United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-00-020
April 2000
Air
HOT Mix ASPHALT PLANTS
E PA KILN DRYER STACK
INSTRUMENTAL METHODS TESTING
ASPHALT PLANT "A"
CLAYTON, NORTH CAROLINA
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HOT MIX ASPHALT PLANTS
KILN DRYER STACK
INSTRUMENTAL METHODS TESTING
Asphalt Plant "A"
Clayton, North Carolina
Prepared for
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Emission Measurement Center (MD-19)
Research Triangle Park, North Carolina 27711
Mr. Michael L. Toney
Work Assignment Manager
EPA Contract No. 68-D-98-027
Work Assignment 3-02
MRI Project No. 104952-1-002-05
April 2000
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PREFACE
This test report was prepared by Midwest Research Institute (MRI) for the U. S.
Environmental Protection Agency (EPA) under EPA Contract No. 68-D-98-027, Work
Assignment No. 3-02. Mr. Michael Toney is the Work Assignment Manager (WAM). Mr. Scott
Klamm is the MRI Work Assignment Leader (WAL). The field test was performed under EPA
Contract No. 68-D2-0165, Work Assignment No. 4-24. A draft report was submitted under EPA
Contract No. 68-W6-0048, Work Assignment No. 2-08, Task 2 and a revised draft was submitted
under Work Assignment 2-10 of 68-D-98-027. Mr. Toney was also the WAM for the previous
work assignments. Dr. Thomas Geyer was the MRI WAL for Work Assignments No. 4-24 and
3-10 and the Task Leader for Task 2. Mr. John Hosenfeld was the MRI WAL for Work
Assignment No. 2-08.
This report consists of one volume (360 pages) with six sections and five appendices.
MIDWEST RESEARCH INSTITUTE
Hosenfeld
Program Manager
Approved:
Jeff Shular
Director, Environmental Engineering Department
April 2000
in
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TABLE OF CONTENTS
'Jage
1.0 INTRODUCTION 1-1
1.1 BACKGROUND 1-1
1.2 PROJECT SUMMARY 1-1
1.3 PROJECT PERSONNEL 1-7
2.0 PROCESS DESCRIPTION AND TEST LOCATIONS 2-1
2.1 PROCESS DESCRIPTION 2-1
2.2 TEST LOCATIONS 2-1
2.2.1 Baghouse Inlet Duct 2-1
2.2.2 Baghouse Outlet - Stack 2-1
2.3 VOLUMETRIC FLOW 2-1
3.0 RESULTS 3-1
3.1 TEST SCHEDULE 3-1
3.2 FIELD TEST PROBLEMS AND CHANGES 3-2
3.2.1 High Particulate at the Inlet 3-2
3.2.2 Method 25A Concentration Spikes 3-2
3.2.3 Addition of a Fourth Test Run 3-3
3.2.4 Method 25A Calibration Checks 3-3
3.2.5 Condenser Sampling 3-3
3.2.6 Inlet Flow Determination 3-3
3.3 METHOD 25A RESULTS 3-4
3.4 FTIR RESULTS .3-7
3.5 ANALYTE SPIKE RESULTS 3-8
4.0 TEST PROCEDURES 4-1
4.1 SAMPLING SYSTEM DESCRIPTION 4-1
4.1.1 Sample System Components 4-1
4.1.2 Sample Gas Stream Flow 4-3
4.2 FTIR SAMPLING PROCEDURES 4-3
4.2.1 Batch Sampling 4-4
4.2.2 Continuous Sampling 4-4
4.3 ANALYTE SPIKING 4-5
4.3.1 Analyte Spiking Procedures 4-5
4.3.2 Analysis of Spiked Results 4-7
4.4 ANALYTICAL PROCEDURES 4-7
4.4.1 Computer Program Input 4-9
4.4.2 EPA Reference Spectra 4-9
4.5 FTIR SYSTEM 4-9
4.6 CONTINUOUS EMISSIONS MONITORING FOR TOTAL
HYDROCARBONS (THC) 4-10
4.6.1 Total Hydrocarbon Sampling Procedures 4-10
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TABLE OF CONTENTS (continued)
5.0 SUMMARY OF QA/QC PROCEDURES 5-1
5.1 SAMPLING AND TEST CONDITIONS 5-1
5.2 FTIR SPECTRA 5-2
5.3 METHOD 25A 5-3
5.3.1 Initial Checks 5-3
5.3.2 Daily Checks 5-3
6.0 REFERENCES 6-1
APPENDIX A - METHOD 25A AND VOLUMETRIC FLOW DATA A-l
A-l METHOD 25A RESULTS A-2
A-2 METHOD 25A CALIBRATION AND QA CHECK DATA A-3
A-3 VOLUMETRIC FLOW DATA A-4
APPENDIX B - FTIR DATA B-l
B-l FTIR RESULTS TABLES B-2
B-2 FTIR FIELD DATA RECORDS B-17
B-3 FTIR FLOW AND TEMPERATURE READINGS B-18
APPENDIX C - EQUIPMENT CALIBRATION CERTIFICATES C-l
C-l CALIBRATION GAS CERTIFICATES C-2
C-2 ENVIRONICS MASS FLOW METER CALIBRATIONS C-3
APPENDIX D - TEST METHODS AND HC1 VALIDATION PAPER D-l
D-l EPA METHOD 320 D-2
D-2 EPA FTIR PROTOCOL D-3
D-3 EPA METHOD 25A D-4
D-4 EPA DRAFT METHOD 205 D-5
D-5 HC1 VALIDATION PAPER D-6
APPENDIX E - PROCESS DESCRIPTION E-l
VI
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LIST OF FIGURES
Figure 2-1. Baghouse inlet 2-2
Figure 2-2. Baghouse outlet (stack) 2-3
Figure 3-1. THC concentration trend graphs 3-6
Figure 4-1. Sampling system schematic 4-2
LIST OF TABLES
Page
TABLE 1-1. SUMMARY OF FTIR RESULTS FOR WET SAMPLES AT PLANT 1-4
TABLE 1-2. SUMMARY OF FTIR RESULTS FOR CONDENSER SAMPLES
AT PLANT A 1-5
TABLE 1-3. SUMMARY OF HYDROCARBON EMISSIONS RESULTS 1-6
TABLE 1-4. PROJECT PERSONNEL 1-7
TABLE 2-1. SOURCE GAS COMPOSITION AND FLOW SUMMARY AT PLANT A ... 2-4
TABLE 3-1. PLANT A FTIR AND 25A TEST SCHEDULE 3-1
TABLE 3-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS 3-7
TABLE 3-3. SPIKE RESULTS IN WET SAMPLES COLLECTED AT THE
BAGHOUSE INLET 3-11
TABLE 3-4. SPIKE RESULTS IN WET SAMPLES AT THE BAGHOUSE OUTLET ... 3-11
TABLE 3-5. SPIKE RESULTS IN CONDENSER SAMPLES AT THE BAGHOUSE
INLET 3-12
TABLE 3-6. SPIKE RESULTS IN CONDENSER SAMPLES AT THE BAGHOUSE
OUTLET 3-12
TABLE 3-7. COMPARISON OF EPA REFERENCE SPECTRA TO SPECTRUM OF
TOLUENE CYLINDER STANDARD 3-13
TABLE 4-1. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA 4-12
TABLE 4-2. PROGRAM INPUT FOR ANALYSIS AND CTS SPECTRA AND PATH
LENGTH DETERMINATION 4-13
TABLE 4-3. RESULTS OF PATH LENGTH DETERMINATION 4-13
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1.0 INTRODUCTION
1.1 BACKGROUND
The Emission Measurement Center (EMC) directed Midwest Research Institute (MRI) to
conduct emissions testing at asphalt concrete production plants. This was in response to a test
request from the Minerals and Inorganic Chemicals Group of the Emission Standards Division
(BSD) and Source Characterization Group of the Emission Monitoring and Analysis Division
(EMAD), both in the Office of Air Quality Planning and Standards (OAQPS), U. S. EPA. The
test program was done in August 1997 under work assignment 4-24, on EPA Contract
No. 68-D2-0165. This draft report was prepared under work assignment 2-08, on EPA Contract
No. 68-W6-0048.
The purpose of this project was to perform an emissions test on the inlet and outlet of a
baghouse that controls emissions from the counterflow rotary dryer process used at asphalt
Plant A in Clayton, NC. Midwest Research Institute used EPA FTIR Draft Method 3201 and
EPA Method 25A. Method 320 is an extractive test method using Fourier Transform infrared
(FTIR) spectroscopy. Method 320 uses quantitative analytical procedures described in the EPA
FTIR Protocol.2 Method 25A is an extractive test method using a Flame lonization Analyzer
(FIA). Data will be used to quantify and characterize hazardous air pollutant (HAP) emissions
and the performance of the control unit.
1.2 PROJECT SUMMARY
Asphalt paving materials are produced by drying and mixing various amounts of raw (and
sometimes recycled) materials in a rotary drum dryer. The product is carried from the dryer by
conveyor to heated storage silos before distribution by truck. The dryer emissions are drawn
through a baghouse for paniculate control before being emitted to atmosphere. Testing was
conducted at the inlet and outlet of the baghouse to determine the amount of measurable
emissions released.
Four test runs were conducted by MRI at each location over a 3-day period concurrently
with manual method testing conducted by Pacific Environmental Services, Inc. (PES). Test
Runs 1, 2, and 3 were conducted during production using reclaimed asphalt pavement (RAP).
Test Run 4 was conducted during production using non-RAP containing material.
1-1
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The FTIR samples were collected by alternately sampling the baghouse inlet and stack,
using a single instrument. Method 25A testing was continuous at both locations using two
analyzers. A summary of the FTIR results for samples collected on a hot/wet basis (i.e.,
extracted stack gas) direct to the instrument for Runs 1-4 is presented in Table 1-1. FTIR results
for samples collected on a cold/dry basis (i.e., stack gas moisture removed with a condenser) for
Runs 1-4 are summarized in Table 1-2. Only detected compounds are shown in Tables 1-1 and
1-2. Toluene is shown because some samples were spiked with toluene. The Method 25A
results are summarized in Table 1-3. The complete Method 25A results are in Appendix A, and
the complete FTIR results are in Appendix B.
The EPA Method 320 uses an extractive sampling procedure. A probe, pump, and heated
line are used to transport sample gas from the test port to a gas distribution manifold in a trailer
that contains the FTIR equipment. Infrared spectra of a series of samples were recorded and
quantitative analysis of the spectra was done after the FTIR data collection was completed. All
spectral data and results were saved on computer media. A compact disk containing all FTIR
data was provided with the draft report.
The FTIR spectra showed evidence that the emissions included a mixture of aliphatic
hydrocarbon compounds. The only HAP's in that classification are 2,2,4-trimethylpentane
(isooctane) and hexane. Therefore, in the draft report, the hydrocarbon emissions were primarily
represented by "hexane." Since the draft report was submitted, MRI has measured reference
spectra of some additional hydrocarbon compounds. The new reference spectra were included in
the revised analysis to obtain a better representation of the hydrocarbon emissions.
The EPA Method 25A also uses an extractive sampling procedure, and the same sample
transport system was used for both the FTIR and Method 25A testing. Volume concentration
data and results obtained from the samples were recorded and saved on computer media and
reviewed after the test was completed.
The "wet" results are from spectra of untreated samples. The "condenser" results are
from spectra of sample gas that was passed through an ice-temperature chiller to remove
moisture from the sample. The condenser results are reported on a dry basis. The condenser, by
reducing moisture interference, can aid the analyses of some compounds, but soluble species
such as formaldehyde are more accurately measured in the wet samples. Even the concentration
1-2
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of non-soluble species can be reduced by the condenser because vapor pressures are lower at the
condenser temperature. Note that the condenser and wet samples cannot be compared directly
because they were measured at different times (see Table 3-1).
1-3
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TABLE 1-1. SUMMARY OF FTIR RESULTS FOR WET SAMPLES AT PLANT Aa
Untreated (wet) Samples
Toluene
Hexane
Ethylene
Methane
Sulfur Dioxide
Carbon Monoxide
Formaldehyde
Butane
2-Methyl- 1-pentene
2-Methyl-2-butene
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
Run 1
Inlet
13.6
1.55
0.70
22.2
1.44
0.65
35.5
9.19
4.17
238.5
27.0
12.3
15.5
1.89
0.86
0.31
0.106
0.048
Outlet
3.22
1.12
0.51
15.6
1.77
0.80
20.8
1.35
0.61
51.8
13.42
6.09
226.9
25.7
11.7
9.0
1.10
0.50
1.1
0.26
0.12
Run 2
Inlet
3.9
0.55
0.25
62.9
5.04
2.28
9.5
3.05
1.38
806.8
113.0
51.2
1.0
0.15
0.07
Outlet
0.46
0.20
0.09
9.5
1.34
0.61
45.7
3.66
1.66
57.1
18.29
8.29
623.7
87.3
39.6
4.7
0.70
0.32
0.66
0.28
0.13
Run 3
Inlet
23.5
1.73
0.79
49.6
6.42
2.91
1.5
0.21
0.10
Outlet
0.49
0.21
0.09
2.30
0.92
0.42
12.5
1.62
0.74
18.1
1.34
0.61
60.1
17.77
8.06
207.5
26.8
12.2
13.0
1.81
0.82
0.089
0.029
0.013
Run 4
Inlet
11.9
1.56
0.71
20.7
1.55
0.70
52.8
15.81
7.16
179.2
23.5
10.6
Outlet
2.00
0.81
0.37
17.6
2.31
1.05
22.2
1.66
0.75
46.5
13.94
6.32
225.4
29.5
13.4
11.4
1.60
0.72
6.5
2.55
1.16
1 Blank space indicates a "non-detect."
1-4
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TABLE 1-2. SUMMARY OF FTIR RESULTS FOR CONDENSER SAMPLES AT PLANT Aa
Condenser Samples
Toluene
Hexane
Ethylene
Methane
Sulfur Dioxide
Carbon Monoxide
Formaldehyde
3-Methylpentane
Isooctane
Butane
2-Methyl-l-pentene
Heptane
1-Pentene
2-Methyl-2-butene
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
lb/hr
kg/hr
ppm
Ib/hr
kg/hr
Run 3
Inlet
12.8
1.27
0.58
7.4
0.42
0.19
49.3
11.2
5.06
291.4
28.9
13.1
9.2
0.98
0.44
1.6
0.49
0.22
0.79
0.16
0.074
9.4
2.8
1.3
7.3
1.84
0.83
Outlet
0.28
0.090
0.041
2.5
0.78
0.35
11.0
1.10
0.50
8.3
0.47
0.21
51.5
11.7
5.30
307.0
30.5
13.8
4.1
0.44
0.20
0.11
0.034
0.016
3.5
1.0
0.47
1.8
0.46
0.21 .
Run 4
Inlet
8.9
3.1
1.4
19.5
2.08
0.94
10.1
0.62
0.28
45.1
11.0
4.97
311.3
33.1
15.0
4.1
0.46
0.21
0.42
0.14
0.062
0.17
0.08
0.03
4.1
1.3
0.60
4.3
1.6
0.73
3.1
0.83
0.37
3.3
0.88
0.40
Outlet
12.4
4.34
1.97
21.2
2.26
1.02
11.4
0.69
0.31
35.1
8.53
3.87
320.3
34.1
15.5
5.3
0.60
0.27
0.09
0.030
0.013
0.0281
0.0122
0.0055
4.4
0.97
0.44
9.9
3.2
1.4
1.2
0.47
0.21
0.52
0.14
0.06
2.0
0.53
0.24
1 Blank space indicates a "non-detect.'
1-5
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TABLE 1-3. SUMMARY OF HYDROCARBON EMISSIONS RESULTS
Test Data
Run No.
Date
1
19-Aug-98
2
20-Aug-98
3
20-Aug-98
Averageb
4
21-Aug-98
Baghouse Inlet
Gaseous Concentrations
THC Concentration, ppm (wet basis)
THC Concentration, ppmc" (wet basis)
THC Concentration, ppmc (dry basis)
Emissions Data
THC Emission Rate, Ib/hr
THC Emission Rate, kg/hr
66.7
199.8
243.4
9.7
4.4
54.0
162.0
206.5
9.7
4.4
27.0
81.0
105.6
4.5
2.0
49.2
147.6
185.2
8.0
3.6
60.1
180.3
222.0
10.1
4.6
Baghouse Outlet ( Stack)
Gaseous Concentrations
THC Concentration, ppm (wet basis)
THC Concentration, ppmc (wet basis)
THC Concentration, ppmc (dry basis)
Emissions Data
THC Emission Rate, Ib/hr
THC Emission Rate, kg/hr
47.4
142.2
173.2
6.9
3.1
47.7
143.1
182.4
8.6
3.9
25.4
76.2
99.3
4.2
1.9
40.2
120.5
151.7
6.6
3.0
38.1
114.3
140.8
6.4
2.9
a ppm is concentration measured as propane; ppmc = ppm as carbon.
b Results from Runs 1 -3 are averaged because these runs were conducted during production using reclaimed asphalt
pavement (RAP). Run 4 was conducted during production using non-RAP material.
1-6
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1.3 PROJECT PERSONNEL
The EPA test program was administered by the EMC. Some key project personnel are
listed in Table 1-4.
TABLE 1-4. PROJECT PERSONNEL
Organization and Title
Plant A Corporation
Environmental/ Safety
Plant A Corporation
Plant Manager/Supervisor
U. S. EPA, EMC
Work Assignment Manager
Work Assignment 4-24
Work Assignment 2-08
U. S. EPA
Minerals and Inorganic
Chemicals Group
MRI
Work Assignment Leader
Work Assignment
MRI
Work Assignment Leader
Work Assignment 4-24
Work Assignment 2-10
Task Leader
Work Assignment 2-08
MRI
Program manager
Work Assignment Leader
Work Assignment 2-08
Name
Phil Adams
George Reeves
Michael L. Toney
Mary Johnson
Scott Klamm
Thomas J. Geyer
John Hosenfeld
Phone Number
(919)291-5165
(919)779-9752
(919)541-5247
(919)541-5025
(816)753-7600
Ext 1228
(919)851-8181
Ext 3 120
(816)753-7600
Ext 1336
1-7
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2.0 PROCESS DESCRIPTION AND TEST LOCATIONS
2.1 PROCESS DESCRIPTION
A process description and process data were provided by EC/R Incorporated. The EC/R
description and data are attached to this report in Appendix E.
2.2 TEST LOCATIONS
Figures 2-1 and 2-2 are drawings of the baghouse inlet and outlet test locations. Samples
from both the baghouse outlet stack and the baghouse inlet were analyzed by FTER and THC
analyzers from the same trailer position.
2.2.1 Baghouse Inlet Duct
The inlet location was a circular duct with a diameter of 48 inches (in.). The testing was
conducted in the vertical segment of the duct immediately upstream of where it connects to the
baghouse. FTER and Method 25A testing was conducted in a 4-inch diameter test port that was
36 in. above the baghouse roof. This port was in a plane about 11 in. above the manual testing
ports and offset by 45 °.
2.2.2 Baghouse Outlet - Stack
The outlet location (stack) was a rectangular duct 49V4 in. wide and 33l/i in. deep. The
wide face of the duct faces toward the baghouse roof. Six 4-in. ports arrayed in a straight line
across the wide side of the duct were used for the manual testing. Another 4-in. port was
installed on the short side of the stack, 24 in. below the top to provide access for the FTIR and
Method 25A sample probe.
2.3 VOLUMETRIC FLOW
Table 2-1 summarizes the gas composition and flow data provided by PES. PES
provided volumetric flow rates, moisture content, gas molecular weight, etc. as part of their
manual testing; therefore, MRI did not conduct these tests.
2-1
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Flow From
Drum Dryer
36'
FTIR
Method 25A
Q Test Port
O
Manual Method
Test Ports
48"
28"
—i J_ Inlet Sampling
* Location
25"
Baghouse
Figure 2-1. Baghouse inlet.
DRAWING NOT TO SCALE
2-2
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49
t
24"
j
FTIR ^
Method 25A
Test Port
\ \ T331/2"
_f-\
r^
\
Manual Method
Test Ports
,
8
-
8"
t
Hand Rail
I
Stack
DRAWING NOT TO SCALE
Figure 2-2. Baghouse outlet (stack).
2-3
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TABLE 2-1. SOURCE GAS COMPOSITION AND FLOW SUMMARY AT PLANT A
Test Data3
Run No.
Date
1
19-Aug-98
2
20-Aug-98
3
20-Aug-98
4
21-Aug-98
Baghouse Outlet ( Stack)b
Oxygen, %
Carbon Dioxide, %
Moisture Content, %
Gas Stream Velocity, fps
Volumetric Flow Rate, dscfm
13.1
5.3
17.9
46
21,344
13.1
5.5
21.6
61
25,198
13.1
5.1
23.3
55
22,749
10.8
3.2
18.8
53
24,410
" Data in Table 2-1 were provided by Pacific Environmental Services (PES). Raw data are in Appendix A-3.
b Manual sampling was terminated at the inlet due to high paniculate loading, therefore no gas measurements were
made at the inlet. Inlet mass emissions for all Runs were calculated using the velocity and gas composition data
measured at the outlet (Section 3.2.6).
2-4
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3.0 RESULTS
3.1 TEST SCHEDULE
The test program at the Plant A facility was completed from August 19 to August 21,
1997. Table 3-1 summarizes the sampling schedule. A complete record of all Method 25A and
FTIR sampling is in Appendices A and B. The FTIR and Method 25A sampling was coordinated
with the manual sampling conducted by PES.
TABLE 3-1. PLANT A FTIR AND 25A TEST SCHEDULE51
Date/Run No.
8/19/97
Run 1
8/20/97
Run 2
8/20/97
Run 3
FTIR
INLET
Wet
834-844 (spike)
900-913
1026-1038
1116-1203
1243-1307
1354-1424
8 12-8 17 (spike)
834-906
950-1030
1126-1158
1549-1617
Dry
1431-1506
1733-1740
(spike)
OUTLET
Wet
754-8 13 (spike)
917-1021
1205-1241
1322-1347
1433-1438
747-800 (spike)
912-944
1036-1108
1205-1239
1341-1401
1513-1542
Dry
1405-1525
1625-1653
1705-1723
(spike)
THC (25A)
Inlet
927-957
1017-1024
1054-1413
1428-1501
840-1242
1307-1725
Outlet
900-1005
1010-1427
840-1242
1307-1656
1727-1743
3-1
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TABLE 3-1. (CONTINUED)
Date/Run No.
8/21/97
Run 4
FTIR
INLET
Wet
943-1015
Dry
8 17-834 (spike)
1106-1132
OUTLET
Wet
732
911-939
1138-1156
Dry
739-809 (spike)
1028-1059
THC (25 A)
Inlet
748-817
829-909
938-1158
Outlet
812-1158
a See Tables and plots in Appendices A and B for details of 25A and FTIR sampling times, respectively.
3.2 FIELD TEST PROBLEMS AND CHANGES
Several factors worth noting are discussed below in separate subsections.
3.2.1 High Particulate at the Inlet
A short time into the first test run, the design of the FTIR sample probe and filter was
found incapable of handling the high particulate loading at the inlet sampling location. The
manual testing at the inlet was stopped because of the high particulate loading at the inlet
location. Therefore, no manual gas data were collected by PES at the inlet. The MRI field crew
tried several filtering designs before finding a solution that worked over a reasonable period. An
additional Balston filter was installed at the probe inlet, offset 90° from the probe and 180° from
the gas stream flow. The plugging of the filters and the removal of the probe for redesign caused
the loss of all inlet THC data and some FTIR data for these periods. MRI took steps to reduce
the loss of inlet data during installation or replacement of the filter.
3.2.2 Method 25A Concentration Spikes
Several times during Run 1 and at the beginning of Run 2, both THC analyzers recorded
process spikes when the THC concentration exceeded the analyzers' scale. All of the 1-minute
averages that exceeded the scale are included in the run averages. Because the exact
concentration was unknown when the instrument scale was exceeded, the 1-minute averages that
include these spikes are biased low. Nevertheless, because the number of out-of-range spikes
was few and their durations brief, the run average should not be significantly affected. This was
3-2
-------
discovered during Run 2 and was corrected by recalibrating the analyzers to a higher (0 to
1,000 ppm) range.
3.2.3 Addition of a Fourth Test Run
The EPA decided during the field test to add a fourth run to provide measurements while
non-RAP material was being used in the process. Run 4 was performed on August 21.
3.2.4 Method 25A Calibration Checks
The low-level THC calibration error check on the outlet analyzer for Run 4 was
5.2 percent, which exceeds the Method 25A performance limit of less than 5 percent. The error
was discovered during MRI's data quality assurance check and was found in the calculation of
the difference between the predicted and actual response. The operator used the calibration gas
value instead of calculating the predicted response. This approach would have been correct if the
instrument zero and span were set to the exact calibration gas values during instrument
linearization, but they were not. The calibration errors were recalculated, and all except this one
were within the required 5 percent. The oversight in the calibration procedure was brought to the
attention of the operator. Since the error is 0.2 percent outside the performance limit, MRI
decided that the effect on these data is small, and the data are presented without correction.
3.2.5 Condenser Sampling
Some samples were passed through a moisture condenser before measurement with the
FTIR system. This was not mentioned in the Site Specific Test Plan (SSTP), but it was a useful
procedure for FTIR analysis because the sample gas contained a relatively high moisture content.
The use of the condenser was approved by the EPA observer at the test site. The condenser was
used for portions of Runs 3 and 4. Moisture removal was accomplished by passing the sample
gas through an impinger immersed in an ice bath just before the FTIR cell. Moisture removal
reduces spectral interference in some frequency regions and can improve the analysis of
compounds that can pass through the condenser. Analyte spiking was successfully performed
through the condenser. Uncertainty results in Section 3.6 show that the quantitation limits are
lower for compounds that can pass through a condenser.
3.2.6 Inlet Flow Determination
For all runs, the flow data collected at the stack were used to calculate the inlet mass
emission rates. Manual testing at the inlet was discontinued due to high paniculate loading, so
3-3
-------
only limited inlet flow information is available from the first test day. MRI monitored the
velocity pressure (AP) and temperature at the FTIR sampling point, but these data are not of
suitable quality for calculating the volumetric flow rate since they were not collected by the EPA
manual method. The use of the outlet flow data to calculate the inlet mass emission rate may
give inlet emission rates with a slightly high bias. The outlet flow rate could potentially be
higher than at the inlet because the ID fan was located at the base of the stack. This design also
can allow dilution air to be pulled into the system if any leaks exist between the inlet sample
location and the fan. The hydrocarbon results summarized in Table 1-3 show that the THC outlet
concentrations were lower in all of the test runs, which indicates the possibility that air in-
leakage across the baghouse occurred.
3.3 METHOD 25A RESULTS
Table 1-3 summarized the Method 25A THC results at both the baghouse inlet and outlet.
The emission data are presented in parts per million as carbon (ppmc), pounds per hour as
carbon (Ib/hr), and kilograms per hour (kg/hr).
The THC emissions for all four runs show high concentration spikes throughout the test
periods. The results for Runs 1 and 2 were very similar in the number and duration of the high-
concentration spikes. In Run 3 fewer high-concentration THC spikes were seen, apparently
because of a burner adjustment, and the Run 3 average THC concentration was half that of
Runs 1 and 2 . Run 4, the non-RAP run, displays the highest average emission rate at the inlet.
The Run 4 results show fewer spikes, but these are of longer duration than in the previous three
runs.
Graphical presentations of outlet results from Runs 2, 3, and 4 are shown in Figure 3-1.
The inset in the Run 3 graph shows the 1400-1500 period on an expanded scale. The expanded
view shows that the Run 3 variations are qualitatively similar to the variations in Run 2 but
smaller in magnitude.
Table 3-2 shows the minimum, maximum, and average THC concentrations for each run.
The 1-minute average THC concentrations range from as low as 50.4 ppmc, during Run 3, to as
high as 639.9 ppmc, during Run 2. This does not mean that the highest spike was 639.9 ppmc
but that the highest 1-minute average was 639.9 ppmc, excluding the first test run because the
3-4
-------
instrument range was set too low to measure the process spikes. THC emission trends similar to
Runs 1, 2, and 3 are what would normally be found at this type of facility.
The complete Method 25A results are included in Appendix A. The concentrations
presented were measured by MRI. The mass emissions data, presented in Section 1.2, were
calculated using volumetric flow results provided by PES. The pre- and post-run calibrations and
QA checks met the Method 25A criteria in all cases except for Run 4 as discussed in Section 3.2.
Calibration QA results are included in Appendix A.
3-5
-------
era
I
O
o
O
o
o
f— t-
3
D.
era
T3
C/l
Concentration, ppn
>— to uj ji. U
08888
8:00
8:15
8:30
8:45
9:00
9:15
9:30
9:45
10:00
10:15
10:30
10:45
11:00
11:15
11:30
11:45
12:00
Concentration, ppn
i— K) u> ji <_/i
O O O O O
o o o o o o
Concentration, ppn
O
o
13:00
13:15
13:30
13:45
14:00
14:15
14:30
14:45
15:00
15:15
15:30
15:45
16:00
16:15
16:30
16:45
17:00
1 - 1
o
a
fir
000
o o o
-
00
o o
o
o
8:30
8:45
9:00
9:15
9:30
9:45
10:00
10:15
H 10:30
« 10:45
11:00
11:15
11:30
11:45
12:00
12:15
12:30
12:45
1 - 1 - 1
O
JO
e
-------
TABLE 3-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS'1
Run No.
Minimum
ppm
ppmc
Maximum
ppm
ppmc
Average
ppm
ppmc
Baghouse inlet
1
2
3
4
42.7
27.4
17.9
31.3
128.1
82.2
53.7
93.9
100.0
213.1
83.2
129.0
300.0b
639.3
249.6
387
66.7
54.9
27.0
60.1
199.8
162.0
81.0
180.3
Baghouse stack
1
2
3
4
25.2
24.0
16.8
20.1
75.6
72
50.4
60.3
100.0
197.4
64.0
94.0
300.0b
592.2
192
282
47.4
47.7
25.4
38.1
142.2
143.1
76.2
114.3
" ppm is the concentration as propane; ppmc = ppm as carbon
b Maximum concentration off scale
3.4 FTIR RESULTS
The two locations were sampled sequentially with the FTIR system. Wet and dry samples
were also measured sequentially. Sampling times are shown in Tables B-l through B-4, and in
the accompanying graphs in Appendix B.
A summary of the FTIR results was presented in Tables 1-1 and 1-2. Complete FTIR
results at the inlet and outlet are presented in Tables B-l to B-4 in Appendix B. The infrared
spectra showed evidence of water vapor, carbon dioxide (CO2), CO, methane, formaldehyde,
sulfur dioxide (SO2), toluene, ethylene, and a mixture of aliphatic (non-aromatic) hydrocarbons.
The FTIR spectra showed evidence that the emissions included a mixture of aliphatic
hydrocarbon compounds. The only HAP's in that classification are 2,2,4-trimethylpentane
(isooctane) and hexane. Therefore, the hydrocarbon emissions were primarily represented by
"hexane" in the draft report results. Since the draft report was submitted, MRI has measured
reference spectra of some additional hydrocarbon compounds. The new reference spectra were
included in the revised analysis to obtain a better representation of the hydrocarbon emissions.
3-7
-------
A description of the analytical procedures used to prepare the FTIR results is given in
Section 4.4. The mass emission rates were calculated using flow data provided by PES. Mass
emission calculations for toluene include the results from samples that were not spiked from the
toluene cylinder standard.
