OLEM 9240.1-66
EPA 542-R-20-006
November 2020
NATIONALFUNCTIONALGUIDELINES
for Inorganic Superfund Methods Data Review
\>EPA
Office of Superfund Remediation and Technology Innovation (OSRTI)
United States Environmental Protection Agency (EPA)
Washington, DC 20460

-------
This page is intentionally left blank.
November 2020

-------
NOTICE
The policies and procedures set forth here are intended as guidance to the United States Environmental
Protection Agency (EPA) and other governmental employees. They do not constitute rule making by the
EPA, 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 EPA's Superfund Analytical Services and Contract Laboratory
Program website at:
https://www.epa.gov/clp/contract-laboratorv-program-national-functional-guidelines-data-review
November 2020
iii

-------
This page is intentionally left blank.
November 2020	iv

-------
Inorganic Data Review
TABLE OF CONTENTS
TABLE OF CONTENTS	v
LIST OF TABLES	vii
ACRONYMS AND ABBREVIATIONS	ix
I. Terminology	ix
INTRODUCTION	1
I.	Purpose of Document	1
II.	Data Reviewer Considerations	1
TIT Document Organization	2
IV. Additional Information	2
PART A: GENERAL DATA REVIEW	3
I.	Preliminary Review	5
II.	Data Qualifier Definitions	6
III.	Data Review Narrative	7
IV.	Performance Evaluation (PE) Sample	7
V.	Field Quality Assurance and Quality Control (QA/QC)	8
VI.	Overall Assessment of Data	9
PART B: METHOD-SPECIFIC DATA REVIEW	13
ICP-AES DATA REVIEW	15
I.	Preservation and Holding Times	17
II.	Calibration	19
III.	Blanks	22
IV.	Interference Check Sample	26
V.	Laboratory Control Sample	29
VI.	Duplicate Sample Analysis	31
VII.	Spike Sample Analysis	33
VIII.	Serial Dilution	36
IX.	Target Analyte Quantitation	38
ICP-MS DATA REVIEW	41
I.	Preservation and Holding Times	43
II.	Tune Analysis	45
III.	Calibration	47
IV.	Blanks	50
V.	Interference Check Sample	53
VI.	Laboratory Control Sample	55
VII.	Duplicate Sample Analysis	57
VIII.	Spike Sample Analysis	59
IX.	Serial Dilution	62
X.	Internal Standards	64
XI.	Target Analyte Quantitation	66
MERCURY DATA REVIEW	69
I.	Preservation and Holding Times	71
II.	Calibration	73
III.	Blanks	76
IV.	Duplicate Sample Analysis	80
V.	Spike Sample Analysis	82
November 2020	v

-------
Inorganic Data Review
VI. Target Analyte Quantitation	84
CYANIDE DATA REVIEW	87
I.	Preservation and Holding Times	89
II.	Calibration	91
III.	Blanks	94
IV.	Duplicate Sample Analysis	98
V.	Spike Sample Analysis	100
VI.	Target Analyte Quantitation	103
ANIONS DATA REVIEW	105
I.	Preservation and Holding Times	107
II.	Calibration	109
III.	Blanks	112
IV.	Laboratory Control Sample	115
V.	Duplicate Sample Analysis	117
VI.	Spike Sample Analysis	119
VII.	Target Analyte Quantitation	121
HEXAVALENT CHROMIUM DATA REVIEW	123
I.	Preservation and Holding Times	125
II.	Calibration	127
III.	Blanks	130
IV.	Laboratory Control Sample	133
V.	Duplicate Sample Analysis	135
VI.	Spike Sample Analysis	137
VII.	Target Analyte Quantitation	139
TOTAL ORGANIC CARBON (TOC) DATA REVIEW	141
I.	Preservation and Holding Times	143
II.	Calibration	145
III.	Blanks	148
IV.	Laboratory Control Sample	151
V.	Duplicate Sample Analysis	153
VI.	Spike Sample Analysis	155
VII.	Target Analyte Quantitation	157
APPENDIX A: GLOSSARY	A-l
APPENDIX B: INORGANIC DATA REVIEW SUMMARY	B-l
November 2020	vi

-------
Inorganic Data Review
LIST OF TABLES
GENERAL DATA REVIEW
General Table 1. Data Qualifiers and Definitions	6
General Table 2. PE Sample Actions	8
ICP-AES DATA REVIEW
ICP-AES Table 1. Preservation and Holding Time Actions	18
ICP-AES Table 2. Calibration Actions	21
ICP-AES Table 3. Blank Actions	24
ICP-AES Table 4. Interference Check Actions	27
ICP-AES Table 5. LCS Actions	30
ICP-AES Table 6. Duplicate Sample Actions	32
ICP-AES Table 7. Spike Sample Actions	34
ICP-AES Table 8. Serial Dilution Actions	37
ICP-MS DATA REVIEW
ICP-MS Table 1. Preservation and Holding Time Actions	44
ICP-MS Table 2. Tune Actions	46
ICP-MS Table 3. Calibration Actions	49
ICP-MS Table 4. Blank Actions	51
ICP-MS Table 5. Interference Check Actions	54
ICP-MS Table 6. LCS Actions	56
ICP-MS Table 7. Duplicate Sample Actions	58
ICP-MS Table 8. Spike Sample Actions	60
ICP-MS Table 9. Serial Dilution Actions	63
ICP-MS Table 10. Internal Standard Actions	65
MERCURY DATA REVIEW
Mercury Table 1. Preservation and Holding Time Actions	72
Mercury Table 2. Calibration Actions	75
Mercury Table 3. Blank Actions	78
Mercury Table 4. Duplicate Sample Actions	81
Mercury Table 5. Spike Sample Actions	83
CYANIDE DATA REVIEW
Cyanide Table 1. Preservation and Holding Time Actions	90
Cyanide Table 2. Calibration Actions	93
Cyanide Table 3. Blank Actions	96
Cyanide Table 4. Duplicate Sample Actions	99
Cyanide Table 5. Spike Sample Actions	101
ANIONS DATA REVIEW
Anions Table 1. Preservation and Holding Time Actions	108
Anions Table 2. Calibration Actions	Ill
Anions Table 3. Blank Actions	113
Anions Table 4. LCS Actions	116
Anions Table 5. Duplicate Sample Actions	118
Anions Table 6. Spike Sample Actions	120
HEXAVALENT CHROMIUM DATA REVIEW
Hexavalent Chromium Table 1. Preservation and Holding Time Actions	126
Hexavalent Chromium Table 2. Calibration Actions	129
Hexavalent Chromium Table 3. Blank Actions	131
November 2020	vii

-------
Inorganic Data Review
Hexavalent Chromium Table 4. LCS Actions	134
Hexavalent Chromium Table 5. Duplicate Sample Actions	136
Hexavalent Chromium Table 6. Spike Sample Actions	138
TOTAL ORGANIC CARBON (TOC) DATA REVIEW
TOC Table 1. Preservation and Holding Time Actions	144
TOC Table 2. Calibration Actions	147
TOC Table 3. Blank Actions	149
TOC Table 4. LCS Actions	152
TOC Table 5. Duplicate Sample Actions	154
TOC Table 6. Spike Sample Actions	156
November 2020	viii

-------
Inorganic Data Review
ACRONYMS AND ABBREVIATIONS
I. Terminology
The following acronyms and abbreviations are applicable to this document. For definitions, see
Appendix A: Glossary at the end of the document.
%D
Percent Difference
%R
Percent Recovery
%RI
Percent Relative Intensity
%RSD
Percent Relative Standard Deviation
%Solids
Percent Solids
CCB
Continuing Calibration Blank
CCV
Continuing Calibration Verification
CLP
Contract Laboratory Program
CLPSS
Contract Laboratory Program Support System
COC
Chain of Custody
DF
Dilution Factor
DL
Detection Limit
DQA
Data Quality Assessment
DQO
Data Quality Objectives
EDM
EXES Data Manager
EPA
United States Environmental Protection Agency
EXES
Electronic Data Exchange and Evaluation System
IC
Ion Chromatography
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
NFG
National Functional Guidelines
OSRTI
Office of Superfund Remediation and Technology Innovation
PE
Performance Evaluation
PDF
Portable Document Format
QA
Quality Assurance
November 2020
ix

-------
Inorganic Data Review
QAPP	Quality Assurance Project Plan
QC	Quality Control
QL	Quantitation Limit
RPD	Relative Percent Difference
SAP	Sampling and Analysis Plan
SEDD	Staged Electronic Data Deliverable
SMO	Sample Management Office
SOP	Standard Operating Procedure
SOW	Statement of Work
SPLP	Synthetic Precipitation Leaching Procedure
TCLP	Toxicity Characteristic Leaching Procedure
TDS	Total Dissolved Solids
TOC	Total Organic Carbon
TSS	Total Suspended Solids
November 2020
x

-------
Inorganic Data Review
Introduction
INTRODUCTION
I.	Purpose of Document
This document provides guidance to aid in the evaluation and documentation of the quality of
analytical data generated for metals by Inductively Coupled Plasma - Atomic Emission Spectroscopy
(ICP-AES), metals by Inductively Coupled Plasma - Mass Spectrometry (ICP-MS), mercury,
cyanide, anions by Ion Chromatography (IC), hexavalent chromium by IC, and Total Organic Carbon
(TOC).
The guidelines presented in this document have been designed to assist United States Environmental
Protection Agency (EPA) Regional offices in evaluating (a) whether the analytical data meet the
technical and Quality Control (QC) criteria established in the project-specific Quality Assurance
Project Plan (QAPP) or in the EPA Superfund Contract Laboratory Program (CLP) Statement of
Work (SOW), and (b) the uncertainty and extent of bias of any data that do not meet these criteria.
These guidance documents have also been used by many outside the CLP community and outside
EPA who evaluate analytical chemistry data, because of the attention to detail, and the decision
matrices in each section.
The specific criteria and QC limits, on which the National Functional Guidelines (NFG) data
qualification recommendations are based, are from the EPA CLP SOW due to the fact that these
guidelines are primarily used for the review and validation of CLP data, both electronically and
manually. The criteria provided in a project-specific QAPP will take precedence over those in the
EPA CLP SOW. It is recognized that some criteria may have become standard for a particular
analytical method. However, when utilizing the NFG for non-CLP data review, the criteria used
should come from the project-specific QAPP (if available), reference method, or applicable Standard
Operating Procedures (SOPs). Therefore, the source of the criteria used for the review should be
clearly documented in the Data Review Narrative.
This document contains guidance for evaluating data quality in areas such as blanks, calibration and
verification, instrument performance checks and performance evaluation samples, in which
performance is fully under a laboratory's control, as well as more general guidance to aid in making
subjective judgments regarding the quality of data for their use in making site decisions.
II.	Data Reviewer Considerations
The guidance provided herein does not eliminate the need to consult other sources of information or
to use professional judgment. Professional judgment is not frequently called for in this guidance
document, but it is essential, in consideration of the intended use of the data. It is frequently necessary
for making the best decision regarding data quality when multiple factors are involved and two
qualifiers are presented. Reliable professional judgment comes from experience gained as a result of
extensive training received from experts, having performed the subject analyses, and from having
reviewed other analysts' and/or laboratories' data generated with similar procedures. The Action
section, in each data element subchapter, provides guidance to assist the reviewer to make the most
appropriate decision on how to represent data quality.
Data quality is impacted by many factors including procedures and events that may have occurred
before the samples arrived at the laboratory. The reviewer would need to have knowledge of these
factors, as well as a complete understanding of the project goals in order to make appropriate
judgments about data usability. Ultimately, these decisions should be made by project management
personnel, using the data review reports which are the product of following this guidance document,
in addition to other information available to them.
Effective use of this guidance document requires the reviewer to understand the cited reference
method(s) and underlying chemistry, the data quality requirements of the project, and the data
provided by the laboratory. The reviewer is advised to evaluate all information provided by the
laboratory to gain a complete understanding of data quality issues. Additional information may be
November 2020
1

-------
Inorganic Data Review
Introduction
needed from the laboratory that was not included in the data package and may be requested as
needed. Findings from the review should be thoroughly documented in the Data Review Narrative,
including additional explanation as needed where professional judgment was applied.
III.	Document Organization
Following this introduction, the document is presented in two major parts: Part A - General Data
Review, which applies to all methods; and Part B - Method-Specific Data Review. In Part B, the
review procedures are addressed for each method in a stand-alone format. A complete list of
acronyms used in this document appears preceding this Introduction, and a Glossary is included as
Appendix A. An Inorganic Data Review Summary is included as Appendix B.
IV.	Additional Information
For additional information about EPA methods and guidance, refer to the links below.
Guidance on Environmental Data Verification and
Data Validation, EPA QA/G-8
https://www.epa.eov/aualitv/euidance-
environmental-data-verification-and-data-
validation
EPA's Contract Laboratory Program (CLP)
https: //www. epa. eov/clp
EPA CLP Statement of Work for Superfund
Analytical Methods (SOW)
https: //www .epa. eov/clp/epa-contract-laboratorv-
proeram-statement-work-superfiind-analvtical-
methods-multi-media-multi-0
Guidance for Labeling Externally Validated
Laboratory Analytical Data for Superfund Use
https://www.epa.eov/clp/superfund-clp-analvtical-
services-euidance-documents
Hazardous Waste Test Methods (SW-846)
https://www.epa.eov/hw-sw846
Clean Water Act Analytical Methods
https: //www .epa. eov/cwa-methods
November 2020
2

-------
Inorganic Data Review	General
PART A: GENERAL DATA REVIEW
November 2020
3

-------
Inorganic Data Review	General
This page is intentionally left blank.
November 2020
4

-------
Inorganic Data Review
General
I. Preliminary Review
A preliminary review of the data should be performed, prior to performing the method-specific
review (Part B). During this process, the necessary elements should be compiled to ensure all
information needed for validation is available and to obtain an overview of the data.
This preliminary review should include, but is not limited to, the verification of the exact number of
samples, their matrix type(s), assigned identifiers (IDs) and analyses. It should take into consideration
all the documentation specific to the sample data package, which may include any modifications to
the project-specific Quality Assurance Project Plan (QAPP), Standard Operating Procedures (SOPs),
or United States Environmental Protection Agency (EPA) Superfund Contract Laboratory Program
(CLP) Statement of Work (SOW) used to generate the data, the sampling documentation [e.g., Chain
of Custody (COC) Records], the associated data package narrative, and other applicable documents.
Sampling events and data packages routinely contain unique field quality control (QC) samples that
may affect the outcome of the review. These samples include field blanks (e.g., equipment blanks,
rinse blanks), field duplicates, and Performance Evaluation (PE) samples that should be identified in
the sampling records. The reviewer should verify that the following information is identified in the
sampling records (e.g., COC Records, field logs, and/or applicable tables):
1. The party responsible for collecting the samples,
The complete list of samples with information on
a.
Sample ID
b.
Sample matrix
c.
Field blanks (if applicable)
d.
Field duplicates (if applicable)
e.
Field spikes (if applicable)
f.
PE samples (if applicable)
g-
Sampling dates
h.
Sampling times
i.
Shipping dates
j-
Preservatives
k.
Types of analysis
1.
Laboratory
The laboratory's data package narrative is another source of general information which may include
notable problems with matrices; insufficient sample volume for analysis or reanalysis; samples
received in broken containers; preservation information, verified by the laboratory; example
calculation(s) used to produce the results; and unusual events. The reviewer should also inspect email
or telephone/communication logs in the data package detailing any discussion of sample logistics,
preparation and/or analysis issues between the laboratory and project manager or other point of
contact. The reviewer should also have a copy of the QAPP, or similar document for the project for
which samples were analyzed, to assist in the validation.
For data obtained through the EPA CLP, the Staged Electronic Data Deliverable (SEDD) generated
by the CLP laboratories is subjected to the following reviews via the Electronic Data Exchange and
Evaluation System (EXES): 1) automated data assessment for compliance with the technical and QC
criteria in the applicable EPA CLP SOW, and 2) automated data validation based on the criteria in the
EPA CLP National Functional Guidelines (NFG) for the applicable Superfund methods. When a
choice of data qualifiers is presented during the data validation process, the qualifier that is more
November 2020
5

-------
Inorganic Data Review
General
protective of human health is selected. For example, the "J" qualifier, which designates a value as
estimated, would be selected over the "R" qualifier, which designates a value as rejected. In addition,
completeness checks are manually performed on the data in the Portable Document Format (PDF)
version of the hardcopy. The results of the SEDD and PDF data review issues are subsequently
included in a method compliance defect report that is provided to the laboratory and the data
requester. The laboratory may then submit a reconciliation package for any missing items or to
correct non-compliant data identified in the method compliance report. The automated data validation
results are summarized in criteria-based NFG reports, which consist of various data summary reports
(e.g., Initial Calibration Data Summary) generated from the SEDD, that are provided to the data
users. The method compliance review and NFG reports can be accessed through the EXES Data
Manager (EDM) via the Superfund Analytical Services Sample Management Office (SMO) Contract
Laboratory Program Support System (CLPSS) Portal and may be used to assist with the validation
process. EXES and EDM can be accessed via the Superfund Analytical Services SMO CLPSS Portal
at: https://www.smoclpss.com.
II. 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. If the reviewer chooses to use
additional qualifiers, a complete explanation of those qualifiers should accompany the data review in
the Data Review Narrative.
General Table 1. Data Qualifiers and 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.
NOTE: 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".
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.
November 2020
6

-------
Inorganic Data Review
General
III.	Data Review Narrative
The reviewer should complete a Data Review Narrative, to include comments that address the
problems identified during the review process and state the limitations of the data related to meeting
project Data Quality Objectives (DQO). The sample identifiers, analytical methods, extent of the
problem(s), and any assigned qualifiers should also be listed in the document. Note that QAPP,
reference method or SOP-specified acceptance criteria may differ from the EPA CLP SOW-specified
acceptance criteria on which the NFG data qualification recommendations are based. Therefore, the
source of the criteria used for the data review and qualification should be clearly indicated. Additional
information in the Data Review Narrative should include, but not be limited to, calculation checks,
documentation of any approved deviations from the reference method and an explanation of any
laboratory-assigned data qualifiers in the data. Finally, the process of reviewing and qualifying the
data should be documented for future reference (i.e., using the Guidance for Labeling Externally
Validated Laboratory Analytical Data for Superfund Use) including the use of any professional
judgment.
The Data Review Narrative, potentially including a summary form like the Inorganic Data Review
Summary form (see Appendix B), should be provided with the laboratory data, marked with data
qualifiers as necessary, to the appropriate recipient(s), including the designated project management
personnel.
IV.	Performance Evaluation (PE) Sample
A.	Review Items
Laboratory Results Reports, sampling documentation (e.g., COC Records), sample receipt forms,
preparation logs, instrument printouts, and raw data.
B.	Objective
The objective is to determine the validity of the analytical results based on the recoveries of analytes
of known concentrations in the PE sample(s). Data associated with PE samples can be used as an
additional evaluation of measurement uncertainty or bias for field samples prepared along with PE
samples.
C.	Criteria
Matrix-specific PE samples should be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by the data user or QAPP. PE samples should be prepared and analyzed together with the
field samples in the data package for the sampling event, using the same procedures, reagents, and
instrumentation. Measured concentrations in PE samples are compared to pre-defined acceptance
criteria developed and supplied by the PE provider or otherwise appropriate acceptance criteria for
the project.
D.	Evaluation
1.	Verify that the PE samples were prepared and analyzed with the field samples and/or field blanks
in the data package, using the Laboratory Results Reports, preparation logs, and raw data.
2.	Verify that the PE sample results are within the specified concentration or recovery limits using
Laboratory Results Reports and any raw data.
3.	If a significant number (e.g., half or more) of the analytes or any specific target analytes critical to
the project in the PE samples fall outside of the acceptance limits in the PE sample(s), or if a
number of false positive results are reported, evaluate the overall impact on the data. Consider all
possible reasons for this finding, including laboratory procedures, changes in the analytical
system, and the PE samples themselves.
November 2020
7

-------
Inorganic Data Review
General
E. Action
Refer to General Table 2 for the evaluation criteria and corresponding actions for detected and non-
detected target analytes in the samples associated with deficient PE sample(s).
1. Obtain additional information from the laboratory if the PE sample was not prepared and
analyzed with the field samples and/or field blanks. If a laboratory did not prepare or analyze the
PE sample(s) provided with field samples and field blanks, or if a laboratory repeatedly fails to
generate acceptable PE sample results for the same method and analyte(s), record the situation in
the Data Review Narrative, and note it for designated project management personnel action.
NOTE: If the PE sample acceptance criteria are not met, the laboratory performance and
measurement accuracy may be in question. For a PE sample that does not meet the
technical acceptance criteria, the reviewer should consider applying the same
interpretation to all samples prepared together. Qualification of field sample data based
on PE sample performance may be most appropriate for those samples in which the
analyte concentration is comparable to the PE sample concentration. Actions should
apply only to specified target analytes that did not meet the PE sample acceptance criteria
unless the failures indicate a problem with a broader scope.
2. Note the potential effects on the data due to out-of-control PE sample results in the Data Review
Narrative.
General Table 2. PE Sample Actions
Criteria
Action
Detect
Non-detect
PE sample not prepared and analyzed with assigned field
samples
Use professional
judgment
Use professional
judgment
PE sample results outside lower action limits provided
with the PE sample or specified for the project
J-
R
PE sample results outside lower warning limits but inside
lower action limits provided with the PE sample or
specified for the project
J-
UJ
PE sample results within limits provided with the PE
sample or specified for the project
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits provided with the PE sample or
specified for the project
J+
No qualification
PE sample results outside upper action limits provided
with the PE sample or specified for the project
J+
No qualification
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
V. Field Quality Assurance and Quality Control (QA/QC)
A. Review Items
Laboratory Results Reports, sampling documentation (e.g., COC Records), instrument printouts, and
other raw data from QA/QC samples in data package.
November 2020
8

