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Hazardous Waste Support Branch
SOP No. HW-3c Revision 1
ISM02.2
Mercury and Cyanide Data Validation
Approvals:
Narendra Kumar
Chemist, Hazardous Waste Support Section
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Date
Date
Chief, Hazardous Waste Support Section
Jon Gwxy
Chief, Hazardous Waste Support Branch
//?*/'7
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NOTICE
The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (hereafter referred to as USEPA) and other governmental
employees. They do not constitute rule making by 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 variance with the policies and procedures in this manual.
This document can be obtained from the USEPA's Region 2 Quality Assurance website at:
http://www.epa. gov/regi on2/qa/ documents, htm
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TABLE OF CONTENTS
NOTICE 1
TABLE OF CONTENTS 2
ACRONYMS 4
TARGET ANALYTE LIST 5
INTRODUCTION 6
DATA QUALIFIER DEFINITIONS 7
DATA PACKAGE INSPECTION 7
PRELIMINARY REVIEW 9
An Example Analytical Sequence for Mercury 10
An Example Analytical Sequence for Cyanide 10
Mercury Preservation and Holding Times 12
Cyanide Preservation and Holding Times 13
Mercury Calibration 14
Cyanide Calibration 16
Mercury/Cyanide Calibration/Preparation Blanks 18
Mercury/Cyanide Laboratory Duplicate Sample Analysis 21
Mercury Spike Sample Analysis 23
Cyanide Spike Sample Analysis 25
Mercury/Cyanide Field Duplicates 27
Mercury/Cyanide Field/Rinsate/Trip Blanks 28
Mercury/Cyanide Linear Ranges 30
Mercury/Cyanide Percent Solids of Sediments 31
Regional Quality Assurance (QA) and Quality Control (QC) 32
Overall Assessment 33
Calculations for Mercury 34
Calculations for Cyanide 35
APPENDIX A: GLOSSARY 37
APPENDIX B: INORGANIC DATA EXECUTIVE NARRATIVE TEMPLATE 41
APPENDIX C: SAMPLE INORGANIC DATA SAMPLE SUMMARY 42
APPENDIX D: ELECTRONIC DATA DELIVERABLE TEMPLATE 43
APPENDEX E: REQUEST FOR STANDARD OPERATIGN PROCEDURE (SOP) CHANGE 44
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LIST OF TABLES
Table 1. Technical Holding Time Actions for Mercury Analysis 12
Table 2. Technical Holding Time Actions for Cyanide Analysis 13
Table 3. Acceptance Criteria for Mercury ICVs and CCVs 14
Table 4. Calibration Actions for Mercury Analysis 15
Table 5. Acceptance Criteria for Cyanide ICVs and CCVs 16
Table 6. Calibration Actions for Cyanide Analysis 17
Table 7. Calibration/Preparation Blank Actions for Mercury/Cyanide Analysis 20
Table 8. Duplicate Sample Actions for Mercury/Cyanide Analysis 22
Table 9. Spike Sample Actions for Mercury Analysis 24
Table 10. Spike Sample Actions for Cyanide Analysis 26
Table 11. Field Duplicate Actions for Mercury/Cyanide Analysis 27
Table 12. Field/Rinsate/Trip Blank Actions for Mercury/Cyanide Analysis 29
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ACRONYMS
ASB
Analytical Services Branch
CCB
Continuing Calibration Blank
CCS
Contract Compliance Screening
CCV
Continuing Calibration Verification
CLP
Contract Laboratory Program
COR
Contracting Officer Representative
CRQL
Contract Required Quantitation Limit
DF
Dilution Factor
DQO
Data Quality Objective
EDD
Electronic Data Deliverable
EDM
EXES Data Manager
ESAT
Environmental Services Assistance Team
EXES
Electronic Data exchange and Evaluation System
HWSS
Hazardous Waste Support Section
ICB
Initial Calibration Blank
ICP
Inductively Coupled Plasma
ICP-AES
Inductively Coupled Plasma - Atomic Emission Spectroscopy
ICP-MS
Inductively Coupled Plasma - Mass Spectrometry
ICS
Interference Check Sample
ICV
Initial Calibration Verification
LCS
Laboratory Control Sample
LEB
Leachate Extraction Blank
MDL
Method Detection Limit
NIST
National Institute of Standards and Technology
OSRTI
Office of Superfund Remediation and Technology Innovation
OSWER
Office of Solid Waste and Emergency Response
PE
Performance Evaluation
%D
Percent Difference
%R
Percent Recovery
% Solids
Percent Solids
PO
Project Officer
QA
Quality Assurance
QAPP
Quality Assurance Project Plan
QC
Quality Control
RPD
Relative Percent Difference
RSCC
Regional Sample Control Center Coordinator
SDG
Sample Delivery Group
SMO
Sample Management Office
SOP
Standard Operating Procedure
SOW
Statement of Work
SLPL
Synthetic Precipitation Leaching Procedure
TCLP
Toxicity Characteristic Leaching Procedure
TR/COC
Traffic Report/Chain of Custody Documentation
USEPA
United States Environmental Protection Agency
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TARGET ANALYTE LIST
CN Cyanide
Hg Mercury
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INTRODUCTION
This document is designed to offer the data reviewer guidance in determining the validity of
analytical data generated through the USEPA Contract Laboratory Program (CLP) Statement of
Work (SOW) ISM02.X Inorganic Superfund Methods (Multi-Media, Multi-Concentration),
hereinafter referred to as the ISM02.2 SOW, and any future editorial revisions of ISM02.2. This
guidance is somewhat limited in scope and is intended to be used as an aid in the formal
technical review process.
The guidelines presented in the document will aid the data reviewer in establishing (a) if data
meets the specific technical and 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 reviewer 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 availability for re-
sampling.
The reviewer should note that while this document is to be used as an aid in the formal data
review process, other sources of guidance and information, as well as professional judgment,
should also be used to determine the ultimate validity of data, especially in those cases where all
data does not meet specific technical criteria.
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DATA QUALIFIER DEFINITIONS
The following definitions provide brief explanations of the national qualifiers assigned to results
in the data review process.
U
The analyte was analyzed for, but was not detected above the level of the reported
sample quantitation limit.
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.
R
The data are unusable. The sample results are rejected due to serious deficiencies in
meeting Quality Control (QC) criteria. The analyte may or may not be present in the
sample.
UJ
The analyte was analyzed for, but was not detected. The reported quantitation limit
is approximate and may be inaccurate or imprecise.
DATA PACKAGE INSPECTION
For data obtained through the Contract Laboratory Program (CLP), the EXES Data Manager
(EDM) is a useful tool in the data review process. For more information about EDM, please refer
to the following Sample Management Office (SMO) website:
https://epasmoweb.fedcsc.com/help/guides/Submit%20and%20Inspect%20Data%20Quick%20G
uide%20%28EXES%29.pdf
EDM will identify any missing and/or incorrect information in the data package. The CLP
laboratory may submit a reconciliation package for any missing items or to correct data.
If there are any concerns regarding the data package, contact the CLP Project Officer (CLP PO)
from the Region where the samples were taken. For personnel contact information, please refer
to the following CLP website:
http ://www. epa. gov/ superfund/programs/clp/contacts.htm
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HWSS DATA VALIDATION PROCESS
After downloading the data package from EDM, the data validator will use the recommendations
in this SOP as well as their own professional judgment to validate the data.
The data will be saved in the following location, under the appropriate case number folder:
Examples: 12345_MBXY12_S2BVE.xls
12345 MBXY12 S2BVEM.xls
When data validation is completed, the data package is uploaded for the client to download from
the HWSS data delivery website.
