SOP# QA-HWSS-A-012
Revision No.: 0
Effective Date: 03/01/22

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| \ U.S. Environmental Protection Agency, Region 2
1 ^1^ / Field Operations Quality Procedures

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ADMINISTRATIVE STANDARD OPERATING PROCEDURE

Standard Operating Procedure for Validation of Cyanide Data

Effective Date

Number

3/1/2022

QA-HWSS-A-012

Author

Name:

Kim Brandon-Bazile





Title:

Chemist





Division/Branch/Section: LSASD/HWSB/HWSS

Signature:

Digitally signed by Brandon-Bazile,

Brandon-Bazile, Kim k™

nat-p- ?n?? n? ik -rm'nrv

Date: 2/16/2022

Review & Approvals

Name:

Narendra Kumar





Title:

Chemist, HWSS





Signature:

NARENDRA KUMAR

Date:

Name:

Donna Ringel





Title:

Chief, HWSS





Signature:

HHMMA DIM^CI Digitally signed by DONNA RINGEL

UU INI INI A K I INI O 11_ Date: 2022.02.16 15:34:51 -0500'

Date:

Name:

Jon Gabry





Title:

Chief, HWSB





Signature:

|/"\|V| r Anny Digitally signed by JON GABRY
J\-/IM vjMDIx I Date: 2022.02.16 15:45:00-05'00'

Date:

Name:

Title:

Signature:

Date:

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SOP# QA-HWSS-A-012
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The table below identifies information about the reviews conducted of this 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

0

Original Issue

(Note: Replaces CN DV in SOP HW-3c, Rev. 1 Mercury and
Cyanide Data Validation, September 2016)







































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	6

5.0 REFERENCES	6

6.0 PROCEDURAL STEPS	7

7.0 DATA AND RECORDS MANAGEMENT	9

8.0 QUALITY ASSURANCE AND QUALITY CONTROL	10

9.0 APPENDICES	10

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 of data review of analytical data generated
through the US EPA Contract Laboratory Program (CLP) Statement of Work (SOW) for
Superfund Analytical Methods SFAM01.1 and any future editorial revisions of SFAM01.1. It is
applicable to the review of Contract Laboratory Program (CLP) data of various matrices (water,
soil, sediment, waste, wipes, etc.) generated using Spectrophotometric Technique for Total
Cyanide analyses.

The 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 do not meet specific technical criteria.

2.0 SUMMARY OF PROCESS OR METHODOLOGY

This document provides the criteria for performing technical quality assurance reviews of
inorganic (cyanide) data generated by the CLP. Criteria are based on the quality
assurance/quality control and technical requirements specified in Exhibit D of SOW SFAM01.1.
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 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), 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 are applicable to this document.

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%D

Percent Difference

%R

Percent Recovery

%R\

Percent Relative Intensity

%RSD

Percent Relative Standard Deviation

%Solids

Percent Solids, (also %S)

ASB

Analytical Services Branch

CCB

Continuing Calibration Blank

CCS

Contract Compliance Screening

CCV

Continuing Calibration Verification

CLP

Contract Laboratory Program

CLPSS

Contract Laboratory Program Support System

DAR

Data Assessment Report

DF

Dilution Factor

DL

Detection Limit

DV

Data Validation

EDD

Electronic Data Deliverable

EDM

EXES Data Manager

EDS

Environmental Data Services

EICC

Electronic Internal Chain of Custody

EPA

Environmental Protection Agency (see also USEPA)

