0 Baiteiie . . . Putting Technology To Work Environmental Technology Verification Program Advanced Monitoring Systems Center Test/QA Plan for Verification of Continuous Emission Monitors for Ammonia at a Coal-Fired Facility ET^ET^EIV ------- TEST/QA PLAN FOR VERIFICATION OF CONTINUOUS EMISSION MONITORS FOR AMMONIA AT A COAL-FIRED FACILITY June 2003 Prepared by Battelle 505 King Avenue Columbus, OH 43201-2693 ------- TABLE OF CONTENTS Page 1.0 INTRODUCTION 1 1.1 Test Description 1 1.2 Test Objective 1 1.3 Organization and Responsibilities 2 2.0 VERIFICATION APPROACH 10 2.1 Introduction 10 2.2 Scope 10 3 .0 SITE DESCRIPTION 12 4.0 EXPERIMENTAL DESIGN 12 4.1 General Design 12 4.2 Test Conditions 14 4.3 Test Procedures 15 4.4 Data Comparisons 19 5.0 STATISTICAL CALCULATIONS 22 5.1 Relative Accuracy 22 5.2 Comparability 23 5.3 Linearity 23 5.4 Precision 23 5.5 Calibration and Zero Drift 24 5.6 Response Time 24 6.0 MATERIALS AND EQUIPMENT 25 6.1 Gases and Chemicals 25 6.2 Reference Method 25 6.3 Facility Monitoring Equipment 26 6.4 Equipment Used for Performance Evaluation Audits 26 ------- TABLE OF CONTENTS (Continued) Page 7.0 QUALITY ASSURANCE/QUALITY CONTROL 28 7.1 Equipment Calibrations 28 7.2 QA/QC Samples 30 7.3 Assessment and Audits 31 8.0 DATA ANALYSIS AND REPORTING 35 8.1 Data Acquisition 35 8.2 Data Review 36 8.3 Reporting 36 9.0 HEALTH AND SAFETY 38 10.0 REFERENCES 39 Tables Table 4-1. Summary of Flue Gas Parameters or Constituent Concentrations Typically Observed at the Host Facility 14 Table 4-2. Summary of Data to be Obtained in Ammonia CEM Verification Test 20 Table 7-1. Summary of PE Audits 32 Table 8-1. Summary of Data Recording Process 37 Figures Figure 1-1. Organization Chart for the Ammonia CEM Verification Test 3 ------- ETV Advanced Monitoring Systems Center Test/QA Plan for Verification of Continuous Emission Monitors for Ammonia at a Coal-Fired Facility Version 1.0 June 25, 2003 APPROVAL: Name Company Date ------- 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 Mr. James Fletcher American Electric Power Company 1 Riverside Plaza Columbus, Ohio 43215-2373 Mr. Charles Dene EPRI 3412 Hillview Avenue Palo Alto, CA 93404-1395 Mr. Jan Grimbrandt Siemens Laser Analytics Box 5065, SE-402 22 Gooteborg, Sweden Mr. Paul Stenberg Opsis, Inc. 1165 Lindavista Drive Suite 112 San Marcos, CA 92069 Karen Riggs Amy Dindal Ken Cowen Zachary Willenberg Battelle 505 King Avenue Columbus, OH 43201 ------- Page 1 of 39 Version 1.0 Date: 6/25/03 1.0 INTRODUCTION 1.1 Test Description This test/quality assurance (QA) plan provides procedures for a verification test of continuous emission monitors (CEMs) used to measure gaseous ammonia in source emissions. 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 have an independent and credible assessment of what they are buying and permitting. 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 The objective of the verification test is to verify the performance of commercial ammonia CEMs, by comparison to reference ammonia measurements, and by challenges with ammonia standard gases, under normal operating conditions in a full-scale coal-fired power plant utilizing a Selective Catalytic Reduction (SCR) NOx control technology. ------- Page 2 of 39 Version 1.0 Date: 6/25/03 1.3 Organization and Responsibilities The verification test will be performed by Battelle in cooperation with EPA, the vendors who will be having their CEMs verified, American Electric Power (AEP), and the Electric Power Research Institute (EPRI). The organization chart in Figure 1-1 shows the individuals from Battelle, the vendor companies, EPA, AEP, and EPRI who will have responsibilities in the verification test. The specific responsibilities of these individuals and organizations are detailed in the following paragraphs. 1.3.1 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, contractor, host site, EPRI, and vendor staff to conduct the verification test Guide the Battelle/contractor/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 ------- Page 3 of 39 Version 1.0 Date: 6/25/03 Figure 1-1. Organizational Chart of Ammonia CEM Verification Test ------- Page 4 of 39 Version 1.0 Date: 6/25/03 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 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 ------- Page 5 of 39 Version 1.0 Date: 6/25/03 Conduct quality review of procedures/documentation provided by the sampling/analysis contractor 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 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 CEMs Assist vendors and test facility staff as needed during the CEM 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 CEMs data as needed Perform statistical calculations specified in this test/QA plan on the analyzer 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 ------- Page 6 of 39 Version 1.0 Date: 6/25/03 audits related to statistics and data reduction as needed. 1.3.2 Vendors Vendor representatives will: Review the draft test/QA plan Approve the final test/QA plan Provide an ammonia CEM for the duration of the verification test Commit or train a technical person to operate, maintain, and repair the CEM throughout the verification test Participate in verification testing, including providing data acquisition for their CEMs Provide to Battelle staff the data from their CEM at the conclusion of each test day Review their respective draft verification report and verification statement. 1.3.3 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).(2) The roles of specific EPA staff under the ETV QMP are as follows: Ms. Elizabeth Betz is EPA's AMS 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 ------- Page 7 of 39 Version 1.0 Date: 6/25/03 Notify the Battelle 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 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. 1.3.4 Host Facility This verification test will be conducted in collaboration with American Electric Power, who will provide a host facility for the test. The responsibilities of AEP and its on-site contractor are: Coordinate the operation of the host facility for the purposes of ETV testing Coordinate the installation of vendors' equipment at the host facility Communicate needs for safety and other training of staff working at the host facility Contribute to the development of the draft test/QA plan Review the draft test/QA plan ------- Page 8 of 39 Version 1.0 Date: 6/25/03 Provide on-site staff to assist during testing Provide calibrated facility monitoring equipment (Sections 6.3 and 7.11) Provide data on facility operations during testing, for the verification reports Provide input in responding to any issues raised in assessment reports and audits related to facility operations Review draft verification reports and statements 1.3.5 Reference Sampling/Analysis Subcontractor(s) Reference method sampling for ammonia will be conducted by one or more subcontractors to Battelle. Analysis