Batteiie
The Business Of Innovation
Environmental Technology
Verification Program
Advanced Monitoring
Systems Center
Quality Assurance Project Plan
for Verification of the Xact 625 Ambient
Particulate Metals Monitor
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QUALITY ASSURANCE PROJECT PLAN
for
Verification of the Xact 625
Ambient Particulate Metals Monitor
Version 1.0
August 19, 2011
Prepared by
Battelle
505 King Avenue
Columbus, OH 43201-2693
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SECTION A
PROJECT MANAGEMENT
Al VENDOR APPROVAL PAGE
ETV Advanced Monitoring Systems Center
Quality Assurance Project Plan for Verification of
the Xact 625 Ambient Particulate Metals Monitor
Version 1.0
August 19, 2011
APPROVAL:
Name:
Company: Pall Corporation
Date:
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A2 TABLE OF CONTENTS
Section Page
PROJECT MANAGEMENT 1
Al Vendor Approval Page 1
A2 Table of Contents 2
A3 List of Acronyms and Abbreviations 4
A4 Distribution List 5
A5 Verification Test Organization 6
A6 Background 14
A7 Verification Test Description and Schedule 16
A8 Quality Objectives for Measurement Data 20
A9 Special Training/Certification 21
A10 Documentation and Records 21
DATA GENERATION AND ACQUISITION 23
Bl Experimental Design 23
B2 Sampling Methods 29
B3 Sample Handling and Custody 30
B4 Analytical Methods 31
B5 Quality Control 34
B6 Instrument/Equipment Testing, Inspection, and Maintenance 36
B7 Instrument Calibration andFrequency 36
B8 Inspection/Acceptance of Supplies and Consumables 38
B9 Non-Direct Measurements 38
BIO Data Management 38
ASSESSMENT AND OVERSIGHT 41
Cl Assessments and Response Actions 41
C2 Reports to Management 44
DATA VALIDATION AND USABILITY 46
Dl Data Review, Verification, and Validation Requirements 46
D2 Verification and Validation Methods 46
D3 Reconciliation with User Requirements 47
REFERENCES 48
APPENDIX A. Quantitation Limits of the Xact 625 49
APPENDIX B. Example PMio Metals Sample Data Sheet 50
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Section
Page
Figures
Figure 1. Organizational Chart
Tables
Table 1. Planned Verification Test Schedule 19
Table 2. Target Analytes for Metals Monitor Test 24
Table 3. Summary of Tests and Testing Frequency 25
Table 4. Target Analytes and Expected Detection Limits for Reference Method IO-3.5 32
Table 5. Summary of Data Recording Process 40
Table 6. Summary of Assessment Reports 45
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A3 LIST OF ACRONYMS AND ABBREVIATIONS
ADQ audit of data quality
AMS Advanced Monitoring Systems
CES Cooper Environmental Services LLC
COC chain of custody
DC data completeness
DQO data quality objective
EPA U.S. Environmental Protection Agency
ERG Eastern Research Group
ETV Environmental Technology Verification
ft foot or feet
hr hour(s)
ICP/MS inductively coupled plasma/mass spectrometry
L liter(s)
LFB laboratory fortified blank
LRB laboratory record book
m meter(s)
|ig/m3 micrograms per cubic meter
min minute(s)
ng nanogram(s)
NIST National Institute of Standards and Technology
NRMRL National Risk Management Research Laboratory
OAQPS Office of Air Quality Planning and Standards
OEPA Ohio Environmental Protection Agency
PE performance evaluation
PM particulate matter
PMio particulate matter with aerodynamic diameter less than 10 micrometers
PO project officer
QA quality assurance
QAO quality assurance officer
QAPP quality assurance project plan
QC quality control
QCS quality control sample
QMP Quality Management Plan
SAT school air toxics
SOP standard operating procedure
RMO Records Management Office
TSA technical systems audit
TSP total suspended particulate
VTC verification test coordinator
XRF X-ray fluorescence
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A4 DISTRIBUTION LIST
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Vendor
Krag Petterson
Pall Corporation
3669 State Route 281
Cortland,NY13045
U.S. EPA
John McKernan
U.S. Environmental Protection Agency (EPA)
National Risk Management Research Laboratory
26 W. ML. King Dr.
Cincinnati, OH 45268
Motria Caudill
U.S. EPA Region 5
Ralph Metcalfe Federal Building
77 West Jackson Blvd.
Chicago, IL 60604-3507
Michael Jones
U.S. EPA
Office of Air Quality Planning and Standards
109 T.W. Alexander Drive
Research Triangle Park, NC 27709
Ohio EPA
Randy Hock
Division of Air Pollution Control
Ohio Environmental Protection Agency
50 West Town Street, Suite 700
Columbus, OH 43215
Battelle
Thomas Kelly
Amy Dindal
Zachary Willenberg
Rosanna Buhl
Battelle
505 King Ave.
Columbus, OH 43201
Peer Reviewers
Dennis Mikel
U.S. Environmental Protection Agency
Office of Air Quality Planning and
Standards
Research Triangle Park, NC 27711
Rudy Eden
Laboratory Services and Source Testing
South Coast Air Quality Management
District
21865E. Copley Drive
Diamond Bar, CA 91765
Other
John Cooper
Cooper Environmental Services LLC
10180 SW Nimbus Avenue
Suite J6
Portland, Oregon 97223
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A5 VERIFICATION TEST ORGANIZATION
The verification test described in this document will be conducted under the Environmental
Technology Verification (ETV) Program. Verification activities will be overseen by Battelle,
which is managing the ETV Advanced Monitoring Systems (AMS) Center through a cooperative
agreement with the U.S. Environmental Protection Agency (EPA) National Risk Management
Research Laboratory (NRMRL). Verification testing will be carried out in collaboration with
EPA Region 5, EPA's Office of Air Quality Planning and Standards (OAQPS), and the Ohio
Environmental Protection Agency (OEPA). The scope of the AMS Center covers verification of
monitoring technologies for contaminants and natural species in air, water, and soil.
This verification test will be conducted at two OEPA monitoring sites in eastern Ohio. The
testing will involve continuous operation of a commercial monitor for determining toxic metals
in atmospheric particulate matter, at sites where reference samples will be collected on filters for
subsequent laboratory analysis for metals. The commercial monitor will be purchased by EPA,
and will be housed for testing in a shelter purchased by EPA and built by the vendor of the
monitor. The continuous monitor results and the filter-based reference results will be compared
to evaluate the monitor's capability for metals monitoring. The vendor of the metals monitor
being tested will install, and if necessary repair or maintain, their monitor during the verification
test, and will train OEPA, EPA Region 5, and OAQPS staff in operation of the monitor.
Quality assurance (QA) oversight of this EPA Category III verification test will be provided by
the Battelle AMS Center Quality Manager and the EPA AMS Center Quality Manager. The
organization chart in Figure 1 identifies the responsibilities of the organizations and individuals
associated with the verification test. Roles and responsibilities are defined further below.
A5.1 Battelle
Dr. Thomas Kelly is the AMS Center Verification Test Coordinator (VTC) for this test. In this
role, Dr. Kelly will have overall responsibility for ensuring that the technical, schedule, and cost
goals established for the verification test are met. Specifically, he will:
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Battelle
Management
Battelle AMS Center
Quality Manager
Rosanna Buhl
Quality Assurance
Officer
Zachary Willenberg
AMS Center
Stakeholders
Battelle AMS
Center Manager
Amy Dindal
Verification Test
Coordinator
Thomas Kelly
Battelle
Support Staff
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EPA AMS Center
Project Officer
John McKernan
EPA AMS Center Quality
Manager
Laurel Staley
EPA Region 5,
OAQPS, OEPA
Figure 1. Organizational Chart
Hold a kick-off meeting approximately one week prior to the start of the verification
test to review the critical logistical, technical, and administrative aspects of the
verification test,
Coordinate with EPA Region 5, OAQPS, and OEPA in performing the verification
test in accordance with this QA project plan (QAPP),
Ensure that all quality procedures specified in the QAPP and in the AMS Center
Quality Management Plan1 (QMP) are followed,
Maintain real-time communication with the Battelle AMS Center Manager and
Quality Manager, and EPA AMS Center Project Officer and Quality Manager on any
potential or actual deviations from the QAPP,
Prepare the draft and final QAPP, verification report, and verification statement,
Revise the draft QAPP, verification report, and verification statement in response to
reviewers' comments,
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Support OEPA as needed in establishing the necessary infrastructure at the test site to
carry out the test,
Coordinate a performance evaluation (PE) audit of the reference sampling and
analysis methods,
Provide test data, including data from the first day of testing, to the Battelle AMS
Center Manager and EPA AMS Center Project Officer and Quality Manager,
Conduct a technical review of all test data,
Perform analysis of the collected data to carry out the statistical evaluations defined
in this QAPP,
Call on Battelle staff as needed for support in test coordination, data analysis, and
reporting,
Respond to any issues raised in assessment reports and audits, including instituting
corrective action as necessary,
Serve as the primary point of contact for vendor representatives and collaborators,
Coordinate distribution of the final QAPP, verification report, and verification
statement, and
Establish a budget for Battelle activities in the verification test and manage staff to
ensure the budget is not exceeded.
Ms. Amy Dindal is Battelle's Manager for the AMS Center. Ms. Dindal will:
Review the draft and final QAPP,
Review the draft and final verification report and verification statement,
Ensure that necessary Battelle resources, including staff and facilities, are committed
to the verification test,
Ensure that confidentiality of sensitive vendor information is maintained,
Review QAPP deviations and any issues raised in assessment reports, audits, or from
test staff observations, and institute corrective action as necessary,
Maintain communication with EPA's AMS Center Project Officer and Quality
Manager, and
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Facilitate a stop work order if Battelle or EPA QA staff discovers adverse findings
that will compromise data quality or test results.
Ms. Rosanna Buhl is Battelle's Quality Manager for the AMS Center. Ms. Buhl will:
Review the draft and final QAPP,
Assign a Quality Assurance Officer (QAO) for this verification test,
Delegate to other Battelle quality staff any QAO responsibilities assigned below as
needed to meet project schedules,
Review any audit checklists prepared by the QAO for completeness and detail,
Review draft and final audit reports prior to release to the VTC and/or EPA for clarity
and appropriate assessment of findings,
Review audit responses for appropriateness,
Review and approve the QAPP and any deviations,
Review draft and final verification report(s) and verification statement(s),
Maintain real-time communication with the QAO on QA activities, audit results, and
concerns,
Work with the QAO, VTC, and Battelle's AMS Center Manager to resolve data
quality concerns and disputes, and
Recommend a stop work order if audits indicate that data quality or safety is being
compromised.
Mr. Zachary Willenberg is Battelle's QAO for this test. Mr. Willenberg will:
Attend the verification test kick-off meeting and lead the discussion of the QA
elements of the kick-off meeting checklist,
Prior to the start of verification testing, verify the presence of applicable training
records, including any vendor-provided training on the metals monitor being tested,
Conduct a technical systems audit (ISA) of the field testing and the reference
analytical laboratory near the beginning of the verification test,
Review results of the PE audit of reference sampling and analysis methods,
Conduct audits of data quality (ADQs) to verify data quality,
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Prepare and distribute an audit report for each audit,
Verify that audit responses for each audit finding and observation are appropriate and
that corrective action has been implemented effectively,
Communicate to the VTC and/or technical staff the need for immediate corrective
action if an audit identifies QAPP deviations or practices that threaten data quality,
Provide a summary of the QA/QC activities and results for the verification report,
Review the draft and final verification report and verification statement,
Maintain real-time communication with the Battelle Quality Manager on QA
activities, audit results, and concerns, including potential schedule and budget
problems, and
Communicate data quality concerns to the VTC and/or Battelle's AMS Center
Quality Manager; recommend the need for a stop work order if audits indicate that
data quality or safety is being compromised.
A5.2 Vendor
The metals monitor to be tested was developed and will be manufactured by Cooper
Environmental Services LLC (CES), but the rights to the metals monitor technology are owned
by Pall Corporation. Pall Corporation and CES will jointly fulfill the following responsibilities
of the metals monitor vendor, except as noted when one or the other organization has
responsibility for a particular item:
Review and provide comments on the draft QAPP,
Pall Corporation will approve the final QAPP prior to test initiation,
Provide a representative to participate in the kick-off meeting for the verification test,
CES will provide all supplies/reagents/consumables needed to operate the metals
monitor for the duration of the verification test upon purchase of the monitor by EPA,
Pall Corporation will supply a representative to assist with installing the metals
monitor at the field site, and to be available for consultation in maintenance or repair
of the monitor,
Provide training to EPA Region 5, OAQPS, and OEPA personnel in operating and
maintaining the metals monitor, and written consent for OEPA staff to operate the
monitor for purposes of verification testing,
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CES will provide written instructions for routine operation of the metals monitor,
such as a user's manual, Standard Operating Procedure (SOP), and/or a daily
checklist of diagnostic and/or maintenance activities, and
Pall Corporation will review and provide comments on the draft verification report
and verification statement.
A5.3 U.S. EPA ETV Program
EPA's responsibilities in the ETV program are based on the requirements stated in the
r\ _^^^
"Environmental Technology Verification Program Quality Management Plan" (ETV QMP).
The roles of specific EPA testing staff in this verification will be as follows:
Dr. John McKernan is EPA's Project Officer for the AMS Center. In this verification Mr. Julius
Enriquez will assist in the role of Project Officer while Dr. McKernan is on another assignment.
Mr. Enriquez will review the draft QAPP. Dr. McKernan will:
Approve the final QAPP,
Review and approve deviations to the approved final QAPP,
Review the first day of data from the verification test and provide immediate
comments if concerns are identified,
Review the draft verification report and statement,
Oversee the EPA review process for the QAPP, verification report, and statement,
and
Coordinate the submission of the QAPP, verification report, and statement for final
EPA approval.
EPA's AMS Center Quality Manager or designated QA representative will:
Review the draft QAPP,
Review deviations to the approved final QAPP,
Review the first day of data from the verification test and provide immediate
comments if concerns are identified,
Perform at his/her option one external TSA and/or audit of data quality during the
verification test,
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Notify the EPA AMS Center Project Officer of the need for a stop work order if an
external audit indicates that data quality or safety is being compromised,
Prepare and distribute an assessment report summarizing results of the external audit,
and
Review the draft verification report and statement.
A5.4 U.S. EPA Region 5 and OAQPS
EPA Region 5 and OAQPS will coordinate with Battelle and OEPA in performance of the
verification test. Ms. Motria Caudill will be the primary EPA Region 5 point of contact, and Mr.
Michael Jones will be the primary OAQPS point of contact. EPA OAQPS will:
Purchase an Xact 625 metals monitor for testing,
Purchase a Partisol Plus 2025 Sequential Ambient Particulate Sampler for use as the
reference sampler in the field test of the Xact 625.
Additional responsibilities of EPA Region 5 and OAQPS will be as follows:
Coordinate with the vendor for training of EPA Region 5, OAQPS, and OEPA staff in
operation of the metals monitor,
Provide an SOP for operation and sample recovery with the reference method
sampling system at the field site,
Arrange for laboratory analysis of collected reference method samples by a certified
analytical laboratory [Eastern Research Group (ERG)],
Review the draft QAPP,
Provide a representative to participate in the kick-off meeting for the verification test,
and
Review the draft verification report and statement.
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A5.5 Ohio EPA
Ohio EPA will provide field sites and supporting infrastructure to carry out the test, and OEPA
staff will operate the metals monitor and conduct reference method sampling at the site. OEPA
staff will be in frequent communication with the Battelle VTC and EPA Region 5 and OAQPS
staff, and with the technology vendor as needed. All such communication will be documented,
and the Battelle VTC will keep EPA's Project Officer for the AMS Centerjnformed of these
communications. Mr. Randy Hock, in OEPA's Columbus, Ohio headquarters, will be the
primary OEPA point of contact. The responsibilities of OEPA staff will be to:
Coordinate with EPA Region 5, OAQPS, and the vendor to install the metals monitor
to be tested at the test sites,
Provide a representative to participate in the kick-off meeting for the verification test,
Prepare the test sites to ensure suitable space and electrical power to perform the
necessary testing activities,
Receive training in operation of the metals monitor from the vendor,
Operate the metals monitor throughout the field test,
Coordinate the operation of the test sites for the purposes of ETV testing,
Communicate needs regarding access, security, and safety to any staff working or
visiting at the test sites,
Perform ambient particulate sampling using an appropriate filter-based collection
method and send samples to the analytical laboratory conducting metals analysis,
Record qualitative observations about the maintenance and operation of the metals
monitor during testing,
Ensure that the metals monitor data and any field records are reviewed within one
week of generation, and transmitted to the Battelle VTC on at least a weekly basis,
Provide input in responding to any issues raised in assessment reports and audits
related to site operations,
Provide input on test procedures, technology operation and maintenance, and field
conditions for the draft verification report, and
Review the draft verification report and statement as needed.
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A5.6. Verification Test Peer Reviewers
This QAPP and the verification report and verification statement based on testing described in
this document will be reviewed by experts in the fields related to paniculate metals and/or
analytical instrumentation. The following experts have agreed to provide a peer review of this
QAPP and the resulting verification report and statement.
Dennis Mikel, EPA/Office of Air Quality Planning and Standards [EPA QA coordinator
for the School Air Toxics (SAT) program]
Rudy Eden, South Coast Air Quality Management District
The responsibilities of verification test peer reviewers include:
Participate in technical panel discussions (when available) to provide input to the test
design,
Review and provide input to the QAPP, and
Review and provide input to the verification report and verification statement.
A6 BACKGROUND
A6.1 Technology Need
The ETV Program's AMS Center conducts third-party performance testing of commercially-
available technologies that detect or monitor natural species or contaminants in air, water, and
soil. Stakeholder committees of buyers and users of such technologies recommend technology
categories, and technologies within those categories, as priorities for testing. Among the
technology categories recommended for testing are continuous monitors for toxic metals present
in atmospheric particulate matter (PM). In particular, the use of metals monitors for determining
toxic metals in PM having aerodynamic diameters smaller than 10 micrometers (known as PMio)
was identified as an area of interest for technology verification.
Many industrial communities are burdened by emissions of toxic metals such as lead (Pb),
manganese (Mn), and chromium (Cr). For example, EPA's SAT Monitoring Initiative3 has
disclosed that Mn, a neurotoxic metal, is one of the pollutants of greatest potential risk near
schools in industrialized locations. Existing monitoring methods for metals in airborne PM have
significant limitations, in that samples are collected over a 24-hour integrated period and must be
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submitted for laboratory analysis, from which results may not be available for several weeks.
Commercially-developed metals monitors are now available that can determine 10 or more toxic
metals simultaneously in ambient PMio with time resolution of one hour or less. The relatively
fast response afforded by such monitors may be useful in identifying emission sources and
allocating the contributions of such sources to local levels of toxic metals. Specifically, the
advantages of hourly metals data (relative to 24-hour average data) are:
Improved ability to follow variations in metals concentrations associated with time of day
or meteorological conditions, and thus to attribute metals risk to a particular source,
Ability to compile a dataset large enough to conduct source receptor modeling, and
Cost reduction and time savings due to the generation of multi-metals data on-site
without waiting for laboratory analysis.
Thus deployment of metals monitoring may lead to better characterization of environmental
metals exposures and more effective source identification, allowing decision-makers to quickly
target industries for enforcement action or voluntary emissions reduction.
A.6.2 Technology Description
Commercial instruments for monitoring of metals in atmospheric PMio are based on the principle
of X-ray fluorescence (XRF), in which X-rays from a source cause removal of an electron from
an inner electronic shell of a metal atom in a sample. The vacancy in the inner shell is then filled
by an electron from an outer shell, with resulting emission of an X-ray whose wavelength is
longer than that of the original excitation and characteristic of the metal in question. The
wavelength (or, equivalently, the energy) and intensity of the emitted X-rays are determined to
identify and quantify the metal in the sample. Multiple metals in the sample are excited and
detected simultaneously. For monitoring of metals in atmospheric PM, an automated moveable
filter tape system is used, in which a sample air flow is drawn through a small spot on the tape,
collecting and concentrating PM onto that spot. After a pre-set sampling interval, the tape
advances, placing the collected sample spot in the X-ray excitation and analysis section of the
instrument, and initiating sampling onto a previously unexposed spot on the tape. The sequence
of sampling and analysis can continue automatically, limited only by the supply of filter tape.
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The duration of sample collection at each spot can be varied to maintain detection performance
in the face of varying atmospheric PM levels.
The specific commercial metals monitor evaluated under this QAPP is the Xact 625, previously
manufactured by Cooper Environmental Services LLC (Portland, OR). Commercial rights to the
Xact technology are owned by Pall Corporation (Port Washington, NY). The following
description of the Xact 625 technology is based on information provided by the vendor (this
information was not verified in this test). The Xact 625 employs energy-dispersive X-ray
fluorescence (EDXRF), in which the detector and electronics resolve emitted X-rays based on
their energy. The EDXRF approach allows use of a relatively simple optical path and a
relatively low power X-ray source, and thus reduces the instrument cost. The EDXRF approach
also provides acquisition of the entire X-ray spectrum very rapidly, so that many elements in the
periodic table can be detected within a few seconds. The Xact 625 samples ambient air at a
constant flow rate of 16.7 L/min (i.e., 1 m3/hr). The Xact 625's sample inlet is designed to
provide uniform sample deposition, and the instrument analyzes approximately 90% of the
sample spot area, to minimize effects of sample inhomogeneity. In addition to the general
features of ambient metals monitors outlined above, the Xact 625 employs automatic internal
stability checks (described in Section B5) to track the monitor's performance
A7 VERIFICATION TEST DESCRIPTION AND SCHEDULE
The purpose of this verification test is to generate performance data on metals monitoring for
airborne PM, with a particular focus on monitoring of toxic metals in atmospheric PMio in
industrialized areas. The data generated from this verification test are intended to provide
organizations and users interested in metals monitoring with information on the potential use of
these monitors for that application and on their performance under such conditions.
A7.1 Verification Test Description
The test described in this QAPP will be conducted by operating a metals monitor at each of two
field sites for up to eight weeks, and comparing the monitor results for several metals to the
results from conventional reference measurements made by laboratory analysis of 24-hour filter
samples collected at the same site. The monitor readings for each metal will be averaged over
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the appropriate 24-hour periods for comparison to the reference results. The metals monitor will
be evaluated on the following performance parameters.
Comparability
Correlation
Bias
Data completeness
Operational factors
Comparability, correlation, and bias will be assessed by comparison of monitor and reference
results, using the statistical approaches described in Section B 1.2. Data completeness will be
determined from the number of hourly periods the metals monitor provides readings of PMio
metals concentrations (allowing for daily periods of approximately 30 minutes in which the Xact
625 performs internal QA checks). Data completeness will be determined both relative to the
entire test period and relative to each 24-hour reference sampling period. Operational
performance factors such as maintenance requirements, ease of use, and effectiveness of data
acquisition will be determined from observations by the field testing staff. This test is not
intended to simulate long-term performance of the metals monitor at a monitoring site, but rather
to assess the feasibility of its use for ambient metals monitoring in near-source locations. In
long-term use, metals monitoring procedures might be tailored to address the specific conditions,
metals concentrations, and sources for a given site. This test also will not evaluate the precision
of the individual metals monitor in repetitive analysis of the same sample, as ambient
atmospheric sampling does not provide known constant samples to assess precision. That
performance factor will be evaluated in a separate project.4 Similarly, with only a single unit of
the metals monitor involved in the test, the unit-to-unit duplication of multiple monitors of the
same type cannot be determined.
Subsequent to the verification test, Battelle will draft a verification report for the metals monitor.
The report will be reviewed by the technology vendor, by EPA Region 5 and OAQPS staff, and
by peer reviewers, and will be revised and submitted to EPA NRMRL for final approval. In
performing the verification test, Battelle will follow the technical and QA procedures specified in
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this QAPP and will comply with the data quality requirements in the AMS Center QMP and the
ETVQMP.1
A7.2 Proposed Testing Schedule
Table 1 shows the expected schedule of testing and data analysis/reporting activities to be
conducted in this verification. The metals monitor field testing is planned to take place from
August to December 2011, with equal time spent at two test sites within that period. Table 1 also
notes the approximate timing of the field and laboratory TSAs and of the ADQs.
A7.3 Test Sites
The sites for testing will be at OEPA air quality monitoring sites in East Liverpool and Marietta,
Ohio, on Ohio's eastern and southeastern border, respectively. Both sites are located near the
Ohio River, in industrialized areas along the river that are characterized by restricted air flow due
to local terrain. Elevated levels of Mn and other metals have been found in ambient total
suspended particulate (TSP) at these sites, and at nearby elementary schools.
The metals monitor to be tested will be installed in an air-conditioned trailer provided by EPA,
parked in a secure location at each OEPA site. The trailer in which the metals monitor will be
installed is approximately 6.9 m (22.5 ft) overall, including the hitch. The air conditioned
enclosure for the metals monitor is approximately 3 m (L) x 2 m (W) x 2.6 m (H) [10 ft (L) x 6.7
ft (W) x 8.5 ft (H)]. The PMio inlet of the Xact 625 metals monitor will be placed on the roof of
this enclosure as close as possible to, and no more than 10 meters from, the inlet of the PMio
reference sampler, and will be connected to the metals monitor by a straight vertical pipe
connection to minimize any loss of ambient particles during passage of sample air to the monitor.
The Xact 625 metals monitor, reference sampler, and other equipment will be powered by fixed
electrical power lines installed at the sites for this test.
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Table 1. Planned Verification Test Schedule
Approximate
Dates
August 9-10,
2011
August 9-11,
2011
August 12 -
October 7,
2011
October 8-1 2,
2011
October 1 3 -
December 8,
2011
December 9-
10,2011
December
2011-
January,
2012
February,
2012
March, 201 2
April, 2012
Location
Columbus,
OH
East
Liverpool,
OH
East
Liverpool,
OH
Marietta,
OH
Marietta,
OH
Marietta,
OH
Columbus,
OH
Columbus,
OH
Columbus,
OH
Columbus,
OH
Verification Activities
Testing
Training in operation of
the monitor
Installation of monitor at
test site
Kickoff meeting with all
participants
Continuous monitoring of
target metals
Reference method
sampling
Installation of monitor at
test site
Refresher train ing in
operation of the monitor
Continuous monitoring of
target metals
Reference method
sampling
Conclusion of verification
test
Remove monitor from test
site
Data Analysis and Reporting
Conduct TSA of field testing and
reference laboratory
Compile data from metals monitor
Review and summarize
observations from field operators
Compile metals data from reference
method
Begin statistical comparisons of
reference and monitor results
Conduct audit of data quality
Develop ETV draft report template
Compile data from metals monitor
Review and summarize
observations from field operators
Compile metals data from reference
method
Continue statistical comparisons of
reference and monitor results
Continue draft ETV report
Complete statistical comparisons of
reference and monitor results
Complete draft ETV report Conduct
final audit of data quality
Submit draft ETV report for peer
review, and revise
Submit draft ETV report for EPA QA
review, and revise
Submit final ETV report for EPA
approval
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AS QUALITY OBJECTIVES FOR MEASUREMENT DATA
The objective of this verification test is to evaluate the performance of the Xact 625 metals
monitor under conditions relevant to ambient particulate metals monitoring. This evaluation will
assess the capabilities of the monitor for determining metals concentrations in the ambient air.
The verification test will also rely upon operator observations to assess other performance
characteristics of the monitor being tested including data completeness, ease of use, and
maintenance requirements.
Data quality indicators (DQIs) ensure that this verification test provides suitable data for a robust
evaluation of performance. DQIs have been established for reference sampler flow rate accuracy
and the accuracy of the reference method measurements. The DQIs were established to ensure
that data used to support the quantitative performance evaluations of the Xact 625 metals
monitor are of sufficient quality.
Quantitative performance of the metals monitor will be assessed by comparison to well-
established reference sampling and analytical methods. To assure that those methods provide
data of sufficient quality for a robust evaluation of metals monitor performance, accuracy data
quality indicators (DQI's) have been established for the reference sampler flow rate and for the
analytical method. Specifically, the measurement quality objective (MQO) for the reference
sampler flow rate is that it be within ฑ5% of the target flow rate for the sampler. The MQO for
the analytical accuracy is that reported metals concentrations be within ฑ10% of the true value.
The degree of attainment of both of these DQO's will be assessed by means of PE audits
conducted during the testing. The procedures and schedule for the PE audits are described in
Section C 1.1.
The Battelle QAO will perform a TSA of laboratory and field-based testing activities to augment
the normal operational and QA/QC requirements of the metals monitor and the reference
sampling and analytical methods. A TSA of the field testing activities will be performed within
the first two weeks of the field testing, and will be followed by a TSA of the analytical
laboratory within the first two weeks that reference samples from the field are being analyzed.
The EPA Quality Manager also may conduct an independent TSA, at her discretion.
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A9 SPECIAL TRAINING/CERTIFICATION
Documentation of training related to technology testing, field testing, data analysis, and reporting
is maintained for all Battelle technical staff in training files at their respective locations. The
Battelle QAO may verify the presence of appropriate training records prior to the start of testing.
Battelle technical staff supporting this verification test will have a minimum of a bachelor's
degree in science/engineering. Training of EPA Region 5, OAQPS, and OEPA staff by the
vendor will be documented, and the vendor will indicate by signature that those staff are suitably
trained to operate the Xact 625 monitor for testing. The metals monitor vendor will only operate
the technology for training of testing staff and as needed for maintenance or repair activities
during the verification test.
The verification test described in this QAPP will be performed at sites operated by the OEPA.
All participants in this verification test (i.e., Battelle, EPA, and vendor staff) will adhere to the
health and safety requirements of the OEPA sites. OEPA testing staff will give a site-specific
safety briefing to all staff visiting either of the test sites. This briefing will include a description
of:
Any emergency operating procedures (i.e., in case of fire, tornado),
Identification, location, and operation of any safety equipment (e.g., fire alarms, fire
extinguishers, eye washes, exits), and
Any personal protective equipment requirements and site-specific procedures.
A10 DOCUMENTATION AND RECORDS
The documents and records for this verification test include this QAPP, chain-of-custody forms,
laboratory record books (LRB), data collection forms, electronic files (both raw data and
spreadsheets), and the final verification report. All of these documents and records will be
maintained at the field site during the test, and will be reviewed on at least a weekly basis by
OEPA to ensure that records have been filled in and are up to date. Copies of all reference
sample chain-of-custody forms will be retained on site. These documents and records will be
transferred to permanent storage at Battelle's Records Management Office (RMO) at the
conclusion of the verification test. Documents and records generated at the test site will be
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stored in a secure location until they can be copied and/or transferred to the VTC. Electronic
documents and records will also be uploaded to a SharePoint site designated for this test and will
be available to EPA upon request. All Battelle LRBs will be stored indefinitely by Battelle's
RMO. EPA will be notified before disposal of any files. Section BIO further details the data
recording practices and responsibilities.
All data generated during the conduct of this project will be recorded directly, promptly, and
legibly in ink. All data entries will be dated on the date of entry and signed or initialed by the
person entering the data. Any changes in entries will be made so as not to obscure the original
entry, will be dated and signed or initialed at the time of the change and shall indicate the reason
for the change. Data recording and chain-of-custody forms for the reference sampling method
will be used in testing at both sites; an example of those forms is shown as Appendix A of this
QAPP. The draft forms will be provided to the Battelle QAO for review prior to use so that
appropriate changes, if any, can be made.
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SECTION B
DATA GENERATION AND ACQUISITION
Bl EXPERIMENTAL DESIGN
The verification test described in this QAPP will be conducted consistent with the requirements
of the ETV AMS Center QMP,1 the ETV Program QMP,2 and the draft SAT Program QAPP.4
This QAPP specifically addresses verification of continuous metals monitors for ambient air
monitoring applications by evaluating the following performance parameters.
Comparability
Correlation
Bias
Data completeness
Operational factors
The verification test will be conducted over a period of approximately four months. The
installation and training period at the first test site is scheduled to begin in early August, 2011.
The Xact 625 monitor undergoing verification will report ambient concentrations of
approximately 20 metals on an hourly basis. The monitored metals concentrations will be
averaged over 24 hour time periods for comparison to ambient concentrations determined from
time-integrated filter sampling and subsequent laboratory analysis. Section Bl.l describes the
test procedures, and Section B1.2 describes the statistical calculations that will be used in those
evaluations.
A verification report will be prepared for the metals monitor upon completion of testing,
presenting the test procedures and test data, as well as the results of the statistical evaluation of
those data. The verification report will briefly describe the ETV program, the AMS Center, and
the procedures used in verification testing. The results of the verification test regarding metals
monitor performance will be stated quantitatively. The draft verification report will be subjected
to review by the metals monitor vendor, EPA, and other peer reviewers. The resulting review
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comments will be addressed in a subsequent revision of the report, and the peer review
comments and responses will be tabulated to document the peer review and QA review process
for EPA. The reporting and review process will be conducted according to the requirements of
the ETV/AMS Center QMP.1
Bl.l Test Procedures
The Xact 625 metals monitor undergoing verification will be installed at an appropriate secure
location at each of the two OEPA test sites in turn, according to the schedule shown in section
A7.1, and between 2 and 10 meters from the inlet of the reference PMio sampler. The Xact 625
metals monitor will operate continuously and on an hourly basis will report the measured
ambient concentration of each of the analytes listed in Table 2.
Table 2. Target Analytes for Xact 625 Metals Monitor
Metal
Antimony
Arsenic
Barium
Bromine
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Manganese
Symbol
Sb
As
Ba
Br
Cd
Ca
Cr
Co
Cu
Fe
Pb
Mn
Metal
Mercury
Molybdenum
Nickel
Potassium
Rubidium
Selenium
Strontium
Thallium
Thorium
Titanium
Zinc
Symbol
Hg
Mo
Ni
K
Rb
Se
Sr
Tl
Th
Ti
Zn
Table 3 presents a summary of the quantitative tests to be performed, showing the performance
parameters, the objective of each parameter, the basis for evaluation of each parameter, and the
number of data points or comparisons to be included in the evaluation. Table 3 assumes that a
24-hour reference sample will be obtained on every day over a 16-week period (112 total
reference samples for each target metal), and that the metals monitor will report data on an
hourly basis (2,688 total measurements of each target metal over the test period). The hourly
monitoring data will be converted to daily averages for comparison with the reference data. The
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numbers of data points indicated in Table 3 apply to each of the more than 20 metals to be
determined in the test.
Table 3. Summary of Tests and Testing Frequency
Performance
Parameter
Comparability
Correlation
Bias
Data
Completeness
Objective
Determine
relationship of
metals monitor
results to
reference results
Determine degree
of correlation of
metals monitor
results with
reference results
Determine
quantitative
agreement of
metals monitor
results and
reference results
Determine data
return of metals
monitor relative to
maximum possible
Determine data
return of metals
monitor relative to
reference
sampling periods
Evaluation
Based On
Slope and intercept of
linear regression of
averaged metals
monitor results against
reference results
Coefficient of
determination of linear
regression of averaged
metals monitor results
against reference
results
Mean, standard
deviation, and range of
percent difference
values of metals
monitor results relative
to corresponding
reference results
Number of hours of
valid data relative to all
hours in the test
Number of 24-hour
reference periods in
which metals data are
obtained for over half
the hours
Number of
Data Points
112a
112a
112a
2,688a
112a
a: For each target metal, if detected in all samples
Throughout the verification test, the metals monitor undergoing testing will be operated by
OEPA staff trained by the vendor. However, the intent of the testing is for the metals monitor to
operate in a manner simulating use by site operators to monitor ambient air with little user
intervention. As a result, it is expected that once the verification test has begun, no adjustment or
recalibration will be performed. Repair or maintenance procedures may be carried out at any
time, but testing will not be interrupted, and data completeness will be reduced if such activities
prevent collection of metals monitor data required for verification. All repair and maintenance
efforts will be documented including the type of repair or maintenance, the length of time needed
to make the repair or conduct maintenance, and the cost of any consumables or replacement
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parts. OEPA staff will download metals monitor data from the monitor's software for transfer to
permanent electronic records.
B1.2 Statistical Methods
The statistical methods and calculations to be used for evaluation of quantitative performance are
described in the following subsections. All measurement results from both the Xact 625
monitor (i.e., hourly data) and the reference method (i.e., 24-hour integrated data) will be
reported as ambient metals concentrations [e.g., in nanograms per cubic meter of air (ng/m3)] and
graphically displayed in the test report. Care will be taken to assure that the volume units used in
reported metals concentrations from the two methods are identical (i.e., standard conditions, or
actual volume). Non-detect results from the reference method for any metal will be flagged as
such, and excluded from any data comparisons. Although data comparisons are nominally based
on a 24 hour sampling period, the Xact 625 data will actually consist of 23 measurements of 1-
hour duration and one measurement of 0.5- hour duration on each test day (due to the
performance of 0.5-hour internal QA checks by the Xact 625 each day). It is planned that the
0.5-hour measurement will be made from 12:30 to 1:00 am, following the performance of the
internal QA checks between midnight and 12:30 am. To assure accurate comparisons, the
reference sampling will also be conducted over the same 23.5 hour duration within each 24-hour
period.
The ambient concentration results from the reference method and the Xact 625 metals monitor
are calculated based on the known sample flow rate and sample duration of each respective
method. Consequently, no further normalization of the concentration results relative to those
factors will be necessary. However, the Xact 625 readings on each test day consist of 23 1-hour
measurements and one 0.5-hour measurement, with all sampling done at the same flow rate (i.e.,
16.7 L/min). Consequently, integration of the Xact 625 results over a daily 23.5 hour time
period requires simple arithmetic averaging of the 24 total concentration results, but with the 0.5-
hour result given half the weight of the 23 1-hour results, i.e.:
23.5 Hour Average = (0.5ci + c2+ ...c24)/23.5 (1)
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Where ci, C2, ... C24 are the metals concentrations reported each hour by the Xact 625. The
resulting daily concentration results from the Xact 625 metals monitor will be compared to the
corresponding 23.5-hour integrated sample results from the reference method.
Statistical comparisons are not needed for evaluation of the qualitative performance of the metals
monitor, i.e., the operational factors. Those factors will include the ease of operation and data
collection, the need for consumables and routine maintenance, the amount and nature of any
waste generated, and the extent of repair or replacement efforts. These factors will be evaluated
based on observations of the OEPA site operators, EPA Region 5 staff, and Battelle staff, and by
communication with vendor representatives. Examples of information to be recorded may
include the daily status of diagnostic indicators, use or replacement of any consumables, the
effort or cost associated with maintenance or repair, vendor effort (e.g., time on site) for repair or
maintenance, the duration and causes of any down time or data acquisition failure, operator
observations about technology startup, ease of use, clarity of the vendor's training, and user-
friendliness of monitor software. Battelle will summarize these observations to aid in describing
the metals monitor performance in the test report.
B1.2.1 Comparability
The overall comparability of the continuous monitors to the reference method will be assessed by
comparison of the ambient metals concentrations determined simultaneously by the two
methods. For each target metal, comparability will be assessed from a linear regression of the
data using the reference method results as the independent variable and the continuous monitor
results as the dependent variable, as follows.
G = (m-Ri) + b (2)
Where R; is the ith reference measurement (for a 23.5-hour period), C; is the average of the Xact
625 continuous metals monitor measurements over the same 23.5-hour time period, and b and m
are the intercept and slope of the linear regression, respectively. Comparability will be reported
in terms of the slope and intercept values obtained from the linear regression for each metal
determined by the metals monitor and the reference method. In the absence of bias, the
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regression slope would be 1.0 and the intercept would be zero. The slope and intercept values
for each metal will be reported, along with associated 95% confidence intervals, by means of the
LINEST linear regression function in Microsoft Excelฎ. The test report will indicate whether
each reported slope or intercept value is significantly different from 1.0 or from zero,
respectively (i.e., whether the 95% confidence interval excludes a slope of 1.0 or an intercept of
zero, respectively).
Bl.2.2 Correlation
The degree of correlation between the metals monitor results and the reference method results
will be determined by the coefficient of determination (r2) of the linear regression between the
23.5-hour reference method results and the corresponding averages of the metals monitor
measurements over the same time periods. A value of r2 close to 1.0 means that the amount of
random error is small, that is, the variability in the continuous measurements is almost entirely
9
explained by the variability in the reference measurements. The r value will be determined and
reported separately for each metal measured.
Bl.2.3 Bias
The bias of the metals monitor readings will be evaluated in terms of the percent difference of
the average metals monitor readings relative to the corresponding 23.5-hour reference method
result. That is, for each target metal (i) in each 23.5-hour reference method period (j), bias for
that metal in that period (B;j) will be calculated as:
By = (Average Monitor Reading - Reference Reading) x IQQ (3)
Reference Reading
Before conducting the calculation shown in Equation 3, the 23.5-hour average concentrations
from the Xact 625 for each test day will be compared to the quantitation limit of the Xact 625 for
each target metal. The quantitation limit is a defined value for each target metal using the Xact
625, and roughly corresponds to 10% uncertainty in an interference-free situation/5-* Daily 23.5-
hour averages for any metal that are less than the Xact 625 quantitation limit for that metal will
be excluded from the calculation of bias using Equation 3. Quantitation limits established by the
vendor for the Xact 625 are listed in Appendix A.
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As noted in Table 3, up to 112 By values will be obtained for each target metal. The impact of
low metals concentrations on the bias results will be investigated by reporting the range, median,
mean, and standard deviation of the individual By results for each metal. Also, the individual
bias results for each metal will be plotted against the ambient metal concentration to determine
whether bias is a function of the ambient concentration of the metal.
Bl.2.4 Data Completeness
Data completeness (DC) will be determined in two different ways. The first will be as the
percentage of all hours in the field period in which the metals monitor reported ambient metals
data, relative to the total number of hours in the field period:
DC1 = (# Hours data return/Total hours in period) x 100 (4)
Data completeness will also be calculated as the percentage of all 24-hour reference
measurement periods during which the monitor reported at least 12 hours of monitoring data
(i.e., produced data for at least half of the reference monitoring period):
DC2 = (# Periods with > 12 hours monitor data/# Reference periods) x 100 (5)
Both forms of data completeness will be calculated for each target metal.
B2. SAMPLING METHODS
Ambient PMio will be sampled for reference metals analysis using a Partisol Plus 2025
Sequential Ambient Particulate Sampler (Thermo Scientific, Hopkinton, MA) equipped with a
PMio size-selective inlet (http://pi.b5z.net/i/u/1640578/f/Thermo/Partisol Plus 2025.pdf).
This sampler is designated by EPA as Reference Method RFPS-1298-127 for sampling of
ambient PMio. The Partisol Plus 2025 exchanges 47 mm diameter Teflon sample filters
automatically after pre-set sampling intervals, and can hold up to 16 filter cassettes, sufficient for
more than two weeks of unattended daily 24-hour sampling. Sample air is pulled by an internal
pump through the filter currently being sampled, with the sample air flow regulated by a mass
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flow controller. Ambient temperature and pressure readings are used along with the mass flow
control to maintain a constant volumetric sampling rate. Previously sampled and yet-to-be-
sampled filters are sealed off within the Partisol Plus 2025 to prevent contamination. The
sampler stores sampling and meteorological data in internal memory, including the average
ambient temperature, ambient pressure, and average ambient relative humidity for each filter
sample.
The Partisol Plus 2025 will be operated by OEPA personnel at the test site. The Partisol Plus
2025 sampling flow rate will be set at approximately 16.7 L/min (equivalent to approximately 1
m3/hr). Samples will be collected every day throughout the field period, with a 23.5 hour
sampling duration (i.e., one sample per day), so that reference sampling does not take place
during the 0.5 hours per day when the Xact 625 performs its internal QA checks. That 0.5 hour
period will be scheduled at the same time of day on every test day so that reference and Xact 625
sampling intervals are consistent throughout the test period. Collected filter samples can be
removed from the Partisol Plus 2025 sampler without interruption of sampling onto the current
filter. Collected samples will be shipped to ERG in batches on a weekly basis, or more
frequently, for extraction and analysis. OEPA staff will download sampling data from the
Partisol Plus 2025 internal software by means of an RS232 interface, and provide the electronic
files of such data to EPA Region 5, OAQPS, Battelle, and ERG.
B3. SAMPLE HANDLING AND CUSTODY
Reference samples for determination of ambient PMio mass and metals concentration will be
collected by OEPA staff using the Partisol Plus 2025 sampler, according to EPA Method IO-3.16
that calls for sampling of ambient air at a known constant flow rate for a specified time interval
through filters that have been weighed before sampling, and that are then weighed again after
sampling. The atmospheric PMio mass concentration [in micrograms per cubic meter (ug/m3)] is
determined from the difference in the filter weights and the volume of air sampled. Method IO-
3.1 also defines procedures for the extraction of metals from the collected parti culate filter for
subsequent analysis.
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Pre-weighed, individually identified 47 mm Teflon filters will be prepared by ERG and shipped
to OEPA personnel. OEPA will install clean filters in the sampler at the field site, document the
identification of each filter, collect ambient PMio samples according to the schedule defined in
Section B2, and ship the collected filter samples back to ERG for weighing, extraction, and
reference metals analysis. Filters will be returned to ERG in the same individual filter containers
in which they were sent to the field. The particulate trace metals to be determined are non-
volatile and not reactive, so no storage temperature or holding time requirements apply to the
collected samples. Chain-of-custody (COC) forms (see example in Appendix B) will accompany
the filter samples on return to ERG, and for each reference sample will indicate the filter
identification number, sampling date, start and stop times, flow rate, and requested analytical
method. COC forms will track sample release from the sampling location to the analysis
laboratory. COC forms will be signed by the person relinquishing samples once that person has
verified that the COC form is accurate. Upon arrival at the analysis laboratory, COC forms will
be signed by the person receiving the sample once that person has verified that all samples
identified on the COC forms are present. All COC forms will be delivered to the VTC and
maintained with the test records.
B4. ANALYTICAL METHODS
The reference PMio filter samples will be analyzed by ERG for metals content according to EPA
Method IO-3.57 where collected PMio is digested using microwave or hot acid according to EPA
Method IO-3.16 and then analyzed by inductively coupled plasma/mass spectrometry (ICP/MS).
All samples will be digested using the same procedure to ensure comparability. This analysis
will be performed according to Standard Operating Procedures (SOPs) that are incorporated into
o
ERG's QAPP for sampling and analysis in EPA's national monitoring programs. The QC
requirements of Method IO-3.5 will be followed, including the use of blanks, quality control
samples (QCSs), laboratory fortified blanks (LFBs), internal standards, and tuning solutions, and
an instrument performance demonstration program that includes duplicate samples, standards,
blanks, interference check standards, continuing calibration blanks and verification standards,
and laboratory control and matrix spikes.8 The QC requirements and acceptance criteria in Table
8 of Method IO-3.57 will serve as the MQO's for the metals analysis.
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The Method IO-3.5 target analyte list for this test is shown in Table 4, along with estimated
detection limits (in ng/m3) provided by ERG for Method IO-3.5 based on the sampling
conditions described in Section B2 and extraction of the entire 47 mm filter. Not all of the
analytes targeted by the metals monitor (Table 2) are on the analyte list for Method IO-3.5;
bromine, calcium, iron, potassium, rubidium, strontium, and titanium are on the Xact 625 list
(Table 2) but not on the Method IO-3.5 list (Table 4).
Table 4. Target Analytes and Expected Detection Limits for Reference Method IO-3.5
Metal
Antimony
Arsenic
Barium
Cadmium
Chromium
Cobalt
Copper
Lead
Expected3
Detection
Limit (ng/m3)
0.010
0.017
0.083
0.26
5.6
0.019
0.66
0.082
Metal
Manganese
Mercury
Molybdenum
Nickel
Selenium
Thallium
Thorium
Vanadium
Zinc
Expected3
Detection
Limit (ng/m3)
0.051
0.13
0.017
0.57
0.14
0.0080
0.020
0.010
5.5
a: The values listed were obtained from ERG personnel as their best estimates of method performance
Reference and Xact 625 metals monitor data will be compared for all metals that are common to
the analyte lists of the two measurement methods, and present at detectable levels in ambient air.
Data for additional metals determined by either method will also be reported to EPA, though not
used in the metals monitor evaluation. ERG will complete the metals analysis of reference filter
samples and provide draft analytical results to EPA Region 5, Battelle, and OEPA within
approximately seven days after receiving each batch of samples. ERG will provide final
analytical results on each batch of samples in electronic format to EPA Region 5, Battelle, and
OEPA immediately after completion of internal QA review of the results. The ERG analytical
laboratory will be subject to a TSA during analysis of the first week's field samples, as stated in
Section A8.
As an additional analytical effort, the first 25% of reference filter samples (i.e., approximately 28
samples) collected in the field will be subjected to laboratory metals analysis by XRF prior to
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analysis by ICP-MS. The laboratory XRF analysis will be conducted by EPA's National
Exposure Research Laboratory according to an established EPA SOP.9 Collected reference
method samples will be shipped with accompanying chain of custody (CoC) documentation from
the field to the EPA laboratory for XRF analysis. That analysis is non-destructive, so upon
completion of the XRF analysis the samples will be forwarded with accompanying CoC
documentation to ERG for ICP-MS analysis. The ICP-MS results will be the reference data used
to assess the performance of the Xact 625, and the laboratory XRF analysis is not a component
of the ETV verification effort. However, the laboratory XRF data may provide additional
insights for EPA and the Xact 625 vendor into the performance of the Xact 625, by virtue of
employing the same analytical principle as the Xact 625 measurement.
As a check on sample integrity in the XRF analysis process, field blank samples will be
submitted along with the reference samples for XRF analysis, at a rate of 20% (i.e., five field
blanks accompanying the 25 reference samples). Blank results exceeding the 95% confidence
interval of the results from field blanks not subjected to XRF analysis will be taken as evidence
of contamination for an individual metal. In addition, the statistical comparison of ICP-MS data
to Xact 625 data defined in Section B 1.2 will be carried out separately for the reference samples
subjected to EPA laboratory XRF analysis and for those not subjected to that analysis. The
results from the two sets of data for comparability, correlation, and bias will be evaluated and
reported separately. Only if the 95% confidence intervals of the linear regression slope, linear
regression intercept, and average bias overlap will the two sets of reference data be judged
equivalent and combined into one complete data set for reporting and comparison of ICP-MS
and Xact 625 results. If those confidence intervals do not overlap, the two data sets will be
reported and compared to the corresponding Xact 625 results separately. In that case the 75% of
reference samples not subjected to XRF analysis will be the primary reference data used to verify
the Xact 625. This approach will indicate whether the additional sample handling and XRF
analysis process affected the reference samples.
The comparison of ICP-MS and laboratory XRF analysis results from the 25% of reference
samples subjected to both analyses is not part of the ETV verification process. None of the XRF
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data will be included in the verification report. Consequently the procedures for comparing
those data are not presented in this QAPP.
B5. QUALITY CONTROL
Quality control efforts for operation of the Xact 625 metals monitor undergoing testing will
include documenting that OEPA and EPA staff have been properly trained to operate the
monitor, and performing both automated and manual QC checks at vendor-specified intervals.
Adequacy of training will be assured by requiring the metals monitor vendor to certify that
specific EPA and OEPA staff have been trained on operation of the metals monitor and are
approved to operate the monitor for testing.
Automated QC checks performed by the Xact 625 during continuous operation will consist of the
following.
Internal energy alignment check, performed by XRF analysis of a copper rod; conducted
over a 15-minute period starting at midnight each day
Upscale rod check, performed by XRF analysis of a metal rod containing chromium,
lead, copper, and cadmium; conducted once per day over a 15-minute period
Flow check, conducted at the same time as the upscale rod check, determines the Xact
625 sample air flow by insertion of a second mass flow meter into the flow path
Palladium rod stability check, conducted by XRF analysis of a palladium rod in every
ambient sample analysis (i.e., hourly)
These automated checks serve to monitor trends in the Xact 625 's status. The criterion for
stability of the palladium rod check is 10 to 15%, that for the flow check is 10%, and that for the
upscale rod check is more stringent, at 5% for each of the four metals. Variations in check
results outside these criteria result in flags in the monitor's data. The data from the metals
monitor will be reviewed by CES personnel and OEPA field staff, and CES personnel will assess
whether adjustment or maintenance of the Xact 625 monitor is needed based on the observed
data flags. If such actions are needed CES will perform them or instruct OEPA staff how to
perform them.
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Manually initiated QC checks will be conducted upon installation of the Xact 625 at each field
site. In long-term operation these checks would then be repeated quarterly. The manually
initiated checks will consist of the following.
Quarterly flow check, in which a NIST-traceable flow measurement standard is used to
verify the Xact 625 's sample flow measurement. Agreement of the NIST and Xact 625
flow measurements must be within 10%, or the Xact 625's flow sensor will be
recalibrated at 15.0, 16.7, and 18.4 L/min.
Quarterly leak check, in which the Xact 625's sample inlet is plugged, the sample pump
is allowed to create a vacuum in the system, and then the pump is turned off. A rise in the
internal system pressure of greater than 150 mm Hg/min is indication of a leak and calls
for identification and correction of the leak.
Quality control efforts for the reference sampling will include operation of the Partisol Plus 2025
according to the manufacturer's instructions, periodic calibration checks of the sampling flow
rate, collection of field blank filter samples for analysis, and completion of chain-of-custody
forms for all samples collected. These efforts are familiar to the OEPA field staff, as they are
carried out for all ambient monitoring efforts conducted by OEPA staff. The target metals will
be determined on all field blank filters, and all blank results for each target metal will be reported
as part of the test data. The blank results will not be subtracted from the sample results.
Quality control efforts for the laboratory analysis of metals by IO-3.56 will include continuation
of the chain-of-custody of received field samples, and adherence to the QC requirements of the
method, as noted in Section B4. Those requirements, including required frequencies and
appropriate corrective actions in case of inadequate results, are stated in Section 10 (Calibration
and Standardization) and Section 11 (Quality Control) of Method IO-3.5.7 Examples of
corrective actions that may be called for based on calibration, instrument performance, and QC
checks include instrument adjustments, repetition of sample preparation, repetition of
procedures, dilution of samples, and flagging of data.7
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B6 INSTRUMENT/ EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE
The metals monitor undergoing testing will be subjected to a daily inspection and diagnostic
check by OEPA staff to assure proper operation. Instrument internal diagnostics and the
completeness of data output (relative to the expected daily set of analyses) will be the primary
items noted in this daily check. Any issues or questions will trigger communication with the
vendor of the metals monitor to assess whether maintenance and/or repair is needed.
The Partisol Plus 2025 sampler will be inspected by OEPA staff prior to the field test and every
time collected filter samples are recovered from the sampler throughout the test. This inspection
will use a brief checklist of key Partisol Plus 2025 operating indicators, such as flow readings,
displays, and data acquisition status. The consistency of the automatic changeover of filters, and
the sampling flow rate displayed and recorded by the sampler's software, will be the primary
features addressed in the inspection. Any issues or questions will trigger communication with
the vendor of the Partisol Plus 2025 to assess whether maintenance and/or repair is needed.
Laboratory analytical equipment used for the reference metals analysis will be tested, inspected,
and maintained according to manufacturer's instructions and ERG SOPs. The results of
maintenance will be documented according to the laboratory procedures.
B7 INSTRUMENT CALIBRATION AND FREQUENCY
The Xact 625 metals monitor undergoing testing will be calibrated by the vendor prior to
delivery to the first field site. Once the Xact 625 is installed at the field site, a calibration check
will be performed using NIST-traceable thin film standards of four metals: chromium, selenium,
lead, and cadmium. Each thin film standard will be analyzed by the Xact 625 at each of three
excitation energy conditions. The analysis results for each metal must agree with the original
calibration within 10%, or a re-calibration will be done. If needed, such a re-calibration will
involve sending the thin film analysis spectra to CES for calculation of a new calibration curve.
Also upon installation at the field site, a QA blank check will be performed, where a blank
portion of the Xact 625's sampling tape is analyzed by the monitor. The blank tape is expected
to show no detectable levels of the target analytes. Failure of the blank check will require
installation of a new tape and conducting the check again.
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In long term operation of the Xact 625, both the calibration check and the QA blank check are
performed on a quarterly basis. In this verification these checks will be performed after
installation of the monitor at each of the two test sites. The metals monitor vendor will conduct
or direct any needed maintenance, repair, and/or recalibration as indicated by the QC checks and
calibration checks and restore the monitor to working order for continuation of testing. The
nature, extent, and cost of any maintenance, repair, and recalibration efforts will be noted and
included in the final report.
Calibration of the Partisol Plus 2025 sampler will be conducted by OEPA staff prior to the start
of testing. Recalibration will be performed by OEPA when necessary based on the flow rate
checks, i.e., recalibration will be triggered by sampler flow rate readings that differ by more than
ฑ5% from the target flow rate set at the start of field sampling.
Battelle will provide NIST-traceable measurement standards for temperature, barometric
pressure, and air flow with which to conduct a PE audit of the Partisol Plus 2025 sampler. All
such measurement standards will have been calibrated by Battelle's Instrument Laboratory
within no more than 6 months prior to its use in the PE audit.
Calibration of the reference metals analysis equipment will be conducted by ERG, based on the
QC procedures stated in Method IO-3.5.7 The Method's requirements focus on both initial
demonstration of analytical performance and continuing checks to confirm that performance is
being maintained. The several types of samples used to document method performance include
blanks, QCSs, LFBs, internal standards, and tuning solutions, and instrument performance
samples that include duplicates, standards, blanks, interference check standards, continuing
calibration blanks and verification standards, and laboratory control and matrix spikes.7 The
balances used to determine PMio mass on the Teflon filters will also be calibrated by ERG using
NIST-traceable mass standards.
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B8 INSPECTION/ACCEPTANCE OF SUPPLIES AND CONSUMABLES
Upon receipt of any sampling supplies or consumables, OEPA and/or Battelle staff will visually
inspect and ensure that the materials received are those that were ordered and that there are no
visual signs of damage that could compromise the suitability of the materials. If damaged or
inappropriate goods are received they will be returned or disposed of and arrangements will be
made to receive replacement materials. Forty-seven (47) mm diameter, 2.0 jim pore size (e.g.,
Zefluor FPTPT247 or equivalent) Teflon filters will be used with the Partisol Plus 2025 sampler.
Certificates of analysis or other documentation of analytical purity will be checked for all
standards (e.g., PE audit standards) to ensure suitability for this verification test. Unsuitable
materials will be returned or disposed of and arrangements for the receipt of replacement
materials will be made.
B9 NON-DIRECT MEASUREMENTS
No non-direct measurements will be used during this verification test.
BIO DATA MANAGEMENT
Various types of data will be acquired and recorded electronically or manually by OEPA, EPA
Region 5, or Battelle staff during this verification test. All manually-recorded data will be
recorded in permanent ink in LRBs or on data forms. The Xact 625 generates electronic data
files. These files will be uniquely named, downloaded to a personal computer, and transferred to
the VTC on a weekly basis, or more often, by the OEPA staff operating the metals monitor in the
field. The metals monitor data will then be uploaded to the project SharePoint site. Data will be
uniquely identified in the Xact 625 data files by the date and time of the measurement and the
identity of the metal.
Laboratory analytical results for all field samples and blanks will be provided to Battelle and
EPA by ERG as a Level III data package in electronic format, and will include supporting QC
information documenting the quality of the data obtained. Sample results will be uniquely
identified by means of the filter number, the associated date and time of sample collection, and
the identity of the target metal. The ERG metals analytical data will be uploaded by Battelle to
the project SharePoint site.
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Table 5 summarizes the types of data that may be recorded. All maintenance activities, repairs,
calibrations, and operator observations relevant to the operation of the monitoring systems being
tested will be documented by OEPA or vendor staff in the laboratory record book maintained at
the field site. Report formats will include all necessary data to allow traceability from the raw
data to final results.
Records received by or generated by any testing staff during the verification test will be
reviewed by a Battelle staff member within 14 days of receipt or generation, respectively, before
the records are used to calculate, evaluate, or report verification results. If a Battelle staff
member generated the record, this review will be performed by a Battelle technical staff member
familiar with the verification test, but not the staff member who originally received or generated
the record. The review will be documented by the person performing the review by adding
his/her initials and date to the hard copy of the record being reviewed. In addition, any
calculations or data comparisons performed by Battelle will be spot-checked by Battelle
technical staff to ensure that calculations are performed correctly. Calculations to be checked
include any statistical calculations described in this QAPP.
Battelle will provide technology test data and associated reference data (including records; data
sheets; notebook records) from the first day of testing within one day of receipt to EPA for
simultaneous review. The goal of this data delivery schedule is prompt identification and
resolution of any data collection or recording issues. These data will labeled as preliminary and
will not have had a QA review before their release.
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Table 5. Summary of Data Recording Process
Data to Be Recorded
Dates, times, and
details of test events
Metals monitor
operating information,
maintenance, down
time, etc.
Metals monitor
readings
Reference method
sampling information
Reference method
analytical results
Where
Recorded
ETV LRB, field
sampling
records, or
electronically
ETV LRB, field
sampling
records, or
electronically
Recorded
electronically and
downloaded to
computer daily
ETV LRB, field
sampling
records, chain of
custody forms
Electronic files of
analytical results
(Level II data
package)
How Often
Recorded
Start/end of
test event
Start/end of
maintenance,
down time,
change of
conditions, etc.
Recorded
continuously by
each metals
monitoring
system
At each
reference
method
sampling
interval
Upon comple-
tion and quality
review of each
batch of
samples
By Whom
OEPA, EPA
Region 5, or
Battelle staff
OEPA, EPA
Region 5, or
Battelle staff
OEPA staff for
transfer to
Battelle
OEPA staff
ERG
analytical staff
Disposition of Data
Used to
organize/check test
results; manually
incorporated in data
spreadsheets as
necessary
Incorporated in
verification report as
necessary
Converted to
spreadsheet for
statistical analysis
and comparisons
Converted to
spreadsheets for
statistical analysis
and comparisons
Converted to
spreadsheets for
statistical analysis
and comparisons
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SECTION C
ASSESSMENT AND OVERSIGHT
Cl ASSESSMENTS AND RESPONSE ACTIONS
Every effort will be made in this verification test to anticipate and resolve potential problems
before the quality of performance is compromised. One of the major objectives of this QAPP is
to establish mechanisms necessary to ensure this. Internal quality control measures described in
this QAPP, that is peer reviewed by a panel of outside experts, implemented by the technical
staff and monitored by the VTC, will give information on data quality on a day-to-day basis.
The responsibility for interpreting the results of these checks and resolving any potential
problems resides with the VTC, who will contact the Battelle AMS Center Manager, Battelle
AMS Center Quality Manager, EPA AMS Center Project Officer, and EPA AMS Center Quality
Manager if any deviations from this QAPP are observed. The VTC will describe any deviations
from this QAPP in a teleconference or by email, and once a path forward is determined and
agreed upon with EPA, a deviation form will be completed. Any deviations from this QAPP will
be noted in the verification report, along with a discussion on the deviation's impact (if any) on
data quality.
Technical staffs, including OEPA, EPA Region 5, and Battelle, have the responsibility to
identify problems that could affect data quality or the ability to use the data. Any problems that
are identified will be reported to the VTC, who will work with the Battelle Quality Manager to
resolve any issues. Action will be taken by the VTC and appropriate testing staff to identify and
address the issue, and minimize losses and correct data, where possible. Independent of any
EPA QA activities, Battelle will be responsible for ensuring that the following audits are
conducted as part of this verification test.
Cl.l Performance Evaluation Audit
Battelle will conduct a PE audit of both the sampling and analysis portions of the reference
metals measurements. The PE audit will be carried out early in the field monitoring period, so
that any issues raised by the PE results can be addressed early in the period.
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Battelle will conduct a PE audit of the Partisol Plus 2025 reference sampling system, by
checking the sampler flow rate and measurements of atmospheric pressure and temperature
during operation at the field site. This PE audit will be done by Battelle staff in the first week of
reference method sampling, using a flow measurement device, thermocouple temperature sensor,
and barometric pressure sensor calibrated by Battelle's Instrument Laboratory with NIST-
traceable standards. The acceptance criterion for the PE flow audit is that the sampler flow be
within ฑ5% of the target sampler flow rate. Acceptance criteria for temperature and barometric
pressure will be ฑ 2 ฐC and ฑ 5 millibars, respectively. Failure to meet the PE audit criterion will
result in a repeat of the audit with the same and/or a new audit device; continued failure to meet
the PE audit criterion will trigger inspection and/or recalibration of the reference sampler.
Battelle will also conduct a PE audit of the reference metals analysis by submitting one or more
sample solutions of selected target metals to ERG for analysis. These PE audit samples will be
prepared by Battelle by dilution of aqueous metals standards traceable to the National Institute of
Standards and Technology (NIST). The metals concentrations in the PE audit samples will be
unknown to ERG, except that the samples will be prepared to be within the normal calibration
range of ERG's analytical equipment for Method IO-3.5. The PE audit samples will contain at
least eight of the 22 target metals listed in Table 2 and among those will be Pb and Mn. The
metals PE audit samples will be submitted to ERG within the first three weeks of the field
period. The acceptance criterion for the PE audit is that the concentrations reported by ERG be
within ฑ10% of the prepared concentrations of the PE audit samples. Failure to meet this
criterion will result in a reanalysis of the PE audit samples, or preparation and submission of new
PE audit samples; continued failure to meet the PE audit criterion will trigger inspection and/or
recalibration of the ERG analytical equipment.
C1.2 Technical Systems Audits
The Battelle QAO will perform a TSA during performance of both laboratory and field-testing
activities. The purpose of these audits is to ensure that the verification test is being performed in
accordance with the AMS Center QMP1 and this QAPP. In the TSA, the Battelle QAO may
compare actual test procedures to those specified or referenced in this plan, and review data
acquisition and handling procedures. The Battelle QAO will prepare a project-specific checklist
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based on the QAPP requirements to guide the ISA, that will include a review of the test location
and general testing conditions; observe the testing activities; and review laboratory record books.
The Battelle QAO will submit an initial ISA report (with no corrective actions documented) to
the EPA Quality Manager and VTC within 10 business days after completion of the audit. A
copy of each final TS A report (with corrective actions documented) will then be provided to the
EPA AMS Center Project Officer and Quality Manager within 20 business days after receipt of
comments on the initial TSA report from the EPA Quality Manager and VTC. At EPA's
discretion, EPA QA staff may also conduct an independent on-site TSA during the verification
test. The TSA findings will be communicated to technical staff at the time of the audit and
documented in a TSA report.
C1.3 Audit of Data Quality
The Battelle QAO, or designee, will audit at least 10% of the sample results data acquired in the
verification test and 100% of the calibration and QC data versus the QAPP requirements. During
this audit, the Battelle QAO, or designee, will trace the data from initial acquisition (as received
from the vendor's technology), through reduction and statistical comparisons, to final reporting.
All calculations performed on the data undergoing the audit of data quality (ADQ) will be
checked. Data must undergo a 100% validation and verification by technical staff (i.e. VTC, or
designee) before it will be assessed as part of the data quality audit. All QC data and all
calculations performed on the data undergoing the audit will be checked by the Battelle QAO.
Results of the ADQ will be documented using the checklist and reported to the VTC and EPA
within 10 business days after completion of the audit. A final ADQ that assesses overall data
quality, including accuracy and completeness of the technical report, will be prepared as a
narrative and distributed to the VTC and EPA within 10 business days of completion of the
audit.
C1.4 QA/QC Reporting
Each assessment and audit will be documented in accordance with Section 3.3.4 of the AMS
Center QMP.1 The results of all audits will be submitted to EPA within 10 business days as
noted above. Assessment reports will include the following.
Identification of any adverse findings or potential problems
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Response to adverse findings or potential problems
Recommendations for resolving problems. (If the QA audit identifies a technical
issue, the VTC or Battelle AMS Center Manager will be consulted to determine the
appropriate corrective action
Confirmation that solutions have been implemented and are effective
Citation of any noteworthy practices that may be of use to others
C2 REPORTS TO MANAGEMENT
During the field and laboratory efforts, any QAPP deviations will be reported immediately to
EPA. The Battelle Quality Manager and/or VTC, during the course of any assessment or audit,
will identify to the technical staff performing experimental activities any immediate corrective
action that should be taken. A summary of the required assessments and audits, including a
listing of responsibilities and reporting timeframes, is included in Table 6. If serious quality
problems exist, the Battelle Quality Manager will notify the AMS Center Manager, who is
authorized to stop work. Once the assessment report has been prepared, the VTC will ensure that
a response is provided for each adverse finding or potential problem and will implement any
necessary follow-up corrective action. The Battelle Quality Manager will ensure that follow-up
corrective action has been taken. The QAPP and final report will be reviewed by the EPA AMS
Center Quality Manager and the EPA AMS Center Project Officer. Upon final review and
approval, both documents will then be posted on the ETV website (www.epa.gov/etv).
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Table 6. Summary of Assessment Reports3
Assessment
Each ISA
(Initial)
Each ISA
(Final)
ADQ#1
ADQ#2
Prepared By
Battelle
Battelle
Battelle
Battelle
Report Submission Timeframe
10 business days after ISA is complete
ISA response is due to QAO within 1 0
business days of receipt from QAO
ISA responses will be verified by the QAO
and provided within 20 business days after
receipt of comments on initial report
10 business days after receipt of first data
set
10 business days after completion of the
verification report review
Submitted To
EPA ETVAMS Center
EPA ETVAMS Center
EPA ETVAMS Center
EPA ETVAMS Center
' Any QA checklists prepared to guide audits will be provided with the audit report
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SECTION D
DATA VALIDATION AND USABILITY
Dl DATA REVIEW, VERIFICATION, AND VALIDATION REQUIREMENTS
The key data review and data verification requirements for this test are stated in Section BIO of
this QAPP. In general, the data review requirements specify that data generated during this test
will be reviewed by a Battelle technical staff member within two weeks of generation of the data.
The reviewer will be familiar with the technical aspects of the verification test. This process will
serve both as the data review and the data verification, and will ensure that the data have been
recorded, transmitted and processed properly. Furthermore, this process will ensure that the
monitoring systems data were collected under appropriate testing.
The data validation requirements for this test involve an assessment of the quality of the data
relative to the data quality objectives for this test referenced in Section A8. Any deficiencies in
these data will be flagged and the data will be excluded from any statistical comparisons, unless
these deviations are accompanied by descriptions of their potential impacts on the data quality.
D2 VERIFICATION AND VALIDATION METHODS
Data verification is conducted as part of the data review as described in Section BIO of this
QAPP. A visual inspection of any handwritten data will be conducted to ensure that all entries
were properly recorded or transcribed, and that any erroneous entries were properly noted (i.e.,
single line through the entry, with an error code, such as "wn" for wrong number, and the initials
of the recorder and date of entry). Electronic data from the metals monitor, Partisol Plus 2025
sampler, and analytical equipment used during the test will be inspected to ensure proper
recording. Calculations used to transform the data will be reviewed to ensure the accuracy and
the appropriateness of the calculations. Calculations performed manually will be reviewed and
repeated using a handheld calculator or commercial software (e.g., Excel). Calculations
performed using standard commercial office software (e.g., Excel) will be reviewed by
inspection of the equations used for the calculations and verification of selected calculations by
handheld calculator. Calculations performed using specialized commercial software (i.e., for
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analytical instrumentation) will be reviewed by inspection and, when feasible, verified by
handheld calculator, or standard commercial office software.
To ensure that the data generated from this test meet the goals of the test, a number of data
validation procedures will be performed. Sections B and C of this QAPP provide a description
of the validation safeguards employed for this verification test. Data validation efforts include
the completion of QC activities and the performance of a TSA as described in Section C. The
data from this test will be evaluated relative to the measurement data quality objectives described
in Section A8 of this QAPP.
An ADQ will be conducted by the Battelle QAO to ensure that data review, verification, and
validation procedures were completed, and to assure the overall quality of the data.
D3 RECONCILIATION WITH USER REQUIREMENTS
The purpose of this verification test is to evaluate the performance of a continuous monitor for
trace metals in ambient PMio. To meet the requirements of the potential user community,
including particularly EPA Region 5, EPA OAQPS, and OEPA, input to this QAPP has been
provided by external experts. Additional performance data regarding operational characteristics
of the metals monitor will be collected by verification test personnel. The data review,
verification, and validation procedures described above will assure that data meeting the test
requirements are accurately presented in the verification report generated from this test, and will
assure that data not meeting these requirements will be appropriately flagged and discussed in
the verification report.
This QAPP and the resulting ETV verification report will be subjected to review by the vendor,
EPA, and expert peer reviewers. The reviews of this QAPP will help to improve the design of
the verification test and the resulting report such that they better meet the needs of potential users
of ambient paniculate metals monitoring systems.
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SECTION E
REFERENCES
1. Battelle, Quality Management Plan for the ETV Advanced Monitoring Systems Center,
Version 7.0, U.S. EPA Environmental Technology Verification Program, prepared by
Battelle, Columbus, Ohio, November 2008.
2. U.S. EPA, Environmental Technology Verification Program Quality Management Plan, EPA
Report No: 600/R-08/009 EPA/600/R-03/021, U.S. Environmental Protection Agency,
Cincinnati, Ohio, January 2008.
3. School Air Toxics Monitoring Initiative, information available at
http ://www. epa.gov/ttn/amtic/airtoxschool .html.
4. Quality Assurance Project Plan for the EPA School Air Toxics Monitoring Program - Phase
II Multimetals (Final) - Revision 1.0, U.S. Environmental Protection Agency, Office of Air
Quality Planning and Standards, Research Triangle Park, North Carolina, May 2011.
5. Currie, Lloyd A., Detection and Quantitation in X-Ray Fluorescence Spectrometry. In X-ray
Fluorescence Analysis of Environmental Samples, Dzubay, Thomas B., ed.; Ann Arbor
Science, Ann Arbor, MI, 1978; pgs. 289-305.
6. Compendium method IO-3.1, Selection, Preparation, and Extraction of Filter Material, in
Compendium of Methods for the Determination of Inorganic Compounds in Ambient Air,
EPA/625/R-96/010a, U.S. Environmental Protection Agency Office of Research and
Development, June 1999.
7. Compendium Method IO-3.5, Determination of Metals in Ambient Particulate Matter Using
Inductively Coupled Plasma/Mass Spectrometry (ICP/MS), in Compendium of Methods for
the Determination of Inorganic Compounds in Ambient Air, EPA/625/R-96/010a, U.S.
Environmental Protection Agency Office of Research and Development, June 1999.
8. Quality Assurance Project Plan for Support for the EPA National Monitoring Programs
(NMOC, UATMP, PAMS, HAPs, and NATTS), EPA Contract EP-D-09-048, ERG,
Morrisville, North Carolina, 2011.
9. Standard Operating Procedure for Elemental Analysis of Particulate Matter on Membrane
Filters by the Kevex XRF Spectrometer, SOP ECAB-048.1E (Alternative Identification SOP
WDE-04-18), U.S. EPA National Exposure Research Laboratory, Research Triangle Park,
NC, November 4, 2009.
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APPENDIX A
QUANTITATION LIMITS OF THE XACT 625
Element
K
Ca
Ti
V
Cr
Mn
Fe
Co
Sn
Sb
Ba
Mn
Fe
Co
Ni
Cu
Zn
Ga
Ge
As
Se
Br
Rb
Sr
Y
Mo
Pt
Au
Hg
TI
Pb
Bi
Ag
Cd
In
Sn
Atomic
Number
19
20
22
23
24
25
26
27
50
51
56
25
26
27
28
29
30
31
32
33
34
35
37
38
39
42
78
79
80
81
82
83
47
48
49
50
60
Minute
QL
(ng/m3)
16.73
6.38
2.69
2.05
2.04
2.00
3.93
3.54
18.00
4.69
6.68
2.80
5.37
2.24
1.60
1.89
1.64
0.76
0.85
0.81
0.99
1.31
2.43
3.16
3.82
6.94
1.62
1.62
1.33
1.30
1.54
1.68
30.60
40.64
47.90
52.72
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APPENDIX B
EXAMPLE PMio METALS SAMPLE DATA SHEET
VERG
ERG Lab ID #
PM10 / TSP METALS DATA SHEET
Lab
Pre-Samp.
T3 9-
03 3
EJ
Field
Recovery
Lab
Recovery
Site Code:
City/State:
AQS Code:
Set-Up Date:
Recovery Date:
Collection Date:
Duplicate Event (Y/N):
Operator:
Sample Duration (i.e. 24 hr):
Status: Valid Void (Circle one)
Received by: Date:
Status: Valid Void (Circle one)
If void, why:
_i
<
HI
Z
Q.
W
0
s"
D_
Sample Date
Sample Date
Sample Date
Start
Time
Stan MFC
Start
Time
Start MFC
Start
Time
Start MFC
End
Time
End MFC
End
Time
End MFC
End
Time
End MFC
Total
Time
Avg Flow (L)
Total
Time
Avg Flow (L)
Total
Time
Avg Flow (L)
System #
System #
System #
Filter #
Filter #
Filter #
Lab ID
Lab ID
Lab ID
Comments:
White: Sample Traveler
Canary: Lab Copy
Pink: Field Copy
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