85 0.87 0.8 2.36 0.74 0.79 1.09 6.87 Mercury 0.66 0.8 0.002 U 0.002 U 0.003 U 0.002 U 0.011 B 0.002 U 0.003 B 0.008 B 0.024 Nickel 26 110 4.01 5.8 5.72 4.52 7.04 4.76 5 5.66 13.1 Selenium 11 >20 0.4 U 0.5 U 0.5 U 0.5 U 0.4 U 0.4 U 0.4 U 0.4 U 0.5 U Silver 0.57 1.7 0.03 0.03 0.03 0.02 U 0.03 0.02 U 0.02 U 0.07 0.1 Zinc 3200 >4,200 10.6 13.3 13.1 11.2 19 10.4 11.2 13.3 35.7 SVOCs (µg/kg dw) LPAHs 2-Methylnaphthalene ------2.2 U 2.2 U 2.5 U 2.2 U 2.2 U 2.2 U 2.2 U 2.2 U 2.2 U Acenaphthene ------1.4 U 1.4 U 1.6 U 1.4 U 1.4 U 1.4 U 1.4 U 1.4 U 1.4 U Acenaphthylene ------1.2 U 1.2 U 1.4 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U Anthracene ------1.6 U 1.6 U 1.8 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U Fluorene ------1.1 U 1.1 U 1.3 U 1.1 U 1.1 U 1.1 U 1.1 U 1.1 U 1.1 U Naphthalene ------2.3 U 2.3 U 2.6 U 2.3 U 2.3 U 2.3 U 2.3 U 2.3 U 2.3 U Phenanthrene ------1.9 J 1.4 U 1.6 U 1.4 U 1.4 U 1.4 U 1.4 U 1.4 U 1.5 J Total LPAH 1.9 J 2.3 U 2.6 U 2.3 U 2.3 U 2.3 U 2.3 U 2.3 U 1.5 J HPAH Fluoranthene ------2.5 J 1.6 U 1.8 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U Pyrene ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.7 J Benz(a)anthracene ------1.7 U 1.7 U 1.9 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U Chrysene ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U Benzofluoranthenes (b+k) ------1.4 U 1.4 U 1.6 U 1.4 U 1.4 U 1.4 U 1.4 U 1.4 U 1.4 U Benzo(j)fluoranthene ------Benzo(a)pyrene ------1.7 U 1.7 U 1.9 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U Indeno(1,2,3-c,d)pyrene ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U Dibenz(a,h)anthracene ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U Benzo(g,h,i)perylene ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U Total HPAH ------2.5 J 1.7 U 1.9 U 1.7 U 1.7 1.7 U 1.7 U 1.7 U 1.7 J Total PAHs 17,000 30,000 Chlorinated hydrocarbons 1,3-Dichlorobenzene ------3 U 3 U 3.4 U 3 U 3 U 3 U 3 U 3 U 3 U 1,4-Dichlorobenzene ------2.9 U 2.9 U 3.3 U 2.9 U 2.9 U 2.9 U 2.9 U 2.9 U 2.9 U 1,2-Dichlorobenzene ------2.9 U 2.9 U 3.3 U 2.9 U 2.9 U 2.9 U 2.9 U 2.9 U 2.9 U 1,2,4-Trichlorobenzene ------2.6 U 2.6 U 2.9 U 2.6 U 2.6 U 2.6 U 2.6 U 2.6 U 2.6 U Hexachlorobenzene (HCB) ------1.2 U 1.2 U 1.4 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U Phthalate esters (µg/kg dw) ------Dimethyl phthalate a ------28 17 1.2 U 1 U 1 U 1 U 1 U 1 U 350 Diethyl phthalate ------3.3 J 3.4 J 2.3 J 2 J 2.3 J 2.2 J 1.8 J 1.9 J 3.2 J

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Table 1-4. 2008 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater Parameter SCO CSL DMMU-8-C8 DMMU-9-C9 DMMU-10-C10 C8-Z(0-1) C8-Z(1-2) C9-Z(0-1) C9-Z(1-2) C10-Z(0-1) C10-Z(1-2) Di-n-butyl phthalate 380 1,000 21 25 19 J 15 J 12 J 11 J 13 J 12 J 13 J Butyl benzyl phthalate ------6.3 J 7.7 J 5.1 J 3.2 U 3.2 U 3.2 U 3.4 J 3.2 U 7.2 J Bis(2-ethylhexyl)phthalate 500 22,000 7.4 J 10 J 8.4 J 12 J 10 J 7 U 7.8 J 8.3 J 8.9 J Di-n-octyl phthalate 39 >1,100 1.7 U 1.7 U 1.9 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U 1.7 U Phenols (µg/kg dw) Phenol 120 210 2 U 2 U 2.3 U 2 U 2 U 2 U 2 U 2 U 2 U 2-Methylphenol ------1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 4-Methylphenol 260 2,000 1.5 U 1.5 U 1.7 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 1.5 U 2,4-Dimethylphenol ------5.5 U 5.5 U 6.2 U 5.5 U 5.5 U 5.5 U 5.5 U 5.5 U 5.5 U Pentachlorophenol 1,200 >1,200 20 U 20 U 23 U 20 U 20 U 20 U 20 U 20 U 20 U Miscellaneous extractables Benzyl alcohol ------18 J 16 J 2.4 U 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U 17 J Benzoic acid 2,900 3,800 96 U 96 U 110 U 96 U 96 U 96 U 96 U 96 U 96 U Dibenzofuran 200 680 1.2 U 1.2 U 1.4 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U 1.2 U Hexachloroethane ------3.1 U 3.1 U 3.5 U 3.1 U 3.1 U 3.1 U 3.1 U 3.1 U 3.1 U Hexachlorobutadiene ------2.5 U 2.5 U 2.8 U 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U 2.5 U N-Nitrosodiphenylamine ------1.6 U 1.6 U 1.8 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U 1.6 U Guaiacols (µg/L) 4-Chloroguaiacol ------3,4-Dichloroguaiacol ------4,5-Dichloroguaiacol ------4,6-Dichloroguaiacol ------3,4,5-Trichloroguaiacol ------3,4,6-Trichloroguaiacol ------4,5,6-Trichloroguaiacol ------Tetrachloroguaiacol ------Resin acids (mg/kg dw) Linoleic acid ------Oleic acid ------Pimaric acid ------Isopimaric acid ------Dehydroabietic acid ------Abietic acid ------9,10-Dichlorostearic acid ------12-Chlorodehydroabietic acid ------14-Chlorodehydroabietic acid ------Dichlorodehydroabietic acid ------Sandracopimaric acid ------Neoabietic acid ------Palustric acid ------Pesticides (µg/kg dw) Total DDT ------0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U p,p'-DDE 21 33 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U p,p'-DDD 310 860 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U 0.11 U p,p'-DDT 100 8,100 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U 0.17 U Aldrin ------0.16 U 0.16 U 0.16 U 0.16 U 0.16 U 0.16 U 0.16 U 0.16 U 0.16 U Total Chlordane ------0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U cis-Chlordane ------0.1 U 0.1 U 0.1 U 0.1 U 0.1 U 0.1 U 0.1 U 0.1 U 0.1 U trans-Chlordane ------0.09 U 0.09 U 0.09 U 0.09 U 0.09 U 0.09 U 0.09 U 0.09 U 0.09 U cis-Nonachlor ------0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U trans-Nonachlor ------0.087 U 0.087 U 0.087 U 0.087 U 0.087 U 0.087 U 0.087 U 0.087 U 0.087 U

Integral Consulting Inc. 2 of 3 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-4. 2008 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel

SMS Freshwater Parameter SCO CSL DMMU-8-C8 DMMU-9-C9 DMMU-10-C10 C8-Z(0-1) C8-Z(1-2) C9-Z(0-1) C9-Z(1-2) C10-Z(0-1) C10-Z(1-2) Oxychlordane ------0.085 U 0.085 U 0.085 U 0.085 U 0.085 U 0.085 U 0.085 U 0.085 U 0.085 U Dieldrin 4.9 9.3 0.14 U 0.14 U 0.14 U 0.14 U 0.14 U 0.14 U 0.14 U 0.14 U 0.14 U Heptachlor ------0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U 0.12 U Lindane ------0.08 U 0.08 U 0.08 U 0.08 U 0.08 U 0.08 U 0.08 U 0.08 U 0.08 U PCB Aroclors (µg/kg dw) Total PCB Aroclors 110 2,500 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U 2.1 U PCDDs/PCDFs (ng/kg dw) PCDDs --- 2,3,7,8-TCDD ------0.0722 U -- -- 0.0453 U 0.0393 U ------1,2,3,7,8-PeCDD ------0.0738 U -- -- 0.0464 U 0.0462 U ------1,2,3,4,7,8-HxCDD ------0.0572 U -- -- 0.0306 U 0.0472 U ------1,2,3,6,7,8-HxCDD ------0.0997 U -- -- 0.0435 JKU 0.0644 U ------1,2,3,7,8,9-HxCDD ------0.0705 U -- -- 0.0325 U 0.0636 JKU ------1,2,3,4,6,7,8-HpCDD ------0.871 JU -- -- 0.26 BJU 0.464 BJU ------OCDD ------7.33 J -- -- 1.35 BJU 3.03 BJU ------PCDFs 2,3,7,8-TCDF ------0.0765 U -- -- 0.0332 U 0.0419 U ------1,2,3,7,8-PeCDF ------0.0489 U -- -- 0.0196 U 0.026 U ------2,3,4,7,8-PeCDF ------0.0507 U -- -- 0.0193 U 0.0267 U ------1,2,3,4,7,8-HxCDF ------0.0458 U -- -- 0.0256 U 0.0221 U ------1,2,3,6,7,8-HxCDF ------0.0476 U -- -- 0.0247 U 0.0215 U ------1,2,3,7,8,9-HxCDF ------0.0536 U -- -- 0.0279 U 0.0221 U ------2,3,4,6,7,8-HxCDF ------0.0505 U -- -- 0.0273 U 0.0225 U ------1,2,3,4,6,7,8-HpCDF ------0.233 J -- -- 0.0898 J 0.107 JKU ------1,2,3,4,7,8,9-HpCDF ------0.0467 U -- -- 0.0389 U 0.0326 U ------OCDF ------0.758 JU -- -- 0.301 JKU 0.385 J ------Total TEQ ------0.0135 J -- -- 0.00834 J 0.0131 J ------Notes: Per the sampling and analysis plan, VOCs were not analyzed. -- = no criteria CSL = cleanup screening level DMMU = dredged material management unit MDL = method detection limit MRL = method reporting limit NA = not applicable PAH = polycyclic aromatic hydrocarbon SCO = sediment cleanup objective SCO = sediment cleanup objective SMS = Sediment Management Standards Qualifiers: B (metals) = The result is an estimated concentration that is less than the MRL but greater than or equal to the MDL. J = estimated concentration K = Ion abundance ratio out of range U = The compound was not detected at or above MRL/MDL.

a Dimethyl phthalate in Sample C10-Z(1-2) exceeded the Sediment Evaluation Framework Screening Level 1 value.

Integral Consulting Inc. 3 of 3 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-5 DMMU-8 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Grain Size Percent fines (calculated) percent -- -- 2.0 J na na 1.8 J na na Clay: 0 to 3.9 microns percent -- -- 0.8 J J 0.1 0.1 0.9 J J 0.1 0.1 Silt: 3.9 to 62.5 microns (calculated) percent -- -- 1.2 na na 0.9 na na Sand: 62.5 to 2,000 microns (calculated) percent -- -- 82.7 na na 97.7 na na Gravel: >2,000 microns (2 mm) (calculated) percent -- -- 15.4 na na 0.5 na na Conventionals N-ammonia mg/kg 230 300 0.33 0.003 0.12 0.12 U U 0.003 0.12 Preserved total solids percent -- -- 76.52 na 0.01 75.93 na 0.01 Total organic carbon percent -- -- 0.108 0.0029 0.02 0.047 0.0029 0.02 Total solids percent -- -- 79.51 na 0.01 74.34 na 0.01 Total sulfides mg/kg 39 61 1.25 UJ U UJ 0.0075 1.25 1.13 UJ U UJ 0.0075 1.13 Total volatile solids percent -- -- 0.91 na 0.01 0.46 na 0.01 Metals Arsenic mg/kg 14 120 2.6 0.04 0.2 0.8 0.04 0.3 Cadmium mg/kg 2.1 5.4 0.1 U U 0.009 0.1 0.1 U U 0.009 0.1 Chromium mg/kg 72 88 12.2 0.08 0.6 3.7 0.09 0.6 Copper mg/kg 400 1200 20.1 0.045 0.6 9.7 0.048 0.6 Lead mg/kg 360 >1300 4.1 J J 0.01 0.1 0.6 J J 0.01 0.1 Mercury mg/kg 0.66 0.8 0.35 0.0014 0.03 0.02 U U 0.0013 0.02 Nickel mg/kg 26 110 11.5 0.02 0.6 5.9 0.022 0.6 Selenium mg/kg 11 >20 1.1 0.039 0.6 0.6 U U 0.042 0.6 Silver mg/kg 0.57 1.7 0.2 U U 0.004 0.2 0.3 U U 0.004 0.3 Zinc mg/kg 3200 >4200 59 0.35 5 18 0.37 5 Organotins Butyltin ion µg/kg 540 >4800 3.6 UJ U UJ 2.6 3.6 3.8 UJ U UJ 2.7 3.8 Dibutyltin ion µg/kg 910 130000 5.1 UJ U UJ 3.3 5.1 5.4 UJ U UJ 3.5 5.4 Tetrabutyltin µg/kg 97 >97 4.4 U U 0.5 4.4 4.7 U U 0.5 4.7 Tributyltin ion µg/kg 47 320 3.4 U U 1.3 3.4 3.6 U U 1.4 3.6 Polycyclic Aromatic Hydrocarbons 1-Methylnaphthalene µg/kg -- -- 19 U U 5.7 19 19 U U 5.6 19 2-Methylnaphthalene µg/kg -- -- 19 UJ U UJ 5.4 19 19 UJ U UJ 5.3 19 Acenaphthene µg/kg -- -- 19 UJ U UJ 4.9 19 19 UJ U UJ 4.8 19 Acenaphthylene µg/kg -- -- 19 UJ U UJ 4.5 19 19 UJ U UJ 4.4 19 Anthracene µg/kg -- -- 19 UJ U UJ 5.6 19 19 UJ U UJ 5.5 19 Benzo(a)anthracene µg/kg -- -- 19 UJ U UJ 4.9 19 19 UJ U UJ 4.8 19 Benzo(a)pyrene µg/kg -- -- 6.7 J J J 6.2 19 19 UJ U UJ 6 19 Benzo(b)fluoranthene µg/kg -- -- 19 U U 6.7 19 19 U U 6.5 19 Benzo(g,h,i)perylene µg/kg -- -- 8.6 J J J 5.5 19 19 UJ U UJ 5.4 19 Benzo(k)fluoranthene µg/kg -- -- 19 UJ U UJ 4.8 19 19 UJ U UJ 4.7 19 Benzofluoranthenes µg/kg -- -- 11 J J J 9.7 38 37 UJ U UJ 9.5 37 Chrysene µg/kg -- -- 19 UJ U UJ 5 19 19 UJ U UJ 4.9 19 Dibenzo(a,h)anthracene µg/kg -- -- 19 U U 5.9 19 19 U U 5.7 19

