Draft Sampling and Analysis Plan Iron King Mine – Humboldt

TO-02-09-10-09-0004:002693.2110.01RA

Draft Sampling and Analysis PlanIron King Mine – Humboldt Smelter

AssessmentYavapai County, Arizona

TDD No.: TO-02-09-10-09-0004Project No.: 002693.2110.01RA

March 2011

Prepared for:

U.S. ENVIRONMENTAL PROTECTION AGENCYRegion IX

Prepared by:

ECOLOGY AND ENVIRONMENT, INC.3700 Industry Avenue Suite 102

Lakewood, CA 90712

SDMS DOCID# 1127634

iii

able of ContentsTSection Page

1 Introduction ..............................................................................1-11.1 Project Organization......................................................................................... 1-21.2 Distribution List ............................................................................................... 1-31.3 Statement of the Specific Problem ................................................................... 1-3

2 Site Background.......................................................................2-12.1 Site Location and Description .......................................................................... 2-12.2 Site History....................................................................................................... 2-1

3 Project Objectives....................................................................3-13.1 Data Use Objectives ......................................................................................... 3-13.2 Project Sampling Objectives ............................................................................ 3-13.3 Action Levels ................................................................................................... 3-23.4 Data Quality Objectives ................................................................................... 3-43.5 Data Quality Indicators (DQIs) ........................................................................ 3-43.6 Schedule of Sampling Activities ...................................................................... 3-43.7 Special Training Requirements/Certifications ................................................. 3-4

4 Sampling Rationale and Design..............................................4-14.1 Small Tailings Pile Sampling........................................................................... 4-24.2 Properties Not Previously Sampled.................................................................. 4-24.3 Properties Previously Sampled......................................................................... 4-34.4 Analytes of Concern......................................................................................... 4-4

5 Request for Analyses...............................................................5-15.1 Laboratory Analysis ......................................................................................... 5-1

6 Field Methods and Procedures ...............................................6-16.1 Field Procedures ............................................................................................... 6-1

6.1.1 Standard Operating Procedures and Equipment................................... 6-16.1.2 Equipment Maintenance....................................................................... 6-16.1.3 Inspection/Acceptance Requirements for Supplies and

Consumables ........................................................................................ 6-16.1.4 Logbooks .............................................................................................. 6-16.1.5 Photographs .......................................................................................... 6-26.1.6 Electronic Sample Logging.................................................................. 6-3

Table of Contents (cont.)

Section Page

iv

6.1.7 Mapping Equipment ............................................................................. 6-36.2 Soil Sampling Procedures ................................................................................ 6-3

6.2.1 Discrete Sampling ................................................................................ 6-36.2.2 Composite Sampling ............................................................................ 6-46.2.3 Surface Soil Collection Procedure ....................................................... 6-4

7 Disposal of Investigation-Derived Waste ...............................7-1

8 Sample Identification, Documentation and Shipment ...........8-18.1 Sample Nomenclature ...................................................................................... 8-18.2 Container, Preservation, and Holding Time Requirements.............................. 8-18.3 Sample Labeling, Packaging, and Shipping..................................................... 8-18.4 Chain-of-Custody Forms and QA/QC Summary Forms.................................. 8-2

9 Quality Assurance and Control (QA/QC)................................9-19.1 Field Quality Control Samples ......................................................................... 9-1

9.1.1 Assessment of Field Contamination (Blanks) ...................................... 9-19.1.1.1 Equipment Blank Samples..................................................... 9-19.1.1.2 Field Blanks ........................................................................... 9-1

9.1.2 Assessment of Sample Variability (Field Duplicate or Co-located Samples) .................................................................................. 9-1

9.1.3 Laboratory Quality Control (QC) Samples .......................................... 9-19.1.4 Confirmation Samples.......................................................................... 9-19.1.5 Field Analytical Quality Control (QC) Samples .................................. 9-2

9.2 Analytical and Data Package Requirements .................................................... 9-29.3 Data Management ............................................................................................ 9-29.4 Data Validation ................................................................................................ 9-39.5 Field Variances................................................................................................. 9-49.6 Assessment of Project Activities...................................................................... 9-4

9.6.1 Assessment Activities .......................................................................... 9-49.6.2 Project Status Reports to Management ................................................ 9-59.6.3 Reconciliation of Data with DQOs ...................................................... 9-5

10 References..............................................................................10-1

A Data Quality Objective Process Document ........................... A-1

B Site Specific Health and Safety Plan...................................... B-1

C Standard Operating Procedures ............................................ C-1

v

ist of TablesL

ist of Figures

ist of TablesL

L

Table 2-1 Iron King Mine - Humboldt Smelter Assessment "Additional ActionRecommended under the TCRA" List ....................................................................... 2-3

Table 3-1 Benchmarks and Data Quality Indicator Goals - Definitive Data for EPAMethod 6010B ........................................................................................................... 3-3

Table 4-1 Small Tailings Pile Historic Data .............................................................................. 4-3

Table 5-1 Assessment Sampling and Analysis Summary.......................................................... 5-2

Figure 2-1 Site Location Map...................................................................................................... 2-2

Figure 2-2 Site Details Map......................................................................................................... 2-4

vi

ist of Abbreviations and AcronymsLADEQ Arizona Department of Environmental Quality

bgs below ground surface

COPC contaminant of potential concern

DQI Data Quality Indicator

DQO Data Quality Objective

EA EA Engineering, Science and Technology, Inc.

E&E Ecology and Environment, Inc.

ERS Emergency Response Section

FOSC Federal On-Scene Coordinator

ft2 square foot

GPS Global Positioning System

IDW investigation-derived waste

LCS laboratory control sample

MS/MSD matrix spike/matrix spike duplicate

mg/kg milligrams per kilogram

PM Project Manager

PPE personal protective equipment

QA quality assurance

QC quality control

RI Report Remedial Investigation Report

RPD relative percent difference

List of Abbreviations and Acronyms (cont.)

vii

RSL Regional Screening Level

SAP Sampling and Analysis Plan

SOP standard operating procedure

SRL Soil Remediation Level

STP Small Tailings Pile

START Superfund Technical Assessment and Response Team

TCRA time-critical removal action

TM Task Monitor

UCL upper confidence limit

U.S. EPA United States Environmental Protection Agency

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1 IntroductionThe United States Environmental Protection Agency (U.S. EPA) tasked Ecology andEnvironment, Inc.’s (E & E’s) Superfund Technical Assessment and Response Team (START)to support a U.S. EPA-funded Removal Assessment of the Iron King Mine – Humboldt SmelterSuperfund Site (the site), located in Dewey-Humboldt, Arizona. In order to support the U.S.EPA’s environmental data collection activities, the START has identified project data qualityobjectives and developed this Sampling and Analysis Plan (SAP).

The U.S. EPA Region IX Emergency Response Section (ERS) will conduct an assessment oflead and arsenic contamination in surface soils within a residential neighborhood at the site, andan assessment of lead, arsenic and cyanide contamination in what is referred to as the SmallTailings Pile (STP) located on a residential property located to the north of the Iron King Minetailings pile. Previous investigations performed by the Arizona Department of EnvironmentalQuality (ADEQ), E & E, and EA Engineering, Science and Technology, Inc. (EA) found thatlead and arsenic are present in site soils at concentrations that exceed the U.S. EPA’s regionalscreening levels for a residential scenario (r-RSL, formerly Preliminary Remediation Goals). Ther-RSL for total lead in soil is 400 milligrams per kilogram (mg/kg), and the r-RSL for arsenic insoil is 0.39 mg/kg. The arsenic r-RSL is well below the typical arsenic concentrationshistorically found in background areas about the site.

The investigations conducted by ADEQ, E & E, and EA identified elevated levels of lead andarsenic on residential properties near the Iron King Mine and Humboldt Smelter. The latestinvestigation was conducted by EA for the U.S. EPA and was documented in a RemedialInvestigation Report, Iron King Mine – Humboldt Smelter Superfund Site, Dewey-Humboldt,Yavapai County, Arizona (Revision 01, March 2010) (RI Report). The RI Report combinedprevious historical data from ADEQ and E & E with data collected by EA in 2008 and 2009 inorder to provide information for a feasibility study of site remediation options. However, the RIReport concluded, “the full extent of residential impacts has not been determined, as many yardshave not yet been sampled.” Because some potentially-impacted parcels had not yet beensampled, and because some already-sampled residential parcels are in need of additionalsampling, the U.S. EPA is performing the Removal Assessment which is the subject of this SAP.

For the Removal Assessment, the START prepared a “hot list” of residential properties whichhad already been sampled and which could potentially be candidates for a Removal Action. Tocompile the list, the START used a database of all available historical residential data for arsenicand lead concentrations in surface soil, which had been compiled by EA. The database includedadditional data obtained by EA in May 2010 which was not part of the RI Report. The 95%upper confidence limit (UCL) for arsenic and lead at each individual property was calculatedusing the data. Each individual property was then placed in a list of descending order (highest tolowest) of its calculated 95% UCL concentration of arsenic and lead This procedure was thesame ranking process that was used in the RI Report. In order to limit the initial scope of theremoval assessment and the potential removal actions, the U. S. EPA determined that only theproperties in the top 10% of that population would be placed on the “hot list.” Additionally,

1. Introduction

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residential properties that had not yet been sampled but which were located in potentially-contaminated areas were added to the hot list. In January 2011, the START and U.S. EPAinspected all the properties on the hot list, and were able to eliminate some of the properties fromthe list due to environmental factors such as adequate landscaping coverage over potentially-contaminated soil or the lack of a dwelling on the property. This process of hot list compilationwas conducted to support a potential U.S. EPA time-critical removal action (TCRA), and is notmeant to preclude any properties that are not on the hot list from the possibility of futureconsideration for remedial action. As of the date of this SAP, the hot list has been renamed the“Additional Action Recommended under the TCRA” list.