of the collected samples will be conducted by Battelle or one or more subcontractors to Battelle. Such subcontractors may include organizations responsible for operation of the host facility. The responsibilities of such subcontractors are: Review the draft test/QA plan Adhere to the quality requirements in this test/QA plan Assemble trained technical staff to conduct reference method sampling for the verification test Oversee and conduct laboratory analysis of the reference method samples as appropriate Report reference method analytical and quality assurance results to Battelle in an agreed-upon format Support Dr. Cowen in responding to any issues raised in assessment reports and audits related to reference method sampling and analysis. ------- 1.3.6 EPRI Page 9 of 39 Version 1.0 Date: 6/25/03 EPRI is providing co-funding for this verification test. EPRI's activities will also include: Review the draft test/QA plan Provide input on the schedule and procedures for reference method sampling and analysis Review the reference method data Review the draft verification reports and statements. ------- Page 10 of 39 Version 1.0 Date: 6/25/03 2.0 VERIFICATION APPROACH 2.1 Introduction This test/QA plan is applicable to the verification testing of commercial CEMs for determining gaseous ammonia in combustion source emissions. This plan is specific for measurement of ammonia from a full-scale coal-fired power plant employing SCR NOx control technology. The CEMs to be tested in this verification test are based on various technologies including tunable diode lasers and differential chemiluminescence NOx measurement. These technologies can be employed either in an extractive mode to remove flue gas from the duct, with a flow-through insertion probe to measure a small sample volume in-situ, or in a cross-stack mode to measure average concentrations across the width of the duct. 2.2 Scope The overall objective of the verification test described in this plan is to provide quantitative verification of the performance of the ammonia CEMs in realistic test conditions. This verification test evaluates the performance of new CEMs, installed in an operational full- scale facility, over a relatively short test period, in the hands of vendor staff skilled in their operation, or on-site support staff who have been trained by the vendors. The performance parameters that are addressed by this test/QA plan include: Accuracy Comparability • Linearity • Precision Calibration drift • Zero drift ------- Page 11 of 39 Version 1.0 Date: 6/25/03 Response time Ease of use Completeness Accuracy will be assessed for the CEMs being verified by determining the degree of agreement with known concentrations of compressed ammonia gas standards. Comparability will be assessed through the degree of agreement with a reference method. Precision will be assessed in terms of the repeatability of the ammonia measurements under stable test conditions. Calibration drift, zero drift, linearity, and response time will be assessed using commercial compressed gas standards of ammonia. This verification test will be conducted concurrently for all CEMs being verified, and will occur over a period of approximately five weeks. The performance of the CEMs over that period will be assessed and reported. It is beyond the scope of this verification test to simulate the aging and exposures that may affect a CEM during routine long-term use. It must be noted that long-term performance may be different from that observed in the testing described here. However, the effort spent in installing and maintaining each CEM will be documented and used to assess ease of use. The amount of time each CEM is operational and maintenance activities performed over the verification test period will be recorded and reported, to help assess data completeness. ------- Page 12 of 39 Version 1.0 Date: 6/25/03 3.0 SITE DESCRIPTION This verification test will be conducted at AEP's Mountaineer Plant which is a coal-fired power plant located in New Haven, West Virginia. The CEMs to be tested will be installed at the exit of the air SCR and upstream of the air heater. At the testing location the duct dimensions are approximately 20 feet by 40 feet. Access to the flue gas for the CEMs and for wet chemical reference sampling will be available through ports in the duct at the testing location. Appropriate ports will be available for those CEMs requiring cross-duct access. The ammonia concentration in the duct will be mapped either prior to or after testing to assess the degree of stratification. Adjustments to the measured concentrations will be made based on the results of this mapping. During the test period, the boiler and SCR are scheduled to operate continuously. 4.0 EXPERIMENTAL DESIGN 4.1 General Design The verification test described in this test/QA plan will be conducted over a period of approximately five weeks. A window of approximately two weeks prior to testing will be available for installing the commercial CEMs at the facility, and conducting a shakedown run of all the CEMs before the verification test begins. The installation/shakedown period is scheduled for approximately June 30 - July 11, 2003. The five weeks of testing will follow immediately after the setup/shakedown period. Testing will not begin until all of the reference method equipment is ready and the facilities are operating normally. Similarly, it is desirable that all the commercial CEMs be fully operational to participate in the verification test. However, to avoid delaying the start of the testing, it will be required that all participating CEMs arrive at the facility, and be ready to begin testing on July 14, or when the facility itself is fully ready, whichever is later. CEMs which are not ------- Page 13 of 39 Version 1.0 Date: 6/25/03 operational at that time may join the testing process if they come on-line before the fifth day of testing. The ammonia CEM testing will involve continuous monitoring of ammonia by the CEMs over the entire test period with reference method sampling conducted on each weekday during the first and fifth weeks of the test period. On each day of reference method sampling, duplicate reference method samples will be collected over each of three different sampling periods. The average CEM readings during these periods will be used for comparisons with the ammonia concentrations measured from the reference method samples. During each day of reference method sampling, a zero and span check will be conducted on the CEMs by challenging each with zero air and an ammonia gas standard. These zero/span checks will be used to assess drift of the CEMs during the test period. During the third week of testing, each of the CEMs will independently be challenged with a series of runs involving dynamic spiking of compressed ammonia gas standards. The results of these runs will be used to assess accuracy of the CEMs as