Some samples in Runs 3 and 4 were measured on a cold/dry basis by passing the gas
through a condenser before the FTIR cell. The condenser was used to remove moisture, which
was typically above 20 percent by volume. Which compounds can pass through the condenser
and be measured in the "dry" samples depends primarily on the vapor pressure and solubility of
the compounds in the sample. Analyte spiking was performed through the condenser using the
toluene calibration standard. The spike results showed that measurements of toluene (and
presumably compounds with similar chemical and physical properties) were unaffected by the
condenser. This was consistent with results from an EPA Method 301 validation test at a coal-
fired boiler.4
Because moisture is removed from the samples and because the calculated uncertainties
depend on the residual noise in the spectra, the calculated uncertainties for non-detects are much
lower in the dried samples. However, this is significant only for compounds that can pass
through the condenser.
3.5 ANALYTE SPIKE RESULTS
A toluene gas standard was used for analyte spiking experiments for quality assurance
only. Preferably, a spike standard combines the analyte and the tracer gas in the same cylinder,
but the SF6 and toluene were contained in two separate cylinders. Therefore, the two components
(SF6 and toluene) were quantitatively mixed (in equal proportions) before being introduced into
the sample gas stream.
The analyte spike results are presented in Tables 3-3 to 3-6. Samples were spiked with a
measured flow of toluene vapor during each run and at each location and through the condenser
in runs during which the condenser was used. The SF6 tracer gas spike was used to determine the
spike dilution factor. A description of the spike procedure is given in Section 4.3.1.
In general, the calculated spike recoveries were greater than 130 percent, which is above
the range specified by Method 301 for a validation correction factor (between 70 and
130 percent). However, for reasons discussed below, this does not reflect on the accuracy of the
3-8
-------
emissions results in Tables B-l to B-4. The residual spectra do not show significant
absorbances, indicating that the computer program did not over- or under-subtract analyte
reference spectra.
One factor contributing to the (calculated) high spike recoveries relates to the use of the
toluene library reference spectra. The toluene spike recoveries and all of the toluene results were
obtained using reference spectra in the EPA library. Spectra of the toluene cylinder standard
used for spiking were recorded on site during the test. If these spectra are used in the analysis,
one obtains results about 40 percent lower (far right column in Tables 3-3 to 3-5) than those
obtained using the library reference spectra.
Table 3-7 presents measured band areas of the EPA toluene reference spectra (deresolved
to 2 cm"1) and the spectrum of the toluene cylinder standard measured at the Plant A test site.
The comparison of the band areas does not agree with the comparison of the concentrations
(corrected for path length and temperature). The comparisons differ by nearly 40 percent. This
observed difference predicts that, if the spectra of the toluene cylinder standard are used in the
analysis rather than the EPA library spectra, then the result would give a toluene concentration
that is about 40 percent lower. This in fact happens when the computer program is modified to
include the cylinder standard spectra.
A similar disagreement was observed in other field tests using this toluene gas standard,
and one possibility is that the certified concentration of the toluene cylinder standard was
incorrect. However, this was a recently prepared cylinder with a quoted analytical accuracy of
± 2 percent. This possibility could be evaluated by purchasing several toluene gas standards
from different sources and doing a comparison similar to that shown in Table 3-7.
This observation about the toluene library spectra is compound specific, and the
information in Table 3-7 does not affect the results for other compounds detected. The
deresolved calibration transfer standard (CTS) (ethylene calibration) spectra give a path length
result (Section 4.4.1) that is consistent with the observed number of laser passes and the
instrument resolution. Additionally, this observation is not related to the deresolution of the
spectra because the band areas in the original 0.25 cm'1 toluene spectra are nearly equal to the
band areas in the deresolved 1 cm"1 versions of these spectra.
3-9
-------
A discrepancy of this type has the greatest effect on the difference, "spike - unspike,"
when the unspiked concentration is near zero. This is because two sets of reference spectra that
disagree will yield the same answer for a zero concentration but will yield different answers for
nonzero concentrations.
A similar disagreement between reference and standard spectra has been observed at least
once previously.5 In that study, which is included in Appendix D, HC1 was the analyte. The
spike recovery results were not significantly affected because there was a stable unspiked HC1
concentration and because both the spiked and unspiked HC1 concentrations were large
compared with the disagreement between the reference spectra and the spectra of the cylinder
standard.
3-10
-------
TABLE 3-3. SPIKE RESULTS IN WET SAMPLES COLLECTED AT THE BAGHOUSE INLET
Run
1
2
Average Toluene Concentration
Spike Unspike Tol (calc)"
24.1 0.0 24.1
17.4 0.0 17.4
39.8 0.0 39.8
Average SF6 Concentration
Spike Unspike SF6 (calc)a DFb
0.541 0.000 0.541 3.7
0.329 0.000 0.329 6.1
0.609 0.000 0.609 3.1
Cexpc Ad % Recovery
16.1 8.0 149.7
9.6 7.7 180.2
19.6 20.2 202.9
% Recovery
Tol Stan
92.1
110.8
124.8
Tol (calc) and SF6(calc) are equal to the difference between the spiked and unspiked concentrations for toluene and SF6, respectively.
bDF is the dilution factor in equation 4.
cCMp is shown in equation 5.
dA is equal to the difference, Tol(calc) - Cexp.
TABLE 3-4. SPIKE RESULTS IN WET SAMPLES AT THE BAGHOUSE OUTLET
Run
1
2
Average Toluene Concentration
Spike Unspike Tol (calc)a
21.2 0.0 21.2
17.3 0.0 17.3
17.1 0.1 17.0
Average SF6 Concentration
Spike Unspike SF6 (calc)a DFb
0.326 0.000 0.326 6.0
0.370 0.000 0.370 5.4
0.170 0.000 0.170 11.3
Cexpc Ad % Recovery
10.1 11.1 209.4
10.9 6.4 159.0
5.5 11.5 311.4
% Recovery
Tol Stan
128.8
97.8
191.5
Tol (calc) and SF6(calc) are equal to the difference between the spiked and unspiked concentrations for toluene and SF6, respectively.
bDF is the dilution factor in equation 4.
°Cejlp is shown in equation 5.
dA is equal to the difference, Tol(calc) - Cejlp.
-------
TABLE 3-5. SPIKE RESULTS IN CONDENSER SAMPLES AT THE BAGHOUSE INLET
Run
3
4
Average Toluene Concentration
Spike Unspike Tol (calc)11
18.0 0.0 18.0
17.1 5.1 12.0
Average SF6 Concentration
Spike Unspike SF6 (calc)a DFb
0.328 0.000 0.328 6.0
0.310 0.098 0.213 9.1
Cexpc Dd % Recovery
9.9 8.1 182.39
6.6 5.4 0.7
% Recovery
Tol Stan
112.1
111.1
Tol (calc) and SF6(calc) are equal to the difference between the spiked and unspiked concentrations for toluene and SF6, respectively.
bDF is the dilution factor in equation 4.
cCexp is shown in equation 5.
dA is equal to the difference, Tol(calc) - CCTp.
TABLE 3-6. SPIKE RESULTS IN CONDENSER SAMPLES AT THE BAGHOUSE OUTLET
Run
3
4
Average Toluene Concentration
Spike Unspike Tol (calc)a
3.3 0.3 3.0
33.3 11.7 1.6
Average SF6 Concentration
Spike Unspike SF6(calc)a DFb
0.607 0.000 0.607 3.2
0.589 0.018 0.572 3.4
Cexpc Dd % Recovery
18.5 14.5 7.18
18.0 3.6 120.2
% Recovery
Tol Stan
109.5
73.9
"Tol (calc) and SF6(calc) are equal to the difference between the spiked and unspiked concentrations for toluene and SF6, respectively.
bDF is the dilution factor in equation 4.
cCexp is shown in equation 5.
dA is equal to the difference, Tol(calc) - C .
-------
TABLE 3-7. COMPARISON OF EPA REFERENCE SPECTRA TO SPECTRUM OF TOLUENE CYLINDER STANDARD
Toluene Spectra
153a4ara(2cm~')
153a4arc(2crrf')
1530819a
Source
EPA library
EPA library
Plant A
Band Area
23.4
4.3
21.9
Frequency
Region (cm"1)
3160.8-2650.1
Spectra comparison
based on band areas
Ratio (Ra)
5.4
1.0
5.1
=l/Ra
0.184
1.000
0.196
Comparison of spectra based on
standard concentrations a
(ppm-m)/K
4.94
1.04
3.18
Ratio (Re)
4.8
1.0
3.1
= l/Rc
0.210
1.000
0.326
aThe comparison of the ratio based on concentrations to the ratio based on band area is equal to 61 percent.
-------
-------
4.0 TEST PROCEDURES
The procedures followed in this field test are described in EPA Method 320 for using
FTIR spectroscopy to measure HAP's, the EPA Protocol for extractive FTIR testing at industrial
point sources, and EPA Method 25A for measuring total gaseous organics. Objectives of the
field test were to use the FTIR method to measure emissions from the processes, screen for
HAP's in the EPA FTIR reference spectrum library, conduct analyte spiking for quality control
measurement, and analyze the spectra for compounds not in the EPA library. Another objective
was to monitor the process hydrocarbon emissions using Method 25A, Additionally, manual
measurements of gas temperature, gas velocities, moisture, CO2, and O2 by PES were used to
calculate the mass emissions rates.
The extractive sampling system shown in Figure 4-1 was used to transport sample gas
from the test ports to the FTIR instrument and the THC analyzers.
4.1 SAMPLING SYSTEM DESCRIPTION
4.1.1 Sample System Components
The sampling system consists of three separate components:
1. Two sample probe assemblies;
2. Two sample lines and pumps; and
3. A gas distribution manifold cart.
All wetted surfaces of the system are made of unreactive materials, Teflon®, stainless
steel, or glass and are maintained at temperatures at or above 300°F to prevent condensation.
The sample probe assembly consists of the sample probe, a pre-filter, a primary
particulate filter, and an electronically actuated spike valve. The sample probe is a standard
heated probe assembly with a pitot tube and thermocouple. The pre-filter is a threaded piece of
tubing loaded with glass wool attached to the end of sample probe. The primary filter is a
Balston particulate filter with a 99 percent removal efficience at 0.1 ^m. The actuated spike
valve is controlled by a radio transmitter connected to a switch on the sample manifold cart. All
sample probe assembly components are attached to or enclosed in an insulated metal box.
4-1
-------
This setup is for alternating (batch) sampling at
two locations.
Vent
Vent
1
Data Storage & Analysis FTIR Spectrometer Heated Cell
Vent #2
Vent#1
Total
Hydrocarbon
Analyzer
#2
Data Retrieval & Processing
Heated Probe #1
Heated Probe «
Sample Transfer Line (Heated Bundle) #1
Sample Transfer Line (Heated Bundle) #2
Calibration Standards
Figure 4-1. Sampling system schematic.
-------
The sample lines are standard heated sample lines with three % in. Teflon tubes in 10, 25,
50, and 100 foot (ft) lengths. The pumps are heated, single-headed diaphragm pumps
manufactured by either KNF Neuberger or Air Dimensions. These pumps can sample at rates up
to 20 liters per minute (Lpm) depending on the pressure drop created by the components installed
upstream.
The gas distribution manifold was specially constructed for FTIR sampling by MRI. It is
built onto a cart that can be operated inside the MRI mobile lab or in an alternate location, if
necessary. The manifold consists of a secondary paniculate filter, control valves, rotameters,
back pressure regulators and gauges, and a mass flow controller. The manifold can control two
sample gas stream inputs, eight calibration gases, and has three individual outputs for analyzers.
Alsoon the cart are a computer work station and controls for the spike valves and mass flow
controller.
4.1.2 Sample Gas Stream Flow
Exhaust gas was withdrawn at both the inlet duct and stack of the strand baghouse
through their respective sample probes and transported to the gas distribution manifold. Inside
the manifold the gas passed through separate secondary paniculate filters. Downstream of the
secondary filters, part of each sample gas stream was directed to separate THC analyzers; one to
measure the inlet concentration and another to measure the outlet concentration. Part of the
remaining sample gas from each stream was either sent to the FTIR instrument for analysis or
exhausted with the remaining portion of the gas stream being sampled (i.e., when the inlet
sample was analyzed the stack sample was exhausted and vice versa). This was accomplished by
rotating the gas selection valves to allow the appropriate sample gas to pass the instrument inlet
port. The gas flow to the instruments was regulated by needle valves on rotameters at the
manifold outlets.
The FTIR instrument was used to sample each location alternately, while the two THC
analyzers were used to sample both locations simultaneously
4.2 FTIR SAMPLING PROCEDURES
Figure 4-1 shows a schematic of the FTIR instrument and connections to the sample
distribution manifold.
4-3
-------
Sampling was conducted using either the batch or the continuous sampling procedures.
All data were collected according to Method 320 sampling procedures, which are described
below.
4.2.1 Batch Sampling
In this procedure, the valve on the manifold outlet was turned to divert part of the sample
flow to the FTIR cell. A positive flow to the main manifold outlet vent was maintained as the
cell was filled to just above ambient pressure. The cell inlet valve was then closed to isolate the
sample, the cell outlet valve was open to vent the cell to ambient pressure, the spectrum of the
static sample was recorded, and then the cell was evacuated for the next sample.
Batch sampling has the advantage that every sample is an independent sample. The time
resolution of the measurements is limited by the interval required to pressurize the cell and
record the spectrum. For this test the time resolution was 4 to 5 minutes. All of the spiked
samples were collected using this procedure.
4.2.2 Continuous Sampling
The cell was filled as in the batch sampling procedure, but the cell inlet and outlet valves
were then opened to keep gas continuously flowing through the cell. The inlet and outlet flows
were regulated to keep the sample at ambient pressure. The flow through the cell was maintained
at about 5 Lpm (about 0.7 cell volumes per min). The cell volume was about 7 liters (L).
The FTIR instrument was automated to record spectra of the flowing sample about every
2 minutes. The analytical program was revised after the field tests, and the spectra were analyzed
to prepare the results reported in Section 3.
This procedure with automated data collection was used for all of the unspiked testing
during Runs 2, 3, and 4. Because spectra were collected continuously as the sample flowed
through the cell, consecutive samples were mixed. The interval between independent
measurements (and the time resolution) depended on the sample flow rate (through the cell), and
the cell volume. The following explanation is taken from Performance Specification 15, for
continuous operation of FTIR systems: 'The Time Constant, TC, is the period for one cell
volume to flow through the cell. The TC determines the minimum interval for complete removal
of an analyte from the cell volume. It depends on the sampling rate (Rs in Lpm), the cell volume
(Vcd, in L) and the analyte's chemical and physical properties."
4-4
-------
v
^
=
Rs
Performance Specification 15 defines 5 * TC as the minimum interval between independent
samples. In this test 5 * TC was about 7 minutes.
A stainless steel tube ran from the cell inlet connection point to the front of the cell. The
outlet vent was at the back of the cell so that the flowing sample passed through the greatest
portion of the cell volume.
4.3 ANALYTE SPIKING
Because no information about possible HAP emissions or flue gas composition was
available for this source before the test, validating specific HAP's at this screening test was not
planned. MRI conducted spiking for QA purposes using a toluene (121 ppm in air) standard.
4.3.1 Analyte Spiking Procedures
The infrared spectrum is ideally suited for analyzing and evaluating spiked samples
because many compounds have distinct infrared spectra.
The reason for analyte spiking is to provide a quality control check that the sampling
system can transport the spiked analyte(s) to the instrument and that the quantitative analysis
program can measure the analyte in the sample gas matrix. If at least 12 (independent) spiked
and 12 (independent) unspiked samples are measured, this procedure can be used to perform a
Method 301 validation.3 No validation was done at this field test.
The spike procedure follows Sections 9.2 and 13 of EPA draft Method 320 in
Appendix D. In this procedure a gas standard is measured directly in the cell. This direct
measurement is then compared with measurements of the analyte in spiked samples. Ideally, the
spike comprises about 1/10 or less of the spiked sample. The actual dilution ratio depends on the
sample flow rate and the spike gas flow rate. The expected concentration (Cexp, the calculated
100 percent recovery) of the spiked component is determined using a tracer gas, SF6. The SF6
concentration in the direct sample divided by the SF6 concentration in the spiked sample(s) is
used as the spike dilution factor (DF). The analyte standard concentration divided by DF gives
the "expected" value (100 percent) of the spiked analyte recovery.
In this test the analyte (121 ppm toluene in air) and the tracer gas (4.01 ppm SF6 in
nitrogen) were in separate cylinders. Flows from the two gas standards were passed through
4-5
-------
separate mass flow meters and then combined into one flow directed up the spike line and
introduced into the sample stream at the back of the sampling probe. Because the two gasses
were mixed, the concentrations of each component were reduced in the combined spike gas flow.
This had to be accounted for in the calculation of the spike dilution factor, DF. For example the
SF6 concentration in the combined spike stream was
FSF6
toluene SF6
(2)
where:
SF6 (djrect) = the SF6 in the spike mixture. This is used in place of the cylinder
standard concentration.
FSF6 and Ftoluene = the measured flows from the toluene and SF6 cylinder standards.
SF6 (standard) = the concentration of the SF6 cylinder standard.
The toluene concentration in the combined spike flow is calculated in the same way.
F
toluene(direct) = «*™ * toluene(standard)
toluene SF6
The value, SF6(spike) is compared to the measured SF6 concentration in the spiked samples to
determine the spike dilution factor.
SF
DF = 6(direct) (A
SF
Or6(spike)
where DF is the spike dilution factor in Section 9.2.2 of Method 320 and SF6(direct) is calculated
using equation 2.
The calculated 100 percent recovery of the toluene spike is analogous to the expected
concentration in Section 9.2.2 of Method 320. In this case:
4-6
-------
toluene,,,.
C___ =
DP
where:
Cexp = the expected toluene concentration in the spiked samples (100 percent
recovery).
Toluene(direct) = from equation 3.
DF = from equation 4.
4.3.2 Analysis of Spiked Results
The toluene and SF6 concentrations used in the evaluation of the spike recoveries in
Tables 3-3 through 3-6 were taken directly from the sample analyses reported in Tables Bl
through B4. The concentrations in the spiked samples included a contribution from the spike gas
and from any analyte present in the flue gas. The component of the toluene concentration
attributed to the spike was determined by subtracting the average of the unspiked samples from
the measured concentration in each spiked sample (spike-unspike in Tables 3-3 through 3-6).
The percent recovery was determined by comparing the differences, spiked - unspiked, to the
calculated 100 percent recovery, Cexp in Section 4.3.1.
4.4 ANALYTICAL PROCEDURES
Analytical procedures in the EPA FTIR Protocol were followed for this test.2 A
computer program was prepared with reference spectra shown in Table 4-1. The computer
program used mathematical techniques based on a K-matrix analysis.6'7
Initially, the spectra were reviewed to determined appropriate input for the computer
program. Next an analysis was run on all of the sample spectra using all of the reference spectra
listed in Table 4-1. Finally, the undetected compounds were removed from the analysis, and the
spectra were analyzed again using reference spectra only for the detected compounds. Reference
spectra of 2-methyl-2-pentene, 3-methylpentane, butane, 2-methyl-l-pentene, n-heptane,
1-pentene, 2-methyl-2-butene, and n-pentane were included in the analysis to measure the
hydrocarbon mixture. These are the recently prepared hydrocarbon reference spectra described in
4-7
-------
Sections 1.2 and 3.4. The results from this second analytical run are summarized in Tables 1-1
and 1-2 and reported in Appendix B.
The same program that did the analysis calculated the residual spectra (the difference
between the observed and least squares fit absorbance values). Three residuals, one for each of
the three analytical regions, were calculated for each sample spectrum. All of the residuals were
stored electronically and are included with the electronic copy of the sample data provided with
this report. Finally the computer program calculated the standard l*sigma uncertainty for each
analytical result, but the reported uncertainties are equal to 4*sigma.
The concentrations were corrected for differences in absorption path length and
temperature between the reference and sample spectra using equation 2.
C
corr
T.
Cca.c (6)
where:
Ccorr = concentration, corrected for path length and temperature.
Ccalc = uncorrected sample concentration.
Lr = cell path length(s) (meters) used in recording the reference spectrum.
Ls = cell path length (meters) used in recording the sample spectra.
Ts = absolute temperature (Kelvin) of the sample gas when confined in the FTIR gas cell.
Tr = absolute temperature(s) (Kelvin) of gas cell used in recording the reference spectra.
The ambient pressure recorded over the three days of the test averaged about 746 mm Hg.
Because the sample pressure in the gas cell is equivalent to the ambient pressure, an addition
concentration correction factor of about 2 percent was included in the reported concentrations.
The sample path length was estimated by measuring the number of laser passes through
the infrared gas cell. These measurements were recorded in the data records. The actual sample
path length, L^ was calculated by comparing the sample CTS spectra to CTS (reference) spectra
in the EPA FTIR reference spectrum library. The reference CTS spectra, which were recorded
with the toluene reference spectra and are included in the EPA library, were used as input for a
K-matrix analysis of the CTS spectra collected at the Plant A field test. The calculated average
cell path length resulting from this analysis and the variation among the Plant A sample CTS
over the 3 days of testing are reported in Section 4.4.1.
4-8
-------
4.4.1 Computer Program Input
Table 4-1 presents a summary of the reference spectra input for the computer program
used to analyze the sample spectra. Table 4-2 summarizes the program input used to analyze the
CTS spectra recorded at the field test. The CTS spectra were analyzed as an independent
determination of the cell path length. To analyze the CTS spectra, MRI used 0.25 cm"1 spectra
"cts0814b" and "cts0814c." These reference CTS spectra were recorded on the same dates as the
toluene reference spectra used in the analysis. These spectra were deresolved in the same way as
the toluene reference spectra: by using Section K.2.2 of the EPA FTIR protocol. The program
analyzed the main two ethylene bands centered near 2,989 and 949 cm"1. Table 4-3 summarizes
the results of the CTS analysis. The cell path length from this analysis was used as L$ in
equation 2.
4.4.2 EPA Reference Spectra
The toluene spectra used in the MRI analysis were taken from the EPA reference
spectrum library (http://www.epa.gov/ttn/emc/ftir/welcome.html). The original sample and
background interferograms were truncated to the first 8,192 data points. The new interferograms
were then Fourier transformed using Norton-Beer medium apodization and no zero filling. The
transformation parameters were chosen to agree with those used to collect the sample absorbance
spectra. The new 2 cm"1 toluene single beam spectra were combined with their deresolved single
beam background spectra and converted to absorbance. This procedure was used to prepare
spectral standards for the HAP's and other compounds included in the analysis.
4.5 FTIR SYSTEM
A KVB/Analect Diamond 20 spectrometer was used to collect all of the data in this field
test. The gas cell is a heated variable path (D-22H) gas cell from Infrared Analysis, Inc. The
path length of the cell was set at 20 laser passes and measured to be about 9.5 meters using the
CTS reference and sample spectra. The interior cell walls have been treated with a Teflon®
coating to minimize potential analyte losses. A mercury/cadmium/telluride (MCT) liquid
nitrogen detector was used. The spectra were recorded at a nominal resolution of 2.0 cm" .
The optical path length was measured by shining a He/Ne laser through the cell and
adjusting the mirror tilt to obtain the desired number of laser spots on the field mirror. Each laser
spot indicates two laser passes through the cell. The number of passes was recorded on the field
4-9
-------
data sheets in Appendix B. The path length in meters was determined by comparing calibration
transfer standard (CTS, ethylene in nitrogen) spectra measured in the field to CTS spectra in the
EPA reference spectrum library. The procedure for determining the cell path length is described
in Section 4.4.
4.6 CONTINUOUS EMISSIONS MONITORING FOR TOTAL HYDROCARBONS (THC)
The guidelines set forth in Method 25A were followed during the sampling at Plant A
with two exceptions. Section 7.2 of Method 25A specifies an analyzer drift determination hourly
during the test period, this instruction was not followed. Also, Section 7.2 specifies that the mid-
level calibration gas is used for the drift determination. For this test program, the high-level
calibration gas was used for the drift determination.
There are two reasons the drift determination was not completed as specified. The first
reason is because of continuity in the FTIR and THC sampling. With run length exceeding four
hours, drift determination as specified would have involved off-line periods of up to 10 minutes
each hour for the THC analyzers and possibly for the FTIR instrument. The loss of this time
could affect the results if significant process events had occurred during these periods. The
second reason is that experience with the analyzers MRI was using show them to be stable over
extended periods when they are operated in a climate-controlled environment.
The need to do hourly drift determinations is somewhat diminished when the stability of
the analyzer is known and when the possibility that being off-line could affect the
representativeness of both the FTIR and THC results.
4.6.1 Total Hydrocarbon Sampling Procedures
The THC sampling was conducted continuously from both locations by using two
separate analyzers. The same sample systems used for the FTIR sampling were used for the THC
sampling. Sample gas was directed to the analyzers through a separate set of rotameters and
control valves. Each test run was conducted from the start to the end of the manual test runs
completed by PES. A summary of specific procedures used is given below.
A brief description of each system component follows.
1. THC Analyzer - The THC concentration is measured using a flame ionization detector
(FED). MRI used two J.U.M. Model VE-7 analyzers. The THC analyzers were operated on the
4-10
-------
zero to 100 ppm range during Run 1 and at the zero to 1,000 ppm range throughout the test
period. The fuel for the FID was a mixture of 40 percent hydrogen and 60 percent helium.
2. Data Acquisition System- MRI uses LABTECH notebook (Windows version), which
is an integrated system that provides data acquisition, monitoring and control. The system
normally writes data to a disk in the background while performing foreground tasks or displaying
data in real time. The averaging period set for this test was one minute.
3. Calibration Gases- Calibration gases were prepared from an EPA Protocol 1 cylinder
of propane (5278 ppm propane in nitrogen) using an Environics Model 2020 gas dilution system
that complies with the requirements of EPA Method 205. High, medium, and low standard gases
were generated to perform analyzer calibration checks. The raw data is recorded in ppm as
propane, but is converted to an as carbon basis for reporting.
4.6.2 Hydrocarbon Emission Calculations
The hydrocarbon data are presented as THC emissions in Table 1-3. To do this the THC
emission data were first converted to an as carbon basis using Equation 7, and then the THC
emission rate was calculated using Equation 8.
Cc=KCmeas (7)
where:
Cc = organic concentration as carbon, ppmv.
Cmeas = organic concentration as measured, ppmv.
K = carbon equivalent correction factor, 3 for propane.
Cc x MW x Q ,. x 60
(8)
_ ws
" 385.3 x 106
where:
ETHC = THC mass emission rate, Ib/hr.
MW = molecular weight of Carbon, 12 Ib/lb-mole.
Bws = moisture fraction in the flue gas stream.
Qstd = volumetric flow rate corrected to standard conditions, dscfm.
60 = conversion to hours, min/hr.
385.3 = molar volume, ft3/mole at standard conditions.
106 = conversion for decimal fraction to ppm
4-11
-------
TABLE 4-1. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA
Compound name
Water
Carbon monoxide
Sulfur dioxide
Carbon dioxide
Formaldehyde
Benzene
Methane
Methyl bromide
Toluene
Methyl chloride
Methyl chloroform
1 , 1 -dichloroe thane
1,3-butadiene
Carbon tetrachloride
Chlorobenzene
Cumene
Ethyl benzene
Hexane
Methylene chloride
Propionaldehyde
Styrene
1 , 1 ,2,2-tetrachloroe thane
p-Xylene
o-Xylene
m-Xylene
Isooctane
Ethylene
SF6
Ammonia
File name
I94clbvj
co20829a
198clbsc
193b4a_a
087b4anb
015a4ara
196clbsb
106a4asb
153a4arc
107a4asa
108a4asc
086b4asa
023a4asc
029a4ase
037a4arc
046a4asc
077a4arb
095a4asd
117a4asa
140b4anc
147a4asb
150b4asb
173a4asa
171a4asa
172a4arh
165a4asc
CTS0820b
Sf60819a
174a4ast
Region No.
1,2,3
1
2
1,2,3
3
3
3
2
3
3
2
2
2
2
2
3
3
3
2
3
2
2
2
3
2
3
2
2
2
ISC"
100"
167.1
89.5
415"
100.0
496.6
80.1
485.3
103.0
501.4
98.8
499.1
98.4
20.1
502.9
96.3
515.5
101.6
498.5
99.4
550.7
493.0
488.2
497.5
497.8
101.4
20.1
4.01
500.0
Reference
Meters
22
22
11.25
3
22
3
3
3
3
2.25
3
3
3
3
3
3
3
2.25
3
2.25
3
3
3
3
10.4
10.4
3
T (K)
394
394
373
298
394
298
298
298
298
373
298
298
298
298
298
298
298
373
298
373
298
298
298
298
394
394
298
Region No.
1
2
3
Upper cm'1
2,142.0
1,275.0
3,160.8
Lower cm1
2,035.6
789.3
2,650.1
1 Indicates an arbitrary concentration was used for the interferant.
4-12
-------
TABLE 4-2. PROGRAM INPUT FOR ANALYSIS AND CTS SPECTRA
AND PATH LENGTH DETERMINATION
Compound name
Ethylene a
Ethylene
File name
cts0814b.spc
cts0814c.spc
ASC
1.007
1.007
ISC
1.014
0.999
% Difference
0.7349
0.7350
aThis spectrum was used in the analysis of the Plant A CTS spectra
TABLE 4-3. RESULTS OF PATH LENGTH DETERMINATION
CTS spectra
100 ppm Ethylene
CTS0819A
CTS0819C
CTS0820A
CTS0820B
CTS0821A
CTS0821B
Average Path Length (M)
Standard Deviation
Path length calculations
Meters
10.82
10.39
10.42
10.58
10.71
10.66
10.60
0.166
Deltaa
0.22
-0.21
-0.17
-0.02
0.11
0.06
% Delta
2.1
-2.0
-1.6
-0.1
1.1
0.6
aThe difference between the calculated and average values.
4-13
-------
-------
5.0 SUMMARY OF QA/QC PROCEDURES
5.1 SAMPLING AND TEST CONDITIONS
Before the test, sample lines were checked for leaks and cleaned by purging with moist
air (250°F). Following this, the lines were checked for contamination using dry nitrogen. This is
done by heating the sampling lines to 250 °F and purging with dry nitrogen. The FTIR cell was
filled with some of the purging nitrogen, and the spectrum of this sample was collected. This
single beam spectrum was converted to absorbance using a spectral background of pure nitrogen
(99.9 percent) taken directly from a cylinder. The lines were checked again onsite before
sampling, after each change of location, and after spiking.
During sampling, spectra of at least 10 different samples were collected during each hour
(five at each of two locations).
Each spectrum was assigned a unique file name and written to the hard disk and a backup
disk under that file name. Each interferogram was also saved under a file name that identifies it
with its corresponding absorbance spectrum. All background spectra and calibration spectra
were also stored on disks with their corresponding interferograms.
Notes on each calibration and sample spectrum were recorded on hard copy data sheets.
Below are listed some sampling and instrument parameters that were documented in these
records.
Sampling Conditions
• Line temperature
• Process conditions
• Sample flow rate
• Ambient pressure
• Time of sample collection
Instrument Configuration
• Cell volume (for continuous measurements)
• Cell temperature
• Cell path length
• Instrument resolution
• Number of scans co-added
5-1
-------
• Length of time to measure spectrum
• Time spectrum was collected
• Time and conditions of recorded background spectrum
• Time and conditions of relevant CTS spectra
• Apodization
Hard copy records were also kept of all flue gas measurements, such as sample flow,
temperature, moisture, and diluent data.