The scope of work and objectives outlined in this SAP are derived from the direction of the U.S.EPA. This SAP describes the project and data use objectives, data collection rationale, dataquality assurance goals, and requirements for sampling and analysis activities. It also defines thesampling and data collection methods that will be used for this project. This SAP is intended toaccurately reflect the planned data-gathering activities for this support activity; however, siteconditions, budget, and additional U.S. EPA direction may warrant modifications. All significantchanges are to be documented in site records.

The specific field sampling and chemical analysis information in this SAP was prepared inaccordance with the following U.S. EPA documents: EPA Requirements for Quality AssuranceProject Plans (EPA QA/R 5, March 2001, EPA/240/B 01/003); Guidance on Systematic PlanningUsing the Data Quality Objectives Process (EPA QA/G 4, February 2006, EPA/240/B-06/001);Guidance on Choosing a Sampling Design for Environmental Data Collection (EPA QA/G 5S,December 2002, EPA/240/R 02/005); Superfund Lead-Contaminated Residential SitesHandbook (OSWER 9285.7-90, August 2003); and Uniform Federal Policy for ImplementingEnvironmental Quality System (EPA/505/F-03/001, March 2005).

1.1 Project OrganizationU.S. EPA Federal On-Scene Coordinator (FOSC) – The U.S. EPA FOSC is Mr. CraigBenson. Mr. Benson is the primary decision-maker and will direct the project, specify tasks, andensure that the project is proceeding on schedule and is within budget. Additional duties includecoordination of communication with the START Project Manager, U.S. EPA Quality Assurance(QA) Office, and community residents.

START Project Manager (PM) – Mr. Michael Schwennesen is the START PM. The PMmanages the project’s data collection efforts and is responsible for implementing the SAP,coordinating project tasks and field sampling, managing field data, and completing allpreliminary and final reporting.

Principal Data Users – Data generated during the implementation of this SAP will be utilizedby the FOSC to make decisions regarding potential removal activities.

START Quality Assurance Coordinator – Mr. Howard Edwards is responsible for thedevelopment of this SAP. Specifically, Mr. Edwards is responsible for the documentation ofproject objectives and for preparation and review of the draft and final SAP document. Mr.Edwards will coordinate with the U.S. EPA’s Quality Assurance Office as needed.

1. Introduction

1-3

Sample Analysis and Laboratory Support – The U.S. EPA’s Region IX Laboratory inRichmond, California, will be responsible for lead and arsenic sample analysis by definitiveanalytical methodologies. This laboratory will GEL Laboratories, LLC will be responsible forcyanide sample analysis by definitive analytical methodologies.

1.2 Distribution ListCopies of the final SAP will be distributed to the following persons and organizations:

■ Craig Benson, U.S. EPA Region IX

■ U.S. EPA Region IX, Quality Assurance Office

■ E & E START Field Team

■ E & E START project files

1.3 Statement of the Specific ProblemThere is public and regulatory concern as to whether residents adjacent to the Iron King Mineand Humboldt Smelter may be currently exposed to, or have potential for exposure to, lead andarsenic contamination documented as being present in residential soil. Additionally, overlandwater flow from the STP discharges directly into the Chaparral Gulch, a natural drainagechannel, which crosses under Highway 69, passes through the residential area and eventuallyflows into the Agua Fria River. Arsenic and lead are the contaminants of concern (COPCs) forthis project. Cyanide was used in the mining process but has historically been found at relativelylow levels and is therefore not considered a COPC. Other metals may also be present but are notconsidered by the U.S. EPA as COPCs. There are documented concentrations of these COPCs onresidential properties at the site that exceed the r-RSLs and the EA-established averagebackground concentrations of 48 mg/kg for arsenic and 44 mg/kg for lead in the residential areasof the site. The U.S. EPA has determined that additional surface and subsurface soil sampling onsome residential properties and at the STP is necessary in order to corroborate and/or refineCOPC concentrations on the properties. In addition, the U.S. EPA has determined that soilsamples should be collected from some residential properties for which there is currently no data.The information obtained will be used to determine whether certain residential properties shouldbe included in a time-critical removal action.

2. Site Background

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2 Site Background

2.1 Site Location and DescriptionThe Iron King Mine – Humboldt Smelter site is located in Dewey-Humboldt, Yavapai County,Arizona (Figure 2-1). Residential properties in the town of Dewey-Humboldt are situated between the

mine and the smelter, and are the focus of this SAP. Lead and arsenic contamination in theresidential neighborhood is attributed to both the mine and the smelter. Properties have beenplaced on a hot list for sampling or additional sampling based on historical samplinginformation, a lack of historical sampling data, or to identify composition and extent ofcontamination. The properties which have been identified as requiring sampling or additionalsampling are presented in Table 2-1 and Figure 2-2.

The approximately 153-acre Iron King Mine property is located west of Highway 69 and isbordered by the Chaparral Gulch and residences to the north; Highway 69 to the east; GalenaGulch to the south; and undeveloped land to the west. The Humboldt Smelter property is locatedless than one mile east of the Iron King Mine property, on the east side of Highway 69. Theapproximately 189-acre smelter property is bounded by residences to the north and west; theAgua Fria River to the east; and Chaparral Gulch to the south. The area to be investigated forthis SAP resides between the mine and the smelter. No sampling will be conducted at the mineor smelter as a part of this SAP.

2.2 Site HistoryADEQ initially sampled sediment near residential parcels throughout the Chaparral Gulch as partof a Preliminary Assessment/Site Inspection (PA/SI) in April, 2002. The investigation revealedarsenic concentrations of up to 509 mg/kg and lead concentrations of up to 513 mg/kg. In 2005,ADEQ requested that U.S. EPA Region 9 ERS assess surface soils at residential properties in thevicinity of the Chaparral Gulch and Iron King Mine.

In 2005, to support the U.S. EPA ERS, E & E conducted a Site Assessment of 17 propertiesalong the Chaparral Gulch. Soil samples were collected to determine arsenic and leadconcentrations on these properties. Ten samples were collected from each property, whichincluded nine surface samples (0-6 inches below ground surface [bgs]) and one subsurfacesample (1.5 feet bgs). Analytical results from the sampling event identified lead and arsenicconcentrations in surface soil samples at four of the properties that were sufficiently high towarrant a removal action, which was conducted by Brown and Caldwell in late 2006.

In 2008, the Iron King Mine – Humboldt Smelter site was listed on the National Priorities Listand a Remedial Investigation was conducted by EA which included additional sampling duringSeptember 2008, and April and May of 2009. An additional 48 parcels, 45 of which wereprivately owned and three associated with an elementary school playground, were part of thestudy. Background Soil Type 1 was identified as the predominant soil type for the study area,and a background concentration of 48 mg/kg for arsenic and 44 mg/kg for lead was established.In May, 2010, EA sampled an additional 117 residential parcels throughout the site as part of thestudy.

Source: ESRI Streetmaps

Figure 2-1Site Location Map

Iron King Mine - Humboldt Smelter AssessmentDewey-Humboldt, Arizona

Yavapai County

Project # 002693.2110.01RATDD# TO 02-09-10-09-0004

!(Dewey-Humboldt

´0 4 8 Miles

Humboldt SmelterHumboldt Smelter

Area ofArea ofDetailDetail

Iron King MineIron King Mine

Table 2-1Iron King Mine - Humboldt Smelter Assessment

"Additional Action Recommended under the TCRA" List

OFS-301(NA-1)

402-06-102V 2985 Sweet Pea Lane

OFS-302(NA-2)

402-07-015B 2795 S. Butte Street

OFS-303(NA-3)

402-07-011A 2860 S. Azurite Street

OFS-305(NA-5)

402-07-013A402-07-014A

2865 S. Butte Street2827 S. Butte Street

OFS-306(NA-6)

402-06-026402-06-027B

13087 E. Main Street13089 E. Main Street

OFS-307(NA-7)

402-10-029A 12982 E. Main Street

OFS-308(NA-8)

402-07-019A 2855 S. Calumet Street

OFS-309(NA-9)

402-08-071K 2975 South Omega Drive

OFS-310(NA-10)

402-10-020A 12858 East Chaparral Alley

OFS-311(NA-11)

402-06-076 2746 Calumet Street

OFS-312(NA-12)

402-07-060A 2680 S. Jones Street

OFS-314(NA-14)

402-05-069 13555 East Lazy River Drive

OFS 002 402-08-034A 12470 East Yavapai RoadOFS 105 402-06-028J 2875 S. AzuriteOFS 108 402-06-028S 2877 South Azurite StreetOFS 111 402-06-102L 2925 South Sweet Pea LaneOFS 114 402-08-012E 2655 Colina LaneOFS 116 402-07-017H 2840 S. Dana StreetOFS 117 402-10-050D 2845 South First StreetOFS 118 402-06-102K 2905 South Sweet Pea LaneOFS 132 402-06-102P 2875 South Third StreetOFS 133 402-07-006 13070 Main StreetOFS 148 402-06-102N 2965 Sweet Pea Lane

OFS 153402-10-023402-10-024

12832 and 12838 East Chaparral Street

OFS 157 402-08-017B 2560 S. Colina Lane

OFS 203402-06-028M402-06-028T

13425 E. Prescott Street

OFS 208 402-09-016D 2565 Hill Street

OFS 227402-07-061A402-07-061B

2670 South Jones Street

OFS 244 402-09-016H 2575 Hill StreetOFS 260 800-27-005T Unsurfaced alley behind Sweet Pea Lane.

