Batteiie
The Business of Innovation
Environmental Technology
Verification Program
Advanced Monitoring
Systems Center
Test/QA Plan for Verification of
Chemiluminescent Ozone Analyzer
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TEST/QA PLAN
for
Verification of
Chemiluminescent Ozone Analyzer
June 6, 2007
Prepared by
Battelle
505 King Avenue
Columbus, OH 43201-2693
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TABLE OF CONTENTS
Section Page
SECTION A PROJECT MANAGEMENT 7
Al Verification Test Organization 7
A2 Background 13
A3 Verification Test Description and Schedule 14
A4 Quality Objectives 17
A5 Special Training/Certification 17
A6 Documentation and Records 18
SECTION B MEASUREMENT AND DATA ACQUISITION 19
Bl Experimental Design 19
B2 Reference Sample Collection 27
B3 Sample Handling and Custody Requirements 27
B4 Laboratory Reference Methods 27
B5 Quality Control Requirements 28
B6 Instrument/Equipment Testing, Inspection, and Maintenance 28
B7 Instrument Calibration and Frequency 29
B8 Inspection/Acceptance of Supplies and Consumables 29
B9 Non-Direct Measurements 30
BIO Data Management 30
SECTION C ASSESSMENT AND OVERSIGHT 32
Cl Assessments and Response Actions 32
C2 Reports to Management 34
SECTION D DATA VALIDATION AND USABILITY 35
Dl Data Review, Validation, and Verification Requirements 35
D2 Validation and Verification Methods 35
SECTION E REFERENCES 37
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List of Figures
Figure 1. Organization Chart for the Verification Test 8
List of Tables
Table 1. Planned Verification Schedule 16
Table 2. Ozone Analyzers 21
Table 3. Interference Testing 22
Table 4. Photochemical Testing 23
Table 5. Summary of Data Recording Process 31
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ACRONYMS AND ABBREVIATIONS
API American Petroleum Institute
AMS Advanced Monitoring Systems
r2 Coefficient of determination
COA Chemiluminescent ozone analyzer
EPA U.S. Environmental Protection Agency
ETV Environmental Technology Verification
FEM Federal equivalent method
GC Gas chromatograph
LRB Laboratory record book
MSD Mass selective detector
m3 Meters cubed
mg Milligrams
ppb Parts per billion
%R percent recovery
PE Performance evaluation
QA Quality assurance
QC Quality control
QMP Quality management plan
RH Relative humidity
TSA Technical systems audit
T Temperature
UV Ultraviolet
VOC Volatile organic compounds
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ETV Advanced Monitoring Systems Center
Test/QA Plan
for
Verification of
Chemiluminescent Ozone Analyzer
June 6, 2007
VENDOR ACCEPTANCE:
Name
Company
Date
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DISTRIBUTION LIST
Elizabeth A. Betz
U.S. Environmental Protection Agency -
HEASD
National Exposure Research Laboratory
E205-01 EPA Mailroom
Research Triangle Park, NC 27711
Robert Fuerst
U.S. Environmental Protection Agency -
HEASD
National Exposure Research Laboratory
D205-05 EPA Mailroom
Research Triangle Park, NC 27711
Amy Dindal
Thomas Kelly
Patricia Holowecky
Darrell Joseph
Zachary Willenberg
Battelle
505 King Ave.
Columbus, OH 43201
Marat Kozliner
OPTEC Inc.
1985 West Henderson Road
Suite 216
Columbus, OH 43220
Dennis Mikel
U.S. Environmental Protection Agency
Office of Air Quality Planning and
Standards
E-143-02
Research Triangle Park, NC 27711
Rudy Eden
Laboratory Services and Source Testing
South Coast Air Quality Management
District
21865E. Copley Drive
Diamond Bar, CA91765
Will Ollison
American Petroleum Institute
1220 L Street
Washington, D.C. 2005-4070
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SECTION A
PROJECT MANAGEMENT
Al VERIFICATION TEST ORGANIZATION
The verification test will be conducted under the auspices of the U.S. Environmental
Protection Agency (EPA) through the Environmental Technology Verification (ETV) Program.
It will be performed by Battelle, which is managing the ETV Advanced Monitoring Systems
(AMS) Center through a cooperative agreement with EPA. The scope of the AMS Center covers
verification of monitoring technologies for contaminants and natural species in air, water, and
soil. The performance of the COA will be judged against a Federal Equivalent Method (FEM)
ultraviolet (UV) continuous monitor for ozone. Specifically, the FEM used for this test will be
method EQOA-0880-047.
The day to day operations of this verification test will be coordinated and supervised by
Battelle personnel, with the participation of the vendor who will be having the performance of
their COA verified. Testing will be conducted at Battelle in Columbus, Ohio. The vendor will
provide Battelle with their COA and will train the Battelle staff in the operation of the COA.
Battelle staff will operate the technology during verification testing.
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. Quality Assurance (QA) oversight will be provided by the Battelle Quality Manager and
also by the EPA AMS Center Quality Manager, at her discretion. The organization chart in
Figure 1 identifies the responsibilities of the organizations and individuals primarily associated
with the verification test. Roles and responsibilities are defined further below.
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Battelle
Management
Amy Dindal
Battelle AMS
Center Manager
Zachary Willenberg
Battelle
Quality Manager
Dr. Thomas
Kelly
Battelle
Verification
Testing Leader
Patricia Holowecky
Battelle
Verification
Test Coordinator
Battelle
Technical Staff
Robert Fuerst
EPA AMS Center
Project Officer
Elizabeth Betz
EPA AMS Center
Quality Manager
Chemiluminescent
Ozone Analyzer
Vendor
Representative
Figure 1. Organization Chart for the Verification Test
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Al.l Battelle
Ms. Patricia Holowecky is the AMS Center's Verification Test Coordinator for this test.
In this role, Ms. Holowecky will have overall responsibility for ensuring that the technical,
schedule, and cost goals established for the verification test are met. Specifically,
Ms. Holowecky will:
• Prepare the draft test/QA plan, verification reports, and verification statements.