The completed data package includes the Executive Narrative (see Appendix B for template), the
Sample Summary Report (see Appendix C for example), and the Electronic Data Deliverable
(EDD) (see Appendix D for a list of the column headers included in this document).
G:\DESADIV\HWSS\DATA VALIDATION
The file naming conventions will consist of
A. Case number
B. SDGname
C. level of validation performed
i.e., 12345
i.e., MBXY12
i.e., S2BVE
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PRELIMINARY REVIEW
This document is for the review of analytical data generated through the ISM02.2 SOW and any
future editorial revisions of ISM02.2. To use this document effectively, the reviewer should have
an understanding of the analytical method and a general overview of the Sample Delivery Group
(SDG) or sample Case at hand. The exact number of samples, their assigned numbers, their
matrix, and the number of laboratories involved in the analysis are essential information.
It is suggested that an initial review of the data package be performed, taking into consideration
all information specific to the sample data package [e.g., Modified Analysis requests, Traffic
Report/Chain of Custody (TR/COC) 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 reviewer should contact the
appropriate Regional Contract Laboratory Program Project Officer (CLP PO) to obtain copies of
the QAPP and relevant site information. This information is necessary in determining the final
usability of the analytical data.
The SDGs or Cases routinely have unique samples that require special attention from the
reviewer. These include field blanks and trip blanks, field duplicates, and Performance
Evaluation (PE) samples which must be identified in the sampling records. The sampling records
(e.g., TR/COC records, field logs, and/or contractor tables) should identify:
1. The Region where the samples were taken, and
2. The complete list of samples with information on:
a.
Sample matrix;
b.
Field blanks*;
c.
Field duplicates*;
d.
Field spikes*;
e.
PE samples*;
f.
Shipping dates;
g-
Preservatives;
h.
Types of analysis; and
i.
Laboratories involved.
* If applicable.
The TR/COC documentation includes sample 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 detailing any
discussion of sample or analysis issues between the laboratory, the CLP Sample Management
Office (SMO), and the USEPA Region.
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An Example Analytical Sequence for Mercury
SO
SO.2
S1.0
S2.0
S5.0
S10.0
ICV
ICB
CCV
CCB
samples
CCV
CCB
samples
CCV
CCB, etc.
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An Example Analytical Sequence for Cyanide
SO
S10
S50
S100
S200
S400
ICV
ICB
CCV
CCB
samples
CCV
CCB
samples
CCV
CCB, etc.
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Mercury Preservation and Holding Times
Action:
NOTE: Apply the action to each sample for which the preservation or holding time
criteria was not met.
1. If the pH of aqueous/water metal samples is > 2 at the time of sample receipt, determine
if the laboratory adjusted the pH of the sample to < 2 at the time of sample receipt. Also
determine if the laboratory adjusted the pH to < 2 for the TCLP and SPLP leachates after
completion of the leaching procedure. If not, use professional judgment to qualify the
samples based on the pH of the sample and the chemistry of the metal(s) of interest.
Qualify results that are > Method Detection Limit (MDL) as estimated low (J-), and
qualify non-detects as unusable (R).
2. If technical holding times are exceeded, use professional judgment to determine the
reliability of the data, based on the magnitude of the additional time compared to the
technical requirement and whether the samples were properly preserved. The expected
bias would be low. Qualify results that are > MDL as estimated low (J-), and qualify non-
detects as unusable (R).
3. Due to limited information concerning holding times for soil/sediment samples, it is left
to the discretion of the data reviewer whether to apply aqueous/water holding time
criteria to soil/sediment samples. If they are applied, it must be clearly documented in the
Data Review Narrative.
4. When the holding times are exceeded, the reviewer should comment in the Data Review
Narrative on any possible consequences for the analytical results.
5. When holding times are grossly exceeded, note it for Contract Laboratory Program
Project Officer (CLP PO) action.
Table 1. Technical Holding Time Actions for Mercury Analysis
Preservation & Holding Time Results
Action for Samples
Aqueous/water mercury and
TCLP/SPLP leachate samples received
with pH > 2 and pH not adjusted
Use professional judgment
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
Technical Holding Time exceeded:
Aqueous/water and TCLP/SPLP
leachate samples > 28 days
Use professional judgment
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
Technical Holding Time exceeded:
Soil/sediment samples > 28 days
Use professional judgment
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
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Cyanide Preservation and Holding Times
Action:
NOTE: Apply the action to each sample for which the preservation or holding time
criteria was not met.
1. If oxidizing agents are detected in aqueous/water cyanide samples at the time of sample
preparation, qualify results that are > Method Detection Limit (MDL) as estimated low
(J-) and non-detects as unusable (R). If sulfides are detected in aqueous/water cyanide
samples at the time of sample preparation and there is no evidence that the laboratory
removed the sulfides (using precipitation and filtration), qualify results that are > MDL as
estimated (J) and non-detects as unusable (R). If the pH of aqueous/water cyanide
samples is < 12 at the time of sample receipt, use professional judgment to qualify the
samples based on the pH of the sample. Qualify results that are > MDL as estimated low
(J-) and qualify non-detects as unusable (R).
2. If technical holding times are exceeded, use professional judgment to determine the
reliability of the data based on the magnitude of the additional time compared to the
technical requirement and whether the samples are properly preserved. The expected bias
would be low. Qualify results that are > MDL as estimated low (J-) and non-detects as
unusable (R).
3. Due to limited information concerning holding times for soil/sediment samples, it is left
to the discretion of the data reviewer whether to apply aqueous/water holding time
criteria to soil/sediment samples. If they are applied, it must be clearly documented in the
Data Review Narrative.
4. When the holding times are exceeded, the reviewer should comment in the Data Review
Narrative on any possible consequences for the analytical results.
5. When holding times are grossly exceeded, note it for Contract Laboratory Program
Project Officer (CLP PO) action.
Table 2. Technical Holding Time Actions for Cyanide Analysis
Preservation & Holding Time Results
Action for Samples
Aqueous/water cyanide samples
received with oxidizing agents present
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
Aqueous/water cyanide samples
received with sulfides present, and
sulfides are not removed
Qualify results that are > MDL as estimated (J)
Qualify non-detects as unusable (R)
Aqueous/water cyanide samples
received with pH < 12
Use professional judgment
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
Technical Holding Time exceeded:
Aqueous/water and SPLP leachate
cyanide samples >14 days
Use professional judgment
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as unusable (R)
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Mercury Calibration
Table 3. Acceptance Criteria for Mercury ICVs and CCVs
Analytical Method
Inorganic Analytes
ICV/CCV Low Limit
(% of True Value)
ICV/CCV High Limit
(% of True Value)
Cold Vapor AA
Mercury
85
115
Action:
NOTES: For initial calibrations or ICVs that do not meet the technical criteria, apply the
action to all samples reported from the analytical run.
For CCVs that do not meet the technical criteria, apply the action 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 run.
NOTE: The data validator shall verify the correlation coefficient by calculating it using
the standard concentrations and the corresponding instrument response.
1. If the instrument was not calibrated daily and each time the instrument was set up or an
ICV standard was not analyzed before field and QC samples, qualify the data as unusable
®. If the instrument was not calibrated with a blank and at least 5 calibration standards,
or if the instrument was not calibrated with standards prepared at the same time as the
samples, use professional judgment to qualify results that are > Method Detection Limit
(MDL) as estimated (J), and non-detects as estimated (UJ). If the calibration curve does
not include standards at required concentrations (e.g., a blank and at least one standard at
or below CRQL), use professional judgment to qualify results that are > MDL as
estimated (J), and non-detects as estimated (UJ).