Residential

Parcel IDParcel Number Physical Address

Purple = No Additional Sampling; Removal Recommended; Yellow = Sample to Assess forPotential Further Action; Red = Additional Sampling Recommended

SchwennesenM

TextBox

Figure 2-2

3. Project Objectives

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3 Project Objectives

3.1 Data Use ObjectivesBased on available information documented by the previous investigations and at the request ofthe Remedial Program of the U.S. EPA, the U.S. EPA ERS is conducting a removal assessmentto:

Determine whether unacceptable risks to human health are present at the site due toelevated lead and arsenic concentrations in residential property surface soils.

Obtain data to determine the horizontal and vertical extent of the STP.

Obtain data for the purposes of potentially performing a removal action.

The lead and arsenic concentration data generated by this assessment will be used to:

Obtain initial data or refine currently-available data on lead and arsenic contaminationfor properties on the “Additional Action Recommended under the TCRA” list.

Determine whether a removal action at any of the properties on the “Additional ActionRecommended under the TCRA” list is warranted.

Better-characterize the Small Tailings Pile (STP) for possible future removal activities.

The cyanide and additional metals concentration data generated by this assessment will be usedto more help characterize the contamination on site for future removal action.

Analytical data collected as part of this removal assessment will be used to answer the followingsite-specific study questions:

What are the lead and arsenic concentrations in areas of exposed residential soils for propertieson the “Additional Action Recommended under the TCRA” list?

What are the lead, arsenic, and cyanide concentrations at, and what are the horizontal andvertical extents of, the Small Tailings Pile?

3.2 Project Sampling ObjectivesThe data obtained through the implementation of this SAP will be used to evaluate lead andarsenic concentrations in surface and subsurface soils at properties on the “Additional ActionRecommended under the TCRA” list. The sampling results will be reviewed to determinewhether certain properties may be candidates for a removal action. The data obtained will also beused to evaluate lead, arsenic, and cyanide concentrations in the STP at various locations anddepths, for the purpose of corroborating data generated by EA and to support determination ofwhether or how the STP should be moved.


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The U.S. EPA tasked the START to prepare this SAP to support the environmental datacollection activities needed to support assessment of the site.

Soil sampling, followed by definitive laboratory sample analysis, will be performed toaccomplish the project objectives. Sampling objectives include:

Obtain data regarding lead and arsenic concentrations in soil that can be used to determinewhich residential properties on the “Additional Action Recommended under the TCRA” listshould be considered for a removal action.

Document the concentrations of lead and arsenic in surface soils in the immediate areatypically accessed by the residents.

More-completely define the area of the STP with regard to arsenic and lead concentrations,in order to provide data pertaining to possible means for relocating the STP to minimize off-site migration of contaminated material.

3.3 Action LevelsThere is no site-specific action level concentration for arsenic or lead that will be used to initiatefurther investigation or removal. Once the data is obtained, these properties will have their 95%UCLs for arsenic and lead calculated or re-calculated. Properties that remain in the top 10%UCL for arsenic and/or lead (when compared to all site properties sampled) will remain on the“Additional Action Recommended under the TCRA” list and the FOSC will then determinewhich properties on the list will be candidates for a removal action.

Table 3-1 presents information regarding data quality indicator goals for this project.


3-3

Table 3-1 Benchmarks and Data Quality Indicator Goals - Definitive Data for EPA Method 6010BIron King Mine – Humboldt Smelter

Yavapai County, ArizonaE & E Project No. 002693.2110.01RA TDD No. TO2-09-10-09-0004

Chemicalof

PotentialConcern

UpperEstimatedRegional

BackgroundConcentration

(mg/kg)

Site-SpecificAction Level

forAssessment

(mg/kg)

U. S. EPARSL

(mg/kg)

U. S. EPARegion IX

LaboratoryReporting

Limits (mg/kg)

SW-846 Method6010B

Accuracy(% Recovery

for MS/ MSD)

Precision(RPD from

MS/MSD andDuplicates)

PercentCompleteness

Lead 44 NA 400 3 75 – 135 <35% > 90%Arsenic 48 NA 0.39 2 75 – 135 <35% > 90%

Notes:mg/kg = milligrams per kilogramRSL = U.S. EPA Regional Screening Level (December 2009)MS/MSD = Matrix Spike/Matrix Spike DuplicateNA = Not applicable. See Section 3.3RPD = Relative Percent Difference

2011 ecology & environment, inc.


3-4

3.4 Data Quality ObjectivesThe data quality objective (DQO) process, as set forth in the U.S. EPA Guidance on SystematicPlanning Using the Data Quality Objectives Process (EPA/240/B-06/001) (U.S. EPA, 2006),was followed to establish the DQOs for this project. An outline of the process and the outputs forthis project are included in Appendix A.

3.5 Data Quality Indicators (DQIs)Data quality indicators (DQIs) are defined as: precision, accuracy, representativeness,completeness, comparability, and method detection limits. The DQIs for this project weredeveloped following the guidelines in the U.S. EPA Requirements for Quality Assurance ProjectPlans (U.S. EPA, 2001). All sampling procedures are documented in Sections 6.2 and 6.3.Standard operating procedures will be followed to ensure representativeness of sample results byobtaining characteristic samples. Approved U.S. EPA methods and standard reporting limits willbe used. All data not rejected will be considered complete. Table 3-1 documents the site-specificDQI goals for lead and arsenic.

3.6 Schedule of Sampling ActivitiesThe field sampling and analysis activities are scheduled to commence on March 7, 2011. Thefield activities are not anticipated to exceed five days. However, because access agreementsmust be obtained from property owners of properties on the “Additional Action Recommendedunder the TCRA” list, additional field sampling episodes may be required if access agreementscannot be obtained in time for all the properties on the list.

3.7 Special Training Requirements/CertificationsData validation requires specialized training and experience. The START PM will ensure that aqualified START chemist will perform a Tier 2 validation of 100 percent of the data (as definedin the U.S. EPA document, Requirements for Quality Assurance Project Plans (March 2001).Specific data validation requirements are discussed in Section 9.4.

Field sampling personnel should be trained and have experience with soil sampling at hazardouswaste sites while wearing appropriate protective equipment. One field sampler should be trainedand familiar with Global Positioning System (GPS) data collection. All sampling personnel musthave appropriate training that complies with 29 Code of Federal Regulations 1910.120. The site-specific health and safety plan for this project is to be appended to this plan by projectmanagement (Appendix B).

4. Sampling Rationale and Design

4-1

4 Sampling Rationale and DesignThe START reviewed available site information, including previous sampling data, and took intoaccount the U.S. EPA FOSC’s objectives for the removal assessment to determine the specificsampling design.

Identification of lead and arsenic concentrations in residential soils within the Iron King Mine –Humboldt Smelter site and further characterization of the Small Tailings Pile are the principalobjectives of this removal assessment.

The sampling rationale and design for the residential properties on the “Additional ActionRecommended under the TCRA” list are discussed below. The locations of the residences inwhich the sampling will be conducted are shown in Figure 2-2. It is possible that additionalresidential properties may be removed or added to the “Additional Action Recommended underthe TCRA” list based on further gained knowledge obtained in the field, and therefore thecomplete list of properties investigated may change. A finalized list of properties sampled willbe included in the removal assessment report that will describe the sampling event.

Properties identified with a yellow color in Table 2-1 and Figure 2-2 have not been previouslysampled, and these sites will be sampled as described in Section 4.2. Properties identified with ared color in Table 2-1 and Figure 2-2 has been sampled in the past and these sites will besampled as described in Section 4.3.

The properties sampled, and the exact methodology used for sampling will be discussed in theremoval assessment report as the exact location of samples and the type of samples collectedcannot be precisely known until the field team is on site. Professional judgment of the field teamwill be used to assess and implement the guidelines outlined in this document.

The U.S. EPA Superfund Lead-Contaminated Residential Sites Handbook (OSWER Directive9285.7-50 (August, 2003) (Lead handbook) was referenced during development of the samplingdesign and will be used as a guideline where applicable. Previous sampling methodology hasalso been considered, in order to obtain data in a similar manner to that historically conducted.After collection, samples will be handled and analyzed according to Sections 5.1, 6.2, and 6.3 ofthis SAP. Sample locations will be recorded in the field logbook as sampling is completed.Individual sample-point locations will be recorded using GPS equipment, whenever possible.The sampling design will generate samples that may have contaminants derived from the IronKing Mine, Humboldt Smelter, lead-based paint, automotive and other mechanical activity, areallead and arsenic deposition, and naturally-occurring lead and arsenic.

In addition to arsenic, lead, and (at the STP) total cyanide analyses, certain samples may beanalyzed for a more-complete metals analytical suite.


4-2

4.1 Small Tailings Pile SamplingSampling will be conducted at the STP with two specific goals in mind: to further-characterizethe source material and to more-adequately define the areal extent of the pile. Both goals willsupport potential STP relocation activities. Subsurface soil samples will be collected to assess thedepth of contamination near the central area of the pile and surface soil samples will be collectedon the periphery of the pile to assess the horizontal extent of contamination.

All samples collected from the STP will be analyzed for lead and arsenic. A subset of samples,to be determined by the START PM in consultation with the FOSC, may be analyzed for totalcyanide. Total cyanide analyses will be performed on some of the samples from the STP inorder to corroborate what appear to be relatively low levels of cyanide previously detected.Historic analytical results for the STP are included in Table 4-1. Sampling design will bedetermined in the field based upon the judgment of the START PM and the FOSC. Inputs tosupport the field decisions for the sampling design will include topography around the STP;observed erosion patterns; and the distribution of tailings material. It is expected that bothvisually-biased and systematic sampling may be used to establish sampling locations.