• Revise the draft test/QA plan, verification reports, and verification statements in
response to reviewers' comments.
• Assemble a team of qualified technical staff to conduct the verification test.
• Establish a budget for the verification test and manage staff to ensure the budget is
not exceeded.
• Direct the team in performing the verification test in accordance with this test/QA
plan.
• 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. Responsibility for each aspect of the verification test will be
confirmed.
• Ensure that all quality procedures specified in this test/QA plan and in the AMS
Center Quality Management Planl (QMP) are followed.
• Serve as the primary point of contact for vendor representatives.
• Ensure that confidentiality of sensitive vendor information is maintained.
• Assist vendors as needed during verification testing.
• Become familiar with the operation and maintenance of the CO A through instruction
by the vendor, if needed.
• Respond to any issues raised in assessment reports, audits, or from test staff
observations, and institute corrective action as necessary.
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• Coordinate distribution of the final test/QA plan, verification reports, and verification
statements.
Dr. Thomas Kelly will serve as Verification Testing Leader. Dr. Kelly will:
• Support Ms. Holowecky in preparing the test/QA plan and designing the test.
• Review the draft and final test/QA plan.
• Attend the verification test kick-off meeting.
• Ensure that confidentiality of sensitive vendor information is maintained.
• Support Ms. Holowecky in responding to any issues raised in assessment reports and
audits.
• Review the draft and final verification reports and verification statements.
Ms. Amy Dindal is Battelle's Manager for the AMS Center. As such, Ms. Dindal will
oversee the various stages of verification testing. Ms. Dindal will:
• Review the draft and final test/QA plan.
• Attend the verification test kick-off meeting.
• Review the draft and final verification reports and verification statements.
• Ensure that necessary Battelle resources, including staff and facilities, are committed
to the verification test.
• Maintain communication with EPA's technical and quality managers.
• Issue a stop work order if Battelle or EPA QA staff discover adverse findings that
will compromise test results.
Technical staff from Battelle will support Ms. Holowecky in planning and conducting the
verification test. The responsibilities of the technical staff will be to:
• Assist in planning for the test, and making arrangements for the receipt of and
training on the CO A.
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• Attend the verification test kick-off meeting.
• Assist vendor staff as needed during technology receipt and training.
• Conduct verification testing using the vendor's COA technology.
• Conduct reference measurements during the testing.
• Perform statistical calculations specified in this test/QA plan on the technology data
as needed.
• Provide results of statistical calculations and associated discussion for the verification
reports as needed.
• Support Ms. Holowecky in responding to any issues raised in assessment reports and
audits related to statistics and data reduction as needed.
Mr. Zachary Willenberg is Battelle's Quality Manager for the AMS Center.
Mr. Willenberg will:
• Review the draft and final test/QA plan.
• Attend the verification test kick-off meeting.
• Conduct a technical systems audit at least once during the verification test, or
designate other QA staff to conduct the audit.
• Audit at least 10% of the verification data or designate other QA staff to conduct the
data audit.
• Prepare and distribute an assessment report for each audit.
• Verify implementation of any necessary corrective action.
• Request that Battelle's AMS Center Manager issue a stop work order if audits
indicate that data quality is being compromised.
• Provide a summary of the Q A/quality control (QC) activities and results for the
verification reports.
• Review the draft and final verification reports and verification statements.
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A1.2 COA Vendor
The responsibilities of the COA vendor are as follows:
• Review and provide comments on the draft test/QA plan.
• Accept (by signature of a company representative) the final test/QA plan prior to
test initiation.
• Provide two units of their technology for evaluation during the verification test.
• Provide all other equipment/supplies/reagents/consumables needed to operate
their technology for the duration of the verification test.
• Supply training on the use of the technology, and provide written consent and
instructions for test staff to carry out verification testing, including written
instructions for routine operation of their technology.
• Provide maintenance and repair support for their technology, on-site if necessary,
throughout the duration of the verification test.
• Review and provide comments on the draft verification report and statement for
their respective technology.
A1.3 EPA
EPA's responsibilities in the AMS Center are based on the requirements stated in the
"Environmental Technology Verification Program Quality Management Plan" (EPA ETV
QMP).2 The roles of specific EPA staff are as follows:
Ms. Elizabeth Betz is EPA's AMS Center Quality Manager. For the verification test,
Ms. Betz will:
• Review the draft test/QA plan.
• Perform at her option one external technical systems audit during the verification test.
• Notify the EPA AMS Center Project Officer of the need for a stop work order if the
external audit indicates that data quality is being compromised.
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• Prepare and distribute an assessment report summarizing results of the external audit.
• Review the draft verification reports and verification statements.
Mr. Robert Fuerst is EPA's Project Officer for the AMS Center. Mr. Fuerst will:
• Review the draft test/QA plan.
• Approve the final test/QA plan.
• Review the draft verification reports and verification statements.
• Oversee the EPA review process for the test/QA plan, verification reports, and
verification statements.
• Coordinate the submission of verification reports and verification statements for final
EPA approval.
A2 BACKGROUND
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. The purpose of ETV is to provide objective and quality assured performance data
on environmental technologies, so that users, developers, regulators, and consultants can make
informed decisions about purchasing and applying these technologies. Stakeholder committees
of buyers and users of such technologies recommend technology categories, and technologies
within those categories, as priorities for testing. Verification reports from previous tests are
available at http://www.epa.gov/etv/verifications/verification-index.html.
