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REVISED SAMPLING AND ANALYSISPLANCOUNTY ROAD X23 SUPERFUND SITELEE COUNTY, IOWA

Date: February 2003 Project No.: 189834697167

CORPORATE REMEDIATION GROUPAn Alliance between

DuPont and URS Diamond

Barley Mill Plaza, Building 27Wilmington, Delaware 19805

40059862SUPERFUND RECORDS

REVISED SAMPLING AND ANALYSISPLANCOUNTY ROAD X23 SUPERFUND SITELEE COUNTY, IOWA





RECEIVED

FEB 26 20WE'JPERFUND DIVISION

Revised Sampling and Analysis Plan Table of Contents

TABLE OF CONTENTS

1.0 Introduction 1

2.0 Site History 2

3.0 Groundwater Sampling 43.1 Well Sampling 4

3.1.1 Water Level Measurements 43.1.2 Purging Procedures 43.1.3 Analytical Method 43.1.4 QA/QC Samples '. 5

3.2 Health and Safety 53.3 Waste Management 5

4.0 Well Abandonment 6

5.0 Reports 7

6.0 References 8

Table 1

Table 2

Table 3

Figure 1

Figure 2

Figure 3

TABLES

Baier Well Construction Information

Analytical List

McCarl Well Construction Information

FIGURES

Site Location Map

Baier Site

McCarl Site

APPENDICES

Appendix A Field Data Sheet

Appendix B Updated Quality Assurance Project Plan (QAPP)

SAPrevisedFeb Feb. 20, 03Wilmington, DE

Revised Sampling and Analysis Plan . Introduction

1.0 INTRODUCTION

The County Road X23 Superfund site (Baier and McCarl sites), located in Lee County,Iowa, is owned by E. I. DuPont de Nemours and Company (DuPont) (see Figure 1).During the early 1990s, an assessment was conducted to evaluate groundwater quality.As a result, periodic sampling was required to monitor groundwater quality along withcorrective measures. From that time to 2000, groundwater was sampled periodically tomonitor it's quality.

During 2002, a five-year review was conducted by the Environmental Protection Agency(EPA) Region VII to evaluate the corrective measures. The EPA concluded that thecorrective measures were still protective of human health and the environment. As aresult, the following activities were required.

Q Continue biennial groundwater monitoring at the Baier site for total metals.

Q Abandon the monitoring wells at the McCarl site.

The purpose of the report is to replace the Remedial Design Report prepared byWoodward-Clyde Consultants in 1992. This document includes the Sampling andAnalysis Plan (SAP) for the Baier site, the Well Abandonment Plan (WAP) for theMcCarl site and the Revised Quality Assurance Project Plan (QAPP).


Revised Sampling and Analysis Plan Site History

2.0 SITE HISTORY

The Baier and McCarl sites (see Figures 2 and 3) are former disposal areas for paintmanufacturing wastes generated by the DuPont Automotive Products facility in FortMadison, Iowa. The manufacture of paint (i.e. coatings) generates a variety of by-products considered by present-day standards to be of environmental concern. Theseincluded heavy metals, base solutions, and organic compounds including solvents andresins.

DuPont contracted with Mr. Charles Knoch for waste disposal at the Baier site from April1949 to November 1953. Mr. Knoch reportedly transported waste material to the Baiersite for both land disposal and burning.

The McCarl site, which was purchased by Mr. Knoch during the period of waste disposal,was reportedly used between November 1952 and November 1953 for waste disposalwhen muddy roads limited access to the Baier site.

The McCarl site derived its name from the former owners (Ray and Olive McCarl) whoowned the site when it was identified in 1984. DuPont purchased the property in 1986.

During April/May 1990, the remedial investigation (RI) for the site began. Groundwatersamples were collected and analyzed for volatile organic compounds (VOCs) andinorganic compounds. The groundwater data identified several metals of potentialconcern in the shallow water-bearing unit at each site. VOCs were detected infrequentlyin shallow monitoring wells at the Baier site and not detected (ND) in the shallowmonitoring wells at the McCarl site. Monitoring wells screened in the deeper water-bearing zone at each site were not impacted by site-related organic or inorganicconstituents.

A baseline risk assessment (RA) indicated that groundwater contamination posed nothreat to human health because a complete exposure pathway did riot exist. Therefore, the"no action" alternative was selected for groundwater and groundwater action levels werenot required.

A Consent Decree was issued in September 1991. In accordance with that decree,DuPont monitored groundwater at the sites for a five-year period following completion ofthe remedial action. The May 1992 Remedial Design Report-Final Design Submittal,Baier Site and McCarl Site, Lee County', Iowa (RDR), was used as a guidance documentfor the groundwater monitoring events.

The Remedial Action Implementation Report (RAT) (WCC, 1993) described post-remedial action groundwater monitoring activities from September 1992 through June1993. DuPont Environmental Remediation Services (DERS) submitted groundwaterreports for post-remedial action groundwater monitoring activities from 1993 through1998. An additional groundwater sampling event occurred during 2000 with resultspresented in the 2000 Groundwater Monitoring Report.

During 2002, EPA conducted a five-year review of the site. EPA deemed the correctivemeasures were still protective of human health and the environment and recommendedthe following activities for the next five years.

SAPrevisedFeb Feb. 20, 03 2Wilmington, DE

Revised Sampling and Analysis Plan • Site History

Q Biennial groundwater sampling at the Baier site for total rnetals. The years wouldbe 2002, 2004, and 2006.

Q Abandonment of the monitoring wells at the McCarl site.


Revised Sampling and Analysis Plan Ground Water Sampling

3.0 GROUNDWATER SAMPLING

As per the five-year review, the monitoring wells at the Baier site will be sampled on abiennial basis for a total of three sampling events (2002, 2004, and 2006). Table 1presents the well information.

3.1 Well Sampling

3.1.1 Water Level Measurements

Prior to any purging or sampling activities, a full round of water levels will be collectedfrom all wells to determine the static water level. All measurements will be recorded onthe Field Data Sheet (see Appendix A).

3.1.2 Purging Procedures

Each well has a dedicated bladder pump placed in each well with the pump intake atapproximately the level of mid-screen or slightly above. Prior to collection of thesamples for analysis, all wells will be purged using a low-flow (minimum drawdown)protocol with purge rates ranging from less than 0.1 L/minute to 0.5 L/minute. The lowflow bladder pump with dedicated tubing will be used to evacuate the groundwater fromthe screen area of the well. Purge water will be managed in accordance with the sitespecific WMP, which will be developed and approved prior to the start of field activities.

The water quality parameters (pH, specific conductivity, dissolved oxygen, andtemperature) will be monitored using a flow-through cell. Purging will be considered tobe complete and formation water accessed when all field measurements have stabilized.Stabilization will be considered achieved when three consecutive readings, taken at 3-5minute intervals are within the following limits:

Q DO (10%)

Q Specific Conductance (3%)

Q Temperature (3%)

Q pH (=0.1 unit)

3.1.3 Analytical Method

All samples will be submitted for analysis of total metals under the Contract LaboratoryProgram (CLP) Statement of Work (SOW) ILMO 5.0. Table 2 lists the specific analytes.

Lancaster Laboratories, Inc. (LLI) of Lancaster, Pennsylvania will conduct all laboratoryanalyses. The updated QAPP can be found in Appendix B for more detail about theAnalytical Method.


Revised Sampling and Analysis Plan GfOUndwater Sampling

3.1.4 QA/QC Samples

To ensure appropriate QA/QC has been followed, one field duplicate sample will becollected. This sample will be used to evaluate analytical precision. Appendix B has anupdated QAPP that gives more detail about QA/QC samples.

3.2 Health and Safety

All field activities will occur as specified in the site specific Health and Safety Plan(HASP).

3.3 Waste Management

All field activities will occur as specified in the site specific Waste Management Plan(WMP). As was done in the past, all purge water will be discharged to the ground. AllPPE will be containerized in plastic bags, transported to the DuPont Fort Madison plant,and disposed with the facility's trash.

SAP Apr. 22, 03Wilmington, DE

Revised Sampling and Analysis Plan Well Abandonment

4.0 WELL ABANDONMENTSeven existing monitoring wells (see Table 3) at the McCarl site will be abandoned inaccordance with Iowa State and Federal Regulations. The Contractor will prepare andsubmit all required well abandonment permits and provide a copy of each to DuPont.The wells range from 40 to 120 feet deep from top of casing (which are above ground)and are constructed out of 2" PVC. Well abandonment will include tremie grouting ofthe well casing from the base of the well to the ground surface using cement bentonitegrout. After the bentonite grout has set for 24 hours, the upper portion of the well casingwill be removed to 2 feet below ground surface. The remaining open hole will be filledwith clean fill.


Revised Sampling and Analysis Plan

5.0 REPORTS

A summary report will be prepared and submitted to EPA Region VII after each samplingevent. The report will, at a minimum, include the following information.

Q Description of sampling activities

Q Tables presenting analytical and field data from the sampling event along withhistorical data

Q Figures/map presenting data (as appropriate)

Q Copy of the analytical report plus CLP package

The report will be submitted to EPA Region VII approximately 60 days followingDuPont's receipt of the analytical data.


Revised Sampling and Analysis Plan ReferGHCGS

6.0 REFERENCESWoodward-Clyde Consultants. 1992. Remedial Design Report. County Road X23

Superfund site, Lee County, Iowa.


TABLES

Table 1Baier Site: Well Information

Well

BRA-1SBRA-1DBRA-2SBRA-2DBRA-3SBRA-3DBRA-4SBRA-4DBRA-5S

TOC(ft)

707.66707.90708.11708.20705.61705.85705.20692.77694.59

WellDepth (ft)

5913766130581365813347

WellDiameter

(inch)222422222

Pump

BladderBladderBladderBladderBladderBladderBladderBladderBladder

2000DTW(ft)

27.1892.838.3297.3951.7

114.0938.8876.6928.32

Edited: 9/23/02 Tables / Table 1

Table 2Analytical List

AluminumAntimonyArsenicBarium

BaryltiumCadmiumCalcium

ChromiumCobaltCopper

IronLead

MagnesiumManganese

MercuryNickel

potassiumSelenium

SilverSodiumThalliumVanadium

Zinc


Table 3McCarl Site: Well Information

Well

MRA-1SMRA-1DMRA-2SMRA-2DMRA-3SMRA-3DMRA-4S

ScreenedInterval (ft)

36 to 46111 to 12131 to 41

111 to 12148 to 5898 to 10829 to 39

WellDepth (ft)

46121411215810839

Diameter(inch)

2222222

ApproximateDTW (ft)

17.7576.1419.4974.5051.0359.257.00


FIGURES

SOURCE: USGS QUADRANGLE: WEST POINT (1964)

Corporate Rwmolatlon GroupAnAlHano*

DuPont and USS Momond

Barley Mill Plaza, Building 27Wilmington, Delaware 1980S

SITE LOCATION MAP

COUNTY ROAD X23

LEE COUNTY. IOWA

Corporal* Remediation GroupMum

DMfmt vid 1019 Ptanwnd

Barley Mill Plaza. Building 27Wilmington. Ddowora 19B05

MONITORING WELLLOCATION MAP

DuPONT BAIER SITELEE COUNTY, IOWA

ft

MRA-1S

MRA-1D

Shallow Monitoring Well

Deep Monitoring Well

0 30 60

^=FEET

Corporate Remediation GroupAUtoand

Barley MM Plaza, Building 27Wilmington. Driawar* 19805

MONITORING WELLLOCATION MAP

DuPONT McCARL SITELEE COUNTY, IOWA

K.P. JOMBOH

OM. ENCUSM

APPENDICES

APPENDIX A

Corporate Remediation Group - Field Book

Personnel;WPH in-

Weather Conditions:^

Well Depth:Depth to Water:Water Column:Well Vol:Well Vol (3x):

Project Manager?

Permit Nn: VO Vannrs? pmiPin m-

Clear D Cloudy E

LNAPL:DNAPL:Casing Dia:Conv. Factor:Purge Rate:

PIDIFID CA:.