-------
Inorganic Data Review
General
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.	Criteria
Criteria are determined by the data user or QAPP.
1.	The frequency of these field and project QA/QC samples should be defined in the QAPP.
2.	Performance criteria for these field and project QA/QC samples should also be defined in the
QAPP.
3.	The Relative Percent Difference (RPD) between field duplicates should fall within the specific
limits in the QAPP or in the project-specific SOPs for data review. The limits may not apply
when the sample and duplicate concentrations are less than 5x the Quantitation Limit (QL) or
limit in the QAPP.
4.	In the absence of other guidance, qualify associated samples for contaminants found in field
blanks based on the criteria for Method Blanks (see the applicable method sections for blank
actions).
D.	Evaluation
1.	Determine whether any non-conforming field QA/QC sample results may impact all samples in
the project or only those directly associated (e.g., in the same data package, collected on the same
day, prepared together, or contained in the same analytical sequence).
2.	Verify precision by recalculating at least one RPD between field duplicates and provide this
information in the Data Review Narrative. Also verify that the RPDs fall within the limits
specified in the QAPP or project-specific SOPs for data review.
3.	Determine whether RPD limits exceedance (poor precision) is the responsibility of the laboratory
or may have resulted from sample non-homogeneity in the field. Laboratory observations of
sample appearance, in the data package narrative, may become important in these situations.
E.	Action
1.	Any action should be in accordance with the project specifications and the criteria for acceptable
field duplicate sample results.
2.	Note where RPDs exceed criteria for field duplicate samples in the Data Review Narrative and
for designated project management personnel action.
3.	Note results greater than or equal to QLs in field blanks for designated project management
personnel action.
4.	In general, for QA/QC performance not within QAPP specification, qualify detects as estimated
(J) and non-detects as estimated (UJ). The impact on overall data quality should be assessed after
consultation with the data user and/or field personnel.
VI. Overall Assessment of Data
A.	Review Items
Entire data package, data review results, and (if available) the QAPP and Sampling and Analysis Plan
(SAP).
B.	Objective
The objective is to provide the overall assessment on data quality, uncertainty, and bias.
November 2020
9

-------
Inorganic Data Review
General
C.	Criteria
1.	Review all available materials to assess the overall quality of the data, keeping in mind the
additive nature of analytical problems.
2.	Reported analyte concentrations should be quantitated according to the appropriate equations, as
listed in the reference method. All sample results should be measured within the calibration
range. Percent Solids (%Solids) should be properly used for all applicable matrix result
calculations.
D.	Evaluation
Examine the raw data to verify that the calculated sample results were correctly reported by the
laboratory. Preparation logs, instrument printouts, etc., should be used to evaluate the final results
reported in the data package.
1.	Evaluate any technical problems that were not previously addressed.
2.	Examine the raw data for anomalies (e.g., baseline shifts, omissions, illegibility).
3.	Verify that the appropriate methods and amounts were used to prepare the samples for analysis. If
reduced sample aliquot amounts were used, verify that any project-required sensitivity was not
compromised and that the laboratory received prior approval.
4.	Verify that there are no transcription or reduction errors (e.g., dilutions, %Solids, sample weights)
on one or more samples. Recalculate the %Solids for one or more of the samples and verify that
the calculated %Solids agree with that reported by the laboratory.
5.	Verify that Detection Limits (DLs) are properly reported and that they are not greater than or
equal to the respective QLs.
6.	Verify that reported target analyte results fall within the calibrated range(s) of the instrument(s).
7.	If appropriate information is available, assess the usability of the data to assist the data user in
avoiding inappropriate use of the data. Review all available information, including the QAPP,
focusing specifically on the acceptance or performance criteria, the SOPs, and communication
with the project manager concerning the intended use and desired quality of these data.
NOTE: For data obtained from the EPA CLP, information regarding noncompliant analyses and
data can be obtained from the NFG reports and may be used as part of the evaluation.
E.	Action
1.	Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria discussed in Data Review Part A and Data Review Part B.
2.	Use professional judgment to qualify detects and non-detects if the Method Detection Limit
(MDL) or DL is greater than or equal to the QL.
3.	If a sample is not diluted properly when sample results exceeded the upper limit of the calibration
range, qualify affected detects as estimated (J).
4.	If the required analyses were not performed at the specified frequency and sequence and/or
sufficient information was not provided for an analysis, notify the designated project management
personnel, who may arrange for the laboratory to repeat the analyses as specified and/or to
provide any missing information. In the event that a reanalysis cannot be performed (e.g., sample
holding times have expired, insufficient amount of remaining sample) or the relevant information
is not available, use professional judgment to assess the existing data.
5.	Write a brief Data Review Narrative (see Part A, Section III) to give the user an indication of the
limitations of the analytical data. Note the issues reported in the data package narrative,
calculation errors (if any), and the General Data Review (Part A) and Method-Specific Data
November 2020
10

-------
Inorganic Data Review
General
Review (Part B) performance criteria that are exceeded in this report. Also include the potential
effects of such discrepancies on the data for designated project management personnel action.
6.	If sufficient information on the intended use and required quality of the data is available, include
an assessment of the usability of the data within the given context. This evaluation may be used
as part of a formal Data Quality Assessment (DQA).
7.	Document the process used for the data review and qualification in accordance with the Guidance
for Labeling Externally Validated Laboratory Analytical Data for Superfund Use (see table in
Section IV of Part A, titled Additional Information).
November 2020
11

-------
Inorganic Data Review	General
This page is intentionally left blank.
November 2020
12

-------
Inorganic Data Review	ICP-AES
PART B: METHOD-SPECIFIC DATA REVIEW
November 2020
13

-------
Inorganic Data Review	ICP-AES
This page is intentionally left blank.
November 2020
14

-------
Inorganic Data Review
ICP-AES
ICP-AES DATA REVIEW
The inorganic data requirements for Inductively Coupled Plasma - Atomic Emission Spectroscopy
(ICP-AES) to be reviewed during validation are listed below:
I.	Preservation and Holding Times	17
II.	Calibration	19
III.	Blanks	22
IV.	Interference Check Sample	26
V.	Laboratory Control Sample	29
VI.	Duplicate Sample Analysis	31
VII.	Spike Sample Analysis	33
VIII.	Serial Dilution	36
IX.	Target Analyte Quantitation	38
ICP-AES Table 1.	Preservation and Holding Time Actions	18
ICP-AES Table 2.	Calibration Actions	21
ICP-AES Table 3.	Blank Actions	24
ICP-AES Table 4.	Interference Check Actions	27
ICP-AES Table 5.	LCS Actions	30
ICP-AES Table 6.	Duplicate Sample Actions	32
ICP-AES Table 7.	Spike Sample Actions	34
ICP-AES Table 8.	Serial Dilution Actions	37
November 2020
15

-------
Inorganic Data Review	ICP-AES
This page is intentionally left blank.
November 2020
16

-------
Inorganic Data Review
ICP-AES
I. 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.	Criteria
1.	Samples received with pH > 2 may be adjusted to pH < 2 by the laboratory. The laboratory must
allow the sample to set for at least 16 hours after acid addition before rechecking the pH. Samples
adjusted to pH < 2 by the laboratory do not require qualification.
2.	The technical holding time is determined from the date of field sample collection, or the date that
Toxicity Characteristic Leaching Procedure (TCLP) or Synthetic Precipitation Leaching
Procedure (SPLP) extraction is completed, to the date of analysis.
3.	The technical holding time criteria for aqueous/water samples and TCLP/SPLP aqueous filtrate
and leachate samples is 180 days or as specified in the Quality Assurance Project Plan (QAPP),
preserved (with nitric acid) to pH < 2.
4.	The technical holding time criteria for soil/sediment and waste samples is 180 days or as
specified in the QAPP.
5.	The technical holding time criteria for wipe samples is 180 days.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, appropriate sample temperature at receipt, pH), or if the pH was adjusted
upon receipt. If there is an indication of problems with the samples, the sample integrity may be
compromised. Also verify that the samples were properly stored at the laboratory.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
3.	Establish the technical holding times by comparing the sample collection dates on the sampling
documentation and the TCLP/SPLP extraction dates with the dates of analysis on the Laboratory
Results Reports and the raw data.
E.	Action
Refer to ICP-AES Table 1 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.
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.
November 2020
17

-------
Inorganic Data Review
ICP-AES
ICP-AES Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples received with pH > 2 and pH adjusted
by laboratory
No qualification
No qualification
Aqueous/water samples received with pH > 2 and pH not
adjusted
J-
R
TCLP/SPLP leachates with pH > 2 and pH not adjusted
J-
R
Technical Holding Time:
Aqueous/water and TCLP/SPLP leachates >180 days
J-
R
Technical Holding Time:
Soil/sediment/waste/wipe samples >180 days
J-
R
Samples properly preserved and analyzed within specified
holding time
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
18

-------
Inorganic Data Review
ICP-AES
II. 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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated each time the instrument is set up, or as
specified in the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW). The
calibration date and time should be included in the raw data.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish each calibration curve. At least one of these standards should
be at or below the Quantitation Limit (QL) in the QAPP or SOW but above the Detection
Limit or the Method Detection Limit (MDL). Calibration standards at and above the QL
should be continuous with none excluded to satisfy Quality Control (QC) requirements.
All measurements should be within the instrument working range where the interelement
correction factors are valid. A minimum of three replicate exposures or the number
specified in the QAPP are required for standardization, for all QC samples, and for
sample analyses. The average result of all the multiple exposures for the standardization,
QC, and sample analyses should be used. The calibration curve may be fitted using linear
regression or weighted linear regression, or other fits as specified in the QAPP. The curve
may be forced through zero. For linear fits, the calibration curve should have a
correlation coefficient greater than the value specified in the QAPP or in the SOW. The
calculated percent differences (%Ds) or other specified statistical test values for all non-
zero standards should fall within the limits in the QAPP or in the SOW.
2.	Initial and Continuing Calibration Verification
a.	Initial Calibration Verification (ICV)
i.	Immediately after each system has been calibrated, the accuracy of the initial calibration
should be verified and documented for each target analyte by the analysis of an ICV
standard. If the ICV Percent Recovery (%R) falls outside of the control limits, the
analysis should be terminated, the problem corrected and documented in the data package
narrative, the instrument recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of the analytes from
an independent standard source, at a concentration level other than that used for
instrument calibration, and near the middle of the calibrated range (within ±30%).
iii.	The ICV solution should be analyzed at each analytical wavelength used for analysis.
iv.	The Percent Relative Standard Deviation (%RSD) of the replicate measurements of the
ICV should not exceed 5% or the limit specified in the QAPP.
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV standard should be
analyzed and reported for each wavelength used for the analysis of each analyte.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every
two hours during an analytical sequence. The CCV standard should also be analyzed at
the beginning of the analytical sequence, and again after the last analytical sample.
November 2020
19

-------
Inorganic Data Review	ICP-AES
iii.	The CCV standard should be prepared using the same source and in the same acid matrix
as the calibration standards by combining compatible analytes at a concentration at or
near the mid-level (within ±30%) of the respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
v.	The %RSD of the replicate measurements of a CCV should not exceed 5% or the limit
specified in the QAPP.
vi.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vii.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified in the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP.
2.	Confirm that the measurements were within the working calibration range, and were the average
result of at least the specified minimum number of replicate exposures.
3.	Confirm that an instrument blank was not analyzed before the CCV.
4.	Verify that the ICV and CCV standards were analyzed for each analyte at the specified frequency
and at the appropriate concentration. Verify that acceptable %R results were obtained.
5.	Verify that the ICV/CCV %RSD does not exceed 5% or the limit specified in the QAPP.
6.	Verify that the ICV and CCV %R values are correct by recalculating one or more of the %Rs
using the raw data and the following equation:
Found (value)
%R= True (value) *10°
Where,
Found (value) = Concentration of each analyte measured in the analysis of the ICV or CCV
solution
True (value) = Concentration of each analyte in the ICV or CCV source
E.	Action
Refer to ICP-AES Table 2 below for the evaluation criteria and corresponding actions for detected
and non-detected target analyte results in the samples associated with deficient initial calibrations or
calibration verification standards.
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 standard 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.
November 2020
20

-------
Inorganic Data Review
ICP-AES
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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
ICP-AES Table 2. 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 or R
UJ orR
For linear fits, correlation coefficient < 0.995
J
UJ
%D outside ±30% or other specified statistical test
values outside limits
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R <75%
J- or R
UJ orR
ICV/CCV %R 75-89%
J-
UJ
ICV/CCV %R 90-110%
No qualification
No qualification
ICV/CCV %R 111-125%
J+
No qualification
ICV/CCV %R> 125%
J+ or R
No qualification
ICV/CCV %RSD > 5%
J
UJ
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
21

-------
Inorganic Data Review
ICP-AES
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed at each wavelength used for analysis after
the analytical standards, but not before analysis of the Initial Calibration Verification (ICV)
standard during the initial calibration of the instrument. The ICB result (absolute value) should
not be greater than or equal to the Quantitation Limit (QL) of each analyte for which analysis is
performed.
3.	A Continuing Calibration Blank (CCB) should be analyzed at each wavelength used for the
analysis, immediately after every Continuing Calibration Verification (CCV) standard. The CCB
should be analyzed at the frequency specified in the Quality Assurance Project Plan (QAPP) or in
the Statement of Work (SOW) during the analytical sequence. The CCB should be analyzed at the
beginning of the analytical sequence, and again after the last CCV that was analyzed after the last
analytical sample of the analytical sequence. The CCB result (absolute value) should not be
greater than or equal to the QL of each analyte for which analysis is performed.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples digested, whichever is more frequent. The Preparation
Blank consists of reagent water or a clean wipe processed through the appropriate sample
preparation and analysis procedure.
5.	If the concentration of any analyte in the Preparation Blank is greater than or equal to the QL, the
lowest concentration of that analyte in the associated samples should be > lOx the Preparation
Blank concentration. Otherwise, all associated samples with the analyte's concentration < lOxthe
Preparation Blank concentration, and > the QL, should be redigested and reanalyzed for that
analyte. The laboratory is not to correct the sample concentration for the blank value.
6.	If the concentration of any analyte in the Preparation Blank is < (-QL), all associated samples
with the analyte's concentration < lOxthe QL should be redigested and reanalyzed.
7.	At least one Leachate Extraction Blank (LEB) should be prepared and analyzed for each batch of
samples extracted by Toxicity Characteristic Leaching Procedure (TCLP) or Synthetic
Precipitation Leaching Procedure (SPLP). The LEB consists of reagent water processed through
the extraction procedure. Post-extraction, the LEB should be processed through the appropriate
sample preparation and analysis procedure.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks and LEBs were prepared and
analyzed as appropriate for the data package (e.g., total number of samples, various types of
matrices present, number of digestion batches, etc.).
2.	For an ICB or a CCB, verify that if the absolute value of any target analyte was greater than or
equal to the QL, the analysis was terminated, the problem corrected and documented in the data
November 2020
22

-------
Inorganic Data Review
ICP-AES
package narrative, the instrument recalibrated, and the preceding 10 analytical samples or all
analytical samples analyzed since the last compliant calibration blank reanalyzed.
3.	For a Preparation Blank, verify that if the concentration of any target analyte was greater than or
equal to the QL, all associated samples with the analyte's concentration > the QL but < lOx the
Preparation Blank concentration were redigested and reanalyzed for that analyte. Verify that if a
concentration was < (-QL) in a Preparation Blank, all associated samples with the analyte's
concentration < 1 Ox the QL were redigested and reanalyzed.
4.	Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to ICP-AES Table 3 below for the evaluation criteria and corresponding actions for detected
and non-detected target analyte results in the samples associated with deficient blanks.
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.	Actions 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 3 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 3 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 negatives exists.
NOTE: 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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
November 2020
23

-------
Inorganic Data Review
ICP-AES
ICP-AES Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J
ICB/CCB
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
ICB/CCB
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank/LEB
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/LEB/
Field Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/LEB/
Field Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/LEB/
Field Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < 1 Ox the Preparation
Blank/LEB Result
Report at Preparation Blank/LEB
Result and qualify J+ or R
> 1 Ox the Preparation
Blank/LEB Result
No qualification
Preparation
Blank/LEB/
Field Blank
<(-QL)
Non-detect
UJ
Detect < QL
J-
> QL but < lOx QL
J-
November 2020
24

-------
Inorganic Data Review
ICP-AES
Blank Type
Blank Result
Sample Result
Action


> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
25

-------
Inorganic Data Review	ICP-AES
IV. Interference Check Sample
A.	Review Items
Laboratory interference checks reports (if available), instrument printouts and raw data in the data
package.
B.	Objective
The objective is to determine the validity of the analytical results based on the instrument's ability to
overcome interferences typical of those found in samples.
C.	Criteria
1.	The Interference Check Sample (ICS) consists of two solutions: Solution A and Solution AB.
Solution A consists of the interferents, and Solution AB consists of the analytes mixed with the
interferents. An ICS analysis consists of analyzing both solutions consecutively, starting with
Solution A, for all wavelengths used for each analyte reported by ICP-AES.
2.	An ICS should be analyzed undiluted at the beginning of each sample analysis sequence. The ICS
is not to be analyzed prior to the Initial Calibration Verification (ICV) standard, and should be
immediately followed by a Continuing Calibration Verification (CCV) standard, followed by a
Continuing Calibration Blank (CCB).
3.	Results for the analysis of the ICS Solution A should fall within the control limits specified in the
Quality Assurance Project Plan (QAPP), or ±QL [or ±15% of the true value (whichever is
greater)] for the analytes and interferents included in the solution.
4.	Results for the analysis of the ICS Solution AB should fall within the control limits specified in
the QAPP or in the SOW.
5.	If the value of an ICS result exceeds the limit in the QAPP or in the Statement of Work (SOW),
the analysis should be terminated, the problem corrected and documented in the data package
narrative, the instrument recalibrated, the new calibration then reverified, and all analytical
samples since the last compliant ICS reanalyzed.
6.	The ICS solutions should be prepared using certified standards with the interferent and analyte
concentrations at the levels specified in the method.
D.	Evaluation
1.	Verify, using the raw data, that the ICS was analyzed at the specified frequency and sequence
during the analytical sequence.
2.	Evaluate the ICS raw data for results with an absolute value that is greater than the Detection
Limit or the Method Detection Limit (MDL) for those analytes that are not present in the ICS
solution.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of each analyte or interferent measured in the analysis of ICS
Solution A or ICS Solution AB
True (value) = Concentration of each analyte or interferent in ICS Solution A or ICS
Solution AB
4.	If the value of an ICS result exceeds the limits specified in the QAPP, the ±QL, or ±15% of the
true value (whichever is greater) criteria, and the laboratory failed to terminate the analysis and
November 2020
26

-------
Inorganic Data Review
ICP-AES
take the appropriate corrective action, note this and record the situation in the Data Review
Narrative. Use professional judgment to assess the data.
E. Action
Refer to ICP-AES Table 4 below for the evaluation criteria and corresponding actions for detected
and non-detected target analyte results in the samples associated with deficient ICSs.
1.	For an ICS analysis that does not meet the technical criteria, apply the actions to all samples
reported from the analytical sequence.
NOTE: The same result units should be used when comparing analyte results in samples to those
in the ICS. Unit conversion may be necessary when soil/sediment/waste or wipe samples
are evaluated.
2.	In general, ICP-AES sample data can be accepted if the concentrations of Aluminum (Al),
Calcium (Ca), Iron (Fe), and Magnesium (Mg) in the sample are found to be less than or equal to
their respective concentrations in the ICS. If these elements are present at concentrations greater
than the level in the ICS, or other elements are present in the sample at > 10 mg/L, investigate the
possibility of other interference effects as given in the ICP-AES method or as indicated by the
laboratory's interelement correction factors for that particular instrument. The analyte
concentration equivalents presented in the method should be considered only as estimated values
since the exact value of any analytical system is instrument-specific. Therefore, estimate the
concentration produced by an interfering element. If the estimate is > 2x the QL and > 10% of the
reported concentration of the affected element, qualify the affected results as estimated (J).
3.	If the raw data does not contain results for the interferents, note this in the Data Review
Narrative. Actions regarding the interpretation and/or the subsequent qualification of ICP data
due to the ICS analytical results can be complex. Use professional judgment to determine the
need for the associated sample data to be qualified. Obtain additional information from the
laboratory, if necessary. Record all interpretive situations in the Data Review Narrative.
ICP-AES Table 4. Interference Check Actions
Criteria
Action
Detect
Non-detect
ICS not analyzed
R
R
ICS not analyzed in the specified sequence
J
UJ
ICSAB %R< 50%
J-
R
ICS %R 50-84% [or ICS found value is < (true value
- QL), whichever is lower]
J-
UJ
ICS %R 85-115%
No qualification
No qualification
ICS %R 116-150% [or ICS found value is > (true
value + QL), whichever is greater]
J+
No qualification
ICS %R > 150%
J+
No qualification
ICSA results > DLs or MDLs, but not present in ICS
(potential false positive)
J+
No qualification
Negative ICSA results, but not present in ICS
(potential false negative)
J-
for results < lOx
( negative sample
result)
UJ
November 2020
27

-------
Inorganic Data Review
ICP-AES
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
28