well as the linearity in instrument response. Throughout the verification test, each CEM undergoing testing will be operated by the CEM vendor's own staff or by on-site staff trained by the vendor. However, the intent of the testing is for the CEM to operate continuously in a manner simulating operation at a combustion facility. As a result, once the verification test has begun, no adjustment or recalibration will be performed, other than what would be conducted automatically by the CEM in normal unattended operation. Repair or maintenance procedures may be carried out at any time, but testing will not be interrupted, and data completeness will be reduced if such activities prevent collection of CEM data required for verification. The procedures of this verification test are described in more detail in the subsequent sections. ------- Page 14 of 39 Version 1.0 Date: 6/25/03 4.2 Test Conditions Table 4-1 shows the approximate levels of ammonia and other constituents that are typical of the flue gas stream at the host facility. Actual concentrations of these parameters and gaseous constituents during the testing period will be measured by the host facility's routine monitoring systems, or by the subcontractor conducting the reference method sampling. In all cases when reference method sampling is being conducted, the fuel loading and ammonia injection rate will be held as constant as possible throughout the entire sampling period (e.g., fuel loading rate within ± 10%, and ammonia injection rate within ± 10%). The intent of this approach is to allow comparisons of CEM data to reference method data under constant conditions. It is expected that during normal operation, the ammonia concentrations in the flue gas will be at or below 2 ppmv, and during dynamic spiking the range of concentrations will be changed to be between approximately 0 and 10 ppmv. Table 4-1. Summary of Flue Gas Parameters or Constituent Concentrations Typically Observed at the Host Facility Parameter/Constituent Typical Cone, or Range nh3 1-2 ppmv NOx 37 ppmv S02 540 ppmv 02 -3.8% Dust loading 4.3 grains/dscf H20 -8% C02 -15% Temperature Typically 600-650 up to 750 F ------- Page 15 of 39 Version 1.0 Date: 6/25/03 4.3 Test Procedures The CEMs undergoing verification will be installed between the exit of the SCR and the inlet of the air heaters. Ports for the reference method sampling will be located on the same duct with the CEMs as close as possible to the sampling locations of the CEMs. The sampling ports will be assigned so that no CEM is affected by the operation of any other CEM or by the reference method sampling. In-situ CEMs should be installed with either an in-line gas cell, or an external gas cell that can be used for calibration and dynamic spiking purposes. Likewise the extractive systems should be installed with a means of spiking compressed gas into the sampling probe upstream of the in-line filter. At either the beginning or the end of each test day during the first and fifth weeks of testing, the CEMs undergoing testing will be supplied (one at a time) with zero gas and then with a commercial compressed gas standard containing ammonia. The order in which the CEMs are to be tested will be varied, as will the time of day during which the CEMs are challenged. After reaching equilibrium, the response to each gas will be recorded for use in assessing the zero and calibration drift of the CEMs. During the second and fourth weeks of the test, the CEMs will continue to operate continuously, though no zero/span checks or reference sampling will take place. 4.3.1 Reference Method During testing, wet chemical reference samples will be collected during the first and fifth weeks. Verification will include comparisons of the CEM results with those from a time- integrated EPA Conditional Test Method for measurement of ammonia in flue gas (CTM027)(4). The conditional test method is similar to a draft ASTM method(5) for measurement of ammonia, which is designed specifically for the measurement of low levels of ammonia, typical of slip concentrations from SCR applications. There are however some notable differences between the two methods. The primary difference between the two methods involves the sample analysis rather than the sample collection. The draft ASTM method(5) calls for analysis by ion selective ------- Page 16 of 39 Version 1.0 Date: 6/25/03 electrode (ISE) whereas the EPA method(4) calls for analysis by ion chromatography (IC). Other differences between the draft ASTM method and the EPA CTM027 include different concentrations and volumes of the H2S04 solution in impingers 1 and 2 of the sampling train. The draft ASTM method calls for a smaller volume of a more dilute acid solution. This is more appropriate than the levels recommended in the EPA CTM027 method for the measurement of low levels of ammonia, so the ASTM levels will be used in the EPA CTM027 method for this verification test. During verification testing, reference sampling will be conducted simultaneously with two trains co-located with the CEMs being tested. The sampling duration for each run will typically be between 30 and 60 minutes. Thus each of the three reference sampling periods during a test day will provide two reference ammonia samples for comparison to the CEM data. Unique sample identification numbers will be implemented so that final data used for verification can be traced back through the analytical process to the original sample. Field blank samples will also be recovered from one blank sampling train on each of three days during each week that reference method samples are collected. Before sample recovery, that blank train will be transported to the sampling location. Care will be taken that the blank train is selected at random from the prepared trains, so that different trains are used as the blank on different days. Additionally, on each of three days during each week of reference sampling, one sample train will be spiked with ammonia solution to serve as a field spike sample. Samples will be recovered from the reference method trains within two hours of sample collection, and each of the reference samples will be split into two portions with one portion analyzed on-site by the draft ASTM method(5) using an ISE (e.g., Thermo-Orion NH3/NH4+ gas sensing electrode, or similar), and the second portion analyzed in the laboratory by the EPA CTM027(4) using an IC (e.g., Dionex Model 2120, or similar). The ISE analysis will be conducted within two hours of sample recovery by Battelle or subcontractor staff, using available on-site facilities. The front and back impingers will be analyzed separately on-site by ISE. If no breakthrough has occurred, the solutions will be combined for IC analysis. The results of the on-site by ISE will not be used for verification of the CEMS. Rather they will be used to assess the ammonia levels being sampled and to ensure that the reference