Other LJ Wind: LJ

Purge Method:Purge Start:Purge Stop:Parameter CollecticWater Level Stable

Temp: ?F

in Time'@:

Parameters

PH

Temperature (?C)Specific Conductance (umho)

Dissolved Oxygen (rng/1)

Redox (mV)

Turbidity (ntu)

Color

Odor

Sample Analysis Time

Sample Date: Sample Collection Time: Sample Method:

Analysis

\nalyst Nam

\nalyst Signs

Volume (ml) # Preservative Zero HS Comments:

f>;

iture: Date: 00850

APPENDIX B

QUALITY ASSURANCE PROJECT PLANGROUNDWATER MONITORINGFOR DUPONT BAIER SITE COUNTYROAD X-23 SUPERFUND SITEFORT MADISON, IOWA




. Barley Mill Plaza, Building 27Wilmington, Delaware 19805

Quality Assurance Project Plan Groundwater Monitoring Table Of Contents

TABLE OF CONTENTS

1.0 Project Description 1

2.0 Project Organization and Responsibility 12.1 Project Manager 22.2 Project Chemist 22.3 Project Field Manager 22.4 Laboratory Personnel 2

3.0 Quality Assurance Objectives For Measurement 43.1 Data Quality Characteristics 43.2 Sampling Quality Objectives 53.3 Laboratory Quality Objectives 5

4.0 Preliminary Field Activities 64.1 Planning 64.2 Field Maintenance 64.3 Field Documentation 74.4 Calibration of Field Instrumentation 74.5 Decontamination Procedure 74.6 Equipment List 8

5.0 Sampling Procedures 95.1 Sample Locations, Types, and Parameters 95.2 Sample Containers 9

5.2.1 Sample Labels 95.3 Sample Preservation 9

5.3.1 Chain-of-Custody Forms 10

6.0 Sample Custody 116.1 Sample Labels and Security Seals 116.2 Field Notebook 116.3 Chain-of-Custody Record 116.4 Laboratory Receipt 12

7.0 Analytical Procedures , 137.1 Laboratory Analytical Methods 137.2 Laboratory Quality Control 137.3 Reporting Limits 13

8.0 Data Reduction, Review, and Reporting 148.1 Data Reduction 148.2 Quality Control Review 148.3 Data Reporting 14

QAPP Feb. 20, 03Wilmington, DE

Quality Assurance Project Plan Groundwater Monitoring Table of Contents

9.0 Quality Control Checks 159.1 Field Quality Control 15

9.1.1 Field Performance Audit 159.1.2 Field System Audit 16

10.0 Assessing Data Quality Characteristics 1810.1 Representativeness 1810.2 Comparability 1810.3 Precision 1910.4 Accuracy 1910.5 Completeness 20

11.0 Corrective Action 21

12.0 Quality Assurance Reports To Management 22

13.0 Document Control 23

TABLES

Table 1 Quality Control Acceptance Limits for Metals Analysis

Table 2 Monitoring Wells

Table 3 Analytical Method Requirements, and Frequency of Field-Collected QCSamples

Table 4 CLP ILM05.2 Contract Required Quantitation Limits (CRQL) for TALMetals in Water

APPENDICES

Appendix A US EPA, Office of Emergency and Remedial Response. Multi-Media,Multi Concentration, Inorganic Analytical Service for Superfund(ILM05.2). EPA Publication 540-f-02-008, October 2002

Appendix B Standard Operating Procedure for Completing Chain-of-Custody Forms


Quality Assurance Project Plan Groundwater Monitoring Table of Contents

I have reviewed this document and attest that it accurately presents the quality assuranceplan in place to ensure data quality objectives for the following investigation are met:

Groundwater MonitoringFor

DuPont Baier SiteCounty Road X-23 Superfund Site,

Fort Madison, Iowa.

. Johnson, Project Manager

Barbara Rhodes, Projecl~€hemist >jeo?Field Manager

Diana Engeman, ERA Remedial Project Manager

QAPP Feb. 20. 03Wilmington, DE

iii

Quality Assurance Project Plan Groundwater Monitoring Project Description

1.0 PROJECT DESCRIPTION

This quality assurance project plan (QAPP) describes measures in place to ensure theconsistent, high quality of data collected to monitor total metals in ground-water sampledbiennially at the DuPont Baier Site. This QAPP describes the project quality assurance(QA) rationale, procedures for sampling handling and tracking, required laboratoryanalyses, quality control (QC), data reporting, and data assessment for the project—all ofwhich are designed to ensure the data quality goals of the sampling program are met.This document supplements the Sampling and Analysis Plan (October 2002) for thiswork, which fully describes the project scope and rationale and site history. Guidance forpreparation of this QAPP was derived from the US EPA document, Guidance for QualityAssurance Project Plans, EPA QA/G5 (EPA/240/R-02/009; December 2002).


Quality Assurance Project Plan Groundwater Monitoring Project Organization and Responsibility

2.0 PROJECT ORGANIZATION AND RESPONSIBILITY

DuPont Engineering's Corporate Remediation Group has contracted with URS Diamond(URSD) of Wilmington, Delaware to conduct the sampling and analytical program.URSD will conduct laboratory service coordination and data quality review. LancasterLaboratories, Inc. of Lancaster, Pennsylvania will conduct laboratory analytical testing.

2.1 Project Director

Hilton Frey, DuPont Engineering, is the project director. Project director responsibilitiesinclude project concept and funding approval, project review, and regulatory liaison.

2.2 Project Manager

Kimberly P. Johnson, URSD, is the project manager. Management responsibilitiesinclude project implementation and staffing; ensuring timely communication of projectinformation (policies, procedures, timetable, etc.) to the project team; sampling eventplanning; final data review to ensure safety, quality, and regulatory requirements are met;design and implementation of any corrective measures warranted; and preparation ofproject reports.

2.3 Project Chemist

Barbara C. Rhodes, URSD, is the project chemist. Project chemist responsibilitiesinclude coordination of laboratory services, collection of all hardcopy and electronicanalytical data reports, and data quality assurance review.

2.4 Project Field Manager

Timothy Ratsep, URSD, is the field manager for this project. In addition to ensuringsafety and completion of the sample collection, the field manager is responsible forensuring adherence to appropriate field QA and documentation procedures; notifying theproject chemist/laboratory of conditions that require change in anticipated sample arrivalor condition; and ensuring sample shipments meet applicable United States Departmentof Transportation (USDOT) regulations.

2.5 Laboratory Personnel

Lancaster Laboratories Inc. (Lancaster) will conduct all sample analysis for this project.The laboratory project manager is the key laboratory personnel for this project. Theanalytical laboratory project manager will be responsible for execution of the analyticaltesting program for the project. The laboratory project manager is responsible forensuring that laboratory analyses are conducted as specified in the analytical protocol andthat laboratory internal QA procedures are followed, and for reporting analytical resultsto URSD. The laboratory project manager will be the point of contact for the projectchemist.

QAPP Feb. 20, 03 2Wilmington, DE

Quality Assurance Project Plan Groundwater Monitoring Project Organization and Responsibility

Lancaster has signed a contract with DuPont detailing the terms and conditions forservices. Disposal of unused sample volumes, sample extracts, and sample digestateswill be in accordance with the laboratory's waste management procedures.


Quality Assurance Project Plan Groundwater MonitoringQualJty Assurance Objectives For Measurement

3.0 QUALITY ASSURANCE OBJECTIVES FORMEASUREMENT

To ensure that the groundwater monitoring data generated are of high and consistentquality for the stated purpose, data quality objectives (DQOs) in terms of precision,accuracy, representativeness, comparability and completeness have been established.Sampling, analysis, and associated QA efforts are designed to achieve these objectives ina safe, timely, and cost-effective manner. Since samples will be analyzed under contractlaboratory program (CLP), many of these quality assurance objectives are predifined.

DQOs are statements of the level of uncertainty that a decision-maker is willing to acceptin results derived from environmental measurements. Uncertainty in analytical resultsmay arise from a combination of factors, including sampling procedures, sample matrixcharacteristics, non-homogeneity of samples, and the inherent accuracy and precisionlimitations of analysis methods.

3.1 Data Quality Characteristics

DQOs are quantitatively and qualitatively described in terms of data qualitycharacteristics that include precision, accuracy, representativeness, completeness, andcomparability (see Section 10). These characteristics are defined as follows:

Q Accuracy

• Accuracy is the degree of agreement of a measurement with an accepted truevalue.

Q Precision

• Precision is defined as the agreement between numeric values for two or moremeasurements that have been obtained in an identical fashion.

Q Completeness

• Completeness is a measure of the amount of the valid data obtained from themeasurement system compared to the amount that was expected under normalconditions.

Q Representativeness

• Representativeness expresses the degree to which sample data accurately andprecisely represents a selected characteristic of a population, parametervariations at the sampling point, a process condition, or an environmentalcondition.

Q Comparability

• Comparability expresses consistency in sampling and analytical procedures sothat one data set can be compared to another.

Accuracy and precision acceptance criteria required for this project are listed in Table 1.All measurement data will be calculated and reported in units consistent with specifiedmethodologies to ensure comparability of historical data. The use throughout the program


Quality Assurance Project Plan GroundwaterMonitoringQualJty Assurance Objectives For Measurement

of the EPA document SW-846 sampling and analytical methods will ensurerepresentative and comparable results of known accuracy and precision.

3.2 Sampling Quality Objectives

All sampling events will follow the guidelines described in the Sampling and AnalysisPlan to provide common ground for data comparison.

3.3 Laboratory Quality Objectives

Laboratory quality objectives (LQOs), as dictated by the CLP, are designed to ensureanalytical results of known and documented quality, and CLP-participating laboratoriesare subject to comprehensive evaluation of performance. Specific laboratory QCprocedures for analyses can be found in the EPA documents describing CLP analyticalmethodologies, including Multi-Media, Multi-Concentration, Inorganic AnalyticalService for Superfund (ILM05.2) (EPA Publication 540-F-02-008, October 2002) (seeAppendix A).

CLP methodologies require the use of instrument performance checks, laboratory controlsamples, method blanks, duplicate samples, calibration checks, and matrix spike samples,etc. for the evaluation of the laboratory's analytical precision and accuracy duringanalysis. The frequency and application of QC sample analysis are further defined in therespective methods.


Quality Assurance Project Plan Groundwater Monitoring Preliminary Field Activities

4.0 PRELIMINARY FIELD ACTIVITIES

4.1 Planning

At a minimum, the sampling personnel will review the following checklist prior to thesampling event:

Q Coordinate with project chemist or laboratory staff to ensure that sample arrival isproperly anticipated (especially if weekend delivery will occur).

Q Determine that all appropriate forms and logbooks are available for use during thesampling event.

Q Establish accountability and responsibility for each activity to be conducted bythe sampling team personnel.

Q Conduct a preliminary inspection, inventory, and cleaning of all field equipment.Ensure that preventive maintenance is up-to-date. Calibrate and recheck all fieldanalytical instrumentation.

Q Review the Sampling and Analysis Plan to ensure that each individual is aware ofthe protocols and required procedures. Ensure personnel are familiar with properpump operation and sample collection procedure.

Q Review the Health and Safety Plan (HASP) for health and safety requirements.Determine what level of personal protective clothing and equipment will beneeded for each location. Review procedures for decontamination of protectiveequipment and use and removal of respiratory and personal protective clothing toavoid personal exposure to potentially hazardous sample materials. Reviewemergency escape and medical emergency procedures.

4.2 Field Maintenance

Preventive maintenance of field equipment is essential to obtaining accurate data.Unnecessary resampling and analysis can also be avoided if equipment is wellmaintained.

A calibration and maintenance checklist for each piece of equipment used on-site will beavailable to the field sampling team. The field sampling team is ultimately responsiblefor ensuring that field equipment is cleaned and maintained according to proceduresdetailed by the manufacturer. Complete manufacturers' instructions for calibration andmaintenance are found with each piece of equipment. The field equipment will beserviced when routine daily inspections indicate the need for maintenance.

Routine maintenance of field equipment includes the following:

Q Removing surface dirt and debris

Q Ensuring proper storage of equipment

Q Inspecting equipment prior to use



Q Calibrating equipment according to Section 6.0

Q Charging battery packs when not in use

Q Maintaining spare and replacement parts in the field to minimize downtime

The following is a representative list of spare parts for this program:

Q Batteries, as required, for all equipment used

Q Health and safety equipment (e.g., gloves, filters, boots, Tyvek® clothing)

Q Flagging tape and sample location stakes

Q Calibration solutions and gases

In the event that a piece of equipment requires repair, a list of manufacturers' addresses,phone numbers, and contact persons will be kept on-site.