-------
Inorganic Data Review	ICP-AES
V. Laboratory Control Sample
A.	Review Items
Laboratory LCS reports (if available), preparation 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 the recovery of the
digested Laboratory Control Sample (LCS).
C.	Criteria
1.	Aqueous/water, soil/sediment/waste, and wipe LCSs should be analyzed for each analyte utilizing
the same sample preparations, analytical methods, and Quality Assurance/Quality Control
(QA/QC) procedures as employed for the samples.
2.	One LCS should be prepared and analyzed for every group of aqueous/water or
soil/sediment/waste samples in a data package, or with each batch of samples digested, whichever
is more frequent. The LCS should be spiked such that the final digestate contains each analyte at
the level specified in the Quality Assurance Project Plan (QAPP) or at 2x the Quantitation Limit
(QL) for the associated matrix.
3.	One LCS should be prepared and analyzed for each group of wipe samples in a data package, or
with each batch of wipe samples digested, whichever is more frequent. The wipe LCS should be
spiked such that the final digestate contains each analyte at the level specified in the QAPP or at
2x the QL.
4.	All LCS Percent Recoveries (%Rs) should fall within the control limits in the QAPP or in the
Statement of Work (SOW). If the %R for the aqueous/water and soil/sediment/waste LCS falls
outside of the control limits, the analysis should be terminated, the problem corrected and
documented in the data package narrative, and the samples prepared with that LCS redigested and
reanalyzed. No corrective actions are required for wipe LCSs when the %R is outside the control
limits.
D.	Evaluation
1.	Verify, using the laboratory reports, preparation logs, and raw data, that the appropriate number
of required LCSs were prepared and analyzed for the data package.
2.	Verify that all results for each analyte fall within the established control limits.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of each analyte measured in the analysis of the LCS
True (value) = Concentration of each analyte in the LCS
4.	Verify that the LCS was prepared at the same time as the associated samples using the same
procedures.
E.	Action
Refer to ICP-AES Table 5 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples associated with deficient LCSs. For an LCS analysis that
does not meet the technical criteria, apply the actions to all samples in the same preparation batch.
November 2020
29

-------
Inorganic Data Review
ICP-AES
Matrix spike data can be reviewed to determine batch quality if an LCS was not prepared and
analyzed with the samples.
ICP-AES Table 5. LCS Actions
Criteria
Action
Detect
Non-detect
LCS not prepared with samples
J
UJ
LCS not prepared at specified concentrations
J
UJ
Aqueous/water and soil/sediment/waste %R < 40%
(< 20% Ag, Sb)
J-
R
Aqueous/water and soil/sediment/waste %R 40-69%
(20-49% Ag, Sb)
J-
UJ
Aqueous/water and soil/sediment/waste %R 70-130%
(50-150% Ag, Sb)
No qualification
No qualification
Aqueous/water and soil/sediment/waste %R 131-150%
(151-170% Ag, Sb)
J+
No qualification
Aqueous/water and soil/sediment/waste %R > 150%
(170% Ag, Sb)
R
No qualification
Wipe %R < 40% (< 20% Ag, Sb)
J-
R
Wipe %R 40-69% (20-49% Ag, Sb)
J-
UJ
Wipe %R 70-130% (50-150% Ag, Sb)
No qualification
No qualification
Wipe %R> 130% (>150% Ag, Sb)
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
30

-------
Inorganic Data Review	ICP-AES
VI. Duplicate Sample Analysis
A.	Review Items
Data package Cover Page, laboratory duplicate reports (if available), instrument printouts, preparation
logs, and raw data in the data package.
B.	Objective
The objective of the duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment/waste) or for each data package.
Duplicates are not required for wipe samples. Duplicates cannot be averaged for reporting on the
Laboratory Results Report. Additional duplicate sample analyses may be required. Alternately,
the data user may require that a specific sample be used for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the QL.
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the Quantitation
Limit (QL) should be used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory report, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that all duplicate results for each analyte fall within the established
control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation:
| S - D |
RPD = 	-1— x 100
(S + D) / 2
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of zero
(0) only for calculating the RPD. This will always yield an RPD of 200%.
November 2020
31

-------
Inorganic Data Review
ICP-AES
E. Action
Refer to ICP-AES Table 6 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples associated with deficient duplicates.
1.	For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the duplicate sample, and that only these samples should be qualified;
or 2) no samples are sufficiently similar to the sample used for the duplicate analysis, and thus
only the field sample used to prepare the duplicate sample should be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3. For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
ICP-AES Table 6. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency.
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x the QL (including non-detects)
and absolute difference between sample and duplicate >
QL*
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, the QAPP or project-specific SOPs for data review may allow the use of less restrictive criteria
(e.g., 35% RPD, 2x QL) to be assessed against duplicate soil samples.
November 2020
32

-------
Inorganic Data Review
ICP-AES
VII. Spike Sample Analysis
A.	Review Items
Data package Cover Page, laboratory matrix spike reports (if available), instrument printouts,
preparation logs, 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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample (pre-digestion) should be prepared and analyzed from each group of
samples with a similar matrix type (e.g., aqueous/water or soil/sediment/waste), or for each data
package. Matrix Spikes are not required for wipe samples. Additional matrix spike sample
analyses may be required. Alternately, the data user may require that a specific sample be used
for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	For sample analyzed under the SOW, when the spike recovery falls outside of the control limits
and the sample result is < 4x the spike added, a post-digestion spike analysis should be performed
for those analytes that do not meet the specified criteria. An aliquot of the remaining unspiked
sample should be spiked at 2x the indigenous level or 2x the Quantitation Limit (QL), whichever
is greater.
NOTE: Post-digestion spikes are not required for Antimony (Sb) and Silver (Ag).
5.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentrations required for the various target analytes are presented in the
methods described in the Quality Assurance Project Plan (QAPP) or in the SOW.
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all matrix spike sample results for each required analyte fall
within the established control limits. If not, verify that a post-digestion spike was prepared and
analyzed.
4.	Verify that the %R values for the matrix spike are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
November 2020
33

-------
Inorganic Data Review
ICP-AES
SSR-SR
%Recovery= ——— x 100
jA
Where,
SSR	=	Spiked Sample Result
SR	=	Sample Result
SA	=	Spike Added
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
E. Action
Refer ICP-AES Table 7 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 to
all samples of the same matrix if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the Matrix Spike sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for the matrix spike
analysis, and thus only the field sample used to prepare the Matrix Spike sample should be
qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
ICP-AES Table 7. 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-digestion spike %R <75%
J-
R
Matrix Spike %R < 30%
Post-digestion spike %R> 75%
J
UJ
Matrix Spike %R 30-74%
Post-digestion Spike %R< 75%
J-
UJ
Matrix Spike %R 30-74%
Post-digestion spike %R> 75%
J
UJ
November 2020
34

-------
Inorganic Data Review
ICP-AES
Criteria
Action
Detect
Non-detect
Matrix Spike %R >125%
Post-digestion spike %R> 125%
J+
No qualification
Matrix Spike %R >125%
Post-digestion spike %R< 125%
J
No qualification
Matrix Spike %R < 30%
No post-digestion spike performed
(not required for Ag and Sb)
J-
R
Matrix Spike %R 30-74%
No post-digestion spike performed
(not required for Ag and Sb)
J-
UJ
Matrix Spike %R 75-125%
No post-digestion spike is required
No qualification
No qualification
Matrix Spike %R >125%
No post-digestion spike performed
(not required for Ag and Sb)
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific SOPs for data review may
allow the use of less restrictive criteria (e.g., 10 %R and 150 %R for the lower and upper
limits) to be assessed against spike and post-digestion spike soil samples.
November 2020
35

-------
Inorganic Data Review
ICP-AES
VIII. Serial Dilution
A.	Review Items
Laboratory serial dilution reports (if available), instrument printouts, and raw data in the data
package.
B.	Objective
The objective of the serial dilution analysis is to determine if significant physical or chemical
interferences exist due to sample matrix.
C.	Criteria
1.	An Inductively Coupled Plasma (ICP) Serial Dilution analysis should be performed on a sample
from each group of samples with a similar matrix type (e.g., aqueous/water or
soil/sediment/waste) or for each data package, whichever is more frequent.
2.	An ICP Serial Dilution analysis is not required for wipe samples.
3.	Field samples should be used as source samples for the ICP Serial Dilution analysis.
4.	If the analyte concentration is sufficiently high [concentration in the original sample is > 5 Ox the
Method Detection Limit (MDL) that is calculated for the sample or the limit in the Quality
Assurance Project Plan (QAPP)], the Percent Difference (%D) between the original determination
and the serial dilution analysis (a five-fold dilution) after correction for dilution [concentration in
the serial dilution sample is > Quantitation Limit (QL)] should be < 20%.
D.	Evaluation
1.	Verify that the serial dilution analysis was performed on a field sample.
2.	Verify that the %D values are correct by recalculating one or more of the %Ds using the raw data
and the following equation:
Where,
I = Initial Sample Result
S = Serial Dilution Result
3. Check the raw data for any evidence of positive or negative interference (results from the diluted
sample which are significantly different from the original sample), possibly due to high levels of
dissolved solids in the sample, ionization effects, etc.
Refer to ICP-AES Table 8 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples associated with deficient serial dilution analyses.
%Difference
E. Action
November 2020
36

-------
Inorganic Data Review
ICP-AES
1.	For a serial dilution sample analysis that does not meet the technical criteria, apply the actions to
all samples of the same matrix if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the serial dilution sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for serial dilution, and thus
only the field sample used to prepare the serial dilution sample should be qualified.
2.	Note the potential effects on the reported data in the Data Review Narrative.
ICP-AES Table 8. Serial Dilution Actions
Criteria
Action
Detect
Non-detect
Serial Dilution not performed at the specified frequency
J
UJ
Sample concentration > 5 Ox MDL, serial dilution sample
concentration > QL, and %D > 20%*
J
No qualification
Sample concentration >5 Ox MDL, serial dilution sample
concentration > QL, and %D < 20%
No qualification
No qualification
Sample concentration > 5x QL and serial dilution sample
concentration < QL
No qualification
No qualification
Interferences present
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above criteria are method requirements for serial dilution samples, regardless of the sample
matrix type. However, for technical review purposes only, the QAPP or the project-specific SOPs for
data review may allow the use of less restrictive criteria (e.g., %D > 25%) to be assessed against serial
dilution soil samples.
November 2020
37

-------
Inorganic Data Review
ICP-AES
IX. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final digestate volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1.	Aqueous/Water and TCLP/SPLP Sample Concentration
Vf
Concentration (|ig/L) = C x — x DF
Where,
C = Instrument value in |a,g/L (the average of all replicate exposures)
Vf = Final digestion volume (mL)
V = Initial aliquot amount (mL)
DF = Dilution Factor
2.	Soil/Sediment and Waste Sample Concentration
Vf
Concentration (mg/kg dry weight) = C x ——- x DF/1000
W X S
Where,
C = Instrument value in |a,g/L (the average of all replicate exposures)
Vf = Final digestion volume (mL)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
38

-------
Inorganic Data Review
ICP-AES
3.	Wipe Mass
Mass (ng) = C x Vf x DF/1000
Where,
C = Instrument value in |a,g/L (The average of all replicate exposures)
Vf = Final digestion volume (mL)
DF = Dilution Factor
4.	Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water or TCLP/SPLP leachate samples, substitute the value of the DL or QL, in the
appropriate units, into the "C" term in the equation above.
Calculate the adjusted DL or adjusted QL for soil/sediment samples as follows:
WM Vf
Adjusted DL or QL (mg/kg) = C x ——- x —— * DF
W x S Vm
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Minimum method required aliquot amount (g)
W = Initial aliquot amount (g)
Vm = Method required final sample digestion volume (mL)
Vf = Final digestion volume (mL)
S = % Solids/100
DF = Dilution Factor
5.	Hardness (Total) in Aqueous/Water Samples
Total Hardness is defined as the sum of calcium and magnesium concentration, expressed as
calcium carbonate in mg/L.
Calculate Total Hardness for Aqueous/Water samples as follows:
Hardness (mg/L) = [Cone. Ca (mg/L) x 2.497] + [Cone. Mg (mg/L) x 4.118]
Where,
Cone. Ca (mg/L)
Cone. Mg (mg/L)
= Calcium concentration ((.ig/L) / 1000
= Magnesium concentration (|_ig/L) / 1000
November 2020
39

-------
Inorganic Data Review	ICP-AES
This page is intentionally left blank.
November 2020
40

-------
Inorganic Data Review
ICP-MS
I CP-MS DATA REVIEW
The inorganic data requirements for Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) to be
reviewed during validation are listed below:
I.	Preservation and Holding Times	43
II.	Tune Analysis	45
III.	Calibration	47
IV.	Blanks	50
V.	Interference Check Sample	53
VI.	Laboratory Control Sample	55
VII.	Duplicate Sample Analysis	57
VIII.	Spike Sample Analysis	59
IX.	Serial Dilution	62
X.	Internal Standards	64
XI.	Target Analyte Quantitation	66
ICP-MS Table 1. Preservation and Holding Time Actions	44
ICP-MS Table 2. Tune Actions	46
ICP-MS Table 3. Calibration Actions	49
ICP-MS Table 4. Blank Actions	51
ICP-MS Table 5. Interference Check Actions	54
ICP-MS Table 6. LCS Actions	56
ICP-MS Table 7. Duplicate Sample Actions	58
ICP-MS Table 8. Spike Sample Actions	60
ICP-MS Table 9. Serial Dilution Actions	63
ICP-MS Table 10. Internal Standard Actions	65
November 2020
41

-------
Inorganic Data Review	ICP-MS
This page is intentionally left blank.
November 2020
42

-------
Inorganic Data Review
ICP-MS
I. 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.	Criteria
1.	Samples received with pH > 2 may be adjusted to pH < 2 by the laboratory. The laboratory must
allow the sample to set for at least 16 hours after acid addition before rechecking the pH. Samples
adjusted to pH < 2 by the laboratory do not require qualification.
2.	The technical holding time is determined from the date of sample collection to the date of
analysis.
3.	The technical holding time criteria for aqueous/water samples is 180 days or as specified in the
Quality Assurance Project Plan (QAPP), preserved (with nitric acid) to pH < 2.
4.	The technical holding time criteria for soil/sediment/waste samples is 180 days or as specified in
the QAPP.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, appropriate sample temperature at receipt, pH), or if the pH was adjusted
upon receipt. If there is an indication of problems with the samples, the sample integrity may be
compromised. Also verify that the samples were properly stored at the laboratory.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
Establish the technical holding times by comparing the sample collection dates on the sampling
documentation with the dates of analysis on the Laboratory Results Reports and the raw data.
E.	Action
Refer to ICP-MS Table 1 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.
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.
November 2020
43

-------
Inorganic Data Review
ICP-MS
ICP-MS Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples received with pH > 2 and pH adjusted by
laboratory
No
qualification
No
qualification
Aqueous/water samples received with pH > 2 and pH not adjusted
J-
R
Technical Holding Time:
Aqueous/water samples >180 days
J-
R
Technical Holding Time:
Soil/sediment/waste samples >180 days
J-
R
Samples properly preserved and analyzed within specified holding
time
No
qualification
No
qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
44

-------
Inorganic Data Review
ICP-MS
II. Tune Analysis
A.	Review Items
Laboratory instrument performance check (Tune) reports (if available), instrument printouts and raw
data in the data package.
B.	Objective
The ICP-MS tune serves as an initial demonstration of instrument stability and precision.
C.	Criteria
1.	Prior to calibration, the laboratory should analyze or scan the ICP-MS tuning solution, containing
the elements and concentrations specified in the Quality Assurance Project Plan (QAPP) or 100
(ig/L of Beryllium (Be), Magnesium (Mg), Cobalt (Co), Indium (In), and Lead (Pb), at least five
times consecutively. The solution should contain all required isotopes of the specified elements.
The laboratory should make any adjustments necessary to bring peak width within the instrument
manufacturer's specifications and adjust the resolution of the mass calibration to within 0.1 u
over the range of 6-210 u.
2.	The Percent Relative Standard Deviation (%RSD) of the absolute signals for all analytes in the
tuning solution should be less than the value specified in the QAPP or in the Statement of Work
(SOW).
D.	Evaluation
1.	Verify, using the raw data that the appropriate number of analyses or scans of the ICP-MS tuning
solution were performed, and that the appropriate analytes were present in the solution.
2.	Verify, using the raw data, that the resolution of the mass calibration falls within the limits for
each isotope of each analyte.
3.	Verify, using the raw data, that the %RSD is less than or equal to the limit for each isotope of
each analyte.
4.	Verify that the average mass and %RSD values are correct by recalculating one or more of the
average masses and %RSDs for an isotope using the raw data and the following equations:
Mean Value
n
ZXi
x = !±-
n
Where,
X = Mean Value
X, = Individual replicate mass reading
n = Number of replicates
Percent Relative Standard Deviation
SD
%RSD = x 100
A
Where,
%RSD = Percent RSD
SD = Standard Deviation of replicates
x = Mean value of replicates
November 2020
45

-------
Inorganic Data Review
ICP-MS
E. Action
Refer to ICP-MS Table 2 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient ICP-MS Tunes. For ICP-
MS tunes that do not meet the technical criteria, apply the actions to all samples reported from the
analytical sequence.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
ICP-MS Table 2. Tune Actions
Criteria
Action
Detect
Non-detect
Tune not performed
R
R
Tune not performed with required isotopes and/or number of scans
J or R
UJ orR
Resolution of mass calibration not within 0.1 u
J
UJ
%RSD > 5%
J
UJ
Tune properly analyzed with required isotopes, mass resolution
and %RSD within specified limits
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
November 2020
46

-------
Inorganic Data Review
ICP-MS
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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated each time the instrument is set up, or as
specified in the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW). The
calibration date and time should be included in the raw data.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish each calibration curve. At least one of these standards should
be at or below the Quantitation Limit (QL) in the QAPP or in the SOW, but above the
Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy QC requirements. All
measurements should be within the instrument working range. A minimum of three
replicate scans or the number specified in the QAPP are required for standardization, for
all Quality Control (QC) samples, and for sample analyses. The average result of all the
multiple scans for the standardization, QC, and sample analyses should be used. The
calibration curve may be fitted using linear regression or weighted linear regression, or
other fits as specified in the QAPP. The curve may be forced through zero. For linear fits,
the calibration curve should have a correlation coefficient greater than the value specified
in the QAPP or in the SOW. The calculated percent differences (%Ds) or other specified
statistical test values for all non-zero standards should fall within the limits in the QAPP
or in the SOW.
2.	Initial and Continuing Calibration Verification
a.	Initial Calibration Verification (ICV)
i.	Immediately after each system has been calibrated, the accuracy of the initial calibration
should be verified and documented for each target analyte by the analysis of an ICV
standard. If the ICV Percent Recovery (%R) falls outside of the control limits, the
analysis should be terminated, the problem corrected and documented in the data package
narrative, the instrument recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of the analytes from
an independent standard source, at a concentration level other than that used for
instrument calibration, and near the middle of the calibrated range (within ±30%).
iii.	The ICV solution should be analyzed at each analytical mass used for analysis.
iv.	The Percent Relative Standard Deviation (%RSD) of the replicate measurements of the
ICV should not exceed 5% or the limit specified in the QAPP.
b.	Continuing Calibration Verification (CCV)
i. To ensure accuracy during each analytical sequence, the CCV should be analyzed and
reported for each mass used for the analysis of each analyte.
November 2020
47

-------
Inorganic Data Review	ICP-MS
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP or every
two hours during an analytical sequence. The CCV standard should also be analyzed at
the beginning of the analytical sequence, and again after the last analytical sample.
iii.	The CCV standard should be prepared using the same source and in the same acid matrix
as the calibration standards by combining compatible analytes at a concentration at or
near the mid-level (within ±30%) of the respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
v.	The %RSD of the replicate measurements of a CCV should not exceed 5% or the limit
specified in the QAPP.
vi.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vii.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified in the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP.
2.	Confirm that the measurements were within the working calibration range, and were the average
result of at least the specified minimum number of replicate exposures.
3.	Verify that the ICV and CCV standards were analyzed for each analyte at the specified frequency
and at the appropriate concentration. Verify that acceptable %R results were obtained.
4.	Verify that the ICV/CCV %RSD does not exceed 5% or the limit specified in the QAPP.
5.	Verify that the ICV or CCV %R values are correct by recalculating one or more of the %Rs using
the raw data and the following equation:
Found (value)
%R= True (value) "10°
Where,
Found (value) = Concentration of each analyte measured in the analysis of the ICV or CCV
solution
True (value) = Concentration of each analyte in the ICV or CCV source
E.	Action
Refer to ICP-MS Table 3 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient initial calibrations or
calibration verification standards.
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.
November 2020
48

-------
Inorganic Data Review
ICP-MS
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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
ICP-MS 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 or R
UJ orR
For linear fits, the correlation coefficient < 0.995
J
UJ
%D outside ±30% or other specified statistical test
values outside limits
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R <75%
J- or R
UJ orR
ICV/CCV %R 75-89%
J
UJ
ICV/CCV %R 90-110%
No qualification
No qualification
ICV/CCV %R 111-125%
J+
No qualification
ICV/CCV %R> 125%
J+ or R
No qualification
ICV/CCV %RSD > 5%
J
UJ
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
49

-------
Inorganic Data Review
ICP-MS
IV. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed at each mass used for analysis after the
analytical standards, but not before analysis of the Initial Calibration Verification (ICV) standard
during the initial calibration of the instrument. The ICB result (absolute value) should not be
greater than or equal to the Quantitation Limit (QL) of each analyte for which analysis is
performed.
3.	A Continuing Calibration Blank (CCB) should be analyzed at each mass used for the analysis,
immediately after every Continuing Calibration Verification (CCV) standard. The CCB should be
analyzed at the frequency specified in the Quality Assurance Project Plan (QAPP) or in the
Statement of Work (SOW) during the analytical sequence. The CCB should be analyzed at the
beginning of the analytical sequence, and again after the last CCV that was analyzed after the last
analytical sample of the analytical sequence. The CCB result (absolute value) should not be
greater than or equal to the QL of each analyte for which analysis is performed.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples digested, whichever is more frequent. The Preparation
Blank consists of reagent water processed through the appropriate sample preparation and
analysis procedure.
5.	If the concentration of any analyte in the Preparation Blank is greater than or equal to the QL, the
lowest concentration of that analyte in the associated samples should be > lOx the Preparation
Blank concentration. Otherwise, all associated samples with the analyte's concentration < lOxthe
Preparation Blank concentration and > the QL should be redigested and reanalyzed for that
analyte. The laboratory is not to correct the sample concentration for the blank value.
6.	If the concentration of any analyte in the Preparation Blank is < (-QL), all associated samples
with the analyte's concentration < lOx the QL should be redigested and reanalyzed.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks were prepared and analyzed
as appropriate for the data package (e.g., total number of samples, various types of matrices
present, number of digestion batches, etc.).
2.	For an ICB or a CCB, verify that if the absolute value of any target analyte was greater than or
equal to the QL, the analysis was terminated, the problem corrected and documented in the data
package narrative, the instrument recalibrated, and the preceding 10 analytical samples or all
analytical samples analyzed since the last compliant calibration blank reanalyzed.
3.	For a Preparation Blank, verify that if the concentration of any target analyte was greater than or
equal to the QL, all associated samples with the analyte's concentration > the QL but < lOx the
Preparation Blank concentration were redigested and reanalyzed for that analyte. Verify that if a
November 2020
50