Integral Consulting Inc. 1 of 8 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-9 DMMU-10 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Grain Size Percent fines (calculated) percent -- -- 1.0 J na na 1.0 na na Clay: 0 to 3.9 microns percent -- -- 0.9 J J 0.1 0.1 0.9 0.1 0.1 Silt: 3.9 to 62.5 microns (calculated) percent -- -- 0.1 na na 0.1 na na Sand: 62.5 to 2,000 microns (calculated) percent -- -- 98.6 na na 96.7 na na Gravel: >2,000 microns (2 mm) (calculated) percent -- -- 0.6 na na 2.4 na na Conventionals N-ammonia mg/kg 230 300 0.13 U U 0.003 0.13 0.13 U U 0.003 0.13 Preserved total solids percent -- -- 72.85 na 0.01 73.73 na 0.01 Total organic carbon percent -- -- 0.064 0.0029 0.02 0.061 J J 0.0029 0.02 Total solids percent -- -- 75.89 na 0.01 74.25 na 0.01 Total sulfides mg/kg 39 61 1.34 UJ U UJ 0.0075 1.34 1.22 U U 0.0075 1.22 Total volatile solids percent -- -- 0.37 na 0.01 0.43 na 0.01 Metals Arsenic mg/kg 14 120 0.8 0.04 0.3 1 0.04 0.3 Cadmium mg/kg 2.1 5.4 0.1 U U 0.009 0.1 0.1 U U 0.009 0.1 Chromium mg/kg 72 88 4.3 0.09 0.6 3.7 0.09 0.6 Copper mg/kg 400 1200 9 0.047 0.6 9.7 0.047 0.6 Lead mg/kg 360 >1300 0.7 J J 0.01 0.1 0.8 0.01 0.1 Mercury mg/kg 0.66 0.8 0.03 U U 0.0017 0.03 0.03 U U 0.0015 0.03 Nickel mg/kg 26 110 8.1 0.021 0.6 6.3 0.021 0.6 Selenium mg/kg 11 >20 0.7 0.04 0.6 0.6 U U 0.04 0.6 Silver mg/kg 0.57 1.7 0.3 U U 0.004 0.3 0.3 U U 0.004 0.3 Zinc mg/kg 3200 >4200 19 0.36 5 20 0.36 5 Organotins Butyltin ion µg/kg 540 >4800 3.7 UJ U UJ 2.7 3.7 3.9 UJ U UJ 2.8 3.9 Dibutyltin ion µg/kg 910 130000 5.2 UJ U UJ 3.4 5.2 5.5 UJ U UJ 3.5 5.5 Tetrabutyltin µg/kg 97 >97 4.5 U U 0.5 4.5 4.8 U U 0.5 4.8 Tributyltin ion µg/kg 47 320 3.5 U U 1.4 3.5 3.7 U U 1.5 3.7 Polycyclic Aromatic Hydrocarbons 1-Methylnaphthalene µg/kg -- -- 20 U U 5.8 20 19 U U 5.7 19 2-Methylnaphthalene µg/kg -- -- 20 UJ U UJ 5.5 20 19 UJ U UJ 5.4 19 Acenaphthene µg/kg -- -- 20 UJ U UJ 5 20 19 UJ U UJ 4.9 19 Acenaphthylene µg/kg -- -- 20 UJ U UJ 4.7 20 19 UJ U UJ 4.6 19 Anthracene µg/kg -- -- 20 UJ U UJ 5.8 20 19 UJ U UJ 5.7 19 Benzo(a)anthracene µg/kg -- -- 20 UJ U UJ 5.1 20 19 UJ U UJ 4.9 19 Benzo(a)pyrene µg/kg -- -- 20 UJ U UJ 6.3 20 19 UJ U UJ 6.2 19 Benzo(b)fluoranthene µg/kg -- -- 20 U U 6.9 20 19 U U 6.7 19 Benzo(g,h,i)perylene µg/kg -- -- 20 UJ U UJ 5.7 20 19 UJ U UJ 5.6 19 Benzo(k)fluoranthene µg/kg -- -- 20 UJ U UJ 4.9 20 19 UJ U UJ 4.8 19 Benzofluoranthenes µg/kg -- -- 39 UJ U UJ 10 39 38 UJ U UJ 9.7 38 Chrysene µg/kg -- -- 20 UJ U UJ 5.1 20 19 UJ U UJ 5 19 Dibenzo(a,h)anthracene µg/kg -- -- 20 U U 6 20 19 U U 5.9 19

Integral Consulting Inc. 2 of 8 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-5 DMMU-8 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Fluoranthene µg/kg -- -- 12 J J J 4.3 19 19 UJ U UJ 4.2 19 Fluorene µg/kg -- -- 19 UJ U UJ 4.7 19 19 UJ U UJ 4.6 19 Indeno(1,2,3-cd)pyrene µg/kg -- -- 19 U U 5.7 19 19 U U 5.6 19 Naphthalene µg/kg -- -- 6.7 J J J 5 19 19 UJ U UJ 4.9 19 Phenanthrene µg/kg -- -- 7.6 J J 4.5 19 19 U U 4.4 19 Pyrene µg/kg -- -- 11 J J J 5.3 19 19 UJ U UJ 5.2 19 Total Polycyclic Aromatic Hydrocarbons µg/kg 17000 30000 63.6 J na na 37 UJ na na Chlorinated Hydrocarbons beta-Hexachlorocyclohexane µg/kg 7.2 11 0.82 U U 0.31 0.82 0.82 U U 0.31 0.82 Phthalates Bis(2-ethylhexyl) phthalate µg/kg 500 22000 48 U U 27 48 47 U U 27 47 Dibutyl phthalate µg/kg 380 1000 18 J J 5.1 19 19 U U 5 19 Di-n-octyl phthalate µg/kg 39 >1100 19 U U 8.3 19 19 U U 8.1 19 Phenols 4-Methylphenol µg/kg 260 2000 19 UJ U UJ 14 19 19 UJ U UJ 14 19 Pentachlorophenol µg/kg 1200 >1200 95 U U 30 95 93 U U 29 93 Phenol µg/kg 120 210 11 J J J 7.8 19 19 UJ U UJ 7.7 19 Miscellaneous Extractables Benzoic acid µg/kg 2900 3800 190 U U 56 190 190 U U 55 190 Carbazole µg/kg 900 1100 19 U U 7 19 19 U U 6.9 19 Dibenzofuran µg/kg 200 680 19 U U 4.4 19 19 U U 4.3 19 Pesticides 2,4′-DDD µg/kg -- -- 1.6 U U 1.4 1.6 1.6 U U 1.4 1.6 2,4′-DDE µg/kg -- -- 1.6 U U 1.5 1.6 1.6 U U 1.5 1.6 2,4′-DDT µg/kg -- -- 1.6 U U 1.6 1.6 1.6 U U 1.6 1.6 4,4-DDD µg/kg -- -- 1.6 U U 0.57 1.6 1.6 U U 0.56 1.6 4,4′-DDE µg/kg -- -- 1.6 UJ U UJ 0.56 1.6 1.6 UJ U UJ 0.56 1.6 4,4′-DDT µg/kg -- -- 1.6 UJ U UJ 0.56 1.6 1.6 UJ U UJ 0.56 1.6 Total of 2,4′ and 4,4′-DDD µg/kg 310 860 1.6 U na na 1.6 U na na Total of 2,4′ and 4,4′-DDE µg/kg 21 33 1.6 UJ na na 1.6 UJ na na Total of 2,4′ and 4,4′-DDT µg/kg 100 8100 1.6 UJ na na 1.6 UJ na na cis-Chlordane µg/kg -- -- 0.82 U U 0.28 0.82 0.82 U U 0.28 0.82 cis-Nonachlor µg/kg -- -- 1.6 U U 0.55 1.6 1.6 U U 0.54 1.6 Dieldrin µg/kg 4.9 9.3 1.6 U U 0.55 1.6 1.6 U U 0.55 1.6 Endrin ketone µg/kg 8.5 8.5 1.6 U U 0.65 1.6 1.6 U U 0.65 1.6 Oxychlordane µg/kg -- -- 1.6 U U 0.76 1.6 1.6 U U 0.76 1.6 trans-Chlordane µg/kg -- -- 0.82 UJ U UJ 0.26 0.82 0.82 UJ U UJ 0.26 0.82 trans-Nonachlor µg/kg -- -- 1.6 U U 1.6 1.6 1.6 U U 1.6 1.6 Polychlorinated biphenyls Aroclor 1016 µg/kg -- -- 3.9 U U 1.5 3.9 3.8 U U 1.5 3.8 Aroclor 1221 µg/kg -- -- 3.9 U U 1.5 3.9 3.8 U U 1.5 3.8 Aroclor 1232 µg/kg -- -- 3.9 U U 1.5 3.9 3.8 U U 1.5 3.8 Aroclor 1242 µg/kg -- -- 3.9 U U 1.5 3.9 3.8 U U 1.5 3.8

Integral Consulting Inc. 3 of 8 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-9 DMMU-10 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Fluoranthene µg/kg -- -- 20 UJ U UJ 4.4 20 19 UJ U UJ 4.3 19 Fluorene µg/kg -- -- 20 UJ U UJ 4.8 20 19 UJ U UJ 4.7 19 Indeno(1,2,3-cd)pyrene µg/kg -- -- 20 U U 5.9 20 19 U U 5.7 19 Naphthalene µg/kg -- -- 20 UJ U UJ 5.1 20 19 UJ U UJ 5 19 Phenanthrene µg/kg -- -- 20 U U 4.6 20 19 U U 4.5 19 Pyrene µg/kg -- -- 20 UJ U UJ 5.4 20 19 UJ U UJ 5.3 19 Total Polycyclic Aromatic Hydrocarbons µg/kg 17000 30000 39 UJ na na 38 UJ na na Chlorinated Hydrocarbons beta-Hexachlorocyclohexane µg/kg 7.2 11 0.79 U U 0.3 0.79 0.78 U U 0.3 0.78 Phthalates Bis(2-ethylhexyl) phthalate µg/kg 500 22000 49 U U 28 49 48 U U 27 48 Dibutyl phthalate µg/kg 380 1000 12 J J 5.2 20 12 J J 5.1 19 Di-n-octyl phthalate µg/kg 39 >1100 20 U U 8.5 20 19 U U 8.3 19 Phenols 4-Methylphenol µg/kg 260 2000 20 UJ U UJ 14 20 19 UJ U UJ 14 19 Pentachlorophenol µg/kg 1200 >1200 98 U U 31 98 95 UJ U UJ 30 95 Phenol µg/kg 120 210 20 UJ U UJ 8.1 20 19 UJ U UJ 7.9 19 Miscellaneous Extractables Benzoic acid µg/kg 2900 3800 200 U U 58 200 190 UJ U UJ 56 190 Carbazole µg/kg 900 1100 20 U U 7.2 20 19 U U 7 19 Dibenzofuran µg/kg 200 680 20 U U 4.5 20 19 U U 4.4 19 Pesticides 2,4′-DDD µg/kg -- -- 1.6 U U 1.4 1.6 1.6 U U 1.4 1.6 2,4′-DDE µg/kg -- -- 1.6 U U 1.4 1.6 1.6 U U 1.4 1.6 2,4′-DDT µg/kg -- -- 1.6 U U 1.6 1.6 1.6 U U 1.6 1.6 4,4-DDD µg/kg -- -- 1.6 U U 0.55 1.6 1.6 U U 0.54 1.6 4,4′-DDE µg/kg -- -- 1.6 UJ U UJ 0.54 1.6 1.6 UJ U UJ 0.54 1.6 4,4′-DDT µg/kg -- -- 1.6 UJ U UJ 0.54 1.6 1.6 UJ U UJ 0.54 1.6 Total of 2,4′ and 4,4′-DDD µg/kg 310 860 1.6 U na na 1.6 U na na Total of 2,4′ and 4,4′-DDE µg/kg 21 33 1.6 UJ na na 1.6 UJ na na Total of 2,4′ and 4,4′-DDT µg/kg 100 8100 1.6 UJ na na 1.6 UJ na na cis-Chlordane µg/kg -- -- 0.79 U U 0.27 0.79 0.78 U U 0.27 0.78 cis-Nonachlor µg/kg -- -- 1.6 U U 0.53 1.6 1.6 U U 0.52 1.6 Dieldrin µg/kg 4.9 9.3 1.6 U U 0.54 1.6 1.6 U U 0.53 1.6 Endrin ketone µg/kg 8.5 8.5 1.6 U U 0.63 1.6 1.6 U U 0.63 1.6 Oxychlordane µg/kg -- -- 1.6 U U 0.74 1.6 1.6 U U 0.73 1.6 trans-Chlordane µg/kg -- -- 0.79 UJ U UJ 0.25 0.79 0.78 UJ U UJ 0.25 0.78 trans-Nonachlor µg/kg -- -- 1.6 U U 1.5 1.6 1.6 U U 1.5 1.6 Polychlorinated biphenyls Aroclor 1016 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9 Aroclor 1221 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9 Aroclor 1232 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9 Aroclor 1242 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9

Integral Consulting Inc. 4 of 8 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-5 DMMU-8 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Aroclor 1248 µg/kg -- -- 3.9 U U 1.5 3.9 3.8 U U 1.5 3.8 Aroclor 1254 µg/kg -- -- 3.1 J J J 1.5 3.9 3.8 U U 1.5 3.8 Aroclor 1260 µg/kg -- -- 3.9 U U 0.57 3.9 3.8 U U 0.56 3.8 Aroclor 1262 µg/kg -- -- 3.9 U U 0.57 3.9 3.8 U U 0.56 3.8 Aroclor 1268 µg/kg -- -- 3.9 U U 0.57 3.9 3.8 U U 0.56 3.8 Total Aroclors µg/kg 110 2500 3.1 J na na na na 3.8 U na na na na Dioxins/Furans 1,2,3,4,6,7,8-Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8,9-Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,6,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8,9-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8-Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8-Pentachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 2,3,4,6,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,4,7,8-Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,7,8-Tetrachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,7,8-Tetrachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Heptachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Octachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Octachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Pentachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Tetrachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Tetrachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na TEQ (U = 1/2 DL) pg/g -- -- na na na na na na na na na na na na TEQ (U = 0) pg/g -- -- na na na na na na na na na na na na

Integral Consulting Inc. 5 of 8 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-9 DMMU-10 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Aroclor 1248 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9 Aroclor 1254 µg/kg -- -- 4 U U 1.5 4 3.9 U U 1.5 3.9 Aroclor 1260 µg/kg -- -- 4 U U 0.58 4 3.9 U U 0.58 3.9 Aroclor 1262 µg/kg -- -- 4 U U 0.58 4 3.9 U U 0.58 3.9 Aroclor 1268 µg/kg -- -- 4 U U 0.58 4 3.9 U U 0.58 3.9 Total Aroclors µg/kg 110 2500 4 U na na na na 3.9 U na na na na Dioxins/Furans 1,2,3,4,6,7,8-Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8,9-Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,6,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8,9-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8-Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 1,2,3,7,8-Pentachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na 2,3,4,6,7,8-Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,4,7,8-Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,7,8-Tetrachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na 2,3,7,8-Tetrachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Heptachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Heptachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Hexachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Hexachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Octachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Octachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Pentachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Pentachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na Tetrachlorodibenzofuran pg/g -- -- na na na na na na na na na na na na Tetrachlorodibenzo-p-dioxin pg/g -- -- na na na na na na na na na na na na TEQ (U = 1/2 DL) pg/g -- -- na na na na na na na na na na na TEQ (U = 0) pg/g -- -- na na na na na na na na na na na

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Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-5 DMMU-8 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Petroleum Hydrocarbons Diesel Range Hydrocarbons mg/kg 340 510 26 1.7 6.2 6.5 U U 1.8 6.5 Residual Range Hydrocarbons mg/kg 3600 4400 220 3.1 12 13 U U 3.2 13

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Table 1-5. 2015 Dredged Material Sediment Characterization Analytical Results—Mount Coffin Channel and Salt Dock

DMMU-9 DMMU-10 SMS Freshwater Qualifiers Qualifiers Analyte Units SCO CSL Result Final Lab Val. MDL MRL Result Final Lab Val. MDL MRL Petroleum Hydrocarbons Diesel Range Hydrocarbons mg/kg 340 510 6.3 U U 1.7 6.3 6.7 U U 1.8 6.7 Residual Range Hydrocarbons mg/kg 3600 4400 13 U U 3.1 13 13 U U 3.3 13 Notes: All results shown are on a dry weight basis.

-- = no criteria CSL = cleanup screening level DMMU = dredged material management unit MDL = method detection limit MRL = method reporting limit na = not PCBl = polychlorinated d biphenyl SCO = TEQdi = t Val.t i = it validation

Qualifiers: B = analyte detected in an associated Method Blank at a concentration greater than one-half of Analytical Resources Inc.'s reporting limit or 5 percent of the regulatory limit or 5 percent of the analyte concentration in the sample EMPC = Estimated maximum possible concentration defined in EPA Statement of WorkDLM02.2 as a value "calculated for 2,3,7,8-substituted isomers for which the quantitation and/or confirmation ion(s) has signal to noise in excess of 2.5, but does not meet identification criteria" (dioxin/furan analysis only)

J = estimated concentration when the value is less than Analytical Resources Inc.'s established reporting limits U = indicates the target analyte was not detected at the reported concentration

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Table 1-6. 2016–2017 Summary of Relevant Incident Information for the Columbia River at Longview from Ecology

Incident ID Incident Date City Address Waterway Material Source Incident Type Impact Activity Summary

CALLER IS REPORTING A DISCHARGE OF `A FEW PETROLEUM - WATER DROPS` HYDRAULIC OIL FROM A PIECE OF LOADING 662414 23-Jan-16 LONGVIEW 3401 Industrial Way Columbia River COMMERCIAL Oil Spill OTHER HYDRAULIC OIL POLLUTION EQUIPMENT INTO COLUMBIA RIVER. NO VISIBLE SHEEN WAS OBSERVED.