2. If the correlation coefficient is < 0.995, percent differences are outside the ±30% limit, or
the y-intercept > CRQL, qualify sample results that are > MDL as estimated (J) and non-
detects as estimated (UJ). If the correlation coefficient is < 0.990, qualify results that are
> MDL as estimated (J) and non-detects as unusable (R).
3. If the ICV or CCV %R falls outside the acceptance windows, use professional judgment
to qualify all associated data. If possible, indicate the bias in the review. The following
guidelines are recommended:
a. If the ICV or CCV %R is < 70%, qualify non-detects as unusable (R). Use
professional judgment to qualify all results that are > MDL as unusable (R).
b. If the ICV or CCV %R falls within the range of 70-84%), qualify sample results
that are > MDL as estimated low (J-), and qualify non-detects as estimated (UJ).
c. If the ICV or CCV %>R falls within the range of 116-130%), qualify sample results
that are > MDL as estimated high (J+).
d. If the ICV or CCV %>R is within the range of 116-130%), non-detects should not
be qualified.
e. If the ICV or CCV %>R is > 130%>, use professional judgment to qualify results
that are > MDL as estimated high (J+). Non-detects should not be qualified.
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f. If the %R is > 165%, qualify all results that are > MDL as unusable (R).
4. If the laboratory failed to provide adequate calibration information, the Region's
designated representative should contact the laboratory and request the necessary
information. If the information is not available, the reviewer must use professional
judgment to assess the data.
5. Note the potential effects on the reported data due to exceeding the calibration criteria in
the Data Review Narrative.
6. If calibration criteria are grossly exceeded, note this for CLP Project Officer (CLP PO)
action.
NOTE: For critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.
Table 4. Calibration Actions for Mercury Analysis
Calibration Result
Action for Samples
Calibration not performed
Qualify all results as unusable (R)
Calibration incomplete
Use professional judgment
Qualify results that are > MDL as estimated (J)
Qualify non-detects as estimated (UJ)
Not at least one calibration
standard at or below the CRQL
for each analyte
Qualify results that are > MDL but < 2x the CRQL as
estimated (J)
Qualify non-detects as estimated (UJ)
Correlation coefficient < 0.995;
%D outside ±30%; y-intercept
> CRQL
Qualify results that are > MDL as estimated (J)
Qualify non-detects as estimated (UJ)
Correlation coefficient < 0.990
Qualify results that are > MDL as estimated (J)
Qualify non-detects as unusable (R)
ICV/CCV %R < 70%
Qualify results that are > MDL as unusable (R)
Qualify all non-detects as unusable (R)
ICV/CCV %R 70-84%
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as estimated (UJ)
ICV/CCV %R 116-130%
Qualify results that are > MDL as estimated high (J+)
ICV/CCV %R > 130%
Qualify results that are > MDL as estimated high (J+)
ICV/CCV %R > 165%
Qualify results that are > MDL as unusable (R)
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Cyanide Calibration
Table 5. Acceptance Criteria for Cyanide ICVs and CCVs
Analytical Method
Inorganic Analytes
ICV/CCV Low Limit
(% of True Value)
ICV/CCV High Limit
(% of True Value)
Colorimetric
Cyanide
85
115
Action:
NOTES: For initial calibrations or ICVs that do not meet the technical criteria, apply the
action to all samples reported from the analytical run.
For CCVs that do not meet the technical criteria, apply the action 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 run.
NOTE: The data validator shall verify the correlation coefficient by calculating it using
the standard concentrations and the corresponding instrument response.
1. If the instrument was not calibrated daily and each time the instrument was set up or an
ICV standard was not analyzed before field and QC samples, qualify the data as unusable
(R). If the instrument was not calibrated with a blank and at least 5 calibration standards,
or if the instrument was not calibrated with standards prepared at the same time as the
samples, use professional judgment to qualify results that are > Method Detection Limit
(MDL) as estimated (J), and non-detects as estimated (UJ). If the calibration curve does
not include standards at required concentrations (e.g., a blank and at least one standard at
or below CRQL), use professional judgment to qualify results that are > MDL as
estimated (J), and non-detects as estimated (UJ).
2. If the correlation coefficient is < 0.995, percent differences are outside the ±30% limit, or
the y-intercept > CRQL, qualify sample results that are > MDL as estimated (J) and non-
detects as estimated (UJ). If the correlation coefficient is < 0.990, qualify results that are
> MDL as estimated (J) and non-detects as unusable (R).
3. If the standards, the ICV, or the CCVs are not distilled for cyanide, qualify sample results
that are > MDL as estimated (J).
4. If the ICV or CCV %R falls outside the acceptance windows, use professional judgment
to qualify all associated data. If possible, indicate the bias in the review. The following
guidelines are recommended:
a. If the ICV or CCV %R is < 70%, qualify non-detects as unusable (R). Use
professional judgment to qualify all results that are > MDL as unusable (R).
b. If the ICV or CCV %R falls within the range of 70-84%), qualify sample results
that are > MDL as estimated low (J-), and qualify non-detects as estimated (UJ).
c. If the ICV or CCV %>R falls within the range of 116-130%), qualify sample results
that are > MDL as estimated high (J+).
d. If the ICV or CCV %>R is within the range of 116-130%), non-detects should not
be qualified.
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e. If the ICV or CCV %R is > 130%, use professional judgment to qualify results
that are > MDL as estimated high (J+). Non-detects should not be qualified.
f. If the %R is > 165%, qualify all results that are > MDL as unusable (R).
5. If the laboratory failed to provide adequate calibration information, the Region's
designated representative should contact the laboratory and request the necessary
information. If the information is not available, the reviewer must use professional
judgment to assess the data.
6. Note the potential effects on the reported data due to exceeding the calibration criteria in
the Data Review Narrative.
7. If calibration criteria are grossly exceeded, note this for CLP Project Officer (CLP PO)
action.
NOTE: For critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.
Table 6. Calibration Actions for Cyanide Analysis
Calibration Result
Action for Samples
Calibration not performed
Qualify all results as unusable (R)
Calibration incomplete
Use professional judgment
Qualify results that are > MDL as estimated (J)
Qualify non-detects as estimated (UJ)
Not at least one calibration
standard at or below the CRQL
for each analyte
Qualify results that are > MDL but < 2x the CRQL as
estimated (J)
Qualify non-detects as estimated (UJ)
Correlation coefficient < 0.995;
%D outside ±30%; y-intercept
> CRQL
Qualify results that are > MDL as estimated (J)
Qualify non-detects as estimated (UJ)
Correlation coefficient < 0.990
Qualify results that are > MDL as estimated (J)
Qualify non-detects as unusable (R)
Standards and QC not distilled
Qualify results that are > MDL as estimated (J)
ICV/CCV %R < 70%
Qualify results that are > MDL as unusable (R)
Qualify all non-detects as unusable (R)
ICV/CCV %R 70-84%
Qualify results that are > MDL as estimated low (J-)
Qualify non-detects as estimated (UJ)
ICV/CCV %R 116-130%
Qualify results that are > MDL as estimated high (J±)
ICV/CCV %R > 130%
Qualify results that are > MDL as estimated high (J±)
ICV/CCV %R > 165%
Qualify results that are > MDL as unusable (R)
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Mercury/Cyanide Calibration/Preparation Blanks
Action:
NOTES: For ICBs that do not meet the technical criteria, apply the action to all samples
reported from the analytical run.