-------
Inorganic Data Review
ICP-MS
concentration was < (-QL) in a Preparation Blank, all associated samples with the analyte's
concentration < 1 Ox the QL were redigested and reanalyzed.
4. Evaluation of field and equipment blanks should be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to ICP-MS Table 4 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient blanks.
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.
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 run, 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: 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
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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
ICP-MS Table 4. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J
ICB/CCB
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
November 2020
51

-------
Inorganic Data Review
ICP-MS
Blank Type
Blank Result
Sample Result
Action


> QL
J+ or no qualification
ICB/CCB
< (-MDL) but
>(-QL)
Non-Detect
UJ
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/Field
Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/Field
Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/Field
Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < lOx the Preparation
Blank Result
Report at Preparation Blank
Result and qualify J+ or R
> lOx the Preparation Blank
Result
No qualification
Preparation
Blank/Field
Blank
<(-QL)
Non-detect
UJ
Detect < QL
J-
> QL but < lOx QL
J-
> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifier.
November 2020
52

-------
Inorganic Data Review	ICP-MS
V. Interference Check Sample
A.	Review Items
Laboratory interference checks reports (if available), instrument printouts and raw data in the data
package.
B.	Objective
The objective is to determine the validity of the analytical results based on the instrument's ability to
overcome interferences typical of those found in samples.
C.	Criteria
1.	The Interference Check Sample (ICS) consists of two solutions: Solution A and Solution AB.
Solution A consists of the interferents, and Solution AB consists of the analytes mixed with the
interferents. An ICS analysis consists of analyzing both solutions consecutively, starting with
Solution A, for all masses used for each analyte or interferent reported by ICP-MS.
2.	An ICS should be analyzed undiluted at the beginning of each sample analysis sequence and
every 12 hours during the analytical sequence. The ICS is not to be analyzed prior to the Initial
Calibration Verification (ICV) standard, and should be immediately followed by a Continuing
Calibration Verification (CCV) standard, followed by a Continuing Calibration Blank (CCB).
3.	Results for the analysis of the ICS Solution A should fall within the control limits specified in the
QAPP, or ±2x the Quantitation Limit (QL) [or ±15% of the true value (whichever is greater)] for
the analytes and interferents included in the solution.
4.	Results for the analysis of the ICS Solution AB should fall within the control limits specified in
the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW).
5.	If the value of an ICS result exceeds the limit in the QAPP or in the SOW, the analysis should be
terminated, the problem corrected and documented in the data package narrative, the instrument
recalibrated, the new calibration then reverified, and all analytical samples analyzed since the last
compliant ICS reanalyzed.
6.	The ICS solutions should be prepared using certified standards with the interferent and analyte
concentrations at the levels specified in the method.
D.	Evaluation
1.	Verify, using the raw data, that the ICS was analyzed at the specified frequency and sequence
during the analytical sequence.
2.	Evaluate the ICS raw data for results with an absolute value that is greater than the Detection
Limit or the Method Detection Limit (MDL) for those analytes that are not present in the ICS
solution.
3.	Verify that the ICS Percent Recovery (%R) values are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
Found (value)
%R=-	r—j—r- x 100
True (value)
Where,
Found (value) = Concentration of each analyte or interferent measured in the analysis of ICS
Solution A or ICS Solution AB
True (value) = Concentration of each analyte or interferent in ICS Solution A or ICS
Solution AB
November 2020
53

-------
Inorganic Data Review
ICP-MS
4. If the value of an ICS result exceeds the limits specified in the QAPP or ±2x the QL, or ±15% of
the true value (whichever is greater) criteria, and the laboratory failed to terminate the analysis
and take the appropriate corrective action, note this and record the situation in the Data Review
Narrative. Use professional judgment to assess the data.
E. Action
Refer to ICP-MS Table 5 below for the evaluation criteria and corresponding actions for detected and
non-detected target analytes results in the samples associated with deficient ICSs.
1.	For an ICS analysis that does not meet the technical criteria, apply the actions to all samples
reported from the analytical sequence.
NOTE: The same result units should be used when comparing analyte results in samples to those
in the ICS. Unit conversion may be necessary when soil/sediment/waste samples are
evaluated.
2.	Actions regarding the interpretation and/or the subsequent qualification of ICP data due to the
ICS analytical results can be complex. Use professional judgment to determine the need for the
associated sample data to be qualified. Obtain additional information from the laboratory, if
necessary. Record all interpretive situations in the Data Review Narrative.
ICP-MS Table 5. Interference Check Actions
Criteria
Action
Detect
Non-detect
ICS not analyzed
R
R
ICS not analyzed in specified sequence
J
UJ
ICSAB %R< 50%
J-
R
ICS %R 50-84% [or ICS found value is < (true value -
2x QL), whichever is lower]
J-
UJ
ICS %R 85-115%
No qualification
No qualification
ICS %R 116-150% [or ICS true value is > (true value
+ 2x QL), whichever is greater]
J+
No qualification
ICS %R > 150%
J+
No qualification
ICSA results > DLs or MDLs, but not present in ICS
(potential false positives)
J+
No qualification
Negative ICSA results, but not present in ICS
(potential false negatives)
J-
for results < lOx
( negative sample
result)
UJ
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
54

-------
Inorganic Data Review	ICP-MS
VI. Laboratory Control Sample
A.	Review Items
Laboratory LCS reports (if available), preparation 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 the recovery of the
digested Laboratory Control Sample (LCS).
C.	Criteria
1. Aqueous/water and soil/sediment/waste LCSs should be analyzed for each analyte utilizing the
same sample preparations, analytical methods, and Quality Assurance/Quality Control (QA/QC)
procedures as employed for the samples.
a.	One LCS should be prepared and analyzed for every group of aqueous/water or
soil/sediment/waste samples in a data package, or with each batch of samples digested,
whichever is more frequent. The LCS should be spiked such that the final digestate contains
each analyte at the level specified in the Quality Assurance Project Plan (QAPP) or at 2x the
Quantitation Limit (QL) for the associated matrix.
b.	All LCS Percent Recoveries (%Rs) should fall within the control limits in the QAPP or in the
Statement of Work (SOW). If the %R falls outside of the control limits, the analysis should
be terminated, the problem corrected and documented in the data package narrative, and the
samples prepared with that LCS redigested and reanalyzed.
D.	Evaluation
1.	Verify, using the laboratory reports, preparation logs, and raw data, that the appropriate number
of required LCSs were prepared and analyzed for the data package.
2.	Verify that all results for each analyte fall within the established control limits.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R=-	x 100
True (value)
Where,
Found (value) = Concentration of each analyte measured in the analysis of the LCS
True (value) = Concentration of each analyte in the LCS
4.	Verify that the LCS was prepared at the same time as the associated samples using the same
procedures.
E.	Action
Refer to ICP-MS Table 6 for the evaluation criteria and corresponding actions for detected and non-
detected target analytes in the samples associated with deficient LCSs. For an LCS analysis that does
not meet the technical criteria, apply the actions to all samples in the same preparation batch.
Matrix spike data can be reviewed to determine batch quality if an LCS was not prepared and
analyzed with the samples.
November 2020
55

-------
Inorganic Data Review
ICP-MS
ICP-MS Table 6. LCS Actions
Criteria
Action
Detect
Non-detect
LCS not prepared with samples
J
UJ
LCS not prepared at specified concentrations
J
UJ
Aqueous/water and soil/sediment/waste %R < 40%
J-
R
Aqueous/water and soil/sediment/waste %R 40-69%
J-
UJ
Aqueous/water and soil/sediment/waste %R 70-130%
No qualification
No qualification
Aqueous/water and soil/sediment/waste %R 131-150%
J+
No qualification
Aqueous/water and soil/sediment/waste %R > 150%
R
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
56

-------
Inorganic Data Review	ICP-MS
VII. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment/waste) or for each data package.
Duplicates cannot be averaged for reporting on the Laboratory Results Report. Additional
duplicate sample analyses may be required. Alternately, the data user may require that a specific
sample be used for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the QL.
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the Quantitation
Limit (QL) should be used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that all duplicate results for each analyte fall within the established
control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation:
| S - D |
RPD = 	-1— x 100
(S + D) / 2
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of zero
(0) only for calculating the RPD. This will always yield an RPD of 200%.
E.	Action
Refer to ICP-MS Table 7 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples associated with deficient duplicates.
1. For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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
November 2020
57

-------
Inorganic Data Review
ICP-MS
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) only some of the samples in the
data package are similar to the duplicate sample, and that only these samples should be qualified;
or 2) no samples are sufficiently similar to the sample used for the duplicate analysis, and thus
only the field sample used to prepare the duplicate sample should be qualified.
2. Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3. For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
ICP-MS Table 7. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency
J
UJ
Both original sample and duplicate sample results are > 5x QL
and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are > 5x QL
and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate > QL*
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, the QAPP or project-specific SOPs for data review may allow the use of less restrictive criteria
(e.g., 35% RPD, 2x QL) to be assessed against duplicate soil samples.
November 2020
58

-------
Inorganic Data Review
ICP-MS
VIII. 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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample (pre-digestion) should be prepared and analyzed from each group of
samples with a similar matrix type (e.g., aqueous/water or soil/sediment/waste), or for each data
package. Additional matrix spike sample analyses may be required. Alternately, the data user may
require that a specific sample be used for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	For samples analyzed under the SOW, when the spike recovery falls outside of the control limits
and the sample result is < 4x the spike added, a post-digestion spike analysis should be performed
for those analytes that do not meet the specified criteria. An aliquot of the remaining unspiked
sample should be spiked at 2x the indigenous level or 2x the Quantitation Limit (QL), whichever
is greater.
5.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentrations required for the various target analytes are presented in the
methods described in the Quality Assurance Project Plan (QAPP) or in the Statement of
Work (SOW).
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all matrix spike sample results for each required analyte fall
within the established control limits If not, verify that a post-digestion spike was prepared and
analyzed.
4.	Verify that the %R values for the matrix spike are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
November 2020
59

-------
Inorganic Data Review
ICP-MS
SSR-SR
%Recovery= ——— x 100
oA
Where,
SSR = Spiked Sample Result
SR = Sample Result
SA = Spike Added
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
E. Action
Refer to ICP-MS Table 8 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 to
all samples of the same matrix, if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the Matrix Spike sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for the matrix spike
analysis, and thus only the field sample used to prepare the Matrix Spike sample should be
qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
ICP-MS Table 8. 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-digestion spike %R< 75%
J-
R
Matrix Spike %R < 30%
Post-digestion spike %R> 75%
J
UJ
Matrix Spike %R 30-74%
Post-digestion spike %R < 75%
J-
UJ
Matrix Spike %R 30-74%
Post-digestion spike %R> 75%
J
UJ
Matrix Spike %R> 125%
Post-digestion spike %R> 125%
J+
No qualification
November 2020
60

-------
Inorganic Data Review
ICP-MS
Criteria
Action
Detect
Non-detect
Matrix Spike %R > 125%Post-digestion spike %R <
125%
J
No qualification
Matrix Spike %R < 30%
No post-digestion spike performed
J-
R
Matrix Spike %R 30-74%
No post-digestion spike performed
J-
UJ
Matrix Spike %R 75-125%
No post-digestion spike is required
No qualification
No qualification
Matrix Spike %R> 125%
No post-digestion spike performed
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific Standard Operating
Procedures (SOPs) for data review may allow the use of less restrictive criteria (e.g., 10 %R
and 150 %R for the lower and upper limits) to be assessed against spike and post-digestion
spike soil samples.
November 2020
61

-------
Inorganic Data Review
ICP-MS
IX. Serial Dilution
A.	Review Items
Laboratory serial dilution reports (if available), instrument printouts, and raw data in the data
package.
B.	Objective
The objective of the serial dilution analysis is to determine if significant physical or chemical
interferences exist due to sample matrix.
C.	Criteria
1.	An ICP Serial Dilution analysis should be performed on a sample from each group of samples
with a similar matrix type (e.g., aqueous/water or soil/sediment/waste) or for each data package,
whichever is more frequent.
2.	Field samples should be used as source samples for the ICP Serial Dilution analysis.
3.	If the analyte concentration is sufficiently high [concentration in the original sample is > 5 Ox the
Method Detection Limit (MDL) that is calculated for the sample or the limit in the Quality
Assurance Project Plan (QAPP)], the Percent Difference (%D) between the original determination
and the serial dilution analysis (a five-fold dilution) after correction for dilution [concentration in
the serial dilution sample is > Quantitation Limit (QL)] should be < 20%.
D.	Evaluation
1.	Verify that the serial dilution analysis was performed on a field sample.
2.	Verify that the %D values are correct by recalculating one or more of the %Ds using the raw data
and the following equation:
Where,
I = Initial Sample Result
S = Serial Dilution Result
3. Check the raw data for any evidence of positive or negative interference (results from the diluted
sample which are significantly different from the original sample), possibly due to high levels of
dissolved solids in the sample, ionization effects, etc.
Refer to ICP-MS Table 9 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples associated with deficient serial dilution analyses.
1. For a serial dilution sample analysis that does not meet the technical criteria, apply the actions to
all samples of the same matrix if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the serial dilution sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for serial dilution, and thus
only the field sample used to prepare the serial dilution sample should be qualified.
%Difference
E. Action
November 2020
62

-------
Inorganic Data Review
ICP-MS
2. Note the potential effects on the reported data in the Data Review Narrative.
ICP-MS Table 9. Serial Dilution Actions
Criteria
Action
Detect
Non-detect
Serial Dilution analysis not performed at the
specified frequency
J
UJ
Sample concentration > 5 Ox MDL, serial dilution
sample concentration > QL, and %D > 20%*
J
No qualification
Sample concentration > 5 Ox MDL, serial dilution
sample concentration > QL, and %D < 20%
No qualification
No qualification
Sample concentration > 5x QL and serial dilution
sample concentration < QL
No qualification
No qualification
Interferences present
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above criteria are method requirements for serial dilution samples, regardless of the sample
matrix type. However, for technical review purposes only, the QAPP or the project-specific SOPs for
data review may allow the use of less restrictive criteria (e.g., %D > 25%) to be assessed against serial
dilution soil samples.
November 2020
63

-------
Inorganic Data Review
ICP-MS
X. Internal Standards
A.	Review Items
Laboratory internal standard reports (if available), instrument printouts and raw data in the data
package.
B.	Objective
The objective of internal standard analysis is to determine the existence and magnitude of instrument
drift and physical interferences.
C.	Criteria
1.	All samples analyzed during an analytical sequence, with the exception of the tune, should
contain internal standards. The minimum number of internal standards specified in the Quality
Assurance Project Plan (QAPP) or in the Statement of Work (SOW) from the list specified in the
QAPP or in the SOW should be added to each sample. If the laboratory uses lithium as an internal
standard, the laboratory should use a Li6-enriched standard. The laboratory should monitor the
same internal standards throughout the entire analytical sequence and should assign each analyte
to at least one internal standard or the number specified in the QAPP.
2.	The intensity of the internal standard response in a sample is monitored and compared to the
intensity of the response for that internal standard in the calibration blank. The Percent Relative
Intensity (%RI) in the sample should fall within the limits specified in the QAPP or in the SOW
of the response in the calibration blank. When collision or reaction cells are used, both the target
analyte and associated internal standard responses should be monitored in the same mode.
3.	If the %RI of the response in the sample falls outside of these limits, the laboratory should
reanalyze the original sample at the specified dilution with internal standard added.
D.	Evaluation
1.	Verify, using the raw data, that the minimum number of internal standards from the specified list
were used for the analysis; that the same internal standards were monitored for the entire
analytical sequence; and that each analyte was associated to the specified number of internal
standard(s).
2.	Verify, using the raw data, that these internal standards were added to each sample in the
analytical sequence, including calibrations, samples, and Quality Control (QC) samples (except
tune).
3.	Verify that the %RI between an internal standard in a sample and the internal standard in the
calibration blank was reported for each sample.
4.	Verify, using the raw data, that if the %RI for a sample was outside the limits in the QAPP or in
the SOW, the sample was reanalyzed at the specified dilution with internal standard added.
E.	Action
Refer to ICP-MS Table 10 for the evaluation criteria and corresponding actions for detected and non-
detected target analyte results in the samples with deficient internal standards. Apply the actions to
the affected analytes for each sample that does not meet the internal standard criteria.
If the Internal Standard %RI grossly exceeds the limits in both the original analysis and the diluted re-
analysis, qualify the data based on the following considerations:
a. If the %RI is greater than 200%, high recoveries are generally due to the natural presence of
the internal standard isotope in the sample(s). This occurrence may have been detected in
earlier sampling of the site. Apply another appropriate internal standard to the affected
analytes, do not qualify the analytes based on the high internal standard.
November 2020
64

-------
Inorganic Data Review
ICP-MS
b. If the Internal Standard %RI is less than 30%, it is possible that some form of signal
suppression is taking place.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
ICP-MS Table 10. Internal Standard Actions
Criteria
Action
Detect
Non-detect
Internal standards not analyzed
R
R
Less than the required number of internal standards analyzed
R
R
Target analyte not associated with internal standard
R
R
%RI 60-125%
No qualification
No qualification
%RI < 60% or > 125% and original sample reanalyzed at
specified dilution with %RI 60-125%
No qualification
No qualification
%RI < 60% or > 125% and original sample reanalyzed at
specified dilution with %RI < 60% or > 125%
J
UJ
Original sample not reanalyzed at specified dilution
J or R
UJ orR
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
November 2020
65

-------
Inorganic Data Review
ICP-MS
XI. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits (QLs) should be calculated according to the correct
equations, taking into account amount of sample prepared, final digestate volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported QLs for non-detected target analytes are calculated and reported by the
laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1.	Aqueous/Water Sample Concentration
/ vf
Concentration (|ig / L) = C / — x DF
Where,
C = Instrument value in |a,g/L (the average of all replicate integrations)
Vf = Final digestion volume (mL)
V = Initial Aliquot Amount (mL)
DF = Dilution Factor
2.	Soil/Sediment and Waste Sample Concentration
Vf
Concentration (mg/kg dry weight) = C x ——- x DF/1000
W X S
Where,
C = Instrument value in |a,g/L (the average of all replicate integrations)
Vf = Final digestion volume (mL)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
66

-------
Inorganic Data Review
ICP-MS
3. Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water samples, substitute the value of the DL or QL into the "C" term in the equation
above.
Calculate the adjusted DL or adjusted QL for soil/sediment samples as follows:
WM Vf
Adjusted DL or QL (mg/kg) = C x ——- x —— x DF
W x S Vm
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Minimum method required aliquot amount (g)
W = Initial aliquot amount (g)
Vm = Method required final sample digestion volume (mL)
Vf = Final digestion volume (mL)
S = %Solids/100
DF = Dilution Factor
November 2020
67

-------
Inorganic Data Review	ICP-MS
This page is intentionally left blank.
November 2020
68

-------
Inorganic Data Review
Mercury
MERCURY DATA REVIEW
The inorganic data requirements for mercury to be reviewed during validation are listed below:
I.	Preservation and Holding Times	71
II.	Calibration	73
III.	Blanks	76
IV.	Duplicate Sample Analysis	80
V.	Spike Sample Analysis	82
VI.	Target Analyte Quantitation	84
Mercury Table 1.	Preservation and Holding Time Actions	72
Mercury Table 2.	Calibration Actions	75
Mercury Table 3.	Blank Actions	78
Mercury Table 4.	Duplicate Sample Actions	81
Mercury Table 5.	Spike Sample Actions	83
November 2020	69

-------
Inorganic Data Review	Mercury
This page is intentionally left blank.
November 2020
70

-------
Inorganic Data Review
Mercury
I. 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.	Criteria
1.	Samples received with pH > 2 may be adjusted to pH < 2 by the laboratory. The laboratory must
allow the sample to set for at least 16 hours after acid addition before rechecking the pH. Samples
adjusted to pH < 2 by the laboratory do not require qualification.
2.	The technical holding time is determined from the date of sample collection, or the date that
Toxicity Characteristic Leaching Procedure (TCLP) or Synthetic Precipitation Leaching
Procedure (SPLP) extraction is complete, to the date of analysis.
3.	The technical holding time criteria for aqueous/water samples and TCLP/SPLP aqueous filtrates
and leachate samples is 28 days or as specified in the Quality Assurance Project Plan (QAPP),
preserved (with nitric acid) to pH < 2.
4.	The technical holding time criteria for soil/sediment and waste samples is 28 days or as specified
in the QAPP.
5.	Soil/sediment and waste samples should be maintained at < 6°C (but not frozen) or as specified in
the QAPP from the time of collection until receipt at the laboratory and should be stored at < 6°C
(but not frozen) or as specified in the QAPP from the time of sample receipt until digestion.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms, to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, appropriate sample temperature at receipt, pH), or if the pH was adjusted
upon receipt. If there is an indication of problems with the samples, the sample integrity may be
compromised. Also verify that the samples were properly stored at the laboratory.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
3.	Establish the technical holding times by comparing the sample collection dates on the sampling
documentation and the TCLP/SPLP extraction dates with the dates of analysis on the Laboratory
Results Reports and the raw data.
E.	Action
Refer to Mercury Table 1 below for the evaluation criteria and corresponding actions for detected and
non-detected mercury 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.
If a discrepancy is found between the sample analysis date 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.
November 2020
71