DESCRIPTION OF INCIDENT - CALLER STATED AN UNKNOWN PIPE IS LEAKING CRUDE OIL DUE TO PETROLEUM - WATER UNKNOWN REASONS. CALLER STATED THIS IS A 662972 17-Feb-16 LONGVIEW 10 Port Way Columbia River Oil Spill OTHER CRUDE OIL POLLUTION DISPUTED PIPELINE AND IS CURRENTLY OUT OF SERVICE. CALLER STATED IT MUST BE RESIDUAL LEFT IN THE LINE. CONSTRUCTIO WATER Caller reported to reception at 12:26 today 3/14/16, turbidity of 663636 14-Mar-16 LONGVIEW 3500 Industrial Way Columbia River MUD/SILT UNKNOWN N SITE POLLUTION 340 NTU.

UNKNOWN SHEEN SIGHTING IN FRONT OF EXPORT Columbia River Mile PETROLEUM - WATER 664417 19-Apr-16 LONGVIEW Columbia River Oil Spill UNKNOWN GRAIN TERMINAL. EXACT SOURCE OF THE SHEEN IS Marker 46 UNKNOWN POLLUTION UNKNOWN AT THIS TIME.

POTENTIAL NEAR Columbia 667459 06-Sep-16 LONGVIEW 250 Baltimore SEWAGE/SLUDGE COMMERCIAL POLLUTION/RE REPAIRING River LEASE

POTENTIAL CALLER IS REPORTING THE DISCOVERY OF TWO 669285 02-Dec-16 LONGVIEW 150 East Mill Rd Columbia River UNKNOWN UNKNOWN POLLUTION/RE DUMPING ABANDONED DRUMS IN THE COLUMBIA RIVER. THERE LEASE IS NO REPORTED RELEASE OR DISCHARGE.

Calcined Coke spill to the Columbia River. 1/2 -1 cubic yards PETROLEUM - OIL Government WATER 671221 07-Mar-17 LONGVIEW 10 Port Way Columbia River Oil Spill OTHER that went into the Columbia River. The Port have put a log OTHER Facilities POLLUTION berm and deployed boom.

Unknown amount of diesel fuel discharged from a sunken vessel (boat used to remove log dams). A sheen is coming 4029 Industrial Way, PETROLEUM - OIL WATER from the boat. The caller said they contained it with river 671589 20-Mar-17 LONGVIEW Columbia River Other - Vessel Oil Spill UNKNOWN River Mile 63 OTHER POLLUTION booms. The caller said this boat holds approx. 30 gallons of diesel.

WATER 672331 18-Apr-17 LONGVIEW 6415 Willow Bldg Columbia River OTHER OTHER OTHER POLLUTION

VESSEL - 673687 12-Jun-17 LONGVIEW Columbia River OTHER OTHER OTHER UNKNOWN

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Table 1-6. 2016–2017 Summary of Relevant Incident Information for the Columbia River at Longview from Ecology

Incident ID Incident Date City Address Waterway Material Source Incident Type Impact Activity Summary

CALLER STATED A TANKER VESSEL WAS SEEN GOING WATER DOWN THE COLUMBIA RIVER AND A TRAIL OF 674187 07-Jul-17 LONGVIEW Columbia River UNKNOWN VESSEL - TANK Oil Spill UNKNOWN POLLUTION RED/BROWN MATERIALS APPEARED TO BE COMING FROM THE VESSEL.

Report of an unknown sheen from an unknown source. An oily substance is bubbling up from the bottom of the Columbia PETROLEUM - WATER 674767 01-Aug-17 LONGVIEW 6021 Willow Grove Rd Columbia River Oil Spill UNKNOWN River at a rate of about 5-6 drops per minute, and it smells like UNKNOWN POLLUTION oil. Possibly from a container. A boom has been placed to contain the sheen.

Notes: Ecology = Washington State Department of Ecology

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Table 1-7. 1999–2017 Spills to the Columbia River in the Vicinity of the NDP Property from National Response Center Database

NRC Sequence # Spill Site Responsible Party Date Description Material(s) Media Affected Sheen Observed 473866 Export Dock WEYERHAEUSER CORP. 2/12/1999 EXPORT DOCK / CONSTRUCTION DEBRIS FALLING INTO THE creosote Columbia River SHEEN SIZE:2 X 2 FT / COLOR: LIGHT RIVER 475075 Chip Barge Dock WEYERHAEUSER COMPANY 2/25/1999 CHIP BARGE CRANE (SHORE MOUNTED) / MATERIAL SPILLED oil; misc: lubricating Columbia River SHEEN SIZE: 30 FT X 1 FT / RAINBOW COLORED DURING MAINTENANCE 491587 WEYERHAEUSER 7/16/1999 UNLOADING CRANE / MATERIAL SPILLED DUE TO A LEAK IN A hydraulic oil Columbia River SHEEN SIZE: 10 FT X 150 FT / RAINBOW HYDRAULIC LINE COLORED 498482 Chip Barge dock WEYERHAEUSER COMPANY 9/13/1999 CHIP BARGE CRANE / HYDRAULIC LINE FAILED / RELEASED hydraulic oil Columbia River HYDRAULIC OIL INTO COLUMBIA RIVER 529465 Chip Barge dock WEYERHAEUSER COMPANY 5/19/2000 CHIP BARGE CRANE / HYDRAULIC HOSE BROKE DUE TO hydraulic oil Columbia River SHEEN SIZE:300 FT X 1 FT / COLOR:UNKNOWN / APPROXIMATELY THREE TO FIVE GALLONS SPILLED / NO ADDITIONAL INFORMATION 541343 WEYERHAEUSER COMPANY 9/7/2000 THE MATERIAL WAS RELEASING FROM A BARGE CRANE DUE hydraulic oil Columbia River TO A BROKEN HYDRAULIC FITTING. 544553 WEYERHAEUSER COMPANY 10/8/2000 A HYDRAULIC LINE CONNECTED TO A TRANSFER PIECE OF hydraulic oil Columbia River Sheen barely discernible EQUIPMENT WAS DISCOVERED LEAKING DUE TO A UNKNOWN CAUSE ONTO THE LAND AND INTO THE COLUMBIA RIVER.

550747 WEYERHAEUSER COMPANY 12/12/2000 THE CALLER IS MAKING AN INITIAL CONTINUOUS RELEASE Columbia River REPORT. 552067 WEYERHAEUSER COMPANY 12/28/2000 A CRANE HYDRAULIC LINE FAILED DUE TO UNKNOWN CAUSES hydraulic oil 10 FT x 10 FT sheen

555942 COLUMBIA RIVER MM65 WEYERHAEUSER COMPANY 2/6/2001 MATERIAL SPILLED FROM LEAKING HYDRUALIC LINE INTO hydraulic oil Columbia River COLUMBIA RIVER 586221 Chip Barge Dock WEYERHAEUSER COMPANY 11/16/2001 CALLER IS REPORTING A PINHOLE LEAK IN A HYDRAULIC LINE hydraulic oil Columbia River CALLER ESTIMATES THE RELEASE TO BE LEADING FROM THE DOCK TO THE BARGE. BETWEEN 4-16 OUNCES; 20 Ft x 20 Ft SHEEN 741811 WEYERHAEUSER COMPANY 11/18/2004 HYDRAULIC OIL SPILLED INTO THE COLUMBIA RIVER FROM A hydraulic oil Columbia River HYDRAULIC HOSE ON A LOG PICKER. 741823 WEYERHAEUSER COMPANY 11/18/2004 HYDRAULIC OIL SPILLED INTO THE COLUMBIA RIVER FROM A hydraulic oil Columbia River HYDRAULIC HOSE ON A LOG PICKER. 742260 WEYERHAEUSER COMPANY 11/23/2004 HYDRAULIC OIL SPILLED INTO THE COLUMBIA RIVER FROM A hydraulic oil Columbia River HAYDRAULIC SYSTEM ON A CRANE. 749839 WEYERHAEUSER COMPANY 2/11/2005 DIESEL FUEL SPILLED INTO THE COLUMBIA RIVER FROM A diesel Columbia River LEAKING GASKET CONNECTED TO A TRANSFER LINE. 779986 Chip barge dock WEYERHAEUSER COMPANY 11/18/2005 CALLER STATED DUE TO EQUIPMENT FAILURE ON A CHIP hydraulic Columbia River Sheen 40 ft x 3 ft BARGE CRANE WHICH IS ON LAND THERE WAS A RELEASE OF MATERIALS. 804849 WEYERHAEUSER COMPANY 7/20/2006 CALLER STATED THERE WAS A RELEASE OF MATERIALS FROM hydraulic oil Columbia River A TRUCK DUE TO EQUIPMENT FAILURE ON THE TRUCK.

810313 TIMBERLAND'S WATER FILL WEYERHAEUSER COMPANY 9/5/2006 CALLER STATES THAT HYDRAULIC OIL HAS DISCHARGED INTO hydraulic oil storm drain/Columbia 30 ft x 7 ft sheen STATION/ ADJACENT TO THE COLUMBIA RIVER VIA A STORM DRAIN DUE TO A LEAK OF River EXPORT DOCK THE OIL FROM A COMMERCIAL TRUCK.

852122 log dock WEYERHAEUSER COMPANY 10/19/2007 CALLER IS REPORTING THAT WHILE A LOG LOADER WAS hydraulic oil Columbia River rainbow sheen 20 ft x 4 ft UNLOADING A BARGE ON A LOG DOCK, THE HYDRAULIC CYLINDER BROKE WHICH CAUSES A DISCHARGE OF HYDRAULIC OIL INTO THE COLUMBIA RIVER. 881343 WEYERHAEUSER COMPANY 8/21/2008 CALLER IS REPORTING AN OIL SHEEN FROM THEIR STORM OIL, MISC: MOTOR LONGVIEW DITCH/ silvery sheen 10 ft x 1 ft WATER DISCHARGE. THEIR OILY WATER SEPARATOR LEAKED COLUMBIA RIVER OIL INTO THE STORM WATER AND THEN INTO LONGVIEW DITCH. AN INVESTIGATION IS UNDERWAY.

Integral Consulting Inc. 1 of 2 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 1-7. 1999–2017 Spills to the Columbia River in the Vicinity of the NDP Property from National Response Center Database

NRC Sequence # Spill Site Responsible Party Date Description Material(s) Media Affected Sheen Observed 934868 WEYERHAEUSER COMPANY 3/23/2010 A LOG BARGE WAS BEING LOADED AND THE SHORE SIDE OF HYDRAULIC OIL Water THE LOG SHOVEL RUPTURED A HYDRAULIC HOSE DISCHARGING A QT OF OIL. SOME OF THE PRODUCT HAD ENTERED THE COLUMBIA RIVER. 941423 WEYERHAEUSER CORP. 5/24/2010 CALLER STATED THAT THERE WAS A RELEASE OF AN ON Hydrogen Peroxide Storm sewer GOING AMOUNT OF HYDROGEN PEROXIDE FROM A RAIL CAR, THE CAUSE WAS DUE TO A LARGE PIECE OF ROLLING STOCK THAT PUNCTURED THE TANK OF THE CAR.

941753 WEYERHAEUSER CORP. 5/26/2010 CALLER STATED THAT THERE IS A VISIBLE SHEEN IN THE Unknown oil CDID Ditch/Columbia Barely discernible 10 ft x 2 ft WATER, FROM A LOG YARD DUE TO HEAVY RAIN. River 969342 WEYERHAEUSER 3/7/2011 APPROXIMATELY 20 POUNDS OF SODIUM DICHROMATE SODIUM Columbia River SPILLED FROM THE BLEACHING OPERATION TO THE DICHROMATE COLUMBIA RIVER DUE TO DUE TO A SHUTDOWN PROCEDURE. Paper Mill 1004479 SEGMENT #25-01-00 WEYERHAEUSER COMPANY 3/1/2012 CALLER IS REPORTING A DISCHARGE OF AN UNKNOWN OIL Oil: Crude CDID DITCH silvery sheen FROM A STORM WATER POND TO A DITCH DUE TO AN #3/Columbia River UNKNOWN CAUSE AT THIS TIME. 1134175 BERTH B WEYERHAEUSER CO 11/23/2015 CALLER IS REPORTING A DISCHARGE OF HYDRAULIC OIL HYDRAULIC OIL Columbia River FROM A SHOVEL THAT WAS UNLOADING LOGS FROM A BARGE DUE TO A BROKEN HYDRAULIC HOSE. CALLER STATED THE AMOUNT SPILL WAS LESS THAN 1 GALLON. 1138775 WEYERHAEUSER 1/23/2016 CALLER IS REPORTING A DISCHARGE OF "A FEW DROPS" HYDRAULIC OIL Columbia River No sheen observed HYDRAULIC OIL FROM A PIECE OF LOADING EQUIPMENT INTO COLUMBIA RIVER. NO VISIBLE SHEEN WAS OBSERVED.

Websites accessed for spill information: NRC. 2008. 1999-2008 from National Response Center Oil and chemical spill database. http://www.nrc.uscg.mil/foia.html Accessed July 28, 2008. NRC. 2015. 2009-2015 from National Response Center Oil and chemical spill database. http://www.nrc.uscg.mil/ Accessed July 17, 2015. NRC. 2017. 2015-2017 from National Response Center Oil and chemical spill database. http://www.nrc.uscg.mil/ Accessed September 28, 2017. Ecology. 2015b. 2009-2015 from State of Washington Department of Ecology http://www.ecy.wa.gov/programs/spills/incidents/main.html Accessed July 21, 2015.

Notes: CDID = Consolidated Diking Improvement District NDP = Nippon Dynawave Packaging NRC = Northern Resource Consulting

Integral Consulting Inc. 2 of 2 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 2-1. Proposed Sampling Locations Mudline Mudline Total sulfides, Latitude Longitude Elevation Elevation Ammonia, Metals, PCB Petroleum a Sample ID (WGS84) (WGS84) (NAVD88) (CRD) Grain size TOC, TS, TVS Mercury Butyltins SVOCs Aroclors Pesticides Hydrocarbons Archive Bioassays G1 46.131745 -122.997852 na na X X X X X X X X X A G2 46.131666 -122.997395 na na X X X X X X X X X A G3 46.131585 -122.996920 na na X X X X X X X X X A G4 46.131303 -122.997291 na na X X X X X X X X X A G5 46.131229 -122.996857 na na X X X X X X X X X A G6 46.131149 -122.996382 -26.4 -23.9 X X X X X X X X X A G7 46.131274 -122.995444 -30.5 -28.0 X X X X X X X X X A G8 46.131180 -122.994892 -28.0 -25.5 X X X X X X X X X A G9 46.131087 -122.994340 -26.9 -24.4 X X X X X X X X X A G10 46.130844 -122.994894 -32.4 -29.9 X X X X X X X X X A G11 46.130751 -122.994342 -31.4 -28.9 X X X X X X X X X A G12 46.130658 -122.993790 -32.5 -30.0 X X X X X X X X X A G13 46.132071 -122.998081 na na A A A A A A A A A A G14 46.131991 -122.997606 na na A A A A A A A A A A G15 46.130911 -122.996611 -30.7 -28.2 A A A A A A A A A A G16 46.130831 -122.996136 -27.7 -25.2 A A A A A A A A A A G17 46.131590 -122.995592 -33.6 -31.1 A A A A A A A A A A G18 46.131497 -122.995040 -26.7 -24.2 A A A A A A A A A A G19 46.130457 -122.994215 -30.5 -28.0 A A A A A A A A A A G20 46.130363 -122.993663 -34.9 -32.4 A A A A A A A A A A G21 46.132362 -122.998259 na na A A A A A A A A A A G22 46.130514 -122.995957 -26.6 -24.1 A A A A A A A A A A G23 46.131902 -122.995774 na na A A A A A A A A A A G24 46.130031 -122.993429 -35.0 -32.5 A A A A A A A A A A Notes: Mudline Elevation (NAVD 88) based on 2017 bathymetry data provided by NDP.

A = sample volume for this parameter will be collected and archived for potential future analysis CRD = Columbia River Datum (add 2.5 ft to NAVD88) na = recent bathymetry not available at this location. NAVD88 = North American Vertical Datum, 1988 PCB = polychlorinated biphenyl SVOC = semivolatile organic compound TOC = total organic carbon TS = total solids TVS = total volatile solids WGS84 = World Geodetic System 1984 X = sample to be analyzed

a All bioassay samples will be archived pending the results of initial chemical evaluation.