For CCBs that do not meet the technical criteria, apply the action to all samples
analyzed between a previous technically acceptable analysis of the CCB and a
subsequent technically acceptable analysis of the CCB in the analytical run.
For Preparation Blanks that do not meet the technical criteria, apply the action to
all samples prepared in the same preparation batch. For LEBs that do not meet the
technical criteria, apply the action to all samples extracted in the same extraction
batch.
NOTES: The preparation blank for mercury is the same as the calibration blank.
Convert soil sample result to mg/kg on wet weight basis to compare with the soil
preparation result on Form III.
Associated samples are all samples digested with the preparation blank.
1. If the appropriate blanks were not analyzed with the correct frequency, the data reviewer
should use professional judgment to determine if the associated sample data should be
qualified. The reviewer may need to obtain additional information from the laboratory.
The situation should then be recorded in the Data Review Narrative, and noted for
Contract Laboratory Program Project Officer (CLP PO) action.
2. Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. The reviewer should note that 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.
3. Some general "technical" review actions include:
a. Any blank (including Preparation Blanks and LEBs) reported with a negative
result, whose value is < (-MDL) but > (-CRQL), should be carefully evaluated to
determine its effect on the sample data. The reviewer shall then use professional
judgment to assess the data. For any blank (including Preparation Blanks and
LEBs) reported with a negative result, whose value is < (-CRQL) qualify results
that are > CRQL as estimated low (J-) and non-detects as estimated (UJ).
b. The blank analyses may not involve the same weights, volumes, or dilution
factors as the associated samples. In particular, soil/sediment sample results
reported on Form I-IN will not be on the same basis (units, dilution) as the
calibration blank data reported on Form III-IN. The reviewer may find it easier to
work with the raw data.
4. Specific "method" actions include:
a. If the absolute value of an ICB or a CCB result is > CRQL, the analysis should be
terminated. If the analysis was not terminated and the affected samples were not
reanalyzed, report non-detects and results that are > MDL, but < CRQL as CRQL-
U. For results that are > CRQL but < Blank Result, report the results at the level
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of the blank with a "U" qualifier. Use professional judgment to qualify results that
are > Blank Result. Note this situation for CLP PO action and record it in the Data
Review Narrative.
b. If the absolute value of the concentration of the Preparation Blank/LEB is <
CRQL, report non-detects and results that are > MDL but < CRQL as CRQL-U.
Use professional judgment to quality results that are > CRQL.
c. If the mercury concentration in the Preparation Blank/LEB is > CRQL, the lowest
concentration of mercury in the associated samples must be lOx the Preparation
Blank/LEB concentration. Otherwise, all samples associated with that blank with
concentrations < lOx the Preparation Blank/LEB concentration and > CRQL
should be redigested and reanalyzed. Raise the CRQL to the concentration found
in the Preparation Blank/LEB and report those samples that do not require
redigestion (that are > MDL but < CRQL) as CRQL-U. Note for CLP PO action
and record in the Data Review Narrative if the laboratory failed to redigest and
reanalyze the affected samples. The reviewer shall then use professional judgment
to assess the data.
d. If the cyanide concentration in the Preparation Blank/LEB is > CRQL, the lowest
concentration of cyanide in the associated samples must be lOx the Preparation
Blank/LEB concentration. Otherwise, all samples associated with that blank with
concentrations < lOx the Preparation Blank/LEB concentration and > CRQL
should be redistilled and reanalyzed. Raise the CRQL to the concentration found
in the Preparation Blank/LEB and report those samples that do not require
redistillation (that are > MDL but < CRQL) as CRQL-U. Note for CLP PO action
and record in the Data Review Narrative if the laboratory failed to redistill and
reanalyze the affected samples. The reviewer shall then use professional judgment
to assess the data.
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Table 7. Ca
ibration/Preparation Blank Actions for Mercury/Cyanide Analysis
Blank Type
Blank Result
Sample Result
Action for Samples
ICB/CCB
> MDL but < CRQL
Non-detect
No action
> MDL but < CRQL
Report CRQL value with a
"U"
> CRQL
Use professional judgment
ICB/CCB
> CRQL
> MDL but < CRQL
Report CRQL value with a
"U"
> CRQL but < Blank
Result
Report at level of Blank
Result with a "U"
> Blank Result
Use professional judgment
ICB/CCB
< (-MDL) but
> (-CRQL)
> MDL, or non-detect
Use professional judgment
ICB/CCB
< (-CRQL)
< 1 Ox the CRQL
Qualify results that are >
CRQL as estimated low (J-)
Qualify non-detects as
estimated (UJ)
Preparation Blank
/LEB
> CRQL
> MDL but < CRQL
Report CRQL value with a
"U"
> CRQL but < lOx the
Blank Result
Qualify results as estimated
high (J+)
> lOx the Blank Result
No action
Preparation Blank
/LEB
> MDL but < CRQL
Non-detect
No action
> MDL but < CRQL
Report CRQL value with a
"U"
> CRQL
Use professional judgment
Preparation Blank
/LEB
< (-CRQL)
< 1 Ox the CRQL
Qualify results that are >
CRQL as estimated low (J-)
Qualify non-detects as
estimated (UJ)
Field/Rinse/Trip
> MDL but < CRQL
Qualify associated samples
in the same as the
ICB/CCB/PB method blank
criteria.
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Mercury/Cyanide Laboratory Duplicate Sample Analysis
Action:
NOTE: For a duplicate sample analysis that does not meet the technical criteria, apply the
action to only the field sample used to prepare the duplicate sample. If it is clearly
stated in the data validation materials that the samples were taken through
incremental sampling or some other method guaranteeing the homogeneity of the
sample group, then the entire sample group may be qualified.
NOTE: Delete from Form IAs.
If one value is > CRQL and the other value is non-detect, calculate the absolute
difference between the value > CRQL and the MDL and use this difference to
qualify sample results.
If more than one lab duplicate sample was analyzed for an SDG, then qualify the
associated samples based on the worst lab duplicate analysis.
1. If the appropriate number of duplicate samples was not analyzed for each matrix using
the correct frequency, use professional judgment to determine if the associated sample
data should be qualified. The reviewer may need to obtain additional information from
the laboratory. Note the situation in the Data Review Narrative, and for CLP Project
Officer (CLP PO) action.
2. If the results from a duplicate analysis for mercury/cyanide fall outside the control limits
for > 5x the CRQL, qualify aqueous sample results that are > CRQL as estimated (J) if
the RPD is between 20% - 100% and as unusable (R) if the RPD is > 100%. Qualify
soil/sediment sample results that are > CRQL as estimated (J) if the RPD is between 35%
- 120% and as unusable (R) if the RPD is > 120%.
3. If the results from a duplicate analysis for mercury/cyanide fall outside the control limits
for < 5x the CRQL, qualify those results that are > MDL as estimated (J) and non-detects
as estimated (UJ).
4. If a field blank or PE sample was used for the duplicate sample analysis, note this for
CLP PO action. All of the other Quality Control (QC) data must then be carefully
checked and professional judgment exercised by the data reviewer when evaluating the
data.
5. Note the potential effects on the data due to out-of-control duplicate sample results in the
Data Review Narrative.