4.3 Field Documentation

The field manager is responsible for maintaining the field notebook. The notebook willprovide a daily record of significant events, observations, and measurements during fieldinvestigations. The notebooks must be bound and waterproof, with each page numberedand completed in waterproof ink. Each page will be signed by the user and dated. Allmembers of the field sampling team will have access to the field notebook. The notebookwill be maintained as a permanent records and will remain the property of DuPont and/orthe DuPont appointed agent.

Field notebooks are intended to provide sufficient data and observations to reconstructevents that occurred during sampling events and to refresh the memories of samplingteam members if required to give testimony during legal proceedings. In legalproceedings, notes, if referred to, are subject to cross-examination and may be admissibleas evidence. The field notebook entries must be legible, factual, detailed, and objective.Field personnel may make corrections by lining out errors, initialing and dating theerrors, and entering correct information.

4.4 Calibration of Field Instrumentation

Calibration of equipment will occur daily prior to its use in the field. The field manageris responsible for ensuring adherence to the calibration schedule and each operator'sunderstanding of the proper usage, maintenance, and storage of each instrument.Calibration information will be recorded in the field notebook, and will include the dateand time of calibration and the calibration measurements. All field measurementequipment will be calibrated according to manufacturers' guidelines.

4.5 Decontamination Procedure

For field equipment and instruments/probes used for multiple sample locations, thedecontamination procedure follows:

Q Wash with laboratory grade detergent, such as alconox.



Q Rinse with potable water.

Q Rinse again with deionized water.

Q Allow to air dry.

4.6 Equipment List

The minimum equipment for this activity is as follows:

Q Decontamination supplies (i.e., Alconox®, sponges, brushes, spray can ofdeionized water, and buckets)

Q Personal protective equipment (i.e., disposable gloves, coveralls, and steel-toedboots)

Q Sample containers, preservative, and COC documentation

Q Field logbooks

Q Office supplies (e.g., pens, calculator, paper, and watch)

Q Field instruments for water level and water quality measurements

Q Plastic bags (e.g., waste disposal and decontamination uses), paper towels

Q Miscellaneous tools


Quality Assurance Project Plan Groundwater Monitoring Sampling Procedures

5.0 SAMPLING PROCEDURES

Groundwater monitoring wells at the DuPont Baier Site will be sampled and analyzedbienially over the period 2002-2006, as required by EPA's five-year Review of the site.The work described in the project's Sampling and Analysis Plan will adhere to theQA/QC policies and procedures outlined in this QAPP.

5.1 Sample Locations, Types, and Parameters

Nine monitoring wells, identified in Table 2, will be sampled once every two years andanalyzed for all 23 Target Analyte List (TAL) metals, using the CLP protocol. Wellsampling procedures to be used in this project are described in Section 3.0 in theSampling and Analysis Plan. These procedures include specific instructions for takingwater level and quality measurements and for low-flow well purging prior to samplecollection.

The Baier Groundwater Monitoring field program will have a bound notebook wherefield data corresponding to each individual sample will be recorded. This field data willlater be entered into the DuPont Corporate Environmental Database (CED), if necessary,for reporting purposes.

Each monitoring well is equipped with a dedicated bladder pump and tubing, thusminimizing the possibility of sample cross contamination via collection equipment.

5.2 Sample Containers

Only new sample containers will be used for sample collection. The laboratory willprovide containers of appropriate number, size and type, with the required preservativefor use in sample collection. The laboratory will analyze all samples within the method-defined holding times, as specified in Table 3.

5.2.1 Sample Labels

Sample labels, bottles, and chain-of-custody (COC) forms will be provided by Lancaster.COC forms, labels, and bottles will be preprinted as much as practicable and will bedelivered at least a day prior to sampling to allow samplers a final check before collectionbegins.

5.3 Sample Preservation

Field samples and QC samples will be collected and placed in sample containers thathave been laboratory prepared with the appropriate preservative, as specified in Table 3.

Each collected sample will be labeled and placed as soon as possible into a sample cooleror shuttle. The cooler will serve as a shipping container and will have been provided bythe laboratory, along with the appropriate sample containers. Since temperature


Quality Assurance Project Plan Groundwater Monitoring Sampling PrOCGdureS

preservation is not required for metals analysis, the chest may or may not be packed withwet ice. Laboratory personnel will include a temperature blank in each cooler.

Reagents used on-site will be provided by the laboratory and will be of sufficient purityto yield blank results at levels below the practical quantitation limit for each parameter.Preservation techniques will be documented on the COC records. Samples will betransported to the laboratory promptly using a delivery service as prearranged with thelaboratory. The project field manager is responsible for ensuring compliance withcurrent United States Department of Transportation regulations concerning the shipmentof environmental samples to a laboratory for analysis.

5.3.1 Chain-of-Custody Forms

The COC records will document samplers and handlers, as well as collection date andtime, container types and numbers, and preservation techniques for each sample. SeeAppendix B for instructions for completing a COC.


Quality Assurance Project Plan Groundwater Monitoring SamplG Custody

6.0 SAMPLE CUSTODY

The sample custody procedures outlined in this section ensure the tracing of possessionand handling of individual samples from the time of field collection through laboratoryanalysis.

6.1 Sample Labels and Security Seals

Each sample container will have a sample label affixed to the outside of the container inan obvious location. The label will specify the sample identification number, locationsampled, preservatives used, and. parameters to be analyzed.

Samples shipped from the facility to the laboratory by a commercial courier will betransported in an insulated shipping container and closed with a custody seal. Iflaboratory personnel receive a cooler with a broken custody seal, that fact will berecorded on the COC form, and the project chemist will be notified.

6.2 Field Notebook

The field sampler will complete the appropriate field documentation in the field notebook(see Section 4.3) for each sample location, noting the following information as required:

Q Sample identification number

Q Sample type, location, date, and time

Q Personnel present

Q Depth of sample

Q Weather conditions

Q Sample appearance (e.g., color, odor, texture)

Q Comments and observations at time of sample withdrawal

Q Signature and date at bottom of notebook page

6.3 Chain-of-Custody Record

The COC, preprinted as much as practicable, will be initiated at the laboratory andaccompany the sample containers shipped to the field. Blank COCs will be included, inthe event extra samples are collected.

Each sample may consist of several individual sample aliquots contained in separatesample containers. Each sample container will be logged on the COC form prior toreturn shipment to the laboratory. The COC must accompany corresponding samplesthroughout handling and shipment.

The following information will be recorded on the COC form:

Q Sample source, location (e.g., monitoring well, stream)


Quality Assurance Project Plan Groundwater Monitoring Sample Custody

Q Collector's name

Q Dates and times of sample collection

Q Sample identification numbers

Q Number of containers for each sample aliquot

Q Container size, type

Q Type of preservation

Q Parameters (analytes from each sample aliquot),

Q Rush analyses (if requested)

Q Special handling instructions (if applicable)

Q Laboratory name

Q Name, date, time, and signature of each individual possessing the samples

Q Condition of shipping container custody seal, used only if transported bycommercial courier; item is recorded by laboratory personnel

The DuPont Corporate Remediation Group's SOP for Completing Chain of CustodyForms is attached as Appendix B of this QAPP.

The field manager or designate will be responsible for custody of samples collected duringthe field investigation. Custody of the samples will be defined as actual physicalpossession, in view after physical possession, or locked and/or sealed in a tamper-resistant container after physical possession.

6.4 Laboratory Receipt

Following procedures mandated in laboratory Standard Operating Procedures (SOPs), theLaboratory QAPP, and the CLP, Laboratory Sample Administration and Sample Storage(SA/SS) Department personnel will inspect and verify correctness of COC records uponsample receipt. They will verify that all samples are accounted for and that custody sealsremain intact. SA/SS personnel will document sample condition, sign the COC, andimmediately notify the laboratory project manager of any discrepancies or problems withsample integrity.

Sample handling and analysis will proceed as dictated by the CLP protocol.

QAPP Feb. 20,03 12Wilmington, DE

Quality Assurance Project Plan Groundwater Monitoring Analytical PrOCGdUTGS

7.0 ANALYTICAL PROCEDURES

DuPont has retained Lancaster to conduct the analytical services for the project thoughother qualified, CLP-participating laboratories may.be used .

The analytical program presented in this document describes the procedures that DuPont,its contractors, and its laboratories will use during implementation of the project. Thelaboratories will follow the QA/QC procedures listed in the methods referenced in thisQAPP.

7.1 Laboratory Analytical Methods

Groundwater samples collected during this project will be analyzed for TAL metals (seeTable 4) using CLP ILM05.2 methodologies.

7.2 Laboratory Quality Control

Equipment calibration documentation, equipment decontamination documentation, androutine preparation of various QA/QC samples will monitor the quality and integrity ofsamples collected and analyzed during the investigation. Laboratory personnel willprepare and analyze the QA/QC (i.e., method blanks, laboratory control samples) asspecified in the CLP analytical methods (see Table 4 for QA/QC samples evaluated inQC review; see complete list of CLP-required QC in Appendix A).

7.3 Reporting Limits

Quantitative reporting limits are sample dependent and may vary as the sample matrixvaries. Factors influencing the reporting limits include the actual method used, samplematrix, interference, and high concentrations of analytes. The target reporting limitspresented in Table 4 of this QAPP are those listed in the CLP as contract requiredquantitation limits (CRQL). Actual PQLs may vary from sample to sample in accordancewith standard laboratory practices (e.g., dilution resulting from high analyteconcentration).


Quality Assurance Project Plan Groundwater Monitoring Data Reduction, ReVJGW, and Reporting

8.0 DATA REDUCTION, REVIEW, AND REPORTING

8.1 Data Reduction

Data reduction is the process of generating qualitative and quantitative sampleinformation through observations, field procedures, analytical measurements, andcalculations.

Data reduction occurs in the following:

Q The Sampling and Analysis Plan through sample locations and namingconventions

Q The field sampling process through use of field notebooks and fieldmeasurements

Q Communications with the laboratory in sample analysis requests

Q Field operations with collection, preservation, and COC documentation

Q Laboratory operations with sample receipt and handling, sample preparation andanalysis, collation of raw data, and generation of laboratory results

Q Post-laboratory operations, with collation of analytical results in a format suitablefor documents such as reports, maps, and trend plots

Specific QC measures developed to ensure accuracy throughout the data reductionprocess are described in Section 10.

8.2 Quality Control Review

The project chemist is responsible for reviewing the analytical data generated by thelaboratory to determine if the DQOs stated in Section 3.1 were met. In addition toevaluating the data relative to accuracy, precision, completeness, and representativeness(see Section 10 for evaluative procedure), the project chemist will ensure correspondencebetween field and laboratory sample records, and consistency between the laboratory'spaper and electronic analysis reports.

8.3 Data Reporting

Significant figure conventions given in EPA document SW-846 or the Handbook forAnalytical Quality Control in Water and Wastewater Laboratories, (EPA-600/4-79-019,March 1979) will be followed. Reported concentrations will not be corrected forcontaminants found in associated method, equipment, and field blanks.

QAPP Feb. 20,03 14Wilmington, DE

Quality Assurance Project Plan Groundwater Monitoring Quality Control Checks

9.0 QUALITY CONTROL CHECKS

Laboratory QA/QC checks are dictated and audited as elements of the CLP. Therefore,this QAPP describes only quality control measures in place to ensure integrity of samplecollection procedures.

QC is an integrated system of activities in the area of quality planning, qualityassessment, and quality improvement designed to give measurable assurance that therequired standards of quality are met. The QC checks described in this documentgenerally fall into several categories: field practices, system and performance audits,corrective action, and QA reports. The interrelation of these QC checks is describedbelow.

9.1 Field Quality Control

The quality and integrity of samples collected at the facility will be monitored by routinepreparation of various QC blanks, equipment calibration documentation, and equipmentdecontamination documentation. Table 3 summarizes the frequency of QC samplecollection. The field manager is responsible for ensuring that all field quality controlsamples are properly collected, labeled, and shipped in the appropriate shippingcontainers.

