4>EPA
United States
Environmental Protection
Agency
Office of Research and
Development
Washington, DC 20460
EPA/600/8-91/004
February 1991
Preparation Aids for the
Development of
Category II Quality
Assurance Project Plans
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EPA/600/8-91/004
February 1991
PREPARATION AIDS
FOR THE DEVELOPMENT OF
CATEGORY II
QUALITY ASSURANCE PROJECT PLANS
by
Guy F. Simes
Risk Reduction Engineering Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, OH 45268
Printed on Recycled Paper
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This material has been funded by the United States Environmental
Protection Agency. Although it has been subject to the Agency's review,
and has been approved for publication as an EPA document, it does not
necessarily reflect EPA policy.
11
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- Foreword
Today's rapidly developing and changing technologies and industrial
products and practices frequently carry with them the increased generation
of materials that, if improperly dealt with, can threaten both public health
and the environment. The U.S. Environmental Protection Agency is
charged by Congress with protecting the Nation's land, air, and water
systems. Under a mandate of national environmental laws, the Agency
strives to formulate and implement actions leading to a compatible balance
between human activities and the ability of natural systems to support and
nurture life. These laws direct the EPA to perform research to define our
environmental problems, measure the impacts, and search for solutions.
The Risk Reduction Engineering Laboratory is responsible for planning,
implementing, and managing the research, development, and
demonstration programs to provide an authoritative, defensible
engineering basis in support of the policies, programs, and regulations of
the EPA with respect to drinking water, wastewater, pesticides, toxic
substances, solid and hazardous wastes, and Superfund-related activities.
This publication is one of the products of a quality assurance outreach
program that provides a vital communication link between the researcher
and the user community.
Perhaps the greatest benefit to the users of this document comes from its
emphasis on up-front planning -- do the right thing, right, the first time.
While this sounds straightforward, managers know that determining the
right course in a complex and uncertain situation is anything but simple.
Determining customer requirements up-front, and then having the
processes and procedures in place to accomplish them, averts costly
mistakes. Resources are conserved in two ways: by avoiding rework to
correct efforts that do not initially meet management or customer
specifications; and by performing to the specifications required and not
beyond them. In these ways, this "Preparation Aids" document can help
management achieve its mission with more effective utilization of
diminishing resources.
E. Timothy Oppelt, Director
Risk Reduction Engineering Laboratory
111
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Abstract
Data collection activities performed for the Risk Reduction Engineering
Laboratory (RREL) of the U.S. Environmental Protection Agency are
divided into four categories, depending on the intended use of the data.
Quality Assurance (QA) Project Plans are written to ensure that project
needs will be met and that quality control procedures are sufficient for
obtaining data of known quality. The level of QA required, however,
depends on the project category selected for a given project. Projects that
are of sufficient scope and substance that their results could be combined
with the results of other projects of similar scope to produce narratives that
would be used for rule-making, regulation making, or policy making are
identified as Category H projects. In addition, projects that do not fit this
pattern, but have high visibility, would also be included in this category.
To assist professional scientists and engineers in preparing QA Project
Plans, separate guidance manuals in an easy-to-read format have been
developed for each category. The Category II manual contains detailed
descriptions of each of the 12 required elements of a Category II QA
Project Plan. Also included are definitions and explanations of frequently
used terms, examples of QA forms and charts, sample equations, and
numerous types of tables suggested for summarizing information.
IV
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Contents
Page
Foreword ......................... . [[[
Abstract ..... . ................................ , [[[
Figures [[[
Tables .................... . [[[ . ........ '""
Acknowledgments ...... . [[[
0.0 Introduction ....................................... . [[[ 1
1.0 Project Description [[[ 7
2.0 Project Organization and Responsibilities ............................. . .................... 17
3.0 Quality Assurance Objectives [[[ 19
4.0 Site Selection and Sampling Procedures ...................................... . ............. 27
5.0 Analytical Procedures and Calibration ................... . ................................... 37
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Page
5
Figures
Number
0-1 QA Project Plan Approval Form •
2-1 Project organization and names of responsible individuals 18
4-1 Example of a chain-of-custody record • 34
4-2 Examples of a typical sample label and a custody seal 35
6-1 Example of a data reduction, validation, and reporting scheme 46
VI
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Tables
Number
Page
1-1 Summary- of Critical and Noncritical Measurements for the
Evaluation of an Hypothetical Electric Arc Incinerator 10
1-2 Summary of Physical Measurements for the Evaluation of an
Hypothetical Electric Arc Incinerator 11
1-3 Summary of Planned Analyses (Including QC) for Chemical
Treatment of Water 12
1-4 Total Number of Analyses (Not Including QC) for Each Treatment
Condition: Hypothetical Solidification Process 13
1-5 Expanded Sample Summary for Non-QC and QC Samples 14
3-1 QA Objectives for Precision, Accuracy, and Method Detection Limits 21
3-2 QA Objectives for Precision, Accuracy, and Detection Limits -
Alternate Form 22
3-3 Required Detection Limits for Volatile Chlorinated Organic
Compounds 23
4-1 Summary of Number of Samples Required for Hypothetical
Incineration Test ; 29
4-2 Summary of Laboratory Analyses and Sample Quantity Requirements .... 30
4-3 Required Containers, Preservation Techniques, and Holding Times 32
5-1 Typical Summary Table of Standard Methods and Procedures 38
5-2 Typical Summary Table of Calibration Requirements for Physical
Process Measurements 43
7-1 Scheduled QC and Calibration 51
vii
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Acknowledgments
The extensive technical contributions of Dr. John R. Wallace of Maxwell
Laboratories and the assistance of Robert Banner, Ann Kern, and William
Mueller of the USEPA in reviewing the document are gratefully
acknowledged. Grateful appreciation is, also, extended to the excellent
editorial and technical comments provided by Dr. Monica Nees.
Vlll
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SECTION 0.0
INTRODUCTION
0.1 PURPOSE OF THE QUALITY ASSURANCE PROJECT PLAN (QAPJP)
The purpose of a QA Project Plan is to relate project objectives to specific measurements
required to achieve those objectives. The QA Project Plan must provide sufficient detail to
demonstrate the following:
• Intended measurements are appropriate for achieving project objectives;
• Quality control procedures are sufficient for obtaining data of known and
adequate quality; and
• Such data will be defensible if challenged technically or legally.
Environmental projects require the coordinated efforts of numerous individuals, including
regulators, managers, engineers, scientists, statisticians, and economists. The QA Project Plan
must integrate the requirements of everyone involved, in a form that permits an easy and painless
review. It must also provide unambiguous instructions to the sampling team, the analytical
laboratory, and any other parties responsible for data generation. Finally, the QA Project Plan
must provide sufficient detail to allow a thorough, detailed review by an independent party not
involved in the project implementation.
0.2 QUALITY ASSURANCE CATEGORIES
Because the end use of the data determines the degree of quality assurance that is required,
RREL uses four categories in its QA Program:
CATEGORY I PROJECTS require the most rigorous and detailed QA, since
the resulting data must be both legally and scientifically defensible. Category I
projects include enforcement actions and projects of significant national or
congressional visibility. Such projects are typically monitored by the Adminis-
trator. Category I projects must produce results that are autonomous; that is,
results that can prove or disprove a hypothesis without reference to comple-
mentary projects.
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CATEGORY H PROJECTS are those producing results that complement other
inputs. These projects are of sufficient scope and substance that their results
could be combined with those from other projects of similar scope to produce
information for making rules, regulations, or policies. In addition, projects that do
not fit this pattern, but have high visibility, would also be included in this
category.
CATEGORY HI PROJECTS are those producing results used to evaluate and
select basic options, or to perform feasibility studies or preliminary assessments
of unexplored areas which might lead to further work.
CATEGORY IV PROJECTS are those producing results for the purpose of
assessing suppositions.
The RREL Technical Project Manager is responsible for assigning the category that accurately
reflects the intended use of the data and the type of work being done.
This document addresses only Category E requirements; separate documents are available for
each of the remaining categories. Be sure to use the Preparation Aids document for the correct
category.
0.3 UNDERLYING LOGIC AND ORGANIZATION OF A QA PROJECT PLAN
A QA Project Plan, regardless of category, must cover the following topics:
• Process being tested and the objectives of the test (i.e., the hypothesis to be
tested);
• Measurements that will be taken to achieve those objectives;
• Quality of data that will be required and how that quality will be obtained; and
• How data will be recorded, calculated, reviewed, and reported in a defensible
manner.
The QA Project Plan is organized according to the topics discussed in the body of this report.
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To be an effective communication tool, the QA Project Plan must be concise, but still contain
essential experimental detail.
Be sure to include:
* Any project-specific Information necessary for the sampling team, analyt-
ical laboratory, data reduction team, and all other project participants.
However, assume these parties are familiar with standard methods.
* Any deviations from standard methods or procedures, or clarification of
such documents whenever there are ambiguities.
* Equations for all project-specific calculations and date reductions,
But don't be repetitious:
* »o hot discuss the same subject matter more than once in a QA Project
Flan. Although the required elements of the QA Project Plan may appear
to overlap in some cases, repetition leads to confusion, and to documents
too long for effective communication. If you are unsure where a subject
should be treated, discuss it once and cross-reference that discussion in the
other sections.
» Bo not repeat material from a Sampling Plan. If a separate Sampling
Plan has been generated, reference the section and page number in the Q A
Project Plan, as needed.