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Table 8. Duplicate Sample Actions for Mercury/Cyanide Analysis
Duplicate Sample Results
Action for Samples
Aqueous:
Both original sample and duplicate sample >
5x the CRQL and 20% < RPD < 100%
Qualify those results that are > CRQL as
estimated (J)
Aqueous:
Both original sample and duplicate sample >
5x the CRQL and RPD > 100%
Qualify those results that are > CRQL as
unusable (R)
Soil/Sediment:
Both original sample and duplicate sample >
5x the CRQL and 35% < RPD < 120%
Qualify those results that are > CRQL as
estimated (J)
Soil/Sediment:
Both original sample and duplicate sample >
5x the CRQL and RPD > 120%
Qualify those results that are > CRQL as
unusable (R)
Original sample or duplicate sample < 5x the
CRQL (including non-detects) and absolute
difference between sample and duplicate >
CRQL
Qualify those results that are > MDL as
estimated (J) and non-detects as estimated (UJ)
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Mercury Spike Sample Analysis
Action:
NOTE: For a Matrix Spike that does not meet the technical criteria, apply the action to
only the field sample used to prepare the Matrix Spike sample. If it is clearly
stated in the data validation materials that the samples were taken through
incremental sampling or some other method guaranteeing the homogeneity of the
sample group, then the entire sample group may be qualified.
NOTE: The final spike concentrations required for mercury are presented in the methods
described in the Statement of Work (SOW).
NOTE: When the sample concentration is < Method Detection Limit (MDL), use SR = 0
only for the purpose of calculating the %R. The actual spiked sample results,
sample results, and %R (positive or negative) shall still be reported on Forms VA-
IN and VB-IN.
NOTES: Disregard the out of control spike recoveries for analytes whose unspiked
concentrations are > 4x the spike added.
Delete "N" from Form IAs.
1. If the appropriate number of Matrix Spike samples was not analyzed for each matrix
using the correct frequency, use professional judgment to determine if the associated
sample data should be qualified. The reviewer may need to obtain additional information
from the laboratory. Note the situation in the Data Review Narrative, and for Contract
Laboratory Program Project Officer (CLP PO) action.
2. If a field blank or PE sample was used for the spiked sample analysis, note this for CLP
PO action. All of the other Quality Control (QC) data must then be carefully checked and
professional judgment exercised by the data reviewer when evaluating the data.
3. If the Matrix Spike %R is < 30%, qualify affected results that are > MDL as estimated
low (J-) and non-detects as unusable (R).
4. If the Matrix Spike %R falls within the range of 30-74% and the sample results are >
MDL, qualify the affected data as estimated low (J-).
5. If the Matrix Spike %R falls within the range of 30-74%> and the sample results are non-
detects, qualify the affected data as estimated (UJ).
6. If the Matrix Spike %>R is > 125%> and the reported sample results are non-detects, the
sample data should not be qualified.
7. If the Matrix Spike %>R is > 125% and the sample results are > MDL, qualify the
affected data as estimated high (J+).
8. Note the potential effects on the data due to out-of-control spiked sample results in the
Data Review Narrative.
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Table 9. Spike Sample Actions for Mercury Analysis
Spike Sample Results
Action for Samples
Matrix Spike %R < 30%
Qualify affected results that are > MDL as estimated low (J-)
and affected non-detects as unusable (R)
Matrix Spike %R 30-74%
Qualify affected results that are > MDL as estimated low (J-)
and affected non-detects as estimated (UJ)
Matrix Spike %R > 125%
Qualify affected results that are > MDL as estimated high (J+)
Non-detects are not qualified
Matrix Spike %R 75-125%
No Qualification.
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Cyanide Spike Sample Analysis
Action:
NOTE: For a Matrix Spike that does not meet the technical criteria, apply the action to
only the field sample used to prepare the Matrix Spike sample. If it is clearly
stated in the data validation materials that the samples were taken through
incremental sampling or some other method guaranteeing the homogeneity of the
sample group, then the entire sample group may be qualified.
NOTE: The final spike concentrations required for cyanide are presented in the methods
described in the Statement of Work (SOW).
NOTE: When the sample concentration is < Method Detection Limit (MDL), use SR = 0
only for the purpose of calculating the %R. The actual spiked sample results,
sample results, and %R (positive or negative) shall still be reported on Forms VA-
IN and VB-IN.
NOTES: Disregard the out of control spike recoveries for analytes whose unspiked
concentrations are > 4x the spike added.
Delete "N" from Form IAs.
1. If the appropriate number of Matrix Spike samples was not analyzed for each matrix
using the correct frequency, use professional judgment to determine if the associated
sample data should be qualified. The reviewer may need to obtain additional information
from the laboratory. Note the situation in the Data Review Narrative, and for Contract
Laboratory Program Project Officer (CLP PO) action.
2. If a field blank or PE sample was used for the spiked sample analysis, note this for CLP
PO action. All of the other Quality Control (QC) data must then be carefully checked and
professional judgment exercised by the data reviewer when evaluating the data.
3. If the Matrix Spike recovery does not meet the evaluation criteria and a required post-
distillation spike was not performed, note this for CLP PO action.
4. If the Matrix Spike %R is < 30%, verify that a post-distillation spike was analyzed if
required. If the post-distillation spike %R is < 75% or is not performed, qualify sample
results that are > MDL as estimated low (J-) and non-detects as unusable (R). If the post-
distillation spike %R is > 75%, qualify sample results that are > MDL as estimated (J)
and non-detects as estimated (UJ).
5. If the Matrix Spike %R falls within the range of 30-74%) and the sample results are >
MDL, verify that a post-distillation spike was analyzed if required. If the %>R for the
post-distillation spike is also < 75% or not performed, qualify the affected data as
estimated low (J-). If the %R for the post-distillation spike is > 75%, qualify the affected
data as estimated (J).
6. If the Matrix Spike %R falls within the range of 30-74%> and the sample results are non-
detects, qualify the affected data as estimated (UJ).
7. If the Matrix Spike %>R is > 125%> and the reported sample results are non-detects, the
sample data should not be qualified.
8. If the Matrix Spike %>R is > 125%) and the sample results are > MDL, verify that a post-
distillation spike was analyzed if required. If the %>R for the post-distillation spike is also
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> 125% or is not performed, qualify the affected data as estimated high (J+). If the %R
for the post-distillation spike is < 125%, qualify the affected data as estimated (J).
9. Note the potential effects on the data due to out-of-control spiked sample results in the
Data Review Narrative.
Table 10. Spike Sample Actions for Cyanide Analysis
Spike Sample Results
Action for Samples
Matrix Spike %R < 30%
Post-distillation spike %R < 75%
Qualify affected results that are > MDL as estimated low
(J-) and affected non-detects as unusable (R)
Matrix Spike %R < 30%
Post-distillation spike %R > 75%
Qualify affected results that are > MDL as estimated (J)
and affected non-detects as estimated (UJ)
Matrix Spike %R 30-74%
Post-distillation Spike %R< 75%
Qualify affected results that are > MDL as estimated low
(J-) and affected non-detects as estimated (UJ)
Matrix Spike %R 30-74%
Post-distillation spike %R > 75%
Qualify affected results that are > MDL as estimated (J)
and affected non-detects as estimated (UJ)
Matrix Spike %R > 125%)
Post-distillation spike %R > 125%
Qualify affected results that are > MDL as estimated high
(J+)
Matrix Spike %R > 125%)
Post-distillation spike %R < 125%
Qualify affected results that are > MDL as estimated (J)
Matrix Spike %R < 30%
No post-distillation spike performed
Qualify affected results that are > MDL as estimated low
(J-) and affected non-detects as unusable (R)
Matrix Spike %R 30-74%
No post-distillation spike performed
Qualify affected results that are > MDL as estimated low
(J-) and non-detects as estimated (UJ)
Matrix Spike %R > 125%)
No post-distillation spike performed
Qualify affected results that are > MDL as estimated high
(J+)
Non-detects are not qualified
Matrix Spike %R 75-125%
No post-distillation spike performed
No Qualification.