-------
Inorganic Data Review
Mercury
Mercury Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples received with pH > 2 and pH adjusted by
laboratory
No
qualification
No
qualification
Aqueous/water samples received with pH > 2 and pH not adjusted
J-
R
TCLP/SPLP leachates with pH > 2 and pH not adjusted
J-
R
Soil/sediment and waste samples received or stored at a temperature >
6°C but < 10°C
J
UJ
Soil/sediment/waste samples received at a temperature >10oC*
J-
R
Technical Holding Time:
Aqueous/water and TCLP/SPLP leachates
>28 days
J-
R
Technical Holding Time:
Soil/sediment and waste samples > 28 days
J-
R
Samples properly preserved and analyzed within specified holding
time
No
qualification
No
qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
* For samples received with shipping container temperatures > 10°C, 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.
November 2020
72

-------
Inorganic Data Review
Mercury
II. 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.	Critical
1.	Initial Calibration
The instruments should be successfully calibrated daily, or as specified in the Quality Assurance
Project Plan (QAPP) or in the Statement of Work (SOW), and each time the instrument is set up.
The calibration date and time should be included in the raw data. For samples analyzed under the
SOW, the calibration curve standards should be prepared by the same method used to prepare the
samples for analysis. The curve should be prepared with the samples that will be analyzed using
this calibration curve.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish the calibration curve. At least one of the calibration standards
should be at or below the Quantitation Limit (QL) in the QAPP or in the SOW but above
the Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy Quality Control (QC)
requirements. The calibration curve may be fitted using linear regression or weighted
linear regression, or other fits as specified in the QAPP. The curve may be forced through
zero. For linear fits, the calibration curve should have a correlation coefficient greater
than the value specified in the QAPP or in the SOW. The calculated percent differences
(%Ds) or other specified statistical test values for all non-zero standards should fall
within the limits in the QAPP or in the SOW.
2.	Initial and Continuing Calibration Verification
For samples analyzed under the SOW, these standards should be prepared by the same method
used to prepare the samples for analysis.
a.	Initial Calibration Verification (ICV)
i.	Immediately after the system has been calibrated, the accuracy of the initial calibration
should be verified and documented by the analysis of an ICV standard. If the ICV Percent
Recovery (%R) falls outside of the control limits, the analysis should be terminated, the
problem corrected and documented in the data package narrative, the instrument
recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of the analyte from an
independent standard source, at a concentration level other than that used for instrument
calibration and near the middle of the calibrated range (within ±30%).
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV should be analyzed and
reported.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every
hour during an analytical sequence. The CCV standard should also be analyzed at the
beginning of the analytical sequence, and again after the last analytical sample.
November 2020
73

-------
Inorganic Data Review	Mercury
iii.	The CCV standard should be prepared using the same source and in the same acid matrix
as the calibration standards at a concentration at or near the mid-level (within ±30%) of
the respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
v.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vi.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified by the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW, but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP. Confirm that calibration standards and samples were prepared at the same
time.
2.	Verify that the ICV and CCV standards were analyzed at the specified frequency and at the
appropriate concentration. Verify that acceptable %R results were obtained.
3.	Confirm that an instrument blank was not analyzed before the CCV.
4.	Verify that the ICV and CCV %R values are correct by recalculating one or more of the %Rs
using the raw data and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of mercury measured in the analysis of the ICV or CCV solution
True (value) = Concentration of mercury in the ICV or CCV source
E.	Action
Refer to Mercury Table 2 below for the evaluation criteria and corresponding actions for detected and
non-detected mercury results in the samples associated with deficient initial calibrations or calibration
verification standards.
1.	For initial calibrations or ICV standard analyses that do not meet the technical criteria, apply the
actions to the associated samples reported from the analytical sequence.
2.	For CCV standard 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).
November 2020
74

-------
Inorganic Data Review
Mercury
NOTE: For critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
Mercury Table 2. 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 or R
UJ orR
For linear fits, correlation coefficient < 0.995
J
UJ
%D outside ±30%, or other specified statistical
test values outside limits
J
UJ
Calibration Standards and/or ICV/CCV not
prepared with samples
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R< 70%
J- or R
UJ orR
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+ or R
No qualification
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
75

-------
Inorganic Data Review
Mercury
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed at the wavelength used for analysis after
the analytical standards, but not before analysis of the ICV standard during the initial calibration
of the instrument. The ICB should be prepared by the same method used to prepare the samples
for analysis. The ICB result (absolute value) should not be greater than or equal to the
Quantitation Limit (QL).
3.	A Continuing Calibration Blank (CCB) should be analyzed immediately after every Continuing
Calibration Verification (CCV) standard. The CCB should be prepared by the same method used
to prepare the samples for analysis. The CCB should be analyzed at the frequency specified in the
Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW) during the analytical
sequence. The CCB should be analyzed at the beginning of the analytical sequence, and again
after the last CCV that was analyzed after the last analytical sample of the analytical sequence.
The CCB result (absolute value) should not be greater than or equal to the QL.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples digested, whichever is more frequent. The Preparation
Blank consists of reagent water processed through the appropriate sample preparation and
analysis procedure.
5.	If the mercury concentration in the Preparation Blank is greater than or equal to the QL, the
lowest concentration of mercury in the associated samples should be > lOx the Preparation Blank
concentration. Otherwise, all associated samples with a mercury concentration < lOx the
Preparation Blank concentration and > the QL should be redigested and reanalyzed. The
laboratory is not to correct the sample concentration for the blank value.
6.	If the mercury concentration in the Preparation Blank is < (-QL), all associated samples with
mercury concentrations < 1 Ox the QL should be redigested and reanalyzed.
7.	At least one Leachate Extraction Blank (LEB) should be prepared and analyzed for each batch of
samples extracted by Toxicity Characteristic Leaching Procedure (TCLP) or Synthetic
Precipitation Leaching Procedure (SPLP). The LEB consists of reagent water processed through
the extraction procedure. Post-extraction, the LEB should be processed through the appropriate
sample preparation and analysis procedure.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks and LEBs are prepared and
analyzed as appropriate for the data package (e.g., total number of samples, various types of
matrices present, number of digestion batches, etc.).
2.	Verify, using the digestion log, that the ICB and CCB were digested by the same method used to
prepare the samples.
November 2020
76

-------
Inorganic Data Review
Mercury
3.	For an ICB or a CCB, verify that if the absolute value of mercury was greater than or equal to the
QL, the analysis was terminated, the problem corrected and documented in the data package
narrative, the instrument recalibrated, and the preceding 10 analytical samples or all analytical
samples analyzed since the last compliant calibration blank reanalyzed.
4.	For a Preparation Blank, verify that if the concentration of mercury was greater than or equal to
the QL, all associated samples with mercury concentration > the QL but < 1 Ox the Preparation
Blank concentration were redigested and reanalyzed. Verify that if the mercury concentration was
< (-QL) in a Preparation Blank, all associated samples with mercury concentration < lOx the QL
were redigested and reanalyzed.
5.	Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to Mercury Table 3 below for the evaluation criteria and corresponding actions for detected and
non-detected mercury results in the samples associated with deficient blanks.
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 3 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 3 below.
7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be checked
against a less dilute run, 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 negatives exists.
NOTE: 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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
November 2020
77

-------
Inorganic Data Review
Mercury
Mercury Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J
ICB/CCB
Not digested
Detect or non-detect
Use professional judgment
ICB/CCB
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
ICB/CCB
< (-MDL) but
>(-QL)
Non-Detect
UJ
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank/LEB
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/LEB/
Field Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/LEB/
Field Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/LEB/
Field Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < lOx the Preparation
Blank/LEB Result
Report at Preparation Blank/LEB
Result and qualify J+ or R
> lOx the Preparation
Blank/LEB Result
No qualification
November 2020
78

-------
Inorganic Data Review
Mercury
Blank Type
Blank Result
Sample Result
Action


Non-detect
UJ
Preparation
Blank/LEB/
Field Blank
<(-QL)
Detect < QL
J-
> QL but < lOx QL
J-


> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
79

-------
Inorganic Data Review	Mercury
IV. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment/waste) or for each data package.
Duplicates cannot be averaged for reporting on the Laboratory Results Report. Additional
duplicate sample analyses may be required. Alternately, the data user may require that a specific
sample be used for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the
Quantitation Limit (QL).
4.	For samples analyzed under the SOW, a control limit of the QL should be used if either the
sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that the duplicate results fall within the established control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation:
S-D
RPD= '	x 100
(S + D) / 2
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of zero
(0) only for calculating the RPD. This will always yield an RPD of 200%.
November 2020
80

-------
Inorganic Data Review
Mercury
E. Action
Refer to Mercury Table 4 below for the evaluation criteria and corresponding actions for detected and
non-detected mercury results in the samples associated with deficient duplicates.
1.	For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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 mercury) in determining similarity between
samples in the data package. Two possible determinations are: 1) only some of the samples in the
data package are similar to the duplicate sample, and that only these samples should be qualified;
or 2) no samples are sufficiently similar to the sample used for the duplicate analysis, and thus
only the field sample used to prepare the duplicate sample should be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
Mercury Table 4. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample results < 5x QL (including non-detects)
and absolute difference between sample and duplicate >
QL*
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, the QAPP or the project-specific SOPs for data review may allow the use of less restrictive
criteria (e.g., 35% RPD, 2x QL) to be assessed against duplicate soil samples.
November 2020
81

-------
Inorganic Data Review	Mercury
V. 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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample should be prepared and analyzed from each group of samples with a
similar matrix type (e.g., aqueous/water or soil/sediment/waste), or for each data package.
Additional matrix spike sample analyses may be required. Alternately, the data user may require
that a specific sample be used for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentration required is presented in the method described in the Quality
Assurance Project Plan (QAPP) or in the SOW.
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log, and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all Matrix Spike sample results fall within the established control
limits.
4.	Verify that the %R values for the matrix spike are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
SSR-SR
%R = ——— x 100
SA
Where,
SSR = Spiking analyte result in the spiked sample
SR = Result of the same analyte in the original sample
SA = Spike added in the spiked sample
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating
the %R.
November 2020
82

-------
Inorganic Data Review
Mercury
E. Action
Refer to Mercury Table 5 below for the evaluation criteria and corresponding actions for detected and
non-detected mercury 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 to
all samples of the same matrix if the samples are considered sufficiently similar. 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 mercury) in determining similarity between
samples in the data package. Two possible determinations are: 1) only some of the samples in the
data package are similar to the Matrix Spike sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for the matrix spike
analysis, and thus only the field sample used to prepare the Matrix Spike sample should be
qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
Mercury Table 5. 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%
J-
R
Matrix Spike %R 30-74%
J-
UJ
Matrix Spike %R 75-125%
No qualification
No qualification
Matrix Spike %R >125%
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific SOPs for data review may
allow the use of less restrictive criteria (e.g., 10 %R and 150 %R for the lower and upper
limits) to be assessed against spike soil samples.
November 2020
83

-------
Inorganic Data Review	Mercury
VI. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final digestate volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1.	Aqueous/Water and TCLP/SPLP Leachate Sample Concentration
Hg Concentration (jxg/L) = C x DF
Where,
C = Instrument value in |a,g/L from the calibration curve
DF = Dilution Factor
2.	Soil/Sediment and Waste Sample Concentration
Vf
Concentration (mg/kg) = C X —		 X DF/1000
W x S
Where,
Concentration = Analyte/Result (mg/kg)
C = Instrument value in |ig/L from the calibration curve
Vf = Final digestion volume (mL)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
84

-------
Inorganic Data Review
Mercury
3. Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water or Total Characteristic Leaching Procedure (TCLP)/Synthetic Precipitation
Leaching Procedures (SPLP) leachate samples, substitute the value of the DL or QL, in the
appropriate units, into the "C" term in the equation above.
Calculate the adjusted DL or adjusted QL for soil/sediment and waste samples as follows:
W
Adjusted DL or QL (mg/kg) = C x m x DF
W X S
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Method required minimum sample weight (g)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
85

-------
Inorganic Data Review	Mercury
This page is intentionally left blank.
November 2020
86

-------
Inorganic Data Review
Cyanide
CYANIDE DATA REVIEW
The inorganic data requirements for cyanide to be reviewed during validation are listed below:
I.	Preservation and Holding Times	89
II.	Calibration	91
III.	Blanks	94
IV.	Duplicate Sample Analysis	98
V.	Spike Sample Analysis	100
VI.	Target Analyte Quantitation	103
Cyanide Table 1. Preservation and Holding Time Actions	90
Cyanide Table 2. Calibration Actions	93
Cyanide Table 3. Blank Actions	96
Cyanide Table 4. Duplicate Sample Actions	99
Cyanide Table 5. Spike Sample Actions	101
November 2020	87

-------
Inorganic Data Review	Cyanide
This page is intentionally left blank.
November 2020
88

-------
Inorganic Data Review
Cyanide
I. 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.	Criteria
1.	The technical holding time is determined from the date of sample collection, or the date that
Synthetic Precipitation Leaching Procedure (SPLP) extraction is complete, to the date of analysis.
2.	The technical holding time criteria for aqueous/water samples, and SPLP aqueous filtrate and
leachate samples is 14 days or as specified in the Quality Assurance Project Plan (QAPP),
preserved (with sodium hydroxide) to pH >10.
3.	The technical holding time criteria for soil/sediment and waste samples is 14 days or as specified
in the QAPP.
4.	Aqueous/water and soil/sediment/waste samples should be maintained at < 6°C (but not frozen) or
as specified in the QAPP from the time of collection until receipt at the laboratory and be stored
at < 6°C (but not frozen) or as specified in the QAPP from the time of sample receipt until
distillation. The SPLP leachates should be stored at < 6°C (but not frozen) or as specified in the
QAPP from the time of the leaching procedure completion until preparation.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, appropriate sample temperature at receipt, pH). If there is an indication of
problems with the samples, the sample integrity may be compromised. Also verify that the
samples were properly stored at the laboratory For aqueous/water samples, look for evidence that
the samples were tested for the presence of sulfides, oxidizing agents, and nitrate/nitrite, and
whether the appropriate preservation steps were taken.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
3.	Establish the technical holding times by comparing the sample collection dates on the sampling
documentation and the SPLP extraction dates with the dates of analysis on the Laboratory Results
Reports.
E.	Action
Refer to Cyanide Table 1 for the evaluation criteria and corresponding actions for detected and non-
detected cyanide 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.
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.
November 2020
89

-------
Inorganic Data Review
Cyanide
Cyanide Table 1. Preservation and Holding Time 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
Aqueous/water and soil/sediment/waste samples received or stored
*1 O ^ ^
at a temperature > 10 C
J-
R
Technical Holding Time:
Aqueous/water 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
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The true direction of any bias may be unknown in this case. Use caution in determining whether some
detected analytes should be qualified as estimated low (J-) or as estimated high (J+), based on
knowledge of the potential presence of other compounds that may react with cyanide or related
compounds (e.g., thiocyanate). Refer to the Note under Part A, Section II, General Table 1. Data
Qualifiers and Definitions for additional guidance on the use of the J+ and J- qualifiers.
** For samples received with shipping container temperatures > 10°C, 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.
November 2020
90

-------
Inorganic Data Review
Cyanide
II. 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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated daily or as specified in the Quality Assurance
Project Plan (QAPP) or in the Statement of Work (SOW) and each time the instrument is set up.
The calibration date and time should be included in the raw data. For samples analyzed under the
SOW, the calibration curve standards should be distilled by the same method used to prepare the
samples for analysis.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish the calibration curve. At least one of the calibration standards
should be at or below the Quantitation Limit (QL) in the QAPP or in the SOW but above
the Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy QC requirements. The
calibration curve may be fitted using linear regression or weighted linear regression, or
other fits as specified in the QAPP. The curve may be forced through zero. For linear fits,
the calibration curve should have a correlation coefficient greater than the value specified
in the QAPP or in the SOW. The calculated percent differences (%Ds) or other specified
statistical test values for all non-zero standards should be within the limits in the QAPP
or in the SOW.
2.	Initial and Continuing Calibration Verification
For samples analyzed under the SOW, these standards should be distilled by the same method
used to prepare the samples for analysis.
a.	Initial Calibration Verification (ICV)
i.	Immediately after each colorimetric system has been calibrated, the accuracy of the initial
calibration should be verified and documented by the analysis of an ICV standard. If the
ICV Percent Recovery (%R) falls outside of the control limits, the analysis should be
terminated, the problem corrected and documented in the data package narrative, the
instrument recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of the analyte from an
independent standard source, at a concentration level other than that used for instrument
calibration and near the middle of the of the calibrated range (within ±30%).
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV standard should be
analyzed and reported.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every
hour during an analytical sequence. The CCV standard should also be analyzed at the
beginning of the analytical sequence, and again after the last analytical sample.
November 2020
91

-------
Inorganic Data Review	Cyanide
iii.	The CCV standard should be prepared using the same source and in the same base matrix
as the calibration standards at a concentration at or near the mid-level (within ±30%) of
the respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
v.	The CCV should be processed and analyzed in the same fashion as an actual sample. If
the %R of the CCV was outside of the control limits, the analysis should be terminated,
the problem corrected and documented in the data package narrative, the instrument
recalibrated, and all analytical samples analyzed since the last compliant CCV
reanalyzed.
vi.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified in the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW, but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements.. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are with the limits
specified in the QAPP.
2.	Verify, using the distillation log, that the calibration standards, the ICV, and the CCV standards
were distilled.
3.	Confirm that an instrument blank was not analyzed before the CCV.
4.	Verify that the ICV and CCV standards were analyzed at the specified frequency and at the
appropriate concentration. Verify that acceptable %R results were obtained.
5.	Verify that the ICV or CCV %R values are correct by recalculating one or more of the %Rs using
the raw data and the following equation:
Found (value)
%R = True (value) " 100
Where,
Found (value) = Concentration of cyanide measured in the analysis of the ICV or CCV solution
True (value) = Concentration of cyanide in the ICV or CCV source
E.	Action
Refer to Cyanide Table 2 for the evaluation criteria and corresponding actions for detected and non-
detects cyanide results in the samples associated with deficient initial calibrations or calibration
verification standards.
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 standard analyses that do not meet the technical criteria, apply the actions to all samples
analyzed between a previous technically acceptable analysis of the Quality Control (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).
November 2020
92

-------
Inorganic Data Review
Cyanide
NOTE: For critical samples, a further in-depth evaluation of the calibration curve may be
warranted to determine if additional qualification is necessary.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
Cyanide Table 2. 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 or R
UJ orR
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%
J- or R
UJ orR
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+ or R
No qualification
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
93

-------
Inorganic Data Review
Cyanide
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed at the wavelength used for analysis after
the analytical standards, but not before analysis of the Initial Calibration Verification (ICV)
standard during the initial calibration of the instrument. The ICB should be distilled by the same
method used to prepare the samples for analysis. The ICB result (absolute value) should not be
greater than or equal to the Quantitation Limit (QL).
3.	A Continuing Calibration Blank (CCB) should be analyzed immediately after every Continuing
Calibration Verification (CCV) standard. The CCB should be distilled by the same method used
to prepare the samples for analysis. The CCB should be analyzed at the frequency specified in the
Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW) during the analytical
sequence. The CCB should be analyzed at the beginning of the analytical sequence, and again
after the last CCV that was analyzed after the last analytical sample of the analytical sequence.
The CCB result (absolute value) should not be greater than or equal to the QL.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples distilled, whichever is more frequent. The Preparation
Blank consists of reagent water processed through the appropriate sample preparation and
analysis procedure.
5.	If the cyanide concentration in the Preparation Blank is greater than or equal to the QL, the lowest
concentration of cyanide in the associated samples should be > 1 Ox the Preparation Blank
concentration. Otherwise, all associated samples with a cyanide concentration < lOx the
Preparation Blank concentration and > the QL should be redistilled and reanalyzed. The
laboratory is not to correct the sample concentration for the blank value.
6.	If the cyanide concentration in the Preparation Blank is < (-QL), all associated samples with a
cyanide concentration < 1 Ox the QL should be redistilled and reanalyzed.
7.	At least one Leachate Extraction Blank (LEB) should be prepared and analyzed for each batch of
samples extracted by Synthetic Precipitation Leaching Procedure (SPLP). The LEB consists of
reagent water processed through the extraction procedure. Post-extraction, the LEB should be
processed through the appropriate sample preparation and analysis procedure.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks and LEBs are prepared and
analyzed as appropriate for the data package (e.g., total number of samples, various types of
matrices present, number of distillation batches, etc.).
2.	Verify, using the distillation log, that the ICB and CCB were distilled by the same method used to
prepare the samples.
3.	For an ICB or a CCB, verify that if the absolute value of cyanide was greater than or equal to the
QL, the analysis was terminated, the problem corrected and documented in the data package
November 2020
94

-------
Inorganic Data Review
Cyanide
narrative, the instrument recalibrated, and the preceding 10 analytical samples or all analytical
samples analyzed since the last compliant calibration blank reanalyzed.
4.	For a Preparation Blank, verify that if the concentration of cyanide was greater than or equal to
the QL, all associated samples with a cyanide concentration > the QL but < 1 Ox the Preparation
Blank concentration were redistilled and reanalyzed. Verify that if the cyanide concentration was
< (-QL) in a Preparation Blank, all associated samples with a cyanide concentration < lOx the QL
were redistilled and reanalyzed.
5.	Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. 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 blanks.
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 3 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 3 below.
7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be checked
against a less dilute run, 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 negatives exists.
NOTE: 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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
November 2020
95

