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Exposure Investigation Workplan



Purpose of Exposure Investigation

The Lower Elwha Klallam Tribe requested that the Washington State Department of Health(DOH) evaluate whether their subsistence-level consumption of shellfish, collected in thevicinity of the Port Angeles Harbor, poses a health threat. Historically, the Harbor receivedeffluent from two paper mills, including the former Rayonier Pulp Mill, which is located closestto the areas used by tribal members for shellfish collection, a plywood mill, and the city of PortAngeles. The effluent from the Rayonier mill is a known source of dioxins and furans. Noinformation is available to indicate dioxins and furans are associated with the other sources;however, there may be potential sources. Dioxins and furans are the primary chemicals ofconcern to the Tribe. The Agency for Toxic Substances and Disease Registry (ATSDR) isproviding a portion of the funding to conduct this exposure investigation (EI).


The above-named historic effluent sources within the harbor are located within the Port Angelescity limits, in Clallam County, Washington. Port Angeles Harbor, which is formed by theextension of Ediz Hook into the Straight, is located immediately north of the city (Figure 1). Themarine waters between the harbor and Dungeness Spit, located to the east, are considered animportant subsistence fishery resource for the Tribe.

One of the effluent sources, the Rayonier pulp mill, which operated from 1929 to 1997, used anammonia-based acid sulfite process for the production of various grades of pulp. Chlorine andchlorine compounds, that contribute to the production of dioxins and furans, were used in thebleaching process.1 Dioxins and furans were also released in effluent from other sources at themill, such as the hog-fuel ash that was removed by the wet direct-contact air emissionscrubbers.2

Prior to the installation of the primary treatment plant at the mill in 1972, effluent (solid andliquid) generated during the pulp-making process, and surface water runoff, were dischargeddirectly along the Port Angeles Harbor shoreline through a number of individual outfalls locatedadjacent to the mill. Data collected by Rayonier in 1963 indicate that effluent generally movedeast from the mill site. Rayonier also found that drift within the bay was generally clockwise andeasterly.1

After the primary treatment system was installed at the mill, clarified and treated effluent wasdischarged to a submerged outfall located near the center of the mouth of the Port AngelesHarbor. The outfall consists of a submerged outfall line approximately 7,900 feet long thatconnects with an approximately 940-foot diffuser section containing 48 vertical outlet ports.Outfall location studies found that the currents rotated clockwise during receding or outgoingtides, and moved toward the east during incoming or rising tides. Secondary treatment was addedto the system in 1979. From the initiation of secondary treatment until operations ceased in 1997,the mill discharged approximately 50,000 pounds of suspended solids per day through thediffuser outfall.1

The Tribe located other studies of current movement that support the earlier findings obtained byRayonier. A pulp mill effluent study conducted in the early 1980s found that the effluentdischarging from the submerged outfall was buoyant, warm, freshwater that migrated in aneasterly direction towards Green Point and Dungeness Spit. During that same study, dyeexperiments indicated that portions of effluent released at the diffuser move to Morse Creek andGreen Point.3 The Tribe also located drift card data, plume tracking data, and toxicity data thatindicates that much of the effluent and emissions from the Rayonier mill site moved in aneasterly direction, towards Dungeness Spit.2 The National Oceanic and AtmosphericAdministration investigated currents near the submerged Rayonier outfall by releasing 700 driftcards in the late 1970s. Of the 273 cards recovered, 65% were recovered between Ediz Hook andDungeness Spit. Less than 10% moved to locations north or west of Ediz Hook.4 A drift cardstudy conducted as part of a proposed pipeline route study found 73% of recovered cardsreleased at the mouth of the Port Angeles Harbor were recovered between Ediz Hook andDungeness Spit.5 While these data indicated that effluent migrated eastward, the data is notconclusive relative to contamination of biota Exiting ATSDR Website. Actual testing is necessary to determine the levelof contamination to the east of the mill site.

Recent effluent dispersion modeling conducted by Rayonier suggests that although there is aneastward component to the effluent, the suspended sediments tended to fall out near the outfall.2These modeling results were not verified by either the Tribe, or the Washington StateDepartment of Ecology. Based on the results of Rayonier's dispersion modeling, the Rayonier RIsampling plan for the marine environment does not provide for sampling at a distance to the eastof the mill site. Exclusion of samples in the Morse Creek to Dungeness Spit area from the RIleaves a data gap that is of concern to the Tribe.