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Mercury/Cyanide Field Duplicates
Action:
NOTES: For field duplicates that do not meet the technical criteria, apply the action to only
the field sample and its duplicate. If it is clearly stated in the data validation
materials that the samples were taken through incremental sampling or some other
method guaranteeing the homogeneity of the sample group, then the entire sample
group may be qualified.
Check the Sampling Trip Report for the field duplicate pair.
Substitute MDL for CRQL when MDL > CRQL.
Do not calculate RPD when both values are non-detects.
If one value is > the CRQL and the other value is non-detect, calculate the
absolute difference between the value > the CRQL and the MDL, and use this
criteria to qualify the results.
1. If a field duplicate pair was collected and analyzed, calculate and report the RPD when
the sample and its field duplicate values are both > 5x the CRQL. Calculate and report
the absolute difference when at least one value (sample or duplicate) is < 5x the CRQL.
2. When aqueous sample and duplicate values are both > 5x the CRQL, and the RPD is >
20%, qualify the sample and its duplicate as estimated (J).
3. When aqueous sample and/or the duplicate value is < 5x the CRQL, and the absolute
difference is > the CRQL, qualify results > the MDL as estimated (J) and non-detects as
estimated (UJ).
4. When soil/sediment sample and duplicate values are both > 5x the CRQL, and the RPD is
> 50%, qualify the sample and its duplicate as estimated (J).
5. When soil/sediment sample and/or the duplicate value is < 5x the CRQL, and the
absolute difference is > 2x the CRQL, qualify results > the MDL as estimated (J) and
non-detects as estimated (UJ).
Table 11. Field Duplicate Actions for Mercury/Cyanide Analysis
Sample Type
Field Duplicate Result
Action for Samples
Aqueous
Sample and its field duplicate > 5x
the CRQL and RPD > 20%
Qualify sample and its duplicate as
estimated (J)
Sample and/or its field duplicate <
5x the CRQL and absolute
difference > the CRQL
Qualify results > the MDL as
estimated (J)
Qualify non-detects as estimated (UJ)
Soil/Sediment
Sample and its field duplicate > 5x
the CRQL and RPD > 50%
Qualify sample and its duplicate as
estimated (J)
Sample and/or its field duplicate <
5x the CRQL and absolute
difference > 2x the CRQL
Qualify results > the MDL as
estimated (J)
Qualify non-detects as estimated (UJ)
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Mercury/Cyanide Field/Rinsate/Trip Blanks
Action:
NOTE: Designate "Field Blank" as such on Form IA.
Field Blank results previously rejected due to other criteria cannot be used to
qualify field samples.
Do not use Rinsate Blank associated with soils to qualify water samples and vice
versa.
If the MDL is > the CRQL, substitute CRQL with 2x the MDL.
1. If the appropriate blanks were not analyzed with the correct frequency, the data reviewer
should use professional judgment to determine if the associated sample data should be
qualified. The reviewer may need to obtain additional information from the laboratory.
The situation should then be recorded in the Data Review Narrative, and noted for
Contract Laboratory Program Project Officer (CLP PO) action.
2. Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. The reviewer should note that 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.
3. Some general "technical" review actions include:
a. Any blank reported with a negative result, whose value is < (-MDL) but > (-
CRQL), should be carefully evaluated to determine its effect on the sample data.
The reviewer shall then use professional judgment to assess the data. For any
blank reported with a negative result, whose value is < (-CRQL) qualify results
that are > CRQL as estimated low (J-) and non-detects as estimated (UJ).
b. The blank analyses may not involve the same weights, volumes, or dilution
factors as the associated samples. In particular, soil/sediment sample results
reported on Form I-IN will not be on the same basis (units, dilution) as the
calibration blank data reported on Form III-IN. The reviewer may find it easier to
work with the raw data.
4. If the absolute value of mercury/cyanide in a Field/Rinsate/Trip Blank is > the CRQL,
then the CRQL shall be raised to the level in the Field/Rinsate/Trip Blank and the
associated sample data below this level shall be reported as CRQL-U.
5. Sample results > the Field/Rinsate/Trip Blank value but < lOx the Field/Rinsate/Trip
Blank value shall be qualified as estimated (J).
6. Sample results > the MDL but < the CRQL shall be reported at the CRQL value with a
"U".
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Table 12. Field/Rinsate/Trip Blank Actions for Mercury/Cyanide Analysis
Blank Result
Sample Result
Action for Samples
> CRQL
> MDL but < CRQL
Report CRQL value with a "U"
> CRQL but < Blank Result
Report at level of Blank Result with
a "U"
> Blank Result but < lOx the
Blank Result
Use professional judgment to
qualify results as estimated (J)
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Mercury/Cyanide Linear Ranges
Action:
1. If any sample result was higher than the highest calibration standard for mercury/cyanide
and the sample was not diluted to obtain the result reported on Form I, qualify the
affected results > MDL as estimated (J).
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Mercury/Cyanide Percent Solids of Sediments
Action:
1. If the percent solids in sediment for a sample are < 50%, qualify the affected results >
MDL as estimated (J) and the non-detects as estimated (UJ).
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Regional Quality Assurance (OA) and Quality Control (OC)
Action:
Any action must be in accordance with Regional specifications and criteria for acceptable PE
sample results. Note any unacceptable PE sample results for Contract Laboratory Program
Project Officer (CLP PO) action.
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Overall Assessment
Action:
1. Use professional judgment to determine if there is any need to qualify data which were
not qualified based on the QC criteria previously discussed.
2. Write a brief Data Review Narrative to give the user an indication of the analytical
limitations of the data. Note any discrepancies between the data and the Sample Delivery
Group (SDG) Narrative for Contract Laboratory Program Project Officer (CLP PO)
action. If sufficient information on the intended use and required quality of the data is
available, the reviewer should include an assessment of the data usability within the given
context.
3. If any discrepancies are found, the laboratory may be contacted by the Region's
designated representative to obtain additional information for resolution. If a discrepancy
remains unresolved, the reviewer may determine that qualification of the data is
warranted.
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Calculations for Mercury
Aqueous/Water Samples:
fV-9\
Hg Concentration (— I = C x DF
Where,
C = Instrument value in [j,g/L from the calibration curve
DF = Dilution Factor
Soil/Sediment Samples:
(mg\ 1 DF
Hq Concentration -— = C x ——- x ——
^ \kg) WxS 10
Where,
C = Instrument value in p,g/L from the calibration curve
W = Initial aliquot amount (g)
„ _ % Solids/100 (see Exhibit D of ISM02.2 - Introduction to Analytical Methods,
Section 1.6).
DF = Dilution Factor
Adjusted Method Detection Limit (MDL)/Adjusted Contract Required Quantitation Limit
(CRQL) Calculation:
To calculate the adjusted MDL or adjusted CRQL for aqueous/water samples, multiply
the value of the MDL ((J,g/L) or CRQL ((J,g/L) by the Dilution Factor (DF). Calculate the
adjusted MDL or adjusted CRQL for soil/sediment samples as follows:
(mg\ WM
Adjusted Concentration -— = C x x DF
1 \kg J WxS
Where,
C = MDL or CRQL (mg/kg)
Wm = Minimum method required aliquot amount (g) (0.50 g)
W = Initial aliquot amount (g)
„ _ %Solids/100 (see Exhibit D of ISM02.2 - Introduction to Analytical Methods,
Section 1.6).