ESAT

Environmental Services Assistance Team

EXES

Electronic Data Exchange and Evaluation System

HWSS

Hazardous Waste Support Section

ICB

Initial Calibration Blank

ICS

Interference Check Sample

ICV

Initial Calibration Verification

LCS

Laboratory Control Sample

LEB

Leachate Extraction Blank

MDL

Method Detection Limit

MS

Matrix Spike

NFG

National Functional Guidelines

OSRTI

Office of Superfund Remediation and Technology Innovation

PDF

Portable Document Format

QA

Quality Assurance

QAPP

Quality Assurance Project Plan

QC

Quality Control

QL

Quantitation Limit

RPD

Relative Percent Difference

RSCC

Regional Sample Control Center Coordinator

SAP

Sampling and Analysis Plan

SDG

Sample Delivery Group

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SEDD

Staged Electronic Data Deliverable

SMO

Sample Management Office

SOP

Standard Operating Procedure

SOW

Statement of Work

SP

SharePoint

SPLP

Synthetic Precipitation Leaching Procedure

TCLP

Toxicity Characteristic Leaching Procedure

TDS

Total Dissolved Solids

TOC

Total Organic Carbon

TOCOR

Task Order Contracting Officer Representative

TR/COC

Traffic Report/Chain of Custody

TSS

Total Suspended Solids

USEPA

United States Environmental Protection Agency

3.3. Data Qualifier Definitions

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

4.0 RESPONSIBILITIES/QUALIFICATIONS

4.1.	Qualifications

Data Validators 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.

5.0 REFERENCES

National Functional Guidelines for Inorganic Superfund Methods Data Review, EPA 540-R-20-

006, November 2020.

Contract Laboratory Program (CLP) Statement of Work (SOW) Superfund Analytical Method

(SFAM) SFAM01.1

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

2015.

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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 web site. 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

Updates to the 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
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

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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 blank, 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 the data.

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

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

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, or telephone/communication logs

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detailing any discussion of sample or analysis issues between the laboratory, the CLP
Sample Management Office 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 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, 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

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

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In addition to the above stated documents, data validators also forward the following EXES
files, which are not uploaded to the 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_MBAB12_S3VEM.xlsx or
12345_BAB12-M_S3VEM .xlsx.

Note: The letter "M" in the beginning of the SDG name or appended as "-M" signifies that
the analyses are inorganic. "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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TABLE OF CONTENTS

I.	DATA QUALIFIER DEFINITIONS	13

CYANIDE Table 1. Data Qualifier Definitions	13

II.	PRESERVATION AND HOLDING TIMES	14

CYANIDE Table 2. Preservation and Holding Times Actions	14

III.	CALIBRATION	15

CYANIDE Table 3. Calibration Actions	16

IV.	BLANKS	16

CYANIDE Table 4. Blanks Actions	17

V.	LABORATORY DUPLICATE SAMPLE ANALYSIS	19

CYANIDE Table 5. Laboratory Duplicate Sample Actions	20

VI.	SPIKE SAMPLE ANALYSIS	20

CYANIDE Table 6. Spike Sample Actions	21

VII.	FIELD DUPLICATES	22

CYANIDE Table 7. Field Duplicate Actions	23

VIII.	TARGET ANALYTE QUANTITATION	23

CYANIDE Table 8. Target Analyte Quantitation Percent Solids of Sediment Actions	24

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I. Data Qualifier Definitions

The following table provides brief explanations of the qualifiers assigned to results during the data
review process. The reviewer should use these qualifiers as applicable.

Cyanide Table 1. Data Qualifier Definitions

Data
Qualifier

Definition

U

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

J

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.

UJ

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

R

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.

NOTES:

1.	Comments for sample results with data qualifiers other than "U" or no qualification based
on professional judgement must be included in the DAR.

2.	With familiarity of project data objectives and/or consultation with project staff, the
reviewer should be able to refine the use of data qualifiers to avoid ambiguity. For example,
if critical site decisions are to be made based on the data, the reviewer may decide to apply
an "R" qualifier rather than a "UJ".

3.	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.

4.	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.

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II. Preservation and Holding Times

A.	Review Items

Laboratory Results Reports, sampling documentation [e.g., Chain of Custody (COC) Records],
sample receipt forms, sample preparation logs, raw data, and narrative in the data package,
checking for: pH, shipping container temperature, holding time, and other sample conditions.

B.	Objective

The objective is to determine the validity of the analytical results based on the sample shipping
and storage conditions and the holding time of the sample.

C.	Action:

1.	Refer to Cyanide Table 2 below for the evaluation criteria and corresponding actions for
detected and non-detected target analyte results in the deficient samples. Apply the actions
to each field sample and field blank for which the preservation or holding time criteria was
not met.