Environmental Contamination

From the initiation of secondary treatment until operations ceased in 1997, the Rayonier Milldischarged approximately 50,000 pounds of suspended solids per day through its outfall.1 Theprimary contaminants of concern are dioxins and furans. These chemicals were measured ineffluent at a concentration of approximately 4.9 mg TEQ/day, until the mill closed in 1997.6

Toxicity tests on receiving water conducted in the area between the tip of Ediz Hook andDungeness Spit in the 1960s and 1970s showed greater than 50% oyster toxicity (percentabnormal development) throughout the area. The toxicity was subsequently linked to pulp milleffluents in Port Angeles Harbor, and indicates that effluent, and associated chemicals, weretransported to areas east of Port Angeles Harbor at concentrations sufficient to cause biologicaleffects.3

There is no available tissue data to determine the Tribe's potential health risk from consumingDungeness Crab (Cancer Magister) and geoduck (Panope Abrupta). Muscle tissue from a redrock crab (Cancer Productus) sample collected at Green Point in 1995 exceeded the 0.021 partsper trillion (ppt) EPA Region 3 Risk-Based Criteria for 2,3,7,8-TCDD.6 The dioxinconcentration in the Green Point sample was 0.11 ppt TEQ, based only on detected congeners.This sample indicates the potential for marine organism uptake at concentrations that exceedEPA criteria.

The presence of effluent from the Rayonier mill in the Morse Creek/Dungeness Spit area, theconcentrations of dioxins present in the effluent, the duration of effluent discharge, and thepresence of dioxins in the Green Point tissue samples have raised concerns among the LowerElwha Klallam Tribe about the safety of subsistence-level consumption of shellfish harvestedfrom that area. The marine waters and associated resources between Port Angeles Harbor andDungeness Spit are important to tribal members. The primary resource species of interest in thisarea are Dungeness crab and geoduck. Geoducks have a significant potential for contaminantbioaccumulation due to their long lifespan.


This section (and the Appendices) describes the sampling and analysis tasks necessary to supportthe joint DOH/Tribe shellfish (Dungeness crab and geoduck) investigation, including thesampling approach and rationale for the number and location of samples to be collected. It alsopresents descriptions of sampling tasks, including descriptions of sampling equipment andcollection methods to be used, the analyses to be performed, specifications for sampleidentification, a description of sample documentation, and identification of appropriate samplehandling and management procedures. Sampling was anticipated to occur in October 2002. Aseparate health consultation will be prepared by DOH evaluating the results of the samplinganalysis.

Sample Collection

Dungeness crabs

Dungeness crabs will be collected from five target sample areas previously identified by theTribe. If Dungeness crabs are not available in sufficient numbers, red rock crabs may becollected as an alternative species, or adjustments may be made at the time and/or place ofsampling. This determination will be made by field personnel in consultation with managementpersonnel. The target areas are situated between Morse Creek and the base of Dungeness Spit(Figure 1). Five individual crabs will be collected from each target area, and combined, torepresent a single, composite crab sample for that area. The five composite samples willrepresent a total of 25 crabs (five crabs per area for five areas). Given the limited resources, thissampling design provides the best combination of sample coverage and sample quantity.Multiple sampling areas and multiple individuals within each sample area will provide areasonable representation of the overall population found in the study area. Individual crabswithin each area will be collected from different sampling locations, perpendicular to theshoreline, to reduce any potential bias caused by sampling from different depths at differentstations. Representative crabs collected from multiple depths will be selected to form thecomposite sample from each area. Individual locations within each area will be selected by theTribe, while in the field. The Tribe anticipates sampling from individual locations between theshoreline, to at least one half mile offshore.

Dungeness crabs will be collected using standard commercial crab pots and ancillary gear. Thepots will be fished from the Tribe's and/or others' boats. Up to 10 pots may be used at eachsample location. Sample collection equipment will be uncontaminated with grease or oil. Thepots will be baited with fish, squid, clams, or similar material. The bait will be placed in smallcontainers inside the trap to disperse the smell of the bait and attract the crabs.