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Table 4-1. Sample Storage Requirements

a Sample Type Holding Time Sample Size Preservation Container Grain size 6 months 100–200 g 4ºC 16 oz. WMG or HDPE Total sulfides b 7 days 50 g Zinc acetate, No headspace, 4ºC 4 oz. WMG Total volatile solids 14 days 50 g No headspace, 4ºC 4 oz. WMG Ammonia 7 days 25 g Total organic carbon 14 days c 125 g Mercury 28 days d 5 g Metals and total solids 6 months c 50 g 4ºC 8 oz. WMG Organometallic compounds 14 days c 100 g Semivolatiles 14 days c,e 40 g Pesticides 14 days c,e 25 g PCB Aroclors 14 days c,e 25 g Archive f 1 year NA -20°C 4 oz. WMG Bioassay testing/archive 8 weeks 4 Lg Zero headspace, 4°C (4) 1 L WMG

Notes: EPA = U.S. Environmental Protection Agency HDPE = high density polyethylene NA = not applicable PCB = polychlorinated biphenyl SVOC = semivolatile organic compound WMG = wide mouth glass

a Recommended minimum field sample sizes for one laboratory analysis. Actual volumes to be collected have been increased to provide a margin of error and allow for retests. b The sulfides sample will be preserved with 5 mL of 2N zinc acetate for every 30 g of sediment. c Holding times for frozen samples are as follows: Total organic carbon—6 months; metals (except mercury)—2 years; SVOCs, pesticides, PCB Aroclors—1 year; Organometallic compounds—1 year. d The holding time for mercury in frozen (i.e., archived) samples is 180 days, as approved by EPA. e Holding time is 14 days to extraction and extracts must be analyzed within 40 days from extraction. f For every sample, a 250-mL container is filled and frozen in case any reanalyses are required. g 4 L will provide sufficient volume to allow two complete runs, if necessary, of the full suite of bioassays.

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Table 5-1. Chemical Parameters, Analytical Methods, and SMS Criteria

SMS Freshwater a Sediment Parameter Prep/Cleanup Method Analysis Method SQLs SCO CSL Conventionals Ammonia (mg/kg) EPA 350.1 (modified) EPA 350.1 (modified) 0.5 230 300 Grain size (%) --- Modified ASTM D-422 ------Total organic carbon (%) EPA 9060 (modified) EPA 9060 (modified) 0.1 ------Total solids (%) --- SM 2540G ------Total sulfides (mg/kg) SM4500 S2-D SM 4500-S2 0.5 39 61 Total volatile solids (%) --- SM 2540G 0.1 ------

Metals (mg/kg dw) Arsenic EPA 3050B EPA 200.8 0.5 14 120 Cadmium EPA 3050B EPA 200.8 0.02 2.1 5.4 Chromium EPA 3050B EPA 200.8 0.2 72 88 Copper EPA 3050B EPA 200.8 0.1 400 1,200 Lead EPA 3050B EPA 200.8 0.05 360 >1,300 Mercury EPA 7471B EPA 7471B 0.2 0.66 0.8 Nickel EPA 3050B EPA 200.8 1 26 110 Selenium EPA 3050B EPA 200.8 0.02 11 >20 Silver EPA 3050B EPA 200.8 0.5 0.57 1.7 Zinc EPA 3050B EPA 200.8 0.02 3,200 >4,200

Organometallic Compounds (bulk, µg/kg dw) Monobutyltin ion ALS SOP SOC-Butyl ALS SOP SOC-Butyl 1 540 >4,800 Dibutyltin ion ALS SOP SOC-Butyl ALS SOP SOC-Butyl 1 910 130,000 Tributyltin ion ALS SOP SOC-Butyl ALS SOP SOC-Butyl 1 47 320 Tetrabutyltin ion ALS SOP SOC-Butyl ALS SOP SOC-Butyl 1.00 97 >97

Semivolatile Organic Compounds (µg/kg dw) PAHs Acenaphthene EPA 3541/3640A EPA 8270D 10 ------Acenaphthylene EPA 3541/3640A EPA 8270D 10 ------Anthracene EPA 3541/3640A EPA 8270D 10 ------Fluorene EPA 3541/3640A EPA 8270D 10 ------Naphthalene EPA 3541/3640A EPA 8270D 10 ------Phenanthrene EPA 3541/3640A EPA 8270D 10 ------1-Methylnaphthalene EPA 3541/3640A EPA 8270D 10 ------

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Table 5-1. Chemical Parameters, Analytical Methods, and SMS Criteria

SMS Freshwater a Sediment Parameter Prep/Cleanup Method Analysis Method SQLs SCO CSL 2-Methylnaphthalene EPA 3541/3640A EPA 8270D 10 ------Fluoranthene EPA 3541/3640A EPA 8270D 10 ------Pyrene EPA 3541/3640A EPA 8270D 10 ------Benz(a)anthracene EPA 3541/3640A EPA 8270D 10 ------Chrysene EPA 3541/3640A EPA 8270D 10 ------Benzo(b)fluoranthene EPA 3541/3640A EPA 8270D 10 ------Benzo(k)fluoranthene EPA 3541/3640A EPA 8270D 10 ------Benzo(a)pyrene EPA 3541/3640A EPA 8270D 10 ------Indeno(1,2,3-cd)pyrene EPA 3541/3640A EPA 8270D 10 ------Dibenz(a,h)anthracene EPA 3541/3640A EPA 8270D 10 ------Benzo(g,h,i)perylene EPA 3541/3640A EPA 8270D 10 ------Total PAHs EPA 3541/3640A EPA 8270D --- 17,000 30,000 Chlorinated hydrocarbons beta-Hexachlorocyclohexane EPA 3541/3640A EPA 8081B 1.0 7.2 11 Phthalate esters Di-n-butyl phthalate EPA 3541/3640A EPA 8270D 20 380 1,000 Bis(2-ethylhexyl)phthalate EPA 3541/3640A EPA 8270D 100 500 22,000 Di-n-octyl phthalate EPA 3541/3640A EPA 8270D 10 39 >1,100 Phenols Phenol EPA 3541/3640A EPA 8270D 30 120 210 4-Methylphenol EPA 3541/3640A EPA 8270D 10 260 2,000 Pentachlorophenol EPA 3541/3640A EPA 8270D 100 1,200 >1,200 Miscellaneous extractables Benzoic acid EPA 3541/3640A EPA 8270D 400 2,900 3,800 Dibenzofuran EPA 3541/3640A EPA 8270D 10 200 680 Carbazole EPA 3541/3640A EPA 8270D 10 900 1,100

Pesticides (µg/kg dw) 2,4'-DDD EPA 3541/3620C/3660B EPA 8081B 1.0 310 860 2,4'-DDE EPA 3541/3620C/3660B EPA 8081B 1.0 21 33 2,4'-DDT EPA 3541/3620C/3660B EPA 8081B 1.0 100 8,100 4,4'-DDD EPA 3541/3620C/3660B EPA 8081B 1.0 310 860 4,4'-DDE EPA 3541/3620C/3660B EPA 8081B 1.0 21 33 4,4'-DDT EPA 3541/3620C/3660B EPA 8081B 1.0 100 8,100 Dieldrin EPA 3541/3620C/3660B EPA 8081B 1.0 4.9 9.3 Endrin ketone EPA 3541/3620C/3660B EPA 8081B 1.0 8.5 >8.5

Integral Consulting Inc. 2 of 3 Nippon Dynawave Packaging Property Sediment Sampling and Analysis Plan October 27, 2017

Table 5-1. Chemical Parameters, Analytical Methods, and SMS Criteria

SMS Freshwater a Sediment Parameter Prep/Cleanup Method Analysis Method SQLs SCO CSL PCB Aroclors (µg/kg dw) Aroclor 1016 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1221 EPA 3541/3665A/3620C/3660B EPA 8082A 0.20 ------Aroclor 1232 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1242 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1248 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1254 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1260 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1262 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Aroclor 1268 EPA 3541/3665A/3620C/3660B EPA 8082A 0.10 ------Total PCB Aroclors EPA 3541/3665A/3620C/3660B EPA 8082A --- 110 2,500

Bulk Petroleum Hydrocarbons (mg/kg dw) TPH-Diesel NWTPH-Dx NWTPH-Dx 25 340 510 TPH-Residual NWTPH-Dx NWTPH-Dx 100 3,600 4,400 Notes: ALS = ALS Environmental ASTM = ASTM International CSL = cleanup screening level Ecology = Washington State Department of Ecology EPA = U.S. Environmental Protection Agency NWTPH = Northwest total petroleum hydrocarbon analytical method PAH = polycyclic aromatic hydrocarbon PCB = polychlorinated biphenyl SCO = sediment cleanup objective SM = Standard Method for the Examination of Water and Wastewater SMS = Sediment Management Standards (Washington State Guidelines) SOP = standard operating procedure SQL = sample quantitation limit TPH = total petroleum hydrocarbons

a SMS Freshwater criteria from SCUM II Table 8-1 (Ecology 2015c).

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Table 5-2. Performance Standards and Interpretive Criteria for Freshwater Bioassays

Performance Standard Biological Test a b c c Endpoint Control Reference SCO CSL Hyalella azteca

10-day Mortality MC < 20% MR < 25% MT – MC > 15% MT – MC > 25%

Chironomus dilutus

20-Day mortality MC < 32% MR < 35% MT – MC > 15% MT – MC > 25%

d MIGC ≥ 0.60 20-Day growth RF / CF ≥ 0.8 MIGT / MIGC < 0.75 MIGT / MIGC < 0.60 mg/individual e

Source: Ecology. 2015c. Sediment Cleanup Users Manual II. Publication No. 12-09-057. March.

Notes: M = Mortality; C = Control; R = Reference; T = Test; F = Final; MIG = Mean Individual Growth at time final; mg = milligrams CSL = cleanup screening level Ecology = Washington State Department of Ecology QA/QC = quality assurance and quality control SCO = sediment cleanup objective

a These tests and parameters were developed based on the most updated American Society for Testing and Materials (ASTM International) protocols.

b Reference performance standards are provided for sites where Ecology has approved a freshwater reference sediment site(s) and reference results will be substituted for control in comparing test sediment to criteria.

c An exceedance of the sediment cleanup objective and cleanup screening level requires statistical significance at p = 0.05.

d Results should be reported on an Ash Free Dry Weight basis.

e The control performance standard for the 20 day test (0.60 mg/individual) is more stringent than for the 10 day test and Ecology may consider, on a case-by-case basis, a 20-day control has met QA/QC requirements if the mean individual growth is at least 0.48 mg/individual.

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Table 6-1. Laboratory QA/QC Requirements

Method Analysis Type Blanks a Duplicates a Triplicates a SRM/LCS MS/MSD a Surrogates b Ammonia X X X X Grain size X TOC X X X g X Total solids X Total sulfides X X X X Total volatile solids X X Metals (including mercury) X X X g X Organometallic Compounds (TBT) X X e X g X SVOCs c, d X X e X g X X Pesticides c X X e X g X X PCBs c X X e X f X X Bulk Petroleum Hydrocarbons X X X X

Notes: LCS = laboratory control sample MS/MSD = matrix spike/matrix spike duplicate PAH = polycyclic aromatic hydrocarbon PCB = polychlorinated biphenyl QA/QC = quality assurance and quality control SRM = standard reference material SVOC = semivolatile organic compound TOC = total organic carbon

a Frequency of analysis is 5 percent or one per batch, whichever is more frequent. b Surrogate spikes required for every sample, including matrix spiked samples, blanks, and reference materials. c Initial calibration required before any samples are analyzed, after each major disruption of equipment, and when ongoing calibration fails to meet criteria. Ongoing calibration required at the beginning of each work shift, every 10–12 samples or every 12 hours (whichever is more frequent), and at the end of each shift. d Includes PAHs, chlorinated hydrocarbons, phthalate esters, phenols, and miscellaneous extractables. e Matrix spike duplicate will be run. f Puget Sound Sediment Reference Material will be analyzed for PCBs at a frequency of one per sampling event. g The following SRMs will be used for this project: - SVOCs: CRM 143-050 - Pesticides: SRM 1944 - Metals/Hg: D079-540 - TOC: NIST-1941B - TBT: PACS-2

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Table 6-2. Project Data Quality Objectives

Duplicate Matrix Spike Blank Spike/LCS Analysis Type RPD %R RPD %R RPD Completeness Conventionals Ammonia 32% 55-135 NA 90-110 32% 95% Grain size 20% NA NA NA NA 95% Total organic carbon 20% 72-122 NA 72-122 20% 95% Total solids 20% NA NA NA NA 95% Total sulfides 20% 45-150 NA 55-130 20% 95% Total volatile solids 20% NA NA 85-115 20% 95%

Metals Arsenic 20% 70-130 20% 78-122 20% 95% Cadmium 20% 70-130 20% 81-119 20% 95% Chromium 20% 70-130 20% 80-119 20% 95% Copper 20% 70-130 20% 83-116 20% 95% Lead 20% 70-130 20% 79-121 20% 95% Mercury 20% 70-130 20% 81-118 20% 95% Nickel 20% 70-130 20% 74-143 20% 95% Selenium 20% 70-130 20% 81-129 20% 95% Silver 20% 70-130 20% 73-121 20% 95% Zinc 20% 80-120 20% 72-128 20% 95%

Organometallic Compounds Monobutyltin ion 40% 10-124 40% 10-150 40% 95% Dibutyltin ion 40% 10-133 40% 12-136 40% 95% Tributyltin ion 40% 10-115 40% 10-122 40% 95% Tetrabutyltin ion 40% 16-126 40% 19-130 40% 95%

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Table 6-2. Project Data Quality Objectives

Duplicate Matrix Spike Blank Spike/LCS Analysis Type RPD %R RPD %R RPD Completeness SVOCs PAHs 2-Methylnaphthalene 40% 19-99 40% 27-96 40% 95% Acenaphthene 40% 10-132 40% 32-91 40% 95% Acenaphthylene 40% 20-106 40% 33-99 40% 95% Anthracene 40% 14-113 40% 40-98 40% 95% Benz(a)anthracene 40% 10-137 40% 44-108 40% 95% Benzo(a)pyrene 40% 13-126 40% 42-110 40% 95% Benzo(b)fluoranthene 40% 23-122 40% 46-106 40% 95% Benzo(g,h,i)perylene 40% 20-121 40% 44-108 40% 95% Benzo(k)fluoranthene 40% 28-119 40% 47-107 40% 95% Chrysene 40% 10-146 40% 46-108 40% 95% Dibenz(a,h)anthracene 40% 27-123 40% 47-106 40% 95% Fluoranthene 40% 10-142 40% 42-104 40% 95% Fluorene 40% 12-129 40% 32-96 40% 95% Indeno(1,2,3-c,d)pyrene 40% 22-129 40% 47-109 40% 95% Naphthalene 40% 12-104 40% 27-93 40% 95% Phenanthrene 40% 15-121 40% 39-98 40% 95% Pyrene 40% 17-129 40% 45-106 40% 95% Chlorinated hydrocarbons (µg/kg dw) beta-Hexachlorocyclohexane 40% 35-110 40% 27-137 40% 95% Phthalate esters (µg/kg dw) Di-n-butyl phthalate 40% 27-125 40% 42-109 40% 95% Bis(2-ethylhexyl)phthalate 40% 20-138 40% 47-110 40% 95% Di-n-octyl phthalate 40% 32-132 40% 45-109 40% 95%

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Table 6-2. Project Data Quality Objectives

Duplicate Matrix Spike Blank Spike/LCS Analysis Type RPD %R RPD %R RPD Completeness Phenols (µg/kg dw) Phenol 40% 15-98 40% 27-97 40% 95% 4-Methylphenol 40% 10-104 40% 17-99 40% 95% Pentachlorophenol 40% 10-123 40% 21-97 40% 95% Miscellaneous extractables (µg/kg dw) Benzoic acid 40% 10-126 40% 10-96 40% 95% Dibenzofuran 40% 21-106 40% 34-92 40% 95% Carbazole 40% 10-136 40% 37-95 40% 95%

Pesticides (µg/kg dw) 2,4'-DDD 40% 29-113 40% 41-121 40% 95% 2,4'-DDE 40% 18-116 40% 34-125 40% 95% 2,4'-DDT 40% 38-110 40% 40-121 40% 95% 4,4'-DDD 40% 31-106 40% 37-136 40% 95% 4,4'-DDE 40% 28-113 40% 42-137 40% 95% 4,4'-DDT 40% 29-122 40% 42-137 40% 95% Dieldrin 40% 33-104 40% 39-130 40% 95% Endrin Ketone 40% 40-106 40% 41-130 40% 95%

Total PCB Aroclors Aroclor 1016 40% 23-145 40% 42-122 40% 95% Aroclor 1221 40% NA NA NA NA 95% Aroclor 1232 40% NA NA NA NA 95% Aroclor 1242 40% NA NA NA NA 95% Aroclor 1248 40% NA NA NA NA 95% Aroclor 1254 40% NA NA NA NA 95% Aroclor 1260 40% 24-148 40% 50-124 40% 95%

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Table 6-2. Project Data Quality Objectives

Duplicate Matrix Spike Blank Spike/LCS Analysis Type RPD %R RPD %R RPD Completeness Aroclor 1262 40% NA NA NA NA 95% Aroclor 1268 40% NA NA NA NA 95% Total PCB Aroclors NA NA NA NA NA 95%

Bulk Petroleum Hydrocarbons TPH-Diesel 40% 23-144 40% 42-34 40% 95% TPH-Residual 40% 29-167 40% 48-141 40% 95% Notes: %R = percent recovery LCS = laboratory control sample NA = not applicable PAH = polycyclic aromatic hydrocarbon PCB = polychlorinated biphenyl RPD = relative percent difference SVOC = semivolatile organic compound TPH = total petroleum hydrocarbon

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APPENDIX A STANDARD OPERATING PROCEDURES

SOP AP‐01 Revision: April 2008

STANDARD OPERATING PROCEDURE (SOP) AP-01

SAMPLE PACKAGING AND SHIPPING

SCOPE AND APPLICATION

This SOP describes specific requirements for sample packaging and shipping to ensure the proper transfer and documentation of environmental samples collected during field operations. Procedures for the careful and consistent transfer of samples from the field to the laboratory are outlined herein. This SOP also presents the method to be used when packing samples that will either be hand delivered or shipped by commercial carrier to the laboratory.