sampling is ------- Page 17 of 39 Version 1.0 Date: 6/25/03 being performed properly. Samples for IC analysis will be stored at 4°C ± 2°C (not frozen) until shipment to the analytical laboratory and will be shipped on blue ice to the analytical laboratory within one week of sample collection. After receipt at the laboratory, the samples will be stored at 4°C ± 2°C until analysis, and will be analyzed within two weeks of receipt. Just prior to IC analysis the samples will be removed from refrigerated storage and allowed to slowly warm to room temperature. At the ammonia concentrations to be used in this verification, it is expected from previous results6 that the precision of duplicate reference method results will be within about 35 percent relative percent difference. It is expected that day-to-day reproducibility of ammonia levels in the facility will also be within that range. Thus, during normal operation it is expected that the ammonia levels will be consistent to ± 35% throughout each week of testing. As a result, the entire set of reference method results, not merely those from a single test day, will be considered in screening for reference data quality. The reference method results will be reviewed before verification comparisons are made, to identify individual statistical outliers from the full set of reference method results. That is, the reference method results will be screened for two factors: • Precision of results from co-located sampling trains • Consistency of results with previous and later results at the respective sampling location Identification of outliers will be based on basic statistical tests such as a t-test comparison of means, or a Q-test evaluation of divergent results. In any case where rejection of a reference result is suggested, effort will be made to find an assignable cause for the divergent result. Reference method results which are identified as statistical outliers on any of these criteria will be reported, but will not be used for verification. The intent of this approach is to provide a valid set of reference data for verification purposes, while also illustrating the degree of variability of the reference methods. ------- Page 18 of 39 Version 1.0 Date: 6/25/03 4.3.2 Dynamic Spiking During the third week of testing, each of the CEMs will be challenged with a series of dynamic spiking runs. During these runs the ammonia concentrations will be increased by approximately 2, 5, and 8 ppmv above the flue gas concentration. At each spike concentration, a series of runs will be conducted including 12 spiked and 12 unspiked sample measurements. These measurements will be performed by sampling pairs of spiked samples, followed by sampling pairs of unspiked samples. Prior to measurement, each CEM will be readied by purging the gas cell (for in-situ analyzers) with at least 10 volumes of zero air or by purging the sampling probe (for extractive CEMs) with at least 10 volumes of sample gas. After this purging is completed, a standard ammonia gas mixture will be introduced, at a measured flow rate, to the gas cell (for in-situ analyzers), or to the sampling probe (for extractive CEMs). The CEM readings of the spiked sample will be recorded after at least 10 volumes of gas have passed through the gas cell or sampling probe. A second spiked sample will be measured after at least five volumes of gas have passed through the sample cell or sampling probe after the measurement of the first spiked sample. After the second spiked sample is measured, a pair of unspiked samples will be measured following the same procedure as the spiked samples with the exception that zero air will be substituted for the ammonia spike gas. The procedures for the collection of the spiked and unspiked samples will be conducted a total of six times at each of the spike concentrations to obtain 12 spiked and 12 unspiked samples at each concentration. For the in-situ CEMs, these dynamic spiking runs will be conducted by flowing compressed ammonia gas standards into the in-line or external gas cell to achieve the desired ammonia concentrations. The ammonia and the zero air will be supplied as described above or until the CEM readings reach equilibrium, at which point the measured concentration and the spike gas flow rate will be recorded. The volume/length of the gas cell, the optical pathlength, and the known concentration of the gas standard will be used to calculate the theoretical increase in cross-stack concentration introduced during the run. For the extractive CEMs, the dynamic spiking will be conducted by injecting ammonia gas into the probe tip upstream of the particulate filter such that the ammonia passes through as ------- Page 19 of 39 Version 1.0 Date: 6/25/03 much of the sampling system as possible. The ammonia gas standard should mix with the flue gas at a ratio of approximately 1 part spike gas to 9 parts flue gas or more dilute. The flow rate of the compressed gas and the dilution ratio of the spike gas will be used in calculate the theoretical increase in concentration introduced during the spiking. 4.4 Data Comparisons This section describes how the reference and CEM data will be used and compared to quantify the performance of the CEMs. Table 4-2 summarizes the data that will be used for the verification comparisons. The results of the dynamic spiking will be used to assess accuracy of the CEM results relative to calculated ammonia concentrations determined from the spike gas concentration and flow rate. For each spiking run, the difference between the ammonia concentration measured by the CEM and the calculated ammonia concentration from spiking will be determined. The differences will be used to assess accuracy of the CEM results as described in Section 5.1. For comparison to the reference method results, the measurements from each of the CEMs will be separately averaged over each of the individual reference sampling periods. Comparability with the reference method will be assessed by comparing the averaged CEM results during the reference sampling periods with the reference results from the respective periods as described in Section 5.2. A total of 30 ammonia reference sampling runs is planned in the verification test (15 during each of the first and fifth weeks of testing), with two reference method sampling trains operating simultaneously in each sampling run. Thus a total of 60 reference samples will be used to evaluate comparability of the CEMs relative to the reference method. Linearity of the CEM response will be assessed from the dynamic spiking results. The measured ammonia concentrations and the calculated ammonia concentrations will be used to assess linearity in the range from the background concentration to approximately 8 ppmv above background. A total of 72 data points (36 background and 12 each at 2, 5, and 8 ppmv above background) will be used for this assessment. ------- Page 20 of 3 9 