2.	If a discrepancy is found between the sample analysis dates on the Laboratory Results
Reports and in the raw data, perform a more comprehensive review to determine the
correct date to be used to establish the holding time.

3.	When the holding times are exceeded, the reviewer should comment in the DAR on any
possible consequences for the analytical results.

4.	When holding times are grossly exceeded, note it for Contract Laboratory Program
Contracting Officer Representative (CLP COR) action.

Cyanide Table 2. Preservation and Holding Times Actions

Criteria

Action

Detect

Non-detect

Aqueous/water samples received with oxidizing agents
present

J

R

Aqueous/water samples received with sulfides present

J

R

Aqueous/water samples received with nitrate/nitrite
present and not treated with sulfamic acid

J

R

Aqueous/water samples received with pH < 10

J

R

Aqueous/water and soil/sediment/waste samples
received or stored at a temperature > 6°C but < 10°C

J

UJ

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Aqueous/water and soil/sediment/waste samples
received or stored at a temperature > 10°C*

J-

R

Technical Holding Time:

Aqueous/water samples and SPLP leachates > 14 days

J

R

Technical Holding Time:
Soil/sediment/waste samples > 14 days

J

R

Samples properly preserved and analyzed within specified
holding time

No qualification

No qualification

* For samples received with shipping container temperatures > 109C, the QAPP or the project-
specific Standard Operating Procedures (SOPs) for data review may allow the use of higher
temperature criteria before assessing any actions for the affected samples.

III. Calibration

A.	Review Items

Laboratory initial calibration and calibration verification reports (if available), preparation logs,
calibration standard logs, instrument logs, instrument printouts, and raw data in the data
package.

B.	Objective

The objective is to determine the validity of the analytical results based on initial calibration
and calibration verification.

C.	Action:

Refer to Cyanide Table 3 below for the evaluation criteria and corresponding actions for
detected and non-detected cyanide results in the samples associated with deficient initial
calibrations or calibration verification standard.

1.	For initial calibrations or ICV standard analyses that do not meet the technical criteria, apply
the actions to all associated samples reported from the analytical sequence.

2.	For CCV standards analyses that do not meet the technical criteria, apply the actions to all
samples analyzed between a previous technically acceptable analysis of the QC sample and
a subsequent technically acceptable analysis of the QC sample in the analytical sequence.

3.	If the instrument was not calibrated with at least the minimum number of standards, or if
the calibration curve does not include standards at required concentrations (e.g., a blank
and at least one at or below the QL but above the MDL), qualify detects as estimated (J) or
unusable (R), and non-detects as estimated (UJ) or unusable (R).

NOTE: For critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.

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Cyanide Table 3. Calibration Actions

Criteria

Action

Detect

Non-detect

Calibration not performed or not performed at specified
frequency

R

R

Calibration incomplete (insufficient number of standards
or required concentrations missing)

J

UJ

For linear fits, the correlation coefficient < 0.995

J

UJ

%D outside ± 30%; or other specified statistical test values
outside limits

J

UJ

Calibration Standards and ICV/CCV not distilled

J

UJ

ICV/CCV not performed at specified frequency

J

UJ

ICV/CCV %R < 70%

R

R

ICV/CCV %R 70 - 84%

J

UJ

ICV/CCV %R 85 -115%

No qualification

No qualification

ICV/CCV %R 116 -130%

J

No qualification

ICV/CCV %R > 130%

J+

No qualification

Instrument blank analyzed prior to CCV

Use
professional
judgment

Use
professional
judgment

IV. Blanks

A.	Review Items

Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument
logs, and raw data in the data package, and sampling trip reports.

B.	Objective

The objective is to determine the validity of the analytical results based on the blank responses
by determining the existence and magnitude of contamination resulting from laboratory (or
field) activities or baseline drift during analysis.

C.	Action:

Refer to Cyanide Table 4 below for the evaluation criteria and corresponding actions for
detected and non-detected cyanide results in the samples associated with deficient blanks.

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1.	For ICB analyses that do not meet the technical criteria, apply the actions to all associated
samples reported from the analytical sequence.

