II Battelle
. . . Putting Technology To Work
Environmental Technology
Verification Program
Advanced Monitoring
Systems Center
Test/QA Plan for
Verification of Ambient
Ammonia Monitors at Animal
Feeding Operations
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TEST/QA PLAN
FOR
VERIFICATION OF AMBIENT AMMONIA
MONITORS AT ANIMAL FEEDING
OPERATIONS
September 2, 2003
Prepared by
Battelle
505 King Avenue
Columbus, OH 43201-2693
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ETV Advanced Monitoring Systems Center
Test/QA Plan for Verification of Ambient Ammonia
Monitors at Animal Feeding Operations
Version: 1.0
September 2, 2003
APPROVAL:
Name
Company
Date
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DISTRIBUTION LIST
Mr. Robert Fuerst
U.S. Environmental Protection Agency
HEADS National Exposure Research
Laboratory
D-205-05 EPA Mailroom
Research Triangle Park, NC 27711
Ms. Elizabeth A. Betz
U.S. Environmental Protection Agency
HEADS National Exposure Research
Laboratory
E-205-01 EPA Mailroom
Research Triangle Park, NC 27711
Karen Riggs
Battelle
505 King Avenue
Columbus, OH 43201
Amy Dindal
Battelle
505 King Avenue
Columbus, OH 43201
Ken Cowen
Battelle
505 King Avenue
Columbus, OH 43201
Zachary Willenberg
Battelle
505 King Avenue
Columbus, OH 43201
Jerry Hatfield
U.S. Department of Agriculture
Agricultural Research Service
2150 Pammel Drive
Ames, IA 50011-4420
Vendors:
Joanne Shorter
Aerodyne Research, Inc.
45 Manning Road
Billerica, MA 01821-3976
Frank Thibodeau
Bruker Daltonics, Inc.
40 Manning Road
Billerica, MA 01821
Rob Metselaar
Managing Director
Mechatronics BV
P.O. Box 225
1620 AEHOORN
THE NETHERLANDS
Andre Bals, COO
OMNISENS SA
Pare Scientifique d'Ecublens
1015 Lausanne
(Switzerland)
Michael E. Webber
Pranalytica
1101 Colorado Ave.
Santa Monica, CA 90401
Kurt Webber
Molecular Analytics
14550 York Rd Ste A
Sparks, MD 21152-9307
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1
1.1 Test Description 1
1.2 Test Objective 1
1.3 Technology Description 2
1.4 Organization and Responsibilities 2
2.0 VERIFICATION APPROACH 10
3.0 TEST DESIGN 12
3.1 Site Description 12
3.2 Schedule 12
3.3 Installation 14
3.4 Reference Method 15
3.5 Accuracy and Linearity Tests 17
3.6 Calibration/Zero Drift Checks 17
3.7 Interference Testing 17
4.0 TEST PROCEDURES 20
4.1 Preparation of Sampling Media 20
4.2 Sample Collection 23
4.3 Sample Retrieval 24
4.4 Sample Extraction 24
4.5 Sample Analysis 25
4.6 Accuracy/Linearity Checks 26
4.7 Calibration/Zero Checks 27
4.8 Interference Checks 28
5.0 STATISTICAL CALCULATIONS 29
5.1 Relative Accuracy 29
5.2 Linearity 29
5.3 Precision 30
5.4 Comparability 30
5.5 Calibration and Zero Drift 31
5.6 Interference Effects 31
5.7 Response Time 31
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TABLE OF CONTENTS (Continued)
Page
6.0 MATERIALS AND EQUIPMENT 33
6.1 Sampling Media and Equipment 33
6.2 Analytical Equipment 34
6.3 Compressed Gases 34
6.4 Meteorological Equipment 35
7.0 QUALITY ASSURANCE/QUALITY CONTROL 36
7.1 Equipment Calibrations 36
7.2 QA/QC Samples 37
7.3 Assessment and Audits 39
8.0 DATA ANALYSIS AND REPORTING 42
8.1 Data Acquisition 42
8.2 Data Review 43
8.3 Reporting 44
9.0 HEALTH AND SAFETY 45
10.0 REFERENCES 46
APPENDIX A 47
APPENDIX B 49
Tables
Table 3-1. Interferent Gases and Approximate Concentrations 18
Table 8-1. Summary of Data Recording Process 38
Figures
Figure 1-1. Organization Chart for the Ammonia Monitor Verification Test 3
Figure 3-1. Proposed Schedule for Verification Test 13
Figure 3-2. Illustration of Potential Installation during Testing 15
Figure 3-3. Illustration of Reference Method Sampling System 16
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Date: September 2, 2003
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1.0 INTRODUCTION
1.1 Test Description
This test/quality assurance (QA) plan provides procedures for a verification test of
monitors used to measure gaseous ammonia at animal feeding operations (AFO). The
verification test will be conducted under the auspices of the U.S. Environmental Protection
Agency's (EPA) Environmental Technology Verification (ETV) program. 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 purchase and application
decisions.
The verification test will be performed by Battelle, of Columbus, OH, which is EPA's
partner for the ETV Advanced Monitoring Systems (AMS) Center. The scope of the AMS
Center covers verification of monitoring methods for contaminants and natural species in air,
water, and soil. In performing the verification test, Battelle will follow procedures specified in
this test/QA plan, and will comply with quality requirements in the "Quality Management Plan
for the ETV Advanced Monitoring Systems Center" (QMP).(1)
1.2 Test Objective
Emissions of atmospheric ammonia have generated considerable interest over the past
many years because of the role ammonia plays in nitrogen deposition, atmospheric acid-base
chemistry, and aerosol formation. In particular, livestock agriculture is identified as the largest
source of atmospheric ammonia in the U.S., and accounts for approximately 70% of emissions in
the U.S.(2) As such, there is a need to accurately quantify these emissions. The objective of this
verification test is to verify the performance of commercial ammonia monitors under normal
operating conditions at two different AFO facilities. The test will also assess various
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performance parameters by supplying the monitors being tested with compressed ammonia gas
standards.
1.3 Technology Description
The monitors to be tested in this verification test include both open-path systems as well
as point source monitors. Open-path systems typically have a light source and sensor, or a retro
reflector, that are installed at a variable distance from one another (typically 100-200 meters).
The light (infrared or ultraviolet) is emitted from the source and passes through the ambient air
to the sensor where it is detected (or to the retro reflector where, it is reflected back to a detector
positioned with the source). Ammonia that is in the optical path will absorb the light resulting in
a decrease in the light intensity that reaches the detector.
Several technologies employ techniques that are classified as point source monitors.
These technologies include photoacoustic monitors, ion selective electrodes, tunable diode
lasers, chemiluminescent monitors, and others.