Effluent was allowed to flow through the entire sampling system for at least 5 minutes
before a sampling run started or after changing to a different test location. FTTR spectra were
continuously monitored to ensure that there was no deviation in the spectral baseline greater than
±5 percent (-0.02
-------
identify the contents. The continuous data are in directories identified by the date on which the
spectra were recorded. The directory titles "BKG," "CTS," "outlet," and "inlet," identify
backgrounds, CTS spectra, and spectra of inlet and outlet samples, respectively. Additional sub-
directories "AIF' and "ASF" identify inferograms and absorbance spectra, respectively. All of
the sample data are in the Analect Instruments software format. The directories "refs" and
"residuals" contain de-resolved reference spectra that were used in the analyses and the residual
spectra, respectively. There are three residual spectra for each sample spectrum, one for each
analytical region. The information on the enclosed disk with the data records in Appendix A
meets the reporting requirements of the EPA FTIR Protocol and Method 320.
To measure HAP's detected in the gas stream MRI used spectra from the EPA library,
when available.
5.3 METHOD 25A
5.3.1 Initial Checks
Before starting the first run, the following system checks were performed.
1. Zero and Span check of the analyzer;
2. Analyzer linearity check at intermediate levels; and
3. Response time check of the system.
Calibration criteria for Method 25 A is ±5 percent of calibration gas value.
5.3.2 Daily Checks
The following checks were made for each test run.
1. Zero/Span calibration and Linearity checks before each test run; and
2. Final Zero and Span calibration check of the analyzer at the end of each test run.
The difference between initial and final zero and span checks agreed within ±3 percent of
the instrument span.
5-3
-------
-------
6.0 REFERENCES
1. Test Method 320 (Draft) "Measurement of Vapor Phase Organic and Inorganic Emissions
by Extractive Fourier Transform Infrared (FTIR) Spectroscopy," 40 CFR Part 63,
Appendix A.
2. "Protocol For the Use of FTIR Spectrometry to Perform Extractive Emissions Testing at
Industrial Sources," Revised, EPA Contract No. 68-D2-0165, Work Assignment 3-12,
September 1996.
3. "Method 301 - Field Validation of Pollutant Measurement Methods from Various Waste
Media," 40 CFR Part 63, Appendix A.
4. Draft Report, "FTIR Method Validation at a Coal-Fired Boiler," EPA Contract
No. 68D20163, work assignment 2, July, 1993.
5. "Validation of EPA FTIR Method For Measuring HC1," T. J. Geyer and G. M. Plummer, Air
and Waste Management Association, Paper Number 97-MP74.05, 1997.
6. "An Examination of a Least Squares Fit FTIR Spectral Analysis Method," G. M. Plummer
and W. K. Reagen, Air and Waste Management Association, Paper Number 96-WA65.03,
1996.
7. "Computer-Assisted Quantitative Infrared Spectroscopy," Gregory L. McClure (ed.), ASTM
Special Publication 934 (ASTM), 1987.
8. Emission Factor Documentation for AP-42 Section 11.1, Hot Mix Asphalt Plants, U. S.
Environmental Protection Agency, Research Triangle Park, NC, Fifth Edition.
6-1
-------
-------
APPENDIX A
METHOD 25A AND VOLUMERTRIC FLOW DATA
-------
-------
A-l METHOD 25A RESULTS
A-l
-------
A-2
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
9:00
9:01
9:02
9:03
9:04
9:05
9:06
9:07
9:08
9:09
9:10
9:11
9:12
9:13
9:14
9:15
9:16
9:17
9:18
9:19
9:20
9:21
9:22
9:23
9:24
9:25
9:26
9:27
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
9:39
9:40
9:41
9:42
9:43
9:44
9:45
9:46
9:47
THC inlet (ppm)
THC Off Line
50.8
50.7
54.6
59.8
65.6
64.4
59.4
58.8
55.9
60.6
55.7
55.0
55.8
56.7
63.5
57.6
55.7
54.8
54.5
THC Inlet (ppmc)
THC Off Line
181.8
167.1
165
167.4
170.1
190.5
172.8
167.1
164.4
163.5
THC outlet (ppm)
35.5
33.8
32.7
31.8
31.5
31.3
32.6
31.7
30.3
30.8
31.0
30.4
30.2
30.2
29.6
28.3
28.6
28.3
27.9
28.2
28.2
28.2
27.9
28.2
28.2
30.6
29.3
29.3
28.4
28.3
28.3
30.9
31.5
29.0
29.4
28.1
27.5
30.1
30.1
27.6
26.3
26.8
26.8
31.1
28.3
27.4
27.2
27.2
THC Outlet (ppmc)
106.5
101.4
98.1
95.4
94.5
93.9
97.8
95.1
90.9
92.4
93
91.2
90.6
90.6
88.8
84.9
85.8
84.9
83.7
84.6
84.6
84.6
83.7
84.6
84.6
91.8
87.9
87.9
85.2
84.9
84.9
92.7
94.5
87
88.2
84.3
82.5
90.3
90.3
82.8
78.9
80.4
80.4
93.3
84.9
82.2
81.6
81.6
Run1, Page 1 of 8
A-3
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
9:48
9:49
9:50
9:51
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10:03
10:04
10:05
10:06
10:07
10:08
10:09
10:10
10:11
10:12
10:13
10:14
10:15
10:16
10:17
10:18
10:19
10:20
10:21
10:22
10:23
10:24
10:25
10:26
1 0:27
10:28
10:29
10:30
10:31
10:32
10:33
10:34
10:35
THC inlet (ppm)
56.9
56.6
55.7
55.3
54.8
52.9
51.0
50.6
51.6
52.7
THC Off Line
56.0
55.5
63.6
61.2
53.1
51.8
59.2
65.3
THC Off Line
THC Inlet (ppmc)
170.7
169.8
167.1
165.9
164.4
158.7
153
151.8
154.8
158.1
THC Off Line
168
166.5
190.8
183.6
159.3
155.4
177.6
195.9
THC Off Line
THC outlet (ppm)
29.0
29.2
28.9
29.1
29.0
28.4
28.1
28.0
29.3
31.4
29.1
28.5
27.9
31.1
32.2
28.9
28.3
27.2
THC Off Line
31.3
29.4
32.3
30.0
32.1
31.6
29.5
28.4
29.5
35.4
36.7
30.1
28.8
33.3
51.8
26.2
31.4
25.2
26.0
25.7
26.8
46.8
36.9
51.8
35.6
44.4
THC Outlet (ppmc)
87
87.6
86.7
87.3
87
85.2
84.3
84
87.9
94.2
87.3
85.5
83.7
93.3
96.6
86.7
84.9
81.6
THC Off Line
93.9
88.2
96.9
90
96.3
94.8
88.5
85.2
88.5
106.2
110.1
90.3
86.4
99.9
155.4
78.6
94.2
75.6
78
77.1
80.4
140.4
110.7
155.4
106.8
133.2
Run1, Page 2 of 8
A-4
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
10:36
10:37
10:38
10:39
10:40
10:41
10:42
10:43
10:44
10:45
10:46
10:47
10:48
10:49
10:50
10:51
10:52
10:53
10:54
10:55
10:56
10:57
10:58
10:59
11:00
11:01
11:02
11:03
1 1 :04
11:05
11:06
11:07
11:08
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:16
11:17
11:18
11:19
11:20
11:21
11:22
11:23
THC inlet (ppm)
49.0
47.8
50.7
51.2
48.5
45.4
44.6
46.0
53.5
45.2
46.7
50.3
50.9
49.2
47.0
46.9
44.2
43.0
44.5
45.6
43.8
45.5
45.0
43.9
42.7
45.1
54.6
60.1
84.5
94.6
THC Inlet (ppmc)
147
143.4
152.1
153.6
145.5
136.2
133.8
138
160.5
135.6
140.1
150.9
152.7
147.6
141
140.7
132.6
129
133.5
136.8
131.4
136.5
135
131.7
128.1
135.3
163.8
180.3
253.5
283.8
THC outlet (ppm)
45.0
37.4
40.1
37.4
31.4
29.6
30.0
33.1
33.9
33.4
32.0
28.9
30.6
33.4
30.3
28.6
29.7
33.0
30.2
29.6
31.9
33.1
31.4
28.6
27.3
27.8
34.0
30.1
27.8
31.9
32.9
32.8
32.8
29.6
28.6
27.6
26.1
29.7
28.4
28.4
28.6
28.4
27.4
26.9
34.1
38.6
54.0
94.5
THC Outlet (ppmc)
135
112.2
120.3
112.2
94.2
88.8
90
99.3
101.7
100.2
96
86.7
91.8
100.2
90.9
85.8
89.1
99
90.6
88.8
95.7
99.3
94.2
85.8
81.9
83.4
102
90.3
83.4
95.7
98.7
98.4
98.4
88.8
85.8
82.8
78.3
89.1
85.2
85.2
85.8
85.2
82.2
80.7
102.3
115.8
162
283.5
Run1, Page 3 of 8
A-5
-------
Run 1
Date :8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
11:24
11:25
11:26
11:27
11:28
11:29
11:30
11:31
11:32
11:33
11:34
11:35
11:36
1 1 :37
11:38
11:39
11:40
11:41
11:42
11:43
11:44
11:45
11:46
11:47
11:48
11:49
11:50
11:51
11:52
11:53
11:54
11:55
11:56
11:57
11:58
11:59
12:00
12:01
12:02
12:03
12:04
12:05
12:06
12:07
12:08
12:09
12:10
12:11
THC inlet (ppm)
59.7
58.2
80.6
97.5
63.8
53.0
78.9
92.7
56.2
65.0
98.9
82.2
65.4
53.8
85.3
71.4
52.6
82.7
54.4
77.5
54.9
70.5
55.1
81.0
53.6
75.8
57.4
72.4
74.1
58.5
93.3
49.5
47.9
48.9
46.9
66.0
97.5
63.7
49.5
64.5
83.2
100.0A
69.2
49.5
71.3
83.2
48.5
84.6
THC Inlet {ppmc)
179.1
174.6
241.8
292.5
191.4
159
236.7
278.1
168.6
195
296.7
246.6
196.2
161.4
255.9
214.2
157.8
248.1
163.2
232.5
164.7
211.5
165.3
243
160.8
227.4
172.2
217.2
222.3
175.5
279.9
148.5
143.7
146.7
140.7
198
292.5
191.1
148.5
193.5
249.6
300
207.6
148.5
213.9
249.6
145.5
253.8
THC outlet (ppm)
57.8
41.2
46.8
94.3
64.8
40.5
45.4
79.3
56.5
38.0
72.8
86.3
57.2
36.5
54.8
71.3
39.5
56.1
51.9
57.1
42.7
58.9
38.0
58.6
47.7
45.1
59.1
40.4
71.6
39.9
76.5
53.3
32.3
34.1
32.2
34.0
79.5
74.5
35.0
41.8
62.7
99.2A
70.3
36.9
44.0
87.2
36.7
56.0
THC Outlet (ppmc)
173.4
123.6
140.4
282.9
194.4
121.5
136.2
237.9
169.5
114
218.4
258.9
171.6
109.5
164.4
213.9
118.5
168.3
155.7
171.3
128.1
176.7
114
175.8
143.1
135.3
177.3
121.2
214.8
119.7
229.5
159.9
96.9
102.3
96.6
102
238.5
223.5
105
125.4
188.1
297.6
210.9
110.7
132
261.6
110.1
168
Run1, Page 4 of 8
A-6
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
12:12
12:13
12:14
12:15
.12:16
12:17
12:18
12:19
12:20
12:21
12:22
12:23
12:24
12:25
12:26
12:27
12:28
12:29
12:30
12:31
12:32
12:33
12:34
12:35
12:36
12:37
12:38
12:39
12:40
12:41
12:42
12:43
12:44
12:45
12:46
12:47
12:48
12:49
12:50
12:51
12:52
12:53
12:54
12:55
12:56
12:57
12:58
12:59
THC inlet (ppm)
62.5
86.7
56.0
95.5
56.5
85.5
74.8
84.4
69.0
78.6
57.4
99.7A
64.4
65.6
98.0
100.0A
93.6
52.8
50.6
57.6
95.2
99.3A
56.7
53.1
78.2
51.0
71.7
91.5
95.4
63.2
48.2
50.3
91.3
99.9*
97.6
71.2
91.2
61.8
88.5
53.8
72.1
86.4
47.6
45.2
53.5
76.1
84.4
55.3
THC Inlet (ppmc)
187.5
260.1
168
286.5
169.5
256.5
224.4
253.2
207
235.8
172.2
299.1
193.2
196.8
294
300
280.8
158.4
151.8
172.8
285.6
297.9
170.1
159.3
234.6
153
215.1
274.5
286.2
189.6
144.6
150.9
273.9
299.7
292.8
213.6
273.6
185.4
265.5
161.4
216.3
259.2
142.8
135.6
160.5
228.3
253.2
165.9
THC outlet (ppm)
61.3
68.6
51.5
80.8
51.0
68.8
63.6
83.8
47.3
81.6
38.9
90.3
64.7
43.7
89.6
100.0A
91.7
45.0
35.2
40.0
80.5
100.0A
56.5
37.0
66.5
41.6
47.3
74.5
96.9
57.1
34.7
33.4
62.0
91.4
95.2
75.4
79.9
60.0
81.2
50.4
44.2
84.8
45.1
31.4
34.7
47.3
98.7
44.7
THC Outlet (ppmc)
183.9
205.8
154.5
242.4
153
206.4
190.8
251.4
141.9
244.8
116.7
270.9
194.1
131.1
268.8
300
275.1
135
105.6
120
241.5
300
169.5
111
199.5
124.8
141.9
223.5
290.7
171^3
104.1
100.2
186
274.2
285.6
226.2
239.7
180
243.6
151.2
132.6
254.4
135.3
94.2
104.1
141.9
296.1
134.1
Run1, Page 5 of 8
A-7
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
13:00
13:01
13:02
13:03
13:04
13:05
13:06
13:07
13:08
13:09
13:10
13:11
13:12
13:13
13:14
13:15
13:16
13:17
13:18
13:19
13:20
13:21
13:22
13:23
13:24
13:25
13:26
13:27
13:28
13:29
13:30
13:31
13:32
13:33
13:34
13:35
13:36
13:37
13:38
13:39
13:40
13:41
13:42
13:43
13:44
13:45
13:46
13:47
THC inlet (ppm)
86.7
72.2
57.9
100.0A
100.0A
97.5
62.6
57.5
85.6
86.2
52.8
89.8
61.8
70.5
72.5
56.5
47.6
49.7
62.0
78.9
80.7
82.1
84.7
63.9
53.1
63.0
65.8
96.0
99.9A
69.7
52.3
75.4
95.0
60.2
53.4
80.5
98.3
78.6
52.1
77.2
97.9
72.1
59.5
51.4
49.2
53.0
85.7
77.8
THC Inlet (ppmc)
260.1
216.6
173.7
300
300
292.5
187.8
172.5
256.8
258.6
158.4
269.4
185.4
211.5
217.5
169.5
142.8
149.1
186
236.7
242.1
246.3
254.1
191.7
159.3
189
197.4
288
299.7
209.1
156.9
226.2
285
180.6
160.2
241.5
294.9
235.8
156.3
231.6
293.7
216.3
178.5
154.2
147.6
159
257.1
233.4
THC outlet (ppm)
61.8
79.6
39.1
78.2
92.0
93.9
69.6
37.2
60.7
91.7
47.3
63.4
75.9
41.8
77.9
44.5
38.5
34.2
42.2
64.2
66.8
67.2
90.8
63.9
39.1
45.9
51.4
80.9
100.0A
70.0
39.7
51.7
90.9
52.9
39.6
56.1
83.6
75.1
40.2
53.0
88.5
66.8
45.8
40.5
33.5
38.3
64.3
82.6
THC Outlet (ppmc)
185.4
238.8
117.3
234.6
276
281.7
208.8
111.6
182.1
275.1
141.9
190.2
227.7
125.4
233.7
133.5
115.5
102.6
126.6
192.6
200.4
201.6
272.4
191.7
117.3
137.7
154.2
242.7
300
210
119.1
155.1
272.7
158.7
118.8
168.3
250.8
225.3
120.6
159
265.5
200.4
137.4
121.5
100.5
114.9
192.9
247.8
Run1, Page 6 of 8
A-8
-------
Run 1
Date: 8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
13:48
13:49
13:50
13:51
13:52
13:53
13:54
13:55
13:56
13:57
13:58
13:59
14:00
14:01
14:02
14:03
14:04
14:05
14:06
14:07
14:08
14:09
14:10
14:11
14:12
14:13
14:14
14:15
14:16
14:17
14:18
14:19
14:20
14:21
14:22
14:23
14:24
14:25
14:26
14:27
14:28
14:29
14:30
14:31
14:32
14:33
14:34
14:35
THC inlet (ppm)
48.1
77.0
84.0
63.3
51.4
72.1
96.5
62.3
46.3
63.0
89.4
78.9
57.9
54.1
52.9
49.8
74.8
88.9
65.4
48.7
64.0
86.7
52.7
82.3
83.7
88.6
Inlet Spike
67.7
53.7
87.6
82.0
65.7
59.2
59.2
58.6
THC Inlet (ppmc)
144.3
231
252
189.9
154.2
216.3
289.5
186.9
138.9
189
268.2
236.7
173.7
162.3
158.7
149.4
224.4
266.7
196.2
146.1
192
260.1
158.1
246.9
251.1
265.8
Inlet Spike
203.1
161.1
262.8
246
197.1
177.6
177.6
175.8
THC outlet (ppm)
35.3
48.9
79.8
55.3
39.8
44.2
93.9
65.4
38.1
35.7
73.6
74.8
49.1
41.7
39.4
36.3
47.1
87.6
60.0
40.3
42.1
85.0
52.1
48.8
88.9
47.6
69.2
85.6
39.8
50.0
76.6
74.7
50.9
42.2
64.6
72.5
60.7
39.0
55.6
87.5
Outlet Spike
THC Outlet (ppmc)
105.9
146.7
239.4
165.9
119.4
132.6
281.7
196.2
114.3
107.1
220.8
224.4
147.3
125.1
118.2
108.9
141.3
262.8
180
120.9
126.3
255
156.3
146.4
266.7
142.8
207.6
256.8
119.4
150
229.8
224.1
152.7
126.6
193.8
217.5
182.1
117
166.8
262.5
Outlet Spike
Run1, Page 7 of 8
A-9
-------
Run 1
Date :8/19/97
Project No: 3804-24-04-03/4701-08-01
Operator: Gulick
Time (24 hour)
14:36
14:37
14:38
14:39
14:40
14:41
14:42
14:43
14:44
14:45
14:46
14:47
14:48
14:49
14:50
14:51
14:52
14:53
14:54
14:55
14:56
14:57
14:58
14:59
15:00
15:01
Minimum=
Maximum=
Average=
THC inlet (ppm)
58.0
57.2
47.2
50.8
53.5
54.0
83.0
89.0
90.4
90.6
86.6
61.2
52.4
52.1
53.7
60.5
64.8
93.4
73.9
51.3
80.7
100.0A
95.6
57.4
79.0
100.0A
42.7
100.0
66.6
THC Inlet (ppmc) THC outlet (ppm) THC Outlet (ppmc)
174
171.6
141.6
152.4
160.5
162
249
267
271.2
271.8
259.8
183.6
157.2
156.3
161.1
181.5
194.4
280.2
221.7
153.9
242.1
300
286.8
172.2
237
300
128.1 25.2 75.6
300 100.0 300
199.8 47.4 142.2
A-10
Run1, Page 8 of 8
-------
Tl-V
Concentration, ppm
I 12:07
O
I
f
Concentration, ppm
c
9:00
9:17
9:34
9:51
10:08
10:25
10:42
10:59
11:16
to -t* ON oc o ho
3 O O O O O O
: J
-
11:33
H 11:5°
1 12:07
12:24
12:41
12:58
13:15
13:32
13:49
14:06
14:23
14:40
14:57
70
s
IS
3
*
H
ac
n
g;
S-
-------
A-12
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
8:40
8:41
8:42
8:43
8:44
8:45
8:46
8:47
8:48
8:49
8:50
8:51
8:52
8:53
8:54
8:55
8:56
8:57
8:58
8:59
9:00
9:01
9:02
9:03
9:04
9:05
9:06
9:07
9:08
9:09
9:10
9:11
9:12
9:13
9:14
9:15
9:16
9:17
9:18
9:19
9:20
9:21
9:22
9:23
9:24
9:25
9:26
9:27
THC inlet (ppm)
39.5
50.1
35.1
55.5
37.6
40.7
49.7
38.9
44.5
59.1
41.6
45.4
58.9
44.7
43.0
38.0
52.1
35.2
43.2
36.2
35.3
35.9
37.2
43.2
39.5
34.6
35.0
35.7
49.6
52.2
51.8
41.2
39.6
53.1
47.3
46.5
46.3
40.3
46.9
29.4
31.7
34.2
32.6
32.1
32.7
32.4
33.6
37.4
THC inlet (ppmc)
118.5
150.3
105.3
166.5
112.8
122.1
149.1
116.7
133.5
177.3
124.8
136.2
176.7
134.1
129.0
114.0
156.3
105.6
129.6
108.6
105.9
107.7
111.6
129.6
118.5
103.8
105.0
107.1
148.8
156.6
155.4
123.6
118.8
159.3
141.9
139.5
138.9
120.9
140.7
88.2
95.1
102.6
97.8
96.3
98.1
97.2
100.8
112.2
THC outlet (ppm)
28.8
40.3
27.6
38.0
35.0
28.5
40.2
32.1
30.9
45.8
35.5
33.0
45.6
37.3
35.2
30.3
41.7
29.2
32.8
30.2
28.3
28.0
29.1
30.3
35.5
28.5
27.1
28.3
32.7
42.8
40.6
36.1
30.2
40.2
37.9
36.7
36.2
33.2
36.7
25.8
24.0
26.9
26.4
25.3
25.7
25.5
26.2
28.9
THC outlet (ppmc)
86.4
120.9
82.8
114
105
85.5
120.6
96.3
92.7
137.4
106.5
99
136.8
111.9
105.6
90.9
125.1
87.6
98.4
90.6
84.9
84
87.3
90.9
106.5
85.5
81.3
84.9
98.1
128.4
121.8
108.3
90.6
120.6
113.7
110.1
108.6
99.6
110.1
77.4
72
80.7
79.2
75.9
77.1
76.5
78.6
86.7
Run2, Page 1 of 6
A-13
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
9:39
9:40
9:41
9:42
9:43
9:44
9:45
9:46
9:47
9:48
9:49
9:50
9:51
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10:03
10:04
10:05
10:06
10:07
10:08
10:09
10:10
10:11
10:12
10:13
10:14
10:15
THC inlet (ppm)
38.3
38.9
40.4
39.0
33.2
33.8
39.2
42.8
42.6
71.5
46.5
41.0
37.6
33.5
31.7
37.0
39.8
38.8
42.3
45.9
46.7
44.5
36.5
34.6
35.9
47.6
32.9
33.1
36.9
75.4
75.9
84.3
87.3
55.9
42.2
43.1
55.8
58.2
58.8
64.9
67.7
78.6
100.0A
100.0A
69.1
69.8
91.7
99.4A
THC inlet (ppmc)
114.9
116.7
121.2
117.0
99.6
101.4
117.6
128.4
127.8
214.5
139.5
123.0
112.8
100.5
95.1
111.0
119.4
116.4
126.9
137.7
140.1
133.5
109.5
103.8
107.7
142.8
98.7
99.3
110.7
226.2
227.7
252.9
261.9
167.7
126.6
129.3
167.4
174.6
176.4
194.7
203.1
235.8
300.0
300.0
207.3
209.4
275.1
298.2
THC outlet (ppm)
29.9
30.1
31.3
30.8
26.2
25.7
28.8
33.0
33.0
55.9
43.5
32.4
29.6
27.0
24.0
28.3
30.3
30.5
32.7
36.8
38.7
38.3
30.9
28.2
27.2
37.7
26.8
25.8
26.3
51.8
62.0
70.8
72.6
58.1
38.3
34.3
40.3
48.7
48.6
50.3
57.6
57.9
96.3
100.0A
82.1
50.7
72.9
90.8
THC outlet (ppmc)
89.7
90.3
93.9
92.4
78.6
77.1
86.4
99
99
167.7
130.5
97.2
88.8
81
72
84.9
90.9
91.5
98.1
110.4
116.1
114.9
92.7
84.6
81.6
113.1
80.4
77.4
78.9
155.4
186
212.4
217.8
174.3
114.9
102.9
120.9
146.1
145.8
150.9
172.8
173.7
288.9
300
246.3
152.1
218.7
272.4
Run2, Page 2 of 6
A-14
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
10:16
10:17
10:18
10:19
10:20
10:21
10:22
10:23
10:30
10:31
10:32
10:33
10:34
10:35
10:36
10:37
10:38
10:39
10:40
10:41
10:42
10:43
10:44
10:45
10:46
10:47
10:48
10:49
10:50
10:51
10:52
10:53
10:54
10:55
10:56
10:57
10:58
10:59
11:00
11:01
1 1 :02
11:03
1 1 :04
11:05
11:06
11:07
11:08
THC inlet (ppm)
100.0A
86.4
59.3
42.9
80.9
100.0A
92.4
49.5
Range Change
50.8
80.5
76.4
63.7
51.6
42.1
37.9
73.6
87.3
196.9
213.1
118.8
65.2
63.3
57.9
59.5
59.7
60.7
60.8
43.4
39.4
74.4
134.2
166.8
167.0
44.4
30.0
31.7
31.5
42.8
58.5
75.8
53.5
38.1
30.2
31.3
53.6
52.5
40.4
THC inlet (ppmc)
300.0
259.2
177.9
128.7
242.7
300.0
277.2
148.5
152.4
241.5
229.2
191.1
154.8
126.3
113.7
220.8
261.9
590.7
639.3
356.4
195.6
189.9
173.7
178.5
179.1
182.1
182.4
130.2
118.2
223.2
402.6
500.4
501.0
133.2
90.0
95.1
94.5
128.4
175.5
227.4
160.5
114.3
90.6
93.9
160.8
157.5
121.2
THC outlet (ppm)
100.0A
91.3
59.1
34.8
53.5
100.0A
83.5
50.8
43.9
63.6
77.7
60.0
49.9
41.5
34.5
60.9
76.6
168.9
197.4
130.9
62.3
58.9
53.8
54.7
54.4
57.0
56.5
43.0
36.6
59.0
117.5
151.1
157.4
59.7
27.4
28.9
28.9
36.1
52.6
69.0
52.6
37.7
28.0
28.1
47.1
49.1
38.8
THC outlet (ppmc)
300
273.9
177.3
104.4
160.5
300
250.5
152.4
131.7
190.8
233.1
180
149.7
124.5
103.5
182.7
229.8
506.7
592.2
392.7
186.9
176.7
161.4
164.1
163.2
171
169.5
129
109.8
177
352.5
453.3
472.2
179.1
82.2
86.7
86.7
108.3
157.8
207
157.8
113.1
84
84.3
141.3
147.3
116.4
Run2, Page 3 of 6
A-15
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:16
11:17
11:18
11:19
11:20
11:21
11:22
11:23
11:24
11:25
11:26
11:27
11:28
11:29
11:30
11:31
11:32
11:33
11:34
11:35
11:36
11:37
11:38
11:39
11:40
11:41
11:42
11:43
11:44
11:45
11:46
11:47
11:48
11:49
11:50
11:51
11:52
11:53
11:54
11:55
11:56
THC inlet (ppm)
38.5
33.4
43.1
45.2
39.8
36.4
34.5
35.7
36.5
36.8
38.0
56.2
117.3
186.7
183.4
160.7
101.8
75.1
52.7
40.0
34.6
35.5
35.3
57.3
65.7
63.0
51.5
36.1
37.5
36.7
71.2
80.1
54.1
50.8
51.7
51.2
40.6
42.3
119.3
119.0
89.5
49.8
42.1
43.9
40.3
33.9
49.1
54.1
THC inlet (ppmc)
115.5
100.2
129.3
135.6
119.4
109.2
103.5
107.1
109.5
110.4
114.0
168.6
351.9
560.1
550.2
482.1
305.4
225.3
158.1
120.0
103.8
106.5
105.9
171.9
197.1
189.0
154.5
108.3
112.5
110.1
213.6
240.3
162.3
152.4
155.1
153.6
121.8
126.9
357.9
357.0
268.5
149.4
126.3
131.7
120.9
101.7
147.3
162.3
THC outlet (ppm)
36.8
30.8
38.2
41.6
38.9
34.7
31.9
32.5
34.1
34.0
34.9
41.7
87.0
173.1
174.3
148.8
118.1
75.1
51.6
42.0
32.2
32.9
32.3
43.2
60.2
61.9
49.6
38.0
34.2
34.2
48.7
80.8
55.1
47.1
48.3
47.0
43.9
34.3
82.6
113.3
92.9
61.1
38.5
40.0
39.8
31.1
39.3
49.6
THC outlet (ppmc)
110.4
92.4
114.6
124.8
116.7
104.1
95.7
97.5
102.3
102
104.7
125.1
261
519.3
522.9
446.4
354.3
225.3
154.8
126
96.6
98.7
96.9
129.6
180.6
185.7
148.8
114
102.6
102.6
146.1
242.4
165.3
141.3
144.9
141
131.7
102.9
247.8
339.9
278.7
183.3
115.5
120
119.4
93.3
117.9
148.8
Run2, Page 4 of 6
A-16
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
11:57
11:58
11:59
12:00
12:01
12:02
12:03
12:04
12:05
12:06
12:07
12:08
12:09
12:10
12:11
12:12
12:13
12:14
12:15
12:16
12:17
12:18
12:19
12:20
12:21
12:22
12:23
12:24
12:25
12:26
12:27
12:28
12:29
12:30
12:31
12:32
12:33
12:34
12:35
12:36
12:37
12:38
12:39
12:40
12:41
12:42
Minimum*
THC inlet (ppm)
85.2
67.2
48.6
39.6
38.9
41.3
43.5
48.5
48.3
48.0
50.5
48.9
41.6
39.0
37.1
37.8
37.9
38.2
36.8
37.5
46.4
62.5
63.8
44.4
35.7
50.8
70.9
67.2
56.5
29.9
27.8
27.4
28.3
29.8
43.6
41.7
29.9
28.3
33.8
34.1
34.8
31.8
30.1
27.8
32.7
35.0
27.4
THC inlet (ppmc)
255.6
201.6
145.8
118.8
116.7
123.9
130.5
145.5
144.9
144.0
151.5
146.7
124.8
117.0
111.3
113.4
113.7
114.6
110.4
112.5
139.2
187.5
191.4
133.2
107.1
152.4
212.7
201.6
169.5
89.7
83.4
82.2
84.9
89.4
130.8
125.1
89.7
84.9
101.4
102.3
104.4
95.4
90.3
83.4
98.1
105.0
82.2
THC outlet (ppm)
67.2
72.2
50.2
37.1
36.5
35.9
40.0
43.8
45.1
43.2
45.9
45.9
38.2
36.0
34.0
34.3
34.5
34.1
33.4
33.9
38.4
57.0
58.0
44.1
32.7
41.4
64.1
61.7
55.0
29.1
25.5
24.7
25.3
26.5
34.5
42.9
27.5
25.9
29.5
31.0
31.7
29.3
27.4
24.8
28.3
32.1
24.0
THC outlet (ppmc)
201.6
216.6
150.6
111.3
109.5
107.7
120
131.4
135.3
129.6
137.7
137.7
114.6
108
102
102.9
103.5
102.3
100.2
101.7
115.2
171
174
132.3
98.1
124.2
192.3
185.1
165
87.3
76.5
74.1
75.9
79.5
103.5
128.7
82.5
77.7
88.5
93
95.1
87.9
82.2
74.4
84.9
96.3
72
Run2, Page 5 of 6
A-17
-------
Run 2
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
Maximum=
Average=
THC inlet (ppm)
213.1
54.0
THC inlet (ppmc)
639.3
162.0
THC outlet (ppm)
197.4
47.7
THC outlet (ppmc)
592.2
143.1
Run2, Page 6 of 6
A-18
-------
Inlet Run 2
a
Q.