<• f
* Do not repeat material from standard methods that are available from the
EPA or the Code of federal Regulations. Provide detailed citations and
assume that the analyst and reviewer have these methods on-hand.
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0.4 CATEGORY II FORMAT NOTES
All Category H QA Project Plans must incorporate the following format requirements:
• Title page.
• QA Project Plan Approval Form (see Figure 0-1).
• Distribution list to ensure that key personnel will receive current copies and
updates.
• Table of Contents as shown at the beginning of this document. If a given
element is not applicable, the text of the QA Project Plan should explain its
omission.
• Document control format. Section number, revision, date, and page should be
recorded in an upper corner of each page. This format requirement is illus-
trated below.
Section No.
Revision:
Date:
Page:
1.0
0
October 20, 1989
3 of 5
0.5 QA PROJECT PLAN APPROVAL FORM (SIGNATURE PAGE)
It is important that the project principals understand and agree on the experimental approach. For this
reason, the QA Project Plan Approval Form must be signed by key project personnel as well as key
personnel from any subcontractors. These signatures—which must be obtained before the final QA
Project Plan is submitted—indicate that the key personnel have read the appropriate sections of the QA
Project Plan and are committed to implementing the plan.
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QUALITY ASSURANCE PROJECT PLAN APPROVAL FORM
for
RREL Contracts/lAGs/Cooperatlve Agreements/In-house Projects
RREL QA ID No:.
Contractor:
RREL Project Category: _
RREL Lab Workplan No:
QA Project Plan Title:
Revision Date:
COMMITMENT TO IMPLEMENT THE ABOVE QA PROJECT PLAN:
Contractor's Project/Task Manager (print)
Signature
Date
Contractor's QA Manager (print)
Signature
Date
Other as Appropriate/Affiliation* (print)
Signature
Date
Other aa Appropriate/Affiliation* (print)
Signature
Date
Other as Appropriate/Affiliation* (print)
Signature
Date
* Commitment signature Is required for any ancillary sampling, analytical, or data
gathering support provided by a subcontractor or RREL principal Investigator.
APPROVAL TO PROCEED IN ACCORDANCE TO THE ABOVE QA PROJECT PLAN:
RREL Technical Project Manager (print)
Signature
Date
CONCURRENCES:
RREL Section or Branch Chief (print)
Guv Slmes,
Signature
RREL QA Manager
Signature
Date
Date
RREL (QAPJP AF)
(March 1989)
Figure 0-1. Quality Assurance Project Plan Approval Form
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SECTION 1.0
PROJECT DESCRIPTION
This section describes the process or environmental system that is to be tested, the project
objectives, a summary of the experimental design, and the proposed project schedule. This
section typically contains the subsections listed below, plus others at the principal investigator's
discretion.
1.1 GENERAL OVERVIEW
This section provides a brief synopsis of the overall project. In one or two paragraphs, describe
the programmatic and regulatory setting in which the project is going to be carried out. The
purpose(s) of the study should be described, along with the decisions that are to be made and the
hypothesis to be tested. Other anticipated uses of the data should also be noted. Explain the
consequences of drawing incorrect conclusions or making invalid decisions. The type of process
or environmental system that is to be tested should also be described briefly.
Category II projects are typically preceded by various preliminary investigations of the site or
process. Results of such preliminary tests are included in this section, with details presented in
an appendix.
Example: Preliminary investigations of the test site indicated an average PCP
concentration of 150 mg/kg, with a range of 10 to 500 mg/kg. A summary of
individual analyses is contained in Appendix...
Category IIQA Project Plans must often demonstrate compliance with applicable regulations.
Such regulations should be summarized if they are applicable to the project.
Example: According to TSCA regulations, PCB emissions from the stack shall be
less than 1 mg/kg of PCB introduced into the incinerator. Combustion efficiency
shall be greater than 99.9999 percent as defined in these regulations (40 CFR
761.70...). According to the State permit, stack emission rates ofHCl must be less
than....
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1.1.1 The Process. Site, Facility, or System
This section describes the process, site, facility, or environmental system that will be tested.
Include flow diagrams, maps, charts, etc., as needed. Approximate mass or volumetric flow rates
should be indicated to permit proper evaluation of the sampling and process monitoring
procedures. Indicate sampling points with alphanumeric designations, either in this section or in
Section 4.0 (Site Selection and Sampling Procedures). Additional diagrams are often included to
unambiguously describe sampling points. Such detailed diagrams can be included either in this
section or in Section 4.0.
This section should contain enough material to permit a technical reviewer who is unfamiliar
with the specific project to assess the proposed sampling strategy.
1.1.2 Statement of Project Objectives
Category n projects typically have multiple objectives. These project objectives should be
summarized and stated clearly in this section. Avoid scattering statements of project objectives
throughout the sampling and analytical sections of the QA Project Plan, or among several
documents. Statements of objectives, when scattered among various sections, often result in an
unfocused effort
Project objectives should be stated in numerical terms whenever possible:
Poor Statement: The bio-oxidation procedure will be characterized with respect
to its ability to remove semivolatile organic compounds.
Better Statement: The major objective is to demonstrate a bio-oxidation
efficiency of 95 percent for the compounds listed in Table...
Best Statement: The objective is to demonstrate a bio-oxidation efficiency of 90
percent or higher at a confidence level of 95 percent for the compounds listed in
Table...
Some objectives cannot be stated in entirely quantitative terms. For example, one objective for a
bio-treatment project might be to determine the dominant microbiological species in a reactor.
Or, for a test of a new incinerator design, one might wish to determine the range of combustion
conditions that result in a molten ("slagging") ash.
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It is common to rank project objectives according to importance (e.g., into primary and
secondary objectives). Although this ranking is not essential, it does help focus effort on the
primary goals of the project.
1.2 EXPERIMENTAL DESIGN
List all measurements that will be made during the project, then classify them as critical or
noncritical measurements. Critical measurements are those that are necessary to achieve
project objectives; they may include either on-site process measurements or chemical
measurements. Thus, for a test of an electric arc furnace as a means of incinerating organics, the
rates of consumption of shield gas (e.g., argon) and electric power are as important as the feed
rate and concentration of pollutant. Noncritical measurements are those used for process
control or background information. Table 1-1 and Table 1-2 illustrate two different means of
designating critical and noncritical measurements.
It is common practice to test pollution control equipment or processes in different operating
modes or stages. For example, an incinerator might be operated under warm-up conditions,
followed by incineration tests at three different feed rates. The various test conditions should be
summarized in this section. Indicate the length of time anticipated for each test condition. When
appropriate, indicate how equilibrium conditions will be established before sample collection
begins.
Example: Total hydrocarbons in the stack gas will be monitored continuously.
Sampling will not begin until THC concentrations are stable within ± 5 percent
over a three-hour period.
Summarize in tabular form all measurements that are planned for each sample. Ideally, this table
should indicate the total number of samples for each sample point, including quality control and
reserve samples, as illustrated in Table 1-3 for a hypothetical chemical treatment project. Relate
the individual samples to the sampling points shown in the process diagram, if applicable. For
projects involving a large number of samples or analyses, it may not be possible to include all
QC and reserve samples in a single table. For such cases, two or more tables may be necessary,
the first to summarize the primary (non-QC) samples, and the others to show which QC samples
are associated with which analyses. See Tables 1-4 and 1-5 for an example of a hypothetical
project involving the solidification of solid wastes. Information on the total number of all
sample types is needed both to perform a comprehensive review and to estimate analytical costs.
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Table 1-1. Summary of Critical and Noncritical Measurements for
the Evaluation of an Hypothetical Electric Arc Incinerator
A. CRITICAL MEASUREMENTS
Chemical
Critical SVOCs" in all feed and discharge
streams
PCBs in all feed and discharge streams
Particulates, NOX, and SO2 in stock gas
TCLP/critical metalsb in slag and feed
TCLP/critical SVOCs3 in slag
Alkalinity of scrubber water
HC1 in stack gas
Organic carbon in feed
Process
Electrical power consumption, of arc furnace
Argon and oxygen consumption (rate and total)
Mass feed rate of soil
Total mass of slag discharged
Cooling requirements (temperatures and flow rates of
cooling water)
B. NONCRTTICAL MEASUREMENTS
Chemical
Noncritical SVOCs in all feed and discharge streams
Permanent gases in stack: N2» 0%, CO2, CO
Percent moisture in stack
Ash fusion temperature of slag
Process
All temperatures and flows not listed above
Opacity of stack gas
Operating pressures
a Critical SVOCs (semivolatile organic compounds) are-pentachlorophenol, the three tetrachlorophenol isomers,
chlorophenol, 1- and 2-methylnaphthalene, anthracene, acenaphthalene, and acetophene. these compounds have
been detected during preliminary studies on the untreated wastes or are suspected decomposition products.
Noncritical SVOCs are all additional compounds detected by Method 8270, as described hi Section of this
QA Project Plan.
b Critical metals are As, Ba, Cd, Cr, Pb, Hg, Ni, Se, and Ag.
; s,V\ ,*|Ms; table i&meaatto ilusttate typical lonbat.
10
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It is common to rank project objectives according to importance (e.g., into primary and
secondary objectives). Although this ranking is not essential, it does help focus effort on the
primary goals of the project.