In general, each of the monitors to be tested in this verification test are continuous
monitors and provide real-time or near real-time measurements of the ammonia concentration.
1.4 Organization and Responsibilities
The verification test will be performed by Battelle in cooperation with EPA, the vendors
who will be having their monitors verified, and the U.S. Department of Agriculture (USDA).
The organization chart in Figure 1-1 shows the individuals from Battelle, the vendor companies,
EPA, and USDA who will have responsibilities in the verification test. The specific
responsibilities of these individuals and organizations are detailed in the following paragraphs.
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Figure 1-1. Organizational Chart for the Verification Test of
Ambient Ammonia Monitors.
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1.4.1 Battelle
Dr. Kenneth Cowen is the AMS Center's Verification Test Coordinator for this test. In
this role, Dr. Cowen will have overall responsibility for ensuring that the technical, schedule,
and cost goals established for the verification test are met. More specifically, Dr. Cowen will:
Coordinate Battelle, test site, USD A, and vendor staff to conduct the verification
test
Guide the Battelle/USDA/vendor team in performing the verification test in
accordance with this test/QA plan
Have overall responsibility for ensuring that this test/QA plan is followed
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
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
Coordinate distribution of final test/QA plan, verification reports, and statements
Establish a budget for the verification test and monitor the effort to ensure that
budget is not exceeded
Ensure that confidentiality of vendor information is maintained.
Ms. Amy Dindal is a Verification Testing Leader for the AMS Center. As such, Ms.
Dindal will provide technical guidance and oversee the various stages of verification testing.
She will:
Support Dr. Cowen in preparing the test/QA plan and organizing the testing
Review the draft test/QA plan
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Review the draft verification reports and statements.
Ms. Karen Riggs is Battelle's AMS Center manager. As such, Ms. Riggs will:
Review the draft test/QA plan
Review the draft verification reports and statements
Ensure that necessary Battelle resources, including staff and facilities, are
committed to the verification test
Ensure that vendor confidentiality is maintained
Support Dr. Cowen in responding to any issues raised in assessment reports and
audits
Maintain communication with EPA's technical and quality managers
Facilitate a stop work order if Battelle or EPA QA staff discovers adverse
findings.
Mr. Zacharv Willenberg is Battelle's Quality Manager for the AMS Center. As such, Mr.
Willenberg will:
Review the draft test/QA plan
Conduct a technical systems audit once during the verification test
Review results of performance evaluation audit(s) specified in this test/QA plan
Audit at least 10% of the verification data
Prepare and distribute an assessment report for each audit
Verify implementation of any necessary corrective action
Issue a stop work order if internal audits indicate that data quality is being
compromised; notify Battelle's AMS Center Manager if such an order is issued
Provide a summary of the QA/QC activities and results for the verification reports
Review the draft verification reports and statements
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Ensure that all quality procedures specified in this test/QA plan and in the QMP(1)
are followed.
Battelle testing staff will support Dr. Cowen in planning and conducting the verification
test. These staff will:
Assist in planning for the test, and making arrangements for the installation of the
monitors
Assist vendors and test site staff as needed during the monitor installation and
verification testing
Assure that test procedures and data acquisition are conducted according to this
test/QA plan
Contribute to the planning of statistical treatment of the ammonia monitor data as
needed
Perform statistical calculations specified in this test/QA plan on the ammonia
monitor data as needed
Provide results of statistical calculations and associated discussion for the
verification reports as needed
Support Dr. Cowen in responding to any issues raised in assessment reports and
audits related to statistics and data reduction as needed.
1.4.2 Vendors
Vendor representatives will:
Review the draft test/QA plan
Approve the final test/QA plan
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Provide one ammonia monitor and the associated supplies for the duration of the
verification test
Commit or train a technical person to operate, maintain, and repair the ammonia
monitor throughout the verification test
Provide to Battelle staff the data from their monitor as requested by Battelle
Review their respective draft verification report and verification statement.
1.4.3 EPA
EPA's responsibilities in the AMS Center are based on the requirements stated in the
"Environmental Technology Verification Program Quality Management Plan" (ETV QMP).(3)
The roles of specific EPA staff under the ETV QMP 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 Manager to facilitate a stop work order if an external
audit indicates that data quality is being compromised
Prepare and distribute an assessment report summarizing the results of the
external audit, if one is performed
Review the draft verification reports and statements.
Mr. Robert Fuerst is EPA's AMS Center Manager. As such, Mr. Fuerst will:
Review the draft test/QA plan
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Approve the final test/QA plan
Notify the Battelle AMS Center Manager to facilitate a stop work order if the
external audit indicates that data quality is being compromised
Review the draft verification reports and statements
Oversee the EPA review process on the verification reports and statements
Coordinate the submission of verification reports and statements for final EPA
approval.
1.4.4 USD A
This verification test will be conducted in collaboration with the USD A, who will
provide co-funding for this test as well as in-kind support. The responsibilities of USD A are:
Assist Battelle with the coordination of the AFO test sites for the purposes of
ETV testing
Assist Battelle with the coordination of the installation of vendors' equipment at
the AFO test sites
Contribute to the development of the draft test/QA plan
Review the draft test/QA plan
Provide on-site and laboratory staff to assist during testing
Provide laboratory facilities for preparation of sampling media, and analysis of
collected samples
Conduct analysis of reference samples
Provide all raw and final field and laboratory data to Battelle
Assist in the operation of the vendor's monitors as needed
Review draft verification reports and statements.
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1.4.5 AFO Test Sites
This test will be conducted at two different AFO test sites. The responsibilities of these
sites are:
Provide access to the sites during testing for Battelle, USD A, EPA, and vendor
representatives
Provide adequate space for installation and testing activities.
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2.0 VERIFICATION APPROACH
The overall objective of the verification test described in this plan is to provide
quantitative verification of the performance of ambient ammonia monitors in realistic test
conditions under continuous operation at two animal feeding operation facilities. The
performance parameters that are addressed by this test/QA plan include:
Accuracy
• Linearity
• Precision
Comparability
• Interference effects
Calibration drift
• Zero drift
Response time
Ease of use
Data completeness.
Accuracy and linearity will be assessed for the monitors being verified by determining
the degree of agreement with compressed gas standards. Precision will be assessed in terms of
the repeatability of the ammonia measurements when supplied with ammonia gas standards.
Comparability will be assessed by comparisons with a ammonia measurements using a reference
method. Interference effects will be assessed by challenging the monitors being tested with
compressed gas standards of various chemical species commonly emitted at AFOs. Calibration
drift, and zero drift will be assessed by supplying the monitors being tested with commercial
compressed gas standards of ammonia and zero gas, respectively. Response time will be
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assessed by monitoring the time required to reach a stable reading when the monitors are
supplied with compressed gas standards.