It is expected that both discrete and composite samples will be collected at the STP.Approximately 10 to 15 discrete samples and 3 to 5 composite samples will be collected. Thesampling locations and sample types (discrete or composite) will be designated by the FOSCwhen in the field. Data generated through the sampling of the STP will be used to better-delineate the extent and depth of the pile. The information gained will be used to prepare anestimate of the volume of the pile.

4.2 Properties Not Previously SampledUsing a similar sampling methodology implemented by E & E in 2005 and by EA during theRemedial Investigation events, for properties not previously sampled (”yellow” sites), theSTART will collect a total of 10 samples from nine locations per property. A judgmentalsampling system based on observed field information will be implemented. The information willinclude observed property use and the observed potential for human target interaction withpotentially contaminated soil. Nine surface soil samples will be collected from a depth of 0-2inches bgs and one deep sample (co-located with one of the shallow samples) will be collectedfrom a depth of 10-12 inches. The objective of the sampling team will be to select sampleplacement providing adequate coverage of each yard. However, sampling locations may bebiased based on factors determined in the field such as use, cover, proximity to structure, playareas, etc. The factors influencing sampling locations will be noted in the field logbook.

The Lead Handbook guidance for sampling in yards greater than 5,000 square foot (ft2)recommends that, at a minimum, composite samples should be collected from each of the fourquadrants of the yard surrounding a residential structure and from the drip zone around theresidential structure (U.S. EPA, 2003). However, to maintain uniformity between the existingdataset and the data that will be generated during this event, grab samples will be collected fromjudgmentally-selected locations throughout the property. The Lead Handbook also recommendssampling play areas and gardens as discrete areas of a yard, and this recommendation will betaken into consideration when determining sample locations in the field. Samples will becollected from open areas rather than from, for example, grass-covered or paved areas.


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The number of samples collected at properties not previously sampled will depend on thenumber of property owners that return access agreements. If all property owners respond, 120samples (not including quality control samples) will be collected at properties not previouslysampled.

Table 4-1 Small Tailings Pile Historic DataIron King Mine – Humboldt Smelter

E & E Project No. 002693.2110.01RATDD No. TO2-09-10-09-0004

Sample ID DateSampled

Depth ofSample (bgs)

Arsenic(mg/kg)

Cyanide(mg/kg)

Lead(mg/kg)

IKJ-537 08/21/2008 4-7 feet 24.7 NR 9.6IKV-117 08/21/2008 4-7 feet 79.5 NR 82.9IKJ-538 08/21/2008 4-7 feet 42.9 NR 22.9IKV-113 08/21/2008 4-7 feet 37.3 NR 26.1IKV-116 08/21/2008 4-7 feet 141 NR 64.2IKJ-539 08/21/2008 4-7 feet 57.3 NR 35.8IKJ-537 08/21/2008 0-2 feet 65.6 NR 36.8IKV-117 08/21/2008 0-2 feet 167 NR 161IKJ-538 08/21/2008 0-2 feet 35 NR 16.1IKV-113 08/21/2008 0-2 feet 144 NR 109IKV-116 08/21/2008 0-2 feet 66.4 NR 34.7IKJ-539 08/21/2008 0-2 feet 22 NR 13.8IKV-115 08/21/2008 0-2 feet 99 NR 105IKJ-578 04/28/2009 0-0.5 feet 1980 NR 2470 JIKJ-579 05/03/2009 0-0.5 feet 985 J NR 1400IKJ-582 04/28/2009 0-0.5 feet 1020 5.5 1580IKJ-580 04/28/2009 0-0.5 feet 1510 NR 1180IKJ-581 04/28/2009 0-0.5 feet 595 NR 480IKV-114 08/21/2008 0-2 feet 54.8 NR 36.4IKJ-582 Unknown 2-10 feet NR 0.22 J NR

Notes:mg/kg: milligrams per kilogrambgs: below ground surfaceNR: not reportedJ: estimated concentration

4.3 Properties Previously SampledAdditional samples will be collected from properties which have previously been sampled (‘red”sites) to supplement the dataset in an attempt to corroborate or further delineate and define theextent of on-site contamination. Two factors that may necessitate further sampling at theseproperties include:

1. historic sample concentration anomalies or data outliers that may be artifacts not relatedto the Iron King Mine – Humboldt Smelter site, that have elevated a particular property’sUCL concentration of lead and/or arsenic to the level that placed it on the “AdditionalAction Recommended under the TCRA” list.

2. inadequate historic sampling areal coverage of a property.

Additional samples collected from “red” sites will be five-point composite samples collectedfrom locations designated by the FOSC.


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The number of composite samples to be collected at properties previously sampled will dependon the number of property owners that return access agreements. If all property owners respond,it is anticipated that between 25 and 50 composite samples will be collected, not includingquality control samples.

4.4 Analytes of ConcernThe analytes of concern are lead and arsenic. All samples collected in the field will be analyzedfor lead and arsenic using the U.S. EPA Region IX Laboratory in Richmond California fordefinitive lead and arsenic analysis by U.S. EPA Method 6010B. Additionally, a subset ofsamples collected from the STP will also be sent to GEL Laboratories for total cyanide analysisby U.S. EPA Method 9010/9012. In addition to arsenic, lead, and (at the STP) total cyanideanalyses, certain samples may be analyzed for a more-complete metals analytical suite. The 17metals included in California Code of Regulations, Title 22 (Cam-17 metals) may be investigatedif a particular property or sampling location is determined by the on-site federal On-SceneCoordinator) FOSC to warrant the additional analyses.

The selected analyses will generate lead and arsenic concentration data that may include lead andarsenic derived from the Iron King Mine and Humboldt Smelter, lead from lead-based paint,areal lead and arsenic deposition from fuel combustion, and naturally-occurring lead and arsenic.

5. Request for Analyses

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5 Request for AnalysesAll samples will be analyzed for lead and arsenic by U.S. EPA SW-846 Method 6010B. Thissame laboratory will perform a Cam-17 metals analysis by EPA Methods 6010B/7471, if such isrequested. A subset of the STP samples will be analyzed for total cyanide by U.S. EPA SW-846Method 9010/9012.

5.1 Laboratory AnalysisThe U.S. EPA Region IX Laboratory in Richmond, California will provide lead and arsenicanalysis and potential Cam-17 metals analysis, and GEL Laboratories, LLC in Charleston SouthCarolina will provide total cyanide analysis. Sample containers, preservatives, and holdingtimes, and estimated number of initial assessment samples, confirmation samples, and qualitycontrol (QC) samples are summarized in Table 5-1.

To provide analytical quality control for the analytical program, the following measures will beutilized:

■ Additional sample volume will be collected for at least five percent of samples for theanalytical method, to be utilized for matrix spike/matrix spike duplicate (MS/MSD) analysis.

■ Duplicate soil samples will be collected from 10 percent of the sampling locations andsubmitted for soil analysis as “blind” duplicates. A duplicate soil sample will be prepared bycollecting a double-volume of soil into a plastic baggie, homogenizing the contents, and thensplitting the soil between two sample jars.

5. Request for Analyses

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Table 5-1 Assessment Sampling and Analysis SummaryIron King Mine – Humboldt Smelter


Method

Lead and Arsenic by U.S.EPA 6010B or CAM-17

MetalsTotal Cyanide by U.S.

EPA 9010/9012

Sample Container 4 or 8 ounce glass jar 4 or 8 ounce glass jar

Preservation 4C 4C

Analysis Holding Time 6 months* 14 days

Estimated Number of Unique CompositeSamples

35 to 65 None

Estimated Number of Unique DiscreteSamples

63 to 125 4 to 8

Estimated Number of Split Duplicate Samples 6 to 12 1

Minimum Total Site Sample Analyses 104 5

Minimum Total Initial Analyses 104 to 202 5 to 9

Matrix Spike/Matrix Spike Duplicates 1 per 20 samples (1)Submit one 8 ounce glass

jar

1 per 20 samples (1)Submit one 8 ounce glass

jar

Equipment Rinse Blanks (if non-dedicated equipment is used)

Sample Container 500 milliliter plastic bottle 1 L

Preservation HNO3 4C, NaOH to pH >12

Analysis Holding Time 14 days 14 Days

Number of Samples 1 per day (maximum of 5) 1 per day (maximum of 1)

*the holding time for mercury is 28 days


6. Field Methods and Procedures

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6 Field Methods and Procedures

6.1 Field ProceduresThe following sections describe the field procedures and equipment that will be used during thesite activities.

6.1.1 Standard Operating Procedures and EquipmentThe equipment listed below may be utilized to obtain environmental samples from the respectivemedia in accordance with the following sampling standard operating procedures (SOPs) or theirequivalent:

■ Environmental Response Team SOP #2012 Soil Sampling

■ Ecology and Environment Inc. SOP # ENV 3.13: Soil Sampling

■ Ecology and Environment Inc. SOP# ENV 3.15: Sampling Equipment Decontamination

The following is a partial list of equipment that is anticipated to come in contact with samples:

■ Shovels, trowels, scoops

■ Stainless steel buckets or glass containers

■ Dedicated plastic baggies and disposable trowels

6.1.2 Equipment MaintenanceField instrumentation for the collection of soil samples will be operated, calibrated, andmaintained by the sampling team in accordance with the SOPs listed in Section 6.1.1 or theirequivalent. Field instrumentation utilized for health and safety purposes will be operated,calibrated, and maintained by the sampling team according to the manufacturer’s instruction.Calibration and field use data will be recorded in the instrument log books.