The purpose of this test/QA plan is to specify procedures for a verification test applicable
to commercial COA's such as the OPTEC 3.02 P-A COA.3 The purpose of the verification test
is to compare the response of the OPTEC COA to the response of a federally designated FEM
UV method for ozone (specifically for this test the FEM will be method EQOA-0880-047). In
performing the verification test, Battelle will follow the technical and QA procedures specified in
this test/QA plan and will comply with the data quality requirements in the AMS Center QMP.1
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A3 VERIFICATION TEST DESCRIPTION AND SCHEDULE
A3.1 Summary of Technology Category
Ozone is a pervasive pollutant that is formed by photochemical processes involving
sunlight, nitrogen oxides and volatile organic compounds (VOC) in air. The U.S. Clean Air Act
and its Amendments established air quality standards for ozone, and pollution control strategies
require state and local authorities to regulate for compliance with the standards. Because of the
costs associated with emission control programs and penalties for those organizations that are not
in compliance, it is essential that the ozone measurements that determine compliance with the
standards be performed accurately.
One of the methods currently utilized for ambient ozone monitoring is UV photometry,
which makes use of the ozone molecule's strong absorption band in the ultraviolet region of the
spectrum, with a maximum coinciding with the strong mercury emission line at 254 nanometers
(nm). Measurements made with a low-pressure mercury light source and an optical cell of
relatively short pathlength (typically 0.1 to 1 m) can achieve ozone detection limits of 5 parts per
billion (ppb) or better. Commercial instruments that employ UV photometry measure the
transmission of UV radiation through an air sample and compare the intensity with that obtained
along the same pathlength through air containing no ozone. Ideally the ozone-free reference
signal should be measured using ambient air containing all of the constituents of the sample air
except ozone. This is because other atmospheric species that absorb 254 nm radiation will
reduce the light intensity and will bias the ozone measurement unless they are present at the
same concentrations in the sample and reference air. In practice, a scrubber (typically MnO2)
has been used to selectively remove ozone from the air. However, any atmospheric constituent
that absorbs 254 nm radiation and is removed by the scrubber represents a potential interference
to the ozone measurements. Several commercial ozone monitors using UV absorption have been
designated by EPA as FEMs; the monitor used specifically for this test will be method EQOA-
0880-047.
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Concerns have been raised over potential interference to the UV photometry method
caused by aromatic hydrocarbons and their atmospheric reaction products, 4'5'6'7 mercury vapor,8
sulfur dioxide,9 and water vapor.8'10'11'12 Wilson and Birks13 have proposed a mechanism that
explains the water vapor interference observed with UV absorption ozone monitors on hot humid
days. They report that the scrubber can act as a reservoir for water vapor, and the water vapor
films formed on cell walls can influence the transmission of reflected UV light through the
measurement cell, thus affecting the ozone measurement signal. To control the water vapor
interference, a Nafion tube that equilibrates humidity in the scrubbed and unscrubbed air samples
is reported to resolve this problem.
The growing evidence for ozone measurement bias with the widely used MnO2 scrubber
has led to renewed interest in another technology that intends to resolve or minimize these
interference problems. For example, the 3.02 P-A CO A from OPTEC Inc. is claimed to be free
from water vapor interference up to 98% relative humidity, as long as condensation does not
occur.3 The 3.02 P-A COA detects ozone by means of its reaction with a solid reagent surface to
produce light (chemiluminescence),14'15'16 which is then detected by a photomultiplier tube. The
ETV test as described in this test/QA plan will explore the effectiveness of COAs and quantify
their response relative to the response of FEM instrumentation (used specifically as FEM
EQOA-0880-047) under various environmental interferent conditions.
A3.2 Verification Schedule
Table 1 shows the planned schedule of activities for the verification testing and data
analysis and reporting. As shown in Table 1, the laboratory activities are planned to begin in
May 2007 with installation of the COA. Testing is expected to begin in June, and the period of
testing will be approximately 2 weeks. A separate ETV verification report will then be drafted
for each COA, and the report will be reviewed by the technology vendor and subsequently by
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Table 1. Planned Verification Schedule
Month
(2007)
May
June
July
August
September
Verification Activity
Testing
Analyzer training by vendor
Set up/install COA
Calibration of COA
Humidity effect testing
Interference testing
Ambient outdoor measurements
Shutdown of test setup
Return of COAs to vendors
Data Analysis and Reporting
Begin preparation of ETV report template
Compile data from humidity effects
Compile data from interferent challenges
Analyze ambient outdoor data
Review and summarize operator observations
Finalize data from all interferents
Finalize data from ambient measurements
Complete common sections of reports
Complete report sections on interferent challenges
and operator observations
Internal review of draft reports
Vendor review of draft reports
Revision of draft reports
Peer review of draft reports
Revision of draft reports
Submission of final reports for EPA approval
peer reviewers. The test/QA plan and final reports will be submitted to EPA for final signature,
and these documents will be made publicly available on both the EPA/ETV and the Battelle
AMS Center websites.
A3.3 Test Facility
Laboratory analyses will be conducted in Battelle laboratories in Columbus, Ohio.
In performing this verification test, Battelle will follow the procedures specified in this
test/QA plan and will comply with quality requirements in the AMS Center QMP.1 The
laboratory that will be used contains a 17.3 m3 environmental chamber. This facility is equipped
for safe handling of chemicals and will be used to maintain controlled testing atmospheres.
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A4 QUALITY OBJECTIVES
This verification test is designed to evaluate the performance of the COAs for
determining ozone in air. This evaluation will include a comparison of the COA results to the
EPA designated FEM (EQOA-0880-047). These methods are both continuous real-time ozone
analyzers. The calibration of the FEM analyzer will be based on delivery of ozone from an
Environics Model 6400 ozone generator that has itself been calibrated against a Dasibi Model
1008-PC UV calibration photometer. The addition of a Nafion dryer to one of the COAs will
also be used during testing to determine the analyzers response to humidity effects. This
comparison will be made between the COAs.
The validity of calibration of the FEM analyzer will be checked by a Performance
Evaluation (PE) audit, performed by direct comparison of the Dasibi 1008 readings to those of a
UV transfer standard photometer operated by the Ohio EPA. That PE audit is described in
sectionC.1.1.
QA/QC requirements will be augmented by a Technical Systems Audit (TSA) and a data
quality audit. These additional QA procedures will be carried out by Battelle. The planned audit
procedures are described in Section Cl. The EPA Quality Manager also may conduct an
independent TSA, at her discretion.