1.2 EXPERIMENTAL DESIGN
List all measurements that will be made during the project, then classify them as critical or
noncritical measurements. Critical measurements are those that are necessary to achieve
project objectives; they may include either on-site process measurements or chemical
measurements. Thus, for a test of an electric arc furnace as a means of incinerating organics, the
rates of consumption of shield gas (e.g., argon) and electric power are as important as the feed
rate and concentration of pollutant. Noncritical measurements are those used for process
control or background information. Table 1-1 and Table 1-2 illustrate two different means of
designating critical and noncritical measurements.
It is common practice to test pollution control equipment or processes in different operating
modes or stages. For example, an incinerator might be operated under warm-up conditions,
followed by incineration tests at three different feed rates. The various test conditions should be
summarized in this section. Indicate the length of time anticipated for each test condition. When
appropriate, indicate how equilibrium conditions will be established before sample collection
begins.
Example: Total hydrocarbons in the stack gas will be monitored continuously.
Sampling will not begin until THC concentrations are stable within ± 5 percent
over a three-hour period.
Summarize in tabular form all measurements that are planned for each sample. Ideally, this table
should indicate the total number of samples for each sample point, including quality control and
reserve samples, as illustrated in Table 1-3 for a hypothetical chemical treatment project. Relate
the individual samples to the sampling points shown hi the process diagram, if applicable. For
projects involving a large number of samples or analyses, it may not be possible to include all
QC and reserve samples in a single table. For such cases, two or more tables may be necessary,
the first to summarize the primary (non-QC) samples, and the others to show which QC samples
are associated with which analyses. See Tables 1-4 and 1-5 for an example of a hypothetical
project involving the solidification of solid wastes. Information on the total number of all
sample types is needed both to perform a comprehensive review and to estimate analytical costs.
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Table 1-1. Summary of Critical and Noncritical Measurements for
the Evaluation of an Hypothetical Electric Arc Incinerator
A. CRITICAL MEASUREMENTS
Chemical
Critical SVOCs* in all feed and discharge
streams
PCBs in all feed and discharge streams
Particulates, NOX, and SO2 in stock gas
TCLP/critical metalsb in slag and feed
TClP/critical SVOCs8 in slag ,
Alkalinity of scrubber water
HC1 in stack gas
Organic carbon in feed
Process
Electrical power consumption of arc furnace
Argon and oxygen consumption (rate and total)
Mass feed rate of soil
Total mass of slag discharged
Cooling requirements (temperatures and flow rates of
cooling water)
B. NONCRITICAL MEASUREMENTS
Chemical
Noncritical SVOCs in all feed and discharge streams
Permanent gases in stack: N2,0%, CO^ CO
Percent moisture in stack
Ash fusion temperature of slag
Process
All temperatures and flows not listed above
Opacity of stack gas
Operating pressures
Critical SVOCs (semivolatile organic compounds) are pentachlorophenol, the three tetrachlorophenol isomers,
chlorophenol, 1- and 2-methylnaphthalene, anthracene, acenaphthalene, and acetophene. These compounds have
been detected during preliminary studies on the untreated wastes or are suspected decomposition products.
Noncritical SVOCs are all additional compounds detected by Method 8270, as described in Section of this
QA Project Plan.
Critical metals are As, Ba, Cd, Cr, Pb, Hg, Ni, Se, and Ag.
- *" ^Ehfs tablejs meant. to liustrate typical forjnal<
Ifhe tests listed. ar^NOTiiecsssarlly those tot would be employed
- --,; .." .. ,fot a process oflbis type.
10
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Table 1-2. Summary of Physical Measurements for the Evaluation
of an Hypothetical Electric Arc Incinerator
Measurement
Measurement
Classification
Measurement
Site (Designation)3
Measurement
Frequency
Electric Power to Arc Furnace
Current Critical
Voltage Critical
kWh Critical
Ar and C«2 Flow
Mass of Soil/Slag
Critical
Critical
Power leads to furnace (PI)
Feeds to furnace (Ql)
Drum balances @ feeder and
discharge (Ml, M2)
15 minutes
15 minutes
Before/after each run
15 minutes
Each batch
Opacity of Stack Gas
Temperatures
Noncritical Stack (S3)
Noncritical (Test points T3-T12)
Continuous
5 minutes
1 Alphanumeric designations of test points are shown in Figure
13ii$ table isiaeajatto illustrate typical formal.
Hie test&llsted are NOT necessarily those that wotfld be employed.
-- , forapiocessofthistype*
11
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Table 1-3. Summary of Planned Analyses (Including QC) for Chemical Treatment of Water
Preliminary
Samples
Number of Tests Performed3
Influent
Water
Effluent
Water
Sample Points:
Cl E2
Sludge
S3
Total
Semivolan'le Organic Compounds (SVOC)b
Non-QC (Primary) 3
Reid Sampling Blank0 1
Field Duplicates 0
Laboratory Duplicates 0
Matrix Spikes (MSs) 1
Matrix Spike Duplicates (MSDs) 1
Spare Samples4* 2
Independent Check Standard 0
Metalse
Non-QC (Primary) 3
Field Sampling Blank0 1
Field Duplicates 0
Laboratory Duplicates 1
Matrix Spikes (MSs) 1
Matrix Spike Duplicates (MSDs) 0
Independent Check Standard 0
Spare Samples^ 2
60
1
0
0
3
3
10
1
60
1
0
3
3
0
1
10
60
0
0
0
10
10
10
0
60
0
0
10
10
0
0
10
10
0
5
0
2
2
0
0
Grand Total
10
0
5
2
2
0
0
0
Grand Total
133
2
5
0
16
16
22
1
195
133
2
5
16
16
0
1
22
195
a Samples will be divided evenly among the ten anticipated runs. More QC samples are planned for the effluent
than for the influent, since the former samples are expected to exhibit more variability. A matrix spike/matrix
spike duplicate or a laboratory duplicate/matrix spike of the effluent stream will be determined for each treatment
condition, because the effluent matrix may vary significantly with each treatment
b Refers to the twelve compounds listed in Table .
0 Trip blanks will be collected but not analyzed unless field blanks indicate a contamination problem.
d Not analyzed unless required.
e Refers to the eight metals in Table .
The tests fisted arekof necessarily those &at would b$ employed
., ','fora process of this type.
•* * * ff f .
12
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Table 1-4. Total Number of Analyses (Not Including QC)
for Each Treatment Condition: Hypothetical Solidification Process
Treatment Condition
Measurement3
On-Site Tests
Slump of Portland Cement Concrete
Homogeneity of Mixing
Leaching Tests/Analyses^
TCLP/Metals
T
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Table 1-5. Expanded Sample Summary for Non-QC and QC Samples
Measurement
TCLP-Metals
VOCs-Total
•
•
Raw
Type • Soil
Non-QC Samples
Leachate Duplicate
Leachate Blank
IRM3
Matrix Spike
*
Non-QC Samples
Sample Duplicate
Sample Equipment Blank
Method Blank
Independent Check Standard
Matrix Spike
Matrix Spike Duplicate
•
•
9
1
1
1
0
•
9
3
1
1
1
1
1
•
Treated
Soil
(28 Days)
9
1
1
1
1
9
0
1
1
' 1
1
1
Reagent
Mix
1
0
0
0
0
1
0
0
0
0
0
0
Long-Term
Treated
Soils
15
3
3
3
0
•
0
0
0
0
0
0
0
•
Total
34
5
5
5
1
•
19
3
2
2
2
2
2
aIRM s Independent reference material
'$*& table ismeautto Mustrate Apical fonaat
The tests listed ^KOTiiecessarlfy &0setf*at wo»l4 be employed
14
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1.3 SCHEDULE
Indicate start-up and ending dates, including those for preliminary studies and field and
laboratory activities.
Be sure to:
Include enough information in this section to permit a technical person
unfamiliar with your project to evaluate^; sampling and analytical
approach.
Avoid repeating material from a sampling or analytical plan. Complete a
necessary description once, then cite it in all other documents Repeating
material inevitably leads to confusion and wastes the valuable time of
project participants, typists, and reviewers. Most important, essential
details are readily overlooked when buried in repetitious or overly lengthy
documentation.
"y/ , ' -
Cite applicable regulations, if any.
15
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SECTION 2.0
PROJECT ORGANIZATION AND RESPONSIBILITIES
This section demonstrates that the project organization is adequate to accomplish project goals,
and that all responsibilities have been assigned.
Provide a table or chart illustrating project organization and lines of authority. For each
organizational entity or subcontractor, identify by name all key personnel and give their
geographic locations and phone numbers. The organizational chart should also include all
subcontractors and their key points of contact. Separate organizational charts for subcontractors
may also be needed. The organizational chart should identify QA Managers, including those of
subcontractors, and should illustrate their relationship to other project personnel. The QA
Managers should be organizationally independent of the project management so that the risk of
conflict of interest is minimized.
Describe the responsibilities of all project participants, including QA Managers. Be sure to
indicate responsibility for each type of analysis, physical measurement, and process measure-
ment. This summary should designate responsibility for planning, coordination, sample
collection, sample custody, analysis, review, and report preparation.
Describe the frequency and mechanisms of communications among the contractor, the
contractor's QA Manager, and the EPA Project Manager, as well as among contractor and
subcontractors. Give the regular schedules for progress reports, site visits, and teleconferences,
and describe which special occurrences would trigger additional communication.
Figure 2-1 illustrates a typical project organizational chart with an independent QA Manager.