Efforts will be made to harvest those crabs with a carapace length greater than 6.25 inches, asthis is the current legal minimum size limit for Dungeness crabs. The preference will be for malecrabs (the current legal catch). However, female crabs, and/or crabs smaller than 6.25 inches willbe used if sufficient numbers of larger male crabs cannot be collected. The determination ofwhich crabs that will be retained for analysis, based upon size and sex, will be made by fieldpersonnel in consultation with management personnel. Individual crabs will be photographed,measured, weighed, and examined for any discoloration, abnormalities, or lesions. Normally,only unbroken crabs will be retained for analysis. Each crab will be killed by a rapid blow to thearea on the underside of the carapace below the eyestalks, or by asphyxiation using dry ice-generated carbon dioxide. The crab will then be wrapped in decontaminated aluminum foil,bagged in a zip loc bag, labeled, and placed in a cooler with Blue Ice®, or similar product, not tobe frozen. The coolers will be secured, labeled, and shipped with the necessary documentationand shipping papers after each day's sampling catch, by overnight delivery to AXYS Analytical,Inc. (AXYS Analytical) for sample processing and analysis. Samples will be shipped no laterthan Thursday of a given week. If samples cannot be shipped by Thursday, they will be helduntil the following Monday.


Geoducks will be collected from the same five target areas as the crabs, although specificlocations within each area may be different, depending on where the geoducks are found. Aswith the crabs, each composite sample will consist of five individual geoducks from each of thefive areas, for a total of 25 geoducks. Individual geoducks within each area will also be collectedfrom different depths. Efforts will be made to collect geoducks representative of the sizestypically harvested and consumed by the Tribe. Geoducks will be collected by divers usinghydraulic pressure excavation (gas-powered water pump or "dig pump" with a 3/4" diameternozzle). Clams will be brought to the surface in a collection bag.

Individual geoducks will be measured, weighed, and examined for any discoloration,abnormalities, or lesions. The geoducks will be photographed, wrapped in decontaminatedaluminum foil, placed in zip lock bags, labeled, and placed in a cooler with Blue Ice®, or similarproduct, not to be frozen. The coolers will be secured, labeled, and shipped with the necessarydocumentation and shipping papers after each day's sampling catch, by overnight delivery toAXYS Analytical for sample processing and analysis. Samples will be shipped no later thanThursday of a given week. If samples cannot be shipped by Thursday, they will be held until thefollowing Monday.

Red rock crabs

If sufficient numbers of Red Rock crabs are available during the field sampling effort, red rockcrabs may be collected at the same time and from the same five areas as the Dungeness crabs andgeoducks to evaluate the correlation (if any) in dioxin levels. To the extent possible, samplecollection, identification, shipping, preparation, and analysis will be identical to those used forthe Dungeness crabs. Deviations from this plan may be made by field personnel in consultationwith management personnel.

Reference area samples

Reference samples will be collected from areas east and west of the study area that are not likelyto be significantly affected by releases from the former Rayonier Mill. Since low levels ofdioxins and furans are ubiquitous in the environment (including in shellfish), it is useful tocompare levels in shellfish that reside in areas likely to have been impacted by industrial sources,such as the former mill site, to levels in shellfish in areas relatively unimpacted by industrialsources (i.e., reference areas). For this exposure investigation, Dungeness Spit and FreshwaterBay are the selected reference locations. Dungeness Bay is a protected, nonurbanized areaapproximately 15 miles east of Port Angeles Harbor. Freshwater Bay is a semi-protected baylocated approximately 10 miles west of Port Angeles (Figure 1).

Since Rayonier is also using Dungeness Spit and Freshwater Bay as reference areas for theirremedial investigation (RI), they agreed to provide the Tribe with splits of their Dungeness craband geoduck samples from both reference areas for the DOH/Tribe exposure investigation. Thiswill provide the necessary reference samples with which to compare the non-reference areashellfish samples collected during the exposure investigation.

Six of Rayonier's split reference shellfish samples will be sent overnight from ColumbiaAnalytical in Houston (where Rayonier's dioxin/furan analysis is being conducted) to AXYSAnalytical for analysis. The six split samples include one individual geoduck sample from eachreference area, and two composite crab samples from each reference area. The composited crabsamples will consist of one composite muscle tissue sample, and one composite crab "butter"sample (which includes the hepatopancreas tissue) from each reference area. Each crab samplewill be a composite of five to eight individuals, depending on the success of the Rayoniersampling effort in obtaining sufficient individuals. Columbia Analytical will ship the compositedand homogenized samples directly to AXYS Analytical.