DF = Dilution Factor
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Calculations for Cyanide
Aqueous/Water Sample Concentration:
mg\ Vf
CN Concentration J = C x — x DF
^ L ' V
Where,
C = Instrument value in [j,g/L CN from the calibration curve
Vf = Final prepared (absorbing solution) volume (mL)
V = Initial aliquot amount (mL)
DF = Dilution Factor
Soil/Sediment Sample Concentration:
/mg\ Vf DF
CN Concentration -— = C x x
\kg) WxS 1000
Where,
C = Instrument value in [j,g/L CN from the calibration curve
Vf = Final prepared (absorbing solution) volume (mL)
W = Initial aliquot amount (g)
„ _ %Solids/100 (see Exhibit D of ISM02.2 - Introduction to Analytical Methods,
Section 1.6)
DF = Dilution Factor
Adjusted Method Detection Limit (MDL)/Adjusted Contract Required Quantitation Limit
(CRQL) Calculation:
To calculate the adjusted MDL or adjusted CRQL for aqueous/water samples, follow the
instructions in Exhibit D of ISM02.2 - Data Analysis and Calculations, Section 11.1.1.
Calculate the adjusted MDL or adjusted CRQL for soil/sediment samples as follows:
(mg\ WM
Adjusted Concentration -— = C x ——- x DF
J \kg) WxS
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Wm
Where,
C = MDL or CRQL (mg/kg)
= Minimum method required aliquot amount (g) (1.00 g for Midi or 0.50 g for
Micro)
W = Initial aliquot amount (g)
„ = %Solids/100 (see Exhibit D of ISM02.2 - Introduction to Analytical Methods,
Section 1.6)
DF = Dilution Factor
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APPENDIX A: GLOSSARY
Analyte — The element of interest, ion, or parameter an analysis seeks to determine.
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 solution or media introduced into an instrument on which an analysis
is performed excluding instrument calibration, Initial Calibration Verification (ICV), Initial
Calibration Blank (ICB), Continuing Calibration Verification (CCV), and Continuing Calibration
Blank (CCB). Note that the following are all defined as analytical samples: undiluted and diluted
samples (USEPA and non-USEPA); Matrix Spike samples; duplicate samples; serial dilution
samples, analytical (post-digestion/post-distillation) spike samples; Interference Check Samples
(ICSs); Laboratory Control Samples (LCSs); and Preparation Blanks.
Associated Samples — Any sample related to a particular Quality Control (QC) analysis. For
example, for Initial Calibration Verification (ICV), all samples run under the same calibration
curve. For duplicates, all Sample Delivery Group (SDG) samples digested/distilled of the same
matrix.
Blank — A sample designed to assess specific sources of contamination. See individual
definitions for types of blanks.
Calibration — The establishment of an analytical curve based on the absorbance, emission
intensity, or other measured characteristic of known standards. The calibration standards are to
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 of the reagents in the same concentration
as those used in the analytical sample preparation. This blank is not subject to the preparation
method.
Calibration Curve — A plot of instrument response versus concentration of standards.
Calibration Standards — A series of known standard solutions used by the analyst for
calibration of the instrument (i.e., preparation of the analytical 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).
Continuing Calibration Blank (CCB) — A reagent water sample that is run 2 hours (ICP-AES,
ICP-MS) or every hour (Hg, CN) 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 USEPA 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 by the analyst and used to verify the stability of the instrument calibration with
time, and the instrument performance during the analysis of samples. The CCV can be one of the
calibration standards. However, all parameters being measured by the particular system must be
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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. The CCV should have a concentration in the
middle of the calibration range and shall be run every 2 hours (ICP-AES, ICP-MS) or every hour
(Hg, CN).
Contract Laboratory Program (CLP) — Supports the USEPA'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.
Contract Laboratory Program Project Officer (CLP PO) — The Regional USEPA official
responsible for monitoring laboratory performance and/or requesting analytical data or services
from a CLP laboratory.
Contract Required Quantitation Limit (CRQL) — Minimum level of quantitation acceptable
under the contract Statement of Work (SOW).
Duplicate — A second aliquot of a sample that is treated the same as the original sample in order
to determine the precision of the method.
Field Blank — Any sample that is submitted from the field and identified as a blank. A field
blank is used to check for cross-contamination during sample collection, sample shipment, and in
the laboratory. A field blank includes trip blanks, rinsate blanks, bottle blanks, equipment blanks,
preservative blanks, decontamination blanks, etc.
Field Duplicate — A duplicate sample generated in the field, not in the laboratory.
Holding Time — The maximum amount of time samples may be held before they are processed.
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.
Technical — The maximum amount of time that samples may be held from the collection date
until analysis.
Initial Calibration — Analysis of analytical standards for a series of different specified
concentrations to define the quantitative response, linearity, and dynamic range of the instrument
to target analytes.
Initial Calibration Blank (ICB) — The first blank standard run to confirm the calibration curve.
Initial Calibration Verification (ICV) — 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 should be traceable to National Institute of
Standards and Technology (NIST) or other certified standard sources when USEPA ICV
solutions are not available.
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.
Interference Check Sample (ICS) — Verifies the contract laboratory's ability to overcome
interferences typical of those found in samples.
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Laboratory Control Sample (LCS) — A control sample spiked at known level(s). LCSs are
processed using the same sample preparation, reagents, and analytical methods employed for the
USEPA samples received.
Matrix — The predominant material of which the sample to be analyzed is composed. For the
purposes of this document, the matrices are aqueous/water, soil/sediment, wipe, and filter.
Matrix Spike — Introduction of a known concentration of analyte into a sample to provide
information about the effect of the sample matrix on the digestion and measurement
methodology (also identified as a pre-distillation/digestion spike).
Method Detection Limit (MDL) — The concentration of a target parameter that, when a sample
is processed through the complete method, produces a signal with 99 percent probability that it is
different from the blank. For 7 replicates of the sample, the mean value must be 3.14s above the
blank, where "s" is the standard deviation of the 7 replicates.
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 USEPA office that provides
policy, guidance, and direction for the USEPA's solid waste and emergency response programs,
including Superfund.
Percent Difference (%D) — As used in this document and the Statement of Work (SOW), is
used to compare two values. The difference between the two values divided by one of the values.
Performance Evaluation (PE) Sample — A sample of known composition provided by USEPA
for contractor analysis. Used by USEPA to evaluate Contractor performance.
Post Digestion Spike — The addition of a known amount of standard after digestion or
distillation (also identified as an analytical spike).
Preparation Blank — An analytical control that contains reagent water and reagents, which is
carried through the entire preparation and analytical procedure.
Relative Percent Difference (RPD) — As used in this document and the Statement of Work
(SOW) to compare two values, the RPD is based on the mean of the two values, and is reported
as an absolute value (i.e., always expressed as a positive number or zero).
Regional Sample Control Center Coordinator (RSCC) — In USEPA 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, which 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:
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).
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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 Management Office (SMO) — A contractor-operated facility operated under the SMO
contract, awarded and administered by the USEPA. Provides necessary management, operations,
and administrative support to the Contract Laboratory Program (CLP).
Serial Dilution — The dilution of a sample by a factor of five. When corrected by the Dilution
Factor (DF), the diluted sample must agree with the original undiluted sample within specified
limits. Serial dilution may reflect the influence of interferents [Inductively Coupled Plasma (ICP)
only].
Statement of Work (SOW) — A document which specifies how laboratories analyze samples
under a particular Contract Laboratory Program (CLP) analytical program.