2.	For CCB analyses that do not meet the technical criteria, apply the actions to all associated
samples analyzed between a previous technically acceptable analysis of the CCB and a
subsequent technically acceptable analysis of the CCB in the analytical sequence.

3.	For Preparation Blank analyses that do not meet the technical criteria, apply the actions to
all associated samples prepared in the same preparation batch. For LEBs that do not meet
the technical criteria, apply the actions to all associated samples extracted in the same
extraction batch.

4.	Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. In instances where more than one blank is associated with a given sample,
qualification should be based upon a comparison with the associated blank having the
highest concentration of contaminant.

5.	If the absolute value of an ICB or a CCB result is > QL, the analysis should have been
terminated and the affected samples re-analyzed. If samples were not re-analyzed, qualify
as described in Table 4 below.

6.	All samples associated with the Preparation Blank with concentrations < lOx the
Preparation Blank concentration and > QL should have been redigested and reanalyzed. If
the associated samples were not redigested and reanalyzed, qualify as described in Table 4
below.

7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be
checked against a less dilute analysis and reported from that analysis. However, if no less-
dilute analysis is reported, use professional judgment to decide whether to report from the
dilution.

8.	For blank results < (-MDL) but > (-QL), the possibility of false negative exists.

NOTE: Do not qualify blanks with blank results. The blank analyses may not involve the same
weights, volumes, or dilution factors as the associated samples. In particular,
soil/sediment or waste sample results reported in the Laboratory Results Reports will
not be on the same basis (units, dilution) as the calibration blank data. It may be easier
to work with the raw data and/or convert the ICB or CCB results to the same units as the
soil/sediment or waste samples for comparison purposes.

Cyanide Table 4. Blanks Actions

Blank Type

Blank Result

Sample Result

Action for Samples

ICB/CCB

Not analyzed at
the specified
frequency

Non-detect

UJ

Detect

J

ICB/CCB

Not distilled

Detect or non-detect

Use professional judgement

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ICB/CCB

Detect < QL

Non-detect

No qualification

Detect < QL

Report at QL and qualify U

>QL

No qualification

ICB/CCB

< (-MDL) but
> (-QL)

Non-detect

UJ

Detect

No qualification

ICB/CCB

>QL

Non-detect

No qualification

Detect < QL

Report at QL and qualify U

> QL but < ICB/CCB Result

Report at ICB/CCB Result
and qualify U

> ICB/CCB Result

No qualification

ICB/CCB

< (-QL)

Non-detect

UJ

Detect < QL

J-

> QL but < lOx QL

J-

> lOx QL

No qualification

Preparation
Blank/LEB

Not analyzed at

specified

frequency

Non-detect

UJ

Detect

J

Preparation
Blank/LEB/
Field Blank/
Rinse Blank

Detect < QL

Non-detect

No qualification

Detect < QL

Report at QL and qualify U

>QL

No qualification

Preparation
Blank/LEB/
Field Blank/
Rinse Blank

< (-MDL) but
> (-QL)

Non-detect

UJ

Detect

No qualification

Preparation
Blank/LEB/
Field Blank/
Rinse Blank

>QL

Non-detect

No qualification

Detect < QL

Report at QL and qualify U

> QL but < the PB/LEB/FB/RB
Result

Report at PB/LEB/FB/RB
Result and qualify U

> PB/LEB/FB/RB Result but
< lOx the PB/LEB/FB/RB
Result

Report at Sample Result and
qualify J+

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> lOxthe Preparation
Blank/LEB/Field Blank/Rinse
Blank Result

No qualification

Preparation
Blank/LEB/
Field Blank/
Rinse Blank

< (-QL)

Non-detect

UJ

Detect < QL

J-

> QL but < lOx QL

J-

> lOx QL

No qualification

V. Laboratory Duplicate Sample Analysis

A.	Review Items

Data Package Cover Page, laboratory duplicate reports (if available), preparation logs,
instrument printouts, and raw data in the data package.

B.	Objective

The objective of the laboratory duplicate sample analysis is to demonstrate acceptable method
precision by the laboratory at the time of analysis.