Be sure to:
Provide »a^es, ioeatisns, wgaH&atlonal affiliatf ons, jrad telephone amttliers for
' ' J '
17
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EPA
PROJECT OFFICER
- CONTRACTOR
PROJECT MANAGER
CONTRACTOR
ENGINEERING
ASSESSMENTS
CONTRACTOR
QA MANAGER
SUBCONTRACTOR:
(COMPANY NAME)
LABORATORY
MANAGER
CONTRACTOR
LABORATORY
SUPERVISOR
SAMPLE
PREPARATION
TRACE METALS
AND CHLORIDE
ANALYSES
DATA
REDUCTION
SAMPLING
GC
ANALYSIS
pH, CEC, RsCI2
ACIDITY, ALKALINITY,
ANDTDS
REPORT
GENERATION
Figure 2-1. Project organization and names of responsible individuals
18
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SECTION 3.0
QUALITY ASSURANCE OBJECTIVES
Quality assurance objectives are specifications that measurements must meet in order to achieve
project objectives. For example, in ordering a pump for a chemical plant, factors such as
capacity, pressure, and materials of construction must be specified. Similarly, precision,
accuracy, detection limits, and completeness must be specified for physical/chemical
measurements. Additional analytical requirements are described qualitatively in terms of repre-
sentativeness and comparability. Quality assurance objectives are needed for all critical
measurements (see Section 1.2) and for each type of sample matrix (soil, water, biota, etc.). Be
sure to include quality assurance objectives for physical as well as chemical measurements.
Once QA objectives are set, the measurement systems are designed to meet them. The project
manager, analytical chemists, and other principals must agree on the feasibility and appro-
priateness of these objectives.
3.1 DETERMINING QA OBJECTIVES
QA objectives must be defined in terms of project requirements, and not in terms of the
capabilities of the intended test methods. Of course, the QA objectives must be achievable by
available methods, and for this reason it is important that the laboratory review the QA
objectives. When QA objectives exceed the capabilities of available methods, either the methods
must be modified or the test plan must compensate for these deficiencies. Modifications may
often be as simple as collecting a larger sample. However, if nonstandard or significantly
modified test methods are required, the QA Project Plan must include laboratory validation data
to prove that the method is capable of achieving the desired performance.
The following are examples of how QA objectives can be determined:
Example 1: Biological treatment ofpentachlorophenol (POP).
Previous experience with this treatment process has indicated that the output concen-
tration typically varies by a factor of two under stable operating conditions with uniform
feed. To avoid contributing additional error, the precision of the analytical methods
should be significantly less than this value, or approximately ±30 percent or less.
19
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3.2
Example 2: Determination of destruction removal efficiency (DRE)for incineration of a
Dinoseb formulation containing 20 percent w/v Dinoseb.
The purpose of this test is to demonstrate a ORE of 99.99 percent or better. Dinoseb in
stack gases will be collected on a Modified Method 5 sampling train. Extracts of all
components of this train -will be combined and reduced to 0.5-mL volume. The following
parameters were used to estimate the required detection limit.
Feed rate of 20% w/v Dinoseb Formulation (120 mL/min)
Dinoseb Feed Rate 24 g/min
Stack Gas Flow Rate 16drym?/min
Expected Concentration of Dinoseb in Stack Gas ifDRE = 0% 1.5 glm3
Maximum Permitted Concentration of Dinoseb, DRE = 99.99 % 15 x W4 gin?
Expected Volume ofMM-5 Sample (3 Hours at 1.5 Llmin) 2.7 dry m3
Dinoseb Collected at DRE = 99.99 % 400 uglsample
To allow a reasonable margin of error, the detection limit required for the Dinoseb
determination mil be 40 uglMMS train. Previous experience with the determination of
Dinoseb on XAD resin has shown that this detection limit can be achieved routinely with
the method attached as Appendix B. Previous experience has also shown that Dinoseb
can be recovered routinely from a MM5 train with a recovery 2=50 percent and a
precision of ^30-percent relative percent difference (RPD), and deviations beyond these
ranges indicate analytical problems. Results of a methods validation study performed in
our laboratory are attached as Appendix C.
QUANTITATIVE QA OBJECTIVES: PRECISION, ACCURACY, METHOD
DETECTION LIMIT, AND COMPLETENESS
QA objectives for precision, accuracy, method detection limit, and completeness should be
presented in a QA objectives table similar to those shown in Tables 3-1 through 3-3. Be sure to
include QA objectives for all matrix types and to indicate the units in which these QA objectives
are given. Summary tables are very helpful to the laboratory which must meet these objectives.
Because precision and accuracy can be measured in various ways, explain the method to be used.
If precision, for instance, is to be determined by duplicates, explain whether sample splitting
will occur in the laboratory, during sampling, or at some other stage. Then summarize all such
information in either text or tabular format.
20
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Table 3-2. QA Objectives for Precision, Accuracy, and Detection Limits - Alternate Form
Data
Quality Parameter
Method of
Determination
Frequency
Required
Objective3^1)
Semivolatile Organic Compounds
Precision
- Water
- TCCP leachates
Accuracy
- Water &TCLP leachates
- Water &TCLP leachates
- Water
- MMStrain
Detection limits
- Water
- MMStrain
Field duplicate
Duplicate leaching
of laboratory - split
sample
Laboratory matrix
spike
Surrogate
NIST standard
reference materials
Spike of XAD resin
7 analyses of .
spiked clean water
3 analyses of
spiked XAD resinw
I/test condition
I/test condition
1 water/test
condition
1 leachate/test
condition
All samples
I/project
3/project
1 before project
1 before project
-.
RPD<50
RPD <60
Recovery = 50-150%
Recovery = 50-150%
(b)
Recovery = 50-150%
Recovery = 50-150%
MDL £ 10 jig/L, neutrals
MDL £ 20 ug/L, phenols
MDL £ 100 jtg/L, bases
MDL £ 20 ng
a RPD = relative percent difference.
MDL = method detection limit
b As specified in Method 8270.
Note (1) Objectives must be met for all critical measurements. (See Section 1.2 of this document.)
Note (2) MDLs must be calculated according to Equation (8), Section 9.0 of this document, which takes into
account the number of low-level samples analyzed.
Th&testsSsted are NOT necessarily those that weMd toe employed
,vAV"^Xx, """^ for; a process of this ty|>ex', t
22
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Table 3-3. Required Detection Limits for Volatile Chlorinated Organic Compounds
,a
Compound
Regulatory
Threshold
Required
MDL (jzg/L)
1,1,1 -Trichloroethane
1,1 -Dichloroethane
1,1 -Dichloroethene
Vinyl chloride
1,2-Dichloroethane
Perchloroethylene
5
5
5
2
1
5
0.5
0.5
0.5
0.2
0.1
0.5
a
Method detection limits for these compounds are critical and will be determined experi-
mentally by the laboratory before sample collection is started. MDLs must be well below the
Regulatory Threshold in order to demonstrate that treated waters meet discharge limits.
The tests listed are NOT necessarily those that would be employed
for a process of this type* -'"
The following statements are examples of descriptions for precision, accuracy, method detection
limits, and completeness:
• Precision objectives for all the listed methods except pH are presented as relative
percent difference (RPD) of field duplicates. Precision objectives for pH are listed in
pH units and expressed as limits for field duplicates. . , ... „,„
• Precision objectives for unconfined compressive strength are given as relative
standard deviation for triplicate sets. .;.'....»
• Accuracy objectives for organic compounds and metals are given as percent recovery
range of laboratory matrix spikes. Accuracy objectives for temperature
measurements are absolute deviations in ° C.
• Detection limits are defined as the method detection limit (MDL) multiplied by the . *
dilution factor required to analyze the sample, MDLs will be determined by replicate (
extraction and analysis of seven identical spiked samples of XAD resin.
23
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• Completeness is defined as the number of measurements judged valid compared to the
number of measurements needed to achieve a specified level of confidence in decision
making. It has been estimated in Section _._ that 10 valid measurements should
suffice to demonstrate that the arsenic concentration in the discharge is less than 50
itgIL at a confidence level of 90 percent. To allow for a margin of error in the
estimated number of samples, 15 valid-measurements are planned, resulting in a
completeness objective of 150 percent. An additional 6 spare samples will be
collected but not analyzed, unless needed to achieve the desired confidence level.
When analyzing for a large number of organic compounds by GC or GC/MS, it is usually
unnecessary to list QA objectives for each compound separately. Instead, list QA objectives
according to compound type, as was done for the semivolatile detection limits in Table 3-2. In
other cases, for example, where detection limits are derived from applicable regulations, list
detection limits for individual compounds, as in Table 3-3.
Finally, the author of the QA Project Plan must explain how the QA objectives are to be
interpreted in a statistical sense. QA objectives are often interpreted in a sense that all data must
fall within these goals; for such projects any data that fail to satisfy the QA objectives are
rejected and corrective action is undertaken. However, other interpretations are possible. For
example, the project requirements may be satisfied if the average recovery is within the
objectives; that is, excursions beyond the objectives might be permitted, but the average recovery
would have to satisfy the goals described in this table. Whatever the case, it is important to
describe in this section how tabulated QA objectives will be interpreted.
3.3 QUALITATIVE QA OBJECTIVES: COMPARABILITY AND
REPRESENTATIVENESS
Comparability is the degree to which one data set can be compared to another. For instance, to
evaluate an environmental cleanup process, analyses of the feed and discharge streams must be
comparable. Similarly, to perform a nationwide environmental survey, methods used at different
locations must be comparable. Comparability is achieved by the use of consistent methods and
by traceability of standards to a reliable source.
Representativeness is the degree to which a sample or group of samples is indicative of the
population being studied. An environmental sample is representative for a parameter of interest
when the average value obtained from a group of such samples tends towards the true value of
that parameter in the actual environment, as the number of representative samples is increased.
24
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Representativeness is normally achieved by collecting a sufficiently large number of unbiased
samples. .
The QA Project Plan should demonstrate that adequate comparability and representativeness will
be achieved.
3.4 OTHER QA OBJECTIVES
Some projects may require additional QA objectives, such as mass balances. Requirements for
all additional QA measurements should be stated in this section.
Example: Soil Washing for Removal of PCP.
A mass balance will be calculated according to the following expression:
Mass Balance = Mass of PCP in output streams/mass of PCP in input streams
For this test to be successful, mass balance should be between 50 and 150
percent. The specific equations for calculating the influent and effluent masses in
terms of the measured quantities are given in Section _._ of this QA Project Plan.
3.5 WHAT IF QA OBJECTIVES ARE NOT MET?
This section should include a discussion of the impact of not meeting one or more QA objectives.
Will the project be a complete loss? Will some, but not all, of the project goals still be realized?
Will the statistical confidence level be reduced? Are there legal or regulatory ramifications?
Answers to such questions help provide a critical perspective on the QA Program.
25
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SECTION 4.0
SITE SELECTION AND SAMPLING PROCEDURES
This section must describe a plan for site selection and sampling which is responsive to those
project objectives stated in Section 1.1.2. A detailed discussion of the sampling plan devel-
opment process is presented in Volume 2 of SW-846, Test Methods for Evaluating Solid Waste
(3rd Ed.). Since SW-846 will likely undergo revisions, be sure to refer to the latest revision or
edition.
This section explains the overall sampling strategy, the specific sampling procedures that will be
employed, sample custody, record keeping, and shipping requirements.
4.1 SAMPLING SITE SELECTION
For most Category II projects, the sampling sites will have been identified already, and pre-
liminary data will be available. However, for certain projects such as those involving surveys at
a number of geographically separate sites, it may be impossible to explicitly delineate sampling
locations in the QA Project Plan. For these projects, explain how sampling sites will be selected
during the project. The following information should be provided:
• A qualitative statement of the sample population to be represented by the
samples;
° A description of the statistical method or scientific rationale to be used in
selecting sample sites;
« Descriptions of the type of sampling strategy (e.g., simple, stratified, system-
atic random sampling);
« A description of the sample types (air, water, soil, biota);
• A qualitative statement regarding potential sources of sample contamination;
° Guidelines for determining sampling frequency and number for each sample
type; and
» A discussion of the extent to which site selection will affect the validity of the
resulting data and project objectives.
27
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4.2 SAMPLING SITE DESCRIPTION
This section includes charts, maps, sampling grids, or tables specifying the exact sampling sites.:
Note any site modifications or additions that will be needed prior to sampling, such as the
extension of duct work or the addition of special valves. Also describe all locations and access
points for critical process measurements such as flow rates, pressures, or temperatures. Discuss
any site-specific factors that may affect sampling procedures.
For each analyte and each sampling point, list the frequency of sample collection and the total
number of samples collected. This summary can best be prepared in tabular form, as shown in
Table 4-1. Note that the numbers given in this table may differ from the number of analyses,
since some samples may be analyzed in replicate, while others may be analyzed only on a
contingency basis. Explain the statistical basis for the sampling scheme, as necessary.
4.3 SAMPLING PROCEDURES
This section describes the specific procedures that will be used for collecting and preserving
samples.
• Discuss each sampling procedure that will be employed. For EPA-approved
procedures, a reference is sufficient. Other sampling procedures should be
summarized in the text, and additional details should be provided in an
Appendix. (Copies of ASTM sampling procedures are frequently appended.)
• Prepare a list of analytes, sample volumes to be collected, and the amount of
sample that is required for each analysis (see Table 4-2). Note whether the
required amount is .intended for matrix spike/matrix spike duplicate determin-
ations or for a single determination only. Be sure to have your laboratory
manager review this table to ensure that the sample volume or mass is suffi-
cient for all intended analyses.
• Describe any compositing or sample splitting procedures that will be employed
in the field or laboratory.
• Describe any sampling equipment that will be used, and how this equipment
will be calibrated.
28
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Table 4-1. Summary of Number of Samples Required for Hypothetical Incineration Test
Description/Use
Slurry
Feed
(Fl)
Scrubber
Sump
(SI)
Scrubber
Slowdown
(S2)
Ash
(S3)
Stack
(S4)
Total
SVOCsa
Non-QC Samples + MS+ MSDb 10
Sample Duplicates 3
Sample Blanks 1
Spare Samples0 5
Modified Method 5
Non-QC Samples 0
Sample Blanks (see text) ' 0
VOCsa
Non-QC Samples , 20
Sample Blanks 1
TripBlanksd 1
Spare Samples6 20
10
0
1
5
0
0
20
1
1
20
10
0
0
5
0
0
20
1
1
20
5
0
0
5
0
0
10
1
1
10
0
0
0
0
4
1
0
0
0
0
35
3
2
20
4
1
70
4
4
70
As designated in Section .
Each sample will provide enough material for an original sample plus a matrix spike and a
matrix spike duplicate.
Not analyzed unless first analysis fails.
Not analyzed unless sample blank is contaminated.
TJie tests listed are NOT necessarily those tfeat -would be employed.
" * " for a process of fejs type.
29
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Table 4-2. Summary of Laboratory Analyses and Sample Quantity Requirements
Sample Quantity
Stream Sampling Method Analysis Parameter Container Size Required for Analysis^1)
Test soil
Treated soil
Scrubber makeup
scrubber liquor
Scrubber solids
Stack
Shelby tubes
ASTM-C172/
composite"'
Grab
Thief
Methods
Midget M-5(2)
Metals train'2)
Modified Method 5
NIOSH-1003(2)
Semivolatiles
Volatiles
Metals scan
Dioxins/furans
EP toxicity
TCLP
Higher heating value
Chlorine
Moisture
Semivolatiles
Volatiles
Metals scan
Dioxins/furans
TCLP
Semivolatiles
Volatiles
Metals scan
Dioxins/furans
Semivolatiles
Volatiles
Metals scan
Dioxins/furans
Paniculate
HC1
Metals
Semivolatiles
Dioxins/furans
Volatiles
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
250 mL
1 L
40 mL VGA vial
1 L
1 L
250 mL
250 mL
250 mL
250 mL
50 g
50 g
100 g
50 g
250 g
500 g
250 g
250 g
100 g
50 g
50 g
100 g
50 g
500 g
1 L
40 mLVOAvial
1 L
1 L
50 g
50 g
100 g
50 g
900 L
900 L
900 L
3000 L
3000 L
20 L
Note (1) Indicate whether the listed quantity suffices for replicates, spikes, and other QC purposes, or if it is
sufficient for only a single analysis. In the latter case, indicate how extra material will be provided for
QC purposes.
Note (2) Copies of these methods would have to be appended because they are not readily available.
v '-:- -", ttols iabte is nsea&tto it»$trate typ&al tnj&at.
teci areKOTiiecessarily Hiosethat weald be $r»|>I0yed.
" s
^,,y , „;?
„ s-rt-v' /• \
^ >••&. -. f > v^^-tX v,-,,
30
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• Explain how sample containers will be cleaned to prevent sample contami-
nation, and how new sample containers will be checked for contaminants.
• Describe the containers used for sample collection, transport, and storage for
each sample type. Include sample preservation methods, noting specific
reagents, equipment, supplies, etc., required for sample preservation, and the
specific time requirements for shipping samples to the laboratory. Note
refrigeration conditions and holding times that will be employed. (See, for
example, Table 4-3.)
• Describe the procedures used to record sample history, sampling conditions,
and any other pertinent information; include examples of forms that will be
employed. Describe the numbering sequence to ensure that each sample will
be assigned a unique number.
• Include an example of the sample label to be used.
-JBtow ar& you ttoing s$ far? At the completion of this sectk«i?
you should be able to easily calculate the required number
,v~,, «£fe9cfe type of sample container* -- * -
4.4 SAMPLE CUSTODY
Occasionally samples are spilled, contaminated, accidentally evaporated to dryness, or otherwise
compromised before or during sampling and analysis. Sample custody allows detection of such
problems should they occur and minimizes such occurrences by assigning responsibility for all
stages of sample handling. Sample custody is maintained when the samples are in a secure area
or are in the view of, or under the control of, a particular individual. Records of everyone
handling samples are maintained so that a sample history can be reconstructed later, should the
need arise.
This section describes how sample custody will be maintained and recorded.
• Give the names of all sample custodians in the field and in each of the
laboratories.
• Give examples of forms that will be used to maintain sample custody in the
field, during shipping, and in the laboratory.
31
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Table 4-3. Required Containers, Preservation Techniques, and Holding Times
Measurement
Type8
Preservation15
Maximum Holding Times0
Extractable organics
Pesticides, PCBs
Metals (except mercury
and chromium VI)
G Coolto4'C,
Teflon-lined septum protect from light
G Coolto4'C,
Teflon-lined septum pH 5-9
P,G
HNO3topH<2
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
6 months
Mercury
Chromium VI
PH
Residue
Organic carbon, total
Sulfide
P,G
P,G
P,G
P,G
P,G
P,G
HNO3topH<2
Cool,4'C
None required
Cool,4°C
Cool,4'C,HClor
1^804 to pH<2
Cool to 4 °C;
add zinc acetate plus
NaOHtopH>9
28 days
24 hours
Analyze water immediately
(on site); none specified for soil
7 days
28 days
7 days
a Polyethylene (P) or glass (G).
° Sample will be preserved immediately upon sample collection.
c Samples will be analyzed as soon as possible after collection. The times listed are the maximum times that
samples will be held before analysis and still be considered valid. All data obtained beyond the maximum
holding times will be flagged.
EttSKalthough *$pical> may noi be ajppropilate for every project
^ss^sS •.«.•»%•.•.
32
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• Seal shipping containers with chain-of-custody seals. Give an example of the
seal that will be used.
• Describe procedures that will be used to maintain chain of custody during
transfer from the field to the laboratory, within the laboratory, and among
contractors and subcontractors.
• Provide for archiving of all shipping documents and other paperwork received
at the laboratory with the samples.
Figures 4-1 and 4-2 give examples of satisfactory chain-of-custody records, official sample seals,
and sample labels. See also Chapter 9 of SW-846 (3rd Ed.) for additional discussion of shipping
and custody procedures. Since SW-846 will likely undergo revisions, be sure to refer to the
latest revision or edition.
Do you want to save time and money?
XJse Standard Operating Procedures ($QPs)J Certain information required
in this section—such as sample custody procedures, forms, labels, and
sampling methods—is not project-specific, but applies to a wide range of
sampling efforts. Typically, a sampling team or a laboratory will use the
same chain-of-custody procedures from one project to the next. Such
procedures may be written as SQPs, which can then be appended to
subsequent QA Project Plans. Be sure to use document control format in the
to alert the reviewer to any recent changes in the procedure^ - -
33
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•0
o
eo
tn
I
34
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Sample Label
(Name of Sampling Organization
Sample psseriptiorv ; ,
Plant- Location!
Date!
Media! Station-
Sample Type! , Preservative!
Sampled by! ..,.
Sample ID Nn.! _ _.„—-. — —
La*> NO
)
«••
03
CD
5
Custody Seal
ivas Aaoisno '-
\
f
I
CUSTODY SEAL
I ,
g Date
P*
Signature
Figure 4-2. Examples of a typical sample label and a custody seal.
35
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-------
SECTION 5.0
ANALYTICAL PROCEDURES AND CALIBRATION
This section of the QA Project Plan must describe.all of the field and laboratory procedures used
for both chemical and physical measurements. Sample preparation methods and cleanup
procedures (such as extraction, digestion, column cleaning) should also be included.
All methods must be appropriate for their intended use and be described in sufficient detail. This
section, when coupled with QC procedures described in Section 7.0, should provide enough
detail to permit the analytical chemists or other measurement specialists to carry out their
procedures unambiguously.
Requirements of this section can often be satisfied by referencing appropriate standard methods.
Most RREL projects rely heavily on EPA-approved methods that have been validated for
environmental samples. Standardized procedures from other organizations, such as the ASTM
and the American Public Health Association, are also commonly employed when approved
validated EPA methods are unavailable. When standard methods are unavailable, nonstandard
methods must be used and described in detail. It is essential to consult the analytical
laboratory and other measurement specialists for guidance during preparation of this
section because they know the intricacies and limitations of the methods.
Begin this section with a summary table of all measurements to be made. For projects involving
many kinds of measurements, consider providing separate tables for each type of test. Specify
the parameter to be measured, the sample type, the method number (when available), the title, the
method type, and a reference. (See Table 5-1 as an example.) Note the revision number of the
method or the edition number of a publication, since nominally identical methods may be
modified by these updates. Provide additional project-specific information in the text of this
section.
37
-------
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39
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5.1 EPA-APPROVED OR OTHER VALIDATED STANDARD METHODS
EPA-approved or similar validated methods can be incorporated by reference, thereby greatly
minimizing the effort required to complete this section. Once a method is cited, do not repeat
information that is already found in the method. Some additional information is almost always
required, however, to assure that project-specific requirements will be met. The following
considerations apply:
• Some EPA-promulgated methods contain only general procedure descriptions
and lack specific QC requirements or applicable validation data. For example,
EPA Method 18 provides general requirements for GC analysis of stack gases,
but contains no QC requirements. For such methods, validation data pertinent
to the specific project must be appended. Alternately, a preliminary method
validation can be specified as a subtask of the project; in that case, however,
specific procedures and acceptance criteria for method validation must also be
included as part of the QA Project Plan.
• Other EPA-approved standard methods, such as those found in Standard
Methods for the Examination of Water and Wastewater, give operating
procedures but omit most QC and calibration requirements. This missing
information must be provided either in this section or in Section 7.0 of the QA
Project Plan. As a minimum, be sure to specify the frequency, acceptance
criteria, and corrective action plans for all QC procedures and calibrations.
• It is not necessary to include copies of methods or sections of methods from
SW-846, the Code of Federal Regulations, Standard Methods for the
Examination of Water and Wastewater, or Methods for Chemical Analysis of
Water and Waste because these sources are readily available. Elowever, do
append ASTM and NIOSH procedures because they may not be so readily
available to other project principals or reviewers.
• EPA-approved or similarly validated methods that are significantly modified
are considered to be unvalidated methods and are treated as described in
Section 5.2.
• Certain EPA methods such as those found in SW-846 specify most operating
details, including quality control and calibration requirements. Such
procedures, however, frequently allow the user to specify certain other options
40
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to satisfy project objectives. For example, for multianalyte methods such as
GC/MS, the user will typically specify the target compound list that is required
for the project. Matrix spike compounds are chosen from the compounds of
interest to the particular project, and are not necessarily those recommended in
the method. Also list the project-specific target compounds to be used as
calibration check compounds and matrix spike compounds. Specify the
acceptance criteria for matrix spike compounds. In certain cases, isotopically
labeled forms of the project analytes may be included as surrogates.
The following is an example of how one might specify various options allowed by Method 8080,
a validated method from SW-846 which contains QC and calibration requirements:
Example: Method 8080.
This method will be employed to determine the 19 pesticides listed in Table _-_ of
this QA Project Plan. Although PCBs can also be determined by this method, the
GC will not be calibrated for these products unless they are observed. The matrix
spike compounds will be the six critical pesticides listed previously in this QA
Project Plan. The surrogates will be tetrachlorometaxylene (not dibutyl-
chlorendate). Detection will be by BCD. Quantitation will be by external
calibration. Acceptance criteria for surrogate recovery will not be determined by
control charts, but must be within a 50-150 percent range. Acceptance criteria for
matrix spike/matrix spike duplicates are those stated in Table _-_ of this QA
Project Plan. Extraction and cleanup procedures are described below...
5.2 NONSTANDARD OR MODIFIED METHODS
Any nonstandard procedure must be described in detail in the form of a Standard Operating
Procedure (SOP) that is appended to the QA Project Plan. Validation data applicable to the
expected samples must also be included. Validation data must demonstrate that the analytes of
interest can be determined without interferences in the expected matrices, and that precision,
accuracy, and detection limits will be adequate for the intended use of the data. The method is
validated only for samples expected from the specific project, and not for general environmental
usage. Once the SOP is written and the validation data are accepted, the method is
validated only for use on that specific project and on the specific sample matrix associated
with that project. This validation process for a project-specific analysis does not constitute
EPA approval for other projects or matrix types.
41
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For Category II projects, all nonstandard methods must be validated prior to approval of the QA
Project Plan.
5.3 CALIBRATION PROCEDURES AND FREQUENCY
This section covers calibration procedures for each analytical or measurement system used to
obtain data for critical measurements. Each description should include the specific calibration
procedure to be used and the frequency of calibration verification.
• In the case of standard EPA-approved methods that include calibration
procedures, a reference to those methods suffices. Simply list the required
frequency and acceptance criteria in a summary table, such as that shown in
Table 7-1. For nonstandard methods that are appended to the QA Project Plan,
reference can be made to the SOP. Describe all other calibration procedures in
detail.
• A list of calibration standards, including source, traceability, and verification
of purity, must be included.
« For process measurements (e.g., flow, mass, etc.) and for chemical or physical
analyses, specify the planned frequency of initial and continuing calibration
checks and the acceptance criteria for all calibration measurements. Table 5-2
illustrates a typical summary for process measurements. For routine,
scheduled calibrations, include the calibration frequency and acceptance
criteria in Section 7.0, along with a summary of QC requirements.
For physical measurements such as temperature and pressure, calibration statements can be quite
brief.
Example: All thermocouples intended for use in the range 50 ° C to 350 ° C will be
calibrated versus an NIST-traceable thermometer at a minimum of two
temperatures, by placing both in an oven simultaneously and noting any
difference between readings. The thermocouple readout must be within 2°C of
the corrected mercury thermometer or the thermocouple device will be replaced
or corrected.