This verification test will be conducted concurrently for all of the monitors being
verified, and will occur in two phases. The two phases will be conducted at separate animal
feeding operations and will last approximately four weeks each. It is expected that the ammonia
concentration will show considerable temporal variations during each phase of testing and that
the average concentrations measured during the two phases will be substantially different. The
performance of the monitors over those two periods will be assessed and reported. The amount
of time each monitor is operational and any maintenance activities performed over the
verification test periods will be recorded and reported, to help assess data completeness.
Observations about the operation of the monitors will be made by the USDA and Battelle staff
conducting the test, and will be used to assess the ease of use of each monitor being tested.
Additionally, siting and installation requirements will be reported for each of the monitors.
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3.0 TEST DESIGN
3.1 Site Description
[to be provided by USDA after clearance from AFOs]
3.2 Schedule
The verification test will be conducted in two phases. The first phase of testing will be
conducted at a hog farm in Ames, Iowa, from approximately September 8 to October 3, 2003.
The second phase of testing will be at a cattle farm in Bushland, Texas, from approximately
October 13 to November 7, 2003. Prior to the beginning of each phase, there will be a
shakedown period during which the vendors will install their monitors, ensure proper operation,
and train Battelle/USDA staff on the routine operation of their monitors.
During each phase, two periods of intensive sampling will be conducted to collect
reference samples using annular denuder technology as described in Section 3.4. The two
intensive periods will be during the first and last weeks of each phase. The reference sampling
will be conducted on a five sample per day schedule on each week day (i.e., Monday - Friday)
during those weeks. Also during the first week of each phase, the monitors will be supplied with
compressed gases to assess accuracy and linearity. The compressed gases will used to assess
calibration drift and zero drift of the monitors. The calibration checks will be done on Monday,
Wednesday, and Friday of the first and last weeks during the two test phases. During week two
of the second phase of testing, the monitors will be supplied with compressed gas standards
containing different interferent species. Figure 3-1 shows the proposed schedule for the testing
activities for this verification test.
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Ambient Ammonia Monitors
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3.3 Installation
Each of the monitors being tested should be installed by the vendor with some means of
supplying or sampling compressed gas standards (i.e., ammonia, zero gas) for the accuracy,
linearity, and interference tests as well as the calibration and zero drift checks. During each
phase the monitors being verified will be located within the fenceline of the AFO, and in the
predominantly downwind direction from the primary ammonia source. Monitors employing
open path techniques will be situated such that the optical path is perpendicular to the prevailing
wind direction. These monitors will be installed such that all the optical paths are parallel to one
another, and to the extent possible, with the same pathlength (or multiple thereof). Monitors
employing point source measurements will be collocated with one another to the extent possible.
These point source monitors will also be positioned such that they are along the pathlength of
any open-path monitors being verified but offset from the optical path such that they do not
interfere with the transmittance of reflectance of the light from the open-path monitors. Figure
3-2 illustrates an example of the potential arrangement of the monitors being tested and the
reference method samplers.
In this figure, the x's represent potential locations where ammonia samples will be
collected according to a reference method. As described below, simultaneous collection of
several reference samples will be made at several points along the pathlength of the open-path
technologies, with at least one sample collected at the location of the point source measurements.
These reference samples will be used for establishing the accuracy of the ammonia monitors.
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Bam
(primary source)
Prevailing wind direction
X - reference measurements
Open-path
technologies
x x
~ ~ ~
Point source technologies
Fenceline
Figure 3-2. Illustration of potential installation during testing.
3.4 Reference Method
Reference samples will be collected using citric acid coated denuder sampling trains (see
Figure 3-3). The method that will be used is based on the EPA Compendium Method 10-4.2
Determination of Reactive Acidic and Basic Gases and Acidity of Fine Particles (< 2.5 |J,m)(4),
with some modifications to the method as described below. For this test, ambient air will first be
drawn through an impactor at a nominal rate of 10 liters per minute (1pm) to remove particulate
matter with aerodynamic diameters greater than 2.5 |j,m. The air will then pass through the citric
acid coated denuder to remove gaseous ammonia. A single Teflon filter will be used to collect
the particulate matter that passes through the denuder.
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To Pump
t
Teflon filter
Denuder
Coating: 1% citric acid
Impactor
Inlet
Figure 3-3. Illustration of Reference
Method Sampling cartridge.
For this verification test, reference samples will be collected during the first and last
week of testing during each phase. In order to capture diurnal variations in ammonia
concentrations sampling is expected to be conducted on approximately the following schedule:
8:00 a.m. to 12:00 p.m., 12:00 p.m. to 2:00 p.m., 2:00 p.m. to 4:00 p.m., 4:00 p.m. to 8:00 p.m.,
and 8:00 p.m. to 8:00 a.m., such that 5 sets of samples are collected in each 24-hour period. The
short term (2-hour and 4-hour) sampling is expected to capture the peaks in ammonia
concentrations, whereas the 12-hour sampling will capture overnight concentrations. After each
sampling period, the sampling media will be retrieved, sealed, and stored until being transported
to the laboratory for analysis, and new sampling media will be installed.
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3.5 Accuracy and Linearity Tests
On one day during the first week of testing during each phase, the monitors being tested
will be supplied with a series of ammonia gas standards to assess accuracy and linearity. Prior to
being supplied to the monitors, these standards will be diluted with zero air to achieve
concenctrations between approximately 200 - 2000 ppb. Measurements will be recorded at each
of five concentration levels. The accuracy and linearity tests will be performed independently
for each monitor and need not be performed on the same day for all monitors.
3.6 Calibration/Zero Drift Checks
On Monday, Wednesday, and Friday, of the first and last weeks of testing during each
phase, the monitors being tested will be supplied with an ammonia gas standard and zero air to
check the calibration and zero drift of the monitors, respectively. It is expected that the order in
which the monitors are to be checked will be randomly varied, as will the time of day.
3.7 Interference Testing
During the second phase of testing, the monitors being tested will each be supplied with
several compressed gas standards containing different interferent compounds. The interference
testing will be conducted performed independently for each of the monitors being tested and
need not be performed on the same day for all monitors. Table 3-1 shows the interferent
compounds to be supplied to the monitors and the approximate concentrations of these species.
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Table 3-1. Interferent Gases and Approximate Concentrations
Interferent Gas
Approximate
Concentration
to be Supplied (ppb)
Nitrogen dioxide
100 ppb
Hydrogen sulfide
100 ppb
Diethylamine
100 ppb
1,3-butadiene
100 ppb
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4.0 TEST PROCEDURES
4.1 Preparation of Sampling Media
The procedures to be used for the preparation of the sampling media are described below
and are based on the procedures given in the EPA Compendium Method 10-4.2 Determination of
Reactive Acidic and Basic Gases and Acidity of Fine Particles (< 2.5 |j,m)(4).