-------
Inorganic Data Review
Cyanide
Cyanide Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J
ICB/CCB
Not distilled
Detect or non-detect
Use professional judgment
ICB/CCB
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
ICB/CCB
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank/LEB
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/LEB/
Field Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/LEB/
Field Blank
< (-MDL) but
>(-QL)
Non-detect
No qualification
Detect
J- or no qualification
Preparation
Blank/LEB/
Field Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but
< 1 Ox the Preparation
Blank/LEB Result
Report at Preparation Blank/LEB
Result and qualify J+ or R
> 1 Ox the Preparation
Blank/LEB Result
No qualification

<(-QL)
Non-detect
UJ
Detect < QL
J-
November 2020
96

-------
Inorganic Data Review
Cyanide
Blank Type
Blank Result
Sample Result
Action
Preparation
Blank/LEB/
Field Blank

> QL but < 1 Ox QL
J-
> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
97

-------
Inorganic Data Review	Cyanide
IV. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment/waste) or for each data package.
Duplicates cannot be averaged for reporting on the Laboratory Results Report. Additional
duplicate sample analyses may be required. Alternately, the data user may require that a specific
sample be used for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the
Quantitation Limit (QL).
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the QL should be
used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed for the
data package.
2.	Verify, using the raw data, that the duplicate results fall within the established control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation:
|S - D|
RPD = —!	x 100
(S + D) / 2
Where,
S = Sample result (original)
D = Duplicate result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of zero
(0) only for calculating the RPD. This will always yield an RPD of 200%.
November 2020
98

-------
Inorganic Data Review
Cyanide
E. Action
Refer to Cyanide Table 4 for the evaluation criteria and corresponding actions for detected and non-
detected cyanide results in the samples associated with deficient duplicates.
1.	For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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) only some of the samples in the
data package are similar to the duplicate sample, and that only these samples should be qualified;
or 2) no samples are sufficiently similar to the sample used for the duplicate analysis, and thus
only the field sample used to prepare the duplicate sample should be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
Cyanide Table 4. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%*
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate > QL*
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, the QAPP or the project-specific SOPs for data review may allow the use of less restrictive
criteria (e.g., 35% RPD, 2x QL) to be assessed against duplicate soil samples.
November 2020
99

-------
Inorganic Data Review	Cyanide
V. 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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample (pre-distillation) should be prepared and analyzed from each group of
samples with a similar matrix type (e.g., aqueous/water or soil/sediment/waste), or for each data
package. Additional matrix spike sample analyses may be required. Alternately, the data user may
require that a specific sample be used for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	For samples analyzed under the SOW, when the spike recovery falls outside of the control limits
and the sample result is < 4x the spike added, a post-distillation spike analysis should be
performed. An aliquot of the remaining unspiked sample should be spiked at 2x the indigenous
level or 2x the Quantitation Limit (QL), whichever is greater.
5.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentration required is presented in the method described in the Quality
Assurance Project Plan (QAPP) or in the SOW.
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all pre-distillation matrix spike sample results fall within the
established control limits. If not, verify that a post-distillation spike was prepared and analyzed.
4.	Verify that the %R values for the matrix spike are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
SSR-SR
%Recovery= ——	 x 100
oA
Where,
SSR = Spiked Sample Result
SR = Sample Result
SA = Spike Added
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
November 2020
100

-------
Inorganic Data Review
Cyanide
E. Action
Refer to Cyanide Table 5 for the evaluation criteria and corresponding actions for detected and non-
detected cyanide 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 to
all samples of the same matrix if the samples are considered sufficiently similar. 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 cyanide) in determining similarity between
samples in the data package. Two possible determinations are: 1) only some of the samples in the
data package are similar to the Matrix Spike sample, and that only these samples should be
qualified; or 2) no samples are sufficiently similar to the sample used for the matrix spike
analysis, and thus only the field sample used to prepare the Matrix Spike sample should be
qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
Cyanide Table 5. Spike Sample Actions
Criteria
Action
Detect
Non-detect
Matrix Spike 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
Matrix Spike %R 30-74%
No post-distillation spike performed
J-
UJ
November 2020
101

-------
Inorganic Data Review
Cyanide
Criteria
Action
Detect
Non-detect
Matrix Spike %R 75-125%
No post-distillation is required
No qualification
No qualification
Matrix Spike %R >125%
No post-distillation spike performed
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific SOPs for data review may
allow the use of less restrictive criteria (e.g., 10 %R and 150 %R for the lower and upper
limits) to be assessed against spike soil samples.
November 2020
102

-------
Inorganic Data Review
Cyanide
VI. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final distillate volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1. Aqueous/Water and SPLP Sample Concentration
Where,
C =	Instrument response in |a,g/L CN from the calibration curve
Vf =	Final prepared (absorbing solution) volume (mL)
V =	Initial aliquot amount (mL)
DF =	Dilution Factor
2. Soil/Sediment and Waste Sample Concentration
Vf
Concentration (mg/kg) = C X —		 X DF/1000
W x S
Where,
Concentration = Analyte/Result (mg/kg)
CN Concentration (|ig/L) = C
C = Instrument response in |ig/L CN from the calibration curve
Vf = Final prepared (absorbing solution) volume (mL)
W = Initial aliquot amount (g)
November 2020
103

-------
Inorganic Data Review
Cyanide
S = %Solids/100
DF = Dilution Factor
3. Adjusted DL (or MDL)/Adjusted QL:
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water or SPLP leachate samples, substitute the value of the DL or QL into the "C" term
in the equation above.
Calculate the adjusted DL or adjusted QL for all soil/sediment and waste samples as follows:
Adjusted DL or QL (mg/kg) = C x M x DF
W X S
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Minimum method required aliquot amount (g)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
104

-------
Inorganic Data Review
Anions by Ion Chromatography
ANIONS DATA REVIEW
The inorganic data requirements for anions to be reviewed during validation are listed below:
I.	Preservation and Holding Times	107
II.	Calibration	109
III.	Blanks	112
IV.	Laboratory Control Sample	115
V.	Duplicate Sample Analysis	117
VI.	Spike Sample Analysis	119
VII.	Target Analyte Quantitation	121
Anions Table 1. Preservation and Holding Time Actions	108
Anions Table 2. Calibration Actions	Ill
Anions Table 3. Blank Actions	113
Anions Table 4. LCS Actions	116
Anions Table 5. Duplicate Sample Actions	118
Anions Table 6. Spike Sample Actions	120
November 2020
105

-------
Inorganic Data Review	Anions by Ion Chromatography
This page is intentionally left blank.
November 2020
106

-------
Inorganic Data Review
Anions by Ion Chromatography
I. 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: 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.	Criteria
1.	The technical holding time is determined from the date and time of sample collection to the date
and time of analysis.
2.	The technical holding time criteria for aqueous/water samples for nitrate, nitrite, and
orthophosphate is 48 hours or as specified in the Quality Assurance Project Plan (QAPP). For all
other analytes the holding time is 28 days or as specified in the QAPP.
3.	The technical holding time criteria for soil/sediment samples is 48 hours for nitrate, nitrite, and
orthophosphate, and 28 days for all other analytes, or as specified in the QAPP.
4.	Aqueous/water samples and soil/sediment samples should be maintained at < 6°C (but not frozen)
or as specified in the QAPP from the time of collection until receipt at the laboratory.
Aqueous/water samples to be analyzed for nitrate, nitrite, orthophosphate, or sulfate, and all
soil/sediment samples should be stored at < 6°C (but not frozen) or as specified in the QAPP from
the time of sample receipt until analysis or extraction. Samples for orthophosphate analysis
should not be held at room temperature for more than 12 cumulative hours.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms to
determine if the samples arrived at the laboratory in proper condition (e.g., received intact,
appropriate sample temperature at receipt). If there is an indication of problems with the samples,
the sample integrity may be compromised. Also verify that the samples were properly stored at
the laboratory. Use professional judgment to evaluate the effect of the problem on the sample
results.
2.	Verify that the analysis dates and times on the Laboratory Results Reports and the raw data are
identical.
3.	Establish the technical holding times by comparing the sample collection dates and times on the
sampling documentation with the dates and times of analysis on the Laboratory Results Reports
and the raw data.
E.	Action
Refer to Anions Table 1 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.
If a discrepancy is found between the sample analysis dates and times 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.
November 2020
107

-------
Inorganic Data Review
Anions by Ion Chromatography
Anions Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples for nitrate, nitrite, orthophosphate, or
sulfate and soil/sediment samples received at a temperature
> 6°C but < 10°C
J
UJ
Aqueous/water samples for nitrate, nitrite, orthophosphate, or
sulfate and soil/sediment samples received at a temperature
> 10°C*
J-
R
Technical Holding Time:
Aqueous/water samples for nitrate, nitrite, or orthophosphate
>48 hours
J-
R
Technical Holding Time:
Aqueous/water samples for all other analytes
>28 days
J-
R
Technical Holding Time:
Soil/sediment samples for nitrate, nitrite, or orthophosphate
>48 hours
J-
R
Technical Holding Time:
Soil/sediment samples for all other analytes > 28 days
J-
R
Samples properly preserved and analyzed within specified
holding time
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
* For samples received with shipping container temperatures > 10°C, 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.
November 2020
108

-------
Inorganic Data Review
Anions by Ion Chromatography
II. 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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated weekly or as specified in the Quality Assurance
Project Plan (QAPP) or in the Statement of Work (SOW), and each time the instrument is set up.
The calibration date and time should be included in the raw data.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW)
should be used to establish the calibration curves. At least one of the calibration standards
should be at or below the Quantitation Limit (QL) in the QAPP or in the SOW but above
the Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy QC requirements. The
calibration curves may be fitted using linear regression or weighted linear regression, or
other fits as specified in the QAPP. The curves may be forced through zero. For linear
fits, the calibration curves should have a correlation coefficient greater than the value
specified in the QAPP or in the SOW. The calculated percent differences (%Ds) or other
specified statistical test values for all non-zero standards should fall within the limits in
the QAPP or in the SOW.
2.	Initial and Continuing Calibration Verification
a.	Initial Calibration Verification (ICV)
i.	Immediately after the system has been calibrated as well as each day prior to the analysis
of the opening Continuing Calibration Verification (CCV) and Continuing Calibration
blank (CCB), the accuracy of the initial calibration should be verified and documented by
the analysis of an ICV standard. If the ICV Percent Recovery (%R) falls outside of the
control limits, the analysis should be terminated, the problem corrected and documented
in the data package narrative, the instrument recalibrated, and all affected samples
reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of the target analytes
from an independent standard source, at concentration levels other than that used for
instrument calibration and near the middle of the calibrated range (within ±30%).
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV should be analyzed and
reported.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every
10 samples during an analytical sequence. The CCV standard should also be analyzed at
the beginning of the analytical sequence, and again after the last analytical sample.
iii.	The CCV standard should be prepared using the same source and in the same matrix as
the calibration standards by combining compatible analytes at a concentration at or near
the mid-level (within ±30%) of the respective calibration curve.
November 2020
109

-------
Inorganic Data Review	Anions by Ion Chromatography
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
v.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vi.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified by the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW, but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP.
2.	Verify that the ICV and CCV standards were analyzed at the specified frequency and at the
appropriate concentration. Verify that acceptable %R results were obtained.
3.	Confirm that an instrument blank was not analyzed before the CCV.
4.	Verify that the ICV and CCV %R values are correct by recalculating one or more of the %Rs
using the raw data and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of the target analyte measured in the analysis of the ICV or
CCV solution
True (value) = Concentration of the target analyte in the ICV or CCV source
E.	Action
Refer to Anions Table 2 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient initial calibrations or
calibration verification standards.
1.	For initial calibration or ICV standard analyses that do not meet the technical criteria, apply the
action to the associated samples reported from the analytical sequence.
2.	For CCV standard analyses that do not meet the technical criteria, apply the actions to all samples
analyzed between a previous technically acceptable analysis of the Quality Control (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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
November 2020
110

-------
Inorganic Data Review
Anions by Ion Chromatography
Anions Table 2. 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 or R
UJ orR
For linear fits, the correlation coefficient < 0.995
J
UJ
%D outside ±30%, or other specified statistical test
values outside limits
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R <75%
J- or R
R
ICV/CCV %R 75-89%
J-
UJ
ICV/CCV %R 90-110%
No qualification
No qualification
ICV/CCV %R 111-125%
J+
No qualification
ICV/CCV %R> 125%
J+ or R
No qualification
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
111

-------
Inorganic Data Review
Anions by Ion Chromatography
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed after the analytical standards, but not
before analysis of the ICV standard during the initial calibration of the instrument. The ICB result
(absolute value) for the target analytes should not be greater than or equal to the respective
Quantitation Limits (QLs).
3.	A Continuing Calibration Blank (CCB) should be analyzed immediately after every Continuing
Calibration Verification (CCV) standard. The CCB should be analyzed at the frequency specified
in the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW) during the
analytical sequence. The CCB should be analyzed at the beginning of the analytical sequence, and
again after the last CCV that was analyzed after the last analytical sample of the analytical
sequence. The CCB result (absolute value) for the target analytes should not be greater than or
equal to the respective QL.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples prepared, whichever is more frequent. The Preparation
Blank consists of reagent water processed through the appropriate sample preparation and
analysis procedure.
5.	If the concentration of any analyte in the Preparation Blank is greater than or equal to the QL, the
lowest concentration of that analyte in the associated samples should be > lOx the Preparation
Blank concentration. Otherwise, all associated samples with the analyte's concentration < lOxthe
Preparation Blank concentration and > the QL should be reprepared and reanalyzed. The
laboratory is not to correct the sample concentration for the blank value.
6.	If the concentration of any analyte in the Preparation Blank is < (-QL), all associated samples
with the analyte's concentration < lOx the QL should be reprepared and reanalyzed.
D. Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks are prepared and analyzed as
appropriate for the data package (e.g., total number of samples, various types of matrices present,
number of preparation batches, etc.).
2.	For an ICB or a CCB, verify that if the absolute value of any target analyte was greater than or
equal to the QL, the analysis was terminated, the problem corrected and documented in the data
package narrative, the instrument recalibrated, and the preceding 10 analytical samples or all
analytical samples analyzed since the last compliant calibration blank reanalyzed.
3.	For a Preparation Blank, verify that if the concentration of any target analyte was greater than or
equal to the QL, all associated samples with the analyte's concentration > the QL but < lOx the
Preparation Blank concentration were reprepared and reanalyzed for that analyte. Verify that if a
concentration was < (-QL) in a Preparation Blank, all associated samples with the analyte's
concentration < 1 Ox the QL were reprepared and reanalyzed.
November 2020
112

-------
Inorganic Data Review
Anions by Ion Chromatography
4. Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to Anions Table 3 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient blanks.
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.
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 3 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 3 below.
7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be checked
against a less dilute run, 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 negatives exists.
NOTE: 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 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 samples for comparison purposes.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
Anions Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J


Non-detect
No qualification
ICB/CCB
Detect < QL
Detect < QL
Report at QL and qualify U


> QL
J+ or no qualification
ICB/CCB

Non-detect
UJ
November 2020
113

-------
Inorganic Data Review
Anions by Ion Chromatography
Blank Type
Blank Result
Sample Result
Action

< (-MDL) but
>(-QL)
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/Field
Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/Field
Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/Field
Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < lOx the Preparation
Blank Result
Report at Preparation Blank
Result and qualify J+ or R
> 1 Ox the Preparation Blank
Result
No qualification
Preparation
Blank/Field
Blank
<(-QL)
Non-detect
UJ
Detect < QL
J-
> QL but < lOx QL
J-
> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
114

-------
Inorganic Data Review	Anions by Ion Chromatography
IV. Laboratory Control Sample
A.	Review Items
Laboratory LCS reports (if available), preparation 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 the recovery of the
prepared Laboratory Control Sample (LCS).
C.	Criteria
1.	Aqueous/water and soil/sediment LCSs should be analyzed for each analyte utilizing the same
sample preparations, analytical methods, and Quality Assurance/Quality Control (QA/QC)
procedures as employed for the samples.
2.	One LCS should be prepared and analyzed for every group of aqueous/water or soil/sediment
samples in a data package or with each batch of samples prepared, whichever is more frequent.
The LCS should be spiked such that it contains each analyte at the level specified in the QAPP or
at 2x the Quantitation Limit (QL) for the associated matrix.
3.	All LCS %Rs should fall within the control limits of in the Quality Assurance Project Plan
(QAPP) or in the Statement of Work (SOW). If the Percent Recovery (%R) for the aqueous/water
and soil/sediment LCS falls outside of the control limits, the analysis should be terminated, the
problem corrected and documented in the data package narrative, and the samples prepared with
that LCS reprepared and reanalyzed.
D.	Evaluation
1.	Verify, using the laboratory reports, preparation logs, and raw data, that the appropriate number
of required LCSs were prepared and analyzed for the data package.
2.	Verify that all results for each analyte fall within the established control limits.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R= T,W,t) *'°0
Where,
Found (value) = Concentration of each analyte measured in the analysis of the LCS
True (value) = Concentration of each analyte in the LCS
4.	Verify that the LCS was prepared at the same time as the associated samples using the same
procedures.
E.	Action
Refer to Anions Table 4 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient LCSs. For an LCS analysis
that does not meet the technical criteria, apply the actions to all samples in the same preparation
batch.
Matrix spike data can be reviewed to determine batch quality if an LCS was not prepared and
analyzed with the samples.
November 2020
115

-------
Inorganic Data Review
Anions by Ion Chromatography
Anions Table 4. LCS Actions
Criteria
Action
Detect
Non-detect
LCS not prepared with samples
J
UJ
LCS not prepared at specified concentrations
J
UJ
Aqueous/water and soil/sediment %R < 50%
J-
R
Aqueous/water and soil/sediment %R 50-79%
J-
UJ
Aqueous/water and soil/sediment %R 80-120%
No qualification
No qualification
Aqueous/water and soil/sediment %R 121-140%
J+
No qualification
Aqueous/water and soil/sediment %R > 140%
R
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
116

-------
Inorganic Data Review	Anions by Ion Chromatography
V. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment) or for each data package. Duplicates
cannot be averaged for reporting on the Laboratory Results Reports. Additional duplicate sample
analyses may be required. Alternately, the data user may require that a specific sample be used
for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the
Quantitation Limit (QL).
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the QL should be
used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that the duplicate results fall within the established control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation::
S-D
RPD= '	x 100
(S + D) / 2
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of
zero (0) only calculating the RPD. This will always yield an RPD of 200%.
E. Action
Refer to Anions Table 5 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient duplicates.
1. For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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]. Additionally, use the
November 2020
117

-------
Inorganic Data Review
Anions by Ion Chromatography
sample data (e.g., similar concentrations of analytes) in determining similarity between samples
in the data package. Two possible determinations are: 1) only some of the samples in the data
package are similar to the duplicate sample, and that only these samples should be qualified; or 2)
no samples are sufficiently similar to the sample used for the duplicate analysis, and thus only the
field sample used to prepare the duplicate sample should be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
Anions Table 5. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified
frequency
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample
or duplicate sample results < 5x QL (including non-
detects) and absolute difference between sample and
duplicate > QL*
J
UJ
For samples analyzed under the SOW, original sample
or duplicate sample result < 5x QL (including non-
detects) and absolute difference between sample and
duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, The QAPP or the project-specific SOPs for data review may allow the use of less restrictive
criteria (e.g., 35% RPD, 2x QL) to be assessed against duplicate soil samples.
November 2020
118

-------
Inorganic Data Review	Anions by Ion Chromatography
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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample should be prepared and analyzed from each group of samples with a
similar matrix type (e.g., aqueous/water or soil/sediment), or for each data package. Additional
matrix spike samples may be required. Alternately, the data user may require that a specific
sample be used for the matrix spike analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentration required is presented in the method described in the Quality
Assurance Project Plan (QAPP) or in the SOW.
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on field sample.
3.	Verify, using the raw data, that all Matrix Spike sample results fall within the established control
limits.
4.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation::
SSR-SR
%Recovery = ——— x 100
uA
Where,
SSR = Spiking analyte result in the spiked sample
SR = Result of the same analyte in the original sample
SA = Spike added in the spiked sample
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
E.	Action
Refer to Anions Table 6 below for the evaluation criteria and corresponding actions for detected and
non-detected target analyte results in the samples associated with deficient matrix spikes.
November 2020
119

-------
Inorganic Data Review
Anions by Ion Chromatography
1.	For a matrix spike sample analysis that does not meet the technical criteria, apply the actions to
all samples of the same matrix if the samples are considered sufficiently similar. 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]. 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) only some of the samples in the data
package are similar to the Matrix Spike sample, and that only these samples should be qualified;
or 2) no samples are sufficiently similar to the sample used for the matrix spike analysis, and thus
only the field sample used to prepare the Matrix Spike sample should be qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
Anions 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 <35%
J-
R
Matrix Spike %R 35-79%
J-
UJ
Matrix Spike %R 80-120%
No qualification
No qualification
Matrix Spike %R > 120%
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific SOPs for data review may
allow the use of less restrictive criteria (e.g., 10 %R and 150 %R for the lower and upper
limits) to be assessed against spike soil samples.
November 2020
120

-------
Inorganic Data Review
Anions by Ion Chromatography
VII. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final sample volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the Quality Assurance Project Plan
(QAPP) or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1. Aqueous/Water Sample Concentration
C	=	Analyte Result from analysis (mg/L)
Vf	=	Final extraction volume (mL)
W	=	Initial aliquot amount (g)
S	=	%Solids/100
DF	=	Dilution Factor
Anion Concentration (mg/L) = C x DF
Where,
C = Instrument value in mg/L from the calibration curve
DF = Dilution Factor
2. Soil/Sediment Sample Concentration
Vf
Concentration(mg/kg) = C X —		 X DF
W x S
Where,
Concentration = Analyte/Result (mg/kg)
November 2020
121