O
I
O
U
225
OO Ox Ox
Time
*•>
o
5
o
Outlet Run 2
250
g; 200 -
150
100
50
0
O -^
o •— "
O •— "
o i— i
Time
-------
A-20
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
13:08
13:09
13:10
13:11
13:12
13:13
13:14
13:15
13:16
13:17
13:18
13:19
13:20
13:21
13:22
13:23
13:24
13:25
13:26
13:27
13:28
13:29
13:30
13:31
13:32
13:33
13:34
13:35
13:36
13:37
13:38
13:39
13:40
13:41
13:42
13:43
13:44
13:45
13:46
13:47
13:48
13:49
13:50
13:51
13:52
13:53
13:54
THC inlet (ppm)
29.9
31.5
49.1
26.7
27.2
25.4
30.1
32.5
26.2
26.1
24.7
23.6
25.0
26.2
35.5
29.7
29.3
38.8
27.3
29.8
30.5
27.4
25.9
27.4
32.3
37.8
31.3
26.4
27.5
28.4
28.9
28.5
26.8
26.6
25.6
25.9
26.7
30.1
29.7
24.2
24.8
25.0
26.6
30.4
27.7
24.7
24.3
26.8
THC inlet (ppmc)
89.7
94.5
147.3
80.1
81.6
76.2
90.3
97.5
78.6
78.3
74.1
70.8
75.0
78.6
106.5
89.1
87.9
116.4
81.9
89.4
91.5
82.2
111
82.2
96.9
113.4
93.9
79.2
82.5
85.2
86.7
85.5
80.4
79.8
76.8
77.7
80.1
90.3
89.1
72.6
74.4
75.0
79.8
91.2
83.1
74.1
72.9
80.4
THC outlet (ppmc)
21.9
28.8
43.5
29.2
24.8
23.8
24.1
33.0
24.7
25.2
24.3
23.0
23.4
24.3
31.3
29.2
25.7
35.7
25.3
26.6
28.1
26.1
23.7
24.9
28.3
33.6
30.0
24.7
24.7
25.8
26.2
26.3
25.0
24.4
23.8
23.6
24.1
26.8
27.8
22.4
22.7
23.1
23.4
27.5
25.7
23.0
22.1
24.3
THC outlet (ppm)
65.7
86.4
130.5
87.6
74.4
71.4
72.3
99
74.1
75.6
72.9
69
70.2
72.9
93.9
87.6
77.1
107.1
75.9
79.8
84.3
78.3
71.1
74.7
84.9
100.8
90
74.1
74.1
77.4
78.6
78.9
75
73.2
71.4
70.8
72.3
80.4
83.4
67.2
68.1
69.3
70.2
82.5
77.1
69
66.3
72.9
Run3, Page 1 of 6
A-21
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
13:55
13:56
13:57
13:58
13:59
14:00
14:01
14:02
14:03
14:04
14:05
14:06
14:07
14:08
14:09
14:10
14:11
14:12
14:13
14:14
14:15
14:16
14:17
14:18
14:19
14:20
14:21
14:22
14:23
14:24
14:25
14:26
14:27
14:28
14:29
14:30
14:31
14:32
14:33
14:34
14:35
14:36
14:37
14:38
14:39
14:40
14:41
14:42
THC inlet (ppm)
26.5
24.9
23.1
22.5
22.1
21.8
20.9
21.8
21.9
21.8
18.9
19.6
20.4
20.8
24.6
36.8
29.0
34.4
26.1
27.5
27.3
27.1
24.7
23.6
24.6
28.1
27.0
25.4
24.7
27.4
26.5
26.5
26.8
23.9
26.2
26.9
27.4
26.6
27.4
27.1
24.9
25.0
25.3
25.0
26.6
25.6
25.7
25.7
THC inlet (ppmc)
79.5
74.7
69.3
67.5
66.3
65.4
62.7
65.4
65.7
65.4
56.7
58.8
61.2
62.4
73.8
110.4
87.0
103.2
78.3
82.5
81.9
81.3
74.1
70.8
73.8
84.3
81.0
76.2
74.1
82.2
79.5
79.5
80.4
71.7
78.6
80.7
82.2
79.8
82.2
81.3
74.7
75.0
75.9
75.0
79.8
76.8
77.1
77.1
THC outlet (ppmc)
24.2
23.0
21.9
20.9
20.7
20.5
19.6
20.2
20.5
20.4
17.8
18.1
18.7
19.2
22.5
26.5
32.7
30.7
24.2
24.8
24.8
24.6
23.2
21.5
22.2
24.7
24.8
23.5
22.4
24.3
24.2
24.1
24.0
22.6
22.9
24.4
24.7
24.3
24.4
25.0
22.8
22.7
22.8
22.3
24.2
23.2
23.2
23.2
THC outlet (ppm)
72.6
69
65.7
62.7
62.1
61.5
58.8
60.6
61.5
61.2
53.4
54.3
56.1
57.6
67.5
79.5
98.1
92.1
72.6
74.4
74.4
73.8
69.6
64.5
66.6
74.1
74.4
70.5
67.2
72.9
72.6
72.3
72
67.8
68.7
73.2
74.1
72.9
73.2
75
68.4
68.1
68.4
66.9
72.6
69.6
69.6
69.6
Run3, Page 2 of 6
A-22
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
14:43
14:44
14:45
14:46
14:47
14:48
14:49
14:50
14:51
14:52
14:53
14:54
14:55
14:56
14:57
14:58
14:59
15:00
15:01
15:02
15:03
15:04
15:05
15:06
15:07
15:08
15:09
15:10
15:11
15:12
15:13
15:14
15:15
15:16
15:17
15:18
15:19
15:20
15:21
15:22
15:23
15:24
15:25
15:26
15:27
15:28
15:29
15:30
THC inlet (ppm)
25.8
24.8
27.6
26.3
25.6
25.5
25.9
26.3
25.1
26.0
24.0
23.4
23.9
23.9
27.1
37.2
32.8
28.5
28.8
31.7
32.4
28.5
26.3
28.2
26.4
25.2
23.2
23.9
27.1
28.6
29.6
25.1
23.3
22.1
24.9
25.0
21.7
17.9
22.8
21.0
19.7
22.7
23.3
24.5
27.3
24.6
22.7
21.9
THC inlet (ppmc)
77.4
74.4
82.8
78.9
76.8
76.5
77.7
78.9
75.3
78.0
72.0
70.2
71.7
71.7
81.3
111.6
98.4
85.5
86.4
95.1
97.2
85.5
78.9
84.6
79.2
75.6
69.6
71.7
81.3
85.8
88.8
75.3
69.9
66.3
74.7
75.0
65.1
53.7
68.4
63.0
59.1
68.1
69.9
73.5
81.9
73.8
68.1
65.7
THC outlet (ppmc)
23.3
22.7
24.6
24.2
23.2
23.1
23.4
24.2
23.6
23.9
23.4
21.7
22.2
22.3
23.3
32.6
30.3
26.2
26.0
26.1
30.8
26.1
24.2
24.9
24.1
23.0
21.4
21.3
23.7
25.2
26.7
23.4
22.0
20.4
22.2
22.9
20.5
16.8
19.6
20.0
17.7
20.8
21.5
22.3
25.1
23.5
21.3
20.3
THC outlet (ppm)
69.9
68.1
73.8
72.6
69.6
69.3
70.2
72.6
70.8
71.7
70.2
65.1
66.6
66.9
69.9
97.8
90.9
78.6
78
78.3
92.4
78.3
72.6
74.7
72.3
69
64.2
63.9
71.1
75.6
80.1
70.2
66
61.2
66.6
68.7
61.5
50.4
58.8
60
53.1
62.4
64.5
66.9
75.3
70.5
63.9
60.9
Run3, Page 3 of 6
A-23
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
15:31
15:32
15:33
15:34
15:35
15:36
15:37
15:38
15:39
15:40
15:41
15:42
15:43
15:44
15:45
15:46
15:47
15:48
15:49
15:50
15:51
15:52
15:53
15:54
15:55
15:56
15:57
15:58
15:59
16:00
16:01
16:02
16:03
16:04
16:05
16:06
16:07
16:08
16:09
16:10
16:11
16:12
16:13
16:14
16:15
16:16
16:17
16:18
THC inlet (ppm)
23.7
25.6
24.1
23.2
23.7
25.7
28.3
25.5
25.2
25.5
23.8
22.5
23.0
25.1
26.2
26.9
32.7
25.7
24.2
22.5
24.3
23.1
22.1
23.3
23.3
23.1
24.4
28.5
27.1
23.4
21.8
22.6
25.0
26.2
24.1
23.1
22.8
23.1
23.5
23.5
24.5
25.4
25.3
24.0
24.0
26.5
26.3
26.6
THC inlet (ppmc)
71.1
76.8
72.3
69.6
71.1
77.1
84.9
76.5
75.6
76.5
71.4
67.5
69.0
75.3
78.6
80.7
98.1
77.1
72.6
67.5
72.9
69.3
66.3
69.9
69.9
69.3
73.2
85.5
81.3
70.2
65.4
67.8
75.0
78.6
72.3
69.3
68.4
69.3
70.5
70.5
73.5
76.2
75.9
72.0
72.0
79.5
78.9
79.8
THC outlet (ppmc)
21.3
23.5
22.5
21.5
21.7
22.6
25.9
23.1
23.0
23.2
22.3
20.6
20.9
22.7
23.5
24.0
29.5
24.1
22.3
21.2
21.6
21.9
20.1
21.5
21.4
21.2
22.1
25.7
25.5
21.7
20.4
20.5
22.1
23.9
22.4
21.3
21.1
21.2
21.1
21.2
22.1
23.0
23.1
21.9
21.3
24.0
23.8
24.5
THC outlet (ppm)
63.9
70.5
67.5
64.5
65.1
67.8
111
69.3
69
69.6
66.9
61.8
62.7
68.1
70.5
72
88.5
72.3
66.9
63.6
64.8
65.7
60.3
64.5
64.2
63.6
66.3
77.1
76.5
65.1
61.2
61.5
66.3
71.7
67.2
63.9
63.3
63.6
63.3
63.6
66.3
69
69.3
65.7
63.9
72
71.4
73.5
A-24
Run3, Page 4 of 6
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
16:19
16:20
16:21
16:22
16:23
16:24
16:25
16:26
16:27
16:28
16:29
16:30
16:31
16:32
16:33
16:34
16:35
16:36
16:37
16:38
16:39
16:40
16:41
16:42
16:43
16:44
16:45
16:46
16:47
16:48
16:49
16:50
16:51
16:52
16:53
16:54
16:55
16:56
16:57
16:58
16:59
17:00
17:01
17:02
17:03
17:04
17:05
17:06
THC inlet (ppm)
25.1
23.0
26.5
30.9
24.9
31.2
25.4
33.0
23.6
24.5
25.9
25.7
23.5
24.0
23.8
24.9
27.0
23.5
26.9
22.0
24.0
25.2
25.3
25.2
25.5
25.5
25.8
25.2
23.4
22.4
24.3
24.2
24.3
23.2
22.8
26.3
31.6
26.8
25.2
24.3
23.0
23.3
24.0
24.6
24.0
24.5
22.8
23.7
THC inlet (ppmc)
75.3
69.0
79.5
92.7
74.7
93.6
76.2
99.0
70.8
73.5
111
77.1
70.5
72.0
71.4
74.7
81.0
70.5
80.7
66.0
72.0
75.6
75.9
75.6
76.5
76.5
77.4
75.6
70.2
67.2
72.9
72.6
72.9
69.6
68.4
78.9
94.8
80.4
75.6
72.9
69.0
69.9
72.0
73.8
72.0
73.5.
68.4
71.1
THC outlet (ppmc)
23.4
21.4
22.9
29.6
21.8
29.5
21.8
30.8
21.6
22.6
23.7
24.0
21.9
22.3
22.2
22.1
25.3
21.6
23.8
21.1
21.2
23.2
22.8
23.1
23.2
23.4
23.5
23.4
21.5
20.6
21.9
22.2
22.3
21.5
21,0
23.1
28.4
25.4
Outlet Spike
THC outlet (ppm)
70.2
64.2
68.7
88.8
65.4
88.5
65.4
92.4
64.8
67.8
71.1
72
65.7
66.9
66.6
66.3
75.9
64.8
71.4
63.3
63.6
69.6
68.4
69.3
69.6
70.2
70.5
70.2
64.5
61.8
65.7
66.6
66.9
64.5
63
69.3
85.2
76.2
A-25
Run3, Page 5 of 6
-------
Run 3
Date: 8/20/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
17:07
17:08
17:09
17:10
17:11
17:12
17:13
17:14
17:15
17:16
17:17
17:18
17:19
17:20
17:21
17:22
17:23
17:24
17:25
17:26
17:27
17:28
17:29
17:30
17:31
17:32
17:33
17:34
17:35
17:36
17:37
17:38
17:39
17:40
17:41
17:42
17:43
Maximum =
Maximum =
Average =
THC inlet (ppm)
24.0
24.6
29.6
49.7
29.9
47.8
30.4
50.9
31.7
49.4
32.6
49.0
34.6
44.1
32.1
37.0
53.9
39.2
83.2
Inlet Spike
17.9
83.2
27.0
THC inlet (ppmc)
72.0
73.8
88.8
149.1
89.7
143.4
91.2
152.7
95.1
148.2
97.8
147.0
103.8
132.3
96.3
111.0
161.7
117.6
249.6
53.7
249.6
81.0
THC outlet (ppmc)
56.7
31.1
55.5
35.2
45.2
43.2
46.8
45.8
38.9
57.5
38.1
64.0
42.0
62.5
38.9
59.6
52.3
16.8
64.0
25.4
THC outlet (ppm)
170.1
93.3
166.5
105.6
135.6
129.6
140.4
137.4
116.7
172.5
114.3
192
126
187.5
116.7
178.8
156.9
50.4
192
76.2
A-26
Run3, Page 6 of 6
-------
a
a.
r-
o
•e
Inlet Run 3
v
?
Time
>
-J
Outlet Run 3
-THC
outlet
(PPmc)
Time
-------
A-28
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
7:48
7:49
7:50
7:51
7:52
7:53
7:54
7:55
7:56
7:57
7:58
7:59
8:00
8:01
8:02
8:03
8:04
8:05
8:06
8:07
8:08
8:09
8:10
8:11
8:12
8:13
8:14
8:15
8:16
8:17
8:18
8:19
8:20
8:21
8:22
8:23
8:24
8:25
8:26
8:27
8:28
8:29
8:30
8.31
8:32
8:33
8:34
8:35
THC inlet (ppm)
62.8
63.3
65.2
65.3
65.4
65.7
65.6
65.9
64.9
65.5
66.5
67.7
67.0
65.8
65.4
74.7
81.0
80.5
83.4
89.5
81.9
89.5
89.9
86.1
80.6
67.6
51.2
45.2
42.1
40.2
Inlet Spike
85.0
85.5
84.8
84.8
84.4
83.8
82.5
THC inlet (ppmc)
188.4
189.9
195.6
195.9
196.2
197.1
196.8
197.7
194.7
196.5
199.5
203.1
201.0
197.4
196.2
224.1
243.0
241.5
250.2
268.5
245.7
268.5
269.7
258.3
241.8
202.8
153.6
135.6
126.3
120.6
255.0
256.5
254.4
254.4
253.2
251.4
247.5
THC outlet (ppmc)
Outlet Spike
54.7
49.6
36.9
32.6
29.8
28.4
27.4
26.5
25.5
25.3
26.8
30.1
32.7
35.0
34.6
36.5
36.9
35.1
34.7
34.3
34.9
34.6
34.4
32.9
THC outlet (ppm)
164.1
148.8
110.7
97.8
89.4
85.2
82.2
79.5
76.5
75.9
80.4
90.3
98.1
105
103.8
109.5
110.7
105.3
104.1
102.9
104.7
103.8
103.2
98.7
Run4, Page 1 of 6
A-29
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
8:36
8:37
8:38
8:39
8:40
8:41
8:42
8:43
8:44
8:45
8:46
8:47
8:48
8:49
8:50
8:51
8:52
8:53
8:54
8:55
8:56
8:57
8:58
8:59
9:00
9:01
9:02
9:03
9:04
9:05
9:06
9:07
9:08
9:09
9:10
9:11
9:12
9:13
9:14
9:15
9:16
9:17
9:18
9:19
9:20
9:21
9:22
9:23
THC inlet (ppm)
83.7
79.6
47.2
45.9
75.7
74.4
43.6
75.8
58.5
67.1
55.8
68.5
58.1
62.4
58.0
95.9
113.2
114.2
111.7
85.7
62.1
58.7
40.8
41.5
44.1
47.4
49.0
47.4
45.2
42.5
40.6
40.0
42.3
42.6
THC inlet (ppmc)
251.1
238.8
141.6
137.7
227.1
223.2
130.8
227.4
175.5
201.3
167.4
205.5
174.3
187.2
174.0
287.7
339.6
342.6
335.1
257.1
186.3
176.1
122.4
124.5
132.3
142.2
147.0
142.2
135.6
127.5
121.8
120.0
126.9
127.8
THC outlet (ppmc)
32.4
33.0
33.1
30.5
42.2
57.2
31.4
41.3
48.9
34.4
47.5
34.8
49.3
33.2
46.1
50.0
76.2
76.0
77.6
62.6
44.3
40.7
30.2
27.7
28.6
30.5
31.9
31.8
30.7
29.1
27.8
26.8
27.9
28.4
28.4
28.0
28.7
34.5
44.4
64.5
40.5
43.0
47.8
31.9
33.2
50.4
33.9
49.3
THC outlet (ppm)
97.2
99
99.3
91.5
126.6
171.6
94.2
123.9
146.7
103.2
142.5
104.4
147.9
99.6
138.3
150
228.6
228
232.8
187.8
132.9
122.1
90.6
83.1
85.8
91.5
95.7
95.4
92.1
87.3
83.4
80.4
83.7
85.2
85.2
84
86.1
103.5
133.2
193.5
121.5
129
143.4
95.7
99.6
151.2
101.7
147.9
Run4, Page 2 of 6
A-30
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
9:24
9:25
9:26
9:27
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
9:39
9:40
9:41
9:42
9:43
9:44
9:45
9:46
9:47
9:48
9:49
9:50
9:51
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10:03
10:04
10:05
10:06
10:07
10:08
10:09
10:10
10:11
THC inlet (ppm)
48.0
40.2
33.3
32.8
32.7
33.5
34.2
34.0
34.3
34.1
34.0
33.8
33.5
33.5
33.3
32.9
32.4
32.2
32.4
32.2
32.2
31.8
31.9
31.7
32.0
31.7
31.5
32.1
34.4
76.3
77.5
58.4
36.8
34.4
THC inlet (ppmc)
144.0
120.6
99.9
98.4
98.1
100.5
102.6
102.0
102.9
102.3
102.0
101.4
100.5
100.5
99.9
98.7
97.2
96.6
97.2
96.6
96.6
95.4
95.7
95.1
96.0
95.1
94.5
96.3
103.2
228.9
232.5
175.2
110.4
103.2
THC outlet (ppmc)
37.2
53.1
35.2
56.3
38.5
79.0
94.0
68.0
60.4
58.5
56.6
36.3
33.2
31.9
31.8
28.5
21.9
21.6
21.4
21.7
22.3
22.0
22.4
22.4
22.3
22.2
22.2
22.0
21.7
21.6
21.3
21.0
21.1
21.0
20.9
20.7
20.8
20.6
20.8
20.9
20.5
20.7
21.0
44.3
50.4
44.0
24.6
23.2
THC outlet (ppm)
111.6
159.3
105.6
168.9
115.5
237
282
204
181.2
175.5
169.8
108.9
99.6
95.7
95.4
85.5
65.7
64.8
64.2
65.1
66.9
66
67.2
67.2
66.9
66.6
66.6
66
65.1
64.8
63.9
63
63.3
63
62.7
62.1
62.4
61.8
62.4
62.7
61.5
62.1
63
132.9
151.2
132
73.8
69.6
Run4, Page 3 of 6
A-31
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
10:12
10:13
10:14
10:15
10:16
10:17
10:18
10:19
10:20
10:21
10:22
10:23
10:24
10:25
10:26
10:27
10:28
10:29
10:30
10:31
10:32
10:33
10:34
10:35
10:36
10:37
10:38
10:39
10:40
10:41
10:42
10:43
10:44
10:45
10:46
10:47
10:48
10:49
10:50
10:51
10:52
10:53
10:54
10:55
10:56
10:57
10:58
10:59
THC inlet (ppm)
31.9
31.4
31.3
31.4
32.4
33.8
33.4
33.8
33.8
33.4
33.7
33.8
34.4
34.3
56.9
64.2
62.6
63.5
129.0
115.1
98.8
90.5
86.2
82.8
80.9
81.2
81.4
80.8
82.3
83.2
84.4
86.6
89.9
88.3
91.1
94.2
92.4
90.2
81.1
53.4
60.4
50.1
60.6
45.2
46.6
46.1
71.1
98.7
THC inlet (ppmc)
95.7
94.2
93.9
94.2
97.2
101.4
100.2
101.4
101.4
100.2
101.1
101.4
103.2
102.9
170.7
192.6
187.8
190.5
387.0
345.3
296.4
271.5
258.6
248.4
242.7
243.6
244.2
242.4
246.9
249.6
253.2
259.8
269.7
264.9
273.3
282.6
277.2
270.6
243.3
160.2
181.2
150.3
181.8
135.6
139.8
138.3
213.3
296.1
THC outlet (ppmc)
21.0
20.6
20.6
20.4
20.8
21.6
21.7
21.9
22.0
21.7
21.7
21.7
22.4
22.3
32.0
41.7
40.9
41.1
72.7
81.6
66.4
60.3
57.2
54.4
53.0
52.8
52.6
52.5
53.2
53.8
54.2
56.0
57.7
57.5
58.1
60.9
60.4
58.6
56.1
37.6
32.4
38.4
34.5
32.9
29.3
29.5
34.2
72.8
THC outlet (ppm)
63
61.8
61.8
61.2
62.4
64.8
65.1
65.7
66
65.1
65.1
65.1
67.2
66.9
96
125.1
122.7
123.3
218.1
244.8
199.2
180.9
171.6
163.2
159
158.4
157.8
157.5
159.6
161.4
162.6
168
173.1
172.5
174.3
182.7
181.2
175.8
168.3
112.8
97.2
115.2
103.5
98.7
87.9
88.5
102.6
218.4
Run4, Page 4 of 6
A-32
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
11:01
11:02
11:03
11:04
11:05
1 1 :06
11:07
1 1 :08
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:16
11:17
11:18
11:19
11:20
11:21
11:22
11:23
11:24
11:25
11:26
11:27
11:28
11:29
11:30
11:31
11:32
11:33
11:34
11:35
11:36
11:37
11:38
11:39
11:40
11:41
11:42
11:43
11:44
11:45
11:46
11:47
THC inlet (ppm)
63.5
57.1
50.3
47.5
39.7
35.1
31.5
31.6
33.0
35.6
35.6
35.1
34.9
35.5
36.1
36.2
36.7
37.8
41.7
43.4
44.4
43.6
49.4
115.7
114.8
120.0
119.6
113.8
111.6
109.2
110.3
108.9
91.6
68.3
62.7
61.5
60.8
60.8
60.7
61.7
62.3
59.8
59.2
58.4
57.8
56.7
56.0
55.7
THC inlet (ppmc)
190.5
171.3
150.9
142.5
119.1
105.3
94.5
94.8
99.0
106.8
106.8
105.3
104.7
106.5
108.3
108.6
110.1
113.4
125.1
130.2
133.2
130.8
148.2
347.1
344.4
360.0
358.8
341.4
334.8
327.6
330.9
326.7
274.8
204.9
188.1
184.5
182.4
182.4
182.1
185.1
186.9
179.4
177.6
175.2
173.4
170.1
168.0
167.1
THC outlet (ppmc)
42.8
37.7
33.1
31.0
26.9
22.8
20.2
20.1
20.5
22.6
22.6
22.4
22.4
22.5
22.9
23.0
23.3
24.0
26.0
28.0
28.4
28.4
27.7
68.6
75.1
77.6
78.4
75.0
72.6
71.8
71.3
71.3
64.5
45.2
40.7
39.6
39.4
39.2
38.9
39.6
40.3
39.0
37.9
37.6
36.9
36.2
36.2
35.4
THC outlet (ppm)
128.4
113.1
99.3
93
80.7
68.4
60.6
60.3
61.5
67.8
67.8
67.2
67.2
67.5
68.7
69
69.9
72
78
84
85.2
85.2
83.1
205.8
225.3
232.8
235.2
225
217.8
215.4
213.9
213.9
193.5
135.6
122.1
118.8
118.2
117.6
116.7
118.8
120.9
117
113.7
112.8
110.7
108.6
108.6
106.2
Run4, Page 5 of 6
A-33
-------
Run 4
Date: 8/21/97
Project No.: 3804-24-04-03
Operator: Gulick
Time (24 hour)
11:48
11:49
11:50
1 1 .51
11:52
11:53
11:54
11:55
11:56
11:57
11:58
THG inlet (ppm)
56.1
56.9
45.0
43.9
69.4
42.1
48.7
78.3
77.6
62.5
45.9
THC inlet (ppmc)
168.3
170.7
135.0
131.7
208.2
126.3
146.1
234.9
232.8
187.5
137.7
THC outlet (ppmc)
35.9
36.2
31.6
25.7
44.5
28.8
29.7
45.9
53.3
42.9
30.9
THC outlet (ppm)
107.7
108.6
94.8
77.1
133.5
86.4
89.1
137.7
159.9
128.7
92.7
Minimum
Maximum
Average
31.3
129.0
60.1
93.9
387.0
180.3
20.1
94.0
38.1
60.3
282
114.3
A-34
Run4, Page 6 of 6
-------
Inlet Run 4
Time
Outlet Run 4
Q.
a
•v
o
*-c
s
1
o
u
THC outlet
(ppmc)
Time
-------
A-36
-------
A-2 METHOD 25A CALIBRATION AND QC CHECK DATA
A-37
-------
A-38
-------
8-19cal
Calibration Error Determination For 8/19/97
THC1
Inlet
THC2
Outlet
Pass Fail
CalGas
Value
0.0
90.4
50.4
35.2
0.0
90.4
50.4
35.2
Criteria is +/-
Predicted Measured
Value Value
0.2
91.0
50.8 49.9
35.6 34.3
0.7
91.5
51.3 50.1
36.1 34.5
5% of Calibration gas.
Difference as
% of CalGas
0.2
0.7
1.8
3.5
0.7
1.2
2.4
4.3
Calibration Drift Determination For 8/19/97
THC 1
Inlet
THC 2
Outlet
Initial
Value
0.2
0.7
Final
Value
0.2
0.0
Instrument Span for THC 1 and THC 2 is 1000
Pass Fail
THC 1
Inlet
THC 2
Outlet
Criteria is +/-
Initial
Value
91.0
91.5
3% of Span.
Final
Value
89.1
93.1
Zero Drift
Difference as
% of Span
0.0%
0.7%
ppm
Span Drift
Difference as
% of Span
1.9%
-1.6%
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and THC 2 is 1000 ppm
Pass Fail Criteria is +/- 3% of Span.
A-39
-------
8-20cal
Calibration Error Determination For 8/20/97 (Run 2)
THC 1
Inlet
THC 2
Outlet
Pass Fail
CalGas
Value
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is +/-
Predicted Measured
Value Value
-0.1
902.0
504.2 495.0
252.0 249.0
0.5
919.0
514.0 505.0
257.2 259.0
5% of Calibration gas.
Difference as
% of CalGas
0.0
0.4
1.8
1.2
0.1
2.3
1.7
0.7
Calibration Drift Determination For 8/20/97 (Run 2)
THC 1
Inlet
THC 2
Outlet
Initial
Value
-0.1
0.5
Final
Value
-1.5
-0.4
Instrument Span for THC 1 and THC 2 is 1000
Pass Fail
THC 1
Inlet
THC 2
Outlet
Criteria is +/-
Initial
Value
902.0
919.0
3% of Span.
Final
Value
906.0
917.0
Zero Drift
Difference as
% of Span
0.1%
0.1%
ppm
Span Drift
Difference as
% of Span
-0.4%
0.2%
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and THC 2 is 1000 ppm
Pass Fail Criteria is +/- 3% of Span.
A-40
-------
8-20cal (2)
Calibration Error Determination For 8/20/97 (Run 3)
THC 1
Inlet
THC 2
Outlet
Pass Fail
CalGas
Value
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is +/-
Predicted Measured
Value Value
-1.5
906.0
505.8 512.0
252.2 252.0
-0.4
917.0
512.4 497.0
256.0 258.0
5% of Calibration gas.
Difference as
% of Cal Gas
0.2
0.9
1.2
0.1
0.0
2.1
3.0
0.8
Calibration Drift Determination For 8/20/97 (Run 3)
THC 1
Inlet
THC 2
Outlet
Initial
Value
-1.5
-0.4
Final
Value
-1.3
0.2
Instrument Span for THC 1 and THC 2 is 1000
Pass Fail
THC 1
Inlet
THC 2
Outlet
Criteria is +/-
Initial
Value
906.0
917.0
3% of Span.
Final
Value
900.0
915.0
Zero Drift
Difference as
% of Span
0.0%
-0.1%
ppm
Span Drift
Difference as
% of Span
0.6%
0.2%
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and THC 2 is 1000 ppm
Pass Fail Criteria is +/- 3% of Span.
A-41
-------
THC 1
Inlet
THC 2
Outlet
Pass Fail
THC 1
Inlet
THC 2
Outlet
CalGas
Value
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is +/-
Initial
Value
0.3
0.5
Predicted Measured
Value Value
0.3
899.0
502.7 501.0
251.5 247.0
0.5
912.0
510.0 499.0
255.3 242.0
5% of Calibration gas.
Calibration Dr
Final
Value
1.4
1.0
8-2lcal
Calibration Error Determination For 8/21/97
Difference as
%ofCalGas
0.0
0.1
0.3
1.8
0.1
1.6
2.2
5.2
1.3
Zero Drift
Difference as
% of Span
-0.1%
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Fail
-0.1%
Pass/Fail
Pass
Pass
Instrument Span for THC I and THC 2 is 1000 ppm
Pass Fail Criteria is +/- 3% of Span.
Span Drift
THC 1
Inlet
THC 2
Outlet
Initial
Value
899.0
912.0
Final
Value
903.0
906.0
Difference as
% of Span
-0.4%
0.6%
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and THC 2 is 1000 ppm
Pass Fail Criteria is +/- 3% of Span.
A-42
-------
A-3 VOLUMETRIC FLOW DATA
A-43
-------
A-44
-------
APPENDIX A
METHOD 25A AND VOLUMERTRIC FLOW DATA
A-45
-------
A-46
-------
Y
AH
Pb.
vm
Tm
PftltiC
T,
V!e
C02
02
N2
CP
Ap"2
©
Dn
An
Vm(«d)
Vm(i«d)
P.
B.
BW«(»*)
V«M
1-B«
Md
M.
V.
A
Q.
Q.