EQUIPMENT AND SUPPLIES REQUIRED

Make sure that you have the equipment and supplies necessary to properly pack and ship environmental samples, including the following: • Project‐specific sampling and analysis plan (SAP) • Project‐specific field logbook • Sealable airtight bags in assorted sizes (e.g., Ziploc®) • Wet ice in doubled, sealed bags; frozen Blue Ice®; or dry ice • Cooler(s) • Bubble wrap • Fiber‐reinforced packing tape, clear plastic packing tape, and duct tape • Scissors or knife • Chain‐of‐custody (COC) forms • COC seals • Large plastic garbage bags (preferably 3 mil [0.003 in.] thick) • Paper towels • “Fragile,” “This End Up,” or “Handle With Care” labels • Mailing labels • Air bills for overnight shipment

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PROCEDURE

Customize the logistics for sample packaging and shipping to each study. If necessary, transfer samples from the field to a local storage facility where they can be frozen or refrigerated. Depending on the logistics of the operation, field personnel may transport samples to the laboratory or use a commercial courier or shipping service. In the latter case, Integral field personnel must be aware of any potentially limiting factors to timely shipping, such as availability of overnight service and weekend deliveries to specific areas, and shipping regulations regarding “restricted articles” (e.g., dry ice, formalin) prior to shipping the samples.

SAMPLE PREPARATION

Take the following steps to ensure the proper transfer of samples from the field to the laboratories: At the sample collection site: 1. Document all samples using the proper logbooks or field forms (see SOP AP‐02), required sample container identification (i.e., sample labels with tag numbers), and COC form (example provided in SOP AP‐03). Fill out the COC form as described in SOP AP‐03, and use the sample labeling techniques provided in SOP AP‐04. 2. Make all applicable laboratory quality control sample designations on the COC forms. Clearly identify samples that will be archived for future possible analysis. Label these samples as follows: “Do Not Analyze: Hold and archive for possible future analysis.” Some laboratories interpret “archive” to mean that they should continue holding the residual sample after analysis. 3. Notify the laboratory contact and the Integral project quality assurance/quality control (QA/QC) coordinator that samples will be shipped and the estimated arrival time. Send copies of all COC forms to Integral’s project QA/QC coordinator or project manager, as appropriate. 4. Keep the samples in the possession of the sampling personnel at all times. Lock and secure any temporary onsite sample storage areas to maintain sample integrity and COC requirements. 5. Clean the outside of all dirty sample containers to remove any residual material that may lead to cross‐contamination. 6. Complete the COC form as described in SOP AP‐03, and retain the back (pink) copy for project records prior to sealing the cooler. Check sample containers against the COC form to ensure all the samples that were collected are in the cooler.

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7. Store each sample container in a sealed plastic bag that allows the sample label (example provided in SOP AP‐03) to be read. Before sealing the bags, ensure that volatile organic analyte (VOA) vials are encased in a foam sleeve or in bubble wrap. 8. If the samples require storage at a specific temperature, place enough ice in the sample cooler to maintain the temperature (e.g., 4°C) throughout the sampling day. At the sample processing area (immediately after sample collection) take the following steps: 1. If the samples require a specific storage temperature, then cool the samples and maintain the temperature prior to shipping. For example, place enough ice in each sample cooler to maintain the temperature at 4°C until processing begins at the testing laboratory. 2. Be aware of holding time requirements for project‐specific analytes and arrange the sample shipping schedule accordingly. 3. Place samples in secure storage (i.e., locked room or vehicle) or keep them in the possession of Integral sampling personnel before shipment. Lock and secure any sample storage areas to maintain sample integrity and COC requirements. 4. Store samples in the dark (e.g., keep coolers shut). At the sample processing area (just prior to shipping), do the following: 1. Check sample containers against the COC form to account for all samples intended for shipment. 2. Choose cooler(s) of appropriate size and make sure they are clean of gross contamination inside and out. If the cooler has a drain, close the drain and secure it with duct tape. 3. Line the cooler with bubble wrap and place a large plastic bag (preferably with a thickness of 3 mil), open, inside the cooler. 4. Individually wrap each glass container (which was sealed in a plastic bag at the collection site) in bubble wrap and secure with tape or a rubber band. Place the wrapped samples in the large plastic bag in the cooler, leaving room for ice to keep the samples cold (i.e., 4°C). 5. If temperature blanks have been provided by the testing laboratory, place one temperature blank in each sample cooler. 6. If the samples require a specific storage temperature, add enough wet ice or Blue Ice ® to maintain that temperature during overnight shipping (i.e., 4°C). Always overestimate the amount of ice that will be required. Keep ice in a sealed plastic bag, which is placed in a second sealed plastic bag to prevent leakage. Avoid separating the samples from the ice with excess bubble wrap because it may insulate the samples from the ice. After adding all samples and ice to the cooler, use bubble wrap (or other

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available clean packing material) to fill any empty space and prevent the samples from shifting during transport. 7. If possible, consolidate all VOA samples in a single cooler and ship them with (a) trip blank(s) if the project‐specific QA project plan calls for them. 8. Sign, date, and include any tracking numbers provided by the shipper on the COC form. Remove the back (pink) copy of the original COC form and retain this copy for the project records. 9. Seal the rest of the signed COC form in a bag and tape the bag to the inside of the cooler lid. Each cooler should contain an individual COC form for the samples contained inside it. If time is short and it becomes necessary to combine all the samples onto a single set of COC forms and ship multiple coolers together, then indicate on the outside of the appropriate cooler, “Chain‐of‐Custody Inside.” 10. After the cooler is sufficiently packed to prevent shifting of the containers, close the lid and seal it with fiber‐reinforced packing tape. Tape the cooler around the opening, joining the lid to the bottom, and around the circumference of the cooler at both hinges. 11. As security against unauthorized handling of the samples, apply two COC seals across the opening of the cooler lid (provided with example field forms). Place one seal on the front right portion of the cooler and one on the back left. Be sure the seals are properly affixed to the cooler to prevent removal during shipment. Additional tape across the seal may be necessary if the outside of the cooler is wet.

SAMPLE SHIPPING

Hand Delivery to the Testing Laboratory

1. Notify the laboratory contact and the Integral project QA/QC coordinator that samples will be delivered to the laboratory and the estimated arrival time. 2. When hand‐delivering environmental samples, make sure the testing laboratory receives them on the same day that they were packed in the coolers. 3. Fax or scan and e‐mail copies of all COC forms to the Integral project QA/QC coordinator. Note: It may be necessary to photocopy the COC form on a slightly darker setting so the form is readable after it has been faxed. Never leave the original COC form in the custody of non‐Integral staff.

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Shipped by Commercial Carrier to the Laboratory

1. Apply a mailing label to the cooler with destination and return addresses, and add other appropriate stickers, such as “This End Up,” “Fragile,” and “Handle With Care.” If the shipment contains multiple coolers, indicate on the mailing label the number of coolers that the testing laboratory should expect to receive (e.g., 1 of 2; 2 of 2). Place clear tape over the mailing label to firmly affix it to the cooler and to protect it from the weather. This is a secondary label in case the air bill is lost during shipment. 2. Fill out the air bill and fasten it to the handle tags provided by the shipper (or the top of the cooler if handle tags are not available). 3. If samples must be frozen (–20°C) during shipping, make sure that dry ice has been placed in the sample cooler. Be aware of any additional shipping, handling, and special labeling requirements that the shipper may require. 4. Make sure that benthic infauna samples have been preserved with formalin in the field prior to shipping. Be aware of any additional shipping, handling, and special labeling requirements that the shipper may require for these samples. 5. Notify the laboratory contact and the Integral project QA/QC coordinator that samples will be shipped and the estimated arrival date and time. If environmental samples must be shipped at 4°C or –20°C, choose overnight shipping for delivery next morning. Fax or scan and e‐mail copies of all COC forms to the Integral project QA/QC coordinator. Note: It may be necessary to photocopy the COC form on a slightly darker setting so the form is readable after faxing. Never leave the original COC form in the custody of non‐Integral staff.

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STANDARD OPERATING PROCEDURE (SOP) AP-03

SAMPLE CUSTODY

SCOPE AND APPLICATION

This SOP describes Integral procedures for custody management of environmental samples. A stringent, established program of sample chain‐of‐custody will be followed during sample storage and shipping activities to account for each sample. The procedure outlined herein will be used with SOP AP‐01, which covers sample packaging and shipping; SOP AP‐02, which covers the use of field logbooks and other types of field documentation; and SOP AP‐04, which covers sample labeling. Chain‐of‐custody (COC) forms ensure that samples are traceable from the time of collection through processing and analysis until final disposition. A sample is considered to be in a person’s custody if any of the following criteria are met: 1. The sample is in the person’s possession 2. The sample is in the person’s view after being in his or her possession 3. The sample is in the person’s possession and is being transferred to a designated secure area 4. The sample has been locked up to prevent tampering after it was in the person’s possession. At no time is it acceptable for samples to be outside of Integral personnel’s custody unless the samples have been transferred to a secure area (i.e., locked up). If the samples cannot be placed in a secure area, then an Integral field team member must physically remain with the samples (e.g., at lunch time one team member must remain with the samples).

CHAIN-OF-CUSTODY FORMS

The COC form is critical because it documents sample possession from the time of collection through final disposition. The form also provides information to the laboratory regarding what analyses are to be performed on the samples that are shipped. Complete the COC form after each field collection activity and before shipping the samples to the laboratory. Sampling personnel are responsible for the care and custody of the samples until they are shipped. The individuals relinquishing and receiving the samples must sign the

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COC form(s), indicating the time and date of the transfer, when transferring possession of the samples. A COC form consists of three‐part carbonless paper with white, yellow, and pink copies. The sampling team leader keeps the pink copy. The white and yellow sheets are placed in a sealed plastic bag and secured inside the top of each transfer container (e.g., cooler). Field staff retain the pink sheet for filing at the Integral project manager’s location. Each COC form has a unique four‐digit number. This number and the samples on the form must be recorded in the field logbook. Integral also uses computer‐generated COC forms. If computer‐generated forms are used, then the forms must be printed in triplicate and all three sheets signed so that two sheets can accompany the shipment to the laboratory and one sheet can be retained on file. Alternatively, if sufficient time is available, the computer‐generated forms will be printed on three‐part carbonless paper. Record on the COC form the project‐assigned sample number and the unique tag number at the bottom of each sample label. The COC form also identifies the sample collection date and time, type of sample, project name, and sampling personnel. In addition, the COC form provides information on the preservative or other sample pretreatment applied in the field and the analyses to be conducted by referencing a list of specific analyses or the statement of work for the laboratory. The COC form is sent to the laboratory along with the sample(s).

PROCEDURES

Use the following guidelines to ensure the integrity of the samples: 1. Sign and date each COC form. Have the person who relinquishes custody of the samples also sign this form. 2. At the end of each sampling day and prior to shipping or storage, make COC entries for all samples. Check the information on the labels and tags against field logbook entries. 3. Do not sign the COC form until the team leader has checked the information for inaccuracies. Make corrections by drawing a single line through any incorrect entry, and then initial and date it. Make revised entries in the space below the entries. After making corrections, mark out any blank lines remaining on the COC form, using single lines that are initialed and dated. This procedure will prevent any unauthorized additions. At the bottom of each COC form is a space for the signatures of the persons relinquishing and receiving the samples and the time and date of the transfer. The time the samples were relinquished should match exactly the time they were received by another party. Under no circumstances should there be any time when custody of the samples is undocumented.

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4. If samples are sent by a commercial carrier not affiliated with the laboratory, such as FedEx or United Parcel Service (UPS), record the name of the carrier on the COC form. Also enter on the COC form any tracking numbers supplied by the carrier. The time of transfer should be as close to the actual drop‐off time as possible. After signing the COC forms and removing the pink copy, seal them inside the transfer container. 5. If errors are found after the shipment has left the custody of sampling personnel, make a corrected version of the forms and send it to all relevant parties. Fix minor errors by making the change on a copy of the original with a brief explanation and signature. Errors in the signature block may require a letter of explanation. 6. Provide a COC form and an Archive Record form for any samples that are archived internally at Integral. Upon completion of the field sampling event, the sampling team leader is responsible for submitting all COC forms to be copied. A discussion of copy distribution is provided in SOP AP‐02.

CUSTODY SEAL

As security against unauthorized handling of the samples during shipping, affix two custody seals to each sample cooler. Place the custody seals across the opening of the cooler (front right and back left) prior to shipping. Be sure the seals are properly affixed to the cooler so they cannot be removed during shipping. Additional tape across the seal may be prudent.

SHIPPING AIR BILLS

When samples are shipped from the field to the testing laboratory via a commercial carrier (e.g., FedEx, UPS), the shipper provides an air bill or receipt. Upon completion of the field sampling event, the sampling team leader will be responsible for submitting the sender’s copy of all shipping air bills to be copied at an Integral office. A discussion of copy distribution is provided in SOP AP‐02. Note the air bill number (or tracking number) on the applicable COC forms or, alternatively, note the applicable COC form number on the air bill to enable the tracking of samples if a cooler becomes lost.

ACKNOWLEDGMENT OF SAMPLE RECEIPT FORMS

In most cases, when samples are sent to a testing laboratory, an Acknowledgment of Sample Receipt form is faxed to the project QA/QC coordinator the day the samples are received by the laboratory. The person receiving this form is responsible for reviewing it, making sure that the laboratory has received all the samples that were sent, and verifying that the correct analyses were requested. If an error is found, call the laboratory immediately, and document

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any decisions made during the telephone conversation, in writing, on the Acknowledgment of Sample Receipt form. In addition, correct the COC form and fax the corrected version to the laboratory. Submit the Acknowledgment of Sample Receipt form (and any modified COC forms) to be copied. A discussion of copy distribution is provided in SOP AP‐02.

ARCHIVE RECORD FORMS

On the rare occasion that samples are archived at an Integral office, it is the responsibility of the project manager to complete an Archive Record form. This form is to be accompanied by a copy of the COC form for the samples, and will be placed in a locked file cabinet. The original COC form remains with the samples in a sealed Ziploc® bag.