Version 1.0 Date: 6/25/03 Table 4-2. Summary of Data to be Obtained in Ammonia CEM Verification Test Performance Parameter Objective Comparison Based On Total Number of Data Points for Verification Accuracy Determine degree of quantitative agreement with compressed gas standard Dynamic spiking with ammonia gas standards 36 Comparability Determine degree of quantitative agreement with reference method Reference method results 60 Linearity Determine linearity of response over a range of ammonia concentrations Dynamic spiking with gas standards 72 Precision Determine repeatability of successive measurements at fixed ammonia levels Repetitive measurements under constant facility conditions measured over the duration of each reference method sampling run, and each dynamic spiking run 66 Cal/Zero Drift Determine stability of zero gas and span gas response over successive days Zero gas and NH3 gas standard 10 Response Time Determine rise and fall time Recording successive readings at start and end of sampling NH3 gas standard 6 Precision of the CEMs will be assessed based on the individual measurements performed by each CEM over the duration of each reference method sampling run. For example, if a CEM provides an updated measurement every 5 minutes, then over a twenty five minute sampling run a total of 5 readings would be obtained. The average and standard deviation of those readings will be calculated to assess precision. This procedure will be applied to each of the 30 of the reference method sampling intervals, and each of the 36 dynamic spiking runs at elevated ammonia concentrations. Calibration and zero drift will be verified based on challenging the CEMs with zero gas and with a compressed gas standard of ammonia on each test day during the first and fifth weeks of the test. Thus up to 10 data points will be used to assess zero drift, and an equal number to assess calibration drift. Calibration drift of the CEMs will be assessed at approximately 80% of full scale for each of the respective CEMs. ------- Page 21 of 39 Version 1.0 Date: 6/25/03 CEM response time will be assessed once in each of the first, third, and fifth weeks of the test, by recording successive CEM readings as the CEM responds to the ammonia gas standard, or returns to baseline after analysis of that standard. The former readings will indicate the CEM rise time, and the latter the CEM fall time. No additional test activities will be required to determine the data completeness achieved by the CEMs. Data completeness will be assessed by comparing the data recovered from each CEM to the amount of data that would be recovered upon completion of all portions of these test procedures. Setup and maintenance needs will be documented qualitatively, both through observation and through communication with the vendors (or their trained representatives) during the test. Factors to be noted include the frequency of scheduled maintenance activities, the downtime of the CEM, and the number of staff operating or maintaining it during the verification test. ------- Page 22 of 3 9 Version 1.0 Date: 6/25/03 5.0 STATISTICAL CALCULATIONS The statistical calculations to be used to verify CEM performance are described below. In all cases, measurement results from both the reference method and the CEMs undergoing testing are to be reported in units of ppmv on a dry basis at 20 °C, 1 atmosphere pressure, and the actual flue gas 02 content. All calculations will be performed using Microsoft Excel™. 5.1 Relative Accuracy The relative accuracy (RA) of the CEMs with respect to the ammonia gas standards will be assessed using Equation 1: d + t n-1 RA = S^_ 4n x 100% (1) x where d refers to the difference between the calculated ammonia concentration from the dynamic spiking and the average of the CEM measurements recorded during the respective spiking periods, and x corresponds to the calculated spike concentration. Sd denotes the sample standard deviation of the differences, while t^ is the t value for the 100(1 - a)th percentile of the distribution with n-1 degrees of freedom. The relative accuracy will be determined for an a value of 0.025 (i.e., 97.5 percent confidence level, one-tailed). The RA calculated in this way can be interpreted as an upper confidence bound for the relative bias of the analyzer, i.e., 4^, where the superscript bar indicates the average value of the differences or of the reference values. Relative accuracy will be calculated separately at each of the spiking levels. ------- Page 23 of 39 Version 1.0 Date: 6/25/03 5.2 Comparability Comparability between the CEM results and the EPA CTM027 reference method results will be assessed using Equation 1, in which d represents the difference between the average of paired reference method results and the average of the CEM results from the period during which the paired reference method samples were collected, and x corresponds to the average of the paired reference method results. Comparability will be calculated using all EPA CTM 027 reference method sample results (assuming all reference method samples can be treated as independent results). The impact of the number of data points (n) on the RA value will be noted in the verification report. 5.3 Linearity Linearity will be assessed by a linear regression analysis of the dynamic spiking data using the calculated ammonia concentrations as the independent variable and the CEM results as the dependent variable. Linearity will be expressed in terms of slope, intercept, and coefficient of determination (r2). 5.4 Precision Precision will be calculated in terms of the percent relative standard deviation (RSD) of a series of CEM measurements made over the duration of each reference method sampling run with ammonia injected at a constant level into the SCR zone, and during each of the dynamic spiking runs. During each reference method sampling run, and during each dynamic spiking run, all readings from a CEM undergoing testing will be recorded, and the mean and standard deviation of those readings will be calculated. Precision (P) will then be determined as: SD p = ^x 100 (1) X ------- Page 24 of 3 9 Version 1.0 Date: 6/25/03 where SD is the standard deviation of the CEM readings and X is the mean of the CEM readings. This calculation will be done for each CEM, using the CEM data collected during every reference method sampling run and dynamic spiking run. The verification report will note that the calculated precision is subject to the variability of the host facility, and not only to the CEM variability. Although no comparison among CEMs will be made, all CEM data from the periods of reference sampling will be reviewed, to assess whether the consensus of the CEM data indicates an unusual variation in the test facility itself. If such a variation is indicated, that finding will be noted in all verification reports. 