Q«(cmtn)
I
Summary of Stack Gas Parameters and
US EPA Test Method 23 - PCDD /
Baghouse Inlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, °F
Stack Static Pressure, inches H2O
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pitot Tube Coefficient
Average Square Root Ap, (in. H2O)1/2
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w b.), lb/lb*mole
Stack Gas Velocity, ft/s
Stack Area, ftz
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
Test Results
PCDF
S-M23-I-1
8/19/97
0915-1010
1.021
1.93
29.90
11.116
90
-2.5
230
84.0
5.3
•13.1
81.6
0.84
0.5927
20
0.312
0.00053
10.940
0.310
29.72
26.5
141.2
3.954
0.735
29.37
26.35
39.9
12.57
30,119
16,819
476.3
77.0
A-47
-------
12 / 17 - 9',
12:08
SL9199410234
PES RTF NC
3)003/015
US EPA
y
AH
PMT
Vm
Tm
P,«ic
T.
Vic
C02
DZ
N2
Cp
Ap1'2
0
Dn
An
Vm(std) cf
Vrnf.*).™
Qm
P,
Bw.
BW«M|)
Vwiki
1-Bw,
Md
M,
V,
A
Q.
Q.cJm
Qjcfnm
I
Summary of Stack Gas Parameters and Test Results
EMC Asphalt Concrete Emissions Testing
US EPA Test Method 29 - Multiple Metals
Baghouse Inlet
Page 1 of 4
RUN NUUBER
RUN DATE
RUN TIME
MEASURED DATA
Meter Box Correction Factor
Avg Meter Omlce Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature. *F
Stack Static Pressure, inches H2O
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pltot Tube Coefficient
Average Square Root Ap, (in. h^O)1"2
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft3
Standard Meter Volume, ft3
Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b.), Ib/lbTnole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
S-M29-M
a/19/97
091S-1010
1 016
1.10
29.90
10.780
92
-2.5
230
78.8
5.3
13.1
81.6
0.84
0.4682
20
0.311
0.000527
10.491
0.297
0.525
29.72
26.1
141.2
3.709
0.739
29.37
26.40
31.5
12.57
23,773
13,353
378
93.6
A-48
-------
1^004/015
10 11 123
Section A
Traverse Point
Number
1
2
3
4
5
6
7
8
9
10
11
12
Distance from
Inside WaH, inches
1.02
3.25
5.72
8.58
12.1
17.3
31.2
36.4
39.9
42.8
45.3
47.5
Figure 3.2 Baghouse Inlet Traverse Point Locations,
Gamer, North Carolina
A-49
-------
: ua
199410234
KTP NC
Summary of Stack Gas Parameters and
US EPA EMC Asphalt Concrete Emissions Testing
US EPA Test Method 23 - PCDD /
Baghouse Outlet
Page 1 of 6
Y
AH
P*~
vm
Tm
PIUUC
T.
Vie
CO2
02
N2
CP
Ap1*
©
Dn
An
Vm(»td)
Vm
-------
u LD
y
AH
P^
vm
Tm
P..-IC
T,
Vlc
C02
02
N2
cp
.1/2
Ap
0
Dn
A,
Vm(,w)
Vm(,W)
P.
B«
BW«M»,
Vwrfd
1-BW.
Md
M,
V,
A
Q.
Q.
Q»(emm)
I
Summary of Stack Gas Parameters and
US EPA Test Method 23 - PCDD /
Baghouse Outlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft3
Average Meter Temperature, *F
Stack Static Pressure, inches H2O
Average Stack Temperature, °F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pitot Tube Coefficient
Average Square Root Ap, (in. HjO)"2
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, dscf
Standard Meter Volume, dscm
Stack Pressure, inches Hg
Moisture, % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft3
Dry Mole Fraction
Molecular Weight (d.b.), Ib/lb-mole
Molecular Weight (w.b .), Ib/lb-mole
Stack Gas Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfm
Stack Gas Volumetric flow, dscfm
Stack Gas Volumetric flow, dscmm
Isokinetic Sampling Ratio, %
Test Results
PCDF
S-M23-0-4
8/21/97
0741-1149
0.987
2.37
29.70
179.969
105
-0.25
180
819.1
3.2
10.8
86.0
0.84
0.8374
240
0.251
0.00034
165.621
4.690
29.68
18.9
51.1
38.555
0.811
28.94
26.88
53.8
11.46
37,027
24,580
696.0
93.7
A-51
-------
l«1007/0 15
Summary of Stick Gaa Parameters and Test Results
US EPA EMC Asphalt Concrete Emissions Testing
US EPA Teat Method 29 - Multiple Metals
Baghouae Outlet
Page 1 of 4
Y
AH
Pb.
vm
Tm
PsUUe
T,
vte
CO2
02
N2
CP
Ap1"
0
Dn
An
Vm(»W) e»
Vm(itd) cm
Qm
P,
Bw.
BWI
-------
®008/015
us
T
AH
PO.T
vm
Tm
P«udc
T,
V|e
CO2
O2
N2
Cp
Ap1/!
0
Dn
Ao
vm(rtd)
vm(iW,
Qn,
P.
BW,
(W.
Vw«d
1-B*
Md
M,
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A
Q.
Q.«.
Q.cm.
I
Summary of Stack Gaa Parameters and Teat Results
EPA EMC Asphalt Concrete Emissions Testing
US EPA Teat Method 29 • Multiple Mettle
Baghouae Outlet
Page 1 of 4
RUN NUMBER
RUN DATE
RUNTIME
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft*
Average Meter Temperature, *F
Stack Static Pressure, inches H2O
Average Stack Temperature, 'F
Condensate Collected, ml
Carbon Dioxide content, % by volume
Oxygen content, % by volume
Nitrogen content, % by volume
Pilot Tube Coefficient
Average Square Root Ap, (in. H2O)1/Z
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
c, Standard Meter Volume, ft*
m Standard Meter Volume, m3
Average Sampling Rate, dscfm
Stack Pressure, Inches Hg
Moisture, % by volume
„ Moisture (at saturation), % by volume
Standard Water Vapor Volume, fV
, Dry Mole Fraction
Molecular Weight (d.b.), lb/!b-mole
Molecular Weight (w.b.), Ib/to-mole
Stack Gaa Velocity, ft/s
Stack Area, ft2
Stack Gas Volumetric flow, acfrn
, Stack Gas Volumetric flow, dscfm
, Stack Gas Volumetric flow, dscmm
Isokinettc Sampling Ratio, %
S-M290-4
8K1/9T
0741-1153
0.965
2.00
29.70
186.221
102
-0.25
180
821.4
3.2
10.8
86.0
0.84
0.8239
240
0.253
0.000349
168.390
4.768
0.702
29.68
18.7
51.1
38.663
0.813
28.94
26.90
53.0
11.46
36,415
24,240
686
95.0
A-53
12/17/97
-------
12/17/97 12:10 S19L99410234
PES RIP \C
015
1
1
1
1
M
- -
1
2
2
2
:
2
2
.......
.......
2
3
3-
*~
3
3
3
3
4
'-.4
* 9 -
^ *r''?
-^«,
4
4
4
4
49
Section B
Traverse Point
Number
Distance from
Inside Wall, inches
1
2
3
4
4.13
12.4
20.6
28.9
Figure 3.4 Baghouse Outlet Traverse Point Locations
Garner, North Carolina
A-54
-------
APPENDIX B
FTIR DATA
-------
-------
B-l FTIR RESULTS TABLES
B-l
-------
B-2
-------
The semi-continuous FTIR analytical results are presented in Tables B-l to B-4. Table B-l
presents results from the inlet (wet) samples. Table B-2 presents results from the outlet (wet)
samples. Tables B-3 and B-4 present results from dry samples collected at the inlet and outlet,
respectively.
The concentration results are presented in ppm with estimated uncertainties indicated by the
symbol "A" in the column heading. Samples that were spiked with toluene and SF6 are indicated
by bold-face type. Refer to the FTIR field data sheets for detailed documentation on each file
name and the sampling conditions.
Concentration versus time plots of the FTIR results are presented immediately after Table B-4.
B-3
-------
B-4
-------
TABLE B-l. FTIR RESULTS OF WET SAMPLES FROM THE PLANT A BAGHOUSE INLET
Date Time File Name
8/19/97 8:34 INLSP101
8:39 INLSP102
Run 1 8:44 INLSP103
9:00 18190001
9:02 18190002
9:05 18190003
9:07 18190004
9:09 18190005
9:11 18190006
9:13 18190007
10:26 18190040
10:28 18190041
10:30 18190042
10:32 18190043
10:34 18190044
10:36 18190045
10:38 18190046
11:16 18190047
11:18 18190048
11:20 18190049
11:22 18190050
11:24 18190051
11:26 18190052
11:29 18190053
11:31 18190054
11:33 18190055
11:35 18190056
11:37 18190057
11:39 18190058
11:41 18190059
11:44 18190060
11:46 18190061
11:48 18190062
11:50 18190063
11:52 18190064
11:54 18190065
11:56 18190066
11:58 18190067
12:01 18190068
12:03 18190069
12:43 18190088
12:45 18190089
12:48 18190090
12:50 18190091
12:52 18190092
Toluene
ppm A
25.0 7.4
23.2 7.3
22.9 6.9
38.5
39.7
40.1
39.4
39.0
38.7
38.4
34.7
41.0
40.4
38.3
35.7
33.9
32.7
42.0
42.5
39.8
33.7
32.2
31.2
31.4
31.0
31.4
30.9
31.4
31.4
30.9
31.8
32.9
32.5
32.7
31.2
29.6
27.5
25.0
5.1
17.0
6.9
14.7
24.1
25.0
25.0
Hexane
ppm A
61.6
60.8
57.3
185.6
191.8
193.5
189.9
188.4
186.5
185.2
167.4
197.6
195.0
185.0
172.2
163.4
157.7
202.7
205.1
192.2
162.6
155.3
150.7
151.3
149.4
151.6
149.1
151.6
151.4
149.1
153.2
158.5
156.9
157.6
150.7
142.8
132.7
120.7
24.6
82.1
33.2
71.1
116.2
120.6
120.8
Ethylene
ppm A
3.1
3.0
2.9
35.6
46.0
45.6
46.1
35.8
35.8
35.8
16.3 8.5
44.7
44.8
35.7
16.7 10.9
16.3 8.3
14.7 7.3
43.7
43.3
44.7
19,1 9.0
21.7 7.4
20.4 6.7
21.1 6.7
20.5 6.5
19.2 6.8
24.0 6.6
18.8 6.8
20.7 7.2
18.8 6.7
18.4 7.0
18.0 7.9
18.9 7.5
19.2 7.8
19.7 6.9
20.9 6.1
14.9 5.3
12.1 4.8
2.5 1.3
7.6 3.6
3.5 1.7
18.9 3.3
28.5 4.7
22.3 4.8
17.7 4.8
SF6
ppm A
0.592 0.059
0.542 0.058
0.548 0.056
0.758
0.978
0.969
0.979
0.762
0.761
0.762
0.197
0.951
0.953
0.760
0.254
0.192
0.168
0.929
0.920
0.951
0.209
0.172
0.154
0.154
0.150
0.158
0.152
0.157
0.167
0.154
0.161
0.183
0.174
0.180
0.161
0.142
0.121
0.110
0.029
0.084
0.040
0.078
0.108
0.111
0.110
Methane
ppm A
9.4 5.1
9.2 5.1
8.6 4.8
25.3 15.3
25.7 15.8
25.4 15.9
25.3 15.6
24.9 15.5
25.4 15.3
24.9 15.2
22.5 13.8
24.8 16.2
24.5 16.0
26.0 15.2
23.6 14.2
22.0 13.5
20.9 13.0
28.0 16.7
27.9 16.9
26.5 15.9
25.8 13.6
26.2 13.2
25.2 12.8
25.5 12.8
25.0 12.6
24.5 12.7
26.4 12.7
24.1 12.7
24.9 12.7
23.4 12.5
24.0 12.8
24.0 13.2
24.5 13.1
24.3 13.2
24.1 12.6
23.8 12.1
20.9 11.2
18.9 10.2
4.6 2.1
13.5 7.0
6.3 2.9
16.3 6.9
25.3 11.1
22.4 10.8
20.6 10.5
S02
ppm A
20.9 11.6
22.1 11.4
19.7 10.9
138.0
178.1
176.5
178.4
138.7
138.7
138.7
75.8 36.2
173.1
173.5
138.4
72.8 46.5
68.0 35.3
64.7 31.0
169.2
167.6
173.1
55.4 38.3
54.2 31.6
50.8 28.5
52.5 28.5
51.8 27.7
53.8 29.1
50.9 28.0
56.1 29.1
58.6 30.7
58.0 28.4
58.0 29.8
59.1 33.7
59.3 32.1
60.3 33.1
57.9 29.7
50.6 26.2
44.5 22.4
34.1 20.3
10.0 5.4
26.5 15.3
12.8 7.3
22.0 14.2
34.0 20.0
38.6 20.5
39.3 20.4
CO
ppm A
80.2 58.0
72.4 56.7
66.4 53.8
198.1 167.5
191.4 173.1
189.0 174.2
186.6 171.1
182.6 168.2
182.4 167.1
183.3 166.5
216.1 155.8
234.3 186.4
208.7 181.8
281.2 176.7
231.5 159.9
206.7 150.8
189.7 144.3
267.6 199.2
302.0 210.8
252.0 187.3
235.3 152.5
254.9 147.7
245.4 142.9
252.4 143.7
249.2 142.6
237.7 143.5
284.8 145.1
236.9 143.5
256.1 145.3
244.7 142.0
234.7 146.6
223.9 148.4
231.9 147.1
233.3 148.1
246.3 142.5
259.4 138.0
211.8 125.4
184.8 112.1
44.6 20.4
139.2 75.8
63.8 27.4
232.5 74.0
347.8 122.4
295.3 122.9
256.0 118.9
Formaldehyde
ppm A
5.7
5.6
5.3
17.2
17.8
17.9
17.6
17.4
22.1 13.7
23.6 13.6
15.5
18.3
18.1
17.1
15.9
15.1
14.6
18.8
19.0
17.8
21.9 12.2
24.9 11.8
23.8 11.4
24.7 11.5
23.5 11.3
22.9 11.4
25.8 11.4
23.1 11.4
24.1 11.4
23.0 11.2
22.7 11.5
21.7 11.8
22.1 11.7
22.2 11.8
22.9 11.3
23.7 10.8
20.5 10.0
17.9 9.1
3.4 1.9
12.8 6.2
5.0 2.6
18.1 6.2
30.0 9.9
26.1 9.6
22.8 9.4
03
-------
TABLE B-l. Continued. Wet Sample Inlet Results.
Date Time File Name
8/19/97 12:54 18190093
Runl 12:56 18190094
12:58 18190095
13:00 18190096
13:02 18190097
13:05 18190098
13:07 18190099
13:54 18190120
13:56 18190121
13:58 18190122
14:00 18190123
14:02 18190124
14:04 18190125
14:06 18190126
14:09 18190127
14:11 18190128
14:17 INLSP104
14:24 INLSP105
Average — >
Toluene
ppm A
25.3
23.8
23.9
24.1
25.0
25.1
25.8
23.9
24.5
24.0
24.6
24.7
24.1
24.7
24.1
23.9
19.4
19.5
Hexane
ppm A
122.0
114.7
115.4
116.4
120.4
121.2
124.3
115.2
118.1
115.9
118.8
119.1
116.3
119.1
116.4
115.5
93.7
94.1
Ethylene
ppm A
18.9 5.0
12.8 4.6
22.8 4.6
20.4 4.6
18.9 4.7
26.8 4.8
19.0 5.1
21.1 4.6
16.5 4.9
19.1 4.6
17.7 5.1
13.7 4.8
18.3 4.9
17.6 4.6
18.9 4.7
19.2 4.7
13.6 4.3
14.9 4.4
13.6
SF6
ppm A
0.114
0.105
0.107
0.106
0.107
0.110
0.116
0.106
0.112
0.107
0.118
0.111
0.112
0.106
0.109
0.108
0.330 0.092
0.327 0.093
Methane
ppm A
21.2 10.6
17.7 9.7
22.4 10.4
21.4 10.2
20.4 10.5
24.1 11.0
20.9 10.8
20.8 10.2
18.7 10.2
19.7 10.1
17.9 9.8
17.1 9.9
19.7 10.1
18.6 10.3
19.6 10.1
19.8 10.1
16.1 8.3
16.6 8.4
22.2
S02
ppm A
39.1 21.2
35.6 19.5
32.2 19.8
35.3 19.7
36.1 19.9
34.9 20.4
37.8 21.6
33.4 19.7
40.7 20.9
37.4 19.8
37.4 21.9
39.4 20.6
35.9 20.8
39.0 19.9
34.7 20.2
35.4 20.0
29.5 16.8
30.6 16.8
35.5
CO
ppm A
265.4 120.0
208.9 109.5
303.8 118.7
295.2 1 16.8
268.8 118.8
333.9 126.7
270.2 123.8
293.0 116.3
249.8 117.1
279.4 117.7
267.4 118.4
223.8 114.6
268.5 116.2
265.5 117.3
276.0 1 16.5
276.7 115.8
246.1 93.8
261.3 95.6
238.5
Formaldehyde
ppm A
22.8 9.5
18.8 8.7
23.9 9.3
23.0 9.2
22.8 9.4
26.9 9.8
24.2 9.7
22.0 9.1
20.7 9.1
21.4 9.0
18.1 8.9
16.4 8.9
20.0 9.0
20.7 9.2
20.9 9.1
21.4 9.1
16.8 7.4
17.7 7.5
15.5
w
ON
Date Time File Name
8/20/97 8:12 INLSP202
Run 2 8:17 INLSP203
8:34 18200001
8:36 18200002
8:38 18200003
8:40 18200004
8:42 18200005
8:44 18200006
8:46 18200007
8:49 18200008
8:51 18200009
8:53 18200010
8:55 18200011
8:57 18200012
8:59 18200013
8/20/97 9:01 18200014
Run 2 9:04 18200015
9:06 18200016
9:50 18200037
9:53 18200038
9:55 18200039
9:57 18200040
9:59 18200041
Toluene
ppm A
46.7 12.9
43.1 13.6
41.4
40.3
40.2
40.9
40.5
40.8
39.8
37.7
37.1
37.7
38.0
37.9
37.3
36.6
35.9
36.7
41.0
40.1
42.5
44.6
44.9
Hexane
ppm A
108.0
114.0
199.6
194.2
194.0
197.5
195.5
196.7
191.8
181.8
179.1
181.7
183.5
182.6
179.8
176.7
173.3
176.9
197.9
193.5
205.0
215.0
216.5
Ethylene
ppm A
13.1 4.9
11.3 5.1
45.6
36.7
46.1
45.7
45.9
45.7
36.0
17.8 13.0
20.7 11.8
23.1 12.2
20.2
16.6 16.3
18.3 12.9
16.8 10.8
17.8 9.0
16.9 9.9
44.5
45.4
44.0
48.8
48.4
SF6
ppm A
0.616 0.104
0.610 0.108
0.969
0.779
0.979
0.971
0.977
0.972
0.764
0.312
0.276
0.284
0.429
0.390
0.300
0.251
0.208
0.230
0.947
0.966
0.936
1.037
1.029
Methane
ppm A
18.7 9.0
18.2 9.5
28.2 16.4
27.8 16.0
29.2 16.0
28.8 16.2
28.5 16.1
28.9 16.2
28.7 15.8
27.8 15.0
27.3 14.8
28.4 15.1
27.4 15.1
27.1 15.1
26.3 14.8
25.6 14.5
25.7 14.3
25.6 14.6
41.6 16.2
32.1 15.9
30.4 16.8
58.6 17.6
90.7 17.8
S02
ppm A
23.7 18.9
28.4 19.7
176.4
142.0
178.4
176.8
177.8
177.1
139.2
56.9
63.6 50.5
63.8 52.1
78.1
71.1
65.6 55.0
65.8 46.0
62.5 38.3
70.2 42.3
172.4
176.0
170.4
188.9
187.4
CO
ppm A
193.6 102.9
176.5 106.1
185.2 176.7
185.4 170.6
211.6 173.5
195.8 176.3
204.3 175.4
206.1 176.1
211.6 169.8
216.6 163.0
214.8 160.4
230.3 164.3
210.5 163.8
208.5 162.6
196.5 159.4
189.2 156.4
198.2 154.1
191.2 157.3
655.7 229.3
420.2 195.2
309.2 197.0
728.8 260.4
1202.8 377.8
Formaldehyde
ppm A
16.0 8.1
10.6
18.5
18.0
18.0
18.3
18.1
18.2
17.8
16.8
16.6
16.8
17.0
16.9
16.6
16.4
16.0
16.4
18.3
17.9
19.0
19.9
20.0
-------
TABLE B-l. Continued. Wet Sample Inlet Results.
Date Time File Name
10:02 18200042
8/20/97 10:04 18200043
Run 2 10:06 18200044
10:09 18200045
10:11 18200046
10:13 18200047
10:15 18200048
10:17 18200049
10:19 18200050
10:21 18200051
10:24 18200052
10:26 18200053
10:28 18200054
10:30 18200055
11:26 18200074
11:29 18200075
11:31 18200076
11:33 18200077
11:35 18200078
11:37 18200079
11:39 18200080
11:41 18200081
11:44 18200082
11:46 18200083
11:48 18200084
11:50 18200085
11:52 18200086
11:54 18200087
11:56 18200088
11:58 18200089
\verage — >
Toluene
ppm A
44.1
43.7
44.6
46.5
47.7
47.8
48.2
48.7
43.9
45.4
50.8
46.6
44.6
44.5
45.9
43.8
43.2
44.3
43.8
43.3
44.4
44.4
44.1
43.9
45.4
44.1
43.2
43.2
43.5
42.9
Hexane
ppm A
212.9
210.9
215.4
224.2
230.3
230.6
232.6
234.9
211.7
219.0
245.2
224.7
214.9
214.6
221.3
211.4
208.3
213.8
211.5
209.0
214.0
214.1
212.6
212.0
218.9
212.7
208.2
208.5
210.0
207.0
Ethylene
ppm A
48.9
49.3
48.4
47.3
46.9
50.4
50.1
48.2
48.9
47.8
49.1
47.1
48.3
48.4
50.6
48.4
43.6
47.9
47.9
48.4
47.4
47.4
47.5
47.7
46.9
47.5
48.2
48.3
47.8
48.1
3.9
SF6
ppm A
.040
.047
.029
.006
0.997
.071
.065
.024
.040
.016
.044
.001
.027
.029
.076
.028
0.926
.019
.018
.029
.008
.009
.010
.013
0.997
.010
.025
.027
.016
.022
Methane
ppm A
71.8 17.5
51.5 17.3
62.9 17.7
73.6 18.4
129.8 18.9
130.9 19.0
112.2 19.1
191.2 19.4
88.9 17.4
114.8 18.0
225.3 20.2
109.3 18.5
68.1 17.6
54.8 17.6
103.4 18.2
55.6 17.4
43.4 17.1
70.1 17.6
65.0 17.4
46.0 17.2
75.5 17.6
72.7 17.6
64.0 17.5
58.8 17.4
128.9 18.0
89.8 17.5
56.5 17.1
47.0 17.1
72.9 17.3
75.7 17.0
62.9
SO2
ppm A
189.4
190.7
187.4
183.2
181.6
195.0
194.0
186.5
189.4
185.1
190.1
182.2
186.9
187.4
196.0
187.3
168.6
185.6
185.3
187.3
183.5
183.7
184.0
184.5
181.6
184.0
186.7
187.0
185.0
186.1
9.5
CO
ppm A
1002.8 308.7
776.2 266.5
951.1 311.0
1058.6 362.4
1702.4 895.7
1703.3 895.5
1651.9 898.0
1894.1 879.7
1001.7 305.1
1236.2 398.1
1967.5 869.2
1718.0 783.8
988.5 326.5
823.1 291.5
1654.1 900.7
824.8 305.4
678.6 269.2
1073.3 383.7
1016.1 359.6
746.1 301.9
1034.1 670.2
1206.2 728.7
988.0 667.8
924.7 395.1
1780.3 888.8
1606.0 905.9
929.6 342.6
763.5 304.6
1149.1 474.8
1192.9 474.1
806.8
Formaldehyde
ppm A
19.7
19.5
19.9
20.8
21.3
21.3
21.5
21.7
19.6
20.3
22.7
20.8
19.9
19.9
20.5
19.6
19.3
19.8
19.6
19.4
19.8
19.8
19.7
19.6
20.3
19.7
19.3
19.3
19.4
19.2
1.0
w
-------
TABLE B-l. Continued. Wet Sample Inlet Results.