During each phase, preparation of the sampling media will be performed at a USD A
National Soil Tilth Laboratory (NSTL) facility nearby to the respective test sites. To the extent
possible the preparation of the denuders will be performed in an ammonia free glove box to
prevent contamination. However, the NSTL has a semi-automated system for denuder
preparation and extraction that will be used in the first phase of this test. This system in not
located in an ammonia free environment but minimizes the exposure of the denuder channels to
the atmosphere, thereby limiting potential contamination.
After the sampling media are prepared, they will be stored in the glove box until they are
transported to the test site for installation in the sampling trains.
4.1.1 Denuder Cleaning
The procedure for cleaning the denuders is given below. This procedure will be used for
all new and used denuders.
1. Wash the denuders thoroughly with distilled water for at least 2 minutes ensuring
that all the channels in the denuder have been flushed.
2. After flushing, rinse the denuder with Milli-Q water at least three times, ensuring
that each channel has been rinsed.
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3. After rinsing, gently tap the denuder on a clean Kimwipe to shake out excess
water.
4. Place all cleaned denuders on a clean Kimwipes on a clean surface and allow the
denuders to air dry. Note: if it is necessary to rapidly dry the denuders, they
may be rinsed in methanol and allowed to air dry, or clean air may be blown
through them.
5. Once dry, cap both ends of the denuder with clean end caps and store them in an
ammonia-free glove box until use.
4.1.2 Denuder Preparation
The procedure used to coat the denuders is given below. There are two types of caps that
are needed for this process. One type of cap should have a solid face and the other should have a
small hole in the center of the face to prevent pressure buildup during the preparation process.
The cap with the hole in the face should not be used to store the denuder after preparation.
Ensure that there are two solid caps available for the denuder storage.
1. Using clean gloves (disposable polyurethane, or comparable), cap one end of the
denuder with a solid face cap and set upright on the capped end. Pour
approximately 10 mL of 1% citric acid solution into the denuder.
2. Cap the open end of denuder using the cap with a hole. Cover the hole in the face
of the cap and gently turn and rotate the denuder to ensure that the solution is
distributed into all channels of the denuder.
3. Remove one cap and pour out excess coating solution. Remove the other cap and
gently shake excess solution from denuder.
4. Attach denuder to drying assembly and flow clean, dry air through the denuder
for approximately 10 minutes at approximately 10 liters per minute (1pm).
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5. Remove denuder from drying assembly, and cap both ends with solid face caps.
Store the capped denuder in the glove box until packed for transport to the site.
Using the unique identification number inscribed on the denuder, record the date
and time that the denuder was coated.
The denuders should be carefully packed to prevent breakage during transport to the test sites.
The denuders should be used within 72 hours of being coated, and should be used within 24
hours of being transported to the field. A completed chain-of-custody form (Appendix B) must
accompany the denuders during transport to and from the field.
4.1.3 Sampling Cartridge Assembly
The following is the procedure for assembling the sampling cartridges. Cartridge
assembly should be performed in the laboratory on a clean bench-top, or in an ammonia-free
glove box if available.
1. With clean (disposable polyethylene, or comparable) gloves, place a glass spacer
on a clean Kimwipe.
2. Place the filter pact outlet port inside the spacer.
3. Place a Teflon™ filter inside the filter pack outlet port followed by three clean
plastic filter screens.
4. Place the cartridge assembly housing inside the filter pack outlet port and fasten
the housing to the top rim of the cartridge.
5. Hold the cartridge housing at a slight angle and insert the following components
in order.
one metal spring
one HDPE ring spacer
one glass spacer
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one HDPE ring spacer
one citric acid coated denuder
one HDPE ring spacer
one glass spacer
a greased inlet impactor plate
(Note: For breakthrough checks substitute a second citric acid denuder for the first glass
spacer.)
6. Slide the sample inlet into the cartridge housing and secure it with the side clips.
7. Place plastic caps on both ends of the cartridge to prevent contamination.
8. Attach label to cartridge indicating date packed,the denuder identification, and the
filter identification.
Cartridges should be assembled in the laboratory at room temperature and transported to the test
sites when possible. A completed chain-of-custody form must accompany the cartridges during
transport to and from the field.
4.2 Sample Collection
Sampling should be performed as closely to the scheduled times as possible, with the
start and stop times ideally within 15 minutes of the scheduled times. The procedure for sample
collection is given below.
1. Allow the pump to warm up for approximately 5 minutes.
2. Assemble the sampling train as shown in Figure 3-2. Seal the open end of the
inlet using a cap or stopper. Run the leak check for 5-10 seconds. The flow
meter should indicate no flow if there are no leaks in the system. If there are no
leaks indicated, turn off the pump and remove the cap or stopper from the inlet. If
a leak is indicated, check the assembly for proper connections. Replace any
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suspect gaskets or defective components. Record activities on field data sheet
(Appendix A).
3. Turn the pump on and set the sample flow rate to 10 1pm.
4. Complete appropriate sections on field data sheet. Begin sampling.
4.3 Sample Retrieval
Sample retrieval should be performed as soon after the end of each sampling period as
possible. Care must be taken to avoid sample contamination during retrieval.
1. After sampling period is over, complete the appropriate sections on the field data
sheet.
2. Turn off pump.
3. With clean gloves (disposable polyethylene, or comparable), remove sampling
cartridge and cap both ends with clean caps.
4. Install new sampling cartridge as needed.
5. Pack the capped sampling cartridge for transport to the laboratory. Complete the
chain of custody form.
4.4 Sample Extraction
Sample extraction should be done as soon after sample collection as feasible (within 24-
hours of sample collection) and should be done on the same day as the analysis. Extraction of
the samples should be performed in an ammonia free glove box to prevent sample
contamination. (Note: for this verification test, only the denuders will be extracted and analyzed.
The filter may be archived for analysis at a later date as needed.)
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1. Remove both caps from the denuder. Wipe the outer surface of the denuder with
a Kimwipe moistened with Milli-Q water.
2. Place a clean solid faced cap on one end of the denuder, and pipet 10 mL of DDW
into the denuder. Cap the open end of the denuder using a cap with a hole in the
face.
3. Cover the hole in the face of the cap and gently turn and rotate the denuder to
ensure that the solution is distributed into all channels of the denuder.
4. Holding the denuder so that the red cap with the hole in its is on top, shake the
denuder to force the liquid to the bottom.
5. Remove the red cap from the top of the denuder. Hold the bottom red cap firmly
and carefully remove the denuder from the cap. Most of the solution should
remain in the cap. Gently shake the denuder again to get the remaining solution
out.