42
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Table 5-2. Typical Summary Table of Calibration Requirements
for Physical Process Measurements
Parameter
Flow rate of dopant
feed
Secondary volume
standard
Secondary time
standard
Temperature
(50-300 'C)
Temperature
(300-800 'C)
Flow rate in stack
Measurement
Classification
Critical
Critical
Critical
Noncritical
Critical
Critical
Device
Mass flow
meter
Dry test
meter
Stopwatch
Thermometer
Thermocouple
Pitottube
and manometer
Calibration
Procedure
Compare to cali-
brated dry test
meter
NIST-traceable
spirometer
NISTtime
base
Comparison to
certified ther-
mometer®
2 temperatures
Comparison to
NIST-calibrated
thermocouple®
2 temperatures
Measure pitot
orifice with NIST-
Frequency
Before/after
field test;
weekly
Before/after
field test
Before field
test
Before project
initiation
Before field
test
Before field
test
Acceptance3
Criteria
5%
2%
.05 sec/min
2'C
5'C
1%
traceable micro-
meter; compare
manometer mark-
ings to NIST-
calibrated meter
stick
a Maximum allowable deviation from standard.
,-/ - IThe te^ f&teel an? WQ¥ Weessariiy te&thatwot&l be employed
'"""- '4'" fora process of Ibis type. _ """
43
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SECTION 6.0
DATA REDUCTION, VALIDATION, AND REPORTING
This section describes how data will be reduced, validated and reported. Deliverables that will
be required from the analytical laboratory must also be specified.
Begin this section with an overall schematic of data flow, such as shown in Figure 6-1. This
flow chart indicates the entire process of data handling, collection, transfer, storage, recovery,
and review for both field and laboratory operations.
6.1 DATA REDUCTION
6.2
• Name the individuals responsible for data reduction.
• Summarize the data reduction procedures that are specific to this project. Data
reduction procedures that are part of standard methods or SOPs cited in Section
5.0 should not be repeated here other than to note any deviations.
« Summarize the planned statistical approach including formulas, units, and
definition of terms. Do not simply reference a "standard text."
• Explain how results from blanks will be treated in calculations.
DATA VALIDATION
Name the individuals responsible for data validation at each stage of data
reduction.
Describe the procedures that will be used for determining outliers. Describe
the guidelines that will be employed for flagging or validating data. (This
requirement is normally satisfied by Section 7.0 with respect to routine quality
control.) In Section 6.0, discuss criteria that are not covered in Section 7.0.
6.3 DATA REPORTING
Name the individuals responsible for the various types of reports.
Indicate the units for each measurement and each matrix, and whether data will
be reported on a wet, dry, or some other reduced basis. If this requirement has
been covered in other sections (e.g., Table 3-1), do not repeat it here.
45
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SAMPLE RECEIPT
SAMPLE
PREPARATION
»
DATA
DATA
DATA-
REPORT
SAMPLE ANALYSIS 1
DATA ACQUISITION
AND REDUCTION
t
I
^ _ J
1
i
RAW DATA ANALYSIS 1 "
BY LAB ANALYSTS | | |
APPROVED? IYES
ANALYTICAL/QC
DATA REVIEW
BY LAB SUPERVISOR
APPROVED? IYES
FINAL DATA REVIEW BY
PROJECT AND Q. A.
MANAGERS
APPROVED? WYES
REPORT
PREPARATION
i
FINAL REPORT
REVIEW BY PROJECT
MANAGER
NO REVIEW RAW DATA,
INDICATED
A
T
1
1
NO REVIEW DATA, TAKE
WHERE INDICATED
i
1
I
1
REVIEW REPORT,
NO te< TAKE CORRECTIVE ACTION.
REANALYZE WHERE
INDICATED
APPROVED? ^ YES
RELEASE REPORT
Figure 6-1. Example of a data reduction, validation, and reporting scheme.
46
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• Indicate data storage requirements that will be expected of the laboratory once
the project is complete. Will the laboratory need to maintain a complete set of
raw data for six months? One year? Five years? Also indicate how long the
actual samples will be stored, in case reanalysis is required.
« List the deliverables that will be expected from the laboratory and from the
field operations. Will the data package include all raw data sufficient to
recalculate any result, if need be? What type of QC data will be reported?
Reporting requirements may vary, depending on the intended use of the data.
« Summarize the data that will be included in the final report. What QC data
will be included? Will analytical and other measurement data be partially
reduced before they are reported, or will all individual measurements be
reported?
Example: The final report will contain the following analytical data:
All analytical results from all primary samples. Data judged to be outliers will be
included, along with a justification for excluding this information from further
interpretation.
All individual results from standard reference materials, independent check
samples, replicates, and matrix spikes, including initial and final concentrations.
Data from the continuous emission monitors will be reported as 15-minute
averages and, when appropriate, will be summarized graphically.
For Category n projects, this section should contain a statement that the final report will include
a QA section that documents QA/QC activities and results. These results must be readily
correlated to the primary data and must clearly indicate the limitations of the data and the range
of validity of the conclusions. The final report should also include a summary of the original QA
objectives, and a statement regarding whether these objectives were met. If QA objectives were
not met, include an explanation of the impact of not meeting the project's QA objectives.
47
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* Indicate data storage requirements that will be expected of the laboratory once
the project is complete. Will the laboratory need to maintain a complete set of
raw data for six months? One year? Five years? Also indicate how long the
actual samples will be stored, in case reanalysis is required.
• List the deliverables that will be expected from the laboratory and from the
field operations. Will the data package include all raw data sufficient to
recalculate any result, if need be? What type of QC data will be reported?
Reporting requirements may vary, depending on the intended use of the data.
• Summarize the data that will be included in the final report. What QC data
will be included? Will analytical and other measurement data be partially
reduced before they are reported, or will all individual measurements be
reported?
Example: The final report will contain the following analytical data:
All analytical results from all primary samples. Data judged to be outliers will be
included, along with a justification for excluding this information from further
interpretation.
All individual results from standard reference materials, independent check
samples, replicates, and matrix spikes, including initial and final concentrations.
Data from the continuous emission monitors will be reported as 15-minute
averages and, when appropriate, will be summarized graphically.
For Category n projects, this section should contain a statement that the final report will include
a QA section that documents QA/QC activities and results. These results must be readily
correlated to the primary data and must clearly indicate the limitations of the data and the range
of validity of the conclusions. The final report should also include a summary of the original QA
objectives, and a statement regarding whether these objectives were met. If QA objectives were
not met, include an explanation of the impact of not meeting the project's QA objectives.
47
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SECTION 7.0
INTERNAL QUALITY CONTROL CHECKS
This section describes all internal quality control (QC) checks that will be used throughout the
project, including field and laboratory activities of all organizations involved. The QC
procedures that are specified should follow from the QA objectives stated in Section 3.0. Thus,
Section 3.0 specifies the analytical requirements, while Section 7.0 describes how these specifi-
cations will be met.
7.1 TYPES OF QC CHECKS
Examples of QC checks that should be considered include the following:
• Samples
- Collocated, split, replicate
• Spikes
- Matrix spikes and matrix spike duplicates
- Spiked blanks
- Surrogates and internal standards
• Blanks
- Sampling, field, trip, method, reagent, instrument
- Zero and span gases
• Others
- Standard reference materials (complex natural materials, pure solutions)
- Mass tuning for mass analysis
- Confirmation on second column for gas chromatographic analyses
- Control charts
- Independent check standard
- Determinations of detection limits
- Calibration standards
- Proficiency testing of analysts
- Any additional checks required by the special needs of your project
Include QC checks for process measurements as well.
49
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Be sure to:
Identify the stage at which replication awl spiking occur, Avoid using
terms such as "sample replicate" without explaining how such replication
will be performed*
^ Ǥ,. ^ ,,. < '"
••v "^ * t?* '• f f f
Explain exactly how Wanks will be prepared* , -
7.2 ITEMS TO INCLUDE
Most information for this section can be summarized in a table, as shown in Table 7-1. This
table should designate the types of QC procedures, required frequencies, associated acceptance
criteria, and corrective action that will occur if the acceptance criteria are not met. When QC
procedures are referenced to a standard method that describes an exact procedure, additional
discussion is not normally needed. However, standard methods lacking exact QC procedures or
nonstandard methods require a detailed explanation, either in this section of the QA Project Plan
or in an appended Standard Operating Procedure.
The tabular format shown in Table 7-1 is also convenient for summarizing routine and ongoing
calibration requkements. If routine calibration is summarized in this section, a reference to that
effect should be included in Section 5.0.
The accompanying text must assure that there are no ambiguities. Particularly troublesome terms
are "duplicate" or "replicate." The text should explain precisely how and when replicates are
taken. Do replicate samples, for instance, refer to samples collected simultaneously or
sequentially in the field; to samples collected at the same sample point but at different times; to
samples that are split upon receipt in the laboratory? The term "QC check sample" must also be
carefully defined. Indicate at which point matrix spiking occurs.
Exact procedures for preparing the numerous kinds of blanks must be described fully in the text.
Never assume that a term such as "field blank" will mean the same to the sampling team or to a
reviewer that it does to you.
50
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Either in this section or in Section 5.0, be sure to specify what compounds or elements will be
employed as matrix spikes and surrogates. Some standard methods recommend surrogate and
matrix spike compounds, which may be incorporated by reference when appropriate. More
typically for RREL projects, some of the matrix spike compounds must be selected on a project-
specific basis.
In some cases, it may also be necessary to provide additional discussion of potential problems
that might be expected with certain QC procedures, along with the proposed solutions. For
example, spiking samples in the field is frequently less reliable and more difficult than spiking in
the laboratory, due to contamination and less controlled conditions. If field spiking is required,
then a discussion of procedures that minimize such problems is also required.