C.	Action:

Refer to Cyanide Table 5 below for the evaluation criteria and corresponding actions for
detected and non-detected cyanide results in the samples associated with deficient duplicates.

1.	For a laboratory duplicate sample analysis that does not meet the technical criteria, apply
the actions to the field sample used to prepare the duplicate sample only. Exercise
professional judgment in determining sample similarity when making use of all available
data, including site and sampling documentation (e.g., location and type of sample,
descriptive data, soil classification); field test data (e.g., pH, Eh, conductivity, chlorine); and
laboratory data for other parameters [e.g., Total Suspended Solids (TSS), Total Dissolved
Solids (TDS), Total Organic Carbon (TOC), alkalinity or buffering capacity, reactive sulfide,
anions]. Additionally, use the sample data (e.g., similar concentrations of analytes) in
determining similarity between samples in the data package. Two possible determinations
are: 1) all of the samples are considered sufficiently similar to the duplicate sample and all
samples should be qualified; or 2) only some of the samples in the data package are similar
to the duplicate sample, and that only these samples should be qualified.

2.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem. Do not calculate RPD when both values are non-detects.

NOTE: The laboratory duplicate analysis is not required for wipe nor air filter samples.

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Cyanide Table 5. Laboratory Duplicate Sample Actions

Criteria

Action

Detect

Non-detect

Laboratory duplicate analysis not performed at the
specified frequency

J

UJ

Aqueous: Both original sample and duplicate sample
results are > 5x QL and 20% < RPD < 100%

J

NA

Soil/Sediment: Both original sample and duplicate sample
results are > 5x QL and 35% < RPD < 100%

J

NA

Aqueous: Both original sample and duplicate sample
results are > 5x QL and RPD < 20%

No qualification

No qualification

Soil/Sediment: Both original sample and duplicate sample
results are > 5x QL and RPD < 35%

No qualification

No qualification

Both original sample and duplicate sample results are > 5x
QL and RPD > 100%

R

NA

Original sample or duplicate sample result < 5x QL
(including non-detects) and absolute difference between
sample and duplicate > QL

J

UJ

Original sample or duplicate sample result < 5x QL
(including non-detects) and absolute difference between
sample and duplicate < QL

No qualification

No qualification

VI. Spike Sample Analysis

A.	Review Items

Data Package Cover Page, laboratory matrix spike reports (if available), preparation logs,
instrument printouts, and raw data in the data package.

B.	Objective

The objective of the spiked sample analysis is to evaluate the effect of each sample matrix on
the sample preparation procedures and the measurement methodology.

C.	Action:

Refer to Cyanide Table 6 below for the evaluation criteria and corresponding actions for
detected and non-detected target and spike analyte results in the samples associated with
deficient matrix spikes.

1. For a matrix spike sample analysis that does not meet the technical criteria, apply the
actions only to the field sample used to prepare the Matrix Spike sample. Exercise

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professional judgment in determining sample similarity when making use of all available
data, including site and sampling documentation (e.g., location and type of sample,
descriptive data, soil classification); field test data (e.g., pH, Eh, conductivity, chlorine); and
laboratory data for other parameters [e.g., Total Suspended Solids (TSS), Total Dissolved
Solids (TDS), Total Organic Carbon (TOC), alkalinity or buffering capacity, reactive sulfide,
anions]. Additionally, use the sample data (e.g., similar concentrations of analytes) in
determining similarity between samples in the data package. Two possible determinations
are: 1) all of the samples are considered sufficiently similar, and all samples should be
qualified; or 2) only some of the samples in the data package are similar to the Matrix Spike
sample, and that only these samples should be qualified.

NOTE: Matrix spike analysis is not required for SDG that contains only field blank samples.

Qualifiers based on matrix spike sample analysis results are to be applied to original
samples only.

Disregard the out-of-control spike recoveries for analytes whose unspiked
concentrations are > 4x the spike added.