Date Time File Name
8/20/97 15:49 18200157
15:51 18200158
Run 3 15:53 18200159
15:55 18200160
15:57 18200161
16:00 18200162
16:02 18200163
16:04 18200164
16:06 18200165
16:08 18200166
16:10 18200167
8/20/97 16:12 18200168
Run 3 16:14 18200169
16:17 18200170
Average — >
Toluene
ppm A
34.0
38.4
40.1
40.6
40.0
38.7
39.7
39.4
40.5
41.6
40.5
39.2
38.5
36.7
Hexane
ppm A
164.2
185.4
193.6
196.0
193.0
186.6
191.7
189.9
195.3
200.7
195.4
189.1
185.5
177.0
Ethylene
ppm A
35.4
43.8
43.2
43.9
43.2
43.7
43.1
43.3
43.2
48.0
48.7
43.3
43.5
44.6
SF4
ppm A
0.752
0.931
0.918
0.934
0.919
0.929
0.917
0.920
0.918
1.021
1.036
0.920
0.925
0.949
Methane
ppm A
21.5 13.7
23.5 15.4
23.8 16.0
24.0 16.2
23.9 16.0
23.3 15.5
23.5 15.9
23.4 15.8
24.4 16.2
24.5 16.6
23.8 16.2
23.0 15.7
22.9 15.4
23.0 14.6
23.5
SO.,
ppm A
137.0
169.6
167.2
170.1
167.3
169.2
167.0
167.6
167.3
185.9
188.7
167.6
168.5
172.7
CO
ppm A
206.1 168.1
272.5 270.7
631.7
630.1
633.3
263.3
632.9
380.5
631.1
626.8
629.8
632.8
299.3
216.1 212.2
49.6
Formaldehyde
ppm A
15.2
17.2
17.9
18.1
17.9
17.3
17.7
17.6
18.1
18.6
18.1
17.5
17.2
21.5 13.1
1.5
Date Time File Name
8/21/97 9:43 18210016
9:45 18210017
Run 4 9:47 18210018
9:49 18210019
9:52 18210020
9:54 18210021
9:56 18210022
9:58 18210023
10:00 18210024
10:02 18210025
10:04 18210026
10:06 18210027
10:09 18210028
8/21/97 10:11 18210029
10:13 18210030
Run 4 10:15 18210031
Average — >
Toluene
ppm A
25.5
28.4
29.5
30.2
30.3
30.0
29.2
28.9
28.8
28.6
28.4
29.5
32.8
31.5
30.7
30.8
Hexane
ppm A
122.9
137.2
142.3
145.5
146.1
144.8
140.6
139.3
138.8
138.0
136.9
142.1
158.1
152.0
148.2
148.7
Ethylene
ppm A
8.9 4.8
10.5 5.4
10.6 5.7
10.7 5.9
10.7 5.9
10.7 5.8
10.5 5.6
10.4 5.6
10.2 5.5
10.3 5.5
10.2 5.5
13.5 5.7
24.6 7.2
15.7 6.5
11.7 6.1
10.9 6.1
11.9
SF<
ppm A
0.110
0.124
0.130
0.135
0.135
0.133
0.129
0.127
0.126
0.126
0.125
0.129
0.165
0.149
0.140
0.139
Methane
ppm A
18.3 10.2
19.9 11.4
20.4 11.8
20.8 12.1
20.8 12.1
20.6 12.0
19.9 11.6
19.7 11.5
19.4 11.5
19.6 11.4
19.3 11.3
21.1 11.8
26.6 13.4
22.7 12.7
20.9 12.3
20.7 12.3
20.7
SO2
ppm A
51.5 20.5
52.7 23.2
52.7 24.3
52.5 25.1
52.4 25.2
52.6 24.9
51.4 24.1
50.8 23.7
50.2 23.7
50.5 23.5
50.3 23.3
52.3 24.2
55.4 30.6
58.2 27.8
56.1 26.1
54.7 26.1
52.8
CO
ppm A
154.4 112.3
169.6 124.7
172.6 128.3
168.5 130.3
164.8 130.2
166.3 129.2
166.1 126.3
168.6 125.6
171.6 125.6
171.0 125.2
169.1 124.0
200.0 131.0
284.3 150.4
201.3 138.3
170.6 133.1
168.4 133.4
179.2
Formaldehyde
ppm A
11.4
12.7
13.2
13.5
13.5
13.4
13.0
12.9
12.8
12.8
12.7
13.2
14.6
14.1
13.7
13.8
cd
oo
-------
TABLE B-l. Continued. Additional Hydrocarbon Results in Wet Inlet Samples at Plant A
Date Time File Name
8/19/97 8:34 INLSP101
8:39 INLSP102
Run 1 8:44 INLSP103
9:00 18190001
9:02 18190002
9:05 18190003
9:07 18190004
9:09 18190005
9:11 18190006
9:13 18190007
10:26 18190040
10:28 18190041
10:30 18190042
10:32 18190043
10:34 18190044
10:36 18190045
10:38 18190046
11:16 18190047
11:18 18190048
11:20 18190049
11:22 18190050
11:24 18190051
11:26 18190052
11:29 18190053
11:31 18190054
11:33 18190055
11:35 18190056
11:37 18190057
11:39 18190058
11:41 18190059
11:44 18190060
11:46 18190061
11:48 18190062
11:50 18190063
11:52 18190064
11:54 18190065
11:56 18190066
11:58 18190067
12:01 18190068
12:03 18190069
12:43 18190088
12:45 18190089
12:48 18190090
12:50 18190091
12:52 18190092
12:54 18190093
12:56 18190094
12:58 18190095
13:00 18190096
13:02 18190097
13:05 18190098
13:07 18190099
13:54 18190120
13:56 18190121
13:58 18190122
14:00 18190123
14:02 18190124
14:04 18190125
14:06 18190126
14:09 18190127
14:11 18190128
14:17 INLSP104
14:24 INLSP105
Average — >
Butane
ppm Uncertainty
68.8
67.9
64.0
207.4
214.3
216.2
212.2
210.5
208.4
207.0
187.1
220.8
218.0
206.7
192.4
182.6
176.2
226.5
229.2
214.7
181.7
173.5
168.4
169.0
167.0
169.4
166.7
169.4
169.1
166.6
171.2
177.1
175.4
176.1
168.4
159.6
148.3
134.9
27.5
91.7
37.1
79.4
129.8
134.8
135.0
136.3
128.1
129.0
130.1
134.5
135.5
138.9
128.7
132.0
129.5
132.7
133.1
130.0
133.1
130.1
129.1
104.6
105.2
2-Methyl-l-pentene
ppm Uncertainty
24.7
24.4
23.0
74.5
77.0
77.7
76.3
75.6
74.9
74.4
67.2
79.4
78.3
74.3
69.1
65.6
63.3
81.4
82.4
77.2
65.3
62.3
60.5
60.7
60.0
60.9
59.9
60.9
60.8
59.9
61.5
63.6
63.0
63.3
60.5
57.3
53.3
48.5
9.9
32.9
13.3
28.5
46.7
48.4
48.5
49.0
46.0
46.4
46.7
48.3
48.7
49.9
46.3
47.4
46.5
10.9 3.1
8.5 3.1
46.7
47.8
46.7
46.4
37.6
37.8
0.3
2-Methyl-2-butene
ppm Uncertainty
17.9
17.7
16,7
54.0
55.8
56.3
55.3
54.8
54.3
53.9
48.7
57.5
56.8
53.8
50.1
47.5
45.9
59.0
59.7
55.9
47.3
45.2
43.9
44.0
43.5
44.1
43.4
44.1
44.0
43.4
44.6
46.1
45.7
45.9
43.9
41.6
38.6
35.1
7.2
23.9
9.7
20.7
33.8
35.1
35.2
35.5
33.4
33.6
33.9
35.0
35.3
36.2
33.5
34.4
33.7
34.6
34.7
33.9
34.7
33.9
33.6
27.3
27.4
B-9
-------
TABLE B-l. Continued. Plant A Wet Sample Inlet Results
Date Time File Name
8/20/97 8:06 INLSP201
8:12 INLSP202
Run 2 8:17 INLSP203
8:34 18200001
8:36 18200002
8:38 18200003
8:40 18200004
8:42 18200005
8:44 18200006
8:46 18200007
8:49 18200008
8:51 18200009
8:53 18200010
8:55 18200011
8:57 18200012
8:59 18200013
9:01 18200014
9:04 18200015
9:06 . 18200016
9:50 18200037
9:53 18200038
9:55 18200039
9:57 18200040
9:59 18200041
10:02 18200042
10:04 18200043
10:06 18200044
10:09 18200045
10:11 18200046
10:13 18200047
10:15 18200048
10:17 18200049
10:19 18200050
10:21 18200051
10:24 18200052
10:26 18200053
10:28 18200054
10:30 18200055
11:26 18200074
11:29 18200075
11:31 18200076
11:33 18200077
11:35 18200078
11:37 18200079
11:39 18200080
11:41 18200081
11:44 18200082
11:46 18200083
11:48 18200084
11:50 18200085
11:52 18200086
11:54 18200087
11:56 18200088
11:58 18200089
Average — >
Butane
ppm Uncertainty
116.4
120.7
127.4
223.1
217.1
216.8
220.7
218.4
219.8
214.4
203.1
200.2
203.0
205.1
204.0
200.9
197.4
193.6
197.7
221.2
216.2
229.1
240.2
241.9
237.9
235.7
240.7
250.5
257.3
257.7
259.9
262.5
236.6
244.7
274.0
251.0
240.2
239.8
247.3
236.2
232.7
238.9
236.3
233.6
239.1
239.3
237.6
236.9
244.6
237.6
232.6
232.9
234.6
231.3
2-Methyl- 1 -pentene
ppm Uncertainty
41.8
43.4
45.8
80.2
78.0
77.9
79.3
78.5
79.0
77.0
73.0
71.9
73.0
73.7
73.3
72.2
70.9
69.6
71.1
79.5
77.7
82.3
86.3
86.9
85.5
84.7
86.5
90.0
92.5
92.6
93.4
94.3
85.0
87.9
98.4
90.2
86.3
86.2
88.9
84.9
83.6
85.8
84.9
83.9
85.9
86.0
85.4
85.1
87.9
85.4
83.6
83.7
84.3
83.1
2-Methyl-2-butene
ppm Uncertainty
30.3
31.4
33.2
58.1
56.5
56.5
57.5
56.9
57.2
55.8
52.9
52.1
52.9
53.4
53.1
52.3
51.4
50.4
51.5
57.6
56.3
59.7
62.6
63.0
61.9
61.4
62.7
65.2
67.0
67.1
67.7
68.4
61.6
63.7
71.3
65.4
62.5
62.5
64.4
61.5
60.6
62.2
61.6
60.8
62.3
62.3
61.9
61.7
63.7
61.9
60.6
60.7
61.1
60.3
B-10
-------
TABLE B-l. Continued. Plant A Wet Sample Inlet Results
Date Time File Name
8/20/97 15:49 18200157
15:51 18200158
Run 3 15:53 18200159
15:55 18200160
15:57 18200161
16:00 18200162
16:02 18200163
16:04 18200164
16:06 18200165
16:08 18200166
16:10 18200167
16:12 18200168
16:14 18200169
16:17 18200170
Average — >
Butane
ppm Uncertainty
183.5
207.2
216.4
219.0
215.7
208.5
214.2
212.2
218.2
224.3
218.4
211.3
207.3
197.8
2-Methy 1- 1 -pentene
ppm Uncertainty
65.9
74.4
77.8
78.7
77.5
74.9
77.0
76.3
78.4
80.6
78.5
75.9
74.5
71.1
2-Methyl-2-butene
ppm Uncertainty
47.8
54.0
56.4
57.0
56.2
54.3
55.8
55.3
56.8
58.4
56.9
55.0
54.0
51.5
Date Time File Name
8/21/97 9:43 18210016
9:45 18210017
Run 4 9:47 18210018
9:49 18210019
9:52 18210020
9:54 18210021
9:56 18210022
9:58 18210023
10:00 18210024
10:02 18210025
10:04 18210026
10:06 18210027
10:09 18210028
10:11 18210029
10:13 18210030
10:15 18210031
Average — >
Butane
ppm Uncertainty
137.4
153.3
159.1
162.6
163.3
161.8
157.2
155.6
155.1
154.2
152.9
158.8
176.7
169.9
165.7
166.1
2-Methyl-l-pentene
ppm Uncertainty
49.4
55.1
57.2
58.4
58.7
58.1
56.5
55.9
55.7
55.4
55.0
57.1
63.5
61.0
59.5
59.7
2-Methyl-2-butene
ppm Uncertainty
35.8
39.9
41.4
42.4
42.5
42.1
40.9
40.5
40.4
40.2
39.8
41.4
46.0
44.2
43.1
43.3
B-ll
-------
TABLE B-2. FTIR RESULTS OF WET SAMPLES FROM THE PLANT A BAGHOUSE OUTLET
Date Time File Name
8/19/97 7:54 WOUAMB01
8:04 OUTSP001
Run 1 8:09 OUTSP102
8:13 OUTSP103
9:17 18190009
9:20 18190010
9:22 18190011
9:24 18190012
9:26 18190013
9:28 18190014
9:30 18190015
9:32 18190016
9:34 18190017
9:37 18190018
9:39 18190019
9:41 18190020
9:43 18190021
9:45 18190022
9:47 18190023
9:49 18190024
9:52 18190025
9:54 18190026
9:56 18190027
9:58 18190028
10:00 18190029
10:04 18190030
10:06 18190031
10:09 18190032
10:11 18190033
10:13 18190034
10:15 18190035
10:17 18190036
10:19 18190037
10:21 18190038
12:05 18190070
12:07 18190071
12:09 18190072
12:11 18190073
12:13 18190074
12:16 18190075
12:18 18190076
12:20 18190077
12:22 18190078
12:24 18190079
12:26 18190080
12:28 18190081
12:30 18190082
12:33 18190083
Toluene
pptn A
2.8
21.7 7.9
21.1 7.8
20.8 8.2
17.6
17.7
17.8
17.7
17.3
17.7
17.8
16.8
17.3
17.6
17.3
17.8
16.8
17.2
17.4
16.7
16.6
16.7
17.1
16.8
17.2
17.0
11.6
8.7
15.1
16.5
16.6
16.8
16.4
16.7
11.3
11.8
11.6
11.6
11.8
12.0
11.7
11.2
11.0
11.1
10.9
11.2
11.3
11.0
Hexane
ppm A
13.6
67.1
66.6
69.6
85.0
85.4
85.9
85.5
83.4
85.5
85.6
81.1
83.5
85.0
83.5
85.8
80.9
82.8
83.8
80.7
79.9
80.7
82.5
81.1
82.8
82.2
3.3
2.5
4.2
79.8
80.3
81.3
79.2
80.5
6.8 0.8
6.6 0.8
6.0 0.8
5.2 0.8
5.9 0.8
6.2 0.8
6.3 0.8
7.0 0.8
6.6 0.8
7.4 0.8
7.5 0.8
10.3 0.8
5.4 0.8
6.6 0.8
Ethylene
ppm A
0.7
9.9 2.9
10.6 2.8
9.5 3.0
12.9 4.4
13.0 4.6
13.1 4.6
13.2 4.4
13.6 4.1
13.5 4.8
13.5 5.0
13.9 3.9
13.5 4.4
13.5 5.0
13.5 4.3
13.1 5.1
13.3 3.9
13.0 4.1
13.1 4.5
13.3 3.8
13.2 3.7
13.0 3.9
13.2 4.3
13.6 3.8
13.2 4.1
13.4 4.1
7.6 2.2
4.9 1.8
11.0 2.9
13.2 3.7
13.4 3.8
13.0 4.0
13.8 3.6
13.3 3.9
20.0 2.2
17.9 2.2
16.7 2.2
15.1 2.3
17.2 2.3
17.9 2.3
17.8 2.2
19.0 2.1
17.5 2.1
20.2 2.2
21.0 2.1
26.8 2.2
12.9 2.2
18.2 2.2
SF6
ppm A
0.016
0324 0.061
0.317 0.060
0336 0.064
0.102
0.106
0.107
0.104
0.095
0.111
0.118
0.090
0.103
0.116
0.099
0.120
0.092
0.096
0.104
0.089
0.086
0.090
0.100
0.089
0.095
0.096
0.051
0.041
0.067
0.086
0.089
0.094
0.084
0.090
0.051
0.052
0.051
0.052
0.052
0.052
0.052
0.050
0.049
0.050
0.049
0.051
0.051
0.050
Methane
ppm A
5.6 1.2
19.8 5.5
19.7 5.5
20.3 5.7
22.5 7.0
22.5 7.0
22.8 7.1
22.5 7.0
22.2 6.9
22.9 7.0
22.8 7.0
21.7 6.7
22.2 6.9
22.7 7.0
22.2 6.9
23.0 7.0
21.3 6.6
21.8 6.8
22.1 6.9
21.3 6.6
21.0 6.6
21.0 6.6
21.4 6.8
21.3 6.7
21.6 6.8
21.3 6.8
17.7 4.6
12.9 3.5
20.3 6.0
20.7 6.6
20.9 6.6
21.1 6.7
21.2 6.5
20.8 6.6
19.8 4.5
19.4 4.7
18.9 4.6
17.9 4.6
19.4 4.7
19.7 4.8
19.1 4.6
19.1 4.4
18.3 4.4
19.1 4.4
19.4 4.3
21.6 4.4
16.8 4.5
18.6 4.4
SO2
ppm A
4.3 2.8
48.4 11.1
49.1 10.9
53.8 11.6
70.6 18.6
72.2 19.5
73.0 19.7
71.9 19.0
68.9 17.5
73.3 20.4
76.1 21.6
67.7 16.6
70.9 19.0
73.8 21.2
69.4 18.2
75.0 22.0
67.2 16.8
69.1 17.7
71.5 19.1
67.0 16.4
66.4 15.8
68.5 16.6
70.4 18.3
68.0 16.4
71.9 17.4
71.4 17.6
53.8 9.3
41.4 7.6
65.6 12.4
68.4 15.9
68.0 16.4
71.2 17.3
66.7 15.5
69.4 16.5
26.1 9.4
32.8 9.6
30.0 9.3
31.6 9.6
33.1 9.7
34.4 9.7
32.0 9.6
28.6 9.2
29.0 9.1
28.4 9.2
27.0 9.1
27.3 9.4
34.4 9.4
29.3 9.3
CO
ppm A
13.8
150.9 60.5
154.8 59.9
161.6 62.8
169.9 75.6
170.6 76.0
174.2 76.5
174.1 76.2
170.0 74.2
190.2 76.7
208.9 77.4
178.1 72.6
177.7 74.4
204.8 77.4
190.9 74.7
223.3 78.5
180.1 72.3
177.5 74.2
184.4 75.4
174.9 72.1
172.9 71.7
177.5 72.8
179.1 73.8
174.3 72.5
179.9 74.1
178.5 74.0
139.0 50.9
1 10.6 39.0
164.5 65.2
170.9 71.8
173.9 72.4
188.1 73.6
179.6 71.5
186.1 72.8
276.2 55.7
248.3 56.7
238.8 55.0
229.4 54.3
252.4 56.2
252.4 57.7
249.7 55.8
266.9 54.6
255.6 53.5
282.3 54.9
288.3 54.4
340.5 58.4
209.7 53.0
269.1 54.2
Formaldehyde
ppm A
l.i
9.9 4.9
10.1 4.9
9.8 5.1
7.9
7.9
8.0
7.9
7.7
7.9
7.9
7.5
7.7
7.9
7.7
7.9
7.5
7.7
7.8
7.5
7.4
7.5
7.6
7.5
7.7
7.6
5.4 4.2
3.8 3.1
6.8
7.4
7.4
7.5
9.9 5.8
7.4
15.7 4.1
16.6 4.2
15.1 4.1
14.5 4.1
15.2 4.2
16.0 4.3
15.9 4.2
16.0 4.0
15.7 3.9
16.3 4.0
16.3 3.9
19.6 4.0
16.0 4.1
15.9 3.9
Cd
i
tx>
-------
TABLE B-2. Continued. Wet Sample Outlet Results.
Date Time File Name
12:35 18190084
12:37 18190085
12:39 18190086
12:41 18190087
13:22 18190106
13:24 18190107
13:26 18190108
13:28 18190109
13:30 18190110
13:32 18190111
13:34 18190112
13:37 18190113
13:41 18190114
13:43 18190115
13:45 18190116
13:47 18190117
14:33 OUTSP104
14:38 OUTSP105
Average — >
Toluene
ppm A
11.5
11.6
11.5
11.7
11.2
11.4
11.4
11.5
11.3
11.2
11.4
11.3
11.2
11.2
11.0
11.2
17.8 5.3
16.8 5.3
Hexane
ppm A
6.8 0.8
5.6 0.8
5.6 0.8
7.7 0.8
7.1 0.8
6.8 0.8
5.1 0.8
8.5 0.8
6.4 0.8
6.9 0.8
5.2 0.8
7.0 0.8
7.2 0.8
5.0 0.8
4.3 0.8
7.1 0.8
4.1 0.7
3.3 0.7
3.2
Ethylene
ppm A
17.7 2.2
15.2 2.2
16.2 2.2
22.0 2.4
21.2 2.2
17.8 2.2
14.3 2.2
24.8 2.3
16.0 2.2
19.3 2.2
13.9 2.2
20.1 2.1
19.6 2.2
13.4 2.1
11.5 2.2
20.0 2.2
10.3 2.1
8.1 2.1
15.6
SF6
ppm A
0.052
0.052
0.051
0.055
0.050
0.051
0.051
0.052
0.050
0.051
0.051
0.049
0.051
0.049
0.050
0.051
0.371 0.044
0.368 0.044
Methane
ppm A
18.8 4.6
17.8 4.6
18.3 4.6
20.1 4.6
19.1 4.5
18.3 4.5
16.4 4.5
20.4 4.5
17.4 4.5
18.5 4.4
16.4 4.5
18.7 4.5
18.5 4.5
15.8 4.5
15.6 4.4
18.1 4.4
13.0 3.6
12.3 3.6
20.8
SO2
ppm A
33.3 9.5
33.0 9.6
31.0 9.4
32.6 10.1
29.8 9.3
34.4 9.6
33.2 9.4
29.6 9.6
33.9 9.3
30.1 9.4
35.7 9.5
30.6 9.2
28.6 9.5
32.9 9.2
31.7 9.3
30.7 9.4
26.5 8.1
26.3 8.0
51.8
CO
ppm A
258.9 55.5
231.1 54.7
242.4 54.8
302.8 57.8
299.3 55.6
268.1 55.3
229.8 53.4
327.5 58.4
260.7 53.5
279.2 55.1
222.0 53.1
289.0 55.8
288.3 55.8
219.2 52.9
198.2 50.7
281.1 55.4
209.7 43.2
180.3 41.6
226.9
Formaldehyde
ppm A
16.8 4.1
15.6 4.1
15.3 4.1
17.7 4.2
15.7 4.0
16.5 4.1
14.5 4.1
17.2 4.1
16.4 4.1
15.8 4.0
14.3 4.1
15.4 4.1
15.6 4.0
14.2 4.0
13.0 3.9
15.2 4.0
11.7 3.3
10.1 3.3
9.0
Date Time File Name
8/20/97 7:47 OUTSP201
7:54 OUTSP202
Run 2 8:00 OUTSP203
9:12 18200019
9:14 18200020
9:16 18200021
9:18 18200022
9:21 18200023
9:23 18200024
9:25 18200025
9:27 18200026
9:29 18200027
9:31 18200028
9:33 18200029
9:36 18200030
9:38 18200031
9:40 18200032
9:42 18200033
9:44 18200034
10:36 18200058
Toluene
ppm A
15.3 6.5
20.2 6.5
15.8 6.3
15.9
16.4
16.6
16.4
17.7
18.7
18.9
18.0
17.2
16.9
15.2
12.5
14.2
18.3
17.6
16.2
18.5
Hexane
ppm A
4.7 0.8
53.9
6.0 0.8
76.8
79.2
80.0
79.2
85.4
90.0
91.2
86.9
83.1
81.5
73.3
3.5 0.9
68.7
88.3
85.0
78.1
89.2
Ethylene
ppm A
12.5 2.4
21.6 2.4
16.3 2.4
17.2 3.3
17.6 3.4
18.1 3.6
16.6 3.6
14.9 4.4
15.8 7.2
15.7 7.3
15.3 5.2
15.7 4.2
16.0 3.8
13.6 3.0
12.6 2.4
19.7 2.7
18.2 6.3
15.2 4.7
14.5 3.4
18.0
SF6
ppm A
0.160 0.051
0.179 0.051
0.172 0.050
0.077
0.079
0.084
0.084
0.103
0.167
0.171
0.120
0.097
0.088
0.068
0.054
0.062
0.147
0.110
0.079
0.382
Methane
ppm A
18.3 4.4
21.9 4.5
19.2 4.3
24.0 6.3
24.7 6.5
24.8 6.6
24.5 6.5
25.1 7.0
25.1 7.4
26.0 7.5
24.8 7.1
24.6 6.8
24.2 6.7
21.4 6.0
18.1 4.9
23.2 5.7
26.3 7.2
24.1 7.0
23.1 6.4
42.0 7.3
S02
ppm A
35.8 9.2
25.4 9.3
26.7 9.1
62.6 14.2
62.4 14.7
63.1 15.5
60.9 15.6
73.2 19.0
80.1 30.6
80.8 31.3
74.2 22.0
68.7 17.9
67.0 16.3
60.5 12.7
36.8 10.1
41.3 11.5
70.0 26.9
74.0 20.2
63.6 14.6
72.5 67.5
CO
ppm A
196.2 51.5
269.1 54.9
224.4 51.5
202.0 69.7
203.9 71.6
205.7 72.3
201.7 71.5
195.4 76.5
181.3 79.5
182.9 80.7
185.1 76.9
188.1 73.7
190.1 72.8
183.9 65.9
180.1 55.5
236.5 64.1
198.1 78.7
205.0 76.3
197.1 70.3
652.6 104.5
Formaldehyde
ppm A
15.3 4.0
16.3 4.0
13.1 3.9
15.4 5.7
16.1 5.8
16.8 5.9
16.3 5.8
13.4 6.3
8.3
8.4
8.0
11.7 6.1
12.0 6.0
11.4 5.4
9.2 4.4
11.7 5.1
12.3 6.5
7.9
11.5 5.7
8.3
-------
TABLE B-2. Continued. Wet Sample Outlet Results.
Date Time File Name
10:38 18200059
10:41 18200060
10:43 18200061
10:45 18200062
10:47 18200063
8/20/97 10:49 18200064
10:51 18200065
Run 2 10:53 18200066
10:56 18200067
10:58 18200068
11:00 18200069
11:02 18200070
11:04 18200071
11:06 18200072
11:08 18200073
12:05 18200092
12:07 18200093
12:09 18200094
12:11 18200095
12:13 18200096
12:16 18200097
12:18 18200098
12:20 18200099
12:22 18200100
12:24 18200101
12:26 18200102
12:28 18200103
12:30 18200104
12:33 18200105
12:35 18200106
12:37 18200107
12:39 18200108
Average — >
Toluene
ppm A
19.7
20.6
19.2
19.2
18.9
18.5
18.8
19.9
18.6
18.2
18.5
18.4
17.2
17.4
17.9
18.4
18.6
18.3
17.8
17.9
18.2
18.3
18.7
18.7
18.8
17.5
17.1
17.2
17.4
17.4
17.2
17.6
Hexane
ppm A
95.0
99.2
92.6
92.6
91.3
89.4
90.5
95.9
89.6
87.8
89.2
88.6
83.1
84.0
86.5
88.8
89.7
88.3
85.8
86.2
87.8
88.1
90.2
90.1
90.7
4.9
82.4
82.7
84.1
84.0
1.2
84.8
0.5
Ethylene
ppm A
22.3
30.0 19.9
22.6
22.6
22.8
23.0
22.9
26.9 20.1
23.0
17.9
18.2
19.0
14.7 5.6
15.0 5.9
17.8
19.5
20.3
18.7
17.9
17.9
17.9
22.9
22.8
22.8
22.7
15.1 8.3
13.3 5.4
13.8 6.1
14.6 7.2
17.9
17.8
17.8
9.5
SF6
ppm A
0.475
0.467
0.480
0.481
0.484
0.488
0.486
0.473
0.489
0.380
0.386
0.403
0.130
0.136
0.379
0.415
0.431
0.397
0.381
0.380
0.381
0.488
0.485
0.485
0.483
0.193
0.126
0.142
0.167
0.381
0.378
0.379
Methane
ppm A
91.7 7.8
184.0 8.2
97.3 7.6
65.2 7.6
62.7 7.5
55.8 7.3
61.2 7.4
147.5 7.9
96.5 7.4
36.5 7.2
42.8 7.3
65.6 7.3
38.6 6.8
40.0 6.9
45.5 7.1
48.6 7.3
50.5 7.4
44.0 7.3
37.5 7.0
35.9 7.1
36.3 7.2
51.8 7.2
55.5 7.4
50.3 7.4
70.2 7.5
40.4 6.9
27.6 6.8
33.2 6.8
36.4 6.9
29.2 6.9
31.8 6.8
28.2 7.0
45.7
SO2
ppm A
83.9
97.1 84.8
84.8
84.9
85.4
86.2
85.8
103.1 85.9
86.3
73.5 67.1
74.6 68.3
78.5 71.3
83.1 23.9
84.5 25.0
77.4 66.9
83.3 73.3
83.2 76.1
80.0 70.2
76.0 67.3
74.6 67.1
75.1 67.4
86.1
85.6
85.7
85.3
85.7 35.3
79.7 23.2
81.1 26.1
84.3 30.5
72.1 67.2
73.0 66.8
71.1 67.0
57.1
CO
ppm A
1097.4 146.4
2023.9 360.8
1159.2 148.6
958.1 131.0
948.9 128.7
873.4 121.5
869.2 121.1
1942.2 364.0
1020.4 128.6
516.3 95.3
649.6 104.2
963.2 125.1
629.8 97.2
647.4 99.0
762.7 109.6
826.8 118.2
847.5 120.4
773.5 114.3
688.5 105.3
655.9 103.2
648.7 105.3
850.7 119.5
903.7 126.7
823.4 120.9
1071.2 142.1
707.5 104.8
496.2 90.0
607.0 97.2
670.3 102.7
536.1 93.9
636.2 101.1
518.7 94.9
623.7
Formaldehyde
ppm A
8.8
9.2
8.6
8.6
8.5
8.3
8.4
8.9
8.3
8.1
8.3
8.2
7.7
7.8
8.0
8.2
8.3
8.2
7.9
8.0
8.1
8.2
8.3
8.3
8.4
7.8
7.6
7.7
7.8
7.8
7.7
7.9
4.7
to
-------
TABLE B-2. Continued. Wet Sample Outlet Results.
Date Time File Name
8/20/97 13:41 OUTUN301
13:49 OUTUN302
Run 3 14:01 OUTUN303
15:13 18200140
15:15 18200141
15:17 18200142
15:19 18200143
15:21 18200144
15:23 18200145
15:25 18200146
15:28 18200147
15:30 18200148
15:32 18200149
15:34 18200150
15:36 18200151
15:38 18200152
15:40 18200153
15:42 18200154
Average — >
Toluene
ppm A
10.1
4.9 1.8
3.9 1.7
14.4
14.3
14.9
15.4
15.5
15.4
15.9
15.9
16.4
16.4
15.8
15.6
15.1
15.4
16.2
0.5
Hexane
ppm A
4.0 0.7
4.4 0.3
4.5 0.2
2.9 1.0
2.7 1.0
2.0 1.0
.9 1.
.3 1.
.3 1.
.5 1.
2.1 1.
.6 1.
.6 1.
.8 1.
2.0 1.
2.4 1.
2.1 1.
1.6 1.
2.3
Ethylene
ppm A
11.1 2.0
8.8 0.7
8.5 0.8
13.3 3.2
13.0 3.2
12.5 3.7
12.8 4.1
11.9 4.1
11.9 4.0
13.0 4.9
13.7 4.5
13.7 6.0
14.2 7.2
13.2 4.8
13.4 5.1
13.5 3.8
13.4 4.1
13.5 5.5
12.5
SF6
ppm A
0.047
0.016
0.018
0.072
0.074
0.084
0.094
0.095
0.091
0.112
0.104
0.140
0.169
0.111
0.118
0.088
0.095
0.128
Methane
ppm A
15.7 4.0
8.2 1.0
9.0 1.1
19.0 5.7
18.8 5.7
18.8 5.9
19.5 6.1
19.2 6.2
19.0 6.1
19.8 6.3
19.9 6.3
20.6 6.5
20.4 6.5
19.9 6.3
19.3 6.2
19.4 6.0
19.6 6.1
20.2 6.4
18.1
S02
ppm A
50.4 8.7
23.7 2.9
49.6 3.4
59.0 13.5
57.9 13.8
63.4 15.7
64.7 17.4
68.4 17.6
66.6 16.9
65.8 20.7
63.6 19.2
68.4 25.8
69.4 30.8
62.8 20.6
62.0 21.7
58.6 16.4
61.2 17.7
67.0 23.6
60.1
CO
ppm A
218.2 48.7
255.1 26.3
297.0 30.5
198.9 65.1
190.9 65.3
188.3 67.9
192.7 70.5
232.2 72.9
202.1 71.0
189.9 73.2
188.1 73.4
213.9 78.1
210.6 77.7
190.4 72.8
186.0 72.7
191.4 69.1
186.3 71.2
202.1 76.2
207.5
Formaldehyde
ppm A
12.4 3.6
4.9 1.0
4.2 1.0
14.4 5.1
14.3 5.1
14.0 5.3
14.1 5.5
13.8 5.5
13.9 5.5
14.0 5.7
14.4 5.7
14.2 5.9
14.3 5.9
14.3 5.7
14.3 5.6
14.5 5.4
14.3 5.5
14.0 5.8
13.0
CO
-------
TABLE B-2. Continued. Wet Sample Outlet Results.