A5 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 Quality Manager may verify the presence of appropriate training records
prior to the start of testing. Battelle technical staff will have a minimum of a bachelor's degree in
science/engineering or have equivalent work experience.
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A6 DOCUMENTATION AND RECORDS
The records for this verification test will be contained in the test/QA plan, chain-of-
custody forms, laboratory record books (LRB), data collection forms, electronic files (both raw
data and spreadsheets), the final verification report and assessment reports. All of these records
will be maintained in the Verification Test Coordinator's office during the test and will be
transferred to permanent storage at Battelle's Records Management Office at the conclusion of
the verification test except for assessment reports which are permanently stored with the Battelle
Quality Manager. All Battelle LRBs are stored indefinitely, either by the Verification Test
Coordinator or Battelle's Records Management Office. EPA will be notified before disposal of
any files. Section BIO further details the data recording practices and responsibilities.
All written records must be in ink. Any corrections to notebook entries, or changes in
recorded data, must be made with a single line through the original entry. The correction is then
to be entered, initialed, and dated by the person making the correction. In all cases, strict
confidentiality of data from the vendor's technology will be maintained. Separate files
(including manual records, printouts, and/or electronic data files) will be kept for the vendor's
technology.
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SECTION B
MEASUREMENT AND DATA ACQUISITION
Bl EXPERIMENTAL DESIGN
This test/QA plan addresses the verification of the COA for ozone by evaluating various
performance parameters created in an environmental testing chamber, and in monitoring of
ozone in ambient air. The accuracy, linearity, comparability, and interference effects of water
vapor, aromatic compounds, mercury, and products of atmospheric photochemistry will be
evaluated. Completeness of the data and operational factors will also be assessed. Specifically
the COA will be evaluated for the following performance parameters:
• Accuracy
• Linearity
• Interference Effects
Comparability
• Data Completeness
• Operational factors such as ease of use, maintenance and data output needs, power
and other consumables use, reliability, and operational costs.
Accuracy and linearity will be determined for the COA by determining the degree of
agreement with ozone calibration standards made in zero air at various ozone concentrations
Comparability will be assessed by comparison of the COA response to the Thermo
Environmental UV Model 49C FEM.
Interference effects will be determined by challenging the COA with various levels of
relative humidity (RH), substituted aromatic compounds, mercury, and products of photo-
chemistry. Data completeness will be assessed as the percentage of maximum data return that is
achieved by the COA over the test period. Operational factors will be evaluated by means of
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operator observations, and records of needed maintenance, vendor activities, and expendables
used. This test/QA plan provides the verification procedures for the COA.
Bl.l Test Procedures
The following sections describe the test procedures that will be used to evaluate each of
the performance parameters listed above. Test atmospheres will be generated in a 17.3 m3
environmental chamber. The ozone analyzers undergoing testing will be connected to the
chamber via a common manifold and will sample through a Teflon filter (nominal 5 um pore
size). Laboratory temperature (T) near the monitors will also be measured. The analyzers that
will be used as part of the verification test are listed in Table 2, together with their Federal
designation (if any), the source of the analyzer, the type of ozone scrubber, and any special notes
regarding the testing. Two COAs will be tested, one operated with and one without a Nafion
drier to control the humidity (and potentially select polar organic component levels) of the
sample air.
The T, RH, and particle concentration of the air in the chamber will be monitored during
each test, using standard T and RH sensors and a Climet particle counter, respectively. During
tests in which organic species are injected into the chamber, the VOC content of the chamber
will be monitored with a total hydrocarbon monitor (flame ionization, VIG Corp.), and an
integrated sample will be collected and analyzed by a gas chromatograph with mass selective
detector (GC/MSD) to confirm the concentration of the organic species. For selected tests,
gaseous elemental mercury will also be added to the chamber using a high emission rate
permeation tube following procedures employed successfully in the chamber during past
projects. An integrated sample will be collected and analyzed as described in Section B. 1.1.2 to
confirm the concentration of elemental mercury in the chamber.
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Table 2. Ozone Analyzers
Analyzer
Thermo Environmental
UV Model 49C
OPTEC 3.02 P- A solid-
phase chemiluminescence
OPTEC 3.02 P- A solid-
phase chemiluminescence
Federal
Status
FEM
~
—
Ozone
Scrubber
MnO2
unheated
NA
NA
Notes
Monitor absorbance tube T
~
Use Nafion drier to reduce RH
of sampled air
The signals from the test analyzers and other ancillary equipment, such as T and RH
monitors and the total hydrocarbon monitor, will be recorded at least every minute using a
Campbell Scientific data acquisition system. The zero signals of the ozone monitors will be set
to 10% of full scale in order to observe any negative shifts in signal during the tests.
Bl. 1.1 Accuracy and Linearity
After the CO A has been calibrated, the accuracy and linearity of the CO A will be
determined by challenges with ozone over a range of concentrations from 0 to 300 ppb,
generated by using an Environics Model 6400 ozone generator (transfer standard) that has itself
been calibrated against a Dasibi 1008 UV calibration photometer. The ozone will be added in
stepwise concentrations at both low (approximately 5%) and high (70 to 80%) relative humidity.
B. 1.1.2 Interference Effects
Interference effects in ozone-free air will be determined by the zero response of the CO A
with both low and high humidity when challenged with chemical interferences. The interference
effects and the response of the CO A will be assessed in Tests 1 and 2 as shown in Table 3. In
these tests, the COA will be challenged with a mixture of four interferents. The interferents are
listed in Table 3 and will be added to the environmental chamber at their respective designated
concentrations. The first interferent will be supplied to the chamber and the response of the
COA monitored. After the analyzer responses stabilize, the next interferent will then be added
into the chamber, and the process of injecting the interferent and recording response will be
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Table 3. Interference Testing
Test
i
i
9
RH
5%
5%
5%
5%
70 to 80%
70 to 80%
70 to 80%
70 to 80%
Interferent
Naphthalene
o-nitrophenol
p-tolualdehyde
Mercury
Naphthalene
o-nitrophenol
p-tolualdehyde
Mercury
Concentration
lOppb
lOppb
lOppb
50 ng/m3
lOppb
lOppb
lOppb
50 ng/m3
repeated until all four interferents have been added. After each injection of an interferent, an
integrated sample will be taken in the environmental chamber to confirm the injected
concentration. The challenges to the COA will occur in Test 1 at low (-5%) and in Test 2 at
high (70 to 80%) RH. In between the tests, the environmental chamber will be purged overnight
and the COA will be backflushed in order to clear the analyzer of any potential carryover of
interferences.