Since all groundwater samples will be collected using dedicated equipment, equipmentblanks will not be needed. Field blanks will be prepared by transferring laboratory-provided blank water to sample containers and handling as other field samples. Fieldblanks will be analyzed for the same parameters as other samples collected during thesampling event

Field duplicate samples will be collected at a frequency of one duplicate for every20 (non-QA/QC) samples. Duplicate samples will be collected in the same manner asroutine monitoring samples. The sample will be analyzed for the same parameters as theoriginal sample, and the analytical results will be compared with those of the originalsample. The analytical results of the original sample and the duplicate sample should beused to evaluate the cumulative precision because of the limitations of the analyticalmethod, sample matrix, and sample collection techniques.

The analytical results for these QC samples become the quantitative focus of the fieldperformance audits.

9.1.1 Field Performance Audit

Performance audits are characterized by a quantitative check for accuracy in fieldmeasurements, field QC sample results, and field data transfer procedures. The fieldperformance audits consist of the periodic evaluation of analytical results of equipment,field and trip blanks to assess the field procedures used, to check for and minimize non-sample-related contamination, and to ensure that representative samples are beingprovided for testing, evaluation, and interpretation.



No field performance audits are planned for this project. However, a performance auditmay be conducted at the discretion of the project manager in the event, for instance, thatacceptance criteria are consistently not met. The field performance audit format will bedeveloped in the same manner described for field system audits. Performance audits will beconducted and reported as described for field system audits.

The project manager is responsible for naming the individual who would conduct thefield performance audits. This person should have a working knowledge of both theanalytical techniques and field sampling procedures being used. All field duplicates andblanks collected during the project should be reviewed. The verification samples will bespot-checked. At a minimum, the performance audits would include the following:

Q Data Integrity Check

• Randomly check if field data have been accurately transferred to final reports;verification of sample location identifications, and areas sampled.

Q Field Blanks

« Prepare a summary report showing all field blank contamination and highlightsamples which may have been affected by the contamination. A sample isconsidered affected if an analyte is detected in the field blank at concentration>PQL, and analyte concentration in the associated sample is <5x the blankresult.

Q Field Duplicates

• Is there a significant difference in reported results for any analyticalparameters between the sample pairs? The acceptance criteria for themaximum % RPD should be less than 20 percent for aqueous results >5x thePQL or ± the PQL if aqueous sample or replicate result is <5xPQL. Prepare asummary report in conjunction with the blank summary report if exceedancesfound.

9.1.2 Field System Audit

System audits are characterized by systematic on-site qualitative reviews and may beconducted in conjunction with all field-related QC activities. The project manager wouldbe responsible for defining the system audit format. The project manager would namethe field system audit team including an individual with extensive experience in fieldsampling activities. The deputy project manager would prepare the final system auditreport, which would be directed to the project manager and project director (see Section14.0).

No field system audits are planned for this project. However, one may be conducted atthe discretion of the project manager in the event of a significant incident involvingsafety, an unfavorable performance audit, or another reason deemed appropriate. At aminimum, the on-site qualitative review would cover the following:

Q Organization and Responsibility

• Is the QA organization effective and efficient?Q Sample Collection



• Are the written procedures for sample collection available and appropriate tomeet regulatory requirements, and are they being followed?

Q Chain-of-Custody

• Have the appropriate steps been followed to ensure the traceability of sampleorigin and integrity?

Q Operational Procedures

• Are the appropriate checks being made in the field, and are records of thesechecks being properly maintained?

Q Equipment

o Is the specified equipment available and maintained in good working order?Q Training

• Are field teams adequately trained?Q Records

• Are record-keeping procedures adequate and functional?Q Corrective Action

• Is the appropriate action being conducted in response to situations? Are thesesituations properly documented? Has follow-up been done to correct thesituation after it has been reported?

Q Health and Safety

• Are the proper procedures, precautions, equipment, training, etc., beingimplemented to protect the team members adequately during the fieldoperation?


Quality Assurance Project Plan Groundwater Monitoring Assessing Data Quality Characteristics

10.0 ASSESSING DATA QUALITY CHARACTERISTICS

DQOs for this project were established in terms of representativeness, comparability,precision, accuracy, and completeness of the data set. Accuracy for this project will bequantitatively assessed through the evaluation of percent recoveries of matrix spikes,matrix spike duplicates, laboratory control samples, and surrogate standards. Precisionwill be quantitatively assessed through the evaluation of % RPD values for matrix spikes,field duplicates, and laboratory replicates. Comparison of results of field duplicates willassist in evaluation of overall representativeness of the data. The appropriate laboratoryQC procedure is specified in each analytical method. Completeness will be determinedfollowing periodic evaluation of the project data sets.

10.1 Representativeness

Representativeness expresses the degree to which data accurately and precisely representsa measured characteristic of a population, parameter variations at the sampling point, aprocess condition, or an environmental condition.

. The degree of representativeness is dependent on the objectives of the measurementresults. Thus, representativeness can be classified into the following four objectivelevels:

Q Level 1

« Sample is only representative of the point of sampling (e.g., drum, storagetank, and single point within a stream or land area).

Q Level 2

• Sample is part of a set and represents a defined area or portion of land orwater, not just the point of sampling (e.g., a stream transect, sampling grid ofa land area, underground aquifer).

Q Level 3• Sample represents a relationship between the source of contamination and the

location sampled (e.g., source and monitoring well, source and stream).Q Level 4

• Sample is non-representative. Sample is used for assessment purposes only(e.g., preliminary assessment, spot check).

The objective of sampling and analysis will be that results are representative of themedium monitored, and its condition, to a degree consistent with the desired objectivelevel. Objective levels 1 and 2 will be used to accomplish project objectives.

10.2 Comparability

For this project, all measurement data will be calculated and reported in units consistentwith standard practice to allow comparability of data. Data comparability also includestrends.


Quality Assurance Project Plan Groundwater Monitoring Assessing Data Quality Characteristics

10.3 Precision

Precision means the measurement of agreement of a set of replicate results amongthemselves without assumption of any prior information as to the true result. Precision isassessed by means of duplicate/replicate sample analysis. To determine the precision ofthe analytical methods, a program of duplicate/replicate analyses will be followed. Thelaboratory will split a sample into two sub-samples and analyze each independently at thefrequency listed in the appropriate method. This approach is followed for laboratoryreplicate samples, field duplicates, matrix spikes, and matrix spike duplicates.

The results of the duplicate/replicate analysis will be used to calculate the QC parameter(% RPD) for precision evaluation. The following equation is used to calculate relative %RPD:

RPD = DZ ~ D' x 100CD, + D 2 ) / 2

where: 'Dl is defined as the first sub-sample valueD2 is defined as the second sub-sample value

In addition to evaluation of the method precision, duplicate samples will be collected inthe field and analyzed independently. The results will be used to evaluate the totalsystem's variability, including sampling variations.

Both the laboratory and URSD will evaluate the analytical precision produced bylaboratory replicate analyses, while field splits will be evaluated only by URSD.Evaluation of both types of data will be in accordance with the referenced methods andthis plan.

10.4 Accuracy

Accuracy means the nearness of a result or the mean of a set of results to the true value.Accuracy is assessed by means of reference samples and percent recoveries. Todetermine the accuracy of an analytical method, a program of sample spiking will befollowed. The spiking frequency is stated in the referenced methods. The results ofsample spiking will be used to calculate the QC parameter percent recovery for accuracyevaluation. The following equation will be used:

% Recovery = SSR ' SR x 100SA

where:SSR = Spiked sample resultSR = Sample resultSA = Spike added


Quality Assurance Project Plan Groundwater Monitoring AsSGSSJng Data Quality Characteristics

10.5 Completeness

Completeness for each parameter is calculated as follows:

Usable DataTotal Data Generated

x 100 = % Complete

Usable data are defined as not rejected during the data review process. The percentcomplete will be used to determine whether the data quality meets the objectives for theproject.

If the completeness objectives are not met for individual parameters, DuPont will reviewthe reasons for the invalid data. Depending on the reasons (e.g., holding time exceeded)and the effect of the incomplete data on the accomplishment of the project objectives,additional samples may be collected and analyzed. A subjective evaluation will also beconducted if a sample does not generate data for a parameter category (e.g., volatileorganic constituents). Such a data gap could result from sample container breakage orloss or sample custody not being maintained. If DuPont determines that the missingresults are critical to accomplishing the Phase IIRFI Work Plan objectives, additionalsampling will be conducted to obtain the missing data.


Quality Assurance Project Plan Groundwater Monitoring CoiTectlVG Action

11.0 CORRECTIVE ACTION

Corrective action is required for any lack of compliance with the requirements of theSampling and Analysis Plan or the QAPP. Each employee working on the project isresponsible for identifying and documenting any QA problems or noncompliance,thereby initiating corrective action. Such documentation will be forwarded to theimmediate supervisor and to the project manager, who. is responsible for design,implementation, and follow-up assessment of appropriate corrective action. In a report tothe project team and to the larger organization, as appropriate, the project manager willdescribe the nonconformance, the applied corrective action, and criteria for determiningthe correction a success. This initial report and subsequent evaluations of the correctiveaction will become part of the project record.

Significant QA corrective actions at the analytical laboratory will be documented andforwarded to the project chemist, who will determine if project data quality has beencompromised by the problem that warranted corrective action. The project chemist willreport these findings to the project manager and to the larger organization, as appropriate.The project manager will decide if further remedy - e.g., sample reanalysis -- is required.These findings will become part of the project record.


Quality Assurance Project Plan Groundwater Monitoring Quality Assurance Reports To Management

12.0 QUALITY ASSURANCE REPORTS TO MANAGEMENT

Periodic reports detailing the results of QA/QC activities described in previous sectionswill be submitted to the project director through the project manager. These documentswill include reports on the following:

Q Significant deviations from protocol as stated in the Groundwater MonitoringSampling and Analysis Plan or the QAPP

Q Field system and performance audits

Q Laboratory system and performance audits

Q Corrective action and follow-up

Copies of quality assurance reports will be submitted to the technical leads, project team,and EPA Region VII, if required.


Quality Assurance Project Plan Groundwater Monitoring Document Control

13.0 DOCUMENT CONTROL

The project manager is accountable for maintaining project record files and storagearchives to meet the requirements of the project and to ensure security, confidentiality,and expeditious access to project records.

The project manager will be responsible for indexing, issuing, and maintaining files forall field notebooks, project correspondence, system and performance audits,non-conformance reports, QC reports, sample data reports, QA reports to management,and other associated documentation. A centralized location will be identified for thispurpose, and a document custodian will be chosen. DuPont will maintain this archivedinformation for seven years following completion of the project. Lancaster will maintainall hard-copy documentation associated with the project for five years. At the end of thisperiod, the laboratory will contact DuPont and request guidance a.s to the final dispositionof the analytical data.


TABLES

Table 1

DuPont Baier Site Groundwater MonitoringQuality Control Acceptance Limits for Metals Analysis

"• • ;-x~ ..:- •'•£;~'-'' -~^:&.' "-, -QC ; Measure f;:-^.

Accuracy (RPR)1

Method Blank

Laboratory Control Spike

Matrix Spike

Post-Digestion Spike

Precision (RPD3)

Matrix Spike Duplicate

Laboratory Replicate

-. All Anaiytes.excepf-Mefcufry .. '••-. v . ',:'• " • ' • ' ' . • • . • . '= ::", '->f :".-..•

<LOQ2

80-120%

75-125%

75-125%

±20% RPD

+20% RPD (for sample >5XLOQ)

;;. * : -/Mercury ; ,

<LOQ

80-120%

75-125%

NA4

±20% RPD

+20% RPD (for sample >5XLOQ)

1RPR = Relative Percent Recovery2LOQ = Limit of Quantitation3RPD = Relative Percent Difference4NA = Not Applicable.

Table 2

DuPont Baier Site Groundwater MonitoringMonitoring Wells

Well ID ; ;;',-

BRA-1S

BRA-1D

BRA-2S

BRA-2D

BRA-3S

BRA-3D

BRA-4S

BRA-4D

BRA-5S

Well DeotMft) Ji;'.. .:... . . - . :'• '«•• '""•' .I-.'

59

137

66

130

58

136

58

133

47

Well Diameter (in).

2

2

2

4

2

2

2

2

2

Table 3

DuPont Baier Site Groundwater MonitoringAnalytical Method Requirements, and Frequency of Field-Collected QC Samples

. _ . : _ :: :M^hod '. ^ /.

Minimum Sample Volume

Sample Container Type

Sample Preservation

Analytical Hold Time

Matrix Spike

Matrix Spike Duplicate

Duplicates

Field Blank

T TAL;M j by;QLP;ILMb5.2

500 mL

Glass

Nitric Acid to pH<2

6 Months, except Mercury.

Mercury: 26 Days

1 per <20 samples of similar matrix



1 per sampling day

Table 4

DuPont Baier Site Groundwater MonitoringCLP ILM05.2 Contract Required Quantitation Limits (CRQL) for

TAL Metals In Water

: C: Analyte

Aluminum

Antimony

Arsenic

Barium

Beryllium

Cadmium

Calcium

Chromium

Cobalt

Copper

Iron

Lead

Magnesium

Manganese

Mercury

Nickel

Potassium

Selenium

Silver

Sodium

Thallium

Vanadium

Zinc

.CLP GRQL:for Water, ug/L. • .;:t--\vt¥<>y.;Y.;r. '.</.' ••;• ,•':•;• „•.-. . . : ; • ; . ' .

200

60

15

200

5

5

5000

10

50

25

100

10

5000

15

0.2

40

5000

35

10

5000

25

50

60

APPENDICES

APPENDIX A

US EPA, OFFICE OF EMERGENCY AND REMEDIALRESPONSE. MULTI-MEDIA, MULTI CONCENTRATION,INORGANIC ANALYTICAL SERVICE FOR SUPERFUND

(ILM05.2). EPA PUBLICATION 540-F-02-008, OCTOBER 2002

United StatesEnvironmental ProtectionAgency

Office ofSolid Waste andEmergency Response

OSWER Document 9240.1-39FSEPA Publication 540-F-02-008October 2002

Multi-Media, Multi-Concentration,Inorganic Analytical Service forSuperfund (ILM05.2)

Office ofAnalytical ItvCenier7S204G) Quick Reference Fact Sheet

Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the ComprehensiveEnvironmental Response, Compensation, and Liability Act of 1980 (CERCLA) and the Superfund Amendments andReauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of variouspollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are ofconcern to EPA at such sites is a series of inorganic analytes and cyanide that are analyzed using Inductively CoupledPlasma-Atomic Emission Spectroscopy (ICP-AES), Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), ColdVapor Atomic Absorption (C VAA), and colorimetric techniques. The Analytical Operations/Data Quality Center (AOC)of the Office of Emergency and Remedial Response (OERR) offers an analytical service that provides data from theanalysis of water/aqueous and soil/sediment samples for inorganic analytes for use in the Superfund decision makingprocess. Through a series of standardized procedures and a strict chain-of-custody, the inorganic analytical serviceproduces data of known and documented quality. This service is available through the Superfund Contract LaboratoryProgram (CLP).

DESCRIPTION OF SERVICES

The inorganic analytical service provides a technicaland contractual framework for laboratories to utilizeEPA/CLP analytical methods. These methods are usedin the isolation, detection and quantitative measurementof 23 target analytc metals (including mercury) andcyanide in both water and soil/sediment environmentalsamples. The CLP provides the methods to be used andthe specific technical, reporting, and contractualrequirements, including Quality Assurance (QA),Quality Control (QC), and Standard OperatingProcedures (SOPs), by which EPA evaluates the data.

Three data delivery turnaround times are available toCLP customers: 7, 14, and 21-day turnaround afterreceipt of the last sample in the set. A 72-hourpreliminary data submission option also is available forall turnaround times. The data associated with thesePreliminary Results is due within 72 hours after receiptof each sample at the laboratory. In addition, data usersmay include, but are not limited to, additional analytesand/or lower quantitation limits.

DATA USES

This analytical service provides data that EPA uses fora variety of purposes. Examples include determining,the nature and extent of contamination at a hazardouswaste site, assessing priorities for response based onrisks to human health and the environment, determiningappropriate cleanup actions, and determining when

remedial actions are complete. The data may be usedin all stages in the investigation of a hazardous wastesite including: site inspections, Hazard Ranking Systemscoring, remedial investigations/feasibility studies,remedial design, treatability studies, and removalactions. In addition, this service provides data that areavailable for use in Superfund enforcement/litigationactivities.

TARGET ANALYTES

The inorganic analytes and quantitation limits for whichthis service is applicable are listed in Table 1. Specificdetection limits are method and matrix dependent.

The list of target analytes for this service was originallyderived from the EPA Priority Pollutant List of 129compounds. In the years since the inception of theCLP, analytes have been added to and deleted from theTarget Analyte List (TAL), based on advances inanalytical methods, evaluation of method performancedata, and the needs of the Superfund program.

METHODS AND INSTRUMENTATION

The Contractor will demonstrate the ability to meetcertain program data quality objectives prior toanalyzing field samples.- The Contractor mustdocument methods used to generate analytical resultsand determine Method Detection Limits (MDLs). ICP-

. Atomic Emission Spectroscopy (ICP-AES) is used toanalyze water, sediment, sludge, and soil samples.

Table 1. Inorganic Tarcet Analvte Lilt and Contract Reouired Ouantitation Limits fCROLs)

1.2.3.4.5.6.7.8.9.10.11.12.13.14.15.16.17.18.19.20.21.22.23.24.

Analvte

AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSodiumThalliumVanadiumZincCyanide

1CP-AES CROL forWater (• t/L)

20060IS

20055

500010502510010

5000150.240

50003510

500025506010

ICP-AES CROL forSoil (mg/kg)

40123

4011

10002105202

10003

0.18

100072

1000510121

ICP-MS CROL forWater (• t/L)

3021

1011

20.52..1..0.5-.1..51..111--

Water and soil samples are treated with acids and heator microwave energy. The digestates are then analyzedfor trace metals by an atomic emission opticalspectroscopic technique. The samples are nebulizedand the aerosol is transported to a plasma torch. Theatomic-line emission spectra arc dispersed and aphotosensitive device monitors line intensities.

ICP-Mass Spectrometry (ICP-MS) is used to determinethe concentration of dissolved and total recoverableelements in water/aqueous samples. The samplematerial is introduced, by nebulization, into radiofrequency plasma where desolvation, atomization, andionization take place. The ions are extracted from theplasma through a differentially pumped vacuuminterface and separated based on their mass-to-chargeratio.

Cold Vapor Atomic Absorption (CVAA) is used toanalyze water, sediment, sludge, and soil samples fortotal mercury. Organomercury compounds may also bepresent and will need to be broken down and convertedto mercuric ions to respond to the CVAA techniques.For water samples, organic compounds are oxidizedand then reacted with a strong reducing agent. Thevolatile free mercury is then driven from the reactionflask by bubbling air through the solution. The airstream carries the mercury atoms to an absorption cell,which is then placed in the light path of the AAspectrophotometer. For soil/sediment, the samplesundergo acid digestion/oxidation followed by reduction

and measurement by conventional cold vaportechnique.

Various water types, sediment, sludge, and soil samplesare also analyzed for total cyanide. Hydrocyanic acid(HCN) is released through a reflux-distillation andabsorbed in a scrubber containing sodium hydroxidesolution. The cyanide ion is determinedcolorimetrically by converting it to cyanogen chloride(CNC1).

Table 2 summarizes the methods and instruments usedin this analytical service.

DATA DELIVERABLES

Data deliverables for this service include bothharcdcopy/electronic data reporting forms andsupporting raw data. The laboratory must submit datato EPA within 7-, 14- or 21-days, or preliminary datamust be submitted within 72 hours after laboratoryreceipt of each sample in the set, if requested. EPAthen processes the data through an automated DataAssessment Tool (DAT). DAT is a complete CLP dataassessment package. DAT incorporates ContractCompliance Screening (CCS) and Computer-AidedData Review and Evaluation (CADRE) review toprovide EPA Regions with electronic reports (PC-compatible reports, spreadsheets, and electronic files)within 24 to 48 hours from the receipt of the data. Thisautomated tool facilitates the transfer of analytical data

Table 2. Methodi and Initnimenti

Analyte

Al, Sb, As. Ba, Be, Cd, Ca, Cr, Co. Cu,Fe, Pb, Mg, Mn, Ni. K. Se, Ag, Na, Tl,V.Zn

Al, Sb. As, Ba, Be, Cd, Cr, Co, Cu, Pb,Mn, Ni, Se, Ag, Tl, V, Zn

Mercury (Hg)

Cyanide (CM)

Instrument

Inductively Coupled Plasma - AtomicEmission Spectroscopy (ICP-AES)

ICP - Mass Spectrametry (ICP-MS)

Cold Vapor Atomic Absorption(CVAA)

Colorimeter or Spectropbotometer

Method

ICP analysis of atomic-line emissionspectra.

ICP analysis of ions separated on basisof mass-to-charge ratio.

Acid digestion/oxidation followed byreduction and CVAA analysis.

Distillation followed by colorimetricanalysis.

Table 3. Quality Control

QC Operation

Instrument Calibration

Initial Calibration Verification

Initial Calibration Blank

Continuing CalibrationVerification

Continuing Calibration Blank

CRQL Check Standard (CRI)

. . , ^ < «

Serial Dilution for ICP

Preparation Blank

Laboratory Control Sample

Spike Sample

Pott Digestion/Distillation Spike

Duplicate Sample Analysis

ICP-MS Tune

Method Detection LimitDetermination

Interelement Corrections

Linear Range Analysis

Frequency

Daily or each time instrument is set up.

Following each instrument calibration for each wavelength or mass used.

Following each instrument calibration, immediately after the Initial CalibrationVerification (ICV).

For each wavelength or mass used, at a frequency of 1 0% or every two hours of a run,whichever is more frequent, and at the beginning and end of each run.

10% or every two hours of a run, whichever is more frequent, and at the beginning andend of each run. Performed immediately after the last Continuing CalibrationVerification (CCV).

Every 20 analytical samples and at the beginning and end of each run, but not beforethe ICV. Performed before the Interference Check Sample.

For ICP-AES, every 20 analytical samples and at the beginning and end of each run,immediately after die CRI. For ICP-MS, at the beginning of the run.

For each matrix type or for each SDG, whichever is more frequent.

For each SDG or each sample preparation and analysis procedure per batch of preparedsamples.

For each SDG or each sample preparation and analysis procedure per batch of preparedsamples, except aqueous mercury and cyanide.


Each time Spike Sample Recovery is outside QC limits.


Prior to calibration.

Prior to contract, annually thereafter, and after major instrument maintenance.

Prior to contract, quarterly thereafter, and after major instrument adjustment.

Quarterly.

into Regional databases. DAT can also be used toassist in the data validation process at the Region. Inaddition to the Regional electronic reports, die CLPlaboratories are provided with a data assessment reportthat documents the instances of noncompliance. Thelaboratory has four business days to reconcile defectivedata and resubmit the data to EPA. EPA then reviewsthe data for noncompliance and sends a final dataassessment report to the CLP laboratory and theRegion.

QUALITY ASSURANCE

The Quality Assurance (QA) process consists ofmanagement review and oversight at the planning,implementation, and completion stages of theenvironmental data collection activity and ensures thatthe data provided are of the quality required. Duringthe data collection effort, QA activities ensure that theQuality Control (QC) system is functioning effectivelyand that the deficiencies uncovered by the QC systemare corrected. After environmental data are collected,QA activities focus on assessing the quality of dataobtained to determine its suitability to supportenforcement or remedial decisions. Each contractlaboratory will establish a Quality Assurance Plan(QAP) with the objective of providing sound analyticalchemical measurements. The QAP must specify thepolicies, organization, objectives, functional guidelines,and specific QA/QC activities designed to achieve thedata quality requirements for this analytical service.

QUALITY CONTROL

The QC process includes those activities requiredduring analytical data collection to produce data ofknown and documented quality. The analytical dataacquired from QC procedures are used to estimate andevaluate the analytical results and to determine thenecessity for, or the effect of, corrective actionprocedures. The QC procedures required for thisanalytical service are shown in Table 3.