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STANDARD OPERATING PROCEDURE (SOP) AP-06

NAVIGATION AND STATION POSITIONING

SCOPE AND APPLICATION

This SOP describes procedures for accurate station positioning required to ensure quality and consistency in collecting samples and in data interpretation and analysis. Station positioning must be both absolutely accurate in that it correctly defines a position by latitude and longitude, and relatively accurate in that the position must be repeatable, allowing field crew to reoccupy a station location in the future (e.g., for long‐term monitoring programs). This SOP describes the most commonly used station positioning method, differential global positioning system (DGPS). Integral uses a Trimble Pathfinder™ Pro XRS DGPS for station positioning for many field efforts. The Pro XRS offers the submeter accuracy often required for documenting sampling station locations and for re‐locating previously sampled stations. A comprehensive discussion of the Trimble Pathfinder™ Pro XRS DGPS is provided in Attachments 1, 2, and 3 of this SOP.

SUMMARY OF METHOD

Global positioning system (GPS) navigation is used to position the sampler at the desired location. GPS is a satellite‐based system that receives positioning data at 1‐second intervals from multiple satellites at known positions in space. Standard GPS is calculated to an accuracy of about 10 m. One can obtain a higher accuracy of approximately 2 m by applying differential corrections to the standard GPS positioning data using DGPS. These differential corrections are applied by sending GPS differential corrections to the GPS receiver via radio transmission. If the sampling location is near the coastal U.S, the U.S. Coast Guard generates differential corrections that are transmitted via radio link to the GPS receiver. If a Coast Guard station is out of range of the sampling area, then a receiver may be set up at a known (i.e., surveyed) reference point on land, or real‐time satellite differential signals can be purchased from a private company (e.g., OmniSTAR). With the Pro XRS, GPS data can be gathered to submeter accuracy using a choice of differential correction sources (i.e., free beacon differential signals such as Coast Guard beacons or OmniSTAR) without establishing a reference station. Data must be corrected to gain submeter accuracy. Free beacon or base station signals allow differential corrections to be

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performed after data collection by using a nearby beacon or base station logging data files. (Note: The station must be within 300 miles of the data collection location.) For satellite‐based signals, a built‐in virtual base station allows for real‐time data correction, eliminating the need for post‐processing data in some cases. However, postprocessing data corrections can obtain accuracies in the range of 30–50 cm. These accuracies are for the horizontal (northing and easting) component only. The vertical component (elevation) accuracy ranges from submeter to 3 times larger than the horizontal accuracy. The GPS receiver displays and transmits differentially corrected positioning data to the computer using an integrated navigation software package (e.g., HYPACK, Terrasync). The computer data are typically displayed and recorded in World Geodetic System of 1984 (WGS‐ 1984) geographic coordinates (latitude/longitude). However, the integrated navigation system can display and record information in other datums (e.g., UTM, NAD83). The integrated navigation system, acting as a data manager, displays the sampler’s position relative to a target station location in plan view on a video screen. The resulting pictorial screen presentation, as well as numeric navigation data (e.g., range and bearing to the target sampling location) assists the vessel operator (when sampling on‐water) in approaching and maintaining the station position while sampling.

SUPPLIES AND EQUIPMENT

• Cable • GPS antenna • Telemetry antenna (for differential corrections) • GPS receiver • Differential corrections receiver • Computer and monitor • Navigation software (e.g., Terrasync) • Logbook or log sheets.

PROCEDURES

Obtain latitude and longitude coordinates at the locations where samples are collected. An average positioning objective is to accurately determine and record the positions of all sampling locations to within 2 m. Positioning accuracies on the order of 1–3 m can be achieved by avoiding the few minutes per day when the satellites are not providing the same level of signal. The GPS provides the operator with a listing of the time intervals during the

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day when accuracies are decreased. Avoiding these times allows for better positioning accuracy.

On-Land Sampling Event

A backpack DGPS unit may be used to direct the sampling team to the proposed sampling location. To expedite field activities, enter the target station coordinates into the navigation system database prior to beginning sampling. Place the DGPS antenna as close as possible to where the sampling will occur. Once the sample(s) have been collected at the appropriate location, record the horizontal coordinates of the station in the field logbook.

On-Water Sampling Event

Mount the GPS antenna vertically at the outboard end of the vessel’s boom, with the GPS antenna cable extended along the boom into the cabin. Mount the telemetry antenna for receiving differential corrections on a convenient fixture outside the cabin. Locate the GPS receiver, the differential corrections receiver, and the computer in the cabin. Orient the video screen for the computer to allow the vessel operator to observe on‐screen positioning data from the helm. Alternatively, use a backpack DGPS unit to position the sampling vessel (e.g., barge) over a proposed sampling location. Place the DGPS beacon as close as possible to where the drilling will occur (i.e., moon pool). Using the DGPS unit, direct the sampling vessel operator to the sample station location. Once the sampling vessel is anchored at the appropriate location, record the horizontal coordinates of the station in the field logbook. To expedite field activities, enter the target station coordinates in the navigation system database prior to beginning sampling.

Positioning System Verification

GPS requires no calibration, as all signal propagation is controlled by the U.S. government (the Department of Defense for satellite signals and the U.S. Coast Guard for differential corrections). Verifying the accuracy of the GPS requires coordinates to be known for one (or more) horizontal control point within the study area. The GPS position reading at any given station can then be compared to the known control point. Verify the GPS accuracy at the beginning and end of each sampling day.

Station Positioning Activities

Use a consistent routine for each day’s positioning activities. After confirming successful reception of differential signals, turn on the computer on, and the boot the software. Verify the accuracy of the system at a horizontal control point, as described in the previous section.

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The sampling team proceeds to a target station location selected by the team leader. That station location is then selected from a number of preselected station locations that have been entered into the integrated navigation system database. Once the station has been selected, the positioning data are displayed on the computer screen or hand‐held unit to assist in proceeding to the station and in maintaining the station position during sampling. A confirmed position is recorded electronically each time a sample collection is attempted. (This means that during sediment grab sampling and coring, the locations of both accepted and rejected grabs or cores are recorded.) Upon recovery of the sampling device, read the station position northing (y) and easting (x) coordinates from the archived computer file and record them in the field logbook or on log sheets as a backup to the computer record. Also record time and water depth, if applicable. Ancillary information recorded in the field logbook may include personnel operating the GPS, tidal phase, type of sampling activity, and time when coordinates were collected.

REFERENCES

Trimble Navigation Limited. 2001. TSC1 Asset Surveyor operation manual. Version 5.20. http://trl.trimble.com/dscgi/ds.py/Get/File‐8145/Oper.pdf. Trimble Navigation Limited. 2007. GPS tutorial. Accessed on January 12, 2007. http://www.trimble.com/gps/index.shtml.

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ATTACHMENT 1 PRO XRS DESCRIPTION

The Pro XRS combines a high‐performance GPS receiver and antenna, beacon differential receiver, and satellite differential receiver in one compact unit. It also includes Trimble’s advanced Everest™ technology, which allows users to collect accurate position data near walls, water, vehicles, or other surfaces that reflect satellite signals. Reflected signals, also called multipath signals, make it difficult for GPS receivers to accurately determine position. Everest™ uses a patented technique to remove multipath signals before measurements are used to calculate position.

Equipment Required

The GPS Pathfinder™ Pro XRS consists of the following: • GPS receiver in backpack casing (with system batteries and cables) • Hand‐held data logger (TSC1) and cable, or laptop computer with Terrasync software installed and cable. (Note: Terrasync procedures are described under separate cover.) • Pro XRS antenna, range poles, and cable • Compass and tape measure • Spare 12‐volt camcorder and 9‐volt batteries (minimum of two each) (use only Kodak, Duracell, or Energizer 9‐volt batteries) • Battery charger and power cord.

Pro XRS Setup

Follow these procedures for the proper setup of the Pro XRS: 1. Ensure that connections between batteries, receiver, and data logger are correct and secure. The coaxial antenna cable connects from the GPS receiver port “ANT” to the base of the antenna. The TSC1 cable (a “pig‐tail”‐type cable) connects from the bottom or top of the TSC1 to the receiver port “B,” where a 9‐pin serial port dongle is attached. The dual Y‐clip cables should be connected from the receiver to the batteries. Alternatively, if AC power is available (e.g., aboard a vessel), then the power cable for the battery charger can be attached directly to the receiver on some models. 2. Screw the three long antenna poles together (the shorter pole may be added if necessary for taller users). Screw on the antenna and connect its cable. 3. Put backpack and/or shoulder strap on. The pouch for the data logger should be in place around the waist strap or in the backpack.

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4. Screw antenna to the attachments on the top of the backpack. Wind cord around pole, and ensure the antenna is secure. Please be aware of overhead hazards, especially if working near low‐hanging power lines. Severe injury or death can result.

Basic Operation of the Pro XRS

Recording a Feature Before beginning field use, ensure that all GPS configurations and settings are set correctly for the particular use of the Pro XRS and that an appropriate data dictionary is loaded onto the TSC1 (see Attachments 2 and 3 for typical settings). These steps outline the basic use of the GPS to document a sample position or any other defined “feature.” Note that the TSC1 has both hard and soft keys that allow for its operation. The hard keys comprise all of the keys (e.g., letters and numbers) on its surface. The soft keys are the F1 through F5 hard keys. The function of these changes depending upon the context. These keys will be referred to with brackets around them (). 1. Turn data logger on outside in an open area. Wait for antenna to receive satellite signals. The display will read Recording Almanac, Too Few SVs, and PDOP Too High. Continue to wait until enough satellites (four) are acquired and the PDOP is below 5.0. 2. Ensure that the real‐time settings are correct according to the parameters listed in Attachment 2. 3. Select Data Collection, and create a new rover file or open an existing file. This file should be named according to the format specified by the project GIS analyst. Note: If opening an existing file, press to access the Antenna Options menu and Start Feature menu. 4. Enter the height of the antenna from the ground to the Measurement Method reference point shown in the Antenna Options menu and then press ENTER to bring up the Start Feature menu. 5. Pick the appropriate data dictionary to use with the rover file. Only one dictionary can be used with a rover file. Consult with the project GIS analyst to formulate the most appropriate data dictionary for the type of sampling you wish to perform. The data dictionary titled Generic contains only a comment field and is appropriate for simple navigation tasks. If using a data dictionary, make sure to become familiar with its attributes before recording information in the field.

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6. Move to the location of the first feature for which you want to record the GPS position. Select the appropriate feature and press ENTER to begin logging. Log data points in accordance with the feature type. Point features should have at least 10 points collected at a stationary location. Line features should be collected while moving. If movement is stopped, press the key. When movement starts again, press the key. Area features should be collected with enough points to define the outline of the area (e.g., a square building would have four single points, collected on each corner, and the key would be used between each of the points). 7. Depending on the setup of the data dictionary, each feature may have one or more feature attributes. An attribute is used to record additional data associated with the feature. For example, the attributes assigned to a sediment sampling station could be the sample number, station ID, sampling gear, sediment color, odor, etc. 8. Use the key while recording feature attributes to avoid too many data points being collected at one point feature. (Body movements while logging attributes for an extended time can decrease the accuracy of collection.) The key must be used when recording attributes of a line or area feature because only one data point should be collected in a single location. 9. Once all attributes are entered and the feature data points are logged, press ENTER to complete and save the feature and move on to a new feature. Pressing ESC instead of ENTER will allow the user to abandon the logged feature without saving. 10. When all features in a given area have been recorded, from the Data Collection menu, press ESC to exit data capture and then press to close the file. Features are appended and saved to the file after each collection, so there is no need to “save” the file. When the Pro XRS is not in use, it should be turned off. If you need to come back to the same rover file later in the day, the rover file may be reopened at that time. Rover files may not be edited after 7 days from the first feature was created. Please consult the project GIS analyst for the best way to handle multi‐week sampling projects. 11. At the end of each day, download the rover file to a PC using Pathfinder Office software.

Feature Collection Options Offsets—The Pro XRS can collect a point or line feature while standing at a set distance away from the feature. This option may be necessary because of obstructions such as tree cover, buildings, or car traffic. For a point feature, measure the distance between the object you want recorded and the Pro XRS antenna. Use the compass to determine the bearing (e.g., west is 270°). The bearing is the direction the point should be moved for it to be located in the correct place (e.g., if you are due north of the feature, the bearing is south, or 180°; i.e., the position you want recorded is south of where you are standing). Estimate the inclination from the

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feature to the GPS antenna (if altitude determination is critical, a clinometer should be used). The inclination is the degree angle up from the feature to the antenna (e.g., if the feature is 5° below the antenna position, enter −5°). During data capture, from within the feature, press the button, and enter the distance, bearing, and inclination. Press OK to complete the feature. Note: This procedure describes an offset of a single feature. A constant offset may be applied to all features collected as well. Nesting—While recording a line feature or an area feature, a point feature may be collected to avoid backtracking. While recording the line or area feature, press and then . The Pro XRS will prompt for collection of a new feature. Move to the feature, and collect data as for any other point feature. When the feature is complete, press OK. The Pro XRS is ready to resume collecting data as part of the line/area feature: press . (Remember to continue moving before pressing resume to avoid having multiple positions recorded in the same place in the line or area feature.) Segmenting—While moving along a line feature, changing the attributes of that line may be necessary (e.g., because of a change in surface type from paved to dirt road). This change may be done without having to begin a new feature by pressing and then . Change the appropriate attributes and then press to continue recording. Repeat—This function allows the collection of a new feature with the same feature attributes as the previous feature. If features are not exactly the same, it also allows editing of the attributes. Quickmark—Allows collection of point features while moving (e.g., from a car or a boat) by estimating the exact location. The use of this feature will not result in positionally accurate locations and is not recommended for most sampling operations.

Reviewing and Editing Features

It is possible to review or edit features collected in the field while still in the data capture mode. For example, it may be necessary to document the GPS location in the field logbook or to edit one of the feature’s attributes. Without exiting data capture, press . (If data capture is already complete, just press and then select the appropriate rover file.) This step will display a list of data points including each feature collected. Scroll to the appropriate feature, and follow the steps below depending on the required action: • To view the GPS location (e.g., lat/lon), press . • To edit the attributes, press ENTER. Make any necessary edits to the attributes by scrolling through. • To change or add an offset, press and then . Make any necessary changes. • To delete a feature collected in error, press .

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Navigating to an Existing Location

Waypoints To use the Pro XRS to navigate to a previously established position, this position must be loaded into the data logger as a waypoint, present as a feature position in the data files, or generated in the field using the GPS unit. Waypoints may be entered into the TSC1 by: • Entering coordinates manually • Choosing previously recorded locations and importing them into the TSC1 by using Pathfinder Office • Defining a location stored in a rover file saved to the TSC1 as a waypoint (see Reviewing/Editing Features, above) • Creating a way point from the current position being shown by the operating GPS unit in the field.

Navigating Usually you will use the Navigation module (accessed by pressing MENU followed by Navigation) to guide yourself to a target (waypoint or feature). You can also use the Map module (accessed by pressing MENU followed by Map) to: 1. Orient yourself in the area where you are working. 2. Get a general indication of the location of a feature or waypoint that you want to find. 3. Find or select features or waypoints to which you wish to navigate toward. 4. Plot a course from one place to another. a. While in the Map screen, the GPS cursor x shows the current position reported by the receiver and is always shown on the Map screen (Note: it may not always be within the visible part of the screen when panning or scrolling). The key can be used to hide or display the GPS trail (line of dots showing up to 60 previous positions), the heading showing the direction of travel, and other options on the map display. b. Select a feature by pressing MENU, Data Collection to reach the Start Feature screen, and then to access all features contained in the data file. Highlight and select the desired feature by pressing the key, which adds a crossed flag to the feature. Reaccess the Map screen by selecting MENU, then Map, which will now show the highlighted feature with a crossed flag symbol on the Map screen. You can then start moving toward the feature, and the current position (shown by the x) will move closer to the target position as the user approaches.

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c. There are two graphical modes of navigation with the Pro XRS in the TSC1 Navigation module. On both modes, text information appears on the right of the screen in the Info panels, which can be configured by the user. The graphical modes available are the Directional Dial screen or the Road screen, which can be toggled between using the key. d. To navigate, select a target and then a start position. Each of these positions can be features from an open data file or a waypoint. Access a list of available features or waypoints by pressing or . Once the item has been chosen as a target, it will show the crossed flags symbol in the list. Once a target has been selected, Distance to Go appears at the bottom of the Navigation screen, which indicates the distance from the current GPS position to the target. Select a start position (not required but useful for calculating crosstrack error and other navigation information) by pressing . A waypoint of the current GPS position can be created for use as the Start point by selecting . Once the Start position is selected, a flag symbol will appear next to the item in the list. e. In the Directional Dial mode, an arrow will appear that will always point at the target. This is the bearing to go. (Note: You need to be moving for this to be accurate, as it will lock if you are moving too slowly or have stopped.) The triangle at the top represents the direction that you are going or heading. This triangle never moves, but by changing directions, you can line up the arrow with the triangle. When the two are aligned, you are heading in the direction of the target. When you are close to the target, a bull’s‐eye (two concentric circles) will appear at the edge of the screen. This is warning you that the unit will be switching to the close up screen. A proximity alarm will sound and the directional arrow will be replaced by the bull’s‐eye on the close up screen. Your current position will be shown by an x and the target by the bull’s‐eye. Move so that the x is in the same location as the bull’s‐eye. f. In the Road mode, navigate by walking down a road. Your position is shown by a stick figure and is always positioned in the center of the screen. The target (crossed flags) shows the point to which you are navigating toward. Your heading is shown by the top center of the screen and the bearing to go is shown by the direction of the road, which will rotate as you change your heading. Change your heading until the road is pointing at the top of the screen (Target is also at the top of the screen) and the edges are parallel to the sides of the screen. As you move toward the target the screen zooms in, so the road appears to get wider.