6. Pour the extraction solution into a labelled sample vial and cap the vial tightly.
7. Store the vial in the glove box until analysis. (Note: if analysis can not be
performed within 24 hours of extraction, the samples should be frozen until
analysis can be performed).
4.5 Sample Analysis
Sample analysis will be performed by Flow injection analysis (FIA). FIA is a continuous
flow method for rapidly processing samples. In this method a peristaltic pump draws sample
from the sampler into the injection valve. Simultaneously, reagents are continuously pumped
through the system. The sample is loaded into the sample loop of one or more injection valves.
The injection valve is then switched to connect the sample loop in line with the carrier stream.
This sweeps the sample out of the sample loop and onto the manifold. The sample and reagents
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then merge in the manifold (reaction module) where the sample can be diluted, dialyzed,
extracted, incubated and derivatized. Mixing occurs in the narrow bore tubing under laminar
flow conditions. For each method, the operating parameters are optimized to address high
sample throughput, high precision and high accuracy.
FIA of the collected samples will be conducted by USD A staff on the same day as the
samples are extracted. The analysis will be done according to the QuikChem Method No. 10-
107-06-2-A (Lachat Company, Loveland, CO). In this method, ammonia is heated with
salicylate and hypochlorite in an alkaline phosphate buffer forming an emerald green color
which is proportional to the ammonia concentration. The color is intensified by the addition of
sodium nitroprusside and monitored photometrically. The FIA instrument will be calibrated on
each day prior to analysis of the samples.
4.6 Accuracy/Linearity Checks
During the first week of each phase of testing the monitors being tested will
independently be supplied with compressed ammonia gas standards to achieve measurements
over a range of concentrations from approximately 0 - 2000 ppb (or the upper range of
measurement of the monitor being tested, whichever is lower). The gases delivered to the
monitors will be prepared by dilution of higher concentration ammonia standard gases (i.e., 100-
500 ppm) in zero air using a calibrated dilution system, and the degree of dilution will be
dependent on the nature of the technology being tested (i.e., point source or open path).
Accuracy and linearity will be assessed by establishing a multipoint calibration curve.
To establish this curve, three non-consecutive measurements will be recorded at each of five
different nominal concentration levels. The gas will be supplied to the monitor for at least two
minutes or until a stable reading is achieved, (i.e., no apparent increase in signal is observed),
whichever is later. Once a stable reading is achieved, the gas will be delivered for two more
minutes, the concentration will be recorded, and the monitor will be supplied the next standard
gas. Table 4-1 shows the nominal concentration values to be supplied to the monitors being
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tested and the order in which the concentrations will be supplied. After the last measurement has
been recorded, the monitor will be flushed with zero air for approximately 5 minutes.
Table 4-1. Nominal Ammonia Concentrations and Order for Accuracy/Linearity Checks
Measurement
Number
Concentration
0 ppb
200 ppb
600 ppb
1200 ppb
2000 ppb
1
2
3
4
5
7
10
6
9
8
11
12
13
14
15
4.7 Calibration/Zero Checks
On Monday, Wednesday, and Friday of the first and last weeks during the two phases of
the verification test, a compressed ammonia gas standard will be supplied to each of the monitors
being tested. The gas should be supplied to the monitor for at least two minutes or until a stable
reading is achieved, (i.e., no apparent increase in signal is observed), whichever is later. Once a
stable reading is achieved, the concentration should be recorded, and the monitor will be
supplied with zero gas. Zero gas will be supplied to the monitor for at least two minutes or until
a stable reading is achieved (i.e., no apparent decrease in signal is observed), whichever is later.
Once a stable reading has been achieved, the concentration should be recorded and the monitor
can resume sampling the ambient air. At least once during each phase, the time required to reach
a stable reading for both the calibration check and the zero checks will be recorded for each
monitor being tested. This time will be used to assess the response time of the monitors.
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4.8 Interference Checks
During week two of testing in the second phase, the monitors being tested will
independently be supplied with a series of interference gases (see Table 3-1). Prior to supplying
the interferent gas, zero air will be supplied to the monitors being tested for at least two minutes
or until a stable reading is achived (i.e., no apparent increase in signal is observed), whichever is
later. Once a stable reading has been achieved the monitor response will be recorded and the
interferent gas will be diluted with zero air and delivered to the monitors seperately for at least
two minutes each or until a stable reading is achieved, (i.e., no apparent increase in signal is
observed), whichever is later. Once a stable reading has been achieved, the concentration should
be recorded, monitor will be flushed for at least two minutes with zero air and approximately 500
ppb of ammonia will be supplied to the monitor gas. The gases will be supplied for at least two
minutes each or until a stable reading is achieved, (i.e., no apparent increase in signal is
observed), whichever is later. Once a stable reading has been achieved, the interferent gas will
be supplied to the monitor for at least two minutes, or until a stable reading is achieved, (i.e., no
apparent increase in signal is observed), whichever is later. Once a stable reading has been
achieved, the concentration should be recorded and zero air will be supplied to the monitor for
approximately five minutes. This process should be repeated for each of the interferent gases.
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5.0 STATISTICAL CALCULATIONS
The statistical calculations to be used to verify the ammonia monitor performance are
described below. All calculations will be performed using Microsoft Excel™.
5.1 Relative Accuracy
The relative accuracy (RA) of the ammonia monitor with respect to the compressed gas
standards will be assessed using Equation 1:
1
RA = —I
"a \d
xt
x 100
(1)
QJ
where d refers to the difference between the standard gas concentration and the average of the
ammonia monitor measurements recorded during sampling period, and x corresponds to the
standard gas concentration. For open path monitors, relative accuracy will be based on the
observed increase in signal over the background concentration measured. Relative accuracy will
be calculated and reported independently for each of the two phases.
5.2 Linearity
Linearity will be assessed by a linear regression analysis using the compressed standard
gas concentrations as the independent variable and results from the ammonia monitors being
tested as the dependent variable. Linearity will be expressed in terms of slope, intercept, and
coefficient of determination (r2), and will be calculated independently for each phase of the
verification test.
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5.3 Precision
Precision will be calculated in terms of the percent relative standard deviation (RSD) of a
series of ammonia monitor measurements made over the duration of each of the calibration and
zero drift check periods. During each calibration and zero check all readings from monitors
testing will be recorded, and the mean and standard deviation of those readings will be
calculated. Precision (P) will then be determined as:
SDn
Pi —X 100 (2)
XD
where SD is the standard deviation of the monitor readings and X is the mean of the monitor
readings. Precision will be calculated independently for each phase of testing.