Tune — Analysis of a solution containing a range of isotope masses to establish Inductively
Coupled Plasma - Mass Spectrometry (ICP-MS) mass-scale accuracy, mass resolution, and
precision prior to calibration.
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APPENDIX B: INORGANIC DATA EXECUTIVE NARRATIVE TEMPLATE
Case Wo,:
Site;
SDGNo
Laboratorv:
QAPP
rows #:
Contractor »*:
Number of Samples:
Sampling da.ce:
SUMMARY:
Critical: Results have an unacceptable leval ofunnartainty and should not b* us»d for
making decisions.
Datahavs b san qtiiifiad "R rejjrtii.
Major: Alr.*»lofuncwtainty «im that may not m*it the data quality objastivas for tlis
projizt Abtis is likily to ba pusir.t in the nsults. Data bars bs«c qualified "F'
istimitKi.
Minor: Tie leval of ui;:iitiiuty is a;:iptibl». No signifcajit bias in th» data was
observed.
Critical Findinga; Hone
Major Fading*! None
Mm r Finding s: Non«
Signs tare:
Km:
AflSBntioBi
Date:
AjtjNrover's Signature:
Mans,#!
AffiKatiaa;
Date:
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APPENDIX C: SAMPLE INORGANIC DATA SAMPLE SUMMARY
l^eNo 00001 Contract XYZ1214
SDG No XY123
Lab Code A8CD
Sample Number XY123 Method ICP_AE8
Sample Location SOME WHERE OUT THERE pH 15
Mo:>rme
Matrix ^LU-r
Sample Date 13322053
*t Solldi
MA. Number: DEFAULT
Sample Time: 24:03:00
Analyte Name
Result
Units
Dilution Factor
Lab Flag
Validation
Reportable
Validation Level
Aluminum
400
ug L
I
Yes
S2BYEM
Antimony
40
ug.L
I
U
V
Yes
S2BYEM
Arsenic
«
ug L
1
u
U
Yes
S2BYEM
Banum
40
I
u
V
Yes
s:b\~em
Beryllium
40
its L
1
r
V
Yes
S2BYEM
C actinium
40
ug L
1
u
u
Ye 4
s:byem
C .iknun
400
ug L
1
Yes
S2BYEM
C hroimum
40
us L
1
u
u
Yes
S-BYEM
C obalt
40
ug'L
1
u
V
Yes
S2BYEM
Copper
40
ue L
1
V
V
Yes
S2BYEM
lion
40
ugX
1
j
u
Yes
S2BYEM
Lead
40
Bg/L
1
u
u
Yes
S2BYEM
Magnesium
400
ug/t
1
Yes
S2BYEM
MaugMiese
400
«g/L
1
Yes
S2BYEM
"Nickel
40
ug L
1
V
V
Yes
S2BYEM
Potassium
400
us L
1
Yes
S2BYEM
Selenium
40
ua'L
1
u
u
Yes
S2BYEM
Stiver
40
us L
1
u
u
Yes
S2BYEM
Sodium
400
ug'L
1
Yes
S2BYEM
Thallium
40
us L
I
u
u
Yes
S2BYEM
Y.uudiuin
40
ug L
1
u
u
Yes
S2BYEM
Zmc
40
ug L
1
u
u
Yes
S2BYEM
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APPENDIX D: ELECTRONIC DATA DELIVERABLE TEMPLATE
DATA PROVIDER
LAB MATRIX CODE
RESULT UNIT
SYS SAMPLE CODE
ANAL LOCATION
DETECTION LIMIT UNIT
SAMPLE NAME
BASIS
TIC RETENTION TIME
SAMPLE MATRIX CODE
CONTAINER ID
RESULT COMMENT
SAMPLE TYPE CODE
DILUTION FACTOR
QC ORIGINAL CONC
SAMPLE SOURCE
PREP METHOD
QC SPIKE ADDED
PARENT SAMPLE CODE
PREP DATE
QC SPIKE MEASURED
SAMPLE DEL GROUP
LEACHATE METHOD
QC SPIKE RECOVERY
SAMPLE DATE
LEACHATE DATE
QC DUP ORIGINAL CONC
SYS LOC CODE
LAB NAME CODE
QC DUP SPIKE ADDED
START DEPTH
QC LEVEL
QC DUP SPIKE MEASURED
END DEPTH
LAB SAMPLE ID
QC DUP SPIKE RECOVERY
DEPTH UNIT
PERCENT MOISTURE
QC RPD
CHAIN OF CUSTODY
SUB SAMPLE AMOUNT
QC SPIKE LCL
SENT TO LAB DATE
SUB SAMPLE AMOUNT UNIT
QC SPIKE UCL
SAMPLE RECEIPT DATE
ANALYST NAME
QC RPD CL
SAMPLER
INSTRUMENT ID
QC SPIKE STATUS
SAMPLING COMPANY CODE
COMMENT
QC DUP SPIKE STATUS
SAMPLING REASON
PRESERVATIVE
QC RPD STATUS
SAMPLING TECHNIQUE
FINAL VOLUME
BREAK 2
TASK CODE
FINAL VOLUME UNIT
SYS SAMPLE CODE
COLLECTION QUARTER
CAS RN
LAB ANL METHOD NAME
COMPOSITE YN
CHEMICAL NAME
ANALYSIS DATE
COMPOSITE DESC
RESULT VALUE
TOTAL OR DISSOLVED
SAMPLE CLASS
RESULT ERROR DELTA
COLUMN NUMBER
CUSTOM FIELD 1
RESULT TYPE CODE
TEST TYPE
CUSTOM FIELD 2
REPORTABLE RESULT
TEST BATCH TYPE
CUSTOM FIELD 3
DETECT FLAG
TEST BATCH ID
COMMENT
LAB QUALIFIERS
CASE
BREAK 1
VALIDATOR QUALIFIERS
CONTRACT NUM
SYS SAMPLE CODE
INTERPRETED QUALIFIERS
SCRIBE SAMPLE ID
LAB ANL METHOD NAME
ORGANIC YN
SAMPLE TIME
ANALYSIS DATE
METHOD DETECTION LIMIT
FRACTION
TOTAL OR DISSOLVED
REPORTING DETECTION LIMIT
PH
COLUMN NUMBER
QUANTITATION LIMIT
DATA VAL LABEL
TEST TYPE
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APPENDIX E: REQUEST FOR STANDARD OPERATING (SOP) PROCEDURE
CHANGE
&EPA
Request I'nr Simulant I I'rort-ilurr (M II*) < luin«jc
In Im maiims
Injij.M.u i h \iK ih '• U k ?:N n ^ ''1\U» Mf!:
S i.-fviihr-v');! N.umv J i\\ s»S m k:m«:v.v< f} V - Y '.'e\ \ w)\ \ssmk i ik
\< >r htk N k-K ufv ami < \ viuuU; 1 MLi \ j1h1,»H4,'M
| ; M.i|s^r Kc\ f -I.'li ['1 \ 1 U W ^
< -<> i f:hniai! if iicu">vu\ r
V.kl ihv* whon \K rct*r\ ( % :u*h)c Pi i t i nt SulkK of
NOTKS:
Rcsuhs between the MS )i and (knl ! > Utoinschos „uc
)u>i reported.
: !•>; vh th'Vi s .
I hoc ciKMiin vUhkvn w v'K1 not ,uKu\"ss,'d u: (hi-. \ ci n»up . -i I he St H*
Aj^ro* :il
" v.,. , .< V
J ./ •i.J.l/J...
rex/
------- |