Downloading Rover Files

Upon returning to the office, download all rover files from the TSC1 to a PC for post‐ processing. You will need the Trimble Pathfinder software installed on your computer. If you

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are not using a field laptop that already has the program installed, contact your project GIS analyst for instructions on how to install the software. Connect the TSC1 to your computer using the appropriate cables. In addition to the “pigtail” cable, you will also need a null modem (a 9‐pin female‐to‐female cable) to plug into a PC serial port. Once connected, power up the TSC1 unit and navigate to MENU>File Manager>File Transfer. Then, open the Pathfinder software and navigate to the Utilities>Data Transfer… window from the menu bar. Select GIS Datalogger on COM1 (for most computer systems), and press the green Connect button. Download files from the TSC1 by selecting the Receive tab and choosing the data file type from the Add pulldown menu (Figure 1). After downloading, remove all rover files and waypoints from the TSC1 to conserve memory. Rover files may be deleted from the File Manager menu as follows: 1. Select MENU>File Manager>Delete File(s) 2. Select the rover file to be deleted, and press 3. Confirm the deletion of this file by pressing . Delete data dictionaries in the same manner by selecting Data Dictionaries from the File Manager menu. Delete waypoints by selecting Utilities from the Main menu and then by selecting Waypoints, followed by .

Figure 1. Transferring File from Terrasync

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ATTACHMENT 2 TSC1 SETTINGS

The following are lists of menus that can be accessed through the TSC1 keypad. Please ensure that settings are correct before proceeding. Do not make changes to the settings unless necessary. Each menu will list all available subheadings, the correct setting, and the available to access additional menus. Comments are included only where necessary.

GPS Rover Options

To access this menu, select Configuration from the main menu and then select GPS Rover Options. The table below lists logging options and settings.

Logging Options Setting Comment Logging intervals Point feature 1s Line/area feature 2s–5s depending upon speed of movement Not in feature None Velocity None Confirm end feature No Minimum pos 10 Carrier Mode Off Carrier phase min. time 10 minutes Dynamics code Land May be changed to sea or air, as appropriate Audible click Yes Log DOP data Yes Log PPRT data Yes Log QA/QC data Yes Allow GPS update Warn First Warning Distance Any Position Mode Manual 3D Elevation Mask 15° Should not go below 13° (accuracy decreases) SNR Mask 6.0 Can raise to 7 if multi-path filtering is poor PDOP Mask 5.0 Can be raised up to 8; reduces accuracy PDOP Switch 6.0

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Real-Time Input Options

Access this menu from the GPS Rover Options menu by selecting Real‐Time Input. The table below shows options and settings for real‐time input.

Options Setting Comment Preferred Correction Source Choice 1 Integrated Beacon Choice 2 Integrated WAAS Choice 3 Use uncorrected GPS Correction Age Limit 20s

Antenna Options

Access this menu from the GPS rover Options menu by selecting Antenna Options. The table below shows antenna options and settings.

Option Setting Comment Height 6 ft Enter correct user antenna height using measurement method indicated below Measure Uncorrected Type Integrated GPS/Beacon/Satellite Confirm Per file Can be changed to “Per feature” if antenna height varies and elevation is critical Part Number 33580-50 Auto selected based on TYPE selected Measurement Bottom of Antenna Method Mount

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ATTACHMENT 3 ADDITIONAL SETTINGS FOR THE TSC1

Additional TSC1 settings can be found in the Configuration menu. Items of particular importance are indicated in italics.

Configuration

This menu can be accessed by selecting Configuration from the main menu. The table below lists options and descriptions for the Configuration menu.

Options Description GPS base station options For using a land base station or beacon for real time corrections NMEA/TSIP output Consult manual Coordinate system Changes coordinate system among latitude/longitude, UTM, and other coordinate systems. System can be converted, if necessary, after data capture by using Pathfinder Office software. Map Display options Change layers, scale, background files and items shown on the TSC1 screen during data collection Navigation options Changes Navigation parameters Units and display Changes various units, for example: length (e.g., feet, meters), altitude reference (e.g., MSL), North reference (i.e., true or magnetic). Units can be converted, if necessary, after data capture by using Pathfinder Office software. Time and date Changes to local time, 24-hour clock, date format, and other options Quickmarks Set-up parameters for use with Quickmarks. Constant offset Set-up parameters for use with a constant offset. External sensors Connections with external sensors. Hardware (TSC1) TSC1 settings such as beep volume, contrast, internal and external battery status, software version, free space.

Contrast and Backlighting

The TSC1 display can be viewed in various light settings. Press FUNC, then L to turn on the display backlight for viewing in dim lighting. Adjust the contrast by pressing FUNC, then E or F.

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ATTACHMENT 4 PRE-SAMPLING ACTIVITIES BEFORE USE OF THE PRO XRS

Determination of Optimal Satellite-Use Time

Positioning accuracies on the order of ±1 to 3 m can be achieved by avoiding the few minutes per day when the satellites are not providing the same level of signal. The GPS unit provides the operator with a listing of the time intervals during the day when accuracies are decreased. Avoiding these time intervals permits the operator to maintain better positioning accuracy.

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ATTACHMENT 5 MANAGING GPS DATA FROM TERRASYNC—A TUTORIAL

Currently, positional data collected in the field is most often done with a Trimble GPS unit (usually rented) interfaced with a laptop via Trimble’s Terrasync software. The Terrasync software sometimes exhibits quirks that interfere with the smooth operation of data collection in otherwise stressful field conditions. This tutorial is meant to supplement the Terrasync software documentation and serve as a guide to field personnel to help them retrieve and collect geographic data as efficiently as possible with existing software.

Scope

This document is intended to be a reference for procedures involving the following: • Fixing files that are more than 7 days old so that they can be updated • Adding features in GPS Pathfinder software (companion to Terrasync) and then importing them as base files in Terrasync.. This document is not intended to be a comprehensive manual for using Terrasync or Pathfinder software. It is assumed that the reader has received at least some training on how to use the basic features of Terrasync and is competent at using MS Windows.

The Basics

GPS data collection currently relies on two pieces of complementary software: • Terrasync—the interface for GPS navigation and data collection. • Pathfinder Office—a multiuse piece of software that acts as a conduit between GIS data files (shape files) and Terrasync GPS files. Pathfinder can also be used as a simple map editor.

Installing the Correct Versions of Terrasync and Pathfinder Important Note: This tutorial uses Pathfinder Office v. 3.00 and Terrasync v. 2.50. It is very important to use the proper versions of this software to avoid compatibility issues. These software versions should be included in the same folder as this tutorial, or can be obtained from GIS staff. http://www.trimble.com/terrasync_ts.asp?Nav=Collection‐4576 Key code for TerraSync 499043‐00110‐05273‐EDD049BC Pathfinder v.3.00 001533‐00300‐04152‐0ee4d11f

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Initial Setup of Terrasync/Pathfinder Certain settings and configuration setups are needed before Pathfinder can talk to Terrasync. Whether you are installing this software for the first time or have an existing installation, check to make sure that these settings are in place. 1. Open Pathfinder Office and go to the Utilities>Data Transfer... menu. A dialog box should appear. This is the interface for communicating with Terrasync. 2. Click the Devices button, and then New… (Figure 1). 3. Click on GIS Folder. 4. Browse to the Terrasync data folder on your computer, which in most cases will be C:\My Documents\TerraSync\. 5. In the next box, Type will be Terrasync, and Version will be v. 2.1x, v.2.2x, v.2.3x, and v2.4x. 6. At the prompt for a name that will display in the device list, enter Terrasync. 7. Go back to the Data Transfer dialog box, select Terrasync from the dropdown menu, press the Connect icon, and look for a green check mark indicating success.

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Figure 2. Selecting Files To Copy to a Different Directory

If this procedure does not work for you, you may have the wrong version of Pathfinder. For some unknown reason, with each version upgrade of Pathfinder, connectivity to older versions of Terrasync is lost. You can check what version of Pathfinder you have installed by going to the Help>About GPS Pathfinder Office... menu. To find out what version of Terrasync you have, go to C:\Program Files\TerraSync\, right‐click on Terrasync.exe, and choose the Version tab.

Handling Expired Files in Terrasync

One of the most common problems that field personnel will have to deal with is the 1‐week expiration date when trying to collect data with Terrasync. This is a built‐in function of Terrasync, and there is no simple way to work around it. The following instructions will guide you through the process to make the files usable. See Figure 3.

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Figure 3. Notice That Terrasync File Older Than 1 Week Will Not Allow User To Collect Features (time begins to elapse when first feature is collected in the field, not when file is created)

Two options are available, depending on your needs. If you do not need to see the previously logged locations and need only to see the targets, use the original files provided by GIS staff (Option 1). If you need to see previously occupied locations in order to make decisions about where to go next, then transfer the file to Pathfinder and back again (Option 2).

Option 1: Move and replace logged files with original targets. At the beginning of the field effort, you should receive a set of files with the target locations, most likely in a zip archive (.zip file extension). There will be six to eight files with the same name but with different extensions (Figure 4). These files will have to go into the C:\My Documents\TerraSync\ folder in order to be available to Terrasync.

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Figure 4. Example of File Set To Be Unzipped into the Terrasync Folder

After you unzip these files to Terrasync, keep this zip archive around in an easy‐to‐find place, such as your computer desktop, because the 1‐week clock does not start until you begin collecting your first point in the field. You can use this unadulterated file again, as long as you make a copy of the work you did the previous week. The detailed steps are as follows: 1. Make sure you have the original files with the target locations available in a handy place. This will probably be the original zip archive. Also, be sure to close Terrasync while performing this process. 2. Navigate to C:\My Documents\TerraSync\ in Windows Explorer. Locate the files that you have been using the previous week. Note: It is crucial to get all of the small files associated with the data set. While it is useful to sort the files by date modified, you can miss some of the small files—it is highly recommended that you sort the files alphabetically.

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3. Copy all of these files to a different directory, preferably one that is named appropriately to reflect the data and time period that you were collecting. For example: C:\Documents and Settings\bpointer\Desktop\lampreyTargets_20060925. These files contain the data you have collected the previous week and should be backed up and/or emailed to the appropriate project manager or GIS staff. 4. You can now safely replace the files you just copied with the ones from the original zip file. Right‐click the zip archive, and click Extract All. When prompted to Select a folder to extract files to, browse to C:\My Documents\TerraSync. (Figure 5). If prompted about replacing existing files, select Yes to All. Note: It is crucial to make copies of the files first (see Step 3 above)—otherwise, you may lose the data. 5. You should now be able to open the file in Terrasync and begin logging as normal.

Figure 5. Extract (or copy) Original Target Files into the Terrasync Directory

Option 2: Transfer files back and forth from Terrasync. If you need to be able to see the previously occupied positions from last week while positioning this week, you need to use Pathfinder to reset the file. This process will essentially combine the targets and actuals from last week into one file. However, this method has its drawbacks; once converted, the actuals from last week will not be able to be corrected, so a backup procedure similar to the one in the previous option should be carried out to maintain data integrity.

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The steps for file transfer are as follows: 1. For good data management, back up the data files from the previous week using the procedure laid out in steps 1 through 3 in Option 1 above. 2. Close Terrasync and open up Pathfinder Office. 3. Go to the Utilities>Data Transfer menu or just click the icon on the left (Figure 6). 4. Ensure that the device listed is Terrasync. If not, follow the initial setup instructions at the beginning of this document. Most of the computers used for GPS logging are already setup for this. 5. There are two tabs, Receive and Send. Make sure that Receive is selected and then go to Add>Data File. Select the file(s) that you are using and select Open. The file should now be in the Files to Receive box. Click Transfer All and wait for the transfer to take place. If you have made the recommended backups, it is fine to replace any files. 6. Now select the Send tab (Figure 7), and go to Add>Data File. Select the file you just transferred (it will have the same name as the Terrasync file) and click Open. Now click Transfer All to move the file back to Terrasync.

By transferring the file back and forth from Terrasync to Pathfinder, you have “reset the clock” and can now update the file for an additional 7 days. This file will have your targets and actual positions from the last week, so it is important to be aware of the features you are selecting for navigation.

Figure 6. Data Transfer Menu

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Figure 7. Sending Data File

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STANDARD OPERATING PROCEDURE (SOP) SD-01

DECONTAMINATION OF SEDIMENT SAMPLING EQUIPMENT

SCOPE AND APPLICATION

This SOP describes procedures for decontaminating sampling and processing equipment contaminated by either inorganic or organic materials. To prevent potential cross contamination of samples, all reusable sediment sampling and processing equipment is decontaminated before each use. At the sample collection site, a decontamination area is established in a clean location that is upwind of actual sampling locations, if possible. All sediment sampling and processing equipment is cleaned in this location. Decontaminated equipment is stored away from areas that may cause recontamination. When handling decontamination chemicals, field personnel must follow all relevant procedures and wear protective clothing as stipulated in the site‐specific health and safety plan (HSP). Sampling equipment (e.g., van Veen, Ekman, Ponar, core tubes) may be used to collect samples that will 1) undergo a full‐suite analysis (organics, metals, and conventional parameters) or 2) be analyzed for metals and conventional parameters only. Decontamination of sampling equipment used for both analyte groups should follow the order of a detergent wash, site water rinse, organic solvent rinses, and final site water rinse. Sample processing equipment (e.g., bowls, spoons) has a final rinse with distilled/deionized water rinse instead of site water. If the surface of stainless steel equipment appears to be rusting (possibly due to prolonged contact with organic‐rich sediment), it should undergo an acid rinse and a site‐water rinse at the end of each sampling day to minimize corrosion.

EQUIPMENT AND REAGENTS REQUIRED

Equipment required for decontamination includes the following: • Polyethylene or polypropylene tub (to collect solvent rinsate) • Plastic bucket(s) (e.g., 5‐gal bucket) • Tap water or site water • Carboy, distilled/deionized water (analyte‐free; received from testing laboratory or other reliable source) • Properly labeled squirt bottles

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• Funnels • Alconox®, Liquinox®, or equivalent industrial detergent • Pesticide‐grade acetone and hexane (consult the project‐specific field sampling plan [FSP], as the solvents may vary by EPA region or state) • 10 percent (v/v) nitric acid (reagent grade) for inorganic contaminants • Baking soda • Long‐handled, hard‐bristle brushes • Extension arm for cleaning core liners • Plastic sheeting, garbage bags, and aluminum foil • Core liner caps or plastic wrap and rubber bands • Personal protective equipment as specified in the health and safety plan.