6.1.3 Inspection/Acceptance Requirements for Supplies and ConsumablesThere are no project-specific inspection/acceptance criteria for supplies and consumables. It isstandard operating procedure that personnel will not use broken or defective materials; items willnot be used past their expiration date; supplies and consumables will be checked against orderand packing slips to verify the correct items were received; and the supplier will be notified ofany missing or damaged items.

6.1.4 LogbooksField logbooks will document where, when, how, and from whom any vital project informationwas obtained. Logbook entries will be complete and accurate enough to permit reconstruction offield activities. A separate logbook will be maintained for each project. Logbooks are bound withconsecutively numbered pages. Each page will be dated and the time of entry noted in militarytime. All entries will be legible, written in ink, and signed by the individual making the entries.Language will be factual, objective, and free of personal opinions. The following informationwill be recorded, if applicable, during the collection of each sample:


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■ Sample location and description

■ Site sketch showing sample location and measured distances

■ Sampler’s name(s)

■ Date and time of sample collection

■ Type of sample (matrix)

■ Type of sampling equipment used

■ Onsite measurement data (e.g., temperature, pH, conductivity)

■ Field observations and details important to analysis or integrity of samples (rain, odors, etc.)

■ Type(s) of preservation used

■ Field instrument reading (such as dust meter readings for health and safety purposes, etc.)

■ Shipping arrangements (air bill numbers)

■ Receiving laboratory(ies)

Several START team members will be on site performing different duties related to samplecollection, processing, and analysis. If more than one sampling team is used, individual logbookswill be maintained for each sampling team. Each logbook will document the informationrelevant to the site activity, and at a minimum will include:

■ Team members and their responsibilities

■ Time of activities

■ Deviations from sampling plans, site safety plans, and SAP procedures

■ Levels of safety protection

■ Calibration information

■ Analytical data

6.1.5 PhotographsPhotographs will be taken at representative sampling locations and at other areas of interest onsite. They will serve to document field operations. When a photograph is taken, the followinginformation will be written in the logbook or will be recorded in a separate field photographylog:

■ Time, date, location, and, if appropriate, weather conditions

■ Description of the subject photographed

■ Name of person taking the photograph


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6.1.6 Electronic Sample LoggingThe sampling team may utilize field management software to prepare sample labels and chain-of-custody forms.

The following information should be entered for each sample after collection:

■ Sample name

■ Sample date and time

■ Number of sample bottles

■ Type of preservation

■ Analyses

In addition to these items, the software may also be used to keep track of other information suchas sample depth, field measurements, and split samples.

The field team will generate chain-of-custody forms for each cooler of samples packaged andsent to a laboratory. Each chain-of-custody form will refer to the shipping method and trackingnumber. Printed chain-of-custody forms will be submitted to the laboratory with the samples.

The use of field management software will require that the field team have access to a computer,a printer, computer paper, and labels while in the field. Field team members will have receivedspecific training in use of the software.

6.1.7 Mapping EquipmentSample points and site features will be located and documented with a GPS unit. The GPS willbe used to assign precise geographic coordinates to sample locations on the site. GPS mappingwill be done by personnel trained in the use of the equipment and will be completed inaccordance with the manufacturer’s instructions. Expected output from the use of GPS mappingwill be site maps with sample locations and major site features.

6.2 Soil Sampling ProceduresAll sample locations will be recorded in the field logbook as sampling is completed. Each fieldsampling team will document each individual sampling location in a field logbook, which willinclude: the site address, area sample was collected with a quick representative sketch of thearea, photographs taken, date, time, and sampling team members.

6.2.1 Discrete SamplingDiscrete sampling methodology will be employed for “yellow” properties (properties that havenot previously been sampled). Individual samples will be collected at each sampling location.Nine surface samples and one subsurface sample (at a one-foot depth) will be collected fromeach “yellow” property. Each sample will be collected directly into a sample jar, or will becollected into a plastic baggie and transferred to a sample jar.


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6.2.2 Composite SamplingFor “red” properties that have previously been sampled, only certain areas of a particularproperty will require additional sampling. Using historic data and maps, the FOSC willdesignate composite sampling locations (decision units) at these properties. Each compositesampling location will be made up of five sub-samples.

At each sub-sample location within a decision unit, samples will be collected from the exposedsoils at the surface (0-2 inches bgs). The Lead Handbook recommends the collection of surfacesoil samples from a depth of 0-1 inch for human health risk assessment purposes; however, dueto the historical operational time period and the subsequent deposition of soils since that time,and to maintain uniformity with past sampling efforts, samples will be collected from 0-2 inchesbgs.

6.2.3 Surface Soil Collection ProcedureSurface soil samples will be collected from a depth of 0-2 inches bgs. Discrete surface sampleswill be collected from individual sample locations using a disposable plastic scoop or stainlesssteel trowel and will be placed in a plastic baggie, homogenized, and then placed in a sample jar.Composite samples will be prepared from five individual sub-sample points within each decisionunit area location. Approximately 2 ounces of soil will be collected from each sub-samplelocation into a plastic baggie; the soil will be homogenized; and then the homogenized soil willbe placed in a sample jar.

7. Disposal of Investigation-Derived Waste

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7 Disposal of Investigation-DerivedWaste

In the process of collecting environmental samples at this site, several different types ofpotentially-contaminated investigation-derived wastes (IDW) will be generated:

■ Used personal protective equipment (PPE)

■ Disposable sampling equipment

■ Decontamination fluids

■ Extra sample soil remaining in plastic baggies

The U.S. EPA’s National Contingency Plan requires that management of IDW generated duringsite investigations comply with all relevant or appropriate requirements to the extent practicable.This sampling plan will follow the Office of Emergency and Remedial Response Directive9345.3-02 (May 1991), which provides the guidance for management of IDW during siteinvestigations. Listed below are the procedures that will be followed for handling IDW. Theprocedures are flexible enough to allow the site investigation team to use its professionaljudgment on the proper method for the disposal of each type of IDW generated at each samplinglocation.

■ Used PPE and disposable sampling equipment will be double-bagged in plastic trash bagsand disposed of in a municipal refuse dumpster. These wastes are not considered hazardousand can be sent to a municipal landfill. Any PPE or dedicated equipment that is to bedisposed of that can still be reused will be rendered inoperable before disposal.

■ Decontamination fluids will consist of water with residual contaminants and/or non-phosphate detergent. These fluids will be placed on the STP.

■ Extra sample soil remaining in plastic baggies will be placed on the STP.

8. Sample Identification, Documentation, and Shipment

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8 Sample Identification, Documentationand Shipment

8.1 Sample NomenclatureA unique, identifiable name will be assigned to each sample. Samples will have a prefixindicating the property from which they were collected (e.g., OFS-208). The property identifierwill be followed by a sequential number starting with 01 corresponding to the sample numberfrom that particular property. The sample identifier will be followed by a number indicatingdepth (002 represents 2 inches bgs). Composite samples will be indicated by the final suffix –COMP, Grab samples will be indicated by the final suffix – GRAB. Equipment rinsate blanksamples will be designated as Metals-EB-(type of equipment [e.g., trowel])-date.

Field duplicate samples will have the same designations as their originals except the samplenumber will have 100 added to it; thus, the field duplicate of OFS-208-001-002-COMP will beOFS-208-101-002-COMP. A summary of this sample naming system is shown in Table 8-1.

Table 8-1 Sample Numbering SystemIron King Mine – Humboldt Smelter


Type of Sample Site Area Sample IDPrimary Field Sample OFS number>-<sequential number starting with 1>-<depth

in inches>-<composite or aliquot if applicable>Example

Surface soil sample from sample atOFS-208

Decision Unit AreaOFS-208-001-002-GRAB

Field Duplicate All OFS Parcel or NA number>-<sequential number startingwith 1 + 100>-<depth in inches>-<composite or grab if

applicable>2011 ecology & environment, inc.

8.2 Container, Preservation, and Holding Time RequirementsAll sample containers will have been delivered to the START in a pre-cleaned condition.Container, preservation, and holding time requirements are summarized in Table 5-1.

8.3 Sample Labeling, Packaging, and ShippingAll samples collected will be labeled in a clear and precise way for proper identification in thefield and for tracking in the laboratory. Sample labels will be affixed to the sample containersand will contain the following information:

■ Sample number

■ Date and time of collection

8. Sample Identification, Documentation and Shipment

8-2

■ Site name

■ Analytical parameter and method of preservation

Samples will be stored in a secure location on site pending on site analysis and shipment to thelaboratory. Sample coolers will be retained in the custody of site personnel at all times or securedso as to deny access to anyone else.

The procedures for shipping soil samples are:

■ If ice is used then it will be packed in double zip-lock plastic bags.

■ The drain plug of the cooler will be sealed with tape to prevent melting ice from leaking.

■ The bottom of the cooler will be lined with bubble wrap to prevent breakage duringshipment.

■ Screw caps will be checked for tightness.

■ Containers will have custody seals affixed so as to prevent opening of the container withoutbreaking the seal.

■ All glass sample containers will be wrapped in bubble wrap.

■ All containers will be sealed in zip-lock plastic bags.

All samples will be placed in coolers with the appropriate chain-of-custody forms. All forms willbe enclosed in plastic bags and affixed to the underside of the cooler lid. If samples requirerefrigeration during shipment then bags of ice will be placed on top of and around samples.Empty space in the cooler will be filled with bubble wrap or Styrofoam peanuts to preventmovement and breakage during shipment. Each ice chest will be securely taped shut withstrapping tape, and custody seals will be affixed to the front, right, and back of each cooler.