5.4 Comparability
Comparability between the ammonia monitor results and the reference method results
will be assessed by linear regression using the reference method ammonia concentrations as the
independent variable and results from the ammonia monitors being tested as the dependent
variable. For the open path monitors, the average of the reference method results along the
optical path will be used as the independent variable. Linearity will be expressed in terms of
slope, intercept, and coefficient of determination (r2), and will be calculated independently for
each phase of the verification test. It is expected that the measured concentration of ammonia
will vary by at least a factor of five during each phase of testing. If this magnitude of variation is
not achieved during either of the phases then comparability for that phase will be calculated
using Equation 1 and reported as a percent difference rather than in terms of the linear regression
results.
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5.5 Calibration and Zero Drift
Calibration and zero drift will be reported in terms of the mean, relative standard
deviation, and range (maximum and minimum) of the readings obtained from the ammonia
monitor in the daily sampling of the same ammonia standard gas, and of zero gas. The
calibration and zero drift will be calculated independently during each phase of testing such that
up to 6 ammonia standard readings (Monday, Wednesday, and Friday for two weeks), and up to
6 zero readings, will be used for this calculation in each phase. This calculation, along with the
range of the data, will indicate the day-to-day variation in zero and standard readings.
5.6 Interference Effects
The extent of interference will be calculated in terms of the ratio of the response of the
monitor to the interfering species, relative to the actual concentration of the interfering species.
For example, if 100 ppb of an interfering species results in a 1 ppb change in the response of the
monitor, the interference effect will be reported as 1% (i.e., 1 ppb/100 ppb). The interference
effects will be reported seperately for each interferent both in the absence and in the presence of
ammonia.
5.7 Response Time
Response time will be assessed in terms of both the rise and fall times of each ammonia
monitor when sampling the ammonia gas standard. Rise time (i.e., 0% - 95% response time) will
be determined by recording all the monitor readings when the gas is supplied to the monitor.
Once a stable response has been achieved with the gas standard, the fall time (i.e., the 100% to
5% response time) will be determined in a similar way, by recording all monitor readings as the
gas supplied is switched from the ammonia standard back to zero gas. For monitors which
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provide periodic rather than continuous readings, determination of rise and fall times may
involve interpolation between readings.
Rise and fall times will each be determined once for each monitor during each phase of
testing. Rise and fall times will be reported in units of seconds.
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6.0 MATERIALS AND EQUIPMENT
6.1 Sampling Media and Equipment
The denuders, filters, and associated sampling equipment for collection of the reference
method(4) sampling will be supplied by Battelle and/or USDA. The sampling cartridges used for
this test will be ChemComb Model 3500 speciation sampling cartridges(5) (Rupprecht &
Patashnick, Co., Inc., Albany, NY). Multiple sampling trains will be available such that five sets
of four trains (i.e., five sampling runs with four trains each) may be sampled in a single day, in
addition to at least two blank samples, two breakthrough checks, and two duplicate samples per
day during the intensive sampling periods.
6.1.1. Denuders
The denuders used for the reference sample collection will be honeycomb type denuders
used in the ChemComb sampling cartridges. The denuders will be coated with a 1% citric acid
solution, analogous to the 1% citric acid solution used in the EPA standard method(3). The
solvents and chemicals used to prepare the denuders for sampling and to extract the denuders
after sampling will be ACS reagent grade, and will be purchased from a reliable supplier.
Reagents and solvents will be analyzed for ammonia prior to use to ensure no contamination is
present.
6.1.2 Filters
The filters to be used for the reference sample collection will be 47 mm diameter Teflo™
filters (e.g., Gelmen Sciences, part number R2PJ047, or comparable).
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6.1.3 Sampling Train Components
Each of the sampling trains will include a pump to draw the air through the sampling
media, and a flow meter, or flow controller to maintain a nominally constant flow rate. The
ChemComb sampling cartridges have an internal impactor to remove particulate matter with an
aerodynamic diameter greater than 2.5 |j,m.
6.2 Analytical Equipment
Analysis of the collected samples will be conducted by flow injection analysis (FIA)
using a Lachat QuikChem Model 8000 FIA+. The equipment and chemicals to be used for
sample analysis will be provided by USDA and will be at the USDA facilities used during each
phase of testing. All chemicals used for the sample extraction and analysis will be reagent grade.
6.3 Compressed Gases
6.3.1 High Purity Nitrogen/Air
The high purity gases used for zeroing of the monitors will be commercial ultra-high
purity (UHP, i.e., minimum 99.999% purity) air or nitrogen.
6.3.2 Ammonia Standard Gases
Compressed gas standards containing ammonia will be obtained for use in the calibration
drift checks of the monitors. These will consist of ammonia in a nitrogen matrix, at levels of
approximately 100-500 ppm. These gases will be diluted as necessary to achieve ammonia
concentrations in the range of approximately 200-2000 ppb.
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6.4 Meteorological Equipment
Meteorological conditions during each phase of testing will be monitored continuously
using a portable meteorological station (i.e., MetOne Instruments, or comparable). The station
will include sensors for ambient temperature, relative humidity, barometric pressure, wind speed,
and wind direction. Data from the station will be recorded continuously using a datalogger, and
will be analyzed by the datalogger to provide hourly averages for the measured parameters.
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7.0 QUALITY ASSURANCE/QUALITY CONTROL
7.1 Equipment Calibrations
7.1.1 Reference Method Sampling Equipment
Reference method sampling will be conducted according to the procedures described in
the EPA standard method(4). A single point calibration of the flow rate through each of the
sampling systems (i.e., pump, flow controller, filter pack, denuder, cyclone) will be performed
prior to the start of each phase using a dry gas meter with NIST-traceable calibration. The flow
rate of each sampler will be checked at least once per day at the beginning and end of one
sampling period using a dry gas meter or other flow meter. The flow rate will be recalibrated if
the calibration check is not within ±5% of the nominal flow rate of 10 1pm (i.e., 9.5 1pm - 10.5
lpm). All calibration results must be documented for inclusion in the verification test data files
and verification report.
7.1.2 Analytical Equipment
Analysis of the reference samples will be conducted in a laboratory using FIA. The FIA
system for the reference sample analysis will be calibrated by USDA staff performing the
analysis. The calibration will be conducted according to the manufacturer recommendations and
will include concentrations of ammonia standard solutions that bracket the expected
concentration of the sample solutions. Calibration standards will be run at the beginning and end
of each analytical session, with one calibration solution run after each tenth reference sample.
The calibration will be acceptable if the r2 of the calibration curve is >0.98, and if the calibration
checks agree within 10% of the standard solution concentration. All calibration results must be
documented for inclusion in the verification test data files and verification report.
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7.1.3. Meteorological Equipment
The sensors used for the meteorological monitoring will be calibrated by the
manufacturer within one year of use in this verification test. All calibration results must be
documented for inclusion in the verification test data files and verification report.