The dioxin/furan analysis requires a minimum of 10-12 grams of shellfish tissue for each samplecomposite. Rayonier has indicated that Columbia Analytical should have this quantity remainingfor analysis by AXYS after completion of their own analysis. If this minimum quantity ofshellfish homogenate is not available from Columbia, reference samples will be collected by theTribe in the same manner as the other samples. If this occurs, the number of non referencesamples analyzed may be reduced due to budget constraints.

Laboratory processing of shellfish samples

As described above, AXYS Analytical will analyze the six split samples provided by Rayonier'slab. In the unlikely event AXYS Analytical determines that additional homogenization ofRayonier's split shellfish homogenate is necessary, they will notify DOH and/or the tribe prior toanalysis. If any other problems are noted (i.e., temperature abnormalities, condition of samples,condition of container, etc.), DOH and the Tribe will be notified.

All shellfish samples collected by the Tribe during the EI will be processed and analyzed byAXYS Analytical according to the procedures outlined in this sampling workplan and asdescribed in the U.S. Environmental Protection Agency Guidance for Assessing ChemicalContaminant Data for Use In Fish Advisories.7 Processing includes sample-logging andinspection, removal of edible portions of the shellfish, compositing, weighing, homogenizing,aliquot preparation, etc. Special instruction for processing or analysis, if any, will be noted by DOH on the analytical request form.


Rayonier's split samples: Columbia Analytical will send, (by overnight delivery) to AXYSAnalytical, pre-composited and pre-homogenized crab muscle tissue (two) and crab butter (two)samples. No additional processing is anticipated for these split reference samples. AXYSAnalytical will evaluate the samples for sample integrity, ensure they are sufficientlyhomogenized, weigh them, and analyze the samples for lipids, and for dioxins/furans by EPAmethod 1613B.

DOH/Tribe EI samples: Whole crabs collected and submitted during the DOH/Tribe exposureinvestigation will be evaluated for sample integrity. Each individual will be measured andweighed prior to dissection and homogenization, and its sex noted. Since tribal members oftenconsume the crab butter and crab muscle portions together, AXYS Analytical will combine andhomogenize the crab butter and crab muscle portions of each sample composite collected by theTribe. Shellfish tissue splits obtained from Columbia Analytical will not be recomposited byAXYS Analytical.

Edible portions of the muscle tissue (legs and body) and crab butter from the five individualcrabs that make up each composite will be removed from the shell, combined, and weighed.Each composite sample (consisting of crab butter and muscle tissue from five crabs) will then behomogenized, for a total of five separate composite crab samples. Aliquots of the samples will beprepared and analyzed by EPA method 1613B for dioxins and furans. In addition, a lipidsanalysis will be conducted for each sample.


Rayonier's split samples: As discussed above, two individual geoduck samples from thereference areas will arrive from Columbia Analytical pre-weighed and homogenized. AXYSAnalytical will evaluate the integrity of the geoduck homogenate. If no additionalhomogenization is necessary, the samples will be analyzed for lipids, and for dioxins/furans byEPA method 1613B.

DOH/Tribe EI samples: AXYS Analytical will evaluate the integrity of the samples, and weighthe geoducks. Edible portions of the geoduck muscle tissue (neck) will be separated from theshell and gutball prior to homogenization. The five individual geoduck samples representingeach sampling area will be composited into a single sample, homogenized, then analyzed, for atotal of five composite samples (one composite representing each area). The samples will beanalyzed for lipids, and for dioxins/furans by EPA method 1613B.

Data reporting and evaluation

Upon completion of the sample analysis, AXYS Analytical will prepare data summary reports.The reports will include the results of the chemical and lipid analysis, and the appropriate qualityassurance and quality control reports as required by EPA method 1613, including initialcalibration, calibration verification, GC column resolution, procedural blank and ongoingprecision and recovery results. A full data package will also be provided which will include anarrative discussion, example calculations, sample receiving records, sample homogenizationrecords, wet chemistry logs and all raw data including window defining results, injection logsand test sample and QA sample chromatograms.