Date Time File Name
8/21/97 7:32 OUTUN401
9:11 18210001
Run 4 9:13 18210002
9:15 18210003
9:17 18210004
9:20 18210005
9:22 18210006
9:24 18210007
9:26 18210008
9:28 18210009
9:30 18210010
9:32 18210011
9:34 18210012
9:37 18210013
9:39 18210014
11:38 18210058
11:40 18210059
11:42 18210060
11:45 18210061
11:47 18210062
11:49 18210063
11:51 18210064
11:54 18210065
11:56 18210066
Average — >
Toluene
ppm A
14.4
13.8
14.4
15.2
15.2
14.6
14.6
15.1
14.8
14.0
13.8
14.2
14.2
13.9
13.8
14.1
14.4
14.6
15.0
14.7
14.6
14.1
13.5
13.4
Hexane
ppm A
69.3
66.3
69.7
73.3
73.1
70.6
70.3
72.9
71.6
67.8
66.7
68.6
68.3
4.6 .0
3.6 .0
4.9 .0
4.9 .0
4.3 .0
3.9 .0
3.7 .0
3.6 .0
3.6 .0
4.7 0.9
6.2 0.9
2.0
Ethylene
ppm A
27.4 2.7
9.5 2.6
10.5 2.8
17.5 3.0
18.1 2.9
15.9 2.8
15.7 2.8
16.6 3.0
17.3 2.9
18.3 2.7
28.1 2.6
27.9 2.7
24.3 2.7
16.7 2.6
14.2 2.6
16.7 2.8
17.2 2.9
17.4 2.9
17.4 2.9
17.0 2.9
16.9 2.9
13.6 2.7
13.7 2.6
15.1 2.6
17.6
SF6
ppm A
0.062
0.059
0.063
0.068
0.067
0.065
0.064
0.068
0.066
0.061
0.061
0.063
0.062
0.060
0.060
0.063
0.065
0.067
0.067
0.067
0.066
0.062
0.059
0.059
Methane
ppm A
27.1 5.7
19.5 5.5
20.5 5.7
23.6 6.1
24.2 6.0
22.9 5.8
22.8 5.8
23.5 6.0
23.6 5.9
23.1 5.6
26.6 5.5
26.6 5.7
24.9 5.6
21.7 5.5
20.6 5.4
20.5 5.6
20.8 5.7
21.0 5.8
21.4 5.9
21.0 5.8
20.7 5.8
19.0 5.6
18.7 5.3
19.1 5.3
22.2
SO2
ppm A
54.6 11.5
42.0 11.1
40.8 11.7
38.2 12.7
39.3 12.6
38.1 12.0
38.1 11.9
41.3 12.7
44.0 12.3
43.1 11.4
37.3 11.3
46.3 11.7
49.9 11.6
51.3 11.3
50.7 11.2
51.8 11.8
51.1 12.2
51.7 12.5
52.6 12.6
53.9 12.5
54.3 12.3
51.3 11.6
48.6 11.1
46.4 11.0
46.5
CO
ppm A
291.7 68.0
131.7 58.6
136.4 61.1
208.1 66.6
215.2 66.7
198.2 64.2
196.8 63.9
202.6 66.1
211.2 65.5
229.2 63.4
307.9 66.1
311.4 68.1
287.6 66.8
221.1 62.9
197.7 61.4
237.2 64.0
240.3 65.3
240.2 66.2
233.5 67.5
234.7 66.8
236.9 66.0
201.1 62.4
211.6 60.7
226.9 60.9
225.4
Formaldehyde
ppm A
19.1 5.2
6.1
6.4
6.8
11.6 5.4
11.0 5.2
10.4 5.2
11.0 5.4
12.0 5.3
13.1 5.0
16.8 5.0
19.0 5.1
18.2 5.1
14.0 5.0
12.1 4.9
11.9 5.0
12.1 5.1
12.1 5.2
11.8 5.4
11.9 5.3
11.9 5.2
10.6 5.0
10.8 4.8
11.0 4.8
11.4
w
1
H-1
ON
-------
TABLE B-2. Continued. Additional Hydrocarbon Results of Wet Outlet Samples at Plant A
Date Time File Name
8/19/97 7:54 WOUAMB01
8:04 OUTSP001
Run 1 8:09 OUTSP102
8:13 OUTSP103
9:17 18190009
9:20 18190010
9:22 18190011
9:24 18190012
9:26 18190013
9:28 18190014
9:30 18190015
9:32 18190016
9:34 18190017
9:37 18190018
9:39 18190019
9:41 18190020
9:43 18190021
9:45 18190022
9:47 18190023
9:49 18190024
9:52 18190025
9:54 18190026
9:56 18190027
9:58 18190028
10:00 18190029
10:04 18190030
10:06 18190031
10:09 18190032
10:11 18190033
10:13 18190034
10:15 18190035
10:17 18190036
10:19 18190037
10:21 18190038
12:05 18190070
12:07 18190071
12:09 18190072
12:11 18190073
12:13 18190074
12:16 18190075
12:18 18190076
12:20 18190077
12:22 18190078
12:24 18190079
12:26 18190080
12:28 18190081
12:30 18190082
12:33 18190083
12:35 18190084
12:37 18190085
12:39 18190086
12:41 18190087
8/19/97 13:22 18190106
13:24 18190107
Runl 13:26 18190108
13:28 18190109
13:30 18190110
13:32 18190111
13:34 18190112
13:37 18190113
13:41 18190114
Butane
ppm A
15.2
16.5
16.4
17.2
20.1
20.2
20.3
20.2
19.7
20.2
20.3
19.2
19.8
20.1
19.8
20.3
19.2
19.6
19.8
19.1
18.9
19.1
19.5
19.2
19.6
19.5
39.8 2.6
31.7 1.9
17.8
18.9
19.0
19.2
18.8
19.1
13.3
13.8
13.6
13.6
13.9
14.1
13.7
13.1
12.9
13.0
12.8
13.2
13.3
13.0
13.5
13.6
13.5
13.7
13.2
13.4
13.4
13.5
13.3
13.1
13.4
13.3
13.2
2-Methyl-l-
pentene
ppm A
0.7
9.6
9.6
10.0
11.6
11.6
11.7
11.6
11.4
11.6
11.7
11.1
11.4
11.6
11.4
11.7
11.0
11.3
11.4
11.0
10.9
11.0
11.3
11.1
11.3
11.2
8.6
6.5
11.1
10.9
11.0
11.1
10.8
11.0
8.4
8.7
8.5
8.5
8.7
8.9
8.6
8.2
8.1
8.2
8.0
8.2
8.4
8.1
8.4
8.5
8.5
8.6
8.3
8.4
8.4
8.4
8.4
8.2
8.4
8.4
8.3
2-Methyl-2-butene
ppm A
0.9
19.5
19.4
20.3
24.7
24.9
25.0
24.9
24.3
24.9
24.9
23.6
24.3
24.7
24.3
25.0
23.5
24.1
24.4
23.5
23.3
23.5
24.0
23.6
24.1
23.9
16.3
12.2
21.2
23.2
23.4
23.6
23.1
23.4
15.9
16.5
16.2
16.3
16.6
16.9
16.4
15.7
15.4
15.6
15.3
15.7
15.9
15.5
16.1
16.2
16.2
16.4
15.8
16.0
16.1
16.1
15.9
15.7
16.0
15.9
15.7
B-17
-------
TABLE B-2. Continued. Wet Sample Outlet Results
Date Time File Name
13:43 18190115
8/19/97 13:45 18190116
13:47 18190117
Run 1
14:33 OUTSP104
14:38 OUTSP105
Average — >
Butane
ppm A
13.2
13.0
13.1
11.3
11.2
1.1
2-Methyl-l-
pentene
ppm A
8.3
8.1
8.2
6.9
6.8
2-Methyl-2-butene
ppm A
15.7
15.5
15.7
12.8
12.6
Date Time File Name
8/20/97 7:47 OUTSP201
7:54 OUTSP202
Run 2 8:00 OUTSP203
9:12 18200019
9:14 18200020
9:16 18200021
9:18 18200022
9:21 18200023
9:23 18200024
9:25 18200025
9:27 18200026
9:29 18200027
9:31 18200028
9:33 18200029
9:36 18200030
9:38 18200031
9:40 18200032
9:42 18200033
9:44 18200034
10:36 18200058
10:38 18200059
10:41 18200060
10:43 18200061
10:45 18200062
10:47 18200063
10:49 18200064
10:51 18200065
10:53 18200066
10:56 18200067
10:58 18200068
11:00 18200069
11:02 18200070
11:04 18200071
11:06 18200072
11:08 18200073
12:05 18200092
12:07 18200093
12:09 18200094
12:11 18200095
12:13 18200096
12:16 18200097
8/20/97 12:18 18200098
12:20 18200099
Run 2 12:22 18200100
12:24 18200101
12:26 18200102
Butane
ppm A
13.8
13.3
13.4
18.2
18.7
18.9
18.7
20.2
21.3
21.6
20.6
19.6
19.3
17.3
14.6
16.3
20.9
20.1
18.5
21.1
22.5
19.7
24.3
21.9
21.6
21.2
21.4
19.0
23.5
20.8
21.1
21.0
19.7
19.9
20.5
21.0
21.2
20.9
20.3
20.4
20.8
20.9
21.3
21.3
21.5
20.6
2-Methyl-l-
pentene
ppm A
8.4
13.2 1.4
8.2
10.5
10.8
10.9
10.8
11.6
12.3
12.4
11.8
11.3
11.1
10.0
9.2
9.3 1.8
12.0
11.6
10.6
12.1
12.9
39.8
13.7
12.6
12.4
12.2
12.3
38.5
13.3
12.0
12.1
12.1
11.3
11.5
11.8
12.1
12.2
12.0
11.7
11.8
12.0
12.0
12.3
12.3
12.4
12.9
2-Methyl-2-butenc
ppm A
15.7
15.7
15.2
22.3
23.0
23.3
23.0
24.9
26.2
26.5
25.3
24.2
23.7
21.3
17.5
20.0
25.7
24.7
22.7
25.9
27.7
28.9
26.9
26.9
26.6
26.0
26.3
27.9
26.1
25.5
26.0
25.8
24.2
24.4
25.2
25.8
26.1
25.7
25.0
25.1
25.5
25.6
26.2
26.2
26.4
24.6
-------
TABLE B-2. Continued. Wet Sample Outlet Results
Date Time File Name
12:28 18200103
8/20/97 12:30 18200104
12:33 18200105
Run 2 12:35 18200106
12:37 18200107
12:39 18200108
Average — >
Butane
ppm A
19.5
19.6
19.9
19.9
20.3
20.1
2-Methyl-l-
pentene
ppm A
11.3
11.3
11.5
11.5
12.7
11.6
0.7
2-Methyl-2-butene
ppm A
24.0
24.1
24.5
24.4
24.2
24.7
Date Time File Name
8/20/97 13:41 OUTUN301
13:49 OUTUN302
Run 3 14:01 OUTUN303
15:13 18200140
15:15 18200141
15:17 18200142
15:19 18200143
15:21 18200144
15:23 18200145
15:25 18200146
15:28 18200147
15:30 18200148
15:32 18200149
15:34 18200150
15:36 18200151
15:38 18200152
15:40 18200153
15:42 18200154
Average — >
Butane
ppm A
11.9
3.0
3.6
16.9
16.9
17.6
18.1
18.2
18.1
18.7
18.6
19.3
19.3
18.6
18.3
17.8
18.2
19.1
2-Methyl-l-
pentene
ppm A
7.5
1.9
2.2
10.6
10.6
11.0
11.4
11.4
11.4
11.7
11.7
12.1
12.1
11.7
11.5
11.2
11.4
12.0
2-Methyl-2-butene
ppm A
14.2
1.6 1.0
1.1
20.2
20.1
21.0
21.7
21.8
21.7
22.4
22.3
23.0
23.0
22.2
21.9
21.3
21.7
22.8
0.1
B-19
-------
TABLE B-2. Continued. Wet Sample Outlet Results
Date Time File Name
8/21/97 7:32 OUTUN401
9:11 18210001
Run 4 9:13 18210002
9:15 18210003
9:17 18210004
9:20 18210005
9:22 18210006
9:24 18210007
9:26 18210008
9:28 18210009
9:30 18210010
9:32 18210011
9:34 18210012
9:37 18210013
9:39 18210014
11:38 18210058
11:40 18210059
11:42 18210060
11:45 18210061
11:47 18210062
11:49 18210063
11:51 18210064
11:54 18210065
11:56 18210066
Average — >
Butane
ppm A
16.6
15.8
16.5
17.4
17.4
16.8
16.7
17.3
17.0
16.1
15.9
16.3
16.2
16.3
16.1
16.5
16.9
17.2
17.6
17.3
17.1
16.5
15.8
15.7
2-Methyl-l-
pentene
ppm A
18.3 1.8
8.1 1.7
8.1 1.8
11.3 1.9
11.4 1.9
10.6 1.8
10.1 1.8
10.3 1.9
10.5 1.9
11.0 1.8
17.4 1.8
16.1 1.8
12.4 1.8
10.2
10.1
10.4
10.6
10.8
11.0
10.9
10.7
10.4
9.9
9.8
6.5
2-Methyl-2-butene
ppm A
20.2
19.3
20.3
21.3
21.3
20.5
20.5
21.2
20.8
19.7
19.4
20.0
19.9
19.5
19.3
19.8
20.2
20.5
21.1
20.7
20.4
19.7
18.9
18.8
B-20
-------
TABLE B-3. FTIR RESULTS OF DRY SAMPLES FROM THE PLANT A BAGHOUSE INLET
Date Time File Name
8/20/97 14:31 18200121
14:34 18200122
Run 3 14:36 18200123
14:38 18200124
14:41 18200125
14:43 18200126
14:45 18200127
14:47 18200128
14:49 18200129
14:51 18200130
14:53 18200131
14:56 18200132
14:58 18200133
15:00 18200134
15:02 18200135
15:04 18200136
15:06 18200137
17:33 INLSP301
17:40 INLSP302
Average — >
Toluene
ppm A
2.3
2.4
2.4
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
35.9 1.5
36.8 1.5
Hexane
ppm A
11.0
11.5
11.8
12.0
12.0
11.9
11.9
11.9
12.0
12.0
11.9
12.0
12.0
12.0
12.1
12.1
12.2
8.2
8.3
Ethylene
ppm A
12.8 0.6
13.5 0.6
13.1 0.6
12.8 0.7
13.1 0.7
12.9 0.7
12.7 0.7
12.4 0.6
12.1 0.6
11.9 0.6
11.7 0.6
11.5 0.6
11.3 0.6
11.3 0.6
10.9 0.6
10.7 0.6
10.5 0.6
9.5 0.5
10.9 0.5
12.8
SF6
ppm A
0.014
0.015
0.015
0.015
0.015
0.015
0.015
0.015
0.015
0.015
0.014
0.014
0.015
0.014
0.014
0.014
0.014
0.657 0.010
0.659 0.010
Methane
ppm A
7.5 .0
7.7 .0
7.6 .0
7.5
7.6
7.4
7.2
7.1
7.0
6.8
6.6
6.7 1.1
6.6 1.1
6.4 1.1
6.4 1.1
6.2 1.1
6.2 1.1
5.9 0.8
6.3 0.8
7.4
SO2
ppm A
52.5 2.6
58.1 2.7
59.1 2.8
60.5 2.8
59.7 2.8
58.6 2.8
57.3 2.8
55.5 2.8
54.0 2.7
52.1 2.7
50.8 2.7
48.8 2.7
47.9 2.7
46.4 2.7
45.4 2.7
43.2 2.7
41.7 2.7
11.0 1.8
13.2 1.8
49.3
CO
ppm A
280.2 29.9
279.2 30.5
277.0 30.7
276.2 31.1
274.6 30.9
276.3 30.9
276.7 30.8
276.8 30.7
275.8 30.9
276.6 30.7
276.8 30.7
277.2 30.7
277.6 30.7
277.1 30.6
277.5 30.6
276.9 30.7
277.3 30.7
218.8 17.7
232.5 18.5
291.4
Formaldehyde
ppm A
4.4 0.9
4.6 1.0
4.6 1.0
4.5 1.0
4.6 1.0
5.3 1.0
6.8 1.0
8.2 1.0
9.6 1.0
11.0 1.0
12.2 1.0
11.4 1.0
12.5 1.0
13.7 1.0
14.7 1.0
15.7 1.0
16.7 1.0
3.8 0.8
4.1 0.8
9.2
03
Date Time File Name
8/21/97 8:17 INLUN401
8:28 INLSP402
Run 4 8:34 INLSP403
11:06 INLUN404
11:13 18210046
11:15 18210047
11:17 18210048
11:19 18210049
11:21 18210050
11:23 18210051
11:25 18210052
11:28 18210053
11:30 18210054
11:32 18210055
Average — >
Toluene
ppm A
4.2 1.4
29.9 1.2
30 3 1.4
2.9
2.6
2.6
2.5
2.6
2.6
2.7
10.8 2.2
12.7 2.3
12.4 2.2
11.7 2.2
8.9
Hexane
ppm A
9.3
7.8
9.1
13.8
12.5
12.3
12.2
12.3
12.6
12.9
13.4
13.6
13.5
13.3
Ethylene
ppm A
9.7 0.6
6.7 0.5
8.3 0.5
13.2 0.8
9.6 0.6
9.8 0.6
10.1 0.6
10.1 0.6
10.3 0.6
17.3 0.7
33.5 0.9
38.0 0.9
37.3 0.9
35.7 0.9
19.5
SF6
ppm A
0.052 0.013
0.568 0.010
0.5*7 0.011
0.020 0.016
0.014
0.014
0.014
0.014
0.014
0.019 0.016
0.030 0.018
0.034 0.019
0.033 0.019
0.032 0.019
Methane
ppm A
6.4 0.8
5.3 0.7
5.9 0.7
7.4 1.2
6.0 1.1
6.1 1.1
6.1 1.1
6.1 1.1
6.1 1.2
8.5 1.2
15.3 1.1
16.8 1.1
16.3 1.1
15.7 1.1
10.1
SO2
ppm A
49.3 2.3
32.0 1.8
31.4 2.0
58.6 3.0
46.1 2.7
45.5 2.6
45.6 2.6
44.9 2.6
43.0 2.7
39.0 2.8
34.3 3.3
34.2 3.5
36.3 3.5
38.4 3.4
45.1
CO
ppm A
212.6 27.7
173.3 20.7
187.2 21.9
266.8 32.6
224.2 28.4
225.7 28.4
229.7 28.5
228.4 28.3
230.1 28.5
289.8 31.5
400.4 37.2
426.7 38.6
425.9 38.3
418.1 37.7
311.3
Formaldehyde
ppm A
2.1 0.8
1.4 0.7
1.7 0.8
4.5 ,1
3.7 .1
3.6 .1
3.6 .0
3.7 .1
3.8 .1
4.0 .2
4.3 .2
5.1 1.2
5.3 1.2
5.4 1.2
4.1
-------
TABLE B-3. Continued. Additional Hydrocarbon Results in Dry Outlet Samples at Plant A
Date Time File Name
8/20/97 14:31 18200121
14:34 18200122
Run 3 14:36 18200123
14:38 18200124
14:41 18200125
14:43 18200126
14:45 18200127
14:47 18200128
14:49 18200129
14:51 18200130
14:53 18200131
14:56 18200132
14:58 18200133
15:00 18200134
15:02 18200135
15:04 18200136
15:06 18200137
17:33 INLSP301
17:40 INLSP302
Average — >
3-Methylpentane
ppm A
2.3
2.4
2.5
0.9
2.5
0.8
0.9 0.8
1.2 0.8
1.3 0.9
1.5 0.9
1.8 0.9
2.3 1.0
3.3 0.9
2.5 1.0
3.7 0.9
4.0 0.9
4.3 0.9
0.9 0.6
1.0 0.6
1.6
Isooctane
ppm A
0.7
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.5
0.5
0.8
Butane
ppm A
2.9
3.1
3.2
3.5
3.2
3.5
3.5
3.5
13.4
3.5
13,3
6.5 3.5
13.4
8.5 3.5
13.5
13.5
13.6
9.2
9.3
0.8
2-Methyl-l-
pentene
ppm A
7.9 0.6
8.3 0.6
8.3 0.6
8.1 0.6
8.3 0.6
8.7 0.6
8.1 1.6
8.7 1.6
9.5 1.6
10.0 1.6
10.6 1,6
7.2 2.0
10.1 1.6
7.7 2.0
11.3 1.7
11.6 1.7
12.1 1.7
5.3 1.2
6.4 1.2
9.4
Heptane
ppm A
4.7
4.9
5.0
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.2
5.2
5.2
3.5
3.5
1-Pentene
ppm A
5.7
6.0
6.1
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.2
6.3
6.3
6.3
4.3
4.3
2-Methyl-2-butene
ppm A
4.6 0.8
5.0 0.9
5.0 0.9
4.9 0.9
5.0 0.9
5.4 0.9
6.3 0.9
7.1 0.9
7.7 0.9
8.5 0.9
9,1 0.9
7.6 0.9
8.4 0.9
8.6 0.9
9.4 0.9
9.9 0.9
10.5 0.9
3.9 0.7
4.6 0.7
7.3
to
to
Date Time File Name
8/21/97 8:17 INLUN401
8:28 INLSP402
Run 4 8:34 INLSP403
11:06 INLUN404
11:13 18210046
11:15 18210047
11:17 18210048
11:19 18210049
11:21 18210050
11:23 18210051
11:25 18210052
11:28 18210053
11:30 18210054
11:32 18210055
Average — >
3-Methylpentane
ppm A
0.7
0.5
0.6
1.0
1.1 0.9
1.1 0.9
1.1 0.9
1.1 0.9
1.2 0.9
1.0
2.8
2.8
2.8
2.8
0.4
Isooctane
ppm A
0.6
0.5
0.6
0.9
0.8
0.8
0.8
0.8
0.8
0.8
0.5 0.3
0.6 0.3
0.6 0.3
0.5 0.3
0.2
Butane
ppm A
2.6
8.8
10.1
4.1
3.7
3.7
3.6
3.7
3.9
4.1
14.9
15.2
15.0
5.8
2-Methyl-l-
pentene
ppm A
1.6
1.1
1.2
8.3 0.7
6.1 1.7
6.2 1.7
6.3 1.7
6.9 1.7
7.6 1.8
12.1 0.7
3.6
5.5
5.4
3.6
4.1
Heptane
ppm A
6.7 0.1
4.7 0.1
4.6 0.1
5.9
5.3
5.2
5.2
5.2
5.4
5.5
8.9 0.5
9.6 0.5
9.6 0.5
9.7 0.5
4.3
1-Pentene
ppm A
4.8
4.1
4.7
7.1
6.5
6.4
6.3
6.4
6.5
6.7
8.9 1.6
10.8 1.7
10.7 1.7
9.9 1.6
3.1
2-Methyl-2-butene
ppm A
0.8
0.7
0.8
5.2 1.1
5.2 1.0
5.3 1.0
5.3 1.0
6.1 1.0
6.9 1.0
8.3 1.1
1.5
1.4
1.4
1.4
3.3
-------
TABLE B-4. FTIR RESULTS IN DRY SAMPLES FROM THE PLANT A BAGHOUSE OUTLET
Date Time File Name
8/20/97 14:05 18200109
14:08 18200110
Run 3 14:10 18200111
14:12 18200112
14:14 18200113
14:16 18200114
14:18 18200115
14:20 18200116
14:22 18200117
14:25 18200118
16:25 18200174
16:27 18200175
16:29 18200176
16:32 18200177
16:34 18200178
16:36 18200179
16:38 18200180
16:40 18200181
16:42 18200182
16:44 18200183
16:46 18200184
16:49 18200185
16:51 18200186
16:53 18200187
17:05 OUTSP304
17:16 OUTSP305
17:23 OUTSP306
Average — >
Toluene
ppm A
2.6
2.5
2.4
6.6 1.9
2.6
2.6
2.6
2.6
2.6
2.6
3.1
2.7
2.6
2.6
2.7
2.7
2.6
2.6
2.6
2.6
2.6
2.7
2.7
2.7
31.8 1.8
34.3 1.7
33.8 1.7
0.3
Hexane
ppm A
12.3
3.7 0.2
11.4
11.2
12.3
12.5
12.5
12.5
12.5
12.3
5.4 0.2
5.5 0.2
12.7
5.0 0.2
4.5 0.2
5.0 0.2
5.0 0.2
4.9 0.2
5.1 0.2
5.2 0.2
5.1 0.2
4.7 0.2
4.8 0.2
4.7 0.2
11.1
9.6
9.4
2.5
Ethylene
ppm A
8.8 0.6
8.8 0.6
10.1 0.6
12.8 0.6
12.1 0.6
11.4 0.6
10.4 0.6
10.9 0.6
10.8 0.6
11.2 0.6
12.0 0.7
12.0 0.6
10.9 0.6
10.1 0.6
9.5 0.6
10.5 0.6
10.4 0.6
10.2 0.6
10.6 0.6
10.7 0.6
10.4 0.6
9.8 0.6
10.1 0.6
9.9 0.6
5.9 0.6
10.3 0.5
9.4 0.5
11.0
SF6
ppm A
0.014
0.014
0.013
0.013
0.014
0.014
0.014
0.014
0.014
0.014
0.016
0.015
0.014
0.015
0.015
0.015
0.014
0.014
0.014
0.014
0.014
0.015
0.015
0.015
0.614 0.012
0.605 0.011
0.602 0.011
Methane
ppm A
7.0 1.1
7.0 1.0
6.9 1.0
8.5 1.0
9.5
8.0
7.6
7.7
7.5
7.4
8.5 .2
8.2 .1
7.0 .1
9.3 .1
11.8 .1
9.1 .1
7.9 .0
7.4 .0
7.6 .0
7.5 .0
7.7 1.0
8.3 1.1
7.9 1.1
8.0 1.1
5.9 1.0
6.4 0.9
6.1 0.9
8.3
S02
ppm A
51.0 2.6
49.6 2.6
43.2 2.4
39.3 2.5
48.1 2.7
47.8 2.6
48.6 2.6
48.0 2.6
47.8 2.7
46.5 2.6
49.1 2.9
52.9 2.7
55.6 2.7
58.5 2.7
65.3 2.8
60.3 2.7
56.3 2.7
54.2 2.6
52.7 2.7
51.8 2.7
53.7 2.7
59.3 2.8
60.1 2.8
60.6 2.8
34.2 2.2
23.3 2.1
19.9 2.0
51.5
CO
ppm A
270.5 28.7
247.9 27.0
236.8 24.7
296.8 27.6
372.4 32.8
281.0 28.4
276.5 28.5
266.2 27.8
266.4 27.9
255.0 27.0
295.6 30.6
281.9 29.2
265.8 28.4
378.9 33.8
514.9 40.6
366.2 33.1
296.5 29.6
264.1 28.1
252.6 27.7
251.1 27.6
275.5 28.9
336.0 32.3
291.3 30.2
301.3 30.9
230.2 22.4
230.7 20.4
219.3 19.3
307.0
Formaldehyde
ppm A
2.9 0.9
2.7 0.9
2.9 0.9
5.1 .0
3.9 .0
3.0 .0
3.0 .0
3.0 .0
4.0 .0
4.0 .0
5.1 .2
4.2 .0
5.1 .0
3.9 .0
3.9 .0
3.7 .0
3.6 .0
3.5 .0
3.5 .0
3.5 .0
3.6 1.0
3.7 1.0
3.7 1.0
3.7 1.0
4.2 1.0
4.3 0.9
4.2 0.9
4.1
Cd
to
-------
TABLE B-4. Continued. Dry Outlet Samle Results
Date Time File Name
8/21/97 7:39 OUTLN402
7:54 OLTSP403
Run 4 8:02 OUTSP404
8:09 OUTSP405
10:28 OUTUN406
10:32 18210032
10:35 18210033
10:37 18210034
8/21/97 10:40 18210035
10:42 18210036
Run 4 10:44 18210037
10:46 18210038
10:48 18210039
10:50 18210040
10:52 18210041
10:54 18210042
10:57 18210043
10:59 18210044
Average — >
Toluene
ppm A
7.5 1.6
32.8 1.2
33.1 1.3
34.0 1.4
2.6
10.9 2.2
19.6 2.6
16.0 2.4
15.1 2.4
15.0 2.3
15.3 2.4
16.2 2.4
16.6 2.5
16.9 2.5
10.3 2.4
2.8
2.8
2.7
12.4
Hexane
ppm A
10.0
7.8
7.9
8.4
12.3
13.4
13.7
13.5
13.4
13.2
13.3
13.5
13.7
13.7
13.5
13.4
13.4
13.2
Ethylene
ppm A
10.5 0.5
10.5 0.5
10.8 0.5
12.3 0.5
12.6 0.6
30.7 0.8
27.8 0.8
24.9 0.8
23.8 0.7
23.6 0.7
23.8 0.7
24.7 0.8
25.9 0.8
26.2 0.8
20.3 0.7
15.0 0.7
13.3 0.6
11.7 0.6
21.2
SF6
ppm A
0.012
0.589 0.010
0.588 0.010
0.590 0.011
0.014
0.025 0.017
0.025 0.017
0.023 0.016
0.022 0.016
0.022 0.016
0.021 0.016
0.023 0.016
0.023 0.017
0.024 0.017
0.020 0.016
0.018 0.015
0.015
0.014
Methane
ppm A
7.3 0.9
6.6 0.7
6.9 0.7
7.4 0.7
7.5 1.1
14.6 1.1
14.1 1.4
13.0 1.3
12.5 1.2
12.3 1.2
12.4 1.2
12.8 1.3
13.3 1.3
13.3 1.3
10.0 1.3
8.1 1.2
7.5 1.2
6.9 1.2
11.4
Sulfur Dioxide
ppm A
38.4 2.3
23.5 1.8
24.3 1.8
30.8 1.9
25.2 2.5
26.2 3.1
33.6 3.0
34.8 2.9
34.5 2.9
33.7 2.9
33.3 2.9
32.5 2.9
32.9 3.0
33.9 3.0
36.2 2.9
36.9 2.7
37.9 2.7
32.5 2.6
35.1
Carbon Monoxk
ppm A
202.1 25.7
205.0 22.1
211.9 22.3
222.1 23.8
242.3 26.8
367.8 34.7
353.4 34.2
337.2 33.2
330.2 32.7
329.9 32.5
331.1 32.6
338.2 33.1
345.5 33.6
347.5 33.6
305.8 31.3
266.4 29.3
249.4 28.4
228.9 26.4
320.3
leFormaldehyde
ppm A
4.6 0.9
1.2 0.6
1.6 0.7
1.9 0.7
3.3 1.0
4.4 1.2
6.3 1.4
7.0 1.3
6.8 1.3
6.9 1.3
6.9 1.3
7.1 1.3
7.1 1.3
7.2 1.3
6.4 1.3
4.2 1.2
4.0 1.1
3.7 1.1
5.3
w
-------
TABLE B-4. Continued. Dry Outlet Sample Results, Additional Hydrocarbon Compounds.
Date Time File Name
8/20/97 14:05 18200109
14:08 18200110
Run3 14:10 18200111
14:12 18200112
14:14 18200113
14:16 18200114
14:18 18200115
14:20 18200116
14:22 18200117
14:25 18200118
16:25 18200174
16:27 18200175
16:29 18200176
16:32 18200177
16:34 18200178
16:36 18200179
16:38 18200180
16:40 18200181
16:42 18200182
16:44 18200183
16:46 18200184
16:49 18200185
16:51 18200186
16:53 18200187
17:05 OUTSP304
17:16 OUTSP305
17:23 OUTSP306
Average — >
3-Methylpentane
ppm A
2.6
2.5
2.4
2.3
2.6
2.6
2.6
2.6
2.6
2.6
1.1
1.0
0.9
0.9
1.0
0.9
0.9
0.9
0.9
0.9
0.9
1.0
1.0
1.0
0.8
0.9 0.7
0.9 0.7
0.1
Isooctane
ppm A
0.8
0.8
0.7
0.7
0.8
0.8
0.8
0.8
0.8
0.8
1.0
0.8
0.8
0.8
0.9
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.9
0.7
0.6
0.6
Butane
ppm A
3.0
2.9
2.8
3.0
3.3
3.1
3.1
3.1
3.3
3.3
4.1
3.6
3.7
3.5
3.6
3.6
3.5
3.4
3.5
3.5
3.5
3.6
3.6
3.7
3.2
10.8
10.5
2-Methyl-l-
pentene
ppm A
5.5 0.6
1.8
6.6 0.6
8.2 0.6
6.9 0.6
7.0 0.6
6.6 0.6
6.9 0.6
6.7 0.6
6.7 0.6
2.6
2.3
7.0 0.7
2.3
2.3
2.3
2.2
2.2
2.2
2.2
2.2
2.3
2.3
2.3
4.4 0.6
5.7 1.3
5.3 1.3
3.5
Heptane
ppm A
5.2
5.1
4.8
4.8
5.2
5.3
5.3
5.3
5.4
5.3
6.3
5.5
5.4
5.4
5.6
5.5
5.3
5.3
5.3
5.3
5.4
5.5
5.6
5.6
4.7
4.1
4.0
1-Pentene
ppm A
6.3
6.1
5.9
5.8
6.4
6.5
6.4
6.5
6.5
6.4
7.7
6.7
6.6
6.6
6.8
6.6
6.5
6.4
6.4
6.5
6.5
6.7
6.7
6.8
5.7
5.0
4.9
2-Methyl-2-
butene
ppm A
2.1 0.9
0.9
2.6 0.8
3.6 0.9
3.8 0.9
3.0 0.9
2.6 0.9
2.8 0.9
4.0 1.0
3.9 0.9
1.3
1.1
4.3 1.0
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
1.1
2.3 0.9
3.7 0.8
3.7 0.8
1.8
Cd
-------
TABLE B-4. Continued. Dry Outlet Sample Results, Additional Hydrocarbon Compounds.
Date Time File Name
8/21/97 7:39 OUTDN402
7:54 OUTSP403
Run 4 8:02 OUTSP404
8:09 OUTSP405
10:28 OUTUN406
10:32 18210032
10:35 18210033
10:37 18210034
10:40 18210035
10:42 18210036
10:44 18210037
10:46 18210038
10:48 18210039
10:50 18210040
10:52 18210041
10:54 18210042
10:57 18210043
10:59 18210044
Average — >
3-Methylpentane
ppm A
2.1
0.9 0.6
0.5
0.6
2.6
2.8
2.9
2.8
2.8
2.7
2.8
2.8
2.9
2.9
2.8
2.8
2.8
1.0
.01
Isooctane
ppm A
0.7
0.5
0.5
0.5
0.8
0.5 0.3
0.5
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.3
Butane
ppm A
11.1
8.8
8.8
9.4
3.3
15.0
33.7 0.8
5.9 3.8
5.6 3.8
5.7 3.7
5.6 3.8
5.9 3.9
6.0 3.9
6.1 3.9
3.9
3.7
3.7
4.0
4.4
2-Methyl-l-
pentene
ppm A
8.0 0.3
4.7 1.1
1.7 0.6
1.4 0.7
8.1 0.6
5.4
5.5
14.9 2.3
14.2 2.2
14.2 2.2
14.7 2.2
15.4 2.3
15.7 2.3
16.0 2.3
13.4 0.8
10.2 0.7
9.3 0.7
9.0 0.7
9.9
Heptane
ppm A
4.2
3.3
3.5 0.3
4.5 0.3
5.3
7.4 0.5
5.8
5.8
5.7
5.6
5.7
5.8
5.9
5.8
5.8
5.7
5.7
5.6
1.2
1-Pentene
ppm A
5.2
4.1
4.1
4.4
6.4
8.9 1.6
7.1
7.0
6.9
6.8
6.9
7.0
7.1
7.1
7.0
6.9
6.9
6.8
0.5
2-Methyl-2-
butene
ppm A
2.9
2.0 0.6
0.7
0.7
4.9 1.0
3.9
4.0
3.9
3.9
3.8
3.9
3.9
4.0
4.0
6.6 1.1
6.6 1.1
6.2 1.1
6.0 1.1
2.0
-------
The graphs on the following pages show concentration-versus-time plots of the FTIR results
presented in Tables B-1 to B-4. Each graph presents results from a single Test Run and for a
single analyte. Run 1 occurred on 8/19/97, Runs 2 and 3 on 8/20/97 and Run 4 occured on
8/21/97. The run times are indicated on each graph.