Cyanide Table 6. Spike Sample Actions

Criteria

Action

Detect

Non-detect

Matrix Spike analysis not performed at the specified
frequency

J

UJ

Matrix Spike not prepared from field sample

J

UJ

Matrix Spike %R < 30%
Post-distillation spike %R < 75%

J-

R

Matrix Spike %R < 30%
Post-distillation spike %R > 75%

J

UJ

Matrix Spike %R 30 - 74%
Post-distillation spike %R < 75%

J-

UJ

Matrix Spike %R 30 - 74%
Post-distillation spike %R > 75%

J

UJ

Matrix Spike %R > 125%
Post-distillation spike %R > 125%

J+

No qualification

Matrix Spike %R > 125%
Post-distillation spike %R < 125%

J

No qualification

Matrix Spike %R < 30%
No post-distillation spike performed

J-

R

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Matrix Spike %R 30 - 74%
No post-distillation spike performed

J-

UJ

Matrix Spike %R 75 -125%
No post-distillation spike required

No qualification

No qualification

Matrix Spike %R > 125%
No post-distillation spike required

J+

No qualification

VII. Field Duplicates

A.	Review Items

Laboratory Results Reports, sampling documentation (e.g., COC Records, Trip Reports when
available), instrument printouts, and other raw data from QA/QC samples in data package.

B.	Objective

The objective is to use results from the analysis of field and project QA/QC samples such as field
blanks and field duplicates to determine the validity of the analytical results.

C.	Action:

Refer to Cyanide Table 7 below for the evaluation criteria and corresponding actions for
detected and non-detected target analyte results in the samples associated with deficient field
duplicates.

1.	If a field duplicate samples pair was collected and analyzed, calculate, and report the RPD
when the sample and its field duplicate values are both > 5x QL. Calculate and report the
absolute difference when at least one value (sample and its duplicate) < 5x QL. Do not
calculate RPD when both values are non-detects.

2.	Any action should be in accordance with the project specifications and the criteria for
acceptable field duplicate sample results.

3.	Note where RPDs exceed criteria for field duplicate samples in the Data Review Narrative
and for designated project management personnel action.

4.	For field duplicate sample analysis that does not meet the technical criteria, apply the
actions to the field sample and the field sample duplicate only. Exercise professional
judgment in determining sample similarity when making use of all available data, including
site and sampling documentation (e.g., location and type of sample, descriptive data, soil
classification); field test data (e.g., pH, Eh, conductivity, chlorine); and laboratory data for
other parameters [e.g., Total Suspended Solids (TSS), Total Dissolved Solids (TDS), Total
Organic Carbon (TOC), alkalinity or buffering capacity, reactive sulfide, anions]. Additionally,
use the sample data (e.g., similar concentrations of analytes) in determining similarity
between samples in the data package. Two possible determinations are: 1) all of the
samples are considered sufficiently similar, and all samples should be qualified; or 2) only

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some of the samples in the data package are similar to the field duplicate sample, and that
only these samples should be qualified.

Cyanide Table 7. Field Duplicate Actions

Criteria

Action

Detect

Non-detect

Aqueous: Both original sample and its field duplicate
sample results are > 5x QL and 20% < RPD <100%

J

NA

Soil/Sediment: Both original sample and its field duplicate
sample results are > 5x QL and 50% < RPD < 100%

J

NA

Both original sample and its field duplicate sample results
are > 5x QL and RPD < 20% (Aqueous) / < 50% RPD
(Soil/Sediment)

No qualification

No qualification

Aqueous: Original sample and/or its field duplicate sample
result < 5x QL (including non-detects) and absolute
difference between sample and duplicate > QL

J

UJ

Soil/Sediment: Original sample and/or its field duplicate
sample result < 5x QL (including non-detects) and absolute
difference between sample and duplicate > 2x QL

J

UJ

Original sample and its field duplicate > 5x QL and
RPD >100%

Use
professional
judgment to
qualify other
than R

NA

VIII. Target Analyte Quantitation

A.	Review Items

Laboratory result reports, sample preparation sheet, data package narrative, instrument
printouts and raw data.

B.	Objective

The objective is to ensure that the reported results and quantitation limits for target analytes
reported by the laboratory are accurate and sufficient to meet requirements.