7.2 QA/QC Samples
7.2.1 Field Blanks
At least 10% of all samples collected will be field blanks. The field blanks will be
collected by installing the sampling media (i.e., denuder and filters) in the sampling train but
without drawing any air through the train. The media will then be recovered and handled like
normal samples. If contamination levels are detectable and are greater than 5% of any of the
measured sample concentrations for that day, no additional reference sampling will be conducted
until the cause of the contamination is identified and rectified. Care will be taken to ensure that
field blanks will be collected at each of the different sampling locations and during each of the
different sampling periods (e.g., 8:00 a.m. to 12:00 p.m., etc.). Field blanks should be analyzed
within 24 hours of collection to allow for prompt corrective action if needed.
7.2.2 Denuder Breakthrough Checks
Back-up denuders will be used with at least 10% of the samples collected to assess the
degree of ammonia breakthrough. These breakthrough checks will be conducted at each of the
four sampling locations and will include checks during each of the five sampling periods. At
least one breakthrough check will be performed during each of the sampling periods during the
first two days of sampling during each phase to allow for prompt corrective action if needed. If
the measured ammonia concentration on the back-up denuders is greater than 10% of the
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concentration on the front denuder, then back-up denuders will be used for all sample collection
during those periods during which breakthrough might be anticipated to occur. Denuder
breakthrough checks should be analyzed within 24 hours of collection to allow for prompt
corrective action if needed.
7.2.3 Duplicate Samples
For at least 10% of samples, duplicate samples will be collected using a co-located
sampling train. These duplicate samples will be collected at each of the sampling locations and
during each of the sampling periods. It is expected that the difference in the measured ammonia
concentrations between duplicate samples will be within 10% of the average concentration (i.e.,
difference divided by average < 10%). If relative differences greater than 10% are observed,
reference sampling will continue and the cause of these differences will be investigated and
rectified if possible.
7.2.2 Laboratory Blanks
Laboratory blank solutions will be prepared for the FIA analysis. These solutions will be
analyzed prior to analysis of the reference samples. A laboratory blank solution will be analyzed
after every 10th reference sample to ensure no drift in the FIA instrumentation. If the blank
levels are greater than 5% of any of the measured concentrations for that day, the cause of the
contamination will be investigated and rectified (if possible). All analyses performed after the
most recent acceptable blank will be invalidated and analysis of those samples will be repeated
(if possible).
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7.2.3 Calibration Checks
Calibration check solutions will be prepared using NIST-traceable ammonia solutions.
The calibration check solutions will be analyzed after every 10th reference sample to ensure no
drift in the FIA instrumentation. If the measured concentrations are not within ±10% of the
standard solution concentration, the cause of the discrepancy will be investigated and rectified if
possible. If such a discrepancy is observed, all analyses performed after the most recent
acceptable spike will be invalidated and analysis of those samples will be repeated (if possible).
7.2.4 Dilution Checks
At each of the nominal ammonia levels to be used for the accuracy and linearity checks,
at least one sample of the diluted will be collected using the reference method. These samples
will be analyzed as regular samples and will used to check the accuracy of the dilution system.
Agreement between the reference sample measurement and the calculated concentration from the
dilution system should be within 10%. If the reference method result and the calculated
concentration do not agree within 10%, no further accuracy or linearity checks will be completed
until the source of the discrepancy is investigated and rectified.
7.3 Assessment and Audits
7.3.1 Technical Systems Audits
Battelle's ETV Quality Manager, will perform a technical systems audit (TSA) once
during at least one phase of this verification test. The purpose of this TSA is to ensure that the
verification test is being performed in accordance with this test/QA plan and that all QA/QC
procedures are being implemented. In this audit, the Battelle ETV Quality Manager may review
the reference sampling and analysis methods used, compare actual test procedures to those
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specified in this plan, and review data acquisition and handling procedures. The Battelle ETV
Quality Manager will prepare a TSA report, the findings of which must be addressed either by
modifications of test procedures or by documentation in the test records and 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 testing staff at the time of the
audit, and documented in a TSA report.
7.3.2 Performance Evaluation Audit
A performance evaluation (PE) audit will be conducted to assess the quality of the
measurements made in this verification test. This audit addresses only those measurements that
factor into the data used for verification, i.e., the sample flow rate, and the analytical laboratory
measurements. This audit will be performed once during the verification test, and must be
performed by analyzing a standard or comparing to a reference that is independent of standards
used during the testing.
The flow rate of the reference method sampling assemblies will be audited once during
each phase of testing using a dry gas meter (or other flow meter) that is independent of the meter
used to calibrate the flow rate. Agreement between the audit flow rate and the nominal flow rate
should be within ±5% (i.e., 9.5 1pm - 10.5 1pm). If agreement between the audit flow rate and
the nominal flow rate is not within ±5%, then the flow rate of the sampler will be recalibrated.
The performance of the FIA used to analyze the reference samples will be audited by
analyzing an ammonium standard that is independent of those used for the calibration. This
sample will be provided as a blind audit sample and the operator of the FIA will not be aware of
the concentration of the sample. If agreement between the measured concentration and the
standard concentration is not within ±10%, the cause of the discrepancy will be investigated and
rectified if possible. This audit will be performed at least once during each phase of the
verification test.
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7.3.3 Data Quality Audit
Battelle's Quality Manager will audit at least 10 percent of the verification data acquired
in the verification test. The Quality Manager will trace the data from initial acquisition, through
reduction and statistical comparisons, and to final reporting. All calculations performed on the
data undergoing audit will be checked.
7.3.4 Assessment Reports
Each assessment and audit will be documented in accordance with Section 3.3.4 of the
QMP for the AMS Center.(1) Assessment reports will include the following:
• Identification of any adverse findings or potential problems
• Space for response to adverse findings or potential problems
• Possible recommendations for resolving problems
• Citation of any noteworthy practices that may be of use to others
Confirmation that solutions have been implemented and are effective.
7.3.5 Corrective Action
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 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 followup corrective action. The Battelle Quality Manager will ensure
that follow-up corrective action has been taken.
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8.0 DATA ANALYSIS AND REPORTING
8.1 Data Acquisition
Data acquisition in this verification test includes recording of the data from the monitors
undergoing testing, documentation of sampling conditions and analytical results from the
reference method, meteorological conditions, and recording of testing activities, such as the
times of test activities, etc.
Data acquisition for the monitors undergoing verification will be performed by the
vendors during the test. Each monitor must have some form of data acquisition device, such as a
printout of analyzer response, or an electronic data recorder that stores individual analyzer
readings. The vendor will be responsible for reporting the response of the monitor, for each of
the phases of the verification test. The data from the monitors are to be retrieved by, or provided
to Battelle regularly, and must include all individual readings of the monitor listed by time of
day. Averaged results, e.g., ammonia data averaged over the period of a reference method
sampling run, may also be provided, if available. If not provided, averaging will be performed
by Battelle in data processing. Electronic data files are the preferred means of data transfer, with
Excel® or comma separated variable file formats preferred. Electronic files requiring vendor's
proprietary software will be supplied along with the software required to view the data.