Each result is plotted as a graphical symbol and the results are connected by a solid line. Four
different symbols represent the wet and dry inlet results and the wet and dry outlet results. The
connecting lines are broken whenever there was a switch between test locations or type of sample
treatment (i.e., wet or dry sample). Taken together, the semi-continuous results on each graph
show the emission pattern for each analyte for that Run.
The samples spiked with toluene gas standard are indicated on the graph. The spiked results were
not included in the toluene run averages, because an unspiked toluene concentration was not
detected in the spiked samples.
B-27
-------
B-28
-------
ouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• Toluene inlet
• Toluene outlet
45
35
Spiked Samples
Spiked Samples
25 -
15
-5
Spiked Samples
I
•HI
7:30 8:30
9:30 10:30
11:30
Time
12:30 13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run! 8/20/97
• Toluene inlet
• Toluene outlet
45
- Spiked Samples
35
W
i
U)
o
25
15 -
Spiked Samples
-5
' 1HE1
7:30
8:30
9:30 10:30
Time
11:30
12:30
-------
OJ fe
*- £4
45 -
35
25
15
5 -
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• Toluene inlet
• Toluene (dry) inlet
• Toluene outlet
• Toluene (dry) outlet
Spiked Samples
Spiked Samples
N
13:30 14:30 15:30 16:30
17:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• Toluene inlet
• Toluene (dry) inlet
• Toluene outlet
• Toluene (dry) outlet
U)
to
a-
a-
45
35
25 -
15 -
Spiked Samples
O OOQQCX
-5
7:30
8:30
9:30
10:30
11:30
Time
-------
16
14
12
10
8
6
4
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• Hexane inlet
• Hexane outlet
0H
0H
\
0
-2
a BCD
7:30
8:30
9:30
10:30 11:30
Time
12:30
13:30
14:30
-------
16
14
12
10
8
6 H
4
2
0
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• Hexane inlet
• Hexane outlet
w
-2
7:30
rr* "••"•••"»*•'
8:30
9:30
10:30
11:30
12:30
Time
-------
18
16
14
12
10
8
6
4
2
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• Hexane inlet
• Hexane (dry) inlet
• Hexane outlet
• Hexane (dry) outlet
cc
-2
13:30
»•»• •*•»<•> •
14:30
15:30
16:30
«—X X—X
17:30
Time
-------
20
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• Hexane inlet
• Hexane (dry) inlet
• Hexane outlet
• Hexane (dry) outlet
CO
18 -
16
14 -
12
10 -
8
6
4
2 -
0 -p x-
-2
7:30
-»—K—X X
8:30
9:30
10:30
11:30
Time
-------
Dd
30
26 -
22
18
14
10
2
-2
7:30
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• Ethylene inlet
• Ethylene outlet
8:30
9:30
10:30
11:30
Time
12:30
13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• Ethylene inlet
• Ethylene outlet
to
I
u>
oo
30
26
22
18
14
10
-2
7:30
8:30
9:30
10:30
11:30
12:30
Time
-------
18
16
14
12
10
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• Ethylene inlet
• Ethylene (dry) inlet
• Ethylene outlet
• Ethylene (dry) outlet
£
6
4 -
2
o H
-2
13:30
•MM MMMM•
14:30
15:30
16:30
17:30
Time
-------
CO
±
O
40
35
30
25
£ 20
15
10
5 -
x
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• Ethylene inlet
• Ethylene (dry) inlet
• Ethylene outlet
• Ethylene (dry) outlet
V
7:30
8:30
9:30
10:30
11:30
Time
-------
35
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
Methane inlet
• Methane outlet
od
0L|
30
25
20
15
10
7:30
8:30
9:30
10:30 11:30
Time
12:30
13:30
14:30
-------
w
.U
to
240
200
\60
no
80
40
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• Methane inlet
• Methane outlet
7:30
8:30
9:30
10:30
11:30
12:30
Time
-------
30
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• Methane inlet
• Methane (dry) inlet
• Methane outlet
• Methane (dry) outlet
25 -
20
15 -
10 -
13:30
14:30
15:30
16:30
17:30
Time
-------
30
25
20
15
10
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• Methane inlet
• Methane (dry) inlet
• Methane outlet
• Methane (dry) outlet
&ya
7:30
8:30
9:30
10:30
11:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• SO2 inlet
SO2 outlet
90
70
50
30
10
-10
7:30 8:30 9:30 10:30
11:30
Time
12:30 13:30 14:30
-------
150
130
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• SO2 inlet
SO2 outlet
» a
^ £
OS CM
110
90
70
50
30
10
-10
7:30
8:30
9:30
10:30
11:30
12:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
SO2 inlet
• SO2 (dry) inlet
SO2 outlet
SO2 (dry) outlet
75
65 -
55
45
35 -
25 -
15 -
5 -
«•••»«••••••»•
13:30
14:30
15:30
16:30
17:30
Time
-------
W
.U
oo
5
CM
CM
70
60
50 -
40
30
20
10
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
SO2 inlet
SQ2 (dry) inlet
• SO2 outlet
• SO2 (dry) outlet
7:30
8:30
9:30
10:30
11:30
Time
-------
w
I
PH
350
300
250
200
150
100
50
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• CO inlet
• CO outlet
7:30
8:30
9:30
10:30
11:30
Time
12:30
13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• CO inlet
- CO outlet
PH
PH
2000
1600
1200
800 -
400 -
7:30
8:30
9:30
10:30
11:30
12:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• CO inlet
• CO (dry) inlet
- CO outlet
• CO (dry) outlet
500
400
300
200
100
0
13
30
14:30
15:30
16:30
17:30
Time
-------
500
400
300
w
i
<-n
to
PM
PM
200
100
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• CO inlet
• CO (dry) inlet
• CO outlet
• CO (dry) outlet
V
V
7:30
8:30
9:30
10:30
11:30
Time
-------
35
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 1 8/19/97
• Formaldehyde inlet
• Formaldehyde outlet
Cfl
30
25
20
15
0
-5
7:30
8:30
9:30
10:30 11:30
Time
12:30
13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 2 8/20/97
• Formaldehyde inlet
• Formaldehyde outlet
w
1
PH
18
14
10
2 -
-2
ill iiiim iiiiij-i
7:30
8:30
9:30
10:30
11:30
12:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 3 8/20/97
• Formaldehyde inlet
• Formaldehyde (dry) inlet
• Formaldehyde outlet
• Formaldehyde (dry) outlet
22
18
14
10
-2
>•••• MMMM
*-*
13:30
14:30
15:30
16:30
17:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time.
Run 4 8/21/97
• Formaldehyde inlet
• Formaldehyde (dry) inlet
• Formaldehyde outlet
• Formaldehyde (dry) outlet
130
18
14 -
10
a,
a,
\p
#>
-2
7:30
8:30
9:30
10:30
11:30
Time
-------
TABLE B-5. PLANT A "METHOD DETECTION LIMIT" ESTIMATES
Compound
Acetaldehyde
ienzene
Carbonyl Sulfide
VIethylchloride
Methylchloroform
[,1-dichloroethane
Toluene
1, 3 -butadiene
vlethanol
Cumene
ithylbenzene
-fexane
Vtethylene chloride
^opionaldehyde
Styrene
1,1,2,2-
retrachloroethane
)-Xylene
a-Xylene
n-Xylene
2,2,4-Trimethylpentane
Jormaldehyde
SU1
0.13
0.14
0.00
0.37
0.04
0.04
0.33
0.18
0.05
0.11
0.31
0.05
0.10
0.04
0.23
0.02
0.18
0.15
0.37
0.02
0.15
MDL2
(ppm)
0.38
0.41
0.01
1.12
0.13
0.11
0.98
0.53
0.14
0.32
0.93
0.16
0.30
0.13
0.69
0.06
0.55
0.44
1.12
0.02
0.46
1 SU = "Statistical Uncertainty" From Proposed ASTM FTIR Method
2 The "Method Detection Limit" from ASTM FTIR method.
Table B-5 contains results from the "Method Detection Limit" calculation procedure suggested
in the September, 1998 version of an FTIR method proposed by the American Society of Testing
and Materials (ASTM).
The procedure, briefly, (1) prepares at least 7 spectra with zero analyte concentrations, but with
interference absorbance equivalent to the sample spectra, (2) runs the analytical program on these
spectra, (3) calculates the standard deviation ("statistical uncertainty," SU) in the results, and (4)
multiplies the SU results by 3 to give the "Method Detection Limit" (MDL)
B-57
-------
The spectra in step 1 were prepared in the laboratory as recommended. Seven independent
spectra of water vapor (approximately 20 percent), at 124°C, and 753 torr, were measured in a
heated cell at a path length of 10 meters. Seven independent spectra of carbon dioxide (CO2, 20
percent) were also measured using the same instrument conditions. Seven interference spectra
were generated by combining pairs of water vapor and CO2 spectra. The CO2 concentrations in
the interference spectra were higher than in the sample spectra. The interference spectra moisture
concentrations were higher than or equivalent to the sample spectra moisture concentrations.
The laboratory moisture and CO2 spectra were measured at 1.0 cm"1. The spectra were then
deresolved to 2.0 cm"1 to match the sampling resolution used at the Plant A test. The deresolution
procedure followed Appendix K of the EPA FTIR Protocol and involved truncating and Fourier
processing the original interfere grams.
In step 2 the interference spectra were analyzed using the computer program that was used in the
sample analyses. The computer program used reference spectra of moisture and CO2 that were
measured in the laboratory independently of the interference moisture and CO2 spectra.
The analytical program calculated concentration results for the target analytes in Table B-5. The
concentrations were all near zero and the estimated MDL values were determined from the
precision of the concentration results for each analyte. The sample results in Tables B-1 to B-4
were prepared using the same computer program, but the program was constrained to measure
only the detected analytes.
The calculation of the "SU" value for a single analyte is given in equation B-l.
SU
= \
i (n-D
o^I) 5 ((
^ - r )2
"i ^M ^
where;
SU = The "Statistical Uncertainty."
N = The number of spectra analyzed.
Q = The concentration result from the 1th spectrum. In this procedure the
absolute value of the results was used in equation B-1.
CM = The average of the concentration results for all of the spectra.
n = The number of measurements. In this case n = 14.
The values "MDL" reported in Table B-5 are equivalent to 3 * SU for each of the target analytes.
B-58
-------
B-2 FOR FIELD DATA RECORDS
B-59
-------
B-60
-------
PROJEC 4701-08-02
PLANT: A
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/19/97
BAROM ETRIC:
OPERATOR: T.Geyer
SAMPLE
TIME
7:20
7:30
7:38
8:30
10:10
10:15
11:09
14:47
15:00
15:17
FILE
NAME
BK60819A
CTS0819A
1530819A
SF60819A
spike 001
BKG0819
Spike 002
CTS0819C
PATH
20 passes
20 passes
20 passes
20 passes
N2 flowing, Background 2 Ipm
Ethylene 20 ppm
Toluene 121 ppm
SF6 4 ppm
spike flow direct to cell-SF6 0.99 1pm,
Toluene 0.98 1pm
Gulick sending propane to outlet spike
Propane spike off
flowing N2 through cell
spike direct to cell SF6 1 .05 1pm, Toluene 0.99 1pm
spike direct to cell SF6 1 .04 1pm, Toluene 0.99 1pm
20 ppm ethylene
NUMBER
SCANS
500
250
250
250
250
500
RES
(cm-1)
2
2
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
130 C
130 C
PRESSURE
759.2
762
762
762
762
763 torr
760.5
BKC
A
A
A
A
B
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
B
NOTES
03
ON
-------
PROJEC 4701-08-02
PLANT: A
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/20/97
BAROMETRIC:
OPERATOR:
T. Gever
SAMPLE
TIME
7:00
7:10.
7:35
13:20
17:54
18:05
FILE
NAME
BKG0820A
CTS0820A
BKG0820B
BKG0820C
Spike 301
CTS0820B
PATH
20 passes
20 passes
20 passes
20 passes
Good leak checks at inlet and outlet
Good leak check cell & juniper line
N2 flowing through cell
20 ppm ethylene through cell
N2 through cell - getting a large ice band
Dectector holding aprox 8 hrs
N2 through cell
spike to cell - SF= 1 .90 1pm, Tol= 1 .95 1pm
20 ppm ethylene to cell
NUMBER
SCANS
500
250
250
500
250
250
RES
(cm-1)
2
2
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
130 C
130 C
PRESSURE
756.8
756.4
756.4
758.4
751.2
757.3
BKC
A
A
C
APOD
NB/med
NB/med
NB/med
NB/med
C
NB/med
NOTES
ON
to
-------
PROJECT NO. 4701-08-02
PLANT: A
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/21/97
BAROMETRIC:,
OPERATOR:
T. G«yer
SAMPLE
TIME
7:15
7:25
8:42 - 8:47
8:57
9:07
12:16
12:22
12:28
12:43
FILE
NAME
BKG0821A
CTS0821A
Spike 401
BKG0821B
N2CON401
ICE00401
BKG0821C
CTS0821B
N2CON402
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
N2 flowing through cell
20 ppm Ethylene through cell
Spike direct to cell — SF6 = 1 96 Ipm, Toluene = 1 9
N2 flowing through cell
NUMBER
SCANS
500
250
250
500
RES
(cm-1)
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
PRESSURE
752.3
752.3
752.3
BKG
A
A
All times are approximately 5 minutes last compared to THC, FI1K computer & manual sampling times
N2 through the condenser
N2 through cell to measure ice band
N2 through cell
20 ppm ethylene through cell
Nitrogen through the condenser flowing @ 5 Ipm
250
250
500
250
250
2
2
2
2
2
130 C
130 C
130 C
130 C
130 C '
754.4
754.3
754.3
755.8
B
C
C
C
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
CO
Os
UJ
-------
PROJECT NO.
PLANT:
4701-08-02
A
FTIR FIELD DATA FORM
(FTIR Sampling Data)
DATE:
8/19/97
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
7:45
7:58
• 8:00
8:10
8:17
8:25
8:37
8:43
9:02
9:05
9:10
9:12
9:17
9:22
9:19
9:50
10:27
10:28
10:45
11:16
FILE
NAME
W1NAMB01
WOUAMB01
OUTSP001
OUTSP102
OUTSP103
INLSP101
INLSP102
INLSP103
18190001
18190007
18190009
18190038
18190040
18190046
PATH
20 passes
20 passes
20 passes
Ambient air through inlet sample line
Ambient sample from outlet
NUMBER
SCANS
RES
(cm-1)
2
Spike w/toluene & SF6, SF6 flow = 0.99, toluene flow = 0.99
Spike w/toluene & SF6, SF6 flow = 0.99, toluene flow = 0.99
Spike w/toluene & SF6, SF6 flow = 0.99, toluene flow = 0.99
Took out glass wool plug at inlet to get better flow
Spike to inlet, SF6 = 1 .06 1pm, Toluene flow = 0.98 Ipm,
Participate is restricting and changing inlet flow.
SF6 flow became erratic around end of scan |
SF6 flow = 0.99 Ipm, toluene flow = 0.98 1pm
SF6 flow = 0.99 1pm, toluene flow = 0.98 1pm
Start sampling at inlet
First spectrum collected at inlet.
Started manual run.
Last spectrum at inlet
Switched to outlet sample.
First outlet spectrum
Manual run restarted
CELL
TEMP(F)
130
130
130
130
130
130
Putting tip in inlet probe so probe can be pointed away from flow to relieve cloggin
Last outlet spectrum
Switched to inlet sample
first good inlet spectrum
250
Using elbow on end of probe oriented with the flow
Flow is still dropping at the inlet
Last good inlet spectrum
Started filling with inlet
2
130
SPIKED/
UNSPIKED
U
U
s
s
s
s
g.
U
SAMPLE
COND.
SAMPLE
FLOW
21pm
2 1pm
3 1pm
3 Ipm
4 1pm
2 Ipm
7 Ipm
4 1pm
BKC
A
A
A
A
A
CO
-------
PROJECT NO.
PLANT:
4701-08-02
A
FTIR FIELD DATA FORM
(FTIR Sampling Data)
DATE:
8/19/97
BAROMETRIC:
OPERATOR:
T. Ceyer
SAMPLE
TIME
11:20
12:02
12:06
12:10
12:46
12:49
12:53
13:21
13:23
13:25
13:54
13:56
13:58
14:16
14:20
14:25-14:30
14.32
14:36-14:40
14:42-14:45
1443
15:10
15:18
15:15
FILE
NAME
18190047
18190067
18190070
18190047
18190090
18190103
1819106
1819117
1819120
18190128
INLSP104
INLSP105
OUTSP104
OUTSP105
CTS0819B
CTS0819C
PATH
20 passes
Started data collect
NUMBER
SCANS
250
Last good inlet sample. Flow is holding steady.
Started filling with outlet sample
First good outlet spectrum
Last good outlet spectrum
Started filling with inlet sample
First good inlet spectrum
Last good inlet spectrum
Switched to outlet
First good outlet sample
Last good spectrum at outlet
Started fill at inlet
First good outlet spectrum
250
250
250
250
250
Spike on to inlet SF6 at 1 .06 1pm, Toluene at 1 .00 1pm
Last good unspiked inlet sample
Spiked batch sample - inlet
Spiked batch sample - inlet
Spike to outlet
Spike to outlet location, SF6 at 1 .04 Ipm,
Toluene at 0.98 1pm.
SF6 = 1 .04 1pm, Toluene = 0.99 1pm
<20 ppm Ethylene direct to cell>
-^Contaminated with propane
250
250
250
Good leak check outlet, inlet -2 Ipm leak under vacuum.
RES
(cm-1)
2
2
2
2
2
2
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
130 C
130 C
130
130
130
130
SPIKED/
UNSPIKED
U
U
U
U
U
U
s
s
s
U
SAMPLE
COND.
SAMPLE
FLOW
4.5 1pm
4.5 1pm
4.5 Ipm
4.5 1pm, good flow
5 1pm
5 Ipm
5 Ipm
5 Ipm
5 Ipm
5 1pm
2 1pm
BKC
B
B
B
B
B
B
B
B
B
B
B
to
cbs
-------
PROJECT NO. 4701-08-02
PLANT: A
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/20/97
SAMPLE
TIME
7:45
7:49-7:54
7:55-8:00
8:02
8:08-8:12
8:13-8:17
8:18-8:23
8:28
8:22
8:32
8:37
9:12
9:20
9:37
9:45
9:54
10:36
10:38
10:42
11:14
11.19
11:30
12:04
12:06
12:09
12:45
13:44
13:49-13:53
FILE
NAME
OUTSP201
OUTSP202
OUTSP203
INLSP201
INLSP202
INLSP203
Spike201
18200001
18200006
18200019
18200034
18200037
18200055
18200058
18200073
18200074
18200089
18200092
182000108
OUTUN301
OUTUN302
PATH
20 passes
20 passes
20 passes
Spike to outlet
Spike to outlet sample
Spike to outlet sample
Spike to outlet sample
NUMBER
SCANS
250
250
250
RES
<«-•)
2
2
2
inlet spike valve was also on spike during above samples
spike to inlet
spike to inlet
spike to inlet
Spike direct to cell
Manual runs started
Start sampling at inlet
first spectrum
Last good inlet spectrum
Started outlet sample
first good outlet sample
250
250
250
250
250
2
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
130 C
130 C
130 C
130 C
Noticed that process conveyor had stopped. But all sampling continues.
Received report that process is warming
Conveyor moving again
last good outlet spectrum
Started inlet sample to cell
first good inlet spectrum
Last good inlet sample
started outlet sample to cell
first good sample outlet
last good outlet sample .
Started inlet sample to cell
first good inlet spectrum
Last good inlet spectrum
Started outlet sample to cell
First good outlet spectrum
250
250
250
250
250
end of Run #2, last good outlet sample
H/W from outlet
Condensor sample/ outlet
250
250
2
2
2
2
2
2
2
130 C
130 C
130 C
130 C
130 C
130 C
130 C
SPIKED/
UNSPIKED
S
S
S
S
S
S
u
u
u
u
u
u
u
u
u
SAMPLE
COND.
Cond
SAMPLE
FLOW
SF6 = 1.95 1pm, toluene = 2.011pm
SF6 = 1 .96 Ipm, toluene = 1 .99 1pm
SF6 = I 96 1pm, toluene = 1 .99 Ipm
SF6 = 1 .96 Ipm, toluene = 1 .99 Ipm
SF6 = 1 .85 Ipm, toluene = 1 .96 Ipm
5 1pm through cell
4 1pm
5 Ipm
5 Ipm
5 1pm
4.5 1pm
4.5 Ipm
5 1pm
4.5 Ipm
BKG
B
B
B
B
B
B
B
B
C
C
ON
ON
-------
PROJECT NO.
PLANT:
4701-08-02
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/20/97
OPERATOR:
SAMPLE
TIME
14:05
14:08
14:30
14:36
15:06
15:19
15:19
15:50
15:52
15:54
15:23
15:28
15:58
17:01
17:08-17:11
17:20
17:26
17:29
17:36-17:39
17:44
FILE
NAME
OUTUN303
18200109
18200118
18200121
18200137
18200140
18200140
18200154
18200157
18200170
18200174
18200187
OUTSP304
OUTSP305
OUTSP306
FNLSP301
INLSP302
PATH
20 passes
NUMBER
SCANS
RES
<«-!)
CELL
TEMP(F)
Condenser same sample after flow through @ 5 1pm through cell
Start continuous collection at outlet
First good outlet condenser sample
Last good outlet condenser sample
first good inlet sample
final outlet sample
first good outlet sample
Outlet first sample
Last outlet sample
Started filling with inlet
first inlet sample
last inlet sample
first outlet sample
last outlet sample
Started spike to outlet
Spiked outlet through condenser
250
250
250
250
250
250
250
250
250
Spike spectrum to outlet after spike flow
Spike on to inlet
Spike to inlet
Spike to inlet through condenser
End of run #3
250
250
2
2
2
2
2
2
2
2
2
2
130 C
130 C
130 C
130 C
130 C
130 C
130 C
130 C
130 C
SPIKED/
UNSPIKED
u
u
u
u
u
u
u
s
s
SAMPLE
COND.
Cond
Cond
Cond
Cond
Cond
Cond
H/W
H/W
H/W
H/W
H/W
Cond
Cond
Cond
Cond
Cond
Cond
Cond
SAMPLE
FLOW
755.3 torr
5 Ipm
5 1pm
4 1pm
41pm
4.5 1pm
5 1pm
5 1pm
5 1pm
51pm
SF6 flow = 1 .99 , toluene = 1 .95 1pm
5 1pm
SF6 flow = 1 95, toluene = 1 .93 1pm
SF6 = 2.00, toluene = 1 .93 Ipm
SF6 = 2 00, toluene = 1 .93 Ipm
BKG
C
C
C
C
C
C
C
C
C
Cd
o\
-------
PROJECT NO. 4701-08-02
PLANT: A
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/21/97
OPERATOR: T. Gever
SAMPLE
TIME
7:32-7:36
7:41
7:40
7:50
7:55-8:00
8:02 .-8:03
8:10-8:15
8:15
8:17-8:22
8:24
8:29 - 8:34
8:36
8:42
9:10
9:14
9:45
9:47
9:52
10:22
10:30-10:35
10:33
11:02
11:02-11:06
11:14
11:39
11:40
12:02
12:16
FILE
NAME
OUTUN401
OUTUN402
OUTSP403
OUTSP404
OUTSP405
INLUN401
INLSP402
INLSP403
18210001
18210014
18210016
18210031
OUTUN406
182100032
18210044
INLUN404
18210046
18210055
18210058
18210066
ICE00401
PATH
20 passes
20 passes
Outlet
Outlet - Condenser
Manual run start
Spike on to outlet
Spiked outlet sample
Spiked outlet sample
Spiked outlet sample
NUMBER
SCANS
250
250
250
250
250
RES
(cm-l)
2
2
2
2
2
CELL
TEMP(F)
130 C
130 C
130 C
130 C
130 C
SPIKED/
UNSPIKED
u
u
s
s
s
SAMPLE
COND.
H/W
Cond
Cond
Cond
Cond
All times are approximately 5 minutes fast relative to the other times (eg. computer, THC, manual)
Spike off to outlet
Unspiked inlet condenser
Spike on to inlet
Spiked inlet sample
Spiked inlet sample
Ethylene is present in samples so will s
Spike off to inlet
Start sample from outlet
first outlet sample
last outlet sample
Started to fill with inlet sample
first full inlet sample
last inlet sample
Started outlet to cell
first automated outlet spectrum
Last condenser sample outlet
Inlet sample
Start automated inlet sample
last inlet sample
Started fill with outlet,
first full outlet sample
End of run
N2 in cell to measure ice band
250
250
250
2
2
2
130 C
130 C
130 C
pike with ethylene @ REA
250
250
250
250
250
250
250
250
250
250
2
2
2
2
2
2
2
2
2
130 C
130 C
130 C
130 C
130 C
130 C
130 C
130 C
130 C
u
s
s
*
u
u
u
u
u
u
u
u
u
Cond
Cond
Cond
H/W
H/W
H/W
Cond
Cond
Cond
Cond
Cond
Cond
H/W
SAMPLE
FLOW
5 1pm
5 1pm
F6 = 1 .96, toluene = 1 .98 1pm (5 Ip
SF6 = 1 .95, toluene = 1 .97 Ipm
SF6 = 1.95, toluene = 1.971pm
5 1pm
SF6 = 1.96, toluene = 1.97
SF6 = 1.96, toluene = 1.97
5 1pm
5 1pm
5 1pm
5 Ipm
5 Ipm
4.5 1pm
4.5 1pm
4.5 Ipm
5 1pm
BKG
A
A
A
A
B
B
B
B
B
B
B
B
B
td
&
oo
-------
Data Sheet: FTIR Background and Calibration Spectra: EPA Work Assignment 4-
, ,.
P*--|'^ o'^^l
Cd
Date
y/
Time
TW
File Name
oo
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Path
•2.0^
Location/Notes
<^_&dfy
Jfa+J
VZ:
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tfscans
Res(cm-i;
^^_
T^F
Cell temp (F)
32_
Pressure
2
BKG
~W~
>t:
/H
•5T-
\
-------
Data Sheet: FT1R Samples:
EPA Work Assignment 4-
Oo^v-
Date
Sample time
Filename | Path
Location/Notes
ffscans
T:
Rea (cm\1> Cell Temp (F)
7i
Spk/Unsp I Sample Cond
Sample Flow
BKG
to
130
j^
-------
f Data Sheet: FTIR Samples:
EPA Work Assignment 4-
Date
Sample time
File name
Path
U>ca»
tion/Notes
#scans
Res (cm- 1)i Cell Temp (F)
Spk/Unsp
Sample Cond
Sample Flow
BKG
W'lLrt'As
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-------
Data Sheel: FTIR Samples:
EPA Work Assignment 4-
Date
6{fr
Sample time
Filename
Path
LocaUon/Nolas'
#scans
cm-1> Cell Temp (F)
Spk/Unsp j Sample Cond
Sample Flow
BKG
*r-
4*
*+~
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to
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LL.
-------
Dala Sheci: FPIR Background ami Calibration Spectra: EPA Work Assignment 4-
Date/;
Time
File Name
Path
Location/Notes
(cm-1)
Cell temp (F)
Pressure I BKG
Apod
^fV
0
^
_djui
-------
Duia Sheet: FTIR Samples:
EPA Work Assignment 4-
ale Sample lima
WL
File name 1 Palh
Location/Noles
•scans
Res (cm 1): Cell Temp (F)
Spk/Unsp
Sample Cond.
Sample Flow
BKG
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-------
Uaia Slicei: FT1R Samples:
EPA Work Assignment 4-
L/
03
-------
a.1
Data Sheet: FTIR Samples:
EPA Work Assignment 4-
ample
time
File name
Path
Location/Notes
tfscans
es (cm-1): Cell Temp (Fj
Spk/Unsp
Sample Cond.
Samle Flow
BKG
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-------
Data Sheet: FTIR Samples:
EPA Work Assignment 4-
-------
Data Sheet: FTIR Background and Calibration Spectra: EPA Work Assignment 4-
Date
Time
File Name
Path
Location/Notes
ffscans
Res (cm-1)
Cell temp (F)
Pressure
BKG
Apod
Jf-o
V»o
. 3
A
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-------
Data Sheer FTIR Samples:
EPA Work Assignment 4-
-i
\o
-------
B-80
-------
B-3 FUR FLOW AND TEMPERATURE READINGS
B-81
-------
B-82
-------
Cd
oo
FTIR FIELD DATA FORM
PROJECT NO. SW-Zy PLANT:
INLET
CLOCK
TIME
1 O /o
11*0
DELTA P
IN. 1120
,<*<
0
STACK
TEMP.
PROBE
TEMP.
PROBE BOX
TEMP.
DATE:
BAROMETRIC:
OUTLET
CLOCK
TIME
n*
DELTA P
IN. 1120
o.vt
0,31
STACK
TEMP.
PROBE
TEMP.
273
27-7
PROBE BOX
TEMP.
OPER «TOR
-------
FTIR FIELD DATA FORM
PROJECT NO. y^H '2 «y PLANT:
W
i
oo
INLET
CLOCK
TIME
DELTA P
IN. H20
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01 03 93 16:38 ®213 786 0320 SCOTT
Scott Specialty Gases
6141 BASTON ROAD PO BOX 310
Prom": PLUMSTBADVILLE PA 18949-0310
Phona: 215-766-8861 Pax: 215-766-2070
CERTIFICATE OF ANALYSIS
— — — -_*_w_**«««««*ww • ww«vw^«*w*«w««vvw*-» — — «A**««««WWVV_ — V«K«B««*VV«..__.. * • « _ •
MIDWEST RESEARCH PROJECT #: 01-88514-001
TOM GEYER P0#: 029257
425 VOLKER BLVD ITEM #: 01021951 1AL
DATE: 3/25/97
KANSAS CITY MO 64110
CYLINDER #: ALM023940 ANALYTICAL ACCURACY: -t--lV
FILL PRESSURE: 2000 PSIG
BLEND TYPE : GRAVIMETRIC MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT CONG MQLBS _IMQLBSJ_
BTHYLENB 20. PPM 20.01 PPM
NITROGEN BALANCE BALANCE
ANALYST:
(r? ^
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01 05 93 18:33 ®213 766 0320 SCOTT
Scott Specialty Gases
] 003
6141 BASTON ROAD PO BOX 310
PLDMSTBADVILLE PA 18949-0310
Phone: 215-766-8861 Fax: 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH PROJECT #: 01-89796-005
DAVE ALBURTY, X1525 PO#: 029872
425 VOLKER BLVD ITBM #: 01023912 4AL
DATE: 5/13/97
KANSAS CITY MO 64110
CYLINDER #: ALM057730 ANALYTICAL ACCURACY: +/- 2%
FILL PRESSURE: 2000 PSIG
BLEND TYPE : CERTIFIED MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT CONG MOLES (MOIRES)
TOLUBNB 120. PPM 121. PPM
AIR BALANCE BALANCE
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GENYA
OUHH«M.NC SOUTH muwfiei.0. NJ 8«W«1*. OWT**«0 . PVUMSTSaOVlUfi. M : P*»»I»U.TX SHSWOBO.
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SCOTT SPECIALTY
Scott Specialty Gases
1290 COMBERMERE STREET
TROY
Phone: 248-589-2950
C E R T I F I
MI 48083
GATE
O F
Fax: 248-589-2134
ANALYSIS
MIDWEST RESEARCH
MELISSA TUCKER; # 026075
425 VOLKER BLVD