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C. Action:

Refer to Cyanide Table 8 below for the evaluation criteria and corresponding actions for
detected and non-detected target analyte results in the samples with deficient quantitation
limits. Apply the actions to the affected analytes for each sample that does not meet the
quantitation criteria.

1.	If sample results are < QLs and > MDLs or limits in the QAPP, qualify as estimated (J).

2.	If any sample result was greater than the linear range for cyanide and the sample was not
diluted to obtain the result reported on Form I, qualify the affected results as estimated (J).

3.	If the percent solids of sediment for a sample are < 50% but > 30%, qualify the affected
results > MDL as estimated, J and the non-detects as estimate, UJ.

4.	If the sample's percent solids of sediment is < 30%, check if the sample was prepared at
greater mass to maintain the QLs. Use professional judgment when this was not completed.

Cyanide Table 8. Target Analyte Quantitation Percent Solids of Sediment Actions

Criteria

Action

Detect

Non-detect

Sample result < QLs and > MDLs or limits in the QAPP

J

NA

Sample result > the linear range for Cyanide and the
sample was not diluted to obtain the result reported on
Form 1

J

NA

Percent solids of sediment sample < 50% but > 30%

J

UJ

Percent solids of sediment sample < 30%, and was not
prepared at greater mass to maintain QLs

Use professional
judgment to
qualify J or R

Use professional
judgment to
qualify UJ or R

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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.

Analyte - The element or ion an analysis seeks to determine, the element of interest.

Analytical Services Branch (ASB) - Directs the Contract Laboratory Program (CLP) from within the
Office of Superfund Remediation and Technical Innovation (OSRTI) in the Office of Solid Waste and
Emergency Response (OSWER).

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, Initial Calibration Verification (ICV),
Initial Calibration Blank (ICB), Continuing Calibration Verification (CCV), Continuing Calibration Blank
(CCB), and tune verifications). The following are also defined as analytical samples: diluted samples;
matrix spike and matrix spike duplicate samples; duplicate samples; serial dilution samples, post-
digestion/post-distillation spike samples; Laboratory Control Samples (LCSs); Performance Evaluation
(PE) samples; Preparation/Method Blanks; Field Blanks (FBs); and Leachate Extraction Blanks (LEBs).

Associated Samples - Any sample related to a particular Quality Control (QC) analysis. For example, for
Initial Calibration Verification (ICV), all samples analyzed under the same calibration curve. For
duplicates, all Sample Delivery Group (SDG) samples digested/distilled of the same matrix.

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, preparation blanks, and field blanks. See the individual definitions for types of
blanks.

Calibration - A set of operations that establish under specific conditions, the relationship between
values indicated by a measuring instrument and the corresponding known values. The calibration
standards should be prepared using the same type of reagents or concentration of acids as used in the
sample preparation.

Calibration Blank - A blank solution containing all reagents and in the same concentration as those
used in the analytical sample preparation. This blank is digested/distilled for mercury and cyanide.
Calibration blanks are used to verify that the instrument baseline is stable, and the instrument is free of
contamination.

Calibration Curve - A plot of instrument response versus concentration of standards.

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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 period from a
particular project site. A case numbers is assigned by the Sample Management Office (SMO) and
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.

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 Blank (CCB) - A reagent water sample that is run at specified interval and
designed to detect any carryover contamination.

Contract Compliance Screening (CCS) - A screening of electronic and hardcopy data deliverables for
completeness and compliance with the contract. This screening is performed under EPA direction by
the Contract Laboratory Program (CLP) Sample Management Office (SMO) contractor.

Continuing Calibration Verification (CCV) - A single parameter or multi-parameter standard solution
prepared from the same source as the initial calibration standards by the analyst and used to
periodically verify the stability of the instrument calibration during analysis of samples. The CCV can be
one of the calibration standards with the concentration near the middle of the calibration range.
However, all parameters being measured by the particular system must be represented in this
standard and the standard must have the same matrix (i.e., the same amount of reagents and/or
preservatives) as the samples.

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.

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

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Contract Required Quantitation Limit (CRQL) - Minimum level of quantitation acceptable under the
contract Statement of Work (SOW).

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

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.

Duplicate - A second aliquot of a sample that is treated the same as the original sample in order to
evaluate the precision.