The results of the analysis will be evaluated by DOH in a health consultation that, uponcompletion, will be available to the Tribe, Rayonier, Ecology, and the public. Since the split crabbutter and crab muscle reference samples obtained from Rayonier will be analyzed separately byAXYS Analytical (as opposed to the combined crab muscle and crab butter analysis conductedfor the EI shellfish samples), the sample mass will be used to compare and evaluate the results of the reference and non-reference crab samples.


  1. The Lower Elwha Klallam tribe collects and consumes Dungeness crabs, geoducks, andother aquatic resources from the marine environment in the vicinity of the Port AngelesHarbor where dioxin and furan-containing effluent may have migrated.

  2. No conclusive data currently exist to determine whether dioxin/furan levels in Dungenesscrabs and geoducks in the marine environment in the vicinity of the Port Angeles Harborpose a health threat to the tribe.

  3. This data gap can be addressed by the collection and analysis of Dungeness crabs andgeoducks in the target areas identified in the Discussion section.


  1. Dungeness crab and geoduck sampling, preparation, and analysis should be conductedaccording to the methods outlined in this exposure investigation workplan.

  2. DOH will evaluate the results of the sampling analysis to determine whether the detectedlevels of dioxins and furans pose a health threat to members of the Lower Elwha Klallamtribe who harvest and consume Dungeness crabs and geoducks from the target sampleareas.

  3. The results of DOH's evaluation will be provided to the Tribe, Ecology, Rayonier, andthe community. Possible recommendations include additional sampling, limits on theamount of crabs and geoducks consumed by the Tribe, or no further action.


Paul Marchant
Washington State Department of Health
Office of Environmental Health Assessments
Site Assessment Section

Designated Reviewer
Robert Duff, Manager
Site Assessment Section
Office of Environmental Health Assessments
Washington State Department of Health

ATSDR Technical Project Officer
Debra Gable
Division of Health Assessment and Consultation
Agency for Toxic Substances and Disease Registry


  1. Rayonier, Port Angeles Mill Site, Current Situations/Site Conceptual Model Report,Foster Wheeler Environmental Corporation, October 1997.

  2. Washington State Department of Health. Exposure Investigation Proposal: Lower ElwhaKlallam Tribe Shellfish Beds. Clallam County, Washington. November 6, 2001.

  3. History, Dispersion and Effects of Pulpmill Effluents on Receiving Waters: Port Angeles,Washington; Shea, G.B., C.C. Ebbesmeyer, Q.J. Stober, H. Pazera, J.M. Cox, H.M.Helseth, and Hemingway, 1981.

  4. Surface Drifter Movements Observed in Port Angeles Harbor and vicinity, April 1978. Ebbesmeyer C.C., J. M. Cox, J. M. Helseth, National Oceanic and AtmosphericAdministration Technical Memorandum ERL MESA-31, 1978.

  5. Drift Card Observations in Northwestern Washington Along Portions of Two Proposed Oil Pipeline Routes; Cox, J.M., C.C. Ebbesmeyer, J.M. Helseth, and C.A. Coomes, 1980.

  6. Port Angeles Bioaccumulation Study, Rayonier Inc., 1995.

  7. U.S. Environmental Protection Agency. Guidance for Assessing Chemical ContaminantData for Use In Fish Advisories. Volume 1: Fish Sampling and Analysis - Third Edition.

  8. Foster Wheeler Environmental Corporation. Volumes 1 - 3, Remedial InvestigationWorkplan for the Marine Environment near the former Rayonier Pulp Mill site, PortAngeles, Washington. July 2002.

  9. Washington State Department of Health. Draft Exposure Investigation Protocol:Marrowstone Island, Washington. April 1998.

  10. Personal communications with Laurie Phillips, AXYS Analytical Services, Ltd.July/August 2002.

  11. Personal communications with Bruce Woods, analytical chemist, United StatesEnvironmental Protection Agency. July 2002.

  12. Personal communication with Roy Hummell, Project Manager, Foster WheelerEnvironmental Corporation. July/August 2002.

Reference Stations for Joint Exposure Investigation
Figure 1. Reference Stations for Joint Exposure Investigation


Following is a description of sampling materials, navigation and positioning, field samplingmethods, documentation, sample packing and shipping, laboratory analytical methods, qualityassurance, data reporting, and data analysis.