PROCEDURES

Decontamination Procedures for Full Suite Analysis (Organic, Metal, or Conventional Parameters)

Two organic solvents are used in this procedure. The first is miscible with water (e.g., ethanol) and is intended to scavenge water from the surface of the sampling equipment and allow the equipment to dry quickly. This allows the second solvent to fully contact the surface of the sampler. Make sure that the solvent ordered is anhydrous or has a very low water content (i.e., < 1 percent). If ethanol is used, make sure that the denaturing agent in the alcohol is not an analyte in the samples. The second organic solvent is hydrophobic (e.g., hexane) and is intended to dissolve any organic chemicals that are on the surface of the equipment. The exact solvents used for a given project may vary by EPA region or state (see project‐specific FSP). Integral uses ethanol and hexane as preferred solvents for equipment decontamination. If specified in the project‐specific FSP, isopropanol or acetone can be substituted for ethanol, and methanol can be substituted for hexane in the decontamination sequence. The choice of solvents is also dependent on the kind of material from which the equipment is made (e.g., acetone cannot be used on polycarbonate), and the ambient temperature (e.g., hexane is too volatile in hot climates). In addition, although methanol is sometimes slightly more effective than other solvents, its use is discouraged due to potential toxicity to sampling personnel. The specific procedures for decontaminating sediment sampling equipment and sediment compositing equipment are as follows:

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1. Rinse the equipment thoroughly with tap or site water to remove visible sediment. Perform this step onsite for all equipment, including core liners that will not be used again until the next day of sampling. After removing visible solids, set aside sampling equipment that does not need to be used again that day; this equipment should be thoroughly cleaned in the field laboratory at the end of the day. 2. Pour a small amount of concentrated laboratory detergent into a bucket (i.e., about 1−2 tablespoons per 5‐gal bucket) and fill it halfway with tap or site water. If the detergent is in crystal form, make sure all crystals are completely dissolved prior to use. 3. Scrub the equipment in the detergent solution using a long‐handled brush with rigid bristles. For the polycarbonate core liners, use a round brush attached to an extension arm to reach the entire inside of the liners, scrubbing with a back‐and‐forth motion. Be sure to clean the outside of core liners, bowls, and other pieces that may be covered with sediment. 4. Double rinse the equipment with tap or site water and set right‐side‐up on a stable surface to drain. The more completely the equipment drains, the less solvent will be needed in the next step. Do not allow any surface that will come in contact with the sample to touch any contaminated surface. 5. If the surface of stainless steel equipment appears to be rusting (this will occur during prolonged use in anoxic marine sediments), passivate 1 the surface as follows (if no rust is present, skip to next step). Rinse with a 10 percent (v/v) nitric acid solution using a squirt bottle, or wipe all surfaces using a saturated paper towel. Areas showing rust may require some rubbing with the paper towel. If using a squirt bottle, let the excess acid drain into the waste container (which may need to be equipped with a funnel). Double‐ rinse equipment with tap or site water and set right‐side‐up on a stable surface to drain thoroughly. 6. Carefully rinse the equipment with ethanol from a squirt bottle, and let the excess solvent drain into a waste container (which may need to be equipped with a funnel). Hold core liners over the waste container and turn them slowly so the stream of solvent contacts the entire surface. Turn the sample apparatus (e.g., grab sampler) on its side and open it to wash it most effectively. Set the equipment in a clean location and allow it to air dry. Use only enough solvent to scavenge all of the water and flow off the surface of the equipment (i.e., establish sheet flow) into the waste container. Allow equipment to drain as much as possible. Ideally, the equipment will be dry. The more thoroughly it drains, the less solvent will be needed in the next step.

1 Passivation is the process of making a material less reactive relative to another material. For example, before sediment is placed in a stainless‐steel container, the container can be passivated by rinsing it with a dilute solution of nitric acid and deionized water.

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7. Carefully rinse the drained or air‐dried equipment with hexane from a squirt bottle, and let the excess solvent drain into the waste container (which may need to be equipped with a funnel). If necessary, widen the opening of the squirt bottle to allow enough solvent to run through the core liners without evaporating. (Hexane acts as the primary solvent of organic chemicals. Ethanol is soluble in hexane but water is not. If water beading occurs, it means that the equipment was not thoroughly rinsed with acetone or that the acetone that was purchased was not free of water.) When the equipment has been rinsed with hexane, set it in a clean location and allow the hexane to evaporate before using the equipment for sampling. Use only enough solvent to scavenge all of the acetone and flow off the surface of the equipment (i.e., establish sheet flow) into the waste container. 8. Do a final rinse with site water for the sampling equipment (i.e., van Veen, Ekman, Ponar, core tubes) and with distilled/deionized water for processing equipment (i.e., stainless‐steel bowls and spoons). Equipment does not need to be dried before use. 9. If the decontaminated sampling equipment is not to be used immediately, wrap small stainless‐steel items in aluminum foil (dull side facing the cleaned area). Seal the polycarbonate core liners at both ends with either core caps or cellophane plastic and rubber bands. Close the jaws of the Ekman and Ponar grab samplers and wrap in aluminum foil.

If the sample collection or processing equipment is cleaned at the field laboratory and transported to the site, then the decontaminated equipment will be wrapped in aluminum foil (dull side facing the cleaned area) and stored and transported in a clean plastic bag (e.g., a trash bag) until ready for use, unless the project‐specific FSP lists special handling procedures. 10. Rinse or wipe with a wetted paper towel all stainless‐steel equipment at the end of each sampling day with 10 percent (v/v) normal nitric acid solution. Follow with a freshwater rinse (site water is okay as long as it is not brackish or salt water). 11. After decontaminating all of the sampling equipment, place the disposable gloves and used foil in garbage bags for disposal in a solid waste landfill. When not in use, keep the waste solvent container closed and store in a secure area. The waste should be transferred to empty solvent bottles and disposed of at a licensed facility per the procedures listed in the project‐specific FSP. When not in use, keep the waste acid container closed and store in a secure area. The acid waste should be neutralized with baking soda and disposed of per the procedures listed in the project‐specific FSP.

Decontamination Procedures for Metals and Conventional Parameters Only

The specific procedures for decontaminating sediment sampling equipment and sediment processing equipment are as follows:

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1. Rinse the equipment thoroughly with tap or site water to remove the visible sediment. Perform this step onsite for all equipment, including core liners that will not be used again until the next day of sampling. Set aside pieces that do not need to be used again that day; these pieces should be and thoroughly cleaned in the field laboratory at the end of the day. 2. Pour a small amount of concentrated laboratory detergent into a bucket (i.e., about 1−2 tablespoons per 5‐gal bucket) and fill it halfway with tap or site water. If the detergent is in crystal form, make sure all crystals are completely dissolved prior to use. 3. Scrub the equipment in the detergent solution using a long‐handled brush with rigid bristles. For the polycarbonate core liners, use a round brush attached to an extension arm to reach the entire inside of the liners, scrubbing with a back‐and‐forth motion. Be sure to clean the outside of core liners, bowls, and other pieces that may be covered with sediment. 4. Double‐rinse the equipment with tap or site water and set right‐side‐up on a stable surface to drain. Do not allow any surface that will come in contact with the sample to touch any contaminated surface. 5. If the surface of stainless steel equipment appears to be rusting (this will occur during prolonged use in anoxic marine sediments), passivate 2 the surface as follows (if no rust is present, skip to next step). Rinse with a 10 percent (v/v) nitric acid solution using a squirt bottle, or wipe all surfaces using a saturated paper towel. Areas showing rust may require some rubbing with the paper towel. If using a squirt bottle, let the excess acid drain into the waste container (which may need to be equipped with a funnel). Double‐rinse sampling equipment with tap or site water and set right‐side‐up on a stable surface to drain. Double‐rinse processing equipment with distilled/deionized water and allow to drain. 6. If the decontaminated sampling equipment is not to be used immediately, wrap small stainless‐steel items in aluminum foil (dull side facing the cleaned area). Seal the polycarbonate core liners at both ends with either core caps or cellophane plastic and rubber bands. Close the jaws of the Ekman and Ponar grab samplers and wrap in aluminum foil.

If the sample collecting or processing equipment is cleaned at the field laboratory and transported to the site, then the decontaminated equipment will be wrapped in aluminum foil (dull side facing the cleaned area) and stored and transported in a clean plastic bag until ready for use, unless the project‐specific FSP lists special handling procedures.

2 Passivation is the process of making a material less reactive relative to another material. For example, before sediment is placed in a stainless‐steel container, the container can be passivated by rinsing it with a dilute solution of nitric acid and deionized water.

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7. After decontaminating all of the sampling equipment, place the disposable gloves and used foil in garbage bags for disposal in a solid waste landfill. When not in use, keep the waste acid container closed and store in a secure area. The acid waste should be neutralized with baking soda and disposed of per the procedures listed in the project‐ specific FSP.

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STANDARD OPERATING PROCEDURE (SOP) SD-04

SURFACE SEDIMENT SAMPLING

SCOPE AND APPLICATION

This SOP defines and standardizes the methods for collecting surface sediment samples from freshwater or marine environments. Surface sediments are defined as those from 0 to at most 10 cm below the sediment-water interface. The actual definition of surface sediments is typically program-specific and depends on the purpose of the study and the regulatory criteria (if any) to which the data will be compared. This SOP utilizes and augments the procedures outlined in USEPA (1997) and ASTM (2003) guidelines. A goal of this SOP is to ensure that the highest quality, most representative data are collected, and that these data are comparable to data collected by different programs that follow the USEPA (1997) guidelines.

SUMMARY OF METHOD

Sediment samples for chemical and toxicity analysis are collected using a surface sediment sampling device (e.g., grab sampler) or hand implements (i.e., spoons, scoops, shovels, or trowels). If a sample meets acceptability guidelines, overlying water is carefully siphoned off the surface in a grab sampler, and the sediment is described in the field logbook. Depending upon the type of analysis to be performed, sediment samples for chemical analysis may be collected directly from an undisturbed surface (e.g., volatile organic compounds and sulfides), or may be homogenized using decontaminated, stainless-steel containers and utensils prior to being placed in sample jars. Sediment from several sampler casts or exposed sediment locations may also be composited and homogenized prior to being placed in sample jars.

SUPPLIES AND EQUIPMENT

A generalized supply and equipment list is provided below. Additional equipment may be required depending on project requirements. • Sampling device − Grab sampler or box corer (see examples below in procedures for “Sediment Sample Collection”)

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− Stainless-steel spoon, scoop, shovel, or trowel • Field equipment − Siphoning hose − Stainless-steel bowls or containers − Stainless-steel spoons, spatulas, and/or mixer − Stainless-steel ruler − Project-specific decontamination supplies (e.g., AlconoxTM detergent, 0.1 N nitric acid, methanol, hexane, distilled/deionized water) − Personal protective equipment for field team (e.g., rain gear, safety goggles, hard hats, nitrile gloves) − First aid kit − Cell phone − Camera − Sample containers − Ziploc® bags − Bubble wrap − Sample jar labels − Clear tape − Permanent markers − Indelible black-ink pens − Pencils − Coolers − Ice • Documentation − Waterproof field logbook − Field sampling plan − Health and safety plan − Correction forms − Request for change forms − Waterproof sample description forms.

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PROCEDURES

Sediment Sample Collection with a Grab Sampler

Use a sampler that obtains a quantifiable volume of sediment with minimal disturbance of the surrounding sediments to collect sediment for chemical and biological analyses. The sampler should be composed of a material such as stainless steel or aluminum, or have a noncontaminating coating such as TeflonTM. Samplers capable of providing high-quality sediment samples include grab-type samplers (e.g., van Veen, Ekman, Smith-McIntyre, Young grab, Power Grab and modified-ponar grab) and box cores (Soutar, mini-Soutar, Gray-O’Hara, spade core). Some programs require a sampler that collects from a specific area (e.g., 0.1 m2). Most sampling devices are typically a standard size; however, some non-standard sizes are available to meet the requirements of specific programs. Grab samplers, especially van Veen grab and Ekman grab, are the most commonly used samplers to collect surface sediment. Power Grab samplers are often used for programs requiring collection of sediment deeper than 10 cm (4 in.) or in areas with debris. Depending on grab weight and water depth, use a hydraulic winch system to deploy the heavier samplers at a rate not exceeding 1 m/second. As the grab nears the bottom, decrease the descent speed to about 0.3 m/second to minimize the bow wake and disturbance of the surface sediment associated with sampler descent. Once the sampler hits the bottom, close the jaws slowly and bring the sampler to the deck of the vessel at a rate not exceeding 1 m/second to minimize any washing and disturbance of the sediment within the sampler. At the moment the sampler hits the bottom, record the time, water depth, and location of sample acquisition in the field logbook. Retrieve and secure the sampler, and carefully siphon off any overlying water. Inspect the sample to determine acceptability using the criteria detailed in USEPA (1997), except when noted in the project-specific field sampling plan. These criteria include but are not limited to the following: • There is minimal or no excessive water leakage from the jaws of the sampler • There is no excessive turbidity in the water overlying the sample • The sampler is not over-penetrated • The sediment surface appears to be intact with minimal disturbance • There is no anthropogenic (i.e., man-made) debris in the sampler • The program-specified penetration depths are attained. If the sample meets acceptability criteria, record the sample collection location using a global positioning system (GPS) and enter observations onto a sample collection form or the field logbook. Depending on programmatic goals, remove the sampling interval specified in the field sampling plan. Use a decontaminated stainless-steel ruler to measure the sample

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collection depth (0 to 10 cm) within the sampler. To prevent possible cross-contamination, do not use sediments touching the margins of the sampler. Take a photograph of the sediment in the grab sampler and in the stainless-steel bowl in the field. Verify that the station number or sample ID, time, and date are shown in the photograph. Typically, sediment from a minimum of three separate casts of the sampler is composited at each station (see project-specific field sampling plan). Once the sample has been characterized, subsample the sediment for chemical and biological analyses using a decontaminated stainless- steel spoon.

Sediment Sample Collection with Hand Implements

Obtain a quantifiable volume of sediment with minimal disturbance of the surrounding sediments to collect sediment for chemical and biological analyses. Hand implements (e.g., spoons, scoops, shovels, or trowels) must be composed of stainless steel. Use GPS to locate the sampling site and approach the location carefully to avoid disturbing the area of sediment to be sampled. Prior to sample collection, describe and characterize the undisturbed surface sediment in the field logbook. If necessary, expose the sediment surface by clearing an approximately 1-ft2 area at the sampling site of any rocks greater than approximately 5 in. Remove any anthropogenic (i.e., man-made) debris and organic material on the sediment surface. Note any material removed from the sampling site in the field logbook. Using a decontaminated, stainless-steel hand implement (i.e., spoon, scoop, shovel, or trowel), excavate the sediment to 10 cm. Place the sediment in a decontaminated stainless-steel bowl and use a decontaminated stainless-steel ruler to confirm that the correct sampling interval has been collected. If the full sample collection interval (i.e., 10 cm) has not been reached, collect additional sediment, place it in the stainless-steel bowl, and reconfirm the sampling interval. Continue this process until the full sample collection interval (0 to 10 cm) has been reached. Take a photograph of the excavated hole from where the sediment sample was removed. Verify that the station number or sample ID, time, and date are shown in the photograph.

Sample Processing

Complete all sample collection forms, labels, custody seals, and chain-of-custody forms, and record sample information in the field logbook. Collect samples for volatile compounds (either organics or sulfides) using a decontaminated stainless-steel spoon while sediment is still in the grab sampler or, if the sample is collected using a hand implement, in the stainless-steel bowl. Sediments for volatile analysis are not homogenized. Tightly pack the volatile organics sample jar with sediment (to eliminate obvious air pockets) and fill it so that no headspace remains in the jar. Alternatively, if there is

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adequate water in the sediment, fill the container to overflowing so that a convex meniscus forms at the top, and then carefully place the cap on the jar. Once sealed, the jar should contain no air bubbles. Place the remaining sediment in the grab sampler in a precleaned, stainless-steel bowl; sediment collected using hand implements are already in a stainless-steel bowl. Once a sufficient amount of sediment has been collected, mix the sediment using a decontaminated stainless-steel spoon until it is of uniform color and texture throughout. If required for analysis, collect samples for grain-size tests before any large rocks are removed from the homogenized sediment. Identify any rocks that are greater than 0.5 in. in diameter. Determine their percentage contribution to the homogenized sediment volume, note it on the sediment field collection form or in the field logbook, and then discard the rocks. Dispense the sediment into precleaned sample jars for the various chemical or biological analyses. For toxicity testing, fill sample jars to the top with sediment to minimize available headspace. This procedure will minimize any oxidation reactions within the sediment. For chemical analysis, sample containers may be frozen for storage. Leave enough headspace to allow for sediment expansion. After dispensing the sediment, place the containers into coolers with ice and either ship them directly to the analytical laboratories or transport them to a storage facility.

REFERENCES

ASTM. 2003. Standard Practice for Collecting Benthic Macroinvertebrates with Ekman Grab Sampler. ASTM Standards on Disc, Volume 11.05. USEPA. 1997. Recommended protocols for sampling marine sediment, water column, and tissue in Puget Sound. Prepared for Puget Sound Estuary Program, U.S. Environmental Protection Agency, Seattle, WA, and Puget Sound Water Quality Action Team, Olympia, WA. U.S. Environmental Protection Agency, Region 10, Seattle, WA.

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APPENDIX B FIELD SAMPLING FORM

SURFACE SEDIMENT SAMPLING FORM Project Name: Page ___ of ___ Sampling Method: Project No.:

Crew: Date: Time Station Rep. Pen. (cm) Texture Color Debris Odor Sample Quality/Comments

Comments: