Region 2 Field Operations Quality Procedures Standard Operating Procedure for Validation of Chlorinated Dibenzo-p-dioxins/Chlorinated Dibenzofurans (CDDs/CDFs) by High Resolution Superfund Methods (HRSM) Data SOP# QA-HWSS-A-013

SOP# QA-HWSS-A-013
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The table below identifies information about the reviews conducted of this Standard Operating
Procedure (SOP).

REVIEW HISTORY

Date

Reviewer Name

Changes Required [Y/N]

The table below identifies changes to this controlled document and the respective effective date(s)
over time.

REVISION HISTORY

Revision
Number

Revision Description

Effective Date

Original Issue

Note: Replaces SOPs HW-19 Rev. 1.1, [Data Validation for SW
846 Method 8290. Polychlorinated Dibenzodioxins (PCDDs)
and Polychlorinated Dibenzofurans (PCDFs) by High-
Resolution Gas Chromatography/High-Resolution Mass
Spectrometry (HRGC/HRMS)], December 2010

NOTICE

The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (USEPA) and other governmental employees. They do not constitute
rule-making by the USEPA and may not be relied upon to create a substantive or procedural right
enforceable by any other person. The Government may take action that is at a variance with the
policies and procedures in this Standard Operating Procedure (SOP).

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TABLE OF CONTENTS

1.0 PURPOSE AND APPLICABILITY 4

2.0 SUMMARY OF PROCESS OR METHODOLOGY 4

3.0 DEFINITIONS 4

4.0 RESPONSIBILITIES/QUALIFICATIONS 7

5.0 REFERENCES 8

6.0 PROCEDURAL STEPS 8

7.0 DATA AND RECORDS MANAGEMENT 10

8.0 QUALITY ASSURANCE AND QUALITY CONTROL 11

9.0 APPENDICES 11

Appendix A - Data Validation Criteria and Actions
Appendix B - Data Assessment Report Template
Appendix C - Definitions/Glossary of Terms
Appendix D- SOP Change Request Form

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1.0 PURPOSE AND APPLICABILITY

This document is designed to promote uniformity during review and validation of analytical
data generated through the USEPA Superfund High Resolution analytical services, High
Resolution Superfund Methods (HRSM02.1) Statement of Work (SOW) or its editorial revisions.
This SOW defines the analytical methods for the isolation, detection, and quantitative
measurement of Chlorinated Dibenzo-p-dioxins/Chlorinated Dibenzofurans (CDDs/CDFs) in
aqueous/water, soil/sediment, sludge, tissue (non-human), biosolids, ash, oil, and oily matrices
by High Resolution Gas Chromatography (HRGC) and High Resolution Mass Spectrometry
(HRMS).

The data validation guidelines presented in this document will aid in establishing (a) if data
meets the specific technical and quality control (QC) criteria established in the SOW, and (b) the
validity and extent of bias of any data not meeting the specific technical and QC criteria
established in the SOW. It must be understood by the user that acceptance of data not
meeting technical requirements is based upon many factors, including, but not limited to, site-
specific technical requirements, the need to facilitate the progress of specific projects, and the
availability for re-sampling. The user should note that while this document is to be used as an
aid in the formal data review process, the site-specific quality assurance project plan (QAPP), as
well as professional judgement, should also be used to determine the ultimate validity of data,
especially in those cases where all data does not meet specific technical criteria. Professional
judgment when used to qualify data including rejection of any data should be explained.

2.0 SUMMARY OF PROCESS OR METHODOLOGY

This document provides the criteria for performing technical quality assurance reviews of
Dioxins/Furans data generated through the Contract Laboratory Program (CLP). Criteria are
based on the quality assurance/quality control and technical requirements specified in Exhibit D
of HRSM02.1. This SOP incorporates much of the content of the National Functional Guidelines
(NFG) and provides additional guidance specific to EPA Region 2.

Upon receipt by EPA Region 2, CLP data in the Sample Delivery Group (SDG) undergoes a
technical quality assurance review based upon the criteria in this document. A report of this
review is prepared by the data validator, reviewed by the EPA Task Order Contracting Officer
Representative (TOCOR) when applicable, and provided to the data user.

3.0 DEFINITIONS

3.1. See Appendix C - Definitions/Glossary of Terms

3.2. Acronyms and Abbreviations

The following acronyms and abbreviations may be found throughout this document.

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Percent Difference

Percent Recovery

%R\

Percent Relative Intensity

%Resolution

Percent Resolution

%RSD

Percent Relative Standard Deviation

%Solids

Percent Solids, (also %S)

%Valley

Percent Valley

ASB

Analytical Services Branch

CCB

Continuing Calibration Blank

CCS

Contract Compliance Screening

CCV

Continuing Calibration Verification

CDD

Chlorinated Dibenzo-p-Dioxin

CDF

Chlorinated Dibenzofuran

Calibration Factor

Mean Calibration Factor (CF Bar)

CLP

Contract Laboratory Program

CLPSS

Contract Laboratory Program Support System

COC

Chain of Custody

CPS

Column Performance Solution

Calibration Standard

DAR

Data Assessment Report

DCB

Decachlorobiphenyl

Dilution Factor

Detection Limit

DQA

Data Quality Assessment

DQO

Data Quality Objectives

Data Validation

EDD

Electronic Data Deliverable

EDL

Estimated Detection Limit

EDM

EXES Data Manager

EMPC

Estimated Maximum Possible Concentration

EICC

Electronic Internal Chain of Custody

EICP

Extracted Ion Current Profile

EPA

Environmental Protection Agency (see also USEPA)

ESAT

Environmental Services Assistance Team

EXES

Electronic Data Exchange and Evaluation System

Gas Chromatography (or Chromatograph or Chromatographic)

HxCDD

Heptachlorinated Dibenzo-p-Dioxin

HxCDF

Heptachlorinated Dibenzofuran

HRGC

High Resolution Gas Chromatograph (or Chromatography)

HRMS

High Resolution Mass Spectrometry (or Spectrometer)

HRSM

High Resolution Superfund Methods

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HWSS

Hazardous Waste Support Section

IAR

Ion Abundance Ratio

ICAL

Initial Calibration

ICB

Initial Calibration Blank

ICV

Initial Calibration Verification

ISC

Isomer Specificity Check

LCS

Laboratory Control Sample

LCSD

Laboratory Control Sample Duplicate

LOC

Level of Chlorination

m/z

Mass-to-Charge Ratio

MDL

Method Detection Limit

Mass Spectrometry (or Spectrometer)

Matrix Spike (different from above depending on use)

MSD

Matrix Spike Duplicate

NFG

National Functional Guidelines

OCDD

Octachlorinated Dibenzo-p-Dioxin

OCDF

Octachlorinated Dibenzofuran

OSRTI

Office of Superfund Remediation and Technology Innovation

PCB

Polychlorinated Biphenyl

PDF

Portable Document Format

Performance Evaluation

PeCDD

Pentachlorinated Dibenzo-p-Dioxin

PeCDF

Pentachlorinated Dibenzofuran

PFK

Perfluorokerosene

Quality Assurance

QAPP

Quality Assurance Project Plan

Quality Control

Quantitation Limit

RPD

Relative Percent Difference

Relative Response

Mean Relative Response (RR Bar)

RRF

Relative Response Factor

RRF

Mean Relative Response Factor (RRF Bar)

RRT

Relative Retention Time

RRT

Mean Relative Retention Time (RRT Bar)

Retention Time

RSCC

Regional Sample Control Center Coordinator

RSD

Relative Standard Deviation

S/N

Signal-to-Noise Ratio

SAP

Sampling and Analysis Plan

SDG

Sample Delivery Group

SEDD

Staged Electronic Data Deliverable

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SI CP

Selected Ion Current Profile

SIM

Selected Ion Monitoring

SMO

Sample Management Office

SOP

Standard Operating Procedure

SOW

Statement of Work

SharePoint

TAL

Target Analyte List

TEF

Toxic Equivalency Factor

TEQ

Toxic Equivalent

TICP

Total Ion Current Profile

TOCOR

Task Order Contracting Officer Representative

TR/COC

Trip Report/Chain of Custody

USEPA

United Stated Environmental Protection Agency

WDM

Window Defining Mixture

WHO

World Health Organization

* The above list may contain abbreviations not used in CDDs/CDFs analysis. Please see National
Functional Guidelines for High Resolution Superfund Methods Data Review (HRSM02.1), EPA 540-R-
20-007, November 2020for additional details.

3.3. Data Qualifier Definitions

Data qualifier definitions are provided in the beginning of Appendix A.

4.0 RESPONSIBILITIES/QUALIFICATIONS

4.1. Qualifications

Data Validator must be familiar with the current CLP SOW, EDM and the documents
referenced in Section 5.0 below.

4.2. Responsibilities

4.2.1. EPA TOCOR (when applicable) - will review data assessments reports and other
deliverables prepared by contract data validators. They will update the MS Planner DV
Flowboard indicating the progress of SDGs, post final deliverables to the EDS
SharePoint site and send notification to clients via the established workflow.

4.2.2. Data Validator- will follow the criteria and actions provided in this document and
prepare Data Assessment Reports (DAR) and Summary Reports, as necessary. If the
validator is an ESAT contractor employee, they will consult the EPA TOCOR when
questions arise. They will update the DV Flowboard indicating progress of SDGs.

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5.0 REFERENCES

The Superfund High Resolution Analytical Services, High-Resolution Superfund Methods
(HRSM02.1) Statement of Work (SOW), available at the following website link:
https://www.epa.gov/clp/high-resolution-superfund-methods-hrsm021

National Functional Guidelines for HRSM Superfund Methods Data Review (HRSM 02.1), OLEM
9240.1-65, EPA 542-R-20-007, November 2020. This document can be obtained from the EPA's
Superfund Analytical Services and Contract Laboratory Program website at:

https://www.epa.gov/clp/superfund-clp-national-functional-guidelines-data-review

FA-0010.1, Standard Operating Procedure for Development and Use of Field SOPs, December
2015.

U.S. EPA, 2007. Guidance for the Preparation of Standard Operating Procedures (SOPs) for
Quality-Related Documents. EPA QA/G-6, EPA/600/B-07/001, April 2007.

QA-HWSS-A-001, Document Control Room, Data Dissemination and Archive Operations.
Revision 0, January 2021.

6.0 PROCEDURAL STEPS

6.1. EXES Processing

At the Sample Management Office (SMO) the data package and electronic data deliverables
(EDD) are checked for compliance with the CLP SOW. A Contract Compliance Screening
Report (CCS) is issued and posted on the SMO portal website. The EDD is processed
electronically to evaluate QC performance against the NFG and Region 2 criteria by EXES. An
electronic report of the EXES review is also posted on the SMO portal website.

6.2. Initial Notification

The EICC SharePoint web application is setup to send an e-mail alert notification to EPA and
ESAT data validators when a new data package is received and available for review and
validation. Entry of data into the EICC SharePoint site will automatically trigger an e-proxy
card to populate on the DV Flowboard in MS Planner.

Alternate electronic systems may be applied in the future.

6.3. DV Flowboard Updates

Update to DV Flowboard will be performed as per SOP QA-HWSS-A-001, Document Control
Room, Data Dissemination and Archive Operations (or most current version).

6.4. Data Package Inspection

The EXES Data Manager (EDM) is a useful tool in the data review process. EDM will identify
any missing and/or incorrect information in the data package. When available, the EDM

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should be reviewed as part of the initial data package inspection. The CLP laboratory may
submit a reconciliation package for any missing items or to correct the data. If there are any
concerns regarding the data package, contact the TOCOR.

An initial review of the data package is to be performed, taking into consideration all
information specific to the sample data package, (e.g., modified analysis requests, trip
report/chain-of-custody documentation, SDG narratives, etc.). The reviewer should also
have a copy of the Quality Assurance Project Plan (QAPP) or similar document for the
project for which the samples were analyzed. The criteria for data validation outlined in the
QAPP will supersede that in this SOP. The reviewer should access the HWSS SP Documents
Dashboard to obtain a copy of the relevant documents.

The SDGs or cases routinely have unique samples that require special attention from the
reviewer. These include field blanks, equipment blanks, trip blanks, and field duplicates
which must be identified in the sample records. The sampling records (i.e., trip reports or
COC records) should identify:

1) The Region where the samples were taken,

2) The case number,

3) The complete list of samples with the following information as applicable:

a. Sample matrix,

b. Field blanks (i.e., equipment, rinsate and trip),

c. Field duplicates,

d. Field spikes,

e. Shipping dates,

f. Preservatives, and

g. Laboratories involved

6.5. Data Review/Validation

The EXES electronic validation will apply most of the criteria and actions provided in
Appendix A. The data validator will examine the EXES report to identify any issues that
warrant further investigation. All EXES rejected data will be manually evaluated. The data
validator will use the criteria and actions in Appendix A, as well as their own professional
judgement to manually assess these data.

To use this SOP effectively, the reviewer should understand the analytical method. The
exact number of samples, their assigned numbers, their matrix, and the number of
laboratories involved in the analysis are essential information for the validator.

The Trip Report/Chain of Custody (TR/COC) documentation includes samples descriptions
and date(s) of sampling. The reviewer must consider lag times between sampling and start
of analysis when assessing technical sample holding times.

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The laboratory's SDG narrative is another source of general information. Notable problems
with matrices, insufficient sample volume for analysis or reanalysis, samples received in
broken containers, preservation and unusual events should be documented in the SDG
narrative. The reviewer should also inspect any email, telephone or any communication logs
detailing any discussion of sample or analysis issues between the laboratory, the CLP
Sample Management Office (SMO) and USEPA Region 2.

All data are initially marked as "Reportable" (YES) in EDM before validation is begun.
Sometimes, due to dilutions and/or re-analyses being performed, there may be multiple
results for a single analyte from a sample. The following criteria and professional judgement
are used to determine which result should be reported:

1) the analysis with the lower QL,

2) the analysis with the better QC results, and/or

3) the analysis with the higher result

Data validator will reconcile results from the multiple runs to provide results in one run and
report. The analyte values and their respective QLs are then transferred into a single sample
run. The runs and results that are not to be used are marked "not reportable" or entered
"NO" in the "Reportable" fields of the EDM.

6.6. Data Assessment Report

The data validator will prepare a Data Assessment Report (DAR) documenting the results of
their data review. This report will be formatted in accordance with the template provided in
Appendix B. Modifications to the template are allowed at the discretion of the user.

6.7. Summary Report

If requested by the client on the Analytical Request Form (ARF), the data validator will
prepare a Summary Report using the HWSS Summary Report application.

7.0 DATA AND RECORDS MANAGEMENT

7.1. DATA MANAGEMENT

Posting data to the SP EDS site is done in accordance with QA-HWSS-A-001, "Document
Control Room, Data Dissemination and Archive Operations".

7.2. RECORDS MANAGEMENT

The data files uploaded to the EDS SharePoint site include:

1) Data Assessment Report (Adobe PDF),

2) Edited/Validated Sample Summary Report from SMO portal (Adobe PDF),

3) Edited/Validated EQulS EDD report from SMO portal (MS Excel),

4) Generated Summary Report (MS Excel), if applicable, and

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5) Generated Summary Report with Hits Only (MS Excel), if applicable.

In addition to the above stated documents, data validator also forwards the following EXES
files, which are not uploaded to EDS SharePoint:

6) The CCS Report from the SMO Portal (Adobe PDF),

7) Edit History Report from the SMO Portal (Adobe PDF)

All files stated above are saved to the Local Area Network (LAN) G: drive at
DESADIV/HWSS/DATA VALIDATION/Site Name/Case #/SDG #. Files are renamed using the
following naming convention, Case#_SDG#_Filetype.*, e.g., 12345_PBAB12_S2AVEM.xlsx or
12345_BAB12-P_S2AVEM .xlsx.

Note: The letter in the beginning of the SDG name or appended as signifies that
the analyses are HRSMs. "M" in the file type signifies that the data has been manually
validated by ESAT and/or EPA Staff.

Additional records management procedures are discussed in QA-HWSS-A-001, "Document
Control Room, Data Dissemination and Archive Operations".

QUALITY ASSURANCE AND QUALITY CONTROL

1. This SOP will be reviewed annually. Reviews will be documented on the Review History
Table on page 2 of the SOP. The SOP shall be updated every 5 years, or more frequently,
when necessary, due to significant changes.

2. The "Request for SOP Change Form", Appendix D is used to document changes and is
appended to the final SOP until such time as the changes are incorporated into the body of
the text of the SOP.

APPENDICES

Appendix A - Data Validation Criteria and Actions

Appendix B - Data Assessment Report Template

Appendix C - Definitions/Glossary of Terms

Appendix D - SOP Change Request Form (CRF)

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Appendix A

Data Validation Criteria and Actions

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Data Validation Criteria and Actions Directions/Notes:

1. This SOP adopts data validation criteria and actions as stated in the National Functional
Guidelines for High Resolution Superfund Methods Data Review, OLEM 9240.1-65, EPA
542-R-20-007, November 2020. A link to this document is provided below:

https://www.epa.gov/sites/default/files/2021-

03/documents/nfg for hrsm superfund methods data review november 2020.pdf
Please refer to this document for details.

2. Data Validation qualifiers as applied by the Electronic Data Exchange and Evaluation
System (EXES) during Electronic Validation will be accepted. Data Validation Qualifier
Definitions are also provided in the table below.

Data Validation Qualifier Definitions

Data
Qualifier

Definition

The analyte was analyzed for but was not detected above the level of the adjusted
detection limit or quantitation limit, as appropriate.

The result is an estimated quantity. The associated numerical value is the
approximate concentration of the analyte in the sample.

J+

The result is an estimated quantity, but the result may be biased high.

J-

The result is an estimated quantity, but the result may be biased low.

The analyte was analyzed for but was not detected. The reported quantitation limit
is approximate and may be inaccurate or imprecise.

The data are unusable. The sample results are rejected due to serious deficiencies in
meeting QC criteria. The analyte may or may not be present in the sample.

3. Criteria, evaluation, quantitation limits (QLs), calculations, acceptable ranges and related
parameters and definitions are detailed in the applicable Statement of Work (SOW)
and/or National Functional Guidelines (NFG) documents referenced above.

4. Such criteria when available in the project specific quality assurance plan (QAPP)
document supersede SOW and/or NFG criteria. Such occurrences should be discussed
with TOCORs.

5. Although a "J+" or a "J-" may be seen as less ambiguous than a "J", the reviewer should
reserve the application of directional bias indicators to those situations when there is an
overwhelming influence in one direction. The exercise of professional judgment is critical,
especially in situations where ambiguity exists due to opposing factors, to objectively
interpret the effects of all factors.

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Appendix B
Data Assessment Report Template

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

REGION 2

LSASD/HWSB/HWSS

2890 Woodbridge Avenue, Edison, NJ 08837

EXECUTIVE NARRATIVE

Case No.:

Site:

Number of Samples:

Analysis:

QAPP:

Contractor:

Reference: DCN Number

SUMMARY OF DEFINITIONS:

Critical: Results have an unacceptable level of uncertainty and should not be used for making decisions.

Data have been qualified "R" rejected.

Major: A level of uncertainty exists that may not meet the data quality objectives for the project. A bias is likely to
be present in the results. Data has been qualified "J" estimated. "J+" and "J-" represent likely direction of the bias.

Minor: The level of uncertainty is acceptable. No significant bias in the data was observed.

Critical Findings:

Major Findings:

Minor Findings:

SDG No.:
Laboratory:
Sampling dates:
Validation SOP:

COMMENTS:

Reviewer Name(s):

Approver's Signature:

Name: Date:

Affiliation: USEPA/R2/LSASD/HWSB/HWSS

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Appendix C

Definitions/Glossary of Terms

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Definitions/Glossary of Terms*

Action Limit - A result for a Performance Evaluation (PE) sample that is outside the 99% (±3o) control
limits. The laboratory may be required to apply and document corrective actions to bring the
analytical results back into control.

Aliquot - A measured portion of a field sample, standard, or solution taken for sample preparation
and/or analysis.

Analyte - A chlorinated dibenzo-p-dioxin (CDD) or chlorinated dibenzofuran (CDF) tested for the
method in the Statement of Work (SOW).

Analysis Date/Time - The date and military time (24-hour clock) of the injection of the sample,
standard, or blank into the Gas Chromatograph/Mass Spectrometer (GC/MS) or GC system.

Analytical Sample - Any prepared field sample or extract thereof that is introduced into an
instrument for the purpose of measuring any target analyte. This definition excludes any instrument
quality control samples [e.g., standards associated with initial calibration, Continuing Calibration
Verification (CCV)], and tune verifications. The following are also defined as analytical samples:
diluted samples; Laboratory Control Samples (LCSs); LCS Duplicates (LCSDs); Performance Evaluation
(PE) samples; Preparation/Method Blanks; and Field Blanks (FBs).

Blank - An analytical sample that has negligible or unmeasurable amounts of a substance of interest.
The blank is designed to assess specific sources of contamination. Types of blanks may include
calibration blanks, instrument blanks, method blanks, and field blanks. See the individual definitions
for types of blanks.

Calibration Factor (CF) - A measure of the Gas Chromatographic response of a target analyte to the
mass injected.

Calibration Standards - A series of known standard solutions used by the analyst for calibration of
the instrument (i.e., preparation of the calibration curve). The solutions may or may not be subjected
to the preparation method but contain the same matrix (i.e., the same amount of reagents and/or
preservatives) as the sample preparations to be analyzed.

Case - A finite, usually predetermined number of samples collected over a given time period from a
particular site. Case Numbers are assigned by the Sample Management Office (SMO). A Case consists
of one or more Sample Delivery Groups (SDGs).

Chain of Custody (COC) Record - A sample identification form completed by the sampler, which
accompanies the sample during shipment to the laboratory and is used to document sample identity,
sample chain of custody, sample condition, and sample receipt by the laboratory.

Cleanup Standard - A standard containing either 37CU-2,3,7,8-TCDD or PCB-28L, PCB-111L, and PCB-
178L that is added to all extracts prior to cleanup. The purpose of this standard is to measure the
efficiency of the cleanup process.

Column Performance Solution (CPS) - When the Window Defining Mixture (WDM) and the Isomer
Specificity Check solutions are combined, the solution is identified as the CPS.

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Contamination - A component of a sample or an extract that is not representative of the
environmental source of the sample. Contamination may result from other samples, sampling
equipment, or from introduction while in transit, from laboratory reagents, from the laboratory
environment, or from analytical instruments.

Continuing Calibration Verification (CCV) - The mid-point calibration standard (CS3) that is used to
periodically verify that the instrument response factors developed during the initial calibration are
still valid.

Contract Compliance Screening (CCS) - A screening of electronic and hardcopy data deliverables for
completeness and compliance with the contract. This screening is performed under the U.S.
Environmental Protection Agency (EPA) direction by the Sample Management Office (SMO)
Contractor.

Contract Laboratory Program (CLP) - Supports the EPA's Superfund effort by providing a range of
state-of-the-art chemical analytical services of known and documented quality. This program is
directed by the Analytical Services Branch (ASB) of the Office of Superfund Remediation and
Technology Innovation (OSRTI) of the EPA.

Contractual Holding Time - The maximum amount of time that the Contract Laboratory Program
(CLP) laboratory may hold the samples from the sample receipt date until analysis and still be in
compliance with the terms of the contract, as specified in the United States Environmental Protection
Agency (EPA).

Control Limits - A range within which specified measurement results should fall to be compliant.
Control limits may be mandatory, requiring corrective action if exceeded, or advisory, requiring that
noncompliant data be flagged.

Data Package Narrative - Portion of the data package which includes laboratory information, and
sample identification, and descriptive documentation of any problems encountered in processing the
samples, along with corrective action taken and problem resolution.

Data Quality Assessment (DQA) - The scientific and statistical evaluation of environmental data to
determine if they meet the planning objectives of the project, and thus are of the right type, quality,
and quantity to support their intended use; refer to EPA QA/G-9R.

Data Quality Objectives (DQO) - Qualitative and quantitative statements that clarify technical and
quality objectives, define the appropriate type of data, and specify tolerable levels of potential
decision errors that will be used as the basis for establishing the quality and quantity of data needed
to support decisions.

Descriptor - A set of specific target analyte mass fragments monitored during a set timeframe.

Detection Limit (DL) - A generic term for the minimum measured concentration of a substance that
can be reported with a specified confidence that the measured concentration is distinguishable from
blank results. Includes Method Detection Limit (MDL), Limit of Detection (LOD), and other means of
establishing this limit.

Dry Weight - The weight of a sample based on percent solids. The weight after drying in an oven.

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EPA Regional CLP Contracting Officer's Representative (EPA Regional CLP COR) - The EPA official
who monitors assigned CLP laboratories (either inside or outside of the Regional CLP COR's respective
Region), responds to and identifies problems in laboratory operations, and participants in on-site
laboratory audits.

Estimated Detection Limit (EDL) - The concentration of an analyte required to produce a signal with
peak height of at least 3 times the background signal level. The EDL is calculated for each 2,3,7,8-
substituted and World Health Organization (WHO) Toxic congener for which the response of the
primary and secondary ions is less than 3 times the background level. Note that some programs
define EDL as the amount of analyte required to produce a signal with a signal-to-noise ratio of at
least 2.5.

Estimated Maximum Possible Concentration (EMPC) - The EMPC is calculated for analytes for which
the quantitation and/or confirmation ion(s) has signal to noise in excess of 3, but does not meet the
ion ratio identification criteria.

Field Blank (FB) - A blank used to provide information about contaminants that may be introduced
during sample collection, shipment, storage, and/or preparation and analysis in the laboratory.
Examples of field blanks include trip blanks, rinse blanks, bottle blanks, equipment blanks,
preservative blanks, decontamination blanks, etc.

Field Duplicate - A duplicate sample generated in the field, not in the laboratory.

Field Quality Control (QC) - Any QC samples submitted from the field to the laboratory. Examples
include, but are not limited to, field blanks, and field duplicates.

Field Sample - A portion of material received from the field to be analyzed for analytes of interest.

Gel Permeation Chromatography (GPC) - A size-exclusion chromatographic technique that is used as
a cleanup procedure for removing large organic molecules, particularly naturally occurring macro-
molecules such as lipids, polymers, viruses, etc.

Homologue - A group of compounds that have the same molecular weight, but not necessarily the
same structural arrangement.

Initial Calibration - Analysis of analytical standards at a series of different concentrations; used to
define the quantitative response, linearity, and dynamic range of the instrument to target analytes.

Initial Calibration Verification (ICV) - Analysis of the calibration standard from an alternate source or
a different lot than that used for the initial calibration (ICAL) standards at the mid-point CS3
concentration of the ICAL standards to ensure the instrument is calibrated accurately.

Instrument Blank - A blank designed to determine the level of contamination either associated with
the analytical instruments or resulting from carryover.

Internal Standard - For chlorinated dibenzo-p-dioxins and dibenzofurans (CDD/CDF), a chemical
compound (usually isotope-labeled) that is used as a reference for quantitation of target chemical
compounds in a sample.

Internal Standard Quantitation - A means of determining the concentration of a target analyte using
a standard that is added to the sample just prior to analysis. In the context of the high resolution Gas

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Chromatography/Mass Spectrometry (GC/MS) methods, internal standard quantitation is applied to
determine the amount recovered, after sample preparation and clean-up, of the labeled compounds
added to the samples prior to initial preparation, that are used for isotope dilution quantitation.

Isomer - Chemical compounds that have the same molecular formula but differ in structural
arrangement and properties.

Isotope Dilution Quantitation - A means of determining the concentration of a target analyte using a
standard that is added to the sample prior to any sample preparation steps. It utilizes isotopically
labeled compounds that are chemically as similar as possible to each target analyte (i.e., a labeled
analog) to mimic the response of the analyte to sample preparation steps, thereby accounting for any
related losses.

Labeled Compounds - Carbon-13 isotopically-labeled compounds that are added to every sample and
are present at the same concentration in every blank, Quality Control (QC) sample, and calibration
solution in the high resolution Gas Chromatography/Mass Spectrometry (GC/MS) methods for the
purpose of measuring recovery or for quantitation.

Laboratory Control Sample (LCS) - A reference matrix spiked with target analytes at a known
concentration. LCSs are analyzed using the same sample preparation, reagents, and analytical
methods employed for the samples received.

Laboratory Control Sample Duplicate (LCSD) - A duplicate of the LCS prepared and analyzed to
measure laboratory precision.

m/z Ratio - The ratio of mass to charge of a charged particle; used in mass spectrometry to focus
specific charged fragments of target analytes on the detector. This specificity is obtained by varying
the electric and magnetic field strengths. Mass-to-charge ratio is synonymous with "m/e".

Mass Resolution - The ability of a mass spectrometer to distinguish the difference between two
charged particles with different mass-to-charge ratios.

Matrix - The predominant material of which the sample to be analyzed is composed. For the purpose
of this document, the sample matrices are aqueous/water, soil/sediment, ash, tissue (non-human),
oil, and biosolids.

Matrix Effect - In general, the effect of a particular matrix on the constituents under study. Matrix
effects may prevent extraction of target analytes. Matrix effects may prevent extraction of target
analytes, may affect purging/extraction efficiencies, and consequently affect Deuterated Monitoring
Compound (DMC)/surrogate recoveries and cause interference for the qualitative and quantitative
analyses of the target analytes.

Matrix Spike (MS) - Aliquot of the sample (aqueous/water or soil/sediment) fortified (spiked) with
known quantities of specific compounds and subjected to the entire analytical procedure to indicate
the appropriateness of the method for the matrix by measuring recovery.

Matrix Spike Duplicate (MSD) - A second aliquot of the same sample as the Matrix Spike (MS)

(above) that is spiked in order to determine the precision of the method.

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Method Blank - A clean reference matrix sample (e.g., reagent water, silica sand, or corn oil) spiked
with labeled compounds and labeled internal standards and carried throughout the entire analytical
procedure to determine whether contamination of any target analytes is introduced during
processing and analysis of samples.

Method Detection Limit (MDL) - The minimum measured concentration of a substance that can be
reported with 99% confidence such that the measured concentration is distinguishable from method
blank results.

Percent Difference (%D) - The difference between two values calculated as a percentage of one of
the values.

Percent Solids (%Solids) - The proportion of solid in a soil/sediment sample determined by drying an
aliquot of the sample.

Percent Relative Standard Deviation (%RSD) - The Percent Relative Standard Deviation is calculated
from the standard deviation and mean measurement of either Relative Response Factors (RRFs) or
Calibration Factors (CFs) from initial calibration standards. Percent Relative Standard Deviation
indicates the precision of a set of measurements.

Perfluorokerosene (PFK) - A mixture of compounds used to calibrate the exact m/z scale in the High
Resolution Mass Spectrometer (HRMS).

Performance Evaluation (PE) Sample - A sample prepared by a third party at known concentrations
that are unknown to the analytical laboratory and is provided to test whether the laboratory can
produce analytical results within specified performance limits.

Preparation Log - A record of sample preparation (e.g., extraction, cleanup) at the laboratory.

Quality Assurance Project Plan (QAPP) - A formal document describing the management policies,
objectives, principles, organizational authority, responsibilities, accountability, and implementation
plan of an agency, organization, or laboratory for ensuring quality in its products and utility to its
users.

Quantitation Limit - The minimum level of acceptable quantitation that is supported by the analysis
of standards.

Raw Data - The originally recorded and unprocessed measurements from any measuring device such
as analytical instruments, balances, pipettes, thermometers, etc. Reported data are processed raw
measurement values that may have been reformatted from the original measurement to meet
specific reporting requirements such as significant figures and decimal precision.

Reconstructed Ion Chromatogram (RIC) - A mass spectral graphical representation of the separation
achieved by a Gas Chromatograph (GC); a plot of total ion current versus Retention Time (RT).

Relative Percent Difference (RPD) - The absolute value of the relative difference between two values
normalized to the mean of the two values expressed as a percentage.

Relative Response (RR) - A measure of the detector response of the native analyte compared to its
labeled compound analog. RRs are determined using the area responses of both the primary and
secondary exact m/z for each compound in each calibration standard.

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Relative Response Factor (RRF) - The ratio of the response of a given compound to its corresponding
internal standard. Response factors are determined using the area responses of both the primary and
secondary exact m/z for each compound in each calibration standard.

Relative Retention Time (RRT) - The ratio of the retention time of an analyte to the retention time of
its associated internal standard. RRT is a unitless quantity.

Relative Standard Deviation (RSD) - The standard deviation times 100 divided by the mean. Also
termed "coefficient of variation".

Resolution - Also termed Separation or Percent Resolution, the separation between peaks on a
chromatogram, calculated by dividing the depth of the valley between the peaks by the peak height
of the smaller peak being resolved, multiplied by 100.

Retention Time (RT) - The time a target analyte is retained on a Gas Chromatograph (GC) column
before elution. The identification of a target analyte is dependent on a target analyte's retention time
falling within the specified retention time window established for that analyte. The RT is dependent
on the nature of the column's stationary phase, column diameter, temperature, flow rate, and other
parameters.

Sample - A portion of material to be analyzed that is contained in single or multiple containers and
identified by a unique sample number.

Sample Delivery Group (SDG) - A unit within a sample Case that is used to identify a group of
samples for delivery. An SDG is defined by the following, whichever is most frequent:

• Each 20 field samples [excluding Performance Evaluation (PE) samples] within a Case; or

• Each 7-calendar day period (3 calendar day period for 7-day turnaround) during which field
samples in a Case are received (said period beginning with the receipt of the first sample in
theSDG).

• All samples scheduled with the same level of deliverables.

• In addition, all samples and/or sample fractions assigned to an SDG must be scheduled under
the same contractual turnaround time. Preliminary Results have no impact on defining the
SDG.

• Samples may be assigned to SDGs by matrix (i.e., all soil/sediment samples in one SDG, all
aqueous/water samples in another) at the discretion of the laboratory. Laboratories shall take
all precautions to meet the 20-sample per SDG criteria.

Sample Management Office (SMO) - A Contractor-operated facility operated under the SMO
contract, awarded, and administered by the EPA.

Sample Number (EPASample Number)-A unique identification numberdesignated bythe EPA to
each sample. An EPA Sample Number appears on the Traffic Report/Chain of Custody (TR/COC)
Record which documents information on that sample.

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SDG Narrative - Portion of the data package which includes laboratory, contract, Case, and sample
number identification, and descriptive documentation of any problems encountered in processing the
samples, along with corrective action taken and problem resolution.

Sampling and Analysis Plan (SAP) - A document which specifies the procedural and analytical
requirements for one-time, or time-limited, projects involving the collection of water, soil, sediment,
or other samples taken to characterize areas of potential environmental contamination.

Sample Identifier - A unique identification number that appears on the Chain of Custody (COC)
Records or sampling forms which document information for a sample.

Selected Ion Current Profile (SICP) - The line described by the signal at an exact m/z.

Select Ion Monitoring (SIM) - A mode of Mass Spectrometry (MS) operation in which specific m/z
ratios are monitored, as opposed to scanning the entire mass range.

Signal-to-Noise Ratio (S/N) - The height of the signal as measured from the mean (average) of the
noise to the peak maximum divided by the width of the noise.

Statement of Work (SOW) - A document which specifies how laboratories analyze samples under a
contract, such as the Contract Laboratory Program (CLP) analytical program.

Storage Blank - Reagent water (two 40.0 mL aliquots) or clean sand stored with volatile samples in a
Sample Delivery Group (SDG). It is analyzed after all samples in an SDG have been analyzed. It is used
to determine the level of contamination acquired during storage.

Target Analyte List (TAL) - A list of analytes designated by the Statement of Work (SOW) for analysis.

Technical Holding Time - The maximum length of time that a sample may be held from the collection
date until extraction and/or analysis.

Toxic Equivalency Factor (TEF) - An estimate of the toxicity of a specific congener relative to 2,3,7,8-
tetrachlorodibenzo-p-dioxin.

Toxic Equivalent Quantity (TEQ) - The product of the concentration of each individual World Health
Organization (WHO) toxic 2,3,7,8-substituted dibenzo-p-dioxin and dibenzofuran multiplied by their
respective Toxic Equivalency Factors (TEFs).

Traffic Report/Chain of Custody Record (TR/COC) - An EPA sample identification form completed by
the sampler, which accompanies the sample during shipment to the laboratory and is used to
document sample identity, sample chain of custody, sample condition, and sample receipt by the
laboratory.

Trip Blank - A blank used to provide information about contaminants that may be introduced during
sample transport.

Warning Limit - A result for a Performance Evaluation (PE) sample that is outside the 95% (±2o)
control limits. The laboratory should apply and document corrective actions to bring the analytical
results back into control.

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Window Defining Mixture (WDM) - Prior to analyzing the calibration solutions, blanks, samples, and
Quality Control (QC) samples, the WDM is analyzed to evaluate descriptor switching times.

*The above list is all inclusive and may contain terms not applicable to Chlorinated Dibenzo-p-dioxins/

Chlorinated Dibenzofurans (CDDs/CDFs) Analysis.

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Appendix D
SOP Change Request Form (CRF)

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REQUEST FOR SOP CHANGE

Requestor
Name:

Date of
Initiation:

Dept.:

SOP#:

Revision #:

Date:

SOP Title:

Please Check One

MINOR REVISION

MAJOR REVISION

CHANGE(S) (Use attachment if necessary):

CHANGE FROM:

CHANGE TO:

REASON(S) FOR CHANGE(S):

APPROVAL

NAME:

Signature/Date

EPA Branch Chief /
Section Chief/Team
Leader

EPA TOCOR

REQUESTOR

Effective Date

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