The response of the COA to photochemical reaction products, present in air along with
ozone, will be tested in Tests 3 and 4 (Table 4). Both tests will be conducted in a series of steps,
starting with monitoring of clean dry air, then of humidified clean air, and then proceeding to
monitoring of that air, spiked with a 17-component hydrocarbon mixture and NO2. Finally,
Tests 3 and 4 will each include the irradiation of the chamber and the monitoring of the COA
response until the ozone photochemical maximum has been passed. The difference between
Tests 3 and 4 will be the four times higher hydrocarbon concentrations and NO2 used in Test 4.
Those higher concentrations are designed to represent an extreme air pollution episode. In
between the tests, the environmental chamber will be purged overnight and the COA will be
backflushed in order to clear the analyzer of any potential concern of remaining interferences.
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Table 4. Photochemical Testing
Test
3
4
Step
Monitor dry zero air
Monitor humidified air
Add 17-component urban hydrocarbon mixture
Add NO2
Irradiate chamber contents
Monitor dry zero air
Monitor humidified air
Add 17-component urban hydrocarbon mixture
Add NO2
Irradiate chamber contents
Concentration
0 to 5 % RH
70 to 80% RH
500 ppbC
50 ppb
NA
0 to 5 % RH
70 to 80% RH
2000 ppbC
200 ppb
NA
NA = not applicable
Bl. 1.3 Comparability
Comparability will be evaluated by comparing the responses of the CO A to the responses
of the Thermo Environmental UV Model 49C FEM with the various challenges. All the
analyzers listed in Table 2 will undergo sampling of the same procedures created in the
environmental chamber. These procedures include the response to humidity effects at low and
high humidity levels and the challenge of ozone concentrations ranging from zero to 300 ppb.
Each analyzer will also be tested with the same interferences. For the purposes of this test/QA
plan, two COAs connected to a common manifold will sample from the environmental chamber,
one with a Nafion Dryer and one without. The effect of the addition of a Nafion drier to one of
the COAs will be evaluated by comparing the resulting response between the two COAs.
The comparability of the CO A response to ambient air will also be evaluated by
comparing the analyzer response to the Thermo Environmental UV Model 49C analyzer during
ambient air monitoring, which will be carried out over four successive days at Battelle. The
CO A will be compared to the UV analyzer by calculating the relative percent difference of the
response of the CO A to the response of the UV analyzer. The analyzers will continuously
monitor for 96 hours and the hourly averages will be calculated for use in this determination.
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B. 1.1.4 Data Completeness
No additional test procedures will be carried out specifically to address data
completeness. This parameter will be assessed based on the overall data return achieved by the
COA.
Bl.1.5 Operational Factors
Operational factors such as maintenance needs, data output, consumables used, ease of
use, etc., will be evaluated based on observations recorded by Battelle staff. A separate
laboratory record book will be maintained and will be used to enter daily observations on these
factors. Examples of information to be recorded in the record books include the daily status of
diagnostic indicators for the COA; 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 the COA down time or data acquisition failure; the
sustainability of the analyzer (e.g. power consumed, wastes generated, disposal costs required);
and operator observations about ease of use of the COA. These observations will be summarized
to aid in describing COA performance in the verification report on each COA.
B1.2 Statistical Analysis
The statistical methods and calculations used for evaluating quantitative performance
parameters are described in the following sections. In all cases, COA readings in mg/m3 will be
converted to ppb, using measured T and barometric data, before comparisons to standard ozone
concentrations and FEM data.
B.I. 2.1 Accuracy
The accuracy of the COA with respect to the ozone transfer standard will be assessed as a
percentage recovery (%R), using Equation 1:
'Y-X'
%R =
1 +
X
xlOO (1)
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Where Y is the COA reading and X is the delivered ozone transfer standard concentration. The
average, minimum, and maximum %R values will be reported for each series of multi level
ozone challenges.
B 1.2.2 Linearity
Linearity will be assessed by a linear regression analysis using the ozone concentration
delivered from the transfer standard as the independent variable and the results from the COA
being tested as the dependent variable. Linearity will be expressed in terms of slope, intercept,
and coefficient of determination (r2).
B 1.2.3 Interference Effects
The interference effects of the COA will be calculated in terms of the ratio of the
response of the COA when challenged with the interferent, to the actual concentration of the
interferent. For example, if 100 ppb of an interferent results in a 1 ppb change in the response of
the analyzer, the interference effect will be reported as 1% (i.e., 1 ppb/100 ppb). Interference
effects will be reported separately for each interferent. The actual interferent concentration
determined by analysis will be used in the calculation, not the nominal concentration shown in
TableS.
Bl.2.4 Comparability
Comparability between the COA results and the FEM analyzer results will be assessed by
linear regressions using the FEM readings as the independent variable and results from the COA
as the dependent variable. Linearity will be expressed in terms of slope, intercept, and r.2 This
calculation will be done separately for each test described in Table 4, and separately with the
FEM data from those tests. This calculation will also be done using the FEM data from the
period of ambient air monitoring. Comparability calculations on the chamber tests will be based
on minute-by-minute average data, whereas this calculation on the ambient data will be based on
the hourly average values.
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Comparability will also be calculated between the COA operated with a Nafion drier and
the one operated without such a drier. This calculation will be done using the data from the
photochemical ozone chamber tests (Table 4) and the period of ambient air monitoring.
