DSHW-2006-002880 - 0901a0688013e873

Changes to the original draft Quality Assurance Project Plan for Emission
Characterization of Open Burning Waste Propellant Materials.
1) CS ortho-chlorobenzylidene malono-nitrile removed from page iv (List of
Abbreviations) ^^j^p DELIVERED
Page 13-2 APR 2 7 2006
131 Field Changes . UTAH DIVISION OF
13.1 Field Changes SOLID & HAZARDOUS WASTE
The URS PM is responsible for all invesfigafive acfivifies. In this role, the URS PM at
times will adjust the field program to accommodate project-specific needs. When it
becomes necessary to modify this program, the URS PM will notify the ATK PM and
URS QAO.
13.2 Laboratory Data
The laboratory will report the types of out-of-control occurrences, how these occurrences
are documented, and who is responsible for correction and documentafion. Generally,
corrective acfion will be inifiated by out-of-control events such as: poor analysis
replication, poor recovery, instrument calibration problems, blank contamination, etc.
Appropriate laboratory personnel will initiate correcfive acfion at any fime during the
analytical process when deemed necessary based on analytical judgment, method
requirements, or when QC data indicate a need for action. Corrective actions may
include, but are not limited to:
Re-analysis
Calculation checks
Instrument recalibration
Preparation of new standards/blanks
Re-extracti on/di gesti on
Dilution
Application of another analysis method
Additional training of analysts
The following items must be documented for out-of-control incidents so that correcfive
action may be taken to set the system back "in control." These items will typically
constitute a corrective action report that is signed by the laboratory director and the
laboratory QA contact:
• Where the out-of-control incident occurred,
• When the incident occurred and was corrected.
• Who discovered the out-of-control incident,
• Who verified the incident, and
• Who corrected the problem.
The laboratory will be responsible for re-sampling and re-analysis costs associated with
gross failure to meet laboratory QA/QC objecfives. In consultafion with the
Environmental Contractor Project Chemist, wither the Environmental Contractor PM or
the QAM may inifiate a request for corrective action.
The invesfigafion report (typically the Letter Report of Findings) will address the status
and results of the sampling and associated QA/QC process for each data generation
activity. The report will typically address and document the following QA/QC items:
Measurement system performance and data quality. This secfion of the report will
present the assessment of precision, accuracy, and completeness in relation to the
specified field and laboratory data acceptance criteria and data assessment procedures.
• Audit findings and correcfive action measures. This section of the report will
present the effecfiveness ofthe data QA program and implementafion, and include
a summary of findings and observations resulfing from audits, as appropriate.
• Final laboratory QA assessment. This section of the report will present a
summary of the laboratory results and performances based upon the data
validafion process.
• The roufine evaluafions of data quality described throughout this QAPP will be
documented and filed along with the data in the project files. A summary of data
quality and the results of checking the sample data against the quality assurance
objecfives will be presented in the final report that presents and summarizes the
data generated.
Reporting nonconformances and field changes to management is discussed in Section 13.
An effective QC program should include fonnal and frequent reports to management and
technical staff of progress in the on-going implementation of the QC plan. At a
minimum, the following parties should receive updates on project status: 1) ATK Project
Manager; 2) URS PM; 3) URS QAO; and 4) other technical staff.
Table A.6, Appendix A List of Analytes, page A 4 has been removed. Table A.6 is now
Other Target Compounds.
Table A.6
Energetics Target Analyte List (EPA SW-846 Draft Method 8330/8095).
Energetics
1,3-Dinitrobenzene
1,3,5-Trinitrobenzene
Nitrobenzene
Nitroglycerine
2,4-Dinitrotoluene
2,6-Dinitrotoluene
2-Nitrotoluene
4-Nitrotoluene
2,4,6-Trinitrotoluene
Tetryl
2-Amino-4,6-dinitrotoluene
4-Amino-2,6-dinitrotoluene
RDX"
PETN"
HMX'
3-Nitrotoluene
"Cyclolrimelhylenetiinitramine; Penlaerylhritoleielranilrale; 'Cyclotetramethylene tetranitramine.
PRELIMINARY DRAFT
QUALITY ASSURANCE PROJECT PLAN
for
EMISSION CHARACTERIZATION OF
OPEN BURNING
WASTE PROPELLANT MATERIALS
Prepared for:
ATK Launch Systems
Promontory Facility
Brigham City, Utah
Prepared by:
URS Corporafion
8181 East Tufts Avenue
Denver, Colorado 80237
April 2006
Preliminary Draft
TABU OF CONTENTS
Section 1
Section 2
Section 3
Section 4
Project Description 1-1
1.1 Background 1-1
1.2 Testing Approach Summary 1-1
1.2.1 Open Detonafion Open Buming Improved Tesfing
Chamber 1-1
1.3 Test Procedures 1-2
Project Organization and Responsibility 2-2
2.1 ATK Launch Systems 2-3
2.2 URS Project Manager 2-3
2.3 URS Quality Assurance Officer 2-3
2.4 URS Technical Specialist and Field Support Staff 2-4
2.5 UTAH Department of Environmental Quality 2-4
2.6 Analyfical Laboratories 2-4
Quality Assurance Objectives for Measurement Data 3-1
3.1 Intended Data Usage 3-1
3.2 General Quality Assurance Considerafions 3-1
3.2.1 Precision 3-1
3.2.2 Accuracy 3-2
3.2.3 Representafiveness 3-2
3.2.4 Comparability 3-2
3.2.5 Completeness 3-2
3.2.6 Sensifivity 3-3
Sample Selection and Collection 4-1
4.1 Sampling Methods 4-1
4.1.1 Total Suspended Particulate 4-1
4.1.2 Particulate Metals Analysis 4-1
4.1.3 PmlOandPm2.5 4-2
4.1.4 Carbonyls 4-2
4.1.5 Semivolatile Organic Compounds 4-2
4.1.6 Dioxins/Furans 4-2
4.1.7 Volafile Organic Compounds and Tracer Gas Analysis 4-3
4.1.8 Hydrogen Chloride/Chlorine Analysis 4-3
4.1.9 Continuous Emission Monitoring 4-3
4.2 Sampling Preparafion, Quality Control, and Measurement 4-3
4.2.1 Calibrafion of Field Instrumentafion 4-3
4.2.2 Preparation of Sampling Equipment and Containers and
Field Decontaminafion 4-4
4.2.3 Field Blanks, Duplicates, Splits, and Quality Control 4-4
4.2.4 Preservation, Transportation, and Storage of Samples 4-5
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TABIi OF CONTENTS
4.3 Documentation 4-5
Sections Sample Analysis 5-1
5.1 Field Operafions 5-1
5.1.1 Sample Container Labeling 5-1
5.1.2 Sample Custody (Custody Seals, Chain-Of-Custody, and
Analysis Request) 5-1
5.2 Laboratory Operafions 5-1
Section 6 Laboratory Calibration Procedures and Frequency 6-1
Section? Analytical Procedures 7-1
Section 8 Data Reduction, Validation, and Reporting 8-1
8.1 Data Reducfion 8-1
8.2 Data Validafion 8-1
8.2.1 Field Data Validafion 8-1
8.2.2 Laboratory Data Reduction and Review 8-2
8.2.3 Independent Review 8-3
8.3 Data Reporting 8-8
Section 9 Field and Laboratory Quality Control Checks 9-1
Section 10 Performance and System Audits 10-1
Section 11 Preventive Maintenance 11-1
11.1 Field Equipment 11-1
11.2 Laboratory Equipment 11-1
Section 12 Data Assessment Procedures 12-1
12.1 Precision 12-1
12.2 Accuracy 12-1
12.3 Completeness 12-1
12.4 Representativeness 12-2
12.5 Comparability 12-2
Section 13 Corrective Action 13-1
13.1 Field Changes 13-2
13.2 Laboratory Data 13-2
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TABIE OF CONTENTS
Section 14 Quality Assurance Reports to Management 14-1
Section 15 Miscellaneous 15-1
15.1 Tumaround Time 15-1
Section 16 References 16-1
List of Tables
Table 1-1 Sampling Analysis Method Lists
Measurement Quality Objectives
Maximum Reporting Limits by Analytical Method
Table 3-1
Table 3-2
Table 3-3 Lisfing of Letters of Instructions for Smoke, Pyrotechnics, and Exploding
Ordnance Tests
Table 4-1 Sample Preservations and Holding Times Requirements
List of Figures
Figure 1-1 ODOBi Test Facility at DPG
Figure 2-1 Project Organizational Chart
List of Appendices
Appendix A Lists of Analytes
Appendix B Letter of Instructions
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List Of Abbreviations
ATK ATK Launch Systems
CDD chlorinated dibenzodioxin
CDF chlorinated dibenzofuran
CEM continuous emission monitor
CFR Code of Federal Regulations
CI2 chlorine
CO carbon monoxide
COC chain of custody
CO2 carbon dioxide
CVAAS cold vapor atomic absorption spectroscopy
DNPH 2,4-dinitrophenylhydrazine
DoD U.S. Department of Defense
DoT U.S. Department of Transportafion
DPG U.S. Army Dugway Proving Ground
DQO Data Quality Objecfive
DStrW Division of Solid and Hazardous Waste
ECD electron capture detector
EPA U.S. Environmental Protection Agency
FID fiame ionization detecfion
GC/MS gas chromatography/mass spectroscopy
HCl hydrogen chloride
HMX octahydro-1,3,5,7-tetrani tro-1,3,5,7-tetrazoci ne
HpCDD Heptachlorodibenzo-p-dioxin
HPLC high-performance liquid chromatography
HRGC high-resolufion gas chromatography
HRMS high resolution mass spectrometry
HpCDF Heptachlorodibenzofuran
HxCDD Hexachlorodibenzo-p-dioxin
HxCDF Hexachlorodibenzofuran
lAW in accordance with
ICAP inductively coupled argon plasma
LCS laboratory control sample
LOl letter of instrucfion
MDL method detecfion limit
MS/MSD matrix spike/matrix spike duplicate
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List Of Abbreviations
NEW net explosive weight
NOx nitrogen oxides
OB open buming
ODOBi Open Detonafion Open Bum-improved
OCDD octachlorodibenzo-p-dioxin
OCDF octachlorodibenzofuran
PARCC precision, accuracy, representafiveness, comparability, and completeness
PeCDD pentachlorodibenzo-p-dioxin
PeCDF pentachlorodibenzofuran
PETN pentaerythritoltetranitrate
PM Project Manager
PM2.5 particulate matter smaller than 2.5 microns
PMio particulate matter smaller than 10 microns
PUF polyeurethane foam plug
QA quality assurance
QAO Quality Assurance Officer
QC quality control
QAPP Quality Assurance Project Plan
RCRA Resource Conservation and Recovery Act
RDX hexahydro-1,3,5-trinitro-l,35-triazine
REC record of environmental consideration
RL reporting limit
RPD relative percent difference
RSD relative standard deviation
SDG sample delivery group
SFG sulfur hexafluoride
SO2 sulfur dioxide
SOP standing operating procedure
SRM standard reference material
SVOC semivolafile organic compound
TCDD tetrachlorodibenzo-p-dioxin
TCDF tetrach I orodi ben zof uran
TIC tentatively identified compound
TM Task Manager
TSP total suspended particulate [matter]
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List Of Abbreviations ^
URS sampling and analysis contractor (formerly Radian Int.)
UV ultraviolet
VOC volafile organic compound
WDTC West Desert Test Center
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SECTIONONE Project Description
1.1 BACKGROUND
ATK Launch Systems (ATK) operates several facilifies within the State of Utah for the
production of solid rocket motors. Rocket motors are produced for a variety of customers and
generally contain either Class 1.1 or Class 1.3 propellant as defined by the Department of
Transportation (DoT).
As part of these facilities, ATK operates three different sites for open buming (OB) of explosive
waste generated during production of these motors. These open bum units are currently
managed as interim status Resource Conservafion and Recovery Act (RCRA) units with
preparafions underway for obtaining full RCRA Subpart X permits. The Utah Department of
Environmental Quality Division of Solid and Hazardous Waste (DSHW) requires human health
and ecological risk assessments as part of the Subpart X permitting process.
Understanding emissions from these units is a necessary component for the risk assessment
process. In 1997, ATK commissioned the U.S. Army to test Class 1.1 materials at the
BANGBOX facility located at the Dugway Proving Grounds in westem Utah. Materials tested
included Class 1.1 propellants along with contaminated materials such as cloth and paper wipes,
plastics, and cleaning items. The tests detennined emission factors for airbome pollutants
produced when these materials are bumed. These emission factors are used with air dispersion
modeling to help determine downwind impact from open buming.
ATK sfill requires emission factors for the other major class of propellant (Class 1.3) produced at
the Utah facilities. Addifional characterization tests are planned in the near future for Class 1.3
materials at the Dugway facilifies. This Quality Assurance Project Plan (QAPP) is to provide the
quality assurance/quality control (QA/QC) required to identify and quanfify emissions from open
buming of these materials.
1.2 TESTING APPROACH SUMMARY
This Quality Assurance Project Plan (QAPP) is to provide the quality assurance/quality control
(QA/QC) required to identify and quanfify the emissions resulting from the open buming of three
test materials using the Open Detonafion Open Buming Improved (ODOBi) tesfing chamber.
Three test materials will be studied. The first material will be 100% Class 1.3 propellant. The
other two test materials will consists of a mixture of Class 1.3 propellant blended with different
percentages of materials such as cloth, paper, paper wipes, plasfics, and cleaning items.
1.2.1 Open Detonation Open Burning Improved Testing Ciiamber
The ODOBi site is located in the west desert area of the West Desert Test Center/Dugway
Proving Ground. The ODOBi test facility, shown in Figure 1-1, includes a test chamber with a
removable stack. The ODOBi test chamber and stack are made of 2.54-cm (1-in) and 0.63-cm
(0.25-in) thick steel, respecfively. The chamber consists of top and bottom sections that, when
bolted together, give an ellipsoidal shape and a volume of approximately 36 m'^. An altemate
configuration is to replace the stack with a ventilafion cover. The venfilafion cover is basically a
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SECTIONTWO Project Organization and Besponsidiiity
framework of angle iron designed to keep shrapnel from the test within the chamber and prevent
overpressure by releasing the gases at the fime of deployment.
Test items are placed in the chamber or suspended in the center and remotely inifiated. Sample
probes are inserted into the test chamber to convey the combusfion products to sampling trains
and instruments for identificafion and quantificafion. There are 21 sampling ports in the
chamber wall. The ports are used for manual method sampling: two ports for sampling TSP, one
port for PM10/PM2.5, two ports for SVOCs, two ports for dioxins/furans, two ports for HCI/CI2,
and one port for VOCs, carbonyls and tracer gas sampling. One port is used for confinuous
monitoring of CO, CO2, NOx, and SO2. An addifional port has been installed for tracer gas
injection. The sample media is located immediately outside the chamber. An electrical firing
circuit remotely deploys the test items and releases the SFG tracer gas. After sampling has
concluded, the chamber door is opened to release the remaining gases. The chamber is then
prepared for the next test.
1.3 TEST PROCEDURES
Confinuous air analyzers will be used on-site to monitor each test bum. Addifional air emissions
samples will be collected and ship off-site for analytical tesfing.
Detonafions will be performed using various conventional means, depending on the test item
characterisfics. The quantity of material will be chosen to achieve a net explosive weight per
trial.
The ATK materials to be tested are placed in the center of the chamber. The tracer gas is
released into the chamber immediately after the deployment of the items. Samplers to measure
total suspended particulate (TSP) matter, metals, particulate matter smaller than 10 microns
(PMio), particulate matter smaller than 2.5 microns (PM2.5), SVOCs, dioxins/furans, HCl and
CI2 are located just outside the chamber (except PM10/PM2.5, which is inside the chamber) and
connected to the chamber by short probes. The sampling rate is monitored and recorded. Two
other probes convey gases from the chamber into two separate manifolds located in a bunker
adjacent to the test chamber. One manifold distributes the gases to the continuous analyzers
(NOx, CO, CO2, SO2, and HCl), and the other manifold distributes gases to the VOCs, tracer, and
carbonyls sampling lines in the bunker.
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SECTIONTWO Proiect Organization and Responsibiiity
The project organizafion chart is shown in Figure 2-1.
2.1 ATK LAUNCH SYSTEMS
The ATK Launch Systems (ATK) Project Manager is responsible for the contracting of URS,
Inc. and will oversee and approves work performed by URS in support of the Emission
Characterizafion of Open Buming Waste Propellant Materials Project.
2.2 URS PROJECT MANAGER
The URS Project Manager (PM) is responsible for overall project management, including
planning, communication with clients and regulators, coordinafion of data acquisition/field
acfivities, the health and safety of project participants, and implementafion ofthe project quality
assurance (QA) program as given in this QAPP. The PM works directly with, and is advised by,
the URS Quality Assurance Officer (QAO) in the implementation of this plan.
Additional responsibilifies include engineering capabilifies, safety, and test report preparafion.
2.3 URS QUALITY ASSURANCE OFFICER
The URS QAO communicates with the URS PM, and Task Managers (TMs) on project QA and
additionally has direct reporting access to the Corporate QA Officer on quality-related matters.
The QAO is responsible for the development, implementafion, and maintenance of the
comprehensive project QA program. The QAO communicates with all levels of program and
project management to assure that a quality product is prepared for submittal. Specific
responsibilifies ofthe QAO are as follows:
• Prepare the project-specific QAPP and provide QA/guidance to the TMs in the development of
any required task-specific instmctions.
• Respond to QA needs, resolve problems, and answer requests for guidance or assistance.
• Review audit and nonconformance reports to determine areas of poor quality or failure to
adhere to established procedures.
• Confer with an audited enfity on the steps to be taken for corrective actions and track
nonconformance until correction. Confer with the URS PM to resolve an inadequate corrective
action.
• Maintain, with the concurrence of the ATK PM, URS PM, URS Health and Safety Manager
the authority to stop work on any task where a critical situation requires slopping work to
prevent further discrepancies, danger to personnel, loss of data, or other problems.
• Establish and maintain a filing system (including LOIs and SOPs) and all correspondence
between ATK and URS for auditing purposes.
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SECTIONTWO Project Organization and Responsibiiity
• Serve as the official contact for all QA matters with the ATK Project Manager.
• Provide training on QA policies, procedures, and methodology as required.
2.4 URS TECHNICAL SPECIALIST AND FIELD SUPPORT STAFF
URS will provide the technical specialists as required to prepare and finalize the test plan, the
health and safety plan (describes the dufies and responsibilities of the assigned URS Health and
Safety Manager) and test report in accordance with the contract and this QAPP. URS will also
provide the test personnel required to execute the approved test plan.
2.5 UTAH DEPARTMENT OF ENVIRONMENTAL QUALITY
Will provide regulatory oversight of the program, and will review and provide comments on the
test plan, QAPP, and test report.
2.6 ANALYTICAL LABORATORIES
Commercial laboratories will analyze sample media after testing. As of this version of the QAPP
the specific labs have not been identified. The listing of the required analytical testing and
associated methodologies are provided in Table 1-1.
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SECTIONTHREE Quaiity Assurance Obiectives for Measurement Data
The overall QA objective for this project is to develop and implement procedures for obtaining
and evaluafing data that meet the DQOs to assure or confirm that the required decisions can be
made at a specified and acceptable level of uncertainty. The procedures defined in this QAPP
and Letter of Instmcfions are established to assure that field measurements, sampling methods,
and analytical data provide infomnation that is comparable and representative of the actual field
conditions, and that the data generated are technically defensible.
The analyfical QA objectives are defined in terms of sensifivity and the PARCC parameters of
precision, accuracy, representafiveness, completeness, and comparability. The primary goal of
this QAPP is to define procedures that assure the quality and integrity of the collected samples,
the representafiveness of the results, the precision and accuracy of the analyses, and the
completeness of the data. Data that meet the QA objecfives and goals will be deemed
acceptable. Data that do not meet objecfives and goals will be reviewed on a case-by-case basis
to ascertain usability.
3.1 INTENDED DATA USAGE
To achieve project DQOs, this QAPP and associated LOIs are designed to assure that a sufficient
number of samples will be collected using technically valid scienfific procedures. Utilization of
the QAPP requires implementation of procedures for obtaining and evaluating data in a manner
that will result in a quanfitafive or qualitafive representation of the PARCC parameters. The
parameters of precision, accuracy, and completeness provide a quantitative measure of the
quality of the data collected using the ODOBi. The parameters of representafiveness and
comparability utilize documentafion ofthe ODOBi and laboratory procedures to qualitafively
evaluate the data. Specificafion of required sensifivity levels is also an integral component of
obtaining data that will safisfy the DQOs. Following the collection and analysis of the samples,
a determinafion will be made whether the DQOs established for the data-collecfion effort were
satisfied.
3.2 GENERAL QUALITY ASSURANCE CONSIDERATIONS
Data quality indicators are defined in terms of the PARCC parameters in the following
subsections. The assessment of the data quality indicators is necessary to determine data
usability. The established precision and accuracy limits are listed in Table 3-1. The laboratory
must meet the QC acceptance criteria presented in Table 3-1. The method duplicate (MD),
matrix spike (MS), and matrix spike duplicate (MSD) limits given in Table 3-1 will be used for
data verificafion. The method detection limits (MDLs) and reporting limits (RLs) for each
analytical method to be contracted by an off-site commercial laboratory are provided in Table 3-
2.
3.2.1 Precision
Precision is a measure of mutual agreement among replicate (or between duplicate) or co-located
sample measurements of the same analyte. The closer the numerical values of the measurements
are to each other, the more precise the measurement. Precision for a single analyte will be
expressed as a relafive percent difference (RPD) between results of field duplicate samples,
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SECTIONTHREE Quaiity Assurance Objectives for Measurement Data
laboratory duplicate samples, or MSD samples for cases where both results are sufficiently large
(i.e., > five times the RL). Otherwise, the absolute difference between the results is compared to
a factor of the RL (the RL is used for nondetect results). In addifion, the lab will assess precision
by conducting roufine instrument checks to demonstrate that operafing characterisfics are within
predetermined limits.
3.2.2 Accuracy
Accuracy is a measure of bias in a measurement system. The closer the value of the
measurement agrees with the true value, the more accurate the measurement. This will be
expressed as the percent recovery of a surrogate, LCS analyte, MS analyte, or of a standard
reference sample.
3.2.3 Representativeness
Representativeness is a qualitative parameter that expresses the degree to which sample data
accurately and precisely represents characteristics of a population, parameter variafions at a
sampling point, or an environmental condifion. The design of, and rafionale for, the sampling
program (in terms of the purpose for sampling, selecfing the sampling locafions, the number of
samples to be collected, the ambient conditions for sample collecfion, the frequencies and fiming
for sampling, and the sampling techniques) assures that the environmental condition has been
sufficiently represented.
3.2.4 Comparability
Comparability is a qualitafive parameter expressing the confidence with which one data set can
be compared to another. Data sets will be considered comparable only when precision and
accuracy are considered acceptable during data validation. Sample data will be collected and
reported in order to be comparable with other measurement data for similar samples and sample
condifions. This goal will be achieved through following standard procedures to collect and then
analyze representative samples and through reporting analytical results in appropriate and
consistent units. Each analytical procedure selected from among the acceptable opfions will be
used for all investigative analyses, unless rafionale is provided for any alteration. In essence,
comparability will be maintained by consistency in sampling conditions, selecfion of sampling
procedures, sample preservafion methods, analyfical methods, and data reporting units.
3.2.5 Completeness
Completeness is a measure of the number of valid measurements obtained in relation to the total
number of measurements planned. The closer the numbers are, the more complete the
measurement process. Completeness will be expressed as the percentage of valid or usable
measurements to planned measurements. An objecfive of the field-sampling program is to
establish the quanfity of data needed to support the invesfigafion. This will be achieved by
obtaining samples for all types of analyses required at each individual location, a sufficient
volume of sample material to complete the analyses, samples that represent all possible
contaminant situafions under investigation, and samples at critical data locations, such as
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SECTIONTHREE Quaiity Assurance Objectives for Measurement Data
background and control samples. The overall completeness goal for investigafive acfivifies is
80% for each sampling event. The effect of any rejected data on project objecfives will be
evaluated in order to assess the need for recollection or reanalysis of these samples.
3.2.6 Sensitivity
To evaluate the ufility of the data for comparison to numeric standards or screening it is
important that the sensifivity ofthe methods ufilized is acceptable. This QAPP specifies the use
of routine and commercially available U.S. Environmental Protection Agency (EPA) approved
analytical methods. In general, these methods provide the necessary level of sensitivity. Table
3-2 and 3-3 provide the required RLs relative to the numeric standards and/or screening criteria
to be used for data collected under this QAPP.
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SECTIONFOUR Sampie Seiection and Coiiection
Air emissions samples generated from buming the ATK test materials using the ODOBi test
chamber will be collected on-site and shipped off-site for analyfical testing.
The ODOBi test chamber and stack are made of 2.54-cm (1-in) and 0.63-cm (0.25-in) thick steel,
respecfively. The chamber consists of top and bottom secfions that, when bolted together, give
an ellipsoidal shape and a volume of approximately 36 m". An altemate configuration is to
replace the stack with a ventilafion cover. The venfilafion cover is basically a framework of angle
iron designed to keep shrapnel from the test within the chamber and prevent overpressure by
releasing the gases at the time of deployment.
Test items are placed in the chamber or suspended in the center and remotely inifiated. Sample
probes are inserted into the test chamber to convey the combustion products to sampling trains
and instruments for idenfification and quanfification. There are 21 sampling ports in the
chamber wall. The ports are used for manual method sampling: two ports for sampling TSP, one
port for PM10/PM2.5, two ports for SVOCs, two ports for dioxins/furans, two ports for HCI/CI2,
and one port for VOCs, carbonyls and tracer gas sampling. One port is used for continuous
monitoring of CO, CO2, NOx, and SO2. An additional port has been installed for tracer gas
injection. The sample media is located immediately outside the chamber. An electrical firing
circuit remotely deploys the test items and releases the SFo tracer gas. After sampling has
concluded, the chamber door is opened to release the remaining gases. The chamber is then
prepared for the next test.
All field-sampling methods that will be used during these tests are based on EPA methodologies
[see letters of instmction (LOIs) in Appendix B for references to corresponding methods].
However, in order to be used in the ODOBi test chamber, some procedure modifications are
needed (e.g., remote operation and relafively short sampling period). Target sampling fimes for
each type of sampler are presented in the LOIs.
4.1 SAMPLING METHODS
A general summary of methods to be used to support this invesfigation is provided in the
following subsections and presented in Table l-l. A list of the target analytes is presented in
Appendix A.
4.1.1 Total Suspended Particulate
The concentrafion of Total Suspended Particulate (TSP) is determined gravimetrically in
accordance with (lAW) 40 Code of Federal Regulafions (CFR) 60 (see DPG LOI-101 in
Appendix B) Method 5. Each filter is weighed before and after testing to determine the net
weight gain of particles. The concentrafion of the TSP is the mass of particles collected on the
filter divided by the volume of air sampled, corrected to standard temperature and pressure
condifions.
4.1.2 Particulate Metals Analysis
The quartz/glass-fiber filter used for the determinafion of TSP will also be used for the
determination of particulate metals. After the filter is weighed to determine the TSP
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concentrafion, the enfire filter will be digested with concentrated acid lAW EPA Method 29 (see
DPG LOI-107 in Appendix B). The digestate will be analyzed for mercury, using cold vapor
atomic absorpfion spectroscopy (CVAAS) modified Method 7470/7471 and all other metals by
inducfively coupled argon plasma (ICAP) emission spectroscopy lAW Method 6010 (DPG LOl-
107 in Appendix B). Appendix A presents the list of target metals.
4.1.3 PMIO AND PM2.5
PMio and PM2.5 will be sampled by using two cyclones and a filter lAW 40 CFR 51 Method
201A (see DPG LOI-304 in Appendix B). The sample is collected from the chamber using a
short probe. The gases then pass through two cyclones in series. The first cyclone removes
particles larger than 10 microns. Particles that pass through the first cyclone, but not the second,
are between 10 and 2.5 microns. PM2.5pass through the second cyclone. Each fracfion will be
measured gravimetrically. The concentrafion of PMio and PM2.5 will be computed as the mass of
collected particles in each range, divided by the volume of air sampled, corrected to standard
conditions.
4.1.4 Carbonyls
The concentrafion of formaldehyde and other TO-11 carbonyl compounds will be determined
lAW EPA Compendium Method TO-11 A (see DPG LOI-109 in Appendix B). A sample stream
of gas will be drawn through tubes that contain sorbent and are coated with 2,4-dinitrophenyl-
hydrazine (DNPH). The tubes will then be capped and shipped to the laboratory for analysis,
using high-performance liquid chromatography with an ultraviolet absorption detector. The
VOC method (see DPG LOI-104 in Appendix B) will be used to quanfify other aldehydes.
4.1.5 Semivolatile Organic Compounds
Semivolatile organic compounds (SVOCs) are measured based on the procedure in SW-846
0010 (see DPG LOI-301 in Appendix B). Sorbent cartridges for the determination of SVOCs in
air will be analyzed based on SW-846 Method 8270C (see DPG LOL301 in Appendix B) plus
tentafively identified compounds (TICs). The samples are collected by using a combinafion
quartz filter/adsorbent cartridge. The cartridge contains XAD-2 polymeric resin beads. After
sampling, the filters and adsorbent cartridge will be extracted with solvent. The effiuent is then
analyzed by gas chromatography (GC) equipped with mass spectrometry (MS) detecfion.
TICs will be reported when the response of the compound is equal or greater than 10 percent of
the response of the associated intemal standard and the mass spectra library match of the TIC
compound is greater than or equal to a hit quality index factor of 90 or greater. Hard copy TIC
reports and spectra will be placed in the appropriate data package.
4.1.6 Dioxins/Furans
Dioxins/furans are measured based on the procedure in 40 CFR 60 Method 23 (see DPG LOl-
301 in Appendix B). Sorbent cartridges for the determination of dioxins/furans in air are
analyzed based on SW-846 Method 8290 (see DPG LOL301 in Appendix B). The samples are
collected using a quartz filter and adsorbent cartridge. The cartridge contains XAD-2 resin
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beads. After sampling, the filters and adsorbent cartridge are extracted with solvent. The
effluent is analyzed by high-resolution GC (HRGC) equipped with high-resolufion MS (HRMS)
detecfion. Appendix A presents the target isomers for this determination.
4.1.7 Volatile Organic Compounds and Tracer Gas Analysis
Gas samples collected in 6-L canisters will be analyzed for volafile organic compounds (VOCs)
by using a GC and multiple detectors as described in EPA Compendium Method TO-14A (see
DPG LOI-104 in Appendix B). Most compounds will be identified via GC/MS full scan. Light
hydrocarbons (e.g., acetylene, ethane, ethylene, and propane) will be idenfified using GC/fiame
ionizafion detection (FED). The target analytes are listed in Appendix A. Total nonspeciated
VOCs will be determined by using appropriate secfions of EPA Compendium Method TO-12
(see DPG LOI-104 in Appendix B). A GC with an electron capture detector will be used to
analyze for the tracer gas SFo in gas samples collected in LO-L canisters.
4.1.8 Hydrogen Chloride/Chlorine Analysis
HCI/C12 will be measured by using the EPA Method 26 sampling train (see DPG LOI-108 in
Appendix B). Gas will be bubbled through dilute solutions of sulfuric acid and sodium
hydroxide in series. The HCl is absorbed in the sulfuric acid solufion, while the CI2 passes
through and is absorbed by the sodium hydroxide solufion. The chloride concentrafion in the
liquid solutions will be measured with an ion chromatograph. For test items that contain
significant amounts of chlorine, the particulate filter from the sampling train will be recovered
and sent to the laboratory for analysis. The filter will be extracted using deion-ized water and the
chlorine concentration will be measured with an ion chromatograph. HCl will also be measured
using CEMS as described in secfion 4.1.9.
4.1.9 Continuous Emission Monitoring
Real-time emissions of NOx, CO, CO2, SO2, and HCl will be measured using CEMs (see DPG
LOl-106 in Appendix B). Chamber gases will be continuously recirculated through a manifold
in the bunker adjacent to the test chamber. A small slipstream will be pulled from the manifold
into each analyzer. Mulfipoint calibrations will be performed on each instrument before the test
series to verify that response is linear. As needed, zero and upscale calibration standards will be
used to check for analyzer drift and bias (at least twice per day). The analyzer outputs during
sampling will be stored by the data acquisifion system.
4.2 SAMPLING PREPARATION, QUALITY CONTROL, AND MEASUREMENT
4.2.1 Calibration of Field Instrumentation
Prior to actual sampling, all field instruments will be calibrated to assure that accurate and
reliable measurements are obtained.
Calibrafion procedures and criteria for sampling equipment are based on the sampling methods
in Appendix B. For sampling trains, this primarily applies to gas sample volume. For CEMs,
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this primarily applies to concentration drift and span. For all analyfical measurements, the range
ofthe instmment calibrafion is specified to encompass the range of probable experimental
values. This approach ensures that all results are based upon interpolafive analyses rather than
extrapolafive analyses. Calibrafions are designed to include, where practicable, at least four
measurement points evenly spaced over the range. This practice minimizes the probability that
false assumpfions of calibrafion linearity will be made. In addifion, it is common practice to
select, when pracficable, at least one calibrafion value that approximates the levels anficipated in
the actual measurement. Typically, calibration frequency is dictated by the need to demonstrate
the stability of the calibration value over the course of measurements.
Sampling media such as polyurethane foam (PUF) plugs, Summa Canisters, sorbent traps, filters,
will be provided by the corresponding commercial laboratories performing the contracted sample
analyses.
4.2.2 Preparation of Sampling Equipment and Containers and Field Decontamination
Calibrafion procedures and criteria for sampling equipment are based on the sampling methods
in Appendix B. For sampling trains, this primarily applies to gas sample volume. For CEMs,
this primarily applies to concentration drift and span. For all analytical measurements, the range
of the instmment calibration is specified to encompass the range of probable experimental
values. This approach ensures that all results are based upon interpolative analyses rather than
extrapolafive analyses. Calibrafions are designed to include, where pracficable, at least four
measurement points evenly spaced over the range. This pracfice minimizes the probability that
false assumpfions of calibrafion linearity will be made. In addition, it is common pracfice to
select, when pracficable, at least one calibration value that approximates the levels anticipated in
the actual measurement. Typically, calibration frequency is dictated by the need to demonstrate
the stability of the calibrafion value over the course of measurements.
Sampling media such as polyurethane foam (PUF) plugs, Summa Canisters, sorbent traps, filters,
will be provided by the corresponding commercial laboratories performing the contracted sample
analyses.
4.2.3 Field Blanl<s, Duplicates, Splits, and Quality Control
QC checks of both field sampling and laboratory sample analysis will be used to assess and
document data quality and to identify irregularities in the measurement process that need
correction.
QC samples will be employed to assess various data quality parameters such as
representativeness of the environmental samples, the precision of sample collecfion and handling
procedures, the thoroughness ofthe field equipment decontamination procedures, and the
accuracy of laboratory analysis. To evaluate bias and contamination from field collecfion
procedures, blanks will be prepared from distilled or deionized water.
In addifion to the field QC samples identified below, the analytical laboratory will use a series of
QC samples as idenfified in the laboratory QA plan and specified in the standard analytical
methods. The types of laboratory QC samples include method blank, LCS, MS, and laboratory
duplicate or MSD. A LCS will be analyzed for each method and batch.
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SECTIONFOUR Sample Selection and Collection
Analyses of QC samples will be performed for samples of similar matrix type and
extracfion/analysis method and for each sample batch. To supplement the use of QC samples,
the laboratory will generate and use control charts to assess performance on the QC samples.
The following sections describe field QC samples that will be collected.
4.2.3.1 Equipment Blanks
Equipment decontamination rinsates will not be required because dedicated sampling equipment
will be used.
4.2.3.2 Field Replicates
Each ATK test material will be bumed three separate times. As a result triplicate samples
represenfing each sample will be collected and submitted to the off-site commercial lab for
tesfing. These samples will be analyzed for all parameters idenfified in Table 1-1.
4.2.3.3 Field Blanks
Field blanks will be used to indicate the presence of extemal contaminants that may have been
introduced into the samples during collecfion. Field blanks will be collected and analyzed for all
parameters of interest. Field blanks will be prepared on site during the sampling event. At least
one field blank sample will be analyzed for each group of samples of a similar matrix type per
event (i.e., one field blank per investigation area per matrix analyzed). The field blanks will be
handled and analyzed in the same manner as all environmental samples.
4.2.3.4 Trip Blanks
Trip blanks will not be prepared or analyzed specific to this investigafion.
4.2.3.5 Performance Evaluation Samples
PE samples will not be prepared or analyzed specific to this invesfigafion.
4.2.4 Preservation, Transportation, and Storage of Samples
Preservafion requirements and associated holding fimes will be in accordance with QC
requirements specified in Tables 4-1 to ensure sample integrity. Samples collected during this
investigation will be either shipped to the laboratory via an ovemight carrier or will be hand
delivered to analyfical laboratory if geographically possible.
4.3 DOCUMENTATION
Field data measurements and observations will be recorded in field logbooks and the appropriate
field forms.
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SECTIONFIVE Sample Analysis
The laboratory QA/QC procedures in this QAPP are intended to be minimum requirements. The
selected laboratories to perform the work will meet, at a minimum, the requirements of this
QAPP and the QA/QC requirements specified in the labs specific laboratory standard operating
procedures (SOPs).
Written documentation of sample custody from the time of sample collecfion through the
generafion of data by analysis of the sample is recognized as a vital aspect of an environmental
invesfigafion. As described below, sample custody applies to both field and laboratory
operafions. Official custody of the sample and its corresponding documentafion will be
maintained throughout the handling of the sample, from the time of collection, through
preparation and analysis, and unfil sample disposal.
5.1 FIELD OPERATIONS
5.1.1 Sample Container Labeling
Sample labels will be filled out in the field. Minimum requirements for information to be
included on sample container labels are included in Test Plan.
5.1.2 Sample Custody (Custody Seals, Chain-of-Custody, and Analysis Request)
For field operations, standard sample collection procedures have been developed for sample
custody, labeling, analysis request, and tracking. All samples will be idenfified, labeled, and
logged onto a COC form, as a part of an overall procedure designed to assure the integrity of the
resulfing data. The record ofthe physical sample (locafion and fime of sampling) will be joined
with the analytical results through accurate accounfing of the sample custody.
5.2 LABORATORY OPERATIONS
All laboratories complefing chemical analyses will be required to maintain samples in a secure
locafion with limited access from the time of sample receipt through sample disposal. Sample
custody procedures within a laboratory will be dependent upon the laboratory quality assurance
plan (QAP) and/or SOPs. The laboratory will be responsible for maintaining logbooks and
records that provide an uninterrupted custody record throughout sample preparation and analysis.
The general steps to be followed by the analyfical laboratory for sample receipt, sample labeling,
and sample custody are:
• Laboratory receives samples
• A sample receipt checklist is filled out. The following items are documented on the
checklist.
- The temperature of the temperature blank (taken and recorded before the samples are
unpacked), where applicable.
Containers are checked for breakage/damage.
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Preservative use (once the cooler is unpacked, all botfies are checked to ensure that
the samples have been preserved properiy), where applicable.
Agreement between bottle labels and the COC form.
Verification that adequate sample volume for each analysis has been provided.
• A lot number or sample delivery group (SDG) number is then assigned
• The sample bottles are then labeled with the laboratory number
• The sample bottle laboratory number labeling is verified
• If any discrepancies were found during login, the laboratory PM will nofify the URS
QAO.
• The samples are placed in refrigerators if applicable.
• After the final report has been issued, samples are moved to archive.
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SECTIONSIX Laboratory Calibration Procedures and Frequency
All laboratory instmments will be calibrated in accordance with the analyfical method
requirements. All analytes reported will be present in the initial and confinuing calibrafions, and
these calibrations will meet the acceptance criteria specified in the method, at a minimum. All
results reported will be within the calibrated range. Records of standards preparation and
instmment calibrafion will be maintained and submitted with the final data package. Calibration
standards for all analyses shall be traceable to a certified Standard Reference Material (SRM)
that idenfifies the chemical composition, purity, property, and expiration date.
The inifial calibrafion will be checked at the frequency specified in the method using standard
materials. Multipoint calibrafions will contain the minimum number of calibration points
specified in the method. It is permissible to drop the highest and lowest concentrafion standards
from the calibrafion as long as the calibration range is adjusted appropriately and as long as the
adjusted calibration includes the minimum number of standards specified in the method. If the
low point standard is omitted, the reporting limit for associated data must be adjusted
accordingly. If linearity criteria cannot be met by dropping either the high or low point standard,
the instrument must be recalibrated.
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SECTIONSEVEN Analytical Procedures
Chemical analysis of samples for invesfigafive activifies will be completed using the methods (or
equivalent methods with approval) listed in Tables 1-1. During the field activities, samples will
be collected and preserved as described in Tables 4-1. Sample holding fimes fisted are calculated
from the date and time of collection.
For organic analyses for which there are mulfiple surrogate standards analyzed (e.g.. Methods
SW-846 8270C, 8290) and one of theses surrogates fail to fall within surrogate recovery limits,
results may be reported without reextracfion and/or reanalysis if all of the following criteria are
met:
• There must be objecfive evidence of sample matrix interferences (e.g., multiple
interfering peaks visible on chromatograms, co-elufing peaks, documented evidence that
extracts solidify before reaching final concentrafion volume, first hand observafion such
as the presence of multiple phases, or results from earlier testing). The laboratory PM
must contact the Environmental Contractor Project Chemist to relay the informafion and
get approval to report without reanalysis.
• Sun-ogate recoveries in LCSs and method blanks from the same extraction batch must be
within surrogate recovery limits for an excepfion to be considered.
• One of the two surrogates for gas chromatographic methods must meet the surrogate
recovery limits, and the recovery for both must be greater than 10%.
• No more than one surrogate compound can be out of surrogate recovery limits for either
the acid or base/neutral fracfion for 8270C, and all surrogate recoveries must be greater
than 10%.
The methods do not and cannot include all analyfical situations. These additional criteria are
provided as a means of applying technically justifiable evaluafion criteria in situafions where
there is clear and documented evidence that a reextracfion and reanalysis will not improve the
quality of the data.
For SW-846 8000 series analyses. Method 8000B Secfions 7.5.1.2.3 and 7.7 require that the data
user must be provided with initial calibration and/or calibrafion verificafion data or a specific list
of those compounds for which the relafive standard deviation (RSD) exceeded 20% and/or a list
of those analyses that exceeded the 15% percent difference or percent drift limits. For analyses
conducted under this QAPP, those compounds outside of these criteria and the actual values of
the RSD and/or percent differences outside of these criteria shall be provided in the laboratory
case narrafive.
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SECTIONEIGHT Data Reduction, Validation, and Reporting
The following secfions describe the process of handling data in terms of data generation,
checking, and formatted reports for both field sampling and laboratory analytical data.
8.1 DATA REDUCTION
This secfion oufiines the methodology for assuring the correctness of the data reduction process.
The procedures describe steps for verifying the accuracy of data reduction. Data will be reduced
either manually on calculafion sheets or by computer on formatted printouts. The following
responsibilifies will be delegated in the data reducfion process:
• Technical personnel will document and review their own work and are accountable for its
correctness,
• Selected calculations will receive both a method and an arithmefic check by an
independent checker. The checker will be accountable for the correctness of the checking
process,
• An intemal technical review will be conducted to assure the consistency and defensibility
of the concepts, methods, assumptions, calculations, etc., and
• The data reduction will be performed in a manner that produces accurate data through
review and approval of calculafions.
8.2 DATA VALIDATION
As appropriate and consistent with DQOs, decisions and recommendafions will be based upon
validated data. The process through which data will be accepted, qualified, or rejected will be
based upon specific data validafion criteria. These criteria are discussed in the following
sections for both field and laboratory data. Personnel experienced with sampling and analytical
protocols and procedures will perform the data validation in accordance with the established
criteria and the intended use of the data.
The screening data generated during this project will not be validated using EPA methodologies
for data validafion. These data will be verified for contract compliance, holding time compliance
(as applicable), QC sample frequency and results, and overall data quality. Data validafion
qualifiers will not be applied to screening data. An overall data usability assessment will be
made.
Qualified chemists not involved with the actual generafion of data will conduct an analyfical data
validafion for the definifive data. The data package will be validated using the criteria contained
in EPA's Funcfional Guidelines (EPA 2002, EPA 1999) that are pertinent to the SW-846
analyfical method and the QA acceptance criteria contained in this QAPP.
8.2.1 Field Data Validation
The purpose of the field data validation process is to evaluate the usability of field data that are
collected or documented in accordance with specified protocols outlined in appropriate LOI.
Field data documentation will be validated against the following criteria, as appropriate:
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Sample locafion and adherence to the plan
Field instrumentation and calibrafion
Sample collection protocol
Sample volume
Sample preservation
Blanks collected and submitted with each respecfive sample set
Duplicates collected and submitted with each respecfive sample set
Sample documentation protocol
Field COC protocol
8.2.2 Laboratory Data Reduction and Review
Data reducfion is the process of converting measurement system outputs to an expression of the
parameter that is consistent with the comparable objecfive idenfified in this plan. Reducfion of
analyfical data will be completed in accordance with the off-site analyfical laboratory's Quality
Assurance Plan (QAP) and SOPs.
The first level of review, which may contain multiple sublevels, will be conducted by the
analyfical laboratory that has initial responsibility for the correctness and completeness ofthe
data. The laboratory data reviewer will evaluate the quality of the analyfical data based on an
established set of laboratory guidelines (laboratory QAP and SOPs) and this QAPP. This person
will review the data packages to confirm the following:
• Sample preparation information is correct and complete
• Analysis information is correct and complete
• The appropriate laboratory SOPs have been followed
• Analytical results are correct and complete
• QC sample results are within established control limits
• Blank results are within appropriate QC limits
• Analyfical results for QC sample spikes, sample duplicates, initial and continuous
calibration verifications of standards and blanks, standard procedural blanks, LCSs, and
inductively coupled plasma (ICP) emission spectrometer interference check samples are
correct and complete
• Tabulafion of reporting limits related to the sample is correct and complete
• Documentation is complete (all anomalies in the preparafion and analysis have been
documented; holding times are documented)
The laboratory will perform the in-house analytical data reducfion and QA review under the
direcfion of the laboratory PM or designee. The laboratory is responsible for assessing data
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SECTIONEIGHT Data Reduction, Validation, and Reporting
quality and advising of any data that were rated "preliminary" or "unacceptable," or were flagged
with any other notafions that would caufion the data user of possible unreliability.
Data reduction, QA review, and reporting by the laboratory will include the following:
•
•
Raw data produced by the analyst are processed and reviewed for attainment of QC
criteria as outlined in this QAPP, the laboratory QAP, and/or established EPA methods.
The raw data will also be reviewed for overall reasonableness.
The data reviewer will check all manually entered sample data for entry errors and will
check for transfer errors in all data electronically uploaded from the instmment output
into the software packages used for calculations and generafion of report forms. Based
on these checks, the reviewer will decide whether any sample re-analysis is required.
• The laboratory will review initial and confinuing calibration data, and calculafion of
response factors, surrogate recoveries, MS/MSD recoveries, post-digestion (analytical)
spike recoveries, intemal standard recoveries, LCS recoveries, sample results, and other
relevant QC measures.
• Upon acceptance of the preliminary reports by the laboratory data reviewer, the
laboratory QA officer or designee will review and approve the data packages prior to the
final reports being generated.
The data reduction and the QC review steps will be documented, signed, and dated by the analyst
and the laboratory project manager or designee.
8.2.3 Independent Review
Secfion 8.2.2 describes the level of review ofthe analyfical data by the off-site laboratory that
has generated the data. The second level of review and verificafion ofthe analytical data will be
performed by data verification personnel independent of the laboratory generating the data. The
purpose ofthis second level of review is to provide an independent review ofthe data package
and will include a review of laboratory performance criteria and sample-specific criteria. The
following subsections discuss the process for independent review of laboratory performance
criteria and sample-specific criteria. The amount and level of data validafion will be based on
the end use of the data and nature of the decisions that will be based on the data.
Since the data review by the off-site analytical laboratory includes a thorough review of
laboratory performance criteria (which are independent ofthe field samples being analyzed), the
independent verification will include evaluation of QA/QC issues idenfified in the laboratory
case narrafive. These QA/QC issues will be evaluated relative to the laboratory performance
criteria (e.g., inifial calibrafion, confinuing calibration verificafion, LCS analysis, interference
check sample analysis) to verify that the laboratory analyses are in compliance with method
specifications. This will be conducted for 100% of data from the off-site laboratory. The review
of laboratory performance criteria is discussed in Secfion 8.2.3.1.
The independent verification will also include a review of sample-specific criteria for 100% of
the data packages for each analysis type for those parameters that are sample-related. The
parameters include: holding times, surrogate recoveries, MS recoveries, field duplicate
agreement, MSD and laboratory duplicate precision, post digesfion (analytical) spike recoveries,
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SECTIONEIGHT Data Reduction, Validation, and Reporting
ICP serial dilution analysis agreement, and qualification of sample data based on analytes
reported as detected in blank analyses.
All analytical data received from the laboratory shall meet the data package requirements
specified in the URS terms and conditions contained in the lab contract. Fully validatable data
packages will be submitted as appropriate. The laboratory will be contacted with regard to any
missing or incorrect deliverables in the data packages noted during the validafion process. The
data reviewer will document all subsequent submittals and resubmittals from the laboratory,
recalculafions, and data reviewer correcfions. The data package will be reviewed for evaluation
and compliance with method specificafions. Method non-compliances idenfified during the
review, professional judgments used, and conclusions reached conceming usability of non-
compliant data will be described in data verificafion and completeness reports. These reports
will also describe the results of the sample-specific review and the impact on the quality and
usability of the data.
8.2.3.1 Review of Laboratory Performance Criteria
Results not meeting method acceptance criteria are documented by the laboratory in the case
narrative. The subsections below discuss how each of the laboratory performance parameters
reported as not meeting acceptance criteria would be identified and documented in the data
review report. The lab perfoiTnance parameters to be reviewed include:
8.2.3.1.1 Initial Calibration
The analyfical method shall be used to determine the QC acceptance criteria for inifial calibration
for those methods covered under this QAPP. If the case narrative or data review process
indicates that the inifial calibration for any analyte did not meet the acceptance criteria, it will be
documented in the data review report.
8.2.3.1.2 Initial and/or Continuing Calibration Verification
The analyfical method will be used to determine the QC acceptance criteria for initial and
continuing calibrafion verification for those methods covered under this QAPP. If the case
nairafive or data validafion process indicates that the initial or confinuing calibrafion verification
for any analyte did not meet the acceptance criteria, it will be documented in the data review
report.
8.2.3.1.3 Internal Standard Data
The analyfical method will be used to determine the QC acceptance criteria for intemal standard
area counts for gas chromatography/mass spectrometry (GC/MS) organic analysis and for
intemal standard quantitation for methods covered under this QAPP. Intemal standard area
counts are not a direct measure of the accuracy of the analysis. If the case narrafive or data
review process indicates that the intemal standard data did not meet the acceptance criteria, it
will be documented in the data review report.
8.2.3.1.4 Dual Column Confimnation Results
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SECTIONEIGHT Data Reduction, Validation, and Reporting
None of the specified analytical methods require second column confirmation as documented in
this QAPP.
8.2.3.1.5 Laboratory Control Sannple Analysis
The analyte recoveries obtained for LCS analyses will be compared to analytical method
requirements and to the acceptance range established by the contract laboratory. If the case
narrative or data review process indicates that the LCS did not meet the acceptance criteria, it
will be documented in the data review report.
8.2.3.1.6 Inductively Coupled Plasma Interference Check Sample for Metals
The analyfical method specifies the QC acceptance criteria for interference check sample (ICS)
analysis for metals analysis methods covered under this QAPP. If the case narrafive or data
review process indicates that the ICS did not meet the acceptance criteria, it will be documented
in the data review report.
8.2.3.2 Review of Method-Specific Requirements
The data verificafion review will also include a review of method -specific criteria for all of the
data packages for each analysis type for those parameters that are sample related. Data
verification and completeness checks will be conducted and documented.
No recalculation of results from the raw data or transcription error checking will be performed
during the review of the sample-specific criteria.
8.2.3.2.1 Other Itenns Identified in the Case Narrative
If analytes identified in the case narrative are not covered by the subsections below and are found
to be noncompliant, the data reviewer shall evaluate the problem based on method requirements.
If the analyfical method does not specify requirements related to the criterion under evaluation,
the data reviewer should utilize professional judgment to evaluate the effect of the reported item
or condifion on the associated analyfical data. All uses of professional judgment shall be
described in the report of the data validafion process.
8.2.3.2.2 Blanks
The results for background and ambient blanks, preparafion blanks, calibrafion blanks, and other
blanks reported in the data package will be reviewed. If the case narrative or data review
process indicates that the blank results could impact the associated sample results, it will be
documented in the data review report.
Preparation blanks are associated with all samples prepared with that sample (preparation batch).
Confinuing calibrafion blank samples are considered to be associated with all samples in a given
analytical mn. The highest confinuing calibrafion blank samples concentrafion will be used in the
data review assessment process.
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SECTIONEIGHT Data Reduction, Validation, and Reporting
8.2.3.2.3 Metals and Inorganic Analyses
Metals data from ICP and other inorganic data will be evaluated for method compliance and will
also undergo evaluafion or for following specific criteria:
Holding times
Duplicate sample analysis
MS sample analysis
MSD or laboratory duplicate precision
Post digesfion (analyfical) spike recoveries
ICP serial dilufions
Field duplicate result agreement
Holding Times
Holding times and sample temperatures will be compared to the holding fime and sample
temperature requirements contained in Table 4-1 of this QAPP. Results for analyses not
performed within holding fime limits will be identified and documented in the data review
report.
Duplicate Sample Analysis
Results for the duplicate sample (laboratory duplicate or MSD) will be compared to the criteria
in Table 3-1. If the duplicate results for an analyte do not safisfy the applicable evaluafion
criterion, results for that analyte in the sample that duplicate was performed on will be
documented in the data review report.
Matrix Spike Sample Analysis
The analyte recoveries obtained for MS (or MSD) analyses will be compared to the acceptance
range contained in Table 3-1 for cases in which the native sample concentrafion is less than four
times the spike concentration, as specified in the EPA Funcfional Guidelines. When sample
concentrations of an analyte are greater than four times the spiking concentrafion, the results are
considered to be inappropriate for assessing accuracy. Data associated with MS recoveries that
are outside the acceptance range will be idenfified and documented in the data review assessment
report.
Post-Digestion Spike Recovery
The analyte recoveries obtained for post-digestion spike analyses will be compared to the
acceptance range for accuracy in the analyfical method. Under some circumstances, laboratories
will quantify results by the method of standard addifions to compensate for low post-digesfion
spike recovery. As such, the low spike recovery would not indicate poor accuracy. However, if
the result for the sample on which the post-digestion spike analysis was performed was not
obtained by the method of standard additions and the post-digestion spike recovery was outside
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SECTIONEIGHT Data Reduction, Validation, and Reporting
of the acceptance limits, the result for the sample on which the post-digesfion spike was run will
be identified and documented in the data review assessment report.
ICP Serial Dilution
ICP serial dilufions are run to help evaluate whether or not significant physical or chemical
interferences exist due to the sample matrix. When analyte concentrafions are sufficiently high
(the concentrafion in the original sample is minimally a factor of 50 above the instrument
detection limit) the results obtained for a five fold-dilution of the original sample are compared
to the original results by means of a percent difference (%D). The %D is compared to a
precision acceptance limit of ±15%. If the absolute value of the percent difference between the
diluted and original result is greater than 15%, all results for that analyte in that SDG will be
identified and documented in the data assessment report.
Field Duplicate Agreement
Criteria in Table 3-1 will be used to assess the reported results. If the criteria are not met for an
analyte, all associated sample data will be idenfified and documented in the data review
assessment report.
8.2.3.2.4 Organic Analyses
For organics by GC or GC/MS, the data will be evaluated for method compliance and will then
also undergo evaluation for following specific criteria:
• Holding fimes
• Laboratory Control Sample
• Surrogate spike results
• MS/MSD analyses
• Intemal standard recoveries for isotopic dilution GC/MS analyses
• Tentafively identified compounds
• Field duplicate result agreement
The data reviewer should use guidance from EPA Funcfional Guidelines to address issues not
covered by this QAPP.
Holding Times
The holding fimes will be compared to the holding fime requirements contained in Tables 4-1..
Results for analyses not performed within holding fime limits will be idenfified and documented
in the data review assessment report.
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SECTIONEIGHT Data Reduction, Validation, and Reporting
Laboratory Control Samples
A laboratory control sample (LCS) is prepared by spiking an aliquot of the standard matrix with
a known concentration of the analyte(s) of interest. The recovery of the target analyte (s) must
be reported within a statisfical recovery limit(s) range. The QC acceptance recovery is
stafisfically calculated based upon historical lab performance. Typically, QC acceptable limits
are reported within 80-100 %. The purpose of the LCS is to monitor laboratory performance for
a specific method.
Surrogate Spike Results
The surrogate recoveries obtained for each sample analysis for which surrogates were analyzed
will be compared to the laboratory historical limits to assess trending and if the percent recovery
is reported within the limits specified in Table 3-1. Results for analytes in the sample associated
with surrogate recoveries outside the acceptance range will be idenfified and documented in the
data review assessment report.
Matrix Spike/Matrix Spike DupHcate Sample Analysis
The analyte recoveries obtained for MS and MSD analyses will be compared to the acceptance
range contained in Table 3-1 for cases in which the nafive sample concentrafion is less than four
fimes the spike concentration. When sample concentrations of an analyte are greater than four
fimes the spiking concentration, the results are considered to be inappropriate for assessing
accuracy. Data associated with MS or MSD recoveries outside the acceptance range will be
identified and documented in the data review assessment report.
Field Duplicate Agreement
Criteria in Table 3-1 will be used to assess the reported results. If the criteria are not met for an
analyte, all associated sample data will be idenfified and documented in the data review
assessment report.
8.3 DATA REPORTING
Field measurements and observations will be recorded in field logbooks. Laboratory data will be
recorded in the standard formats described in the Laboratory Statement of Work.
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SECTIONNINE Field and Laboratory Quality Control Checks
QC checks of both field sampling and laboratory sample analysis will be used to assess and
document data quality and to idenfify discrepancies in the measurement process that need
correction. Field QC samples are discussed in detail in Secfion 4.2.3.
The analytical laboratory will use a series of QC samples as identified in the laboratory QA plan
and specified in the standard analyfical methods. The types of laboratory QC samples include
method blank, LCS, MS, and laboratory duplicate or MSD. A LCS will be analyzed for each
method and batch. Analyses of QC samples will be performed for samples of similar matrix type
and extracfion/analysis method, and for each sample batch. To supplement the use of QC
samples, the laboratory will generate and use control charts to assess performance on the QC
samples.
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SECTIONTEN Performance and System Audits
Performance or system audits will not be performed under this QAPP.
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SECTIONELEVEN Preventive Maintenance
11.1 FIELD EQUIPMENT
All field equipment and instmments used to generate data will be adjusted and maintained to
operate within manufacturers' specificafions. Maintaining the necessary accuracy, precision,
sensifivity, and traceability ofthe equipment helps assure that reliable measurements and
representative data will be obtained. Methods and intervals of inspecfion and maintenance will
be based on the type of equipment, stability characterisfics, required accuracy, intended use, and
environmental factors (such as temperature, humidity, etc.). As appropriate, back-up equipment
and crifical spare parts will be maintained in order to quickly correct equipment malfunction.
As appropriate, inspection records and maintenance schedules will be maintained for instmments
and equipment and will be stored in the project files. Equipment that is idenfified to be
malfunctioning will be removed from operafion and tagged until repaired.
11.2 LABORATORY EQUIPMENT
Guidelines for inspecfion and prevenfive maintenance of laboratory equipment will be
established in the laboratory QAP. Essenfially, inspecfion and prevenfive maintenance will be
implemented on a scheduled basis to minimize downfime and to assure accurate measurements
from laboratory equipment. This program is designed to achieve results commensurate with the
specified capabilities of equipment operation, thus generafing data of known quality without
concem for misapplication. In addifion, back-up equipment and crifical spare parts will be
maintained in order to quickly correct equipment malfuncfion.
All equipment and instruments used to generate data will be adjusted and maintained to operate
within manufacturers' specifications and the method requirements. Maintaining the necessary
accuracy, precision, sensitivity, and traceability of the equipment helps assure that reliable
measurements and representative data will be obtained. Methods and intervals of inspection and
maintenance will be based on the type of equipment, stability characteristics, required accuracy,
intended use, and environmental factors (such as temperature, humidity, etc.). Such an effort
will be conducted by trained technicians using service manuals or through service agreements
with a qualified maintenance contractor. In addifion, procedures will assure that equipment is
properly used by trained personnel.
Inspecfion and maintenance, schedules and records will be maintained for the equipment, as
appropriate. Both equipment and equipment records will be located in a controlled access
facility. Each instrument will be assigned a unique identificafion number to document and track
usage and maintenance. Equipment that is identified to be malfuncfioning will be removed from
operation until repaired.
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SECTIONTWELVE Data Assessment Procedures
All data generated for the project will be assessed for accuracy, precision, completeness,
representafiveness, and comparability. This section establishes the methods for calculafing
accuracy, precision and completeness and for evaluafing representafiveness and comparability
12.1 PRECISION
Precision examines the spread of data about their mean (Secfion 3.2.1). The spread represents
how different the individual reported values are from the average reported values. Precision is
thus a measure of the magnitude of errors and will be expressed as the RPD or the RSD for all
methods. The lower these values are, the more precise are the data. These quantities are defined
as follows:
RPD(%) = 100 x |S-D|
(S -I- D)/2
RSD(%) = (s/X)xlOO
where: D = Concentration or value of an analyte in a duplicate sample
S = Concentration or value of an analyte in a original sample
X = Mean of replicate analyses
s = Standard deviation
12.2 ACCURACY
Accuracy measures the average or systematic error of an analytical method (Section 3.2.2). This
measure is defined as the difference between the measured value and the actual value. Accuracy
will be expressed as the percent recovery. This quantity is defined as follows:
Recovery (%) = |SC-UC| x 100
KC
where: SC = Measured concentration of an analyte in spiked sample or LCS
UC - Measured unspiked concentration of an analyte (assume to be zero for
LCS and surrogates)
KC = Known concentration of an analyte added
12.3 COMPLETENESS
Completeness establishes whether a sufficient amount of valid measurements were obtained
(Secfion 3.2.5). The closer this value is to 100%, the more complete the measurement process.
The overall project completeness goal is 80%. Completeness will be calculated as follows:
Completeness (%) = V x 100
R
where: V = Number of valid measurements (includes data qualified
as estimated)
R = Numberof planned measurements
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SECTIONTWELVE Data Assessment Procedures
12.4 REPRESENTATIVENESS
Representativeness expresses the degree to which data accurately and precisely represents the
environmental condifion (Secfion 3.2.3). A statement on representativeness will be presented in
data validation reports nofing the degree to which data represents the environment.
12.5 COMPARABILITY
Comparability expresses the confidence with which one set of data can be compared to another
(Secfion 3.2.4). A statement on comparability nofing the degree to which data meet the
comparability goal will be presented in data validation reports.
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SECTIONTHIRTEEN Corrective Action
Provisions for establishing and maintaining QA reporting to the appropriate management
authority will be insfituted to assure that early and effecfive correcfive action can be taken when
data quality falls outside of established acceptance criteria. In this context, correcfive action
involves the following steps:
• Discovery of a nonconformance
• Idenfification of the root cause of the problem and the responsible individual(s)
• Discuss, plan and schedule correcfive/preventive acfion
• Review the corrective action taken
• Confirmation that the desired results were achieved
It is the intent of the QA process to minimize corrective acfions through the development and
implementafion of effecfive intemal controls. To accomplish this, procedures will be
implemented as described in this section to acfivate a corrective action for each measurement
system when acceptance criteria have been exceeded. In addifion, reviews and audits will be
conducted on a periodic basis to check this implementafion. Results of QA reviews and audits
typically identify the requirement for corrective action. When this occurs, a corrective action
plan will be prepared to include: idenfificafion ofthe corrective acfion, organizafional level
responsible for the action taken, steps to be taken for correction, and approval for the correcfive
action.
Acfivifies subject to QA and QC will be evaluated for compliance with applicable standard
procedures. This includes both field and laboratory operafions as described in this QAPP and
LOIs. A lack of compliance with these procedures will consfitute a nonconformance. The URS
Quality Assurance Officer (QAO), or any URS project member who discovers or suspects a
nonconformance, is responsible for initiating a nonconformance report (NCR). The QAO will be
responsible for reviewing all audit and NCRs to determine areas of poor quality or failure to
adhere to established procedures. The QAO will report nonconformances to the URS PM. The
PM will assure that no additional work, which is dependent on the nonconforming acfivity, is
performed until a confirmed nonconformance is corrected.
The URS PM will be responsible for evaluafing all NCRs, conferring with the QAO on the steps
to be taken for correcfion, and execufing the corrective acfion as developed and scheduled.
Corrective acfion measures will be selected to prevent or reduce the likelihood of future
nonconformances and address the causes to the extent identifiable. Selected measures will be
appropriate to the seriousness of the nonconformance and realisfic in terms of the resources
required for implementation.
Upon complefion ofthe corrective acfion, the QAO will evaluate the adequacy and completeness
of the acfion taken. If the acfion is found to be inadequate, the QAO and URS PM will confer to
resolve the problem and determine any further actions. Implementation of any further acfion will
be scheduled by the URS PM. If the corrective action is found to be adequate, the QAO will
notify the URS PM of the safisfactory correcfive acfion and the completion of the audit.
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SECTIONTHIRTEEN Corrective Action
13.1 FIELD CHANGES
The URS PM is responsible for all invesfigafive acfivifies. In this role, the URS PM at fimes will
adjust the field program to accommodate project-specific needs. When it becomes necessary to
modify this program, the URS PM will notify the ATK PM and URS QAO.
13.2 LABORATORY DATA
The laboratory will report the types of out-of-control occurrences, how these occurrences are
documented, and who is responsible for correction and documentation. Generally, corrective
action will be inifiated by out-of-control events such as: poor analysis replicafion, poor recovery,
instmment calibrafion problems, blank contamination, etc.
Appropriate laboratory personnel will inifiate correcfive action at any fime during the analyfical
process when deemed necessary based on analytical judgment, method requirements, or when
QC data indicate a need for action. Correcfive acfions may include, but are not limited to:
Re-analysis
Calculation checks
Instmment recalibrafion
Preparation of new standards/blanks
Re-extraction/digestion
Dilufion
Applicafion of another analysis method
Addifional training of analysts
The following items must be documented for out-of-control incidents so that corrective action
may be taken to set the system back "in control." These items will typically consfitute a
corrective action report that is signed by the laboratory director and the laboratory QA contact:
• Where the out-of-control incident occurred,
• When the incident occurred and was corrected,
• Who discovered the out-of-control incident,
• Who verified the incident, and
• Who corrected the problem?
The laboratory will be responsible for re-sampling and re-analysis costs associated with gross
failure to meet laboratory QA/QC objecfives. In consultation with the Environmental Contractor
Project Chemist, wither the Environmental Contractor PM or the QAM may initiate a request for
correcfive acfion.
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SECTIONFOURTEEN Quality Assurance Reports to Management
The invesfigafion report (typically the Letter Report of Findings) will address the status and
results of the sampling and associated QA/QC process for each data generafion acfivity. The
report will typically address and document the following QA/QC items:
Measurement system performance and data quality. This section of the report will present the
assessment of precision, accuracy, and completeness in relation to the specified field and
laboratory data acceptance criteria and data assessment procedures.
• Audit findings and correcfive acfion measures. This section of the report will present the
effectiveness of the data QA program and implementation, and include a summary of
findings and observations resulting from audits, as appropriate.
• Final laboratory QA assessment. This secfion of the report will present a summary of the
laboratory results and performances based upon the data validation process.
• The roufine evaluations of data quality described throughout this QAPP will be
documented and filed along with the data in the project files. A summary of data quality
and the results of checking the sample data against the quality assurance objecfives will
be presented in the final report that presents and summarizes the data generated.
Reporting nonconformances and field changes to management is discussed in Secfion 13.
An effective QC program should include formal and frequent reports to management and
technical staff of progress in the on-going implementafion of the QC plan. At a minimum, the
following parties should receive updates on project status: 1) ATK Project Manager; 2) URS
PM; 3) URS QAO; and 4) other technical staff.
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SECTIONFIFTEEN Miscellaneous
15.1 TURNAROUND TIME
Reporting of data will occur within the fime frames specified in the Work Orders to the
laboratory. In case of any anticipated delays, the laboratory PM for the project will notify the
Environmental Contractor Project Chemist.
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SECTIONSIXTEEN References
EPA, see U.S. Environmental Protecfion Agency.
Headquarters, Department ofthe Army, Washington, DC, Technical Manual (TM) 9-1370-203-
34&P, Military Pyrotechnics, March 1996.
Office of Solid Waste and Emergency Response, Washington, DC, Environmental Protection
Agency Test Methods for Evaluating Solid Waste Physical/Chemical Methods (SW-846),
Methods 0010, 8270, and 8290,, November 1986.
U.S. Army Defense Ammunifion Center and School, Logisfics Review & Assistance Office,
Savanna, Illinois, Hazard Classificafion of United States Military Explosives and
Munifions, Rev. 11, February 2001.
U.S. Army Defense Ammunifion Center, McAlester, Oklahoma, MIDAS Home Page,
http://206.37.241.30/.
U.S. Army Developmental Test Command (DTC), Aberdeen Proving Ground, Maryland, Test
Authorization in the Test Resource Management System for West Desert Test Center
(WDTC), U.S. Army Dugway Proving Ground (DPG), Utah, to perform Emission
Products Characterization of Munifions Study (Phase IV), Test Project No. 8-CO-160-
000-067, 14 March 2001.
U.S. Army Dugway Proving Ground (DPG), Utah, Detailed Test Plan, Emission Characteri-
zation of Training Ordnance Phase I, II, III, & IV Smoke & Simulators in the
BANGBOX™ Test Facilifies, DPG Document No. DPG-TP-98-026, March 1998.
U.S. Army Dugway Proving Ground (DPG), Utah, Hazardous Waste Management Plan,
Environmental Acfivifies, June 2000.
U.S. Army Dugway Proving Ground (DPG), Utah, Record of Environmental Considerafion for
Phase-V Emission Characterization for Exploding Ordnance and Smoke/Pyrotechnics
(BangBox™ FY03) Tesfing at U.S. Army Dugway Proving Ground (DPG), Dugway,
Utah. TRMS Number 8-CO-160-000-067, 30 July 2003.
U.S. Army Dugway Proving Ground (DPG), Utah, Regulafion 350-104, Training and Certi-
ficafion Program for Convenfional Ammunifion, Chemical Laboratory, and Chamber
Test Facility Operafions, June 1996.
U.S. Army Dugway Proving Ground (DPG), Utah, Standing Operafing Procedure (SOP) DP-
OOOO-P-851, Rev. 4, Propellant Explosive and Pyrotechnic Thermal Treatment Evaluation
Test Facilities (PEP-TTET) (BANG BOXES), 1 August 2005.
U.S. Army Dugway Proving Ground (DPG), Utah, Standing Operafing Procedure (SOP) DP-
OOOO-H-138, Rev. 6, Munitions Demilitarization - Open Buming of Propellant,
Propellant Charges, Bulk Explosives (HMX or RDX), 4 June 2002.
U.S. Army Dugway Proving Ground (DPG), Utah, Standing Operafing Procedure (SOP) DP-
OOOO-G-139, Rev. 8, Munifions Demilitarizafion - Open Detonafion of Explosives, and
Emergency Procedures, 13 December 2004.
U.S. Army Environmental Center, Pollufion Prevenfion & Environmental Technology Division
FY99 Annual Report, Innovative Technology Demonstration, Evaluafion and Transfer
Acfivifies, Doc. No. SFlM-AEC-ET-TR-99070, January 2000.
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SECTIONSIXTEEN References
U.S. Environmental Protection Agency (EPA). 1999. Final USEPA Contract Laboratory
Program National Functional Guidelines for Organic Data Review. EPA 540-R-99-008,
Office of Emergency and Remedial Response, Washington, D.C.
U.S. Environmental Protecfion Agency (EPA). 2002. Final USEPA Contract Laboratory
Program National Functional Guidelines for Inorganic Data Review. EPA 540-R-Ol-
008, Office of Emergency and Remedial Response, Washington, D.C.
UDEQ, see Utah Department of Environmental Quality.
USEPA QA/G-4. 2000. Guidance fro the Data Quality Objectives Process, U.S.
Environmental Protection Agency Office of Research and Development, Washington,
D.C, EPA/600/R-96/056.
USEPA QA/R-5. 2001. EPA Requirements for Quality Assurance Project Plans for
Environmental Data Operations. U.S. Environmental Protection Agency, Washington,
D.C, EPA/240/B-01/003.
USEPA QA/G-5. 2002. EPA Guidance for Quality Assurance Project Plans. U.S.
Environmental Protection Agency Office of Research and Development, Washington,
D.C, EPA/240/R-02/009.
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Figures
Preliminary Draft
Figure M ODOBi Test Facility at DPG
Preliminary Draft
URS
QA Officer
Steve Baca, CQA
Alliant Thiokol
Project Manager
Blair Palmer
URS
Project Manager
John Carson
Commercial
Laboratories
URS
Administrafive
URS
Health & Safety
Sally Miller, CIH
URS
Technical Specialists
(i.e.. Chemists, Data
Managers)
URS
Field Support Staff
Figure 2-1 Project Organizational Chart
^''^^iminary Draft
Tables
Preliminary Draft
Table 1-1
Sampling and Analysis Method
Analyfical
Target
Sampling
Equipment Sampling Method^ Analytical Method Laborator)
TSP Particulate filter Method 5 in Appendix A of 40
CFR 60
Method 5 in Appendix A of
40 CFR 60 TBD
Metals Particulate filter Method 5 in Appendix A of 40
CFR 60
Method 29 in Appendix A of
40 CFR 60;
SW-846 Methods 6010/7470''
TBD
PM,o/PM2
Cyclones/
particulate filters
Method 201A in 40 CFR 51
with PMio and PM2.5 cyclones Method 201A in 40 CFR 51 TBD
Dioxins/
Furans
Modified Method 5 Method 23 in Appendix A of
40 CFR 60 SW-846 Method 8290" TBD
SVOCs Modified Method 5 SW-846 Method 0010 SW-846 Method 8270" plus
TICs TBD
VOCs SUMMA canisters EPA Compendium Methods
TO-12 and TO-14
EPA Compendium Methods
TO-12 and TO-14 plus TICs TBD
Tracer
Compound
(SF5)
Canisters Grab GC/Electron Capture
Detector TBD
HC1/C12 Impinger Train Method 26 in 40 CFR 60 Method 26 in 40 CFR 60 TBD
Carbonyls DNPH-Iaced
sorbent tube
EPA Compendium Method
TO-11 A
EPA Compendium Method
TO-11 A TBD
CO, CO2, NOx
SO2, HCl CEM Methods 3A, 6C, 7E, and 10
in Appendix A of 40 CFR 60
Methods 3A, 6C, 7E, and 10
in Appendix A of 40 CFR 60 NA
''The sampling equipment and methods used during the tests will be
indicated (see Appendix B for details). Method modifications will
testing characteristics ofthe smoke chamber.
"Analyses of TSP.
'^Analysis of soluble TSP fraction.
'^ Filter and adsorbent.
NA: Not Applicable
TBD: To be determined
3ased on standard methods, as
be necessary to accommodate the
Preliminary Draft
Table 3-1
Measurement Quality Objectives
Test Parameter
TSP
PM10/PM2.5
Metals
VOCs
Tracer Compound
SVOCs
Dioxins/Furans
HC1/C12
Carbonyls
NOx, CO, CO2, SO2,
HCl
Accuracy Objective
95 to 105% accuracy of flow and
filter-weighing devices
95 to 105% accuracy of flow and
filter weighing devices
75 to 125% recovery of post
digestion matrix spike from filter
70 to 130% recovery of laboratory
media spike (laboratory
calibration check material,
transferred into a canister, and
analyzed with the field samples)
60 to 140% for polar compounds
80 to 120% recovery of laboratory
media spike
40 to 120% surrogate spike
recoveries
40 to 135% surrogate spike
recoveries
85-115% recovery for matrix
spike
70 to 130% recovery of media
spike
±5% of span for zero and upscale
bias checks
Precision Objective
RPD <25% for multiple runs on a single event
RPD <25% for multiple runs on a single event
<20% RPD for recovery of post digestion MS/MSD
from filter
<25% RPD for top ten peaks on laboratory duplicate
analyses
±10% RPD for laboratory duplicate analyses
<50% RPD for MS/MSD for all compounds
<20% RPD for MS/MSD
<25% RPD for MS/MSD
<25% RPD for duplicate media spikes
±3% of span for zero and upscale drift checks
CO = carbon monoxide
CO2 = carbon dioxide
Cl2 = chlorine
HCl = hydrogen chloride
HCN = hydrogen cyanide
MS/MSD = matrix spike/matrix spike duplicate
NH3 = ammonia
NOv = nitrogen oxides
PM2.5 = particulate matter smaller than 2.5 microns
PMio= particulate matter smaller than 10 microns
RPD = relative percent difference
SO2 = sulfur dioxide
SVOC = semivolatile or ganic compound
TSP = total suspended particulate [matter]
VOC = volatile organic compound
Preliminary Draft
Table 3-2
Laboratory Method Detection Limits and Reporting Limits
The contract lab will provide this information.
Preliminary Draft
Table 3-3
Listing of LOIs for Smoke and Pyrotechnics, and Exploding Ordnance Tests
LOI
Number
101
104
106
107
108
109
301
304
Revision
Number
3
3
3
4
3
3
1
1
Revision Date
02 February 2005
02 February 2005
24 October 2005
02 February 2005
02 February 2005
02 February 2005
02 February 2005
02 February 2005
Test Chamber
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
Title
TSP Sampling and Analysis
Procedure
VOCs and Tracer Compounds
Sampling and Analysis
Procedure
CEM Sampling and Analysis
Procedure
Particulate Metals Sampling
and Analysis Procedure
HC1/C12/NH3 Sampling and
Analysis Procedure
Carbonyls Sampling and
Analysis Procedure
SVOCs & Dioxins/Furans
Sampling and Analysis
Procedure
PM2.5/PM10 Sampling and
Analysis Procedure using
Cyclones
r^ ll
Responsible
Organization URS
URS
URS
URS
URS
URS
URS
URS
OEM = Continuous Emission Monitor
€1:= Chlorine
HCl = Hydrogen Chloride
HCN = Hydrogen Cyanide
NHj = ammonia
ODOBi = Open Detonation Open Bum-improved
PM23 = Particulate Matter < 2.5 microns
PMio = Particulate Matter < 10 microns
SVOC = Semivolatile Organic Compound
TSP = Total Suspended Particulate Matter
URS = sampling and analysis contractor (formerly Radian Int.)
voc = Volatile Organic Compound
Preliminary Draft
Table 4-1
Sample Preservations and Holding Time Requirements
Metals
HC1/C12
SVOCs
VOCs
Dioxins/furans
Carbonyls
Tracer Compound
Preservation
None
None
4°C
None
4°C
None
None
1 1
Holding time
Mercury - 28 days.
All others- 180 days.
28 days
Extract within 14 days; analyze within 40 days following
extraction.
30 days.
Extract within 14 days; analyze within 40 days following
extraction.
Extract within 14 days; analyze within 30 days following
extraction.
30 days.
HCl = hydrogen chloride
pH = hydrogen ion concentration
SVOC = semivolatile organic compound
VOC = volatile organic compound
Appendix A
Usts Of Analytes
Preliminary Draft
Appendix A
Lists of Analytes
Table A.l.
VOC Target Analyte List (EPA Compendium Method TO-14).
1,1,1-Trichloroethane
1,1,2,2-Tetrachloroethane
1,1,2-Trichloroethane
1,1-Dichloroethane
1,1-Dichloroethene
1,2,3-Trimethylbenzene
1,2,4-Trichlorobenzene
1,2,4-Trimethylbenzene
1,2-Dibromoethane (EDB)
1,2-Dichlorobenzene
1,2-Dichloroethane
1,2-Dichloropropane
1,3,5-Trimethylbenzene
1,3-Butadiene
1,3-Dichlorobenzene
1,3-Diethylbenzene
1,4-Dichlorobenzene
1,4-Diethy Ibenzene
1,4-Dioxane
1-Butene
I-Hexene
1-Pentene
2,2-Dimelhylbutane
2,3,4-Trimethylpentane
2,3-Dimethylbutane
2,3-Dimethylpentane
2,4-DimethyIpentane
2-Butanone (Methyl Ethyl Ketone)
2-Ethyltoluene
2-Hexanone
2-Methylheptane
2-Methylhexane
2-Methylpentane
2-Nitropropane
2-Propanol
3-Chloropropene
VOCs
3-Ethyltoluene
3-Methylheptane
3-Methylhexane
3-Methylpentane
4-Ethyltoluene
4-Methy 1-2-pentanone
Acetone
Acetonitrile
Acetylene
Acrylonitrile
alpha-Chlorotoluene
Benzene
Bromodichloromethane
Bromoform
Bromomethane
Butane
Carbon Disulfide
Carbon Tetrachloride
Chloroacetonitrile
Chlorobenzene
Chloroethane
Chloroform
Chioromethane
cis-1,2-Dichloroethene
cis-1,3-Dichloropropene
cis-2-Butene
cis-2-Pentene
Cumene
Cyclohexane
Cyclopentane
Decane
Dibromoehloromethane
Ethane
Ethanol
Ethene
Ethyl Benzene
Ethyl Ether
Ethyl Methacrylate
Freon 11
Freon 113
Freon 114
Freon 12
Heptane
Hexachlorobutadiene
Hexane
Isobutane
Isopentane
Isoprene
m,p-Xylene
Methacrylonitrile
Methyl Acrylate
Methyl Methacrylate
Methyl tert-butyl ether
Methylcyclohexane
Methylcyclopentane
Methylene Chloride
n-Butylchloride
Nitrobenzene
Nonane
Octane
o-Xylene
Pentane
Propane
Propylbenzene
Propylbenzene
Propylene
Styrene
Tetrachloroethene
Tetrahydrofuran
TNMHC"
Toluene
trans-1,2-
Dichloroethene
trans-1,3-
Dichloropropene
trans-2-butene
trans-2-Pentene
Trichloroethene
Undecane
Vinyl Acetate
Vinyl Chloride
Vinyl Chloride
'Total nonmethane hydrocarbon.
URS C:\D0CUMENTS AND SETTINGS\G00CHGBL0CAL SEmNGS\TEMPORARY INTERNET FILES\OLK448\QAPP DRAFT 03172006.DOCVt-APR-06\\ A-1
Preliminary Draft
Appendix A
Lists of Analytes
Table A.2.
SVOC Target Analyte List (EPA SW-846 Method 8270).
SVOCs
1,2,4,5-
Tetrachlorobenzene
1,2,4-Trichlorobenzene
1,2-Dichlorobenzene
1,2-Diphenylhydrazine
1,3,5-Trinitrobenzene
1,3-Dichlorobenzene
1,3-Dinitrobenzene
1,4-Dichlorobenzene
1-Chioronaphthalene
1-Naphthylamine
2,3,4,6-
Tetrachlorophenol
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
2,4-Dichlorophenol
2,4-Dimethylphenol
2,4-Dinitrophenol
2,4-Dinitrotoluene
2,6-Dichlorophenol
2,6-Dinilrotoluene
2-Acetylaminofluorene
2-Chloronaphthalene
2-Chlorophenol
2-Methylnaphthalene
2-Methylphenol
2-Naphthylamine
2-Nitroaniline
2-Nitrophenol
3,3'-Dichlorobenzidine
3,3'-Dimethylbenzidine
3-Methylcholanthrene
3-Methylphenol & 4-
Methylphenol
3-Nitroaniline
4,6-Dinitro-2-methylphenol
4-Aminobiphenyl
4-Bromophenyl phenyl ether
4-Chloro-3-methylphenol
4-Chloroaniline
4-Chlorophenyl phenyl ether
4-Nitroaniline
4-Nitrophenol
7,12-
Dimethylbenz(a)anthracene
Acenaphthene
Acenaphthylene
Acetophenone
Aniline
Anthracene
Benz(a)anthracene
Benzidine
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(ghi)perylene
Benzo(k)fluoranthene
Benzoic acid
Benzyl alcohol
bis(2-Chloroethoxy)methane
bis(2-ChIoroethyl) ether
bis(2-Chloroisopropyl) ether
bis(2-Ethylhexyl)
phthalate
Butyl benzyl phthalate
Carbazole
Chrysene
Dibenz(a,h)anthracene
Dibenzofuran
Diethyl phthalate
Dimethyl phthalate
Di-n-butyl phthalate
Di-n-octyl phthalate
Dinoseb
Diphenylamine
Ethyl methanesulfonate
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachloroethane
Hexachloropropene
lndeno( 1,2,3-cd)pyrene
Isophorone
Isosafrole
Methyl methanesulfonate
Naphthalene
Nitrobenzene
N-Nitro-o-toluidine
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitrosodi-n-butylamine
N-Nitrosodi-n-propylamine
N-Nitrosodiphenylamine
N-Nitrosomethylethylamine
N-Nitrosomorpholine
N-Nitrosopiperidine
N-Nitrosopyrrolidine
o-Toluidine
Pentachlorobenzene
Pentachloroethane
Pentachloronitrobenzene
Pentachlorophenol
Phenacetin
Phenanthrene
Phenol
Pyrene
Pyridine
Safrole
URS C:\DOCUMENTS AND SETTINGS\GOOCHGBLOCAL SETTINGS\TEMPORARY INTERNET FILES\0LK44B\QAPP DRAFT 03172006.DOC\4-APR-06\\ A-2
Preliminary Draft
Appendix A
Lists of Analytes
Table A.3.
Carbonyls Target Analyte List (EPA Compendium Method TO-llA).
Carbonyls |
2,5-Dimethylbenzaldehyde
Acetaldehyde
Acetone
Benzaldehyde
Crotonaldehyde
Formaldehyde
Hexanal
Isopentanal
M,p-Tolualdehyde
MEK/Butyraldehydes
o-Tolualdehyde
Pentanal
Propanal
Table A.4.
Metals Target Analyte List (EPA Method 29).
Metals
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Cobalt
Copper
Lead
Magnesium
Manganese
Mercury
Nickel
Phosphorus
Selenium
Silver
Thallium
Zinc
Table A.S.
Dioxins/Furans Target Analyte List (EPA SW-846 Method 8290).
Dioxins
2,3,7,8-Tetrachlorodibenzo-
p-dioxin (TCDD)
1,2,3,7,8,9-
Hexachlorodibenzo-p-dioxin
(HxCDD)
1,2,3,7,8-
Pentachlorodibenzo-p-dioxin
(PeCDD)
1,2,3,4,6,7,8-
Heptachlorodibenzo-p-
dioxin (HpCDD)
1,2,3,4,7,8-
Hexachlorodibenzo-p-dioxin
(HxCDD)
1,2,3,4,6,7,8,9-
Octachlorodibenzo-p-dioxin
(OCDD)
1,2,3,6,7,8-
Hexachlorodibenzo-p-
dioxin (HxCDD)
Furans
2,3,7,8-
Tetrachlorodibenzofuran
(TCDF)
1,2,3,6,7,8-
Hexachlorodibenzofuran
(HxCDF)
1,2,3,4,7,8,9-
Heptachlorod i benzofuran
(HpCDF)
1,2,3,7,8-
Pentachlorodibenzofuran
(PeCDF)
2,3,4,6,7,8-
Hexachlorodibenzofuran
(HxCDF)
1,2,3,4,6,7,8,9-
Octachlorodibenzofuran
(OCDF)
2,3,4,7,8-
Pentachlorodibenzofuran
(PeCDF)
1.2,3,7,8,9-
Hexachlorodibenzofuran
(HxCDF)
1,2,3,4,7,8-
Hexachlorodibenzofuran
(HxCDF)
1,2,3,4,6,7,8-
Heptachlorodibenzofuran
(HpCDF)
UiRSc:\DOCUMENTS AND SETTINGS\GOOCHGBLOCAL SETTINGSNTEMPORARY INTERNET FILES\OLK448\QAPP DRAFT 03172006.DOC\4-APR-06\\ A-3
Preliminary Draft
Appendix A
Lists of Analytes
Table A.6
Other Target Compounds
Other Target Compounds
Hydrogen Chloride
Particulate Matter (TSP,
PM,o, PM2.5)
Chlorine
CEM gases (CO2, CO, SO2,
and NOx)
CEM = continuous emission monitor
CO = carbon monoxide
CO: = carbon dioxide
NO, = nitrogen oxides
PM15 = particulate matter smaller than 2.5 microns
PMIO = particulate matter smaller than 10 microns
SO: = sulfur dioxide
TSP = total suspended particulate matter
URS C:\D0CUMENTS AND SETTINGS\G00CHGBL0CAL SETTINGS\TEMPORARY INTERNET FILES\0LK448\QAPP DRAFT 03172006.DOC\4-APR-06\\ A-4
Appendix B
Letters Of Instruction
Preliminary Draft
Appendix B
Letters Of Instruction
This Appendix will include each full LOI identified below:
LOI
Number
101
104
106
107
108
109
301
304
Revision
Number
3
3
3
4
3
3
1
I
Revision Date
02 February 2005
02 February 2005
24 October 2005
02 February 2005
02 February 2005
02 February 2005
02 February 2005
02 February 2005
Test Chamber
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
ODOBi
ODBi
ODOBi
Title
TSP Sampling and Analysis
Procedure
VOCs and Tracer Compounds
Sampling and Analysis
Procedure
CEM Sampling and Analysis
Procedure
Particulate Metals Sampling
and Analysis Procedure
HC1/C12/NH3 Sampling and
Analysis Procedure
Carbonyls Sampling and
Analysis Procedure
SVOCs & Dioxins/Furans
Sampling and Analysis
Procedure
PM2.5/PM10 Sampling and
Analysis Procedure using
Cyclones
=^ ^
Responsible
Organization
URS
URS
URS
URS
URS
URS
URS
URS
CEM = Continuous Emission Monitor
Cl:= Chlorine
HCl = Hydrogen Chloride
HCN = Hydrogen Cyanide
NH.i = ammonia
ODOBi = Open Detonation Open Bum-improved
PM;5 = Particulate Matter < 2.5 microns
PMIO = Particulate Matter < 10 microns
SVOC = Semivolatile Organic Compound
TSP = Total Suspended Particulate Matter
URS = sampling and analysis contractor (formerly Radian Int.)
voc = Volatile Organic Compound
URS CADOCUMENTS AND SETTINGSNGOOCHGBLOCAL SETTINGSNTEMPORARY INTERNET FILES\0LK448\QAPP DRAFT 03172006.DOC\4-APR-06\\ B-l