Because standard methods often include extensive QC requirements, it is natural to ask why such
QC procedures must be summarized in this section. Why not simply state that QC will be
performed as required in the method? In some cases, EPA standard methods are sufficiently
complete for this approach, but frequently they are not. First, many EPA-approved methods do
not include specific QC procedures. Second, even the more complete EPA methods allow
options, such as the choice of matrix spike compounds, or the use of either control charts or fixed
acceptance limits. Third, the analytical and measurement requirements of RREL are often
project-specific and require project-specific QC guidelines.
Thus, this section of the QA Project Plan must provide an unambiguous description of QC
procedures. There is no need, however, to repeat in the text any material that is already described
in a standard method.
52
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SECTION 8.0
PERFORMANCE AND SYSTEMS AUDITS
Each Category IIQA Project Plan should describe the QA audits planned for monitoring the
system to be used for obtaining critical measurements. A schedule of all contractor-planned
audits should be included, along with identification of the responsible personnel. This section
should also indicate what audit reports will be generated and who will receive these reports. If
no audits are planned, include an explanation. .
QA audits for RREL projects may include one or more Technical Systems Audits (TSAs),
Performance Evaluation Audits (PEAs), and Audits of Data Quality (ADQs).
A TS A is a qualitative evaluation of all components of the total measurement system, including
technical personnel and QA management. This type of audit includes a careful evaluation of
both field and laboratory QC procedures. TSAs are normally performed before, or shortly after,
measurement systems are operational; they should also be performed on a regularly scheduled
basis throughout the lifetime of the project.
After measurement systems are operational and begin generating data, PEAs are conducted
periodically to determine the bias of the total measurement system(s) or component parts. As
part of a PEA, the laboratory analyzes a performance evaluation sample. QA Project Plans
should also indicate any scheduled participation in other interlaboratory performance evaluation
studies. Long-term projects should provide for regularly scheduled PEAs.
ADQs are retrospective evaluations of data. Typically, a representative portion of the results in
an analytical report is reviewed in detail, starting with raw data and chromatograms, and
proceeding through the calculation of final results. ADQs are often used to resolve specific
questions regarding the quality of a data set.
53
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SECTION 9.0
CALCULATION OF DATA QUALITY INDICATORS
This section describes how data quality indicators will be calculated and reported. As a mini-
mum, equations must be provided for precision, accuracy, completeness, and method detection
limits. In addition, equations must be given for other project-specific calculations, such as mass
balance, emission rates, confidence ranges, etc.
Make sure that this section complements Section 3.0 (QA Objectives) and Section 7.0 (Internal
QC Checks) of the QA Project Plan. Section 3.0 specifies which particular data quality indi-
cators will be employed. Section 7.0 then uses these specific indicators to generate acceptance
criteria. Because groups can use different equations to calculate data quality indicators, Section
9.0 must provide the exact equations to avoid misunderstandings among future data users.
Listed below are general guidelines for calculating the more common data quality indicators.
9.1 COMMON DATA QUALITY INDICATORS
9.1.1 Precision
If calculated from duplicate measurements, relative percent difference is the normal measure of
precision:
- C)
100%
RPD
C2)/2
where:
RPD = relative percent difference
G! = larger of the two observed values
C2 = smaller of the two observed values.
If calculated from three or more replicates, use relative standard deviation rather than RPD:
RSD = (s/y) x 100%
where: RSD =• relative standard deviation
s = standard deviation
y = mean of replicate analyses.
55
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Standard deviation is defined as follows:
s =
n
n - 1
(3)
where: s = standard deviation
y £ = measured value of the fth replicate
y = mean of replicate measurements
n= number of replicates.
For measurements, such as pH, where the absolute variation is more appropriate, precision is
usually reported as the absolute range, D, of duplicate measurements:
where:
D = | m-L - r&2 I
D = absolute range
-L = first measurement
U = second measurement
(4)
The standard deviation, s, given above, can also be used.
9.1.2 Accuracy
For measurements where matrix spikes are used, calculate the percent recovery as follows:
%R = 100% x
S - U
sa
(5)
where:
%R =
O i_r.ii
U =
csa =
percent recovery
measured concentration in spiked aliquot
measured concentration in unspiked aliquot
actual concentration of spike added.
56
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When a standard reference material (SRM) is used:
where:
%R = 100% x
m
srm
%R = percent recovery
Cm = measured concentration of SRM
csrm = actual concentration of SRM.
9.1.3 Completeness
Completeness is defined as follows for all measurements:
(6)
%C = 100% x
n
(7)
where: %c = percent completeness
V = number of measurements judged valid
n = total number of measurements necessary to achieve a specified level of
confidence in decision making.
Note: This more rigorous definition of completeness is an improvement on the conventional
definition in which "n" is replaced by "T," the total number of measurements.
9.1.4 Method Detection Limit (MDL)
MDL is defined as follows for all measurements:
i-l, l-o-O. 99)
(8)
where: MDL
s
t(n-l,l-o=0.99)
method detection limit
standard deviation of the replicate analyses
students' t-value for a one-sided 99% confidence level
and a standard deviation estimate with n-1 degrees of freedom.
57
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9.2 PROJECT-SPECIFIC INDICATORS
RREL projects frequently incorporate data quality indicators in addition to those discussed in the
previous sections. The following is an example'of a project-specific data quality indicator:
Example: Mass balance calculation for a soil washing process being tested with
POP-contaminated soils. Mass balance (MB) will be calculated according to
(9)
where MQUt and Min denote the total mass of POP in the output and input
streams for each test condition.
58
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SECTION 10.0
CORRECTIVE ACTION
Each QA Project Plan must incorporate a corrective action plan. This corrective action plan must
include the predetermined acceptance limits, the corrective action to be initiated whenever such
acceptance criteria are not met, and the names of the individuals responsible for implementing
the plan.
Routine QC procedures already included in Section 7.0 need not be repeated here. This section
is reserved primarily for nonroutine corrective action not described elsewhere. Nonroutine
corrective action may result from common monitoring activities, such as:
• Performance evaluation audits,
• Technical systems audits, and
• Interlaboratory comparison studies.
It may also arise from conditions unique to specific projects, as seen below.
Example: Bio-oxidation study of hazardous waste in municipal sludge carried
out over a one-year period.
The prime contractor's Quality Assurance Manager will submit to the laboratory
a blind performance evaluation (PE) sample containing some or all of the target
analytes before any analytical work begins and on a monthly basis thereafter.
The average percent recovery of all target analytes must be between 80 and 120
percent, with no outliers less than 50 or greater than 150 percent. If these limits
are exceeded, analytical work will stop until the problems are identified and
solved. Before work is restarted, another blind PE sample must be analyzed and
results must meet the acceptance criteria. Results of these PE samples will be
included in the final report.
59
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SECTION 11.0
QUALITY CONTROL REPORTS TO MANAGEMENT
This section of a Category IIQA Project Plan identifies the individuals responsible for QA
reports, and describes the type and frequency of reports (weekly oral presentations and discus-
sions, monthly written reports, etc.) that will be used to keep project management informed. As
a minimum, such reports include:
« Changes in the QA Project Plan
• Summary of QA/QC programs, training, and accomplishments
• Results of technical systems and performance evaluation audits
• Significant QA/QC programs, recommended solutions, and results of correc-
tive actions
• Data quality assessment in terms of precision, accuracy, representativeness,
completeness, comparability, and method detection limit
• Discussion of whether the QA objectives were met, and the resulting impact on
decision making
• Limitations on use of the measurement data.
Managers receiving these detailed reports will then be able to monitor data quality easily
and effectively.
61
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SECTION 12.0
REFERENCES
References, if any, can be included in the body of the text, as footnotes, or collected in this
section. If a reference is not readily available, attach a copy to the QA Project Plan. References
must uniquely identify the cited material. In particular, when citing various compendia of
standard methods published by the EPA, ASTM, American Public Health Association, etc., be
sure to include the edition number, since such methods can change substantially from one edition
to the next.
For example, the following are references applying to Table 5-1 of this document.
1. American Society for Testing and Materials. Annual Book of Standards. ASTM.
Philadelphia, PA. Parts 14 and 19 (updated yearly).
2. U.S. Environmental Protection Agency. "A Procedure for Estimating Monofilled Solid
Waste Leachate Composition" Technical Resource Document SW-924, 2nd ed.
Hazardous Waste Engineering Research Laboratory, Office of Research and
Development. Cincinnati, OH, and Office of Solid Waste and Emergency Response.
Washington, D.C., 1986.
3. American Nuclear Society. ANSI/ANS-16.1-1988. American National Standard
Measurement of the Leachability of Solidified Low-Level Radioactive Wastes by a Short-
Term Test Procedure. American Nuclear Society. LaGrange Park, IL, 1986.
4. U.S. Environmental Protection Agency. Office of Solid Waste. Test Methods for
Evaluating Solid Waste, 3rd ed. Available from U.S. Government Printing Office.
Washington, D.C., 1986.
5. Alford-Stevens, A., T. A. Bellar, J. W. Eichelberger, and W. L. Budde. Method 680,
Determination of Pesticides and PCS in Water and Soil/Sediment by Gas
ChromatographylMass Spectrometry. Available from the U.S. Environmental Protection
Agency. Cincinnati, OH, 1985.
6. Klute, A. (Ed.). Methods of Soil Analysis, Part I. American Society of Agronomy.
Madison, WI, 1986.
63
•&U.S. GOVERNMENT PRINTING OFFICE: 1993 - 75O-002/60I84
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