-------
Inorganic Data Review
Anions by Ion Chromatography
3. Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for aqueous/water
substitute the value of the DL or QL, in the appropriate units, into the "C" term in the equation above.
Calculate the adjusted DL or adjusted QL for soil/sediment samples as follows:
W
Adjusted DL or QL (mg/kg) = C x m x DF
W X S
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Method required minimum sample weight (g)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
122

-------
Inorganic Data Review
Hexavalent Chromium
HEXAVALENT CHROMIUM DATA REVIEW
The inorganic data requirements for hexavalent chromium to be reviewed during validation are listed
below:
I.	Preservation and Holding Times	125
II.	Calibration	127
III.	Blanks	130
IV.	Laboratory Control Sample	133
V.	Duplicate Sample Analysis	135
VI.	Spike Sample Analysis	137
VII.	Target Analyte Quantitation	139
Hexavalent Chromium Table 1.	Preservation and Holding Time Actions	126
Hexavalent Chromium Table 2.	Calibration Actions	129
Hexavalent Chromium Table 3.	Blank Actions	131
Hexavalent Chromium Table 4.	LCS Actions	134
Hexavalent Chromium Table 5.	Duplicate Sample Actions	136
Hexavalent Chromium Table 6.	Spike Sample Actions	138
November 2020
123

-------
Inorganic Data Review	Hexavalent Chromium
This page is intentionally left blank.
November 2020
124

-------
Inorganic Data Review
Hexavalent Chromium
I. 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.	Criteria
1.	The technical holding time is determined from the date of sample collection to the date of
analysis.
2.	The technical holding time criteria for properly preserved (pH > 8, free chlorine <0.1 mg/L)
aqueous/water samples is 14 days or as specified in the Quality Assurance Project Plan (QAPP).
3.	Aqueous/water samples may be maintained at < 6°C (but not frozen) or as specified in the QAPP
from the time of collection until receipt at the laboratory, and should be stored at < 6°C (but not
frozen) or as specified in the QAPP from the time of sample receipt until analysis.
D.	Evaluation
1.	Review the data package narrative, sampling documentation, and sample receipt forms to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, pH, free chlorine). If there is an indication of problems with the samples,
the sample integrity may be compromised. Also verify that the samples were properly stored at
the laboratory. Use professional judgment to evaluate the effect of the problem on the sample
results.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
3.	Establish the technical holding times by comparing the sample collection dates) on the sampling
documentation with the dates of analysis on the Laboratory Results Reports and the raw data.
E.	Action
Refer to Hexavalent Chromium Table 1 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium 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.
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.
November 2020
125

-------
Inorganic Data Review
Hexavalent Chromium
Hexavalent Chromium Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples received with chlorine present
J*
R
Aqueous/water samples received with pH < 8
J*
R
Aqueous/water samples received at a temperature
> 6°C but < 10°C
J
UJ
Aqueous/water samples received at a temperature > 10°C*
J-
R
Technical Holding Time:
Aqueous/water samples >14 days
J-
R
Samples properly preserved and analyzed within specified holding
time
No
qualification
No
qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The true direction of any bias may be unknown in this case. Use caution in determining whether some
detected analytes should be qualified as estimated low (J-) or as estimated high (J+), based on
knowledge of the potential presence of other compounds that may react with the Cr042" ion form.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for
guidance on the use of the J+ and J- qualifiers.
** For samples received with shipping container temperatures > 10°C, 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.
November 2020
126

-------
Inorganic Data Review
Hexavalent Chromium
II. 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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated weekly or as specified in the Quality Assurance
Project Plan (QAPP) or Statement of Work (SOW), and each time the instrument is set up. The
calibration date and time should be included in the raw data.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish the calibration curve. At least one of the calibration standards
should be at or below the Quantitation Limit (QL) in the QAPP or in the SOW but above
the Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy QC requirements. The
calibration curve may be fitted using linear regression or weighted linear regression, or
other fits as specified in the QAPP. Forcing the curve through zero is not recommended.
For linear fits, the calibration curve should have a correlation coefficient greater than the
value specified in the QAPP or in the SOW. The calculated percent differences (%Ds) or
other specified statistical test values for all non-zero standards should fall within the
limits in the QAPP or in the SOW.
2.	Initial and Continuing Calibration Verification
a.	Initial Calibration Verification (ICV)
i.	Immediately after the system has been calibrated, the accuracy of the initial calibration
should be verified and documented by the analysis of an ICV standard. If the ICV Percent
Recovery (%R) falls outside of the control limits, the analysis should be terminated, the
problem corrected and documented in the data package narrative, the instrument
recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution(s) of hexavalent
chromium from an independent standard source, at concentration levels other than that
used for instrument calibration and near the middle of the calibrated range (within
±30%).
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV should be analyzed and
reported.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every
10 samples during an analytical sequence. The CCV standard should also be analyzed at
the beginning of the analytical sequence, and again after the last analytical sample.
iii.	The CCV standard should be prepared using the same source and in the same matrix as
the calibration standards at a concentration at or near the mid-level (within ±30%) of the
respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
November 2020
127

-------
Inorganic Data Review
Hexavalent Chromium
v.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vi.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified by the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW, but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP.
2.	Verify that the ICV and CCV standards were analyzed at the specified frequency and at the
appropriate concentration. Verify that acceptable Percent Recovery (%R) results were obtained.
by recalculating one or more of the %Rs
x 100
Where,
Found (value) = Concentration of hexavalent chromium measured in the analysis of the ICV
or CCV solution
True (value) = Concentration of hexavalent chromium in the ICV or CCV source
E.	Action
Refer to Hexavalent Chromium Table 2 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium results in the samples associated with deficient
initial calibrations or calibration verification standards.
1.	For initial calibrations or ICV standard analyses that do not meet the technical criteria, apply the
actions to the associated samples reported from the analytical sequence.
2.	For CCV standard analyses that do not meet the technical criteria, apply the actions to all samples
analyzed between a previous technically acceptable analysis of the Quality Control (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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
3. Verify that the ICV and CCV %R values are correct
using the raw data and the following equation:
Found (value)
^	1
True (value)
November 2020
128

-------
Inorganic Data Review
Hexavalent Chromium
Hexavalent Chromium Table 2. 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 or R
UJ orR
For linear fits, the correlation coefficient < 0.995
J
UJ
%D outside ±30%, or other specified statistical test
values outside limits
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R < 70%
J- or 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+ or R
No qualification
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
129

-------
Inorganic Data Review
Hexavalent Chromium
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed after the analytical standards, but not
before analysis of the ICV standard during the initial calibration of the instrument. The ICB result
(absolute value) should not be greater than or equal to the Quantitation Limit (QL).
3.	A Continuing Calibration Blank (CCB) should be analyzed immediately after every Continuing
Calibration Verification (CCV) standard. The CCB should be analyzed at the frequency specified
in the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW) during the
analytical sequence. The CCB should be analyzed at the beginning of the analytical sequence, and
again after the last CCV that was analyzed after the last analytical sample of the analytical
sequence. The CCB result (absolute value) should not be greater than or equal to the QL.
4.	At least one Preparation Blank should be prepared and analyzed with every data package, or with
each batch of samples prepared, whichever is more frequent. The Preparation Blank consists of
reagent water processed through the appropriate sample preparation and analysis procedure.
5.	If the hexavalent chromium concentration in the Preparation Blank is greater than or equal to the
QL, the lowest concentration of hexavalent chromium in the associated samples should be > lOx
the Preparation Blank concentration. Otherwise, all associated samples with a hexavalent
chromium concentration < lOx the Preparation Blank concentration and > the QL should be
reprepared and reanalyzed. The laboratory is not to correct the sample concentration for the blank
value.
6.	If the hexavalent chromium concentration in the Preparation Blank is < (-QL), all associated
samples with a hexavalent chromium concentration < lOx the QL should be reprepared and
reanalyzed.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks are prepared and analyzed as
appropriate for the data package (e.g., total number of samples, various types of matrices present,
number of preparation batches, etc.).
2.	For an ICB or a CCB, verify that if the absolute value of the hexavalent chromium concentration
was greater than or equal to the QL, the analysis was terminated, the problem corrected and
documented in the data package narrative, the instrument recalibrated, and the preceding 10
analytical samples or all analytical samples analyzed since the last compliant calibration blank
reanalyzed.
3.	For a Preparation Blank, verify that if the concentration of hexavalent chromium was greater than
or equal to the QL, all associated samples with a hexavalent chromium concentration > the QL
but < lOx the Preparation Blank concentration were reprepared and reanalyzed. Verify that if the
hexavalent chromium concentration was < (-QL) in a Preparation Blank, all associated samples
with hexavalent chromium concentration < 1 Ox the QL were reprepared and reanalyzed.
November 2020
130

-------
Inorganic Data Review
Hexavalent Chromium
4. Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to Hexavalent Chromium Table 3 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium results in the samples associated with deficient
blanks.
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.
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 3 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 3 below.
7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be checked
against a less dilute run, 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 negatives exists.
NOTE: The blank analyses may not involve the same volumes or dilution factors as the
associated samples. It may be easier to work with the raw data for comparison purposes.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
Hexavalent Chromium Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J
ICB/CCB
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
ICB/CCB
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
November 2020
131

-------
Inorganic Data Review
Hexavalent Chromium
Blank Type
Blank Result
Sample Result
Action
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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/Field
Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/Field
Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/Field
Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < lOx the Preparation
Blank Result
Report at Preparation Blank
Result and qualify J+ or R
> 1 Ox the Preparation Blank
Result
No qualification
Preparation
Blank/Field
Blank
<(-QL)
Non-detect
UJ
Detect < QL
J-
> QL but < lOx QL
J-
> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
132

-------
Inorganic Data Review	Hexavalent Chromium
IV. Laboratory Control Sample
A.	Review Items
Laboratory LCS reports (if available), preparation 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 the recovery of the
prepared Laboratory Control Sample (LCS).
C.	Criteria
1.	Aqueous/water LCSs should be analyzed for hexavalent chromium utilizing the same sample
preparations, analytical methods, and Quality Assurance/Quality Control (QA/QC) procedures as
employed for the samples.
2.	One LCS should be prepared and analyzed for every group of aqueous/water samples in a data
package or with each batch of samples prepared, whichever is more frequent. The LCS should be
spiked such that it contains hexavalent chromium at the levels specified in the Quality Assurance
Project Plan (QAPP) or at 2x the Quantitation Limit (QL).
3.	All LCS Percent Recoveries (%Rs) should fall within the control limits of in the QAPP or in the
Statement of Work (SOW). If the %R for the aqueous/water LCS falls outside of the control
limits, the analysis should be terminated, the problem corrected and documented in the data
package narrative, and the samples prepared with that LCS reprepared and reanalyzed.
D.	Evaluation
1.	Verify, using the laboratory reports, preparation logs, and raw data, that the appropriate number
of required LCSs were prepared and analyzed for the data package.
2.	Verify that all results for each analyte fall within the established control limits.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of each analyte measured in the analysis of the LCS
True (value) = Concentration of each analyte in the LCS
4.	Verify that the LCS was prepared at the same time as the associated samples using the same
procedures.
E.	Action
Refer to Hexavalent Chromium Table 4 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium results in the samples associated with deficient
LCSs. For an LCS analysis that does not meet the technical criteria, apply the actions to all samples in
the same preparation batch.
Matrix spike data can be reviewed to determine batch quality if an LCS was not prepared and
analyzed with the samples.
November 2020
133

-------
Inorganic Data Review
Hexavalent Chromium
Hexavalent Chromium Table 4. LCS Actions
Criteria
Action
Detect
Non-detect
LCS not prepared with samples
J
UJ
LCS not prepared at specified concentration
J
UJ
Aqueous/water %R < 40%
J-
R
Aqueous/water %R 40-69%
J-
UJ
Aqueous/water %R 70-130%
No qualification
No qualification
Aqueous/water %R 131-150%
J+
No qualification
Aqueous/water %R > 150%
R
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
134

-------
Inorganic Data Review	Hexavalent Chromium
V. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed for each data package. Duplicates
cannot be averaged for reporting on the Laboratory Results Report. Additional duplicate sample
analyses may be required. Alternately, the data user may require that a specific sample be used
for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the
Quantitation Limit (QL).
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the QL should be
used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that the duplicate results fall within the established control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation::
|S - D|
RPD = —!	x 100
(S + D) / 2
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of zero
(0) only for calculating the RPD. This will always yield an RPD of 200%.
E.	Action
Refer to Hexavalent Chromium Table 5 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium results in the samples associated with deficient
duplicates.
1. For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples if the samples are considered sufficiently similar. Exercise professional judgment in
determining sample similarity. Use the sample data (e.g., similar concentrations of analytes) in
determining similarity between samples in the data package. Two possible determinations are: 1)
only some of the samples in the data package are similar to the duplicate sample, and that only
these samples should be qualified; or 2) no samples are sufficiently similar to the sample used for
November 2020
135

-------
Inorganic Data Review
Hexavalent Chromium
the duplicate analysis, and thus only the field sample used to prepare the duplicate sample should
be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
Hexavalent Chromium Table 5. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample results < 5x QL (including non-detects) and
absolute difference between sample and duplicate > QL
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
November 2020
136

-------
Inorganic Data Review	Hexavalent Chromium
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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample should be prepared and analyzed for each data package. Additional
matrix spike sample analyses may be required. Alternately, the data user may require that a
specific sample be used for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentration required is presented in the method described in the Quality
Assurance Project Plan (QAPP) or in the Statement of Work (SOW).
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, and raw data, that the appropriate
number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all Matrix Spike sample results fall within the established control
limits.
4.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw
data and the following equation::
SSR-SR
%Recovery = ——— x 100
uA
Where,
SSR = Spiking analyte result in the spiked sample
SR = Result of the same analyte in the original sample
SA = Spike added in the spiked sample
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
E.	Action
Refer to Hexavalent Chromium Table 6 below for the evaluation criteria and corresponding actions
for detected and non-detected hexavalent chromium results in the samples associated with deficient
matrix spikes.
November 2020
137

-------
Inorganic Data Review
Hexavalent Chromium
1.	For a matrix spike sample analysis that does not meet the technical criteria, apply the actions to
all samples if the samples are considered sufficiently similar. Exercise professional judgment in
determining sample similarity. Use the sample data (e.g., similar concentrations of analytes) in
determining similarity between samples in the data package. Two possible determinations are: 1)
only some of the samples in the data package are similar to the Matrix Spike sample, and that
only these samples should be qualified; or 2) no samples are sufficiently similar to the sample
used for the matrix spike analysis, and thus only the field sample used to prepare the Matrix Spike
sample should be qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
Hexavalent Chromium 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%
J-
R
Matrix Spike %R 30-74%
J-
UJ
Matrix Spike %R 75-125%
No qualification
No qualification
Matrix Spike %R >125%
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
138

-------
Inorganic Data Review
Hexavalent Chromium
VII. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final sample volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP, qualify as
estimated (J).
F.	Example Equations
1.	Aqueous/Water Sample Concentration
Cr(VI) Concentration (jxg/L) = C x DF
Where,
C = Instrument value in |a,g/L from the calibration curve
DF = Dilution Factor
2.	Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water samples, substitute the value of the DL or QL, in the appropriate units, into the
"C" term in the equation.
Cr(VI) DL or QL (^ig/L) = C x DF
Where,
C = DL or QL for Instrument in |ag/L
DF = Dilution Factor
November 2020
139

-------
Inorganic Data Review	Hexavalent Chromium
This page is intentionally left blank.
November 2020
140

-------
Inorganic Data Review
Total Organic Carbon (TOC)
TOTAL ORGANIC CARBON (TOC) DATA REVIEW
The inorganic data requirements for TOC to be reviewed during validation are listed below:
I.	Preservation and Holding Times	143
II.	Calibration	145
III.	Blanks	148
IV.	Laboratory Control Sample	151
V.	Duplicate Sample Analysis	153
VI.	Spike Sample Analysis	155
VII.	Target Analyte Quantitation	157
TOC Table 1. Preservation and Holding Time Actions	144
TOC Table 2. Calibration Actions	147
TOC Table 3. Blank Actions	149
TOC Table 4. LCS Actions	152
TOC Table 5. Duplicate Sample Actions	154
TOC Table 6. Spike Sample Actions	156
November 2020
141

-------
Inorganic Data Review	Total Organic Carbon (TOC)
This page is intentionally left blank.
November 2020
142

-------
Inorganic Data Review
Total Organic Carbon (TOC)
I. 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 or
storage conditions and the holding time of the sample.
C.	Criteria
1.	The technical holding time is determined from the date of sample collection to the date of
analysis.
2.	The technical holding time criteria for aqueous/water samples 28 days or as specified in the
Quality Assurance Project Plan (QAPP), preserved (with sulfuric or phosphoric acid) to pH < 2.
3.	The technical holding time criteria for soil/sediment samples is 28 days, or as specified in the
QAPP.
4.	Aqueous/water samples and soil/sediment samples should be maintained at < 6°C (but not frozen)
or as specified in the QAPP from the time of collection until receipt at the laboratory and should
be stored at < 6°C (but not frozen) or as specified in the QAPP from the time of sample receipt
until analysis.
D.	Evaluation
1.	Review the data package narrative, sampling Record documentation, and sample receipt forms to
determine if the samples were properly preserved and arrived at the laboratory in proper condition
(e.g., received intact, appropriate sample temperature at receipt, pH). If there is an indication of
problems with the samples, the sample integrity may be compromised. Also verify that the
samples were properly stored at the laboratory. Use professional judgment to evaluate the effect
of the problem on the sample results.
2.	Verify that the analysis dates on the Laboratory Results Reports and the raw data are identical.
3.	Establish the technical holding times by comparing the sample collection dates on the sampling
documentation with the dates of analysis on the Laboratory Results Reports and the raw data.
E.	Action
Refer to TOC Table 1 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC 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.
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.
November 2020
143

-------
Inorganic Data Review
Total Organic Carbon (TOC)
TOC Table 1. Preservation and Holding Time Actions
Criteria
Action
Detect
Non-detect
Aqueous/water samples received with pH > 2
J-
R
Aqueous/water and soil/sediment samples received at a
temperature > 6°C but < 10°C
J
UJ
Aqueous/water and soil/sediment samples received at a
temperature > 10°C*
J-
R
Technical Holding Time:
Aqueous/water samples >28 days
J-
R
Technical Holding Time:
Soil/sediment samples > 28 days
J-
R
Samples properly preserved and analyzed within specified holding
time
No
qualification
No
qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
* For samples received with shipping container temperatures > 10°C, 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.
November 2020
144

-------
Inorganic Data Review
Total Organic Carbon (TOC)
II. 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.	Criteria
1.	Initial Calibration
The instruments should be successfully calibrated daily, or as specified in the Quality Assurance
Project Plan (QAPP) or the Statement of Work (SOW), and each time the instrument is set up.
The calibration date and time should be included in the raw data.
NOTE: A blank and the number of calibration standards specified in the QAPP or in the SOW
should be used to establish the calibration curve. At least one of the calibration standards
should be at or below the Quantitation Limit (QL) in the QAPP or in the SOW but above
the Detection Limit or the Method Detection Limit (MDL). Calibration standards at and
above the QL should be continuous with none excluded to satisfy Quality Control (QC)
requirements. The calibration curve may be fitted using linear regression or weighted
linear regression, or other fits as specified in the QAPP. The curve may be forced through
zero. For linear fits, the calibration curve should have a correlation coefficient greater
than the value specified in the QAPP or in the SOW. The calculated percent differences
(%Ds) or other specified statistical test values for all non-zero standards should fall
within the limits in the QAPP or in the SOW.
2.	Initial and Continuing Calibration Verification
a.	Initial Calibration Verification (ICV)
i.	Immediately after the system has been calibrated, the accuracy of the initial calibration
should be verified and documented by the analysis of an ICV standard. If the ICV Percent
Recovery (%R) falls outside of the control limits, the analysis should be terminated, the
problem corrected and documented in the data package narrative, the instrument
recalibrated, and all affected samples reanalyzed.
ii.	Analyses of the ICV should be conducted using a certified solution of TOC from an
independent standard source, at concentration levels other than that used for instrument
calibration and near the middle of the calibrated range (within ±30%).
b.	Continuing Calibration Verification (CCV)
i.	To ensure accuracy during each analytical sequence, the CCV standard should be analyzed
and reported.
ii.	The CCV standard should be analyzed at the frequency specified in the QAPP, or every 10
samples during an analytical sequence. The CCV standard should also be analyzed at the
beginning of the analytical sequence, and again after the last analytical sample.
iii.	The CCV standard should be prepared using the same source and in the same acid matrix
as the calibration standards at a concentration at or near the mid-level (within ±30%) of
the respective calibration curve.
iv.	The same CCV standard solution should be used throughout the analysis for a data
package.
November 2020
145

-------
Inorganic Data Review	Total Organic Carbon (TOC)
v.	The CCV should be analyzed in the same fashion as an actual sample. If the %R of the
CCV was outside of the control limits, the analysis should be terminated, the problem
corrected and documented in the data package narrative, the instrument recalibrated, and
all analytical samples analyzed since the last compliant CCV reanalyzed.
vi.	An instrument blank should not be analyzed before the CCV.
D.	Evaluation
1.	Verify that the instrument was calibrated as specified in the QAPP or in the SOW and each time
the instrument was set up, utilizing a blank and at least the minimum number of standards
specified by the QAPP or in the SOW. Confirm that at least one of the calibration standards was
analyzed at or below the QL in the QAPP or in the SOW, but above the Detection Limit or MDL
and that all subsequent calibration standards are consecutive with none removed to satisfy QC
requirements. For linear fits, verify that the correlation coefficient of the calibration curve is
greater than the value specified in the QAPP or in the SOW. Verify that the %Ds for all non-zero
standards are within the SOW limits or that other statistical test values are within the limits
specified in the QAPP.
2.	Verify that the ICV and CCV standards were analyzed at the specified frequency and at the
appropriate concentration. Verify that acceptable %R results were obtained.
3.	Confirm that an instrument blank was not analyzed before the CCV.
4.	Verify that the ICV and CCV %R values are correct by recalculating one or more of the %Rs
using the raw data and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of TOC measured in the analysis of the ICV or CCV solution
True (value) = Concentration of TOC in the ICV or CCV source
E.	Action
Refer to TOC Table 2 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC results in the samples associated with deficient initial calibrations or calibration
verification standards.
1.	For initial calibrations or ICV standard analyses that do not meet the technical criteria, apply the
actions to the associated samples reported from the analytical sequence.
2.	For CCV standard analyses that do not meet the technical criteria, apply the actions to all samples
analyzed between a previous technically acceptable analysis of the Quality Control (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.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
November 2020
146