Other data will be recorded in laboratory record books provided by Battelle and
maintained by Battelle, vendor, and subcontractor staff involved in the testing. These records
will be reviewed by Battelle to identify and resolve any inconsistencies. 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 each vendor's monitor, and strict
separation of data from different monitors, will be maintained. Separate files (including manual
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records, printouts, and/or electronic data files) will be kept for each monitor. At no time during
verification testing will Battelle or USDA staff engage in any comparison in performance of the
participating monitors.
Table 8-1 summarizes the types of data to be recorded; where, how often, and by whom
the recording is made; and the disposition or subsequent processing of the data. The general
approach is to record all test information immediately and in a consistent format throughout all
tests. Data recorded by the vendors is to be retrieved by, or turned over to Battelle or USDA
staff regularly during each phase of testing. Identical file formats will be used to make
quantitative evaluations of the data from all of the monitors tested, to assure uniformity of data
treatment. This process of data recording and compiling will be overseen by the Verification
Test Coordinator.
8.2 Data Review
Records generated in the verification test will be reviewed by a Battelle staff member
within two weeks after the completion of each phase of testing, before these records are used to
calculate, evaluate, or report verification results. These records may include laboratory record
books; data from the monitors; or reference method analytical results. This review will be
performed by a Battelle technical staff member involved in the verification test, but not the staff
member that originally generated the record. The test site, USDA staff, and/or vendor
representatives will be consulted as needed to clarify any issues about the data records. The
review will be documented by the person performing the review by adding his/her initials and
date to a hard copy of the record being reviewed. Data relating to the reference samplinge from
the first week of each phase will be reviewed by a Battelle staff member within 48 hours of
generation to allow for any corrective actions to be implemented promptly.
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Table 8-1. Summary of Data Recording Process
Data to be Recorded
Responsible
Party
Where Recorded
How Often
Recorded
Disposition of
Data(a)
Dates, times of test
events (site activities,
etc.)
USD A/
Battelle staff
Laboratory record
books/field data sheet
Start/end of test,
and at each test
activity.
Used to
organize/check test
results; manually
incorporated in data
spreadsheets as
necessary.
Reference method
sampling data
USD A/
Battelle staff
Laboratory record
books, CoC forms, or
file data sheets as
appropriate
At least at start/end
of reference sample,
and at each change
of a test parameter.
Used to
organize/check test
results; manually
incorporated in data
spreadsheets as
necessary.
Meteorological
conditions
Battelle
Meteorological
station datalogger
Continuously
Used to assess
meteorological
conditions during
testing as necessary.
Ammonia monitor
readings
Vendor or
designee
Data acquisition
system (data logger,
PC, laptop, etc.).
Continuously at
specified
acquisition rate
throughout monitor
operation.
Electronically
transferred to
spreadsheets
Reference sample
analysis, and results
USD A/
Battelle staff
Laboratory record
books, data sheets, or
data acquisition
system, as
appropriate.
Throughout sample
handling and
analysis process
Transferred to
spreadsheets
(a) All activities subsequent to data recording are carried out by Battelle.
8.3 Reporting
The statistical data comparisons described in Section 5.0 will be conducted separately for
each commercial ammonia monitor tested. Separate verification reports will then be prepared,
each addressing the monitor provided by one commercial vendor. The verification report will
present the test data, as well as the results of the statistical evaluation of those data.
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The verification report will briefly describe the ETV program and the AMS Center, and
will describe the procedures used in verification testing. These sections will be common to each
verification report resulting from this verification test. The results of the verification test will
then be stated quantitatively, without comparison to any other monitor tested, or comment on the
acceptability of the monitor's performance. The preparation of draft verification reports, the
review of reports by vendors and others, the revision of the reports, final approval, and the
distribution of the reports, will be conducted as stated in the Generic Verification Protocol for
the Advanced Monitoring Systems Pilot.(6) Preparation, approval, and use of Verification
Statements summarizing the results of this test will also be subject to the requirements of that
same Protocol.
9.0 HEALTH AND SAFETY
The first phase of the verification test described in this test/QA plan will be performed in
Ames, Iowa, and the second phase of the verification test will be performed in Bushland, Texas.
All visiting staff at the AFO test site may be given a site-specific safety briefing by a
representative of the test site .prior to the installation and operation of the monitors. All
participants in this verification test (i.e., Battelle, USD A, EPA, and vendor staff) will adhere to
the health and safety requirements of the test site. All equipment brought onto the test site will
conform to the biosecurity protocol of the test site.
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Date: September 2, 2003
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10.0 REFERENCES
1. Quality Management Plan (QMP) for the ETV Advanced Monitoring Systems Center,
U.S. EPA Environmental Technology Verification Program, prepared by Battelle,
Columbus, Ohio, Version 4.0 December 2002.
2. National Air Pollutant Trends, 1900-1998. EPA-454/R-00-02, U.S. Environmental
Protection Agency, Office of Air Quality Planning and Standards, Research Triangle
Park, NC, 27711.
3. Environmental Technology Verification Program Quality Management Plan, EPA/600/R-
03/021, December 2002.
4. Determination of the Strong Acidity of Atmospheric Fine Particles (<2.5 |j,m) Using
Annular Denuder Technology, EPA/600/R-93/037, U.S. Environmental Protection
Agency, Office of Research and Development, Research Triangle Park, North Carolina,
27711.
5. Operating Manual - ChemComb Model 3500 Speciation Sampling Cartridge, Revision A,
Rupprecht & Patashnick, Co., Inc., Albany, NY, January 2000.
6. Generic Verification Protocol for the Advanced Monitoring Systems Pilot, Battelle,
Columbus, Ohio, November 1998.
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Appendix A
Example Field Data Sheet
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ETV Verification of Ambient Ammonia Monitors
Reference Method Field Data Sheet
GENERAL
Site: Date:
Sample ID: Operator:
EQUIPMENT
MFC No.: Denuder ID:
Flow Rate Set Point: Filter ID:
Set Up Operator:
Start Time:
Leak Check Before:
SAMPLING DATA
Retrieval Operator:
Stop Time:
Leak Check After:
Time
Flow Rate
(1pm)
Ambient
Temp. (C)
Barometric
Pressure
(mm Hg)
Rel.
Humidity
(%)
Comments
Operator Comments:
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Date: September 2, 2003
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Appendix B
Example Chain of Custody Sheet
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