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 CEM in the daily sampling of the same ammonia standard gas, and of zero gas. Up to 10 ammonia standard readings, and up to 10 zero readings, will be used for this calculation. This calculation, along with the range of the data, will indicate the day-to-day variation in zero and standard readings. 5.6 Response Time Response time will be assessed in terms of both the rise and fall times of each ammonia CEM when sampling the ammonia gas standard. Rise time (i.e., 0% - 95% response time) will be determined by recording all CEM readings as the gas supplied to the CEM is switched from zero gas to the ammonia standard. 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 CEM readings as the gas supplied is switched from the ammonia standard back to zero gas. For CEMs which 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 CEM in each of the first, third, ------- Page 25 of 39 Version 1.0 Date: 6/25/03 and fifth weeks of the test. Thus a total of six data points will be obtained relevant to response time for each CEM. Rise and fall times will be reported in units of seconds. 6.0 MATERIALS AND EQUIPMENT 6.1 Gases and Chemicals 6.1.1 High Purity Nitrogen/Air The high purity gases used for zeroing of the CEMs will be commercial ultra-high purity (UHP, i.e., minimum 99.999% purity) air or nitrogen. 6.1.2 Ammonia Standard Gases Compressed gas standards containing ammonia will be obtained for use in the calibration checks and the dynamic spiking activities of the CEMs. These will consist of ammonia in a nitrogen matrix, at levels appropriate to achieve increases above background concentrations of approximately 2, 5, and 8 ppmv during dynamic spiking, and for use in the calibration checks performed during the first and last weeks of testing. Multiple cylinders of uniform concentration will be obtained, if required to meet the gas consumption rates of the CEMs during the test. 6.2 Reference Method 6.2.1 Sampling Trains The glassware, filters, and associated equipment for performance of the reference method(4) sampling will be supplied by the subcontractor and will meet the requirements of the EPA conditional test method for ammonia measurement. Multiple trains will be supplied so that six trains (i.e., three sampling runs with two trains each) may be sampled in a single day, in ------- Page 26 of 3 9 Version 1.0 Date: 6/25/03 addition to at least three blank trains and three spiked trains per week. Preparation, sampling, sample recovery, and cleaning of used trains will be the responsibility of the contractor in this verification test. 6.2.2 Analysis Equipment Laboratory equipment for sample recovery and analysis will be provided by either the subcontractor or by Battelle, depending on who will conduct the analysis. This equipment will include all chemicals and solutions for preparation of the samples for analysis as well as for the analysis of the samples. An ISE will be provided for on-site analysis, and an IC will be available for laboratory analysis. 6.3 Facility Monitoring Equipment This verification will make use of monitoring equipment already integrated into the host facility. This equipment includes monitors for major flue gas constituents (02, C02) and for chemical contaminants (CO, NOx, S02), as well as sensors for temperature and pressure and may include ammonia CEM systems already installed at the facility. These devices are considered part of the host facility for purposes of this test, and will be operated by the host facility during this verification according to normal facility procedures. 6.4 Equipment Used for Performance Evaluation Audits As described in Section 7.3.2, performance evaluation (PE) audits will be performed for the 02, C02, temperature, and pressure measurements in the flue gas. Those PE audits will be performed by conducting a parallel measurement using an independent monitoring device. The devices to be used will be provided by Battelle, and may include the following: Paramagnetic 02 monitor ------- Page 27 of 3 9 Version 1.0 Date: 6/25/03 • Infrared C02 monitor Thermocouple temperature indicator • Aneroid barometer Magnehelic differential pressure indicator • Flow meter. These devices will have been calibrated by the manufacturer or by Battelle's Instrument Laboratory within the six months immediately preceding the verification test, or calibrated on site as necessary. In addition, a calibrated set of weights will be used, to audit the balance used to weigh impingers from the reference method trains (used for determining flue gas H20 content). A NIST-traceable ammonia standard will also be used to spike three blank reference method trains, in each of the first and fifth weeks of the test to assess the overall ammonia measurement. NIST-traceable ammonia standards will be used to prepare blind audit samples to assess the performance of both the ISE and the IC. ------- Page 28 of 39 Version 1.0 Date: 6/25/03 7.0 QUALITY ASSURANCE/QUALITY CONTROL The subcontractor^s) performing the reference method sampling must perform all required quality assurance/quality control (QA/QC) activities stated in the method(4). This includes provision of blank sampling trains (three per week), and of blank sampling materials (filters, reagent solution blanks) in the field. Documentation of these activities will be required for inclusion in the verification data file. Deviation from the reference method(4) will occur in that the concentrations and volumes of the solutions used in the impingers will be those identified in the draft ASTM method(5). Spiking of reference trains will be performed by Battelle staff, as described in Section 7.3.2. 7.1 Equipment Calibrations 7.1.1 Host Facility Equipment The host facility CEMs and other monitoring devices noted in Section 6.3 will be calibrated by host facility staff according to normal facility procedures. All calibration results must be documented for inclusion in the verification test data files and verification report. 7.1.2 Reference Method Sampling Equipment Equipment used for the collection of the reference samples will be calibrated by the subcontractor(s) according to the procedures described in the reference method(4). All calibration results must be documented for inclusion in the verification test data files and verification report. 