Samples will be shipped for immediate delivery to the contracted laboratory. Upon shipping, thelaboratory will be notified of:

■ Sampling contractor’s name.

■ The name of the site.

■ Shipment date and expected delivery date.

■ Total number of samples, by matrix and the relative level of contamination for each sample(i.e., low, medium, or high).

■ Carrier; air bill number(s), method of shipment (e.g., priority).

■ Irregularities or anticipated problems associated with the samples.

■ Whether additional samples will be sent; whether this is the last shipment.

8.4 Chain-of-Custody Forms and QA/QC Summary FormsA chain-of-custody form will be maintained for all samples to be submitted for analysis, from thetime the sample is collected until its final disposition. Every transfer of custody must be noted

8. Sample Identification, Documentation and Shipment

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and a signature affixed. Corrections on sample paperwork will be made by drawing a single linethrough the mistake and initialing and dating the change. The correct information will be enteredabove, below, or after the mistake. When samples are not under the direct control of theindividual responsible for them, they must be stored in a container sealed with a custody seal.The chain-of-custody form must include the following:

■ Sample identification numbers

■ Identification of sample to be used for MS/MSD purposes

■ Site name

■ Sample date

■ Number and volume of sample containers

■ Required analyses

■ Signature and name of samplers

■ Signature(s) of any individual(s) with control over samples

■ Note(s) indicating special holding times and/or detection limits

The chain-of-custody form will be completed and sent with the samples for each laboratory andeach shipment. Each sample cooler should contain a chain-of-custody form for all sampleswithin the sample cooler.

A QA/QC sample summary form will be completed for each method and each matrix of thesampling event. The sample number for all blanks, reference samples, laboratory QC samples(MS/MSDs), and duplicates will be documented on this form. This form is not sent to thelaboratory. The original form will be sent to the reviewer who is validating and evaluating thedata; a photocopy of the original will be made for the project manager master file.

9. Quality Assurance and Control (QA/QC)

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9 Quality Assurance and Control(QA/QC)

9.1 Field Quality Control SamplesThe QA/QC samples described in the following subsections, which are also listed in Table 5-1,will be collected during this investigation.

9.1.1 Assessment of Field Contamination (Blanks)9.1.1.1 Equipment Blank SamplesIf non-dedicated equipment, such as stainless steel trowels or hand augers, is used to collectsamples, equipment rinsate blanks will be collected at a rate of one per day to evaluate fieldsampling and decontamination procedures.

9.1.1.2 Field BlanksField blanks will not be collected to evaluate whether contaminants have been introduced intothe samples during soil sampling procedures.

9.1.2 Assessment of Sample Variability (Field Duplicate or Co-located Samples)Duplicate soil samples will be collected at selected sample locations. These locations will bechosen randomly in the field based on field observations and will be collected at a rate of 1 forevery 10 field samples. The duplicate of a composite sample will be comprised of an equivalentnumber randomly selected individual sample points from within the same decision unit area.

9.1.3 Laboratory Quality Control (QC) SamplesA laboratory QC sample, also referred to as an MS/MSD, is not an extra sample; rather, it is asample that requires additional QC analyses and therefore may require a larger sample volume.The chain-of-custody records for these samples will identify them as laboratory QC samples. Thelocation of laboratory QC samples will be selected at random. A minimum of one laboratory QCsample will be submitted per 20 samples (or one per delivery group), per matrix, to be analyzedfor each analytical parameter. If the DQIs for analytical parameters are not achieved, further datareview will be conducted to assess the impact on data quality. Laboratory QC samples, includinglaboratory MS/MSD and field duplicate samples, will be selected randomly.

Additional sample volume will be submitted for all lead and arsenic samples designated aslaboratory QC samples and will be designated as MS/MSD samples on the chain-of-custody tothe fixed-base laboratory.

9.1.4 Confirmation SamplesSamples collected under this SAP are not confirmation samples. However, should a removalaction take place at the site in the future, this SAP may be modified in the future to addressconfirmation samples.


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9.1.5 Field Analytical Quality Control (QC) SamplesNo field analytical procedures will be conducted for this site.

9.2 Analytical and Data Package RequirementsIt is required that all samples be analyzed in accordance with the U.S. EPA Method listed inTable 5-1. The laboratory is required to supply documentation to demonstrate that their datameet the requirements specified in the method. A preliminary data summary is expected within20 working days after submission of samples for analysis. A full validation data package will berequired five weeks after submission of samples. The laboratory will also provide all dataelectronically in a Microsoft Excel-compatible format or delimited text file.

Deliverables for this project must meet the guidelines in Laboratory DocumentationRequirements for Data Evaluation (EPA Region IX R9/QA/00.4.1, March 2001). The followingdeliverables are required. Note that the following data requirements are included to specify andemphasize general documentation requirements and are not intended to supersede or changerequirements of each method.

■ A copy of the chain-of-custody, sample log-in records, and a case narrative describing theanalyses and methods used.

■ Analytical data (results) for up to three significant figures for all samples, method blanks,MS/MSD, Laboratory Control Samples (LCS), duplicates, Performance Evaluation samples(if applicable), and field QC samples.

■ QC summary sheets/forms that summarize the following:

MS/MSD/LCS recovery summary

Method/preparation blank summary

Initial and continuing calibration summary (including retention time windows)

Sample holding time and analytical sequence (i.e., extraction and analysis)

Calibration curves and correlation coefficients

Duplicate summary

Detection limit information

■ Analyst bench records describing dilution, sample weight, percent moisture (solids), samplesize, sample extraction and cleanup, final extract volumes, and amount injected.

■ Standard preparation logs, including certificates of analysis for stock standards.

■ Detailed explanation of the quantitation and identification procedure used for specificanalyses, giving examples of calculations from the raw data.

■ The final deliverable report consisting of sequentially numbered pages.

9.3 Data ManagementSamples will be collected and described in a logbook, as discussed in Section 6.1.4. Samples willbe kept secure in the custody of the sampler at all times; the sampler will ensure that all


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preservation parameters are being followed. All samples that are to be sent to the off siteanalytical laboratory will be collected and logged on chain-of-custody forms as discussed inSection 8.4. A START member will only submit samples to the analytical laboratory with chain-of-custody documentation. All submitted samples will be in a properly custody-sealed container.Specifics are discussed in Section 8.3. The laboratories will note any evidence of tampering uponreceipt.

All data summary reports and complete data packages will be archived by the project manager.The data validation reports and laboratory data summary reports will be included in the finalreport to be submitted to the EPA.

9.4 Data ValidationData validation of all data will be performed by the START or their subcontractor in accordancewith U.S. EPA Region IX Superfund Data Evaluation/Validation Guidance R9QA/006.1,December 2001.

The standard data quality review requirements of a Tier 2 validation of 100 percent of the data(as defined in the U.S. EPA document, Requirements for Quality Assurance Project Plans,March 2001) will satisfy the data quality requirements for this project. Upon completion ofvalidation, data will be classified as one of the following: acceptable for use withoutqualifications, acceptable for use with qualifications, or unacceptable for use.

If during or after the evaluation of the project’s analytical data it is found that the data containexcess QA/QC problems or if the data do not meet the DQI goals, then the independent reviewermay determine that additional data evaluation is necessary. Additional evaluation may includeU.S. EPA Region IX Superfund Data Evaluation/Validation Guidance R9QA/006.1 forevaluation Tier 3.

To meet evaluation and project requirements, the following criteria will be evaluated during aTier 2 evaluation:

■ Data package completeness

■ Laboratory QA/QC summaries

■ Holding times

■ Blank contamination

■ Matrix related recoveries

■ Field duplicates

■ Random data checks

■ Preservation and holding times

■ Initial and continuing calibration

■ Blank analyses


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■ Interference check samples

■ Laboratory control samples

■ Duplicate sample analysis

■ Matrix spike sample analyses

■ Sample serial dilution

■ Field duplicate/replicate

■ Overall assessment of data.

Upon completion of evaluation, an analytical data evaluation Tier 2 review report will bedelivered to the project manager, and the data will be classified within the report as one of thefollowing:

■ acceptable for use without qualifications

■ acceptable for use with qualifications

■ unacceptable for use

The data with applicable qualifications will be attached to the report. Unacceptable data may bemore thoroughly examined to determine whether corrective action could mitigate data usability.

9.5 Field VariancesAs conditions in the field may vary, it may become necessary to implement minor modificationsto this plan. When appropriate, the START QA Coordinator and U.S. EPA FOSC will benotified of the modifications and a verbal approval obtained before implementing themodifications. Modifications to the original plan will be recorded in site records and documentedin the final report.

9.6 Assessment of Project Activities9.6.1 Assessment ActivitiesThe following assessment activities will be performed by the START:

■ All project deliverables (SAP, Data Summaries, Data Validation Reports, InvestigationReport) will be peer reviewed prior to submission to the U.S. EPA. In time critical situations,the peer review may be concurrent with the release of a draft document to the U.S. EPA.Errors discovered in the peer review process will be reported by the reviewer to theoriginator of the document, who will be responsible for corrective action.

■ The QA Coordinator will review project documentation (logbooks, chain-of-custody forms,etc.) to ensure the SAP was followed and that sampling activities were adequatelydocumented. The QA Coordinator will document deficiencies, and the PM will beresponsible for corrective actions.


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9.6.2 Project Status Reports to ManagementIt is standard procedure for the START PM to report to the U.S. EPA Task Monitor (TM) anyissues, as they occur, that arise during the course of the project that could affect data quality, datause objectives, the project objectives, or project schedules.

As requested, the START will provide XRF results to the U.S. EPA TM daily and unvalidateddata will be provided as the data are received from the laboratory.