PERFORMANCE MONITORING ACTIVITIES

Laboratory performance monitoring activities areprovided primarily by AOC and the Regions to ensurethat contract laboratories are producing data of theappropriate quality. EPA performs on-site laboratoryaudits, data package audits, and evaluates laboratoryperformance with blind performance evaluationsamples.

For more information, or for suggestions to improvethis analytical service, please contact:

John NebelsickInorganic Program ManagerUSEPA/AOCAriel Rios Building (5204O)1200 Pennsylvania Avenue, NWWashington, D.C. 20460Tel: 703-603-8845Fax:703-603-9112

APPENDIX B

STANDARD OPERATING PROCEDURE FOR COMPLETINGCHAIN-OF-CUSTODY FORMS

STANDARD OPERATING PROCEDUREFOR COMPLETING CHAIN-OF-CUSTODYFORMS

Date: May 11, 200J Prepared for: DuPont Remediation Group




Kelly A. Rinehimer John C. McVoy Alan P. EglerURS Diamond URS Diamond URS Diamond

ADQM Project Chemist ADQM Manager Quality Assurance Officer

Standard Operating Procedure for Completing Chain-of-Custody Forms SOP Number 1Issued: May 11,2001

Revision: 0Page 2 of 9

TABLE OF CONTENTS

1. Purpose 4

2. General Information 4

3. Procedures 43.1 Chain-of-Custody (COC) 4

3.1.1 Option A (Pre-printed COC originated by Laboratory Personnel) 43.1.2 Option B (Pre-printed/Blank COC Originated in the Field) 5

4. Signatures 54.1 Option A 54.2 OptionB 6

5. Derived COCs 6

6. "Cross Outs" on COC 8

7. Location of COC with respect to cooler 8

8. Bottle Labels 8

9. Date/Time of Sample Collection 8

10. Custody Seals 9

11. Cooler Numbers 9

12. Special Requests/Concerns 9

13. Step-By-Step Instructions 9

FIGURES

Figure 1 Example of laboratory originated COC sent to the field

Figure 1A Example of laboratory originated COC after completed in the field

Figure 2 Example of COC to be originated in the field

Figure 2A Example of COC to be originated in the field once completed in the field.

Figure 3 Original COC/Derived COC from original COC

Figure 4 COC Exception Report Form

4017SOPforCompletingCOCform.doc Jun. 4, 01 Wilmington, DE

Standard Operating Procedure for Completing Chain-of-Custody Forms SOP Number 1Issued: May 11, 2001


APPENDICES

Appendix A Sample Identifier Coding

Appendix B Example Custody Seal

Appendix C Step-by-Step Instructions on How to Complete a Chain-of-Custody

4017SOPforCompletingCOCform.doc Jun.4, 01 Wilmington, DE



1. PURPOSE

The purpose of this standard operating procedure is to establish a CRG/URSD proper chain-of-custody (COC) standard for tracking samples from the field to the laboratory. A proper COC isnecessary if there is any possibility that the analytical data or conclusions based upon theanalytical data will be used in litigation (SW846, Chapter 9, Section 9.2.2.7). The personsentering information on the COC are responsible for ensuring the document can withstandscrutiny during litigation.

2. GENERAL INFORMATION

The COC is a legal document/record that must include: facility name, facility address, phonenumbers (primary contact and laboratory), sample identification, preservation, dates and times ofcollection of samples, possession, analyses, and laboratory performing the analyses.

3. PROCEDURES

3.1 Chain-of-Custody (COC)

The policy is to use either Option A or Option B as stated below.

3.1.1 Option A (Pre-printed COC originated by Laboratory Personnel)

If the regulatory agency requires initiation of the COC at the laboratory, use Option A. SeeFigures 1 and 1A for examples of COC Option A.

Laboratory Personnel do the following:

Q Originate the pre-printed COC by relinquishing the bottles with a signature.The pre-printed COC contains the following information: header information (e.g.,facility name, facility address, facility supervisor, project name), location code, matrixcode, sample source (e.g., KIN-G-MW1), sample depths, sample type, volume,preservative (if applicable), quantity, bottle type, method and/or analyte.

Q If the sample IDs are known at the time of bottle preparation, pre-print the location code,matrix code, and sample location (e.g., KIN-G-MW1) on the COC.

Q If the sample IDs are not known at the time of bottle preparation, either pre-print thelocation code and matrix code only on the COC (e.g., KIN-G) or leave the sample JDblank.

Field Personnel do the following:

Q If a sample is pre-printed on the COC but will never be collected:

1. Cross out the sample on the COC.

2. Date and initial next to the cross-out and give reason on the COC (e.g., well is dry).




Q If an extra sample is collected that was not pre-printed on the laboratory relinquishedCOC, add this sample to a blank COC not the COC that was relinquished by LaboratoryPersonnel.

Q If all of the samples listed on the laboratory relinquished COC cannot be collected in oneday, use derived COC (see Section 5). (A way to avoid using derived COC is to have onewell or boring location per COC.)

Q If a sample is moved from one cooler to another:

1. Add the comment "Moved to COC Y" (where Y is the unique COC number locatedon the top right-hand of the COC) in the date and time field on COC X next to thesample being moved.

2. Add the sample to COC Y.

3. Add the comment "moved sample from COC X" (where X is the unique COCnumber located on the top right-hand of the COC) in the margin of the COC Y nextto the sample that was moved.

3.1.2 Option B (Pre-printed/Blank COC Originated in the Field)

Q Laboratory Personnel issue forms along with the bottles to be used as chains-of-custody.These forms can be pre-printed or left blank.

Q Field Personnel do the following:

1. Collect the samples, write the sample ID according to the nammg convention asdescribed in Appendix A, if not already present, on the COC.

2. Write the date and time of sample collection on die COC.

3. Enter the remaining information on the COC [i.e., sample type, volume, preservative(if applicable), quantity, bottle type, method and/or analyte (if not already pre-printedon the COC)].

4. Once the samples are ready to be shipped to the laboratory and all of theaforementioned information has been entered for the samples collected, relinquish thesamples to the laboratory with his/her signature, date, and time (see Figure 2 and 2Afor examples of Option B).

4. SIGNATURES

4.1 Option A

If Laboratory Personnel initiate the COC:

1. Laboratory Personnel relinquish the bottles with a signature.

2. Project Manager designates Field Personnel.

3. Field Personnel receive the cooler(s) from the courier (i.e., Laboratory/FederalExpress/Airborne).At this time, Field Personnel sign the shipping paperwork. OR, if someone other than

4017SOPforCompletingCOCform.doc Jun..4, 01 Wilmington, DE



Field Personnel is designated by Project Manager to receive the bottles from Courier, thatperson signs the shipping paperwork upon receipt of the coolers.

4. Field Personnel:

a Check contents of cooler against COC

Q Sign the COC in the "Received By" box.

a Relinquish the samples to the laboratory once they have finished sampling. (Note: Ifmore than one person is in the field sampling, the person receiving thebottles/samples must also relinquish the bottles/samples.

5. Laboratory personnel:

Q Cross-out the unused "Received By/Relinquished By" boxes prior to signing.

Q Sign the COC upon receipt of the samples.

6. Field Personnel file and keep the Federal Express/Airborne bill of lading to and from thesite (if possible).

4.2 Option B

If Laboratory Personnel did not initiate the COC:

1. Field Personnel sign the COC upon completion of sampling in the Relinquished By box.

2. Laboratory Personnel sign the COC upon receipt of the samples and cross-out the unused"Received By/Relinquished By" boxes.

3. Field Personnel file and keep the Federal Express/Airborne bill of lading from the site (ifpossible).

5. DERIVED COCS

(Necessary to complete the record of custody when using COC Option A and all of the sampleson the pre-printed COC cannot be collected on a single day.)

a If the COC was originated by Laboratory Personnel with a relinquished signature and allof the samples listed on the COC cannot be collected and sent in one shipment, FieldPersonnel must use the Derived COCs. (One way to avoid the Derived COC is to list onewell or boring location per COC.)

a Field Personnel must write the sample IDs of the samples that were collected that day andare to be shipped to the laboratory on the Derived COC. It is important that FieldPersonnel:

1. Transcribe all of the information pertaining to the sample (e.g., correct sample ID,parameters, preservative, etc.) on the Derived COC.

2. Reference the Derived COC# on the Original COC in the "Date and Time" boxes ofthe sample that was transcribed onto the Derived COC.

3. If the Derived COC doesn't have a number, Field Personnel must assign a number.The assigned number may be the original COC number followed by a -1.




a The original COC remains in the field until all the samples listed on the COC have beencollected.

Q Field Personnel send the original COC with the last shipment of samples listed on theoriginal COC (see Figure 3 and 3A for examples of "Derived COC").




6. "CROSS OUTS" ON COC

a If corrections are made to the COC while in the field, Field Personnel must date andinitial next to the item that was crossed out.

a If corrections are to be made to the COC after it has left the field, ADQM Personnel:

1. Document the error (i.e., email or send out the COC Exception Report form).

2. Send the email/COC Exception Report form to the person requesting the correction(if other than ADQM Personnel) for signature.

a Once the requestor has reviewed the documentation, he/she sends an emailacknowledging the correction or mails the COC Exception Report form back, to ADQMpersonnel with a signature.

a ADQM keeps the original with the file and sends a copy to Laboratory Personnel and tothe project manager.

7. LOCATION OF COC WITH RESPECT TO COOLER

Laboratory Personnel:

1. Print the COC on carbon paper so that all parties handling the samples can maintain acopy in their files.

2. Place the original COC or form (which will become a COC once a signature has beenadded) inside the cooler when shipped to the field.

Field Personnel:

1. Place the original COC and laboratory copy in the cooler containing the samples listed onthat COC.

2. Keep one carbon copy of the COC for their files.

8. BOTTLE LABELS

Field Personnel must make sure that the bottle label contains the full sample ID (see AppendixA), the preservative added, the number of bottles, the analyses, and whether or not the sample isfiltered. The information on the bottle label must match the information on the COC.

9. DATE/TIME OF SAMPLE COLLECTION

Field Personnel must:

1. Write the date on COC as MM/DD/YY (e.g., 8/31/99)

2. Write the time on COC in 24 hour or military time (e.g. 1330). The time of collection isrecorded as the time the sample was initially taken. A separate time of collection is notrequired for each parameter (e.g., time for volatiles, time for semivolatiles, etc.) The dateand time of collection of the matrix spike and matrix spike duplicate samples are the samedate and time as the original sample.




10. CUSTODY SEALS

a Laboratory Personnel include custody seals with each cooler shipment.

a Field Personnel:

1. Pack the samples on ice in the cooler.

2. Once the cooler is ready for shipment, tape the custody seals to the broad side of thecooler lid opposite the hinges in such a way that the seals will be broken if the cooleris opened.

3. Sign and date the custody seals prior to shipment to Laboratory Personnel.If Field Personnel break the seals of the cooler prior to shipment (e.g., to re-ice thesamples), Field Personnel must attach another set of seals to the cooler with the FieldPersonnel's signature and the date.

4. If specified in the QAPP, attach custody seals to the bottles. Place the seal over thecap of the bottle and down both sides in such a way that, if the cap is unscrewed, theseal will be broken (see Appendix B for example custody seal).

11. COOLER NUMBERS

ADQM Personnel instruct the laboratories to write cooler numbers on coolers and associatedCOC containing samples to be analyzed for volatiles (e.g., label attached with cooler number orcooler number written directly on cooler).

12. SPECIAL REQUESTS/CONCERNS

Field Personnel use comment section of COC for special requests/concerns such as analyzewithin 7 days, high PID reading, etc.

13. STEP-BY-STEP INSTRUCTIONS

All personnel can follow the step-by-step instructions on how to complete a COC (see AppendixC).