7.1.3 Analytical Equipment Analysis of the reference samples will be conducted both on-site using an ISE and in a laboratory using IC. The ISE analysis will be used only for initial QA purposes to ensure that ------- Page 29 of 3 9 Version 1.0 Date: 6/25/03 the ammonia levels in the duct are within the expected range and to ensure that the reference sampling is being conducted properly. The ISE will be calibrated according to the manufacturer's recommendations using at least three different solutions prepared from NIST- traceable ammonia standards. Immediately after calibration, at least three standard solutions will be reanalyzed using the ISE. If the ISE reading does not agree between the standard concentration of the solutions within 10% the calibration will be repeated. The calibration will be conducted on-site daily during each week of reference sampling and will include ammonia concentrations that will bracket the concentrations expected in the reference samples. The equipment used for the IC analysis will be calibrated by staff of the laboratory performing the analysis. The calibration will be conducted according to the manufacturer recommendations and the requirements of the reference method,(4) and will include concentrations of ammonia standard solutions that bracket the expected concentration of the sample solutions. The calibration will be acceptable if the r2 of the calibration curve is >0.95. All calibration results must be documented for inclusion in the verification test data files and verification report. 7.1.4 Calibration Check/Dynamic Spiking Equipment The dry gas meter used for measurement of the spike gas flow rate during the calibration checks and the dynamic spiking activities will be calibrated by the Battelle Instrument Laboratory against a NIST-traceable flow transfer standard. The date of the calibration will be within one year of the date of the dynamic spiking activities. ------- Page 30 of 39 Version 1.0 Date: 6/25/03 7.2 QA/QC Samples 7.2.1 Field Blanks During each week of reference method sampling, a total of three sampling trains will be used as field blank samples. These trains will be prepared and transported to the sampling location but will not be used to collect a sample of flue gas. The trains will then be disassembled and the field blank solutions will be analyzed on-site by ISE to ensure that the background concentration due to on-site handling and exposure is negligible relative to the ammonia content of the samples. If background levels are greater than 10% of the sample concentrations, no additional reference sampling will be conducted until the cause of the contamination is identified and rectified. The field blank solutions will also be analyzed in the laboratory by IC. 7.2.2 Laboratory Blanks Laboratory blank solutions will be prepared for both ISE and the IC analysis. The solutions will be analyzed prior to analysis of the reference samples. A laboratory blank solution will be analyzed after every 10th reference method sample to ensure no drift in the ISE or IC instrumentation. If the blank levels are greater than 10% of the expected sample concentrations, the cause of the contamination is identified and rectified, and all analyses performed after the most recent acceptable blank will be invalidated and analysis of those samples will be repeated (if possible). 7.2.3 Laboratory Spikes Laboratory spike solutions will be prepared with concentrations approximately equal to ammonia concentrations expected from the collection of a 5 ft3 sample of flue gas with 2 ppmv ammonia. These solutions will be prepared for both ISE and the IC analysis using NIST- traceable ammonia solutions. The solutions will be analyzed prior to analysis of the reference ------- Page 31 of 39 Version 1.0 Date: 6/25/03 samples. A laboratory spike solution will be analyzed after every 10th reference method sample to ensure no drift in the ISE or IC instrumentation. If the measured concentrations are not within ±10% of the spike 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). 7.3 Assessment and Audits 7.3.1 Technical Systems Audits Battelle's ETV Quality Manager, Mr. Zachary Willenberg, will perform a technical systems audit (TSA) once during the performance 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, Mr. Willenberg may review the reference sampling and analysis methods used, compare actual test procedures to those specified in this plan, and review data acquisition and handling procedures. Mr. Willenberg 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 CEMs being verified and the vendors operating these CEMs are not the subject of the performance evaluation audit. This audit will be performed once during the verification test, and must be performed by analyzing a standard or ------- Page 32 of 39 Version 1.0 Date: 6/25/03 comparing to a reference that is independent of standards used during the testing. For most of the key measurements, this audit will be done by comparing data from the facility equipment to that from a second analyzer or monitor, operated simultaneously. For example, the PE audit of 02 data will involve sampling with a second 02 analyzer at the same point in the duct, and comparing results. The will be calculated as the difference between the two readings divided by the audit reading. Similar comparisons will be made for temperature, pressure, and C02. In addition, the balance used to determine flue gas H20 content by means of the reference method impinger samples will be checked with a calibrated set of weights different from those used to calibrate the balance for use. Table 7-1 summarizes the PE audits that will be done. These audits will be the responsibility of Battelle staff, and will be carried out with the cooperation of host facility staff. Table 7-1. Summary of PE Audits Parameter Audit Procedure Expected Tolerance 02 Compare to independent 02 measurement ±1% of 02 reading co2 Compare to independent C02 measurement ±10% of C02 reading Temperature Compare to independent temperature measurement ±2% absolute temperature Barometric Pressure Compare to independent pressure measurement ±0.5 inch of H20 Flue Gas Differential Pressure Compare to independent pressure measurement ±0.5 inch of H20 Mass (H20) Check balance with calibrated weights ±1% or 0.5 g, whichever is larger Ammonia (overall measurement) Spike reference method trains ± 20% bias in spike recovery Ammonia (ISE analysis) Blind audit sample ± 10% of standard concentration Ammonia (IC analysis) Blind audit sample ± 10% of standard concentration These PE audits will be carried out once during the period of operation at the host facility. Battelle will supply the equipment or standards needed to make the independent PE measurements. If agreement outside the indicated tolerance is found, the PE audit will be ------- Page 33 of 39 Version 1.0 Date: 6/25/03 repeated. Further failure to achieve agreement will result in re-calibration of the independent measurement device, and continued lack of agreement will result in all relevant data being flagged. The PE audit will include spiking reference method sampling trains with known amounts of ammonia, and conducting sample analysis on the train without sampling the combustion gas. A NIST-traceable ammonium standard solution will be used for that purpose. During each week of sampling, three blank trains will be prepared spiked with a known amount of an ammonia standard solution, such that the ammonia concentration in the sample solution is approximately equal to the concentration expected from the collection of a 