9.6.3 Reconciliation of Data with DQOsAssessment of data quality is an ongoing activity throughout all phases of a project. Thefollowing outlines the methods to be used by the START for evaluating the results obtained fromthe project.

Review of the DQO outputs and the sampling design will be conducted by the START QACoordinator prior to sampling activities. The reviewer will submit comments to the START PMfor action, comment, or clarification. This process will be iterative.

A preliminary data review will be conducted by the START. The purpose of this review is tolook for problems or anomalies in the implementation of the sample collection and analysisprocedures and to examine QC data for information to verify assumptions underlying the DQOsand the SAP. When appropriate to sample design, basic statistical quantities will be calculatedand the data will be graphically represented. When appropriate to the sample design and ifspecifically tasked to do so by the U.S. EPA TM, the START will select a statistical hypothesistest and identify assumptions underlying the test.

10. References)

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10 References

U.S. EPA, 1991. Management of Investigation-Derived Wastes During Site Inspections, Officeof Emergency and Remedial Response, OERR Directive 9345.3-02, May.

U.S. EPA, 2001. Laboratory Documentation Requirements for Data Evaluation (EPA Region IXR9/QA/00.4.1), March.

U.S. EPA, 2001. Requirements for Quality Assurance Project Plans (EPA QA/R 5, EPA/240/B01/003), March.

U.S. EPA, 2002. Guidance on Choosing a Sampling Design for Environmental Data Collection(EPA QA/G 5S, EPA/240/R 02/005), December.

U.S. EPA, 2003. Superfund Lead-Contaminated Residential Sites Handbook (OSWER Directive9285.7-90), August.

U.S. EPA, 2005. Uniform Federal Policy for Implementing Environmental Quality System(EPA/505/F-03/001), March.

U.S. EPA, 2006. Guidance on Systematic Planning Using the Data Quality Objectives Process(EPA/240/B-06/001), February.

U.S. EPA, 2009. Regional Screening Levels for Chemical Contaminants at Superfund Sites,December.

A-1

A Data Quality Objective ProcessDocument

Iron King Mine – Humboldt Smelter Assessment Ecology and Environment, Inc.1

Iron King Mine – Humboldt Smelter Assessment

Data Quality Objectives (DQO) Process DocumentObjective Outputs

Contract: EP-S5-08-01TDD No.: TO2-09-10-09-0004Job No.: 002693.2110.01RA

In September 2010, the United States Environmental Protection Agency (U.S. EPA) Region IX EmergencyResponse Section) tasked Ecology and Environment, Inc.’s (E&E’s) Superfund Technical Assessment andResponse Team (START) to support a U.S. EPA-funded Removal Assessment of the Iron King Mine –Humboldt Smelter Superfund Site (the site), located in Dewey-Humboldt, Arizona. To support the U.S.EPA’s data collection activities, the START has developed these project data quality objectives (DQOs),which will be used to develop the Mojave River Pyrotechnics Assessment Sampling and Analysis Plan(SAP). These DQOs are included as Appendix B of the SAP.

1. THE PROBLEM

Background:Through previous investigations conducted by the U.S. EPA and the Arizona Department ofEnvironmental Quality (ADEQ), lead and arsenic concentrations in surface soil in certain areas of thetown of Dewey-Humboldt are known to exceed Arizona- and U.S. EPA-recommended levels forresidential soil. The lead and arsenic contamination can be attributed to two now-closed businesses: theIron King Mine and the Humboldt Smelter. The town of Dewey-Humboldt is situated between the mineand the smelter.

The latest investigation was conducted by EA Engineering, Science and Technology, Inc. (EA) on behalfof the U.S. EPA, and was documented in a Remedial Investigation Report, Iron King Mine – HumboldtSmelter Superfund Site, Dewey-Humboldt, Yavapai County, Arizona (Revision 01, March 2010) (RIReport). The RI Report combined previous historical data from ADEQ and E&E (the latter on behalf ofthe U.S. EPA) with data collected by EA in 2008 and 2009, in order to provide information for afeasibility study of site remediation options. However, the RI Report concluded, “the full extent ofresidential impacts has not been determined, as many yards have not yet been sampled.” Because somepotentially-impacted parcels had not yet been sampled, and because some already-sampled residentialparcels were found to have elevated concentrations of arsenic and lead in surface soils or are in need ofadditional sampling in order to be fully characterized, the U.S. EPA is performing a Removal Assessmentin the town of Dewey-Humboldt (the site), which is the subject of the SAP.

As discussed in the SAP, the focus of the SAP and the DQOs addressed in this document is a list ofresidential properties in the town of Dewey-Humboldt, which are described in an “Additional ActionRecommended under the Time Critical Removal Action (TCRA)” list (SAP Table 2-1 and SAP Figure 2-2).

Based on the previous data obtained, the contaminants of potential concern at the site are limited to


arsenic and lead concentrations in the surface soil of some residential properties. Total cyanideconcentrations will be investigated at one of the properties that contains a small tailings pile (STP), butthis analyte is only being investigated to corroborate previous results, in case the U.S. EPA determinesthat the STP should be moved.

Conceptual Site Model: The media of concern is surface soil at the site.

The contaminants of potential concern (COPCs) are lead and arsenic. The soil at the site was potentially contaminated with lead and arsenic through activities

historically conducted at the Iron King Mine and the Humboldt Smelter (IKM-HS). The suspected historical release of arsenic and lead from the IKM-HS has resulted in surface soils

that are impacted by these two metals.

Exposure Scenario:

Current Conditions

Due to current site conditions, direct exposure of human and/or environmental receptors to arsenicand lead in surface soils may occur.

Removal Action Conditions The conditions at the site during any future removal action may pose an additional threat to

human health and the environment. Direct exposure of human and/or environmental receptors toarsenic- and lead-contaminated soils is of concern during a removal.

Soils removed from the site may also pose a threat to human health during transportation anddisposal.

Post-Removal While the removal of soil contaminated with arsenic and lead from the site may significantly

reduce the potential for human and/or environmental exposure to these metals, residual arsenicand lead concentrations in site soils could still pose a threat to human health and the environment.

Planning Team:Mr. Craig Benson, U.S. EPA Federal On-Scene Coordinator (FOSC)Mr. Howard Edwards, START Quality Assurance OfficerMr. Michael Schwennesen, START Project ManagerAnalytical Laboratory – U.S. EPA Region 9 Laboratory and START Basic Ordering Agreement (BOA)lab.

The Roles and Responsibilities for this investigation are as follows: Craig Benson, U.S. EPA FOSC, will be the primary decision-maker and will direct the project,

specify tasks, and ensure that the project is proceeding on schedule and within budget. Additionalduties include coordination of all preliminary and final reporting and communication with theSTART Project Manager.

Howard Edwards, START Quality Assurance Officer, will provide quality assurance oversightto ensure that planning and plan implementation are in accordance with U.S. EPA regional qualityassurance/quality control (QA/QC) protocol. He will provide technical direction concerning QA/QCas needed to the U.S. EPA FOSC and the START project manager.

Michael Schwennesen, START Project Manager, will coordinate with the planning team to


develop objectives and complete an approved SAP. The START Project Manager will have theresponsibility for implementation of the SAP, coordination of project tasks, coordination of fieldsampling, project management, and completion of all preliminary and final reporting.

Available Resources:The current START budget for environmental data collection and reporting is $130,500.00, which includesactivities related to the planning, sampling, laboratory analysis, data evaluation, and reporting for the IKM-HS Assessment.

Other Considerations and Constraints Related to Problem and Resources: The scheduling of data collection activities is determined by the U.S. EPA-funded assessment

schedule. Mobilization to the site for assessment activities is scheduled to begin on March 7, 2011.Additional mobilizations may be necessary in order to obtain samples from as many of the sites on

the “Additional Action Recommended under the TCRA” list as possible. Soil analytical results available for assessment are not always useful for determining disposal and

remediation costs. Additional waste testing of excavated soil is usually necessary to determinedisposal requirements.

Additional contamination could be found during a removal if the sample areas are not adequatelydefined during the assessment.

2. THE DECISION

Primary and Secondary Study Questions:

Primary Study Question #1: Will any properties on the “Additional Action Recommended under theTCRA” list have concentrations of arsenic and/or lead that would place them in the top 10% of 95% upperconfidence limits (UCLs) for arsenic and/or lead when compared to all site properties historicallyinvestigated?

Primary Study Question #2: What are the horizontal and vertical boundaries of the STP?

Actions that could Result from Resolution of the Study Questions:

For the Primary Study Question #1:

If it is determined that a property investigated has a 95% UCL for arsenic or lead that is in the top 10%when compared to all properties historically investigated, then the U.S. EPA will consider that propertyto be a potential candidate for a U.S. EPA removal action.

If it is determined that a property investigated does not achieve the top 10% of 95% UCLs for eitherarsenic or lead when compared to all properties historically investigated, then the property will bedropped from the “Additional Action Recommended under the TCRA” list and the property will not bea candidate for a U.S. EPA removal action.

For the Primary Study Question #2:

Sampling at depth on the STP and at locations specified by the FOSC on the perimeter of the STP are


expected to resolve this question.

Decision Statement:

If soil analytical data for arsenic and/or lead at an investigated property are found to have a 95% UCL inthe top 10% when compared to all properties historically assessed, the property will be evaluated by theU.S. EPA for a potential removal action.

3. DECISION INPUTS

Sources of Information Currently Available: Database of historical site property data that includes 95% UCLs for arsenic and lead, as compiled

by EA (see Section 1 of the SAP).