Figure 1Lancaster Laboratories2425 New Holland Pike PO Box 12425 Lancaster, PA 17605-2425

Example of laboratory originated COC sent to the field

No. 123

Facility Name: DllPont Cape Fear 1telephone Number: 9 1 0-37 1 -4409

Facility Address: State Road 1426, Leland, NC 28451

Facility Supervisor: Bill JOHCS

Process Producing Sample: Indicator GW

Employee(s) Sampling:

Other Employee(s) Handling:

Sample. Description

CAP-G-MW-30

Date

/f-

Bottles Relinquished by ffjtl MUM,

Bottles Relinquished by



TimeSampleType

WW

BottleVolume

(ml)

40

Job Number: 7035-504116-772000

Method of Shipping: Fed ExShipping

instructions: Priority Overnight

Comments:

Preservative

HCL

Quantity

2

Laboratory relinquishes the bottles by signinc

//

[/

K

Date/ Time (,3/22/01

Date; Time

Date/ Time

Dale/ Time

/

/

10:00

//

BottleType

V

COo<oCNJCO

X

and dating here

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

Date/Time

Date/Time

Date/Time

Date/Time

Condition of samples upon arrival:

Signature:

Date:

Temp of Samples on Arrival: C

FigureLancaster Laboratories2425 New Holland Pike PO Box 12425 Lancaster, PA 17605-2425

Example of laboratory originated COCafter completed in the field

No. 123.

Facility Name: DuPont Cape Fear •r.lephone Number: 910-371 -4409


Facility Supervisor: Bill JOIieS


Employee(s) Sampling: Joe Sample

Other Employee(s) Handling: Dave White

Sample Description

CAP-G-MW-30

Date

03/22/01

Time

1200

SampleType

WW

BottleVolume

(ml)

40

ob Number: 7035-504116-772000

Method of Shipping: Fed EXShipping

instructions: Priority Overnight

Comments:

Preservative

HCL

Quantity

2

BottleType

V

COOCDCNCO

X

Laboratory personnel will accept receipt of the samples by signing and dating here.

Person who received the bottles must also relinquish the bottles by signing here/

Laboratory relinquishes the bottles by signing and dajtfig herlhe point of contact receives the bottles by signing and dating here.

\

\\.A





\^\

&4 A^It

J« 4,nA

.

s /^

/

Date/

Time 03/21/01

Date/

Time 03/22/01

Date/Time

Date/Time

10:00

1600

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

U^A

Ut> £JtflilVV

-^

lijatr AdnimL

^

^

^^^

Date/Time 03/22/01

Date/ /

Time /~—

DateVTime ^/

Date/

Time 03/23/01

,

'*'

^Xo

......

^930

s

/

//

//

//

/s

/s

/

/

/ /

//

/ /Condition o^/samples upon arrival: Good

Signature-. &l- j'l(/tu(!te

Date: 03/23/01

Temp of Samples on Arrival: 2_C

Figure 2

Lancaster Laboratories

2425 New Holland Pike PO Box 12425 Lancaster, PA 17605-2425

Example of COG to be originated in the field

No. 124

Facility Name: DuPont Cape Feaf Telephone Number: 910-371-4409

Facility Address: State Road 1426, Leiand, NC 28451

Facility Supervisor: Bill JOHSS


Employee(s) Sampling:

Other Employec(s) Handling:

Sample Description

CAP-G-MW-30





Date TimeSampleType

WW

Date/Time

Date/Time

Date/TimeDate/Time

BottleVolume

(ml)

40

Job Number:

Method of Shipping:Shipping

Instructions:

Comments:

Preservative

HCL

Quantity

2

BottleType

V

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

moCDCMCO

X

Date/Time

Date/TimeDate/TimeDate/Time


Signature:

Date:


FigureLancaster Laboratories


Example of COC to be originated in the field

once completed in the field

No. 124

Facility Name: DuPont Cape Fear telephone Number: 910-371-4409


Facility Supervisor. Bill JOCICS


Employee(s) Sampling: Bob Adams

Other Employee(s) Handling: Dave White

Sample Description

CAP-G-MW-30

Date

03/22/01

Time

1030.

SampleType

WW

BottleVolume

(ml)

40

Job Number: 7035-504116-772000

FederalMethod of Shipping: Express

Shippinginstructions: Priority Overnight

Comments:

Preservative

HCL

Quantity

2

Field Personnel initiates the COC upon relinquishment





of the samples by signing and dat'm

\\*uw Mwuv*

._.

\\

-1- ^Date/Time 03/22/01

Date/Time

Date/Time

Date/Time ._

15:00

3 here.

BottleType

V

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

CDOCOCMCO

X

Laboratory personnel will accept receipt

of the samples by signiru

— /. J

/r

w* .IwiiA

Y

Date/ Time

Date) Time

Date/ Time ._/4

Date/ Time Q3/23/01

and dating here.

/

.//

900

Condition of samples upon arrival: Good

Signature: Jo* k-.iA

Date: 03/23/01

Temp of Samples on Arrival: 3C

Figure 3

ORIGINAL COC

Lancaster Laboratories


Original COC

No. 123

Job Number: 7035-504116-772000

Facility Name: DuPOflt Cape F63 Felephone Number: ' 910-371-4409


Facility Supervisor: Bill JoneS



Other Employee(s) Handling:

Sample Description

CAP-G-MW-30

CAP-G-MW-28

CAP-G-MW-28D

CAP-G-MW-29





Date Time

See COC 123-1

(i». ImA

SampleType

WW

WW

WW

WW

Date/Time 03/22/01

DatefTimeDate/TimeDate/Time

BottleVolume

(ml)

40

40

40

40

9:00

Method or Shipping: Fed ExShipping

instructions-. Priority Overnight

Comments:

Preservative

HCL

HCL

HCL

HCL

Quantity

2

2

2

2

BottleType

V

V

V

V

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

mo(0CMCO

X

X

X

X

Copy all of the Information wrt CAP-G-MW-30 onto derived COC

Date/Time

Date'Time

Date/Time

Date/Time


Signature:

Date:


Figure 3DERIVED COC FROM ORIGINAL COC

Lancaster LaboratoriesDerived COC


Facility Name: DuPOIlt Cape F63 Telephone Number: 910-371-4409


Facility Supervisor: Bill JOCieS



Other Employee(s) Handling: D3V6 White

Sample Description

CAP-G-MW-30

Date

03/23/01

Time

1000

SampleType

WW

Field Personnel must relinquish

the samples by signing and dating here.





/

&,[: xU.«tt,

J,DatefTime 03/23/01

Date/Tims

Date/Time

Date/Time

BottleVolume

(ml)

40

15:00

No. 123-1 k.Job Number: 7035-504116-772000 \

Method of Shipping: Fed ExShipping \

instructions: Priority Overflight

Comments: \

\\Number of derived COC to tie

Preservative

HCL

Quantity

2

BottleType

V

Bottles Received by

Bottles Received by

Bottles Received by

Bottles Received by

m0coCM00

X

it back to the original COC.

Add all information wrt CAP-G-MW-30

from original COC.

Laboratory personnel will accept the

samples by signing and dating here.

.

/

-2w

J* l*&

/Date!/Tim*

(fate/Time

Date/Time

/

/

. .

.-4Date/Time 03/24/01

--/-/_.

930

/

/

/

Condition of samples upon arrival: Good

Signature: f™ ArnA

Date: 03/24/01

Temp of Samples on Arrival: 3 C

Figure 4COC Exception Report Form

Job Name: Site:Form Initiated By/Date: Date Samples Collected:Responsible Party:

Nonconformance (check appropriate box):

Category I: Sample Collection Category III: Other

t 1. Sample Containers Broken in Field t 14.t 2. Requested Measurements Not Performed t 15.t 3. Sample Not Collectedt 4. Sample ID IncorrectExplanation

Category II: Sample Receiving

t 5. Holding Time Exceeded By"t 6. Test added by Client After Login (specify)t 7. Sample Received Broken/Leaking11 8. Sample Received in Improper Container"t 9. No Sample ID on Containert 10. Sample ID Does Not Match Paperwork1" 11. Volatile Sample Received With Headspacet 12. COC Not Completedt 13. Sample Temperature Exceeds 4°C

CORRECTIVE ACTION

Root Cause:

Initials! Date:Corrective Action:

Initials/Date:Action to Prevent Recurrence;

Initials/Date:

Manager Review:

Date Manager Aware of Problem: Manager's Initials:Manager's Comments:

SAMPLE IDENTIFIER CODING

APPENDIX A

PURPOSE

Sample identifiers are used in the sampling plan, on the Chain-of-Custody, and on sample bottles toidentify samples as they are created in the field. When the samples are delivered to the laboratory foranalysis, the sample identifier on each sample bottle is verified on the Chain-of-Custody, and then it isentered into the laboratory's information system. When the laboratory analyses are completed, alaboratory report and an electronic deliverable are provided by the lab. The sampleid ties these resultsto the appropriate sample.

By encoding the sample identifier with certain pieces of information about the sample, several thingsare accomplished. l)lt provides a mechanism for identifying the samples uniquely. 2)It conveysinformation about the type and location of the sample to those who are setting up the samplingprogram, those that are working in the field, and those that are reviewing the data. 3)It enables thedata management system to automatically decode the information and store the individual data items inseparate database fields for later use in data analysis and reporting.

FORMAT

Figure 1 illustrates the sample identifier coding format. The fields making up the sample identifier aredescribed in detail on the following page. Examples of different sample identifiers are also provided.

S a m p l e s w i t h o u t d e p t h sL O G ( 3 C h a r a c t e r s )

M A T K I X ( I C h a r a c t e r )

— S A M P L I N G P O I N T( M i i i n t u m 1 6 C h i r a c

S P E C I A L S A M P L ED E S I G N A T I O N(Maw i t h 3 c h a n c i e r ! e a c hi c p a r a i c d by a d i * h )

E x a m p l e : C W K - a - K I i - M 0 I B - D U P

S a m p l e s w i t h d e p t h s

L O C ( 3 C h a r i c t e r l )

~ M A T R I X ( I C h a r a c t e r )

S A M P L I N G P O I N T( M a x i m u m V C h a r a e i e r i )

D E P T HI N T E R V A L( F e e l O n l y .M a x i m u m 4 I S P E C I A L SC h a n c i e r ! E a c h . D E S 1 0 N A TD e c i m a l Fo i l , . « I + ( M a x i m u m 1

S P E C I A L S A M P L ET l O N

D e t i f n a t i o nh 3 c h a r a c t

E x a m p l e : C W K - S - C P T - 0 0 1 ( 1 0 . 5 - I 1 . 5 J - D U P

Modified.Ian 6. 1999

Figure I

Page 1


FIELDS

Sample identifiers should consist of the fields listed below concatenated in the order they are listed.The LOG, MATRIX, and SAMPLING POINT are required for all samples. The other fields areoptional depending on the type of sample.

LOG — A three character code designating the plant location or site where the sampling is being done.For example, CWK designates Chambers Works; REP designates Repauno. See Table 1 fora listing of codes. Contact the Lab Service Coordinator for locations not listed. It is requiredon all sample identifiers and must be the first item in the sample identifier.

SAMPLE TYPE — A one character code designating the sample type. It is required on all sampleidentifiers and must immediately follow the LOG code with a dash separating it from the LOGcode. If an unusual sample type is being sampled that needs to be specifically classified,contact the Lab Service Coordinator to obtain a new code.

G = Ground Water S = Soil A = AirW = Surface Water E = Sediment N = Animal TissueD = Drinking Water U = Sludge R = Plant TissueK = Blank Water P = Wipe M = MicrobiologicalL = Leachate T = Waste X = Toxicological

Z = Other

SAMPLING POINT NAME — The sampling point name. This may be a well identifier, soil samplecode, outfall point, etc. These identifiers should conform to the plant naming convention.Thus, if the official name of a well as defined by the plant is MW-2, then MW2, MW_2, M-2,2, etc. should not be used. Only MW-2 should be used. Dashes are permitted within thesampling point name.

A sampling point is required in all Sample Identifiers and must immediately follow the matrixcode with a dash separating it from the Matrix. For sampling points without depths, themaximum length of the sampling point is 16 characters. For sampling points with depths, themaximum length of the sampling point is 9 characters. Blanks are not permitted but may bedenoted by an underscore, i.e. OUTFALL_023.