-------
Inorganic Data Review
Total Organic Carbon (TOC)
TOC Table 2. 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 or R
UJ orR
For linear fits, the correlation coefficient < 0.995
J
UJ
%D outside ±30%, or other specified statistical test
values outside limits
J
UJ
ICV/CCV not performed at specified frequency
J
UJ
ICV/CCV %R <65%
J- or R
R
ICV/CCV %R 65-79%
J-
UJ
ICV/CCV %R 80-120%
No qualification
No qualification
ICV/CCV %R 120-135%
J+
No qualification
ICV/CCV %R> 135%
J+ or R
No qualification
Instrument blank analyzed prior to CCV
Use professional
judgment
Use professional
judgment
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
147

-------
Inorganic Data Review
Total Organic Carbon (TOC)
III. Blanks
A.	Review Items
Laboratory blanks reports (if available), preparation logs, calibration standard logs, instrument logs,
and raw data in the data package.
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.	Criteria
1.	No contaminants should be found in the blank(s).
2.	The Initial Calibration Blank (ICB) should be analyzed after the analytical standards, but not
before analysis of the ICV standard during the initial calibration of the instrument. The ICB result
(absolute value) should not be greater than or equal to the Quantitation Limit (QL).
3.	A Continuing Calibration Blank (CCB) should be analyzed immediately after every Continuing
Calibration Verification (CCV) standard. The CCB should be analyzed at the frequency specified
in the Quality Assurance Project Plan (QAPP) or in the Statement of Work (SOW) during the
analytical sequence. The CCB should be analyzed at the beginning of the analytical sequence, and
again after the last CCV that was analyzed after the last analytical sample of the analytical
sequence. The CCB result (absolute value) should not be greater than or equal to the QL.
4.	At least one Preparation Blank should be prepared and analyzed for each matrix, with every data
package, or with each batch of samples prepared, whichever is more frequent. The Preparation
Blank consists of reagent water processed through the appropriate sample preparation and
analysis procedure.
5.	If the TOC concentration in the Preparation Blank is greater than or equal to the QL, the lowest
concentration of TOC in the associated samples should be > 1 Ox the Preparation Blank
concentration. Otherwise, all associated samples with a TOC concentration < 1 Ox the Preparation
Blank concentration and > the QL should be reprepared and reanalyzed. The laboratory is not to
correct the sample concentration for the blank value.
6.	If the TOC concentration in the Preparation Blank is less than or equal to the limit in the QAPP
multiplied by -1 or < (-QL), all associated samples with a TOC concentration < lOx the limit
specified in the QAPP or the QL should be reprepared and reanalyzed.
D.	Evaluation
1.	Verify that an ICB was analyzed after the calibration; the CCB was analyzed at the specified
frequency and sequence during the analysis; and Preparation Blanks are prepared and analyzed as
appropriate for the data package (e.g., total number of samples, various types of matrices present,
number of preparation batches, etc.).
2.	For an ICB or a CCB, verify that if the absolute value of the TOC concentration was greater than
or equal to the QL the analysis was terminated, the problem corrected and documented in the data
package narrative, the instrument recalibrated, and the preceding 10 analytical samples or all
analytical samples analyzed since the last compliant calibration blank reanalyzed.
3.	For a Preparation Blank, verify that if the concentration of TOC was greater than or equal to the
QL in a Preparation Blank, all associated samples with a TOC concentration > the QL but < 1 Ox
the Preparation Blank concentration were reprepared and reanalyzed. Verify that if the TOC
concentration was < (-QL) in a Preparation Blank, all associated samples with a TOC
concentration < 1 Ox the QL were reprepared and reanalyzed.
November 2020
148

-------
Inorganic Data Review
Total Organic Carbon (TOC)
4. Evaluation of field and equipment blanks should also be performed according to the QAPP or
appropriate guidance.
E. Action
Refer to TOC Table 3 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC results in the samples associated with deficient blanks.
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.
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 3 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 3 below.
7.	If an analyte result in a diluted sample analysis is < QL, the final analyte result should be checked
against a less dilute run, 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 negatives exists.
NOTE: 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 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 samples for comparison purposes.
When two separate qualifiers are listed as actions, use professional judgment to qualify detects and
non-detects based on the extent to which the criteria is not met.
TOC Table 3. Blank Actions
Blank Type
Blank Result
Sample Result
Action
ICB/CCB
Not analyzed at
the specified
frequency
Non-detect
UJ
Detect
J


Non-detect
No qualification
ICB/CCB
Detect < QL
Detect < QL
Report at QL and qualify U


> QL
J+ or no qualification
ICB/CCB

Non-detect
UJ
November 2020
149

-------
Inorganic Data Review
Total Organic Carbon (TOC)
Blank Type
Blank Result
Sample Result
Action

< (-MDL) but
>(-QL)
Detect
J- or 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
J+ or no qualification
ICB/CCB
<(-QL)
Non-detect
UJ orR
Detect < QL
J-
> QL
J-
Preparation
Blank
Not analyzed at
specified
frequency
Non-detect
UJ
Detect
J
Preparation
Blank/Field
Blank
Detect < QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL
J+ or no qualification
Preparation
Blank/Field
Blank
< (-MDL) but
>(-QL)
Non-detect
UJ
Detect
J- or no qualification
Preparation
Blank/Field
Blank
> QL
Non-detect
No qualification
Detect < QL
Report at QL and qualify U
> QL but < lOx the Preparation
Blank Result
Report at Preparation Blank
Result and qualify J+ or R
> 1 Ox the Preparation Blank
Result
No qualification
Preparation
Blank/Field
Blank
<(-QL)
Non-detect
UJ
Detect < QL
J-
> QL but < lOx QL
J-
> lOx QL
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
150

-------
Inorganic Data Review	Total Organic Carbon (TOC)
IV. Laboratory Control Sample
A.	Review Items
Laboratory LCS reports (if available), preparation 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 the recovery of the
prepared Laboratory Control Sample (LCS).
C.	Criteria
1.	Aqueous/water and soil/sediment LCSs should be analyzed for TOC utilizing the same sample
preparations, analytical methods, and Quality Assurance/Quality Control (QA/QC) procedures as
employed for the samples.
2.	One LCS should be prepared and analyzed for every group of aqueous/water or soil/sediment
samples in a data package or with each batch of samples prepared, whichever is more frequent.
The LCS should be spiked such that it contains TOC at the levels specified in the Quality
Assurance Project Plan (QAPP) or at 2xthe Quantitation Limit (QL) for the associated matrix.
3.	All LCS Percent Recoveries (%Rs) should fall within the control limits of in the QAPP or in the
SOW. If the %R for the aqueous/water and soil/sediment LCS falls outside of the control limits,
the analysis should be terminated, the problem corrected and documented in the data package
narrative, and the samples prepared with that LCS reprepared and reanalyzed.
D.	Evaluation
1.	Verify, using the laboratory reports, preparation logs, and raw data, that the appropriate number
of required LCSs were prepared and analyzed for the data package.
2.	Verify that all %R values fall within the established control limits.
3.	Verify that the %R values are correct by recalculating one or more of the %Rs using the raw data
and the following equation:
Found (value)
%R= True (value) * '°0
Where,
Found (value) = Concentration of each analyte measured in the analysis of the LCS
True (value) = Concentration of each analyte in the LCS
4.	Verify that the LCS was prepared at the same time as the associated samples using the same
procedures.
E.	Action
Refer to TOC Table 4 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC results in the samples associated with deficient LCSs. For an LCS analysis that
does not meet the technical criteria, apply the actions to all samples in the same preparation batch.
Matrix spike data can be reviewed to determine batch quality if an LCS was not prepared and
analyzed with the samples.
November 2020
151

-------
Inorganic Data Review
Total Organic Carbon (TOC)
TOC Table 4. LCS Actions
Criteria
Action
Detect
Non-detect
LCS not prepared with samples
J
UJ
LCS not prepared at specified concentration
J
UJ
Aqueous/water and soil/sediment %R <45%
J-
R
Aqueous/water and soil/sediment %R 45-74%
J-
UJ
Aqueous/water and soil/sediment %R 75-125%
No qualification
No qualification
Aqueous/water and soil/sediment %R 126-145%
J+
No qualification
Aqueous/Water and soil/sediment %R> 145%
R
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
November 2020
152

-------
Inorganic Data Review
Total Organic Carbon (TOC)
V. 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 duplicate sample analysis is to demonstrate acceptable method precision by the
laboratory at the time of analysis.
C.	Criteria
1.	Field samples should be used as source samples for duplicate analysis.
2.	At least one duplicate sample should be prepared and analyzed from each group of samples of a
similar matrix type (e.g., aqueous/water or soil/sediment) or for each data package. Duplicates
cannot be averaged for reporting on the Laboratory Results Reports. Additional duplicate sample
analyses may be required. Alternately, the data user may require that a specific sample be used
for the duplicate sample analysis.
3.	The Relative Percent Difference (RPD) control limit specified in the Quality Assurance Project
Plan (QAPP) or of 20% should be used for original and duplicate sample values > 5x the
Quantitation Limit (QL).
4.	For samples analyzed under the Statement of Work (SOW), a control limit of the QL should be
used if either the sample or duplicate value is < 5x the QL.
D.	Evaluation
1.	Verify, from the data package Cover Page, laboratory reports, preparation log and the raw data,
that the appropriate number of required duplicate samples were prepared and analyzed.
2.	Verify, using the raw data, that the duplicate results fall within the established control limits.
3.	Verify that the duplicate analysis was performed on a field sample.
4.	Verify that the RPD values are correct by recalculating one or more of the RPDs using the raw
data and the following equation:
Where,
S = Sample Result (original)
D = Duplicate Result
NOTE: When the Sample or Duplicate Result is reported as a non-detect, use a value of
zero (0) only for calculating the RPD. This will always yield an RPD of 200%.
November 2020
153

-------
Inorganic Data Review
Total Organic Carbon (TOC)
E. Action
Refer to TOC Table 5 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC results in the samples associated with deficient duplicates.
1.	For a duplicate sample analysis that does not meet the technical criteria, apply the actions to all
samples of the same matrix if the samples are considered sufficiently similar. 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), alkalinity or
buffering capacity, reactive sulfide, anions]. Additionally, use the sample data (e.g., similar
concentrations of TOC) in determining similarity between samples in the data package. Two
possible determinations are: 1) only some of the samples in the data package are similar to the
duplicate sample, and that only these samples should be qualified; or 2) no samples are
sufficiently similar to the sample used for the duplicate analysis, and thus only the field sample
used to prepare the duplicate sample should be qualified.
2.	Note the potential effects on the data due to out-of-control duplicate sample results in the Data
Review Narrative.
3.	For high RPDs (i.e., > 100%), use professional judgment to qualify the data as this may be
indicative of a sampling problem.
TOC Table 5. Duplicate Sample Actions
Criteria
Action
Detect
Non-detect
Duplicate analysis not performed at the specified frequency
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD > 20%*
J
UJ
Both original sample and duplicate sample results are
> 5x QL and RPD < 20%
No qualification
No qualification
RPD > 100%
Use professional
judgment
Use professional
judgment
For samples analyzed under the SOW, original sample or
duplicate sample results < 5x QL (including non-detects) and
absolute difference between sample and duplicate > QL*
J
UJ
For samples analyzed under the SOW, original sample or
duplicate sample result < 5x QL (including non-detects) and
absolute difference between sample and duplicate < QL
No qualification
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
* The above control limits are method requirements for duplicate samples, regardless of the sample
matrix type. However, it should be noted that laboratory variability arising from the sub-sampling of
non-homogenous soil samples is a common occurrence. Therefore, for technical review purposes
only, The QAPP or the project-specific Standard Operating Procedures (SOPs) for data review may
allow the use of less restrictive criteria (e.g., 35% RPD, 2x QL) to be assessed against duplicate soil
samples.
November 2020
154

-------
Inorganic Data Review	Total Organic Carbon (TOC)
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.	Criteria
1.	Field samples should be used as source samples for matrix spike analysis.
2.	At least one spiked sample should be prepared and analyzed from each group of samples with a
similar matrix type (e.g., aqueous/water or soil/sediment), or for each data package. Additional
matrix spike sample analyses may be required. Alternately, the data user may require that a
specific sample be used for the matrix spike sample analysis.
3.	The spike Percent Recovery (%R) should be within the established acceptance limits. However,
for samples analyzed under the Statement of Work (SOW), spike recovery limits do not apply
when the sample concentration is > 4x the spike added. In such an event, the data should be
reported unqualified, even if the %R does not meet the acceptance criteria.
4.	If the spiked sample analysis was performed on the same sample that was selected for the
duplicate sample analysis, spike calculations should be performed using the results of the sample
designated as the "original sample". The average of the duplicate results cannot be used for
determining the %R.
NOTE: The final spike concentration required is presented in the method described in the Quality
Assurance Project Plan (QAPP) or in the SOW.
D.	Evaluation
1.	Verify, using the data package Cover Page, laboratory reports, preparation log and raw data, that
the appropriate number of required spiked samples was prepared and analyzed.
2.	Verify that the matrix spike analysis was performed on a field sample.
3.	Verify, using the raw data, that all Matrix Spike sample results fall within the established control
limits.
4.	Verify that the %R values for the matrix spike are correct by recalculating one or more of the
%Rs using the raw data and the following equation:
SSR-SR
%Recovery = ——— x 100
uA
Where,
SSR = Spiking analyte result in spiked sample
SR = Result of the same analyte in the original sample
SA = Spike added in the spike sample
NOTE: When the Sample Result is reported as a non-detect, use SR = 0 only for calculating the
%R.
E.	Action
Refer to TOC Table 6 below for the evaluation criteria and corresponding actions for detected and
non-detected TOC results in the samples associated with deficient matrix spikes.
November 2020
155

-------
Inorganic Data Review
Total Organic Carbon (TOC)
1.	For a matrix spike sample analysis that does not meet the technical criteria, apply the actions to
all samples of the same matrix if the samples are considered sufficiently similar. 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), alkalinity
or buffering capacity, reactive sulfide, anions]. Additionally, use the sample data (e.g., similar
concentrations of TOC) in determining similarity between samples in the data package. Two
possible determinations are: 1) only some of the samples in the data package are similar to the
Matrix Spike sample, and that only these samples should be qualified; or 2) no samples are
sufficiently similar to the sample used for the matrix spike analysis, and thus only the field
sample used to prepare the Matrix Spike sample should be qualified.
2.	Note the potential effects on the data due to out-of-control spiked sample results in the Data
Review Narrative.
TOC 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 <25%
J-
R
Matrix Spike %R 25-69%
J-
UJ
Matrix Spike %R 70-130%
No qualification
No qualification
Matrix Spike %R > 130%
J+
No qualification
Criteria listed in the Table are the EPA CLP SOW and NFG criteria; however, alternate criteria may be
specified in the QAPP or project-specific SOPs.
Refer to the Note under Part A, Section II, General Table 1. Data Qualifiers and Definitions for guidance
on the use of the J+ and J- qualifiers.
NOTE: The above control limits are method requirements for spike samples, regardless of the
sample matrix type. However, it should be noted that laboratory variability arising from the
sub-sampling of non-homogenous soil samples is a common occurrence. Therefore, for
technical review purposes only, the QAPP or the project-specific Standard Operating
Procedures (SOPs) for data review may allow the use of less restrictive criteria (e.g., 10 %R
and 150 %R for the lower and upper limits) to be assessed against spike soil samples.
November 2020
156

-------
Inorganic Data Review	Total Organic Carbon (TOC)
VII. Target Analvte Quantitation
A.	Review Items
Laboratory Result Reports, sample preparation sheets, 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.
C.	Criteria
Final target analyte results and quantitation limits should be calculated according to the correct
equations, taking into account amount of sample prepared, final sample volume, dilution factor, and
percent solids, as appropriate.
D.	Evaluation
1.	Verify that the results for all positively identified target analytes are calculated and reported by
the laboratory according to the equations specified in the Quality Assurance Project Plan (QAPP)
or in the Statement of Work (SOW).
2.	Verify that the reported Quantitation Limits (QLs) for non-detected target analytes are calculated
and reported by the laboratory according to the equations in the QAPP or in the SOW.
3.	Verify that all reported results and QLs have been adjusted to reflect percent solids, original
sample mass/volume, and any applicable dilutions.
E.	Action
1.	If sample results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
2.	If the sample percent solids is < 30%, check if the sample was prepared at greater mass to
maintain the QLs. Use professional judgment when this was not completed.
F.	Example Equations
1.	Aqueous/Water Sample Concentration
TOC Concentration (mg/L) = C x DF
Where,
C = Instrument value in mg/L from the calibration curve
DF = Dilution Factor
2.	Soil/Sediment Sample Concentration
Vf
Concentration(mg/kg )= C X —		 X DF
W x S
Where,
Concentration = Analyte/Result (mg/kg)
C = Analyte Result from analysis (mg/L)
Vf = Final digestion volume mL
W = Initial aliquot amount g
S = %Solids/100
DF = Dilution Factor
November 2020
157

-------
Inorganic Data Review
Total Organic Carbon (TOC)
3. Adjusted DL (or MDL)/Adjusted QL
To calculate the adjusted Detection Limit (DL) or adjusted Quantitation Limit (QL) for
aqueous/water substitute the value of the DL or QL, in the appropriate units, into the "C" term in
the equation above.
Calculate the adjusted DL or adjusted QL for soil/sediment samples as follows:
W
Adjusted DL or QL (mg/kg) = C x m x DF
W X S
Where,
C = Detection Limit (DL) or Quantitation Limit (QL) (mg/kg)
Wm = Method required minimum sample weight (g)
W = Initial aliquot amount (g)
S = %Solids/100
DF = Dilution Factor
November 2020
158

-------
Inorganic Data Review
Appendix A
APPENDIX A: GLOSSARY
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 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.
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.
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 designed to detect any carryover
contamination.
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.
November 2020
A-l

-------
Inorganic Data Review
Appendix A
Control Limits - A range within which specified measurement results should fall to be
compliant. Control limits may be mandatory, requiring corrective action if exceeded, or advisory,
requiring that noncompliant data be flagged.
Data Package Narrative - Portion of the data package which includes laboratory information, sample
identification, and descriptive documentation of any problems encountered in processing the samples,
along with corrective action taken and problem resolution.
Data Quality Assessment (DQA) - The scientific and statistical evaluation of environmental data to
determine if they meet the planning objectives of the project, and thus are of the right type, quality, and
quantity to support their intended use; refer to EPA QA/G-9R.
Data Quality Objectives (DQO) - Qualitative and quantitative statements that clarify technical
and quality objectives, define the appropriate type of data, and specify tolerable levels of potential
decision errors that will be used as the basis for establishing the quality and quantity of data needed to
support decisions.
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 - A duplicate sample generated in the field, not in the laboratory.
Field Quality Control (QC) - Any QC samples submitted from the field to the laboratory. Examples
include, but are not limited to, field blanks, and field duplicates.
Field Sample - A portion of material received from the field to be analyzed for analytes of interest.
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.
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 - The place where the samples are processed and tested.
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.
November 2020
A-2

-------
Inorganic Data Review
Appendix A
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 of
this 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.
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 - An analytical control that contains reagent water and reagents, which is carried
through the entire preparation and analytical procedure. For ICP-AES analysis of wipes, when possible a
preparation blank includes a clean wipe.
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 - 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.
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 portion of material to be analyzed that is contained in single or multiple containers and
identified by a unique sample number.
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.
November 2020
A-3

-------
Inorganic Data Review
Appendix A
Sample Identifier - A unique identification number that appears on the Chain of Custody (COC)
Records or sampling forms which documents information for a sample.
Serial Dilution - 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.
Technical Holding Time - The maximum amount of time that samples may be held from the collection
date until analysis.
Tune - A solution containing a range of isotope masses analyzed to serve as an initial demonstration of
Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) accuracy, resolution, and precision prior to
calibration. May also be called Instrument Performance Check sample (IPC).
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.
November 2020
A-4

-------
Inorganic Data Review
Appendix B
APPENDIX B: INORGANIC DATA REVIEW SUMMARY
Event ID/Case No. (if applicable).
Laboratory	
Modified Analysis No. (if applicable).
Reference Method (if applicable)	
Reviewer Name	
Action	
Validation Label
Site
No. of Samples/Matrix.
Data Package ID (if applicable).
Project/EPA Region (if applicable)
Completion Date	
FY I
REVIEW CRITERIA
METHOD/ANAL YTE
1.	Preservation and Holding
Time
2.	Tune Analysis
3.	Calibration
4.	Blanks
5.	Interference Check Sample
6.	Laboratory Control Sample
7.	Duplicate Sample Analysis
8.	Spike Sample Analysis
9.	Serial Dilution
10.	Internal Standards
11.	Performance Evaluation
Sample
12.	Quality Assurance and
Quality Control
13.	Overall Assessment of Data
November 2020
B-l

-------
Inorganic Data Review
Appendix B
This page is intentionally left blank.
November 2020	B-2

-------