New Environmental Data Required to Resolve the Decision Statements: Definitive analytical data for arsenic and lead concentrations on properties on the “Additional

Action Recommended under the TCRA” list.

Sources of Information to Resolve the Decision Statements: Analytical data from proposed sampling. Global Positioning System (GPS) location data from proposed sampling.

Information Needed to Establish Site Action Level:Not applicable. No specific action levels will be relevant to the investigation described in the SAP.

Measurement Methods:Soil samples collected can be definitively analyzed to determine arsenic and lead concentrations by thefollowing U.S. EPA analytical method:

Total metals by U.S. EPA Method 6010B.

Confirm that Appropriate (Analytical) Methods Exist to Provide the Necessary Data:The indicated definitive method has sufficient sensitivity, accuracy, precision, and other quality parametersto generate data of sufficient quality for this project. See Table 3-1 of the SAP for additional information.

4. DEFINE THE STUDY BOUNDARIES

Specific Characteristics that Define Population Being Studied:

The distribution of arsenic and lead in surface soils within the specified spatial and temporalboundaries.

The concentrations of arsenic and lead in soils within the specified spatial and temporal boundaries.

Spatial Boundaries:

For site properties on the “Additional Action Recommended under the TCRA” list:The horizontal boundaries are the boundaries of each property investigated. The vertical boundaries are a 0to 2-inch depth for “red” sites and a 0 to 1-foot depth for “yellow” sites (see SAP Sections 4.2 and 4.3 for


descriptions of “yellow” and “red”sites).

For the STP:The horizontal boundaries are the boundaries of the STP, which will be defined through sampling. Thevertical boundary will be from the surface to approximately a 5-foot depth (the expected limit of handaugering in tailings material).

Temporal Boundaries:If possible, the sampling should occur between weather extremes, i.e., in the spring or fall. The initialsampling is scheduled for the week of March 7, 2011.

Access agreements must be obtained from the owner of each property to be investigated. Date of samplecollection will be dependent upon receipt of the access agreements.

Practical Constraints on Data Collection:

Physical Constraints:

Sampling at depth in the STP may be constrained by the hand auger sampling method, whichgenerally cannot exceed a depth of approximately five feet, and by the tailings material itself,which may be susceptible to cave-in.

Other Constraints on Data Collection

The turnaround times on data are always estimated and cannot be assured. Sample and systemproblems may indiscriminately increase data turnaround times.

Definitive data will undergo a U.S. EPA Region 9 Tier 2 validation prior to final reporting. Access agreements must be obtained from the owner of each property to be investigated.

5. DECISION RULE

Statistical Parameter:The statistical parameters of interest are the 95% UCLs for arsenic and lead, for each property investigated.

Action Level:There will be no specific action level for the study. Instead of an action level, properties with 95% UCLsin the top 10% (when compared to all properties historically investigated) will be considered for potentialremoval action.

Decision Rule:If soil analytical data for arsenic and/or lead at an investigated property are found to have a 95% UCL inthe top 10% when compared to all properties historically assessed, then the property will be evaluated bythe U.S. EPA for a potential removal action.

If soil analytical data for arsenic and/or lead at an investigated property are not found to have a 95% UCLin the top 10% when compared to all properties historically assessed, then the property will be droppedfrom the “Additional Action Recommended under the TCRA” list and no further action will be taken underthe TCRA.

6. LIMITS ON DECISION ERRORS


Range of the Parameter(s) of Interest:Based on historical data for the site, for all properties to be investigated, the range of concentrations insurface soil that may be expected are:

Arsenic: 7.8 milligrams per kilogram (mg/kg) to 1,980 mg/kg. Lead: 7.6 mg/kg to 18,100 mg/kg.

Baseline Condition (The Null Hypothesis):The data for a property indicates that the 95% UCL for arsenic or lead is not in the top 10% for allproperties (based on historic data) when it actually is (a false negative condition).

Alternative Condition (The Alternative Hypothesis):The data for a property indicates that the 95% UCL for arsenic or lead is in the top 10% for all properties(based on historic data) when it actually is not (a false positive condition).

Decision Error:A discussion of decision error is presented in Table 6-1.


TABLE 6-1 DECISION ERRORSSurface Soil Sampling

Iron King Mine – Humboldt Smelter Assessment

E&E Project No.: 002693.2110.01RA TDD No.: TO2-09-10-09-0004

Decision Error Determining that data for a propertyindicates that the 95% UCL for arsenicor lead is not in the top 10% for allproperties (based on historic data) whenit actually is.

Determining that data for a property indicates thatthe 95% UCL for arsenic or lead is in the top 10%for all properties (based on historic data) when itactually is not.

True Nature ofDecision Error

The sample concentrations are either notrepresentative or are biased low.

The sample concentrations are either notrepresentative or are biased high.

The Consequence ofError

The property would be removed from the“Additional Action Recommended underthe TCRA” list and would not beconsidered for a potential removalaction. This condition could negativelyimpact human health and theenvironment.

Resources of time, money, and manpower could beexpended for a removal that was not necessary.

Which Decision ErrorHas More SevereConsequences Nearthe Screening Level?

MORE SEVERESince the contaminated soil left at thesite may pose risks to human healthand/or the environment.

LESS SEVERETo human health, but with appreciable economicconsequences.

Error TypeBased onConsequences

False Rejection Decisions

A decision that the area is notcontaminated when it is.

False Acceptance Decisions

A decision that the area is contaminated when it isnot.

DefinitionsFalse Acceptance Decisions = A false acceptance decision error occurs when the null hypothesis is not rejected when itis false.False Rejection Decisions = A false rejection decision error occurs when the null hypothesis is rejected when it is true.



7. OPTIMIZED DESIGN FOR OBTAINING DATA

General:All activities and documentation related to the project should proceed under a Quality Management Plan.All sampling, analytical, and quality assurance activities will proceed under a U.S. EPA-approved SAP. Arecord of sampling activities and deviation from the SAP must be documented in a bound field log book.Prior to sample collection, all project sampling personnel will review relevant sampling procedures andrelevant QA/QC requirements for selected analytical methods.

Decision Error Minimization:

Average ConcentrationsIn order to minimize a decision error related to data uncertainty, the decision-maker should considerstatistical evaluations of the data prior to making decisions.

Data from Individual Sample LocationsThe decision-maker should consider data uncertainty when making decisions based upon sampling data andassociated estimated values based upon a single location. For any reported values near the methoddetection limit, the uncertainty of any given value is greater. Thus the probability of decision error isgreatly increased at COPC concentrations near detection limits. The uncertainty for estimated data (i.e.,data based on extrapolations and interpolations) is typically greater than for actual data. Therefore, theprobability of decision errors is greatly increased for extrapolated data.

Due to the nature of the deposition of contamination, it is reasonable to assume that data from anyindividual sample locations on this site can represent a larger area. However, there are insufficient data todetermine the confidence of any single sampling location. Thus the decision-maker should acknowledgethat discrete data points could potentially not be representative of any greater area.

Contamination Distribution MapData from sampling locations can be used to create a contamination distribution map. The mappedcontaminant concentrations indicated within an area should generally be based upon the sample data fromthat area and the sample data from adjacent locations (particularly if discrete sample data are being used).The generated map model could be used to estimate the concentrations of contamination throughout theproperty. The decision-maker should consider the data source and statistical sophistication of thedistribution map prior to making decisions based upon the map.

Search Grid SizeDecision-makers should consider the sizes and probability of missing a contamination hot spot whenevaluating sampling grid data.

Decision Error LimitsThere is a significant amount of historical data regarding site properties. Based on historic data mapswhich generally show an even contaminant distribution, and on the probable mechanism of sitecontamination (which can mainly be attributed to wind deposition), sampling locations can be determinedthat will minimize decision errors.

Specific Design Optimization:Based upon the project’s goals and objectives, the Planning Team considered the following designelements as necessary to achieve the DQOs:


The collection of shallow soil samples for arsenic and lead analysis. Biased judgmental soil sampling at individual properties of concern, selected based on visual

observations. Generation of data that will indicate the geographical distribution of contamination (GPS data).

The objectives of the sampling are to:

Determine whether unacceptable risks to human health are present at the site due toelevated lead and arsenic concentrations in some residential surface soils.

Obtain data for the purposes of potentially performing a removal action. Obtain data to determine the horizontal and vertical extent of the STP.

Judgmental (biased) surface soil sampling (0 to 2 inches below ground surface [bgs]) will be conducted at

properties listed on the “Additional Action Recommended under the TCRA” list. One soil sampleat a 1-foot depth will additionally be collected at properties which have not previously beensampled. Soil samples will also be collected at depth at the STP, using a hand auger. Allsampling locations will be determined in the field by the FOSC. Additional sampling information ispresented in the SAP.

All samples will be placed in coolers and chilled with ice for storage and shipping. Duplicates, equipmentblanks, and other appropriate QA/QC samples will be collected and are specified in the SAP. Data review,independent of the laboratory, will be performed on all analytical data that may be used in decision-making. The GPS coordinates (latitude and longitude) of each sampling location will be determined anddocumented during sampling.

Analysis:All samples will be analyzed for lead and arsenic by U.S. EPA SW-846 Method 6010B at the U.S. EPARegion IX Laboratory in Richmond, California. This same laboratory will perform a Cam-17 metalsanalysis by EPA Methods 6010B/7471, if such is requested. A subset of the STP samples will be analyzedby GEL Laboratories, LLC in Charleston, South Carolina for total cyanide by U.S. EPA SW-846 Method9010/9012.

B-1

B Site Specific Health and Safety Plan

C-1

C Standard Operating Procedures

Documents

Draft Sampling and Analysis Plan Iron King Mine – Humboldt