Blank samples used for QC should be identified as follows: Equipment blanks should beidentified as EQBLK-#. Field blanks should be identified as FBLK-#. Trip blanks should beidentified as TBLK-#. The # should be replaced with 1 to the number of the particular typeof blank included in the sampling event, which may extend over several days. For example, ifthree trip blanks are included in a sampling event extending over two days, they would bedesignated TBLK-1, TBLK-2, and TBLK-3

DEPTH INTERVAL- The depth to the top of the sampling interval followed by the depth to thebottom of the sampling interval. The depth interval must be in feet, and it must be surroundedby parentheses with the top and bottom depths separated by a dash. Each depth may have amaximum of 4 characters with a decimal point counting as one character. Thus, with twodecimal places, the maximum depth is 9.99 feet; with one decimal place, the maximum depthis 99.9 feet; with no decimals, the maximum depth is 9999 feet. The depth interval is requiredfor all soil samples.

Modified.Jan 6, 1999 Page 2


SPECIAL SAMPLE DESIGNATIONS - Designates samples used for QC purposes or requiringspecial handling in the field. The code must be preceded by a dash. Do not specify these ifthey do not apply.

DUP — 2nd sample in a duplicate sample setDIS — Sample filtered in the field for dissolved metals analysis.ACR — This sample is for Acrolein/Acrylonitrile analysis. It requires different preservation

than standard VOA samples.MS — Matrix Spike sample.MSD - Matrix Spike Duplicate sample.

EXAMPLES

1. Groundwater Monitoring Well K16-M05B primary sample at Chambers Works

CWK-G-K16-M05B

2. Groundwater Monitoring Well K16-M05B duplicate sample at Chambers Works

C WK-G-K16-M05B-DUP

3. Groundwater Monitoring Well K16-M05B primary sample for dissolved metals at Chambers Works

C WK-G-K16-M05B-DIS

4. Groundwater Monitoring Well MW-44 Matrix Spike samples at Repauno

REP-G-MW-44-MSREP-G-MW-44-MSD

5. Monitoring Well K16-M05B duplicate sample for dissolved metals at Chambers Works

CWK-G-K16-M05B-DIS-DUP

6. Surface Water at Outfall 023 primary sample for Acrolein/Acrylonitrile at Niagara

NIA-W-OUTFALL_023-ACR

7. Surface Water at Outfall 23 duplicate sample for Acrolein/Acrylonitrile at Niagara

NIA-W-OUTFALL _023-ACR-DUP

8. Soil boring D5534 primary sample at Chambers Works taken at a depth of 6.5 feet to 7 feet

CWK-S-D5534(6.5-7)

9. Soil Sample P123 duplicate sample at Chambers Works taken at a depth from 6 to 12 inches

CWK-S-P123(.5-1)-DUP

10. Two Trip Blanks and an Equipment Blank for sampling at Cookson

CKS-K-TBLK-1CKS-K-TBLK-2CKS-K-EQBLK-1

Modified Jan 6. 1999 Page 3

TABLE 1

LOC CODES

Page 4

LOG CODES

l liQ* ^ ^^^ rStfE^MijE- i :M^^A^^^^KS^^^^^^SK^^e ff ^^^ \ABD ABERDEEN.MS ! FLO

ABN ABERDEEN.NC | FMN

ALB ALBANY GEA

ACT ! ALLIS CHALMERS TRUST SITE GCC

ANT ANTIOCH ! GLV

iASH ASHEPOO GCK

AST ASTON GLA

ATH ATHENA 1 GLN

^FLORENCE

FORT MADISON

! GEASLIN

GEON - CALVERT CITY

GEON - LOUISVILLE

GILL CREEK

GLASGOW

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BETHANY

BOERKE SITE

BREVARD

BRIDGEPORT

IBURNSIDE

i CAPE FEAR

JCARLYSS

CARTERET

CHAMBERS WORKS

1 CHATTANOOGA-DUPONT

i CHESAPEAKE

•CHESTNUT RUN

CHOCOLATE BAYOU

CHRISTINA LABS

CINCINNATI

CIRCLE RIDGE

CIRCLB/ILLE

CLEVELAND

CLIFTON

CLINTONCOOKSON

COOPER RIVER

CORPUS CHRISTI

DACULADEL CITY

DELISLE

DOVER

DUPONT AUTOMOTIVES PLANT

DUPONT-ELSTON AVENUE

EAGLE RUN

EAST CHICAGO

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ELK RIVER LEARNING CENTER

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Page 5

LOC CODES

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VALLEY CENTER "j

VICTORIA |

WASHINGTON WORKS :

WAYNESBORO j

WEST ALTON |

WILMINGTON, PA j

WURTLAND j

WYSHOCK 1

f

(SEN | SENECA

Page 6

LOC CODES

Modifications:

August 26, 1998: Original issued.

Jan 6, 1999 Changed MATRIX to SAMPLE TYPE. Changed G Sample Type from Groundwater toGround Water. Changed A Sample Type from Air Sample to Air. Changed P Sample Type from WipeSample to Wipe.

Page 7

APPENDIX B

Lancaster Laboratories -—3484 N«w Hoftad Pikf . Lawwasr, M 1 7W1 *3?4 (7 f7) 956-5350

C&stodySeal

Appendix CChain of Custody Flow Diagram

Lab personnel relinquish bottles with asignature on COC.

—Yes-»» See page 2.

No

Field personnel receive cooler fromcourier, sign the shipping paperwork,

and verify contents of the cooler.

Field personnel collect samples.

Field personnel enter sample ID on COC if not already present, enter dateand time of collection of sample on COC, enter remaining information(e.g., sample type, preservative) on COC if not already pre-printed onCOC, and enter their names on COC in Employee Sampling box (if

present on COC).

Field personnel pack cooler for shipment to the laboratory (i.e., addsufficient ice to maintain temperature of samples between 2-6°C and

attach custody seals to cooler and bottles, if applicable) and relinquishsamples to transporter's courier with signature, date, & time in first

available "Relinquished By" box.

If corrections are required, field personnel strikethrough the error and write the date and their

initials next to the line.

If corrections to COC are required aftersamples have been submitted to

laboratory, ADQM personnel documentthe error.

ADQM personnel send an e-mailmessage or the COC Exception Report

form to the person requesting thecorrection for his/her signature &

acknowledgment.

Person requesting correction sends ane-mail message or the signed COC

Exception Report form to ADQM to befiled.

Stop

5/18/2001 1 of 7 4017COC.vsd

Chain of Custody Flow Diagram

Lab personnel relinquishbottles with a signature

on COC.Yes»

Field personnel receivecooler(s) from courier andsign shipping paperwork.

—NO->

NO -Yes-

If someone other than fieldpersonnel is designated to

receive cooler, this person signsthe shipping paperwork and

holds cooler(s) until fieldpersonnel pick them up.

See page 1.Field personnel checkcontents of cooler(s)

against COC. Are contentscorrect/complete?

1YBS

No »Field personnel contactADQM personnel with

discrepancies.1* ADQM resolves problem(s)

with laboratory.

Field personnel sign and datethe COC in the first available

"Received By" box.

-Yes- Can field personnel collectall samples listed on COC?

-No-

Did field personnelcollect extra sample(s)not pre-printed on labrelinquished COC?

Field personnel collect samples withappropriate containers as listed onpre-printed COC, enter date andtime of collection of sample onCOC, and enter their names on

COC in Employee Sampling box (ifpresent on COC).

Are all samples in cooler listed onCOC to be shipped with cooler?

Yes

Any corrections to COC bottles andlabels needed?

Yes

Cross out error and date and initialnext to the crossed-out item.

See page 5.

Will field personneleventually collect

sample(s)?-NO-*

Yes4

Create derived COC.

Cross-out sample,dateout

and initial cross-and indicate

samplewhy

was notcollected.

1r

Stop

Field personnel write sample IDs of the samplescollected that day on derived COC in addition to

all other information pertaining to sample(parameters, preservation, etc.).

Field personnel reference derived COC # onoriginal COC in date/time box of sample

transcribed onto derived COC.

If no number on derived COC, field personnelassign one (i.e., original COC number-1).

Field personnel pack cooler (i.e., add sufficient ice tomaintain temperature of samples between 2-6°C and

attach custody seals to coolers and bottles, if applicable)and relinquish samples with a signature, date, and time

on derived COC in "Relinquished By" box.

See page 6.

5/18/2001 2 of 7 4017COC.vsd


Did field personnel collectextra sample(s) not pre-

printed on lab relinquishedCOC?

-Yes-Field personnel add extra sample(s)to a blank COC not relinquished by

laboratory personnel.

No

JLSee page 2.

Field personnel enter headerinformation, sample information (i.e.

bottle type, preservation method/analyte) to COC if not already

present.

Field personnel collect sample(s)into appropriate containers, enter

date and time of collection ofsample on COC, and enter their

names on COC in EmployeeSampling box

(if present on COC).

Are all samples in cooler listed onCOC to be shipped with cooler?

IYes

-No- See page 4.

Any corrections to COC/bottle label needed?

Yes

Cross out error and dateand initial next to the

crossed-out item.

Field personnel pack samples in cooler;(i.e., add sufficient ice to maintain

temperature of samples between 2-6°Cand attach custody seals to coolers andbottles, if applicable) relinquish sampleswith signature, date, and time on COC;

and ship to the laboratory.

Correction to COCrequired?

-Yes-

ADQM personnel document error in an email message or COC Exception Report formand send to person requesting correction.'

Requester reviews documentation and sends email message or COC ExceptionReport form to ADQM with signature.

ADQM files email message or COC Exception Report form in project file.

5/18/2001 3 of 7 4017COC.vsd


Continued from page 2. -Yes- Are all samples in cooler listed onCOC to be shipped with cooler?

No

Because sample has been moved toanother cooler, add comment "moved

sample to COC Y" (where Y is the uniqueCOC number located on the top right-handcomer of COC) to COC X, next to the pre-printed sample ID of the sample moved.

Add comment "moved sample from COCX" (where X is the unique COC numberloated on the top right-hand comer of

COC) COC Y next to the sample added.

Any corrections to COC orbottle label?

Yes

1

Cross out error and date and initial nextto the crossed-out item.

Field personnel pack samples in cooler(add sufficient ice to maintain temperature

of samples between 2-6°C and attachcustody seals to coolers and bottles, if

applicable); relinquish samples withsignature, date, and time in "Relinquished

By" box on COC; and ship samples tolaboratory.

Corrections to COCrequired?

-Yes-

ADQM personnel document error in an email message or COC ExceptionReport form and send to person requesting correction.

No

Requester reviews documentation and sends email message or COCException Report form to ADQM with, signature.


5/18/2001 4 of 7 4017COC.vsd


Continued from page 2.

Cross out error and date and initialnext to the crossed-out item. .

Field personnel pack samples in cooler (i.e., add sufficient iceto maintain temperature of sampler between 2-6°C and attachcustody seals to coolers and bottles, if applicable); relinquishsamples with signature, date, and time in "Relinquished By"

box on COC; and ship samples to laboratory.

Corrections to COCrequired?

IYes

I


Requester reviews documentation and sends email message or COCException Report form to ADQM with signature.


5/18/2001 5 of 7 4017COC.vsd



Field personnel pack cooler (i.e., add sufficient ice, tomaintain temperature of samples between 2-6°C and attach

custody seals to coolers and bottles, if applicable) andrelinquish samples with signature, date, and time on

derived COC in Relinquished By box.

Field personnel sendcooler(s) to laboratory-

Field personnel keep original pre-printed COC in field until they collect

all of the samples listed on COC.

Field personnel send original COCwith last shipment of samples, sign

the original COC in the next available"Relinquished By" box, and ship

cooler to laboratory.

Corrections to COCrequired? Stop

Yes


Requester reviews documentation and sends email message or COCException Report form to ADQM with signature.


5/18/2001 6 of 7 4017COC.vsd



Field personnel pack samples in cooler (i.e.,add sufficient ice to maintain temperature ofsamples between 2-6°C and attach custodyseals to coolers and bottles, if applicable)

relinquish samples with signature, date andtime on COC, and ship samples to

laboratory

Correction to COC required?

Yes

ADQM personnel document error inan email message or COC

Exception Report form and send toperson requesting correction.

Requestor reviews documentationand sends email message or COCException Report form to ADQM

with signature.

ADQM files email message or COCException Report form in project file.

5/18/2001 7 of 7 4017COC.vsd

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