B.I.2.5 Data Completeness
Data Completeness will be calculated as the percentage of the total possible data return
over the entire set of tests that is achieved by the COA. This calculation will use the total hours
of data recorded from the COA divided by the total hours of data in the entire set of tests. No
distinction will be made in this calculation between data recorded during different test activities.
The causes of any substantial incompleteness of data return will be established from operator
observations, and noted in the discussion of data completeness results.
B1.3 Reporting
The statistical comparisons described above will be conducted separately for each COA
being tested, and information on the operational parameters will be compiled and reported. The
data for each COA will be kept separate from data for all other COA's, and no intercomparison
of the data from different vendors' analyzers will be performed at any time. A verification report
will be prepared for the COA tested, that presents the test procedures and test data, as well as the
results of the statistical evaluation of those data.
Operational aspects of the COA will be recorded by testing staff at the time of
observation during the environmental chamber tests and field testing, and summarized in the
verification report. For example, descriptions of the data-acquisition procedures, use of vendor-
supplied proprietary software, consumables used, repairs and maintenance needed, and the nature
of any problems will be presented in the report. The verification report will briefly describe the
ETV program, the AMS Center, the test equipment and test conditions, and the procedures used
in verification testing. The results of the verification test will be stated quantitatively, without
comparison to any other COA's tested, or comment on the acceptability of the technology's
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performance. The draft verification report will first be subjected to review by the technology
vendor, then revised and subjected to a review by EPA, and/or other peer reviewers. The EPA
comments and the peer review comments will be addressed in further revisions of the report, and
the comments and responses will be tabulated to document the peer review process. The
reporting and review process will be conducted according to the requirements of the AMS Center
QMP.
B2 REFERENCE SAMPLE COLLECTION
Sample collection does not apply in this verification, because ozone cannot readily be
collected in sampling devices. In lieu of the collection of reference samples the CO A will be
challenged with ozone using an Environics Model 6400 ozone generator (transfer standard) that
has itself been calibrated against a Dasibi 1008 UV calibration photometer. In addition, CO A
response to photochemical ozone mixtures and ambient air will be compared with the
corresponding response of the FEM as designated by their respective analyzers. In addition,
independent audits of sampling procedures will be performed by Battelle as part of the Technical
Systems Audit procedure (Section Cl.l).
B3 SAMPLE HANDLING AND CUSTODY REQUIREMENTS
No reference samples will be collected in this test. However, samples will be collected
for confirmation of the chamber concentrations of the interferent compounds. Such samples will
be collected by, and remain in the custody of, the Battelle analyst who performs the confirming
analysis.
B4 LABORATORY REFERENCE METHODS
The reference method used for ozone determination in this test is an EPA designated UV
absorption FEM (EQOA-0880-047) that is a continuous real-time ozone analyzer. The FEM
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analyzer will be operated by Battelle staff according to the manufacturers' instructions, including
those for warm-up and stabilization time before testing.
The FEM will be calibrated at the start of each day of testing using the ozone transfer
standard described in Sections B1.1.4 and B2. This transfer standard itself will be calibrated
against the Dasibi 1008 UV calibration photometer at the start of the series of chamber tests.
Laboratory measurements to confirm the interferent compound (i.e., naphthalene, o-
nitrophenol, p-tolualdehyde) concentrations will be made using GC/MSD, with samples
collected from the test chamber using commercially prepared sorbent traps. Prior to any
chamber tests the sorbent method will be validated by tests of sorbent trap recovery and transfer
of the interferent compounds to the GC/MSD. The GC/MSD response will be calibrated using
standards prepared in Battelle's laboratories from the pure compounds. A linear regression of
peak area versus compound mass will be established as the calibration curve, and used to
calculate the actual chamber interferent concentrations. Similar procedures will be used for
mercury determination by sampling on a gold trap and analysis in Battelle's laboratories by cold
vapor atomic fluorescence on a Tekran series 2600 instrument.
B5 QUALITY CONTROL REQUIREMENTS
Quality of the reference ozone measurements will be assured by calibration of the FEM
analyzer at the start of each day of testing, using the ozone transfer standard. The calibration
slope must equal 1 ± 0.01 and the r2 greater than 0.95 in order for the reference measurement to
meet QC requirements. Blank samples will be generated by challenging the ozone analyzers
through the chamber sampling manifold with zero gas. If measurements fall outside of the
required tolerances, the QC procedures will be repeated.
B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAINTENANCE
The Thermo Environmental FEM used for the reference sampling and analysis will be
tested, inspected, and maintained as per the manufacturers operating instructions, so as to meet
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the performance requirements established in the ozone reference method for ozone measure-
ments. The GC/MSD and mercury fluorescence instrument used for the reference sampling and
analysis will be tested, inspected, and maintained as per the standard operating procedures of
Battelle. Battelle staff will operate and maintain the COA undergoing testing, those activities
will be done as directed by the vendor. Otherwise, repair and maintenance of the COA will be
the responsibility of the technology vendor. Other equipment such as T and RH instruments will
be obtained from the Battelle Instrument Services Laboratory and will have been calibrated
within the past year.
B7 INSTRUMENT CALIBRATION AND FREQUENCY
Prior to the start of the environmental chamber tests a multipoint calibration will be
performed on the FEM using an Environics Model 6400 ozone generator (transfer standard) that
has itself been calibrated against a Dasibi 1008 UV calibration photometer. The ozone
calibration standards will be generated in dry zero air. On each day of testing the ozone monitors
will be challenged through the chamber sampling manifold with zero gas and a single point
ozone span, both using dry zero air. In addition, the COA will be calibrated before the start of
each test, using its internal ozone source. The GC/MSD and mercury fluorescence instrument
will be calibrated prior to analyses and a minimum of a one point calibration will be performed
on consecutive analyses days.
B8 INSPECTION/ACCEPTANCE OF SUPPLIES AND CONSUMABLES
All materials, supplies, and consumables will be ordered by the Verification Test
Coordinator or designee. Where possible, Battelle will rely on sources of materials and
consumables that have been used previously as part of ETV verification testing without
problems. Battelle will also rely on previous experience or recommendations from EPA advisors
or the COA vendor.