5 ft3 sample of flue gas with 2 ppmv ammonia. The spiked trains will be transported to the sampling location but will not be used to collect a sample of flue gas. The trains will then be disassembled and the spiked samples will be analyzed on-site by ISE and the percent recovery will be calculated. Agreement of ammonia determined in sample analysis with that spiked into the sample train is expected to be within 20 percent. If the recovery of the field spikes is not >80% and <120%, no additional reference sampling will be conducted until the cause of the discrepancy is investigated and rectified if possible. Because reference sample analysis is performed on site by ISE, PE audit results for the overall ammonia measurement will be available during the test, and will be used to improve reference method procedures, if necessary. The performance of the ISE and the IC 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 ISE and the IC should 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. ------- Page 34 of 39 Version 1.0 Date: 6/25/03 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. ------- Page 35 of 39 Version 1.0 Date: 6/25/03 8.0 DATA ANALYSIS AND REPORTING 8.1 Data Acquisition Data acquisition in this verification test includes recording of the data from the CEMs undergoing testing, documentation of sampling conditions and analytical results from the reference method, and recording of operational data such as combustion source conditions, test temperatures, the times of test activities, etc. Data acquisition for the commercial CEMs undergoing verification will be performed by the CEM vendors during the test. Each CEM must have some form of data acquisition device, such as a digital display whose readings can be recorded manually, 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 CEM for the entire test period. The CEM data are to be provided to Battelle regularly, and must include all individual readings of the CEM 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 ASCII 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 CEM, and strict separation of data from different CEMs, will be maintained. Separate files (including manual records, printouts, and/or electronic data files) will be kept for each CEM. At no time during verification testing will Battelle staff engage in any comparison in performance of the participating CEMs. ------- Page 36 of 39 Version 1.0 Date: 6/25/03 Table 8-1 summarizes the types of data to be recorded; how, 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 turned over to Battelle staff immediately upon completion of each test day. Identical file formats will be used to make quantitative evaluations of the data from all CEMs 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 the test, before these records are used to calculate, evaluate, or report verification results. These records may include laboratory record books; operating data from the combustion source; data from the CEMs; 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 host facility, subcontractor and/or vendor staff 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. 8.3 Reporting The statistical data comparisons described in Section 5.0 will be conducted separately for each commercial ammonia CEM tested. Separate verification reports will then be prepared, each addressing the CEM 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. ------- Page 37 of 39 Version 1.0 Date: 6/25/03 Table 8-1. Summary of Data Recording Process Data to be Recorded Responsible Party Where Recorded How Often Recorded Disposition of Data00 Dates, times of test events Battelle/AEP Laboratory record books Start/end of test, and at each change of a test parameter. Used to organize/check test results; manually incorporated in data spreadsheets as necessary. Test parameters (temperature, analyte/interferant identities and concentrations, gas flows, etc.) AEP/ subcontractor Laboratory record books When set or changed, or as needed to document stability. Used to organize/check test results, manually incorporated in data spreadsheets as necessary. NH3 CEM readings Vendor or designee Data acquisition system (data logger, PC, laptop, etc.). Continuously at specified acquisition rate throughout CEM operation. Electronically transferred to spreadsheets Reference method sampling data Subcontractor Laboratory record books 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. Reference method sample analysis, chain of custody (CoC), and results Subcontractor or Battelle Laboratory record books, CoC forms, 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. 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 CEM tested, or comment on the acceptability of the CEM'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.(3) Preparation, approval, and use of Verification ------- Page 38 of 39 Version 1.0 Date: 6/25/03 Statements summarizing the results of this test will also be subject to the requirements of that same Protocol. 9.0 HEALTH AND SAFETY The verification test described in this test/QA plan will be performed at the AEP host facility. All participants in this verification test (i.e., Battelle, EPA, subcontractor, and vendor staff) will adhere to the health and safety requirements of the facility. Vendor staff will only be operating their CEMs during the verification test. They are not responsible for, nor permitted to, operate the combustion source, or perform any other verification activities identified in this test/QA plan. Operation of the CEMs themselves does not pose any known chemical, fire, mechanical, electrical, noise, or other potential hazard. All visiting staff at the host facility will be given a site-specific safety briefing prior to the installation and operation of the CEMs. This briefing will include a description of emergency operating procedures (i.e., in case of fire, tornado, laboratory accident) and identification and location and operation of safety equipment (e.g., fire alarms, fire extinguishers, eye washes, exits). ------- Page 39 of 39 Version 1.0 Date: 6/25/03 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. Environmental Technology Verification Program Quality Management Plan, EPA/600/R- 03/021, December 2002. 3. Generic Verification Protocol for the Advanced Monitoring Systems Pilot, Battelle, Columbus, Ohio, November 1998. 4. Procedure for the Collection and Analysis of Ammonia in Stationary Sources, Conditional Test Method 027, U.S. Environmental Protection Agency, Research Triangle Part, North Carolina, August 1997. 5. Standard Specification for Collection and Analysis of Ammonia Nitrogen in Flue Gas Using Wet Chemical Sampling and Specific Ion Analysis, Draft Standard, ASTM, West Conshohocken, Pennsylvania, October, 2000. 6. Field Test of Ammonia Collection/Analysis Method, Draft Report, U.S. Environmental Protection Agency, Research Triangle Park, North Carolina, September 1995. ------- |