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 (FD) - A duplicate sample generated in the field, not in the laboratory.

Field Quality Control (FQC) - 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.

Holding Time - The maximum amount of time samples may be held before they are processed.

Holding Time (Contractual) - 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 CLP Analytical Services Statement of
Work (SOW). These times are the same or less than technical holding times to allow for sample
packaging and shipping.

Holding Time (Technical) - The maximum amount of time that samples may be held from the collection
date until analysis.

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

Initial Calibration Blank (ICB) - The first blank standard analysis to confirm the calibration curve.

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Initial Calibration Verification (ICV) - The analysis of solution(s) prepared from stock standard
solutions, metals, or salts obtained from a source separate from that utilized to prepare the calibration
standards. The ICV is used to verify the concentration of the calibration standards and the adequacy of
the instrument calibration. The ICV solution(s) should be traceable to National Institute of Standards
and Technology (NIST) or other certified standard sources.

Interference Check Sample (ICS) - A solution containing both interfering and analyte elements of
known concentration that can be used to verify background and interelement correction factors.

Internal Standard - A non-target element added to a sample at a known concentration after
preparation but prior to analysis. Instrument responses to internal standards are monitored as a means
of assessing overall instrument performance.

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.

Leachate Extraction Blank (LEB) - A blank carried through the entire Toxicity Characteristic Leaching
Procedure (TCLP) or Synthetic Precipitation Leaching Procedure (SPLP) extraction with the resulting
leachate extracted, digested, or distilled by an appropriate aqueous method from the analytical
method.

Matrix-The predominant material of which the sample to be analyzed is composed. For the purposes
ofthis document, the matrices are aqueous/water, soil/sediment, and wipe. Matrix is not synonymous
with phase (liquid or solid).

Matrix Spike - Aliquot of a sample (aqueous/water or soil/sediment) fortified (spiked) with known
quantities of specific analytes and subjected to the entire analytical procedure to estimate recovery.

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. Additional information about the procedure is provided in Title 40 of the Code of Federal
Regulations (CFR), Chapter 1, Subchapter D, part 136, Appendix B, Definition and Procedure for the
Determination of the Method Detection Limit, Revision 2.

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

Office of Solid Waste and Emergency Response (OSWER) - The EPA office that provides policy,
guidance, and direction for the EPA's solid waste and emergency response programs, including
Superfund.

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Percent Difference (%D) - The relative difference between two values (e.g., a measured and expected
value) expressed as a percentage of one of the values (e.g., expected value).

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

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.

Post-Digestion Spike/Post-Distillation Spike - The addition of a known amount of standard after
digestion or distillation (also identified as an analytical spike).

Preparation Blank (PB) - An analytical control that contains reagent water and reagents, which is
carried through the entire preparation and analytical procedure.

Preparation Log - A record of sample preparation (e.g., digestion, extraction, distillation) 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 (QL) - 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.

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

Regional Sample Control Center Coordinator (RSCC) - In EPA Regions, coordinates sampling efforts
and serves as the central point-of-contact for sampling questions and problems. Also assists in
coordinating the level of Regional sampling activities to correspond with the monthly projected
demand for analytical services.

Relative Standard Deviation (RSD) - As used in this document and the Statement of Work (SOW), the
mean divided by the standard deviation, expressed as a percentage.

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

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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:

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

b.	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
the SDG).

c.	Scheduled at the same level of deliverable.

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.

Sample Identifier - A unique identification number that appears on the Chain of Custody (COC)

Records or sampling forms which documents information for a sample.

Sample Management Office (SMO) - A contractor-operated facility operated under the SMO contract,
awarded, and administered by the EPA. Provides necessary management, operations, and
administrative support to the Contract Laboratory Program (CLP).

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.

Serial Dilution (SD) - The dilution of a sample by a factor of five. When corrected by the Dilution Factor
(DF), the diluted sample should agree with the original undiluted sample within specified limits. Serial
dilution may reflect the influence of interferents [Inductively Coupled Plasma (ICP) only].

Soil - Synonymous with soil/sediment and sediment as used herein.

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

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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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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