The materials needed for sampling and shipping should be verified with AXYS Analytical (thecontract laboratory that will conduct the analysis). The following list of materials is anticipated:

Boat (provided by the Tribe)
Cotton gloves
Latex gloves
Chain-of-custody forms
Chain-of-custody sealing tape
Sampling log forms
Rite-in-the Rain® paper
Global positioning system (GPS) unit
Ice chests
Blue Ice® (or equivalent)
Packing material
Aluminum foil (2 packages, minimum)
Plastic ziplock bags.
Plastic wrap or bags (rain protection for forms)
Black markers with waterproof ink
Digital camera (substitute disposable camera in foul weather)
Crab pots, crab bait, and appurtenant gear
Tape measure
Crab measure
New, clean, decontaminated spray can (one gallon size)
Distilled water for final rinse of decontaminated equipment
Geoduck collection equipment (geoduck harvest pump or "dig" pump) per standard tribal harvesting practices

Navigation and positioning:

Vessel navigation and positioning during the EI sampling effort will consist of fielddeterminations of sample locations based on the information contained in the discussion aboveand the attached figures, with particular emphasis on the depths of the samples. The locations ofthe sample transects were chosen to match prominent geographical features to aid in positioningthe vessel during sampling. Actual sample locations will then be noted by use of GlobalPositioning System (GPS) equipment. The objective of the sample location positioningprocedure is to accurately identify and record the location of all sampling locations. The GPSwill generate positions (latitude/longitude), to at least 10 meters of accuracy.

Field Sampling Methods:

The following steps will be used to collect, document, and process the shellfish samples:

  1. Collect marine biota samples using conventional sampling techniques and equipment, asdescribed in the discussion section.

  2. Using clean, unused, disposable, un-powdered gloves, place sample in decontaminatedaluminum foil (dull side in) and place in a plastic Ziploc ® bag, along with a sample IDtag.

  3. Cool samples to a temperature less than 4º C by placing in an insulated cooler andsurrounding with Blue Ice® packs, or similar product. Do not freeze the samples. Protectsamples from light.

  4. Label and manage sample containers. Labels should include the project name, site andsample number (i.e., Pt. Angeles Exposure Investigation, Site 1, Location 2). Samplecollection information should be entered on a sample collection data form, whichincludes sufficient information for future determination of GPS data. Finally, a chain ofcustody form should be filled out and placed in a large ziplock bag inside the chest sealedwith either chain of custody tape or other device. Iced samples should be sent to thedesignated laboratory by overnight delivery, or as soon thereafter as possible, as specifiedby the contracted laboratory for initial sample preparation.

  5. Decontaminate sampling equipment in accordance with EPA Guidance for AssessingChemical Contaminant Data for Use In Fish Advisories, if such equipment will be re-used.
  6. Sources of extraneous tissue contamination include contamination from sampling gear,grease from ship winches or cables, spilled engine fuel (gasoline or diesel), engineexhaust, dust, ice chests, and Blue Ice® used for cooling. All potential sources ofcontamination in the field should be identified and appropriate steps taken to minimize oreliminate them. For example, during sampling, the boat should be positioned so thatengine exhausts do not fall on the deck. Ice chests should be scrubbed clean withdetergent and rinsed with distilled water, and sealed before being taken on the boat. Toavoid contamination, samples should be handled with new, clean, disposable gloves only,after being taken aboard the boat. When not being handled, samples must only be placedon the dull side of unused foil or kept in life tanks with clean, fresh seawater. After fieldmeasurements, tagging, and wrapping in foil, the samples shall placed in waterproofplastic bags. Sampling equipment that has obviously been contaminated by oils, grease,diesel fuel, or gasoline should not be used. All utensils or equipment that will be useddirectly in handling shellfish (e.g., shellfish measuring board or calipers) should becleaned prior to each sampling trip, rinsed in acetone and pesticide-grade hexane orAlconox,distilled water decon, and stored in aluminum foil until use. Between samplingsites, the field collection team should clean each measurement device by rinsing it withambient water, followed by a rinse with distilled water, and rewrapping it in aluminumfoil to prevent contamination.