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B9 NON-DIRECT MEASUREMENTS
Data published previously in the scientific literature will not be used during this
verification test.
BIO DATA MANAGEMENT
Various types of data will be acquired and recorded electronically or manually by
Battelle during this verification test. Table 5 summarizes the types of data to be recorded. All
maintenance activities, repairs, calibrations, and operator observations relevant to the operation
of the COA will be documented by Battelle staff in laboratory record books. A separate record
book will be provided for each COA. Results from the COA and the FEM reference methods
will be recorded in electronic format. All Battelle LRBs, record books and files are stored
indefinitely, either by the Verification Test Coordinator or Battelle's Records Management
Office. EPA will be notified before disposal of any files.
Records generated by any Battelle staff during the verification test will be reviewed by a
Battelle staff member within two weeks of generation, before the records are used to calculate,
evaluate, or report verification results. This review will be performed by a Battelle technical
staff member involved in 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 performed by Battelle staff will be spot-checked by another Battelle technical staff
member to ensure that calculations are performed correctly. Calculations to be checked include
any statistical calculations described in this test/QA plan. The data obtained from this
verification test will be compiled and reported independently for each COA tested.
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Table 5. Summary of Data Recording Process
Data to Be Recorded
Dates, times, and
details of test events,
COA maintenance,
down time, etc.
COA calibration
information
COA ozone readings
Reference method
procedures,
calibrations, QA, etc.
Reference method
ozone results
Results of analyses
for interferents in
chamber tests
Where Recorded
ETV test notebooks
ETV test notebooks, or
electronically
Recorded electronically
for each analyzer
Laboratory record
books, or data recording
forms
Recorded electronically
from each reference
method
Electronically by
GC/MSD instrument;
summarized in analysts
laboratory record book
How Often Recorded
Start/end of test
procedure, and at each
change of a test
parameter or change of
COA status
At COA calibration or
re-calibration
Recorded continuously
throughout testing
process
At each calibration,
QA check, or change
in method status
Recorded continuously
throughout testing
process
At every sample
analysis
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
Retained as documentation
of reference method
performance
Converted to spreadsheets
for statistical analysis and
comparisons
Converted to spreadsheet
for calculation of
interferent effects
Among the QA activities conducted by Battelle QA staff will be an audit of data quality.
This audit will consist of a review by the Battelle Quality Manager of at least 10% of the test
data. During the course of any such audit, the Battelle Quality Manager will inform the technical
staff of any findings and any immediate corrective action that should be taken. If serious data
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 Verification Test
Coordinator 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.
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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
test/QA plan is to establish mechanisms necessary to ensure this. The procedures described in
this test/QA plan, which is peer reviewed by a panel of outside experts, implemented by the
technical staff and monitored by the Verification Test Coordinator, 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 Verification Test Coordinator. Technical staff
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 Verification Test Coordinator, who
will work with the Battelle Quality Manger to resolve any issues. Action will be taken to control
the problem, identify a solution to the problem, 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
A Performance Evaluation (PE) audit will be conducted to establish the traceability of the
ozone measurements made in this verification test An ozone transfer standard photometer
provided by Ohio EPA, care of Mr. Christopher Galilei, will be used to compare to the
measurements made by the Dasibi 1008 calibration photometer. Ozone will be generated by an
Environics Model 6400 ozone generator and a series of simultaneous measurements made by the
transfer standard and Dasibi photometer over the range of zero to at least 300 ppb ozone will be
compared. The ozone transfer standard is traceable to the primary ozone standard reference
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photometer located at the EPA Region 5, Chicago, Illinois. Documentation of that traceability
will be obtained and kept in the test records. If the readings of the Dasibi instrument are not the
same as the readings of the ozone transfer standard, the data generated throughout this
verification test will be corrected to comply with the values generated from the transfer standard.
This audit will be performed once during the verification test
C1.2 Technical Systems Audit
The Battelle Quality Manager will perform a technical systems audit (TSA) at least once
during this verification test. The purpose of this audit is to ensure that the verification test is
being performed in accordance with the AMS Center QMP,1 this test/QA plan, using the EPA
designated reference method, and any Standard Operating Procedures (SOPs) used by Battelle.
In the TSA, the Battelle Quality Manager or a designee may review the reference methods used,
compare actual test procedures to those specified or referenced in this plan, and review data
acquisition and handling procedures. The Battelle Quality Manager will tour the environmental
chamber laboratory, observe the ozone monitoring and review test chamber procedures, and
review COA-specific record books. He will also check calibration certifications for test
measurement devices. A TSA report will be prepared, including a statement of findings and the
actions taken to address any adverse findings. The EPA AMS Center Quality Manager will
receive a copy of Battelle's TSA report. 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 Data Quality Audit
The Battelle Quality Manager will audit at least 10% of the verification data acquired in
the verification test. The Battelle Quality Manager will trace the data from initial acquisition,
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through reduction and statistical comparisons, to final reporting. All calculations performed on
the data undergoing the audit will be checked.
C1.4 QA/QC Reporting
Each assessment and audit will be documented in accordance with Sections 3.3.4 and
3.3.5 of the AMS Center QMP.1 The results of the technical systems audit will be submitted to
EPA. Assessment reports will include the following:
• Identification of any adverse findings or potential problems
• Response to adverse findings or potential problems
• Recommendations for resolving problems
• 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
The Battelle Quality Manager, 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. 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 Verification Test Coordinator 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 test/QA plan and final report will be reviewed by EPA AMS Center QA staff and EPA AMS
Center program management staff. Upon final review and approval, both documents will then be
posted on both the EPA/ETV and the Battelle AMS Center websites.
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SECTION D
DATA VALIDATION AND USABILITY
Dl DATA REVIEW, VALIDATION, AND VERIFICATION REQUIREMENTS
The key data review requirements for the verification test are stated in Section BIO of
this test/QA plan. The QA audits described within Section C of this document, including the
audit of data quality, are designed to assure the quality of the data. Data will be verified for
completeness, correctness, and compliance with the procedures as written in this test/QA plan.
D2 VALIDATION AND VERIFICATION METHODS
Section C of this test/QA plan provides a description of the validation safeguards
employed for this verification test. Data validation and verification efforts include the use of the
EPA designated FEM and ozone calibration equipment, and the performance of ISA, PE, and
data audits as described in Section C. An audit of data quality will be conducted by the Battelle
Quality Assurance Manager to ensure that data review and validation procedures were
completed, and to assure the overall quality of the data. Any findings will be communicated to
technical staff at the time of the audit and documented in a report.
D3 RECONCILIATION WITH USER REQUIREMENTS
The purpose of the verification test is to compare the response of the OPTEC CO A to the
response of a federally designated FEM UV method for ozone (specifically method EQOA-
0880-047). The data obtained should include thorough documentation of the performance of
each COA. The data review and validation procedures described in the previous sections will
assure that data meet these requirements and are accurately presented in the evaluation reports
generated from this test.
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This test/QA plan and the resulting ETV verification report(s) will be subjected to review
by the COA vendor, EPA, and expert peer reviewers. These reviews will assure that this test/QA
plan and the resulting report(s) meet the needs of potential users and permitters of CO As. The
final report(s) will be submitted to EPA in Word and Adobe PDF format, both 508 compliant,
and subsequently posted on the on the EPA/ETV and the Battelle AMS websites.
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SECTION E
REFERENCES
1. Quality Management Plan for the ETV Advanced Monitoring Systems Center, Version 6.0,
U.S. EPA Environmental Technology Verification Program, Battelle, Columbus, Ohio,
March 2005.
2. Environmental Technology Verification Program Quality Management Plan, EPA/600/R-
03/021, U.S. Environmental Protection Agency, Cincinnati, Ohio, December 2002
3. M.Y. Arshinov, B.D. Belan, O.A. Krasnov, V.K. Kovalevskii, V.A. Pirogov, A.P Plotnikov,
G.N. Tolmachev, and A.V. Fofonov, "Comparison of Ultraviolet and Chemiluminescent
Ozonometers", Atmos.Oceanic Opt.. 15, 656-658 (2002).
4. T. E. Kleindienst, E. E. Hudgens, D. F. Smith, F. F. McElroy, and J. J. Bufalini, "Comparison
of Chemiluminescence and Ultraviolet Ozone Monitor Responses in the Presence of
Humidity and Photochemical Pollutants, Air & Waste Mgmt. Assoc.. 43, 213-222 (1993).
5. T. E. Kleindienst, Mclver, C. D., and Ollison, W. M., "A Study of Interferences in Ambient
Ozone Monitors", VIP-74, proceedings A&WMA Measurement of Toxic and Related Air
Pollutants Conference, Research Triangle Park, NC, pp. 215-225 (1997).
6. J. A. Huntzicker and R. L. Johnson, "Investigations of an Ambient Interference in the
Measurement of Ozone by Ultraviolet Photometry", Env. Sci. & Tech.. H, 1414 (1979).
7. D. Grosjean and J. Harrison, "Response of Chemiluminescent NOx Analyzers and Ultraviolet
Ozone Analyzers to Organic Air Pollutants", Env. Sci. & Tech., 19, 862 (1985).
8. A. Leston, W. M. Ollison, "Estimated Accuracy of Ozone Design Values: Are They
Compromised By Method Interferences?", Tropospheric Ozone: Nonattainment and Design
Value Issues, Air & Waste Mgmt. Assoc., Pittsburgh, PA, p. 451 (October 27-30, 1992).
9. EPA, "Air Quality Criteria for Ozone and Related Photochemical Oxidants", EPA/600/P-
93004aF, Vol. 1, Section 3.5, National Center for Environmental Assessment, U.S. EPA,
Research Triangle Park, NC (1996).
10. E. E. Hudgens, T. E. Kliendienst, T. E., McElroy, F. F., and Ollison, W. M., "A Study of
Interferences in Ozone UV and Chemiluminescence Monitors", in Measurement of Toxic and
Related Air Pollutants, VIP-39, Air & Waste Mgmt. Assoc.. Pittsburgh, PA, pp. 405-415
(1994).
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11. C. P. Meyer, C. M. Elsworth, I. E. Galbally, "Water Vapor Interference in the Measurement
of Ozone in Ambient Air by Ultraviolet Absorption", Rev. Sci. Instr.. 62, 223 (1991).
12. J. A. Maddy, "A Test that Identifies Ozone Monitors Prone to Anomalous Behavior While
Sampling Hot and Humid Air", Paper 98-MPB.02P, Proceedings A&WMA 91st Annual
Meeting, June 14-18, 1998, San Diego, CA, Air & Waste Mgmt. Assoc., Pittsburgh, PA
(1998).
13. K.L. Wilson and J.W. Birks, "Mechanism and Elimination of a Water Vapor Interference in
the Measurement of Ozone by UV Absorbance", Environ. Sci. and Technol., 40, 6361-6367
(2006)
14. L. A. Topham, J. W. Drummond, G. I. Mackay, and H. I. Bufalini, "A New Lightweight
Ozone Monitor Based On Chemiluminescence With Eosin Y", 90-87.5, A&WMA 83rd
Annual Meeting and Exhibition, Pittsburgh, PA, pp. 1-5 (1990).
15. P.I. Domnin and V.P. Chelibanov, "Accuracy and Operating Characteristics of Instruments
for Ozone Content Measurements in Tlie Atmosphere", State Univ. of St. Petersburg, 1-9
(1989)
16. V. Grigorieva and M. Mihalev, "The Possible Uncertainties Over Quality of the Surface
Ozone Data", 12~ International School on Qua
Applications, Bulgaria, 5226, 285-289 (2003)
Ozone Data", 12~ International School on Quantum Electronics: Laser Physics and
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