  7. Marine biota (shellfish) samples collected as part of the EI will be composited in thelaboratory.


Photographs will be taken throughout the field sampling effort to document samples. In addition,field sampling information should be recorded with, at a minimum, the following information foreach target sampling area:

AREA # GPS Coordinates Location Description Species - Number Collected Notes Date

Sub-Area 1

Sub-Area 2

Sub-Area 3
Sub-Area 4

Sub-Area 5

Sample packing and shipping

All samples collected will be assigned unique sample numbers, labeled, noted in waterproof inkin a bound, Rite-in-the-Rain® field logbook, and recorded on the chain-of-custody form. Labelsfor sample containers will be filled out completely with all appropriate information. Samples willthen be packed for shipment to the laboratory according to the current U.S. Department ofTransportation (DOT) and Washington Administrative Code (WAC) 173-303-071(3)(1)requirements. Sample containers will be packed in coolers with a low-density packing material,and Blue Ice® (or equivalent). The coolers will be securely sealed.

All samples will be shipped via express delivery for overnight delivery to the contractedlaboratory (AXYS Analytical). A commercial invoice supplied by AXYS Analytical will be usedto facilitate delivery of the containers across the U.S. - Canadian border. Custody seals will beused on coolers. Samples will be shipped no later than Thursday of a given week. If samplescannot be shipped by Thursday, they will be held on ice until the following Monday. Aminimum of 10 bags of Blue Ice® per chest will be necessary to hold temperature for as long astwo days in the event samples are delayed in shipment.

Upon receipt at the laboratory, the custody seal will be broken, and the receiver will record thecondition of the samples. The chain-of-custody form will be signed. The samples will be loggedinto the Laboratory Information Management System (LIMS) to allow the samples to be trackedwhile in the custody of the Laboratory. Sample security will be assured since the AXYSAnalytical premises are locked with restricted access at all times. After homogenization, thesamples will be maintained frozen until analyses are completed. Final disposition of anyremaining sample will be decided in consultation with the DOH and the Tribe.

Laboratory Analytical Methods

AXYS Analytical Services (Sydney, B.C.) will analyze shellfish samples received from bothColumbia Analytical (Rayonier's lab), and from the joint DOH/tribal exposure investigation.Samples received from Columbia Analytical will be pre-homogenized. Shellfish samples fromthe EI will be sent whole. The sample analysis will be performed by EPA method 1613B, usinghigh resolution GC/MS. The method includes analysis of 17 dioxin and furan congeners. Methoddetection limits are expected to be in the range of 0.02 per trillion (ppt) to 1 ppt, depending onthe congener and sample size available for analysis. Lipid analysis will also be performed oneach sample.

Quality Assurance/Quality Control

Split shellfish tissue samples will be obtained from Rayonier, to be analyzed separately byAXYS Analytical. The results will be included with the analysis report for the EI samples.Standard laboratory quality control procedures will be utilized, including method and instrumentblanks, surrogate recoveries, and laboratory control samples. In addition AXYS Analytical willinclude a sixth initial calibration point (5 times lower than the method stated CS-1) to allowreporting uncensored data to the lowest level possible. All method QA/QC requirements will bemet for instrument tuning, resolution and calibration prior to sample analysis.

Data Reporting

AXYS Analytical will prepare data analysis reports within two weeks of completing the analysis,summarizing the results of all samples (field, split, and lab QA). The reports will include theresults of the chemical and lipid analysis, and all quality assurance and quality control reports asrequired by EPA Method 1613 including initial calibration, calibration verification, GC columnresolution, procedural blank and ongoing precision and recovery (OPR) results.

Data Analysis

AXYS Analytical will provide a data analysis package upon completion of the project. The datawill be evaluated by DOH in a health consultation, which will be provided to the Tribe, Ecology,Rayonier, and the community.


This Health Consultation was prepared by the Washington State Department of Health under acooperative agreement with the Agency for Toxic Substances and Disease Registry (ATSDR). Itis in accordance with approved methodology and procedures existing at the time the healthconsultation was begun.

Debra Gable
Technical Project Officer,

The Division of Health Assessment and Consultation, ATSDR, has reviewed this public healthconsultation and concurs with the findings.

Roberta Erlwein
Section Chief,

Table of Contents The U.S. Government's Official Web PortalDepartment of Health and Human Services
Agency for Toxic Substances and Disease Registry, 4770 Buford Hwy NE, Atlanta, GA 30341
Contact CDC: 800-232-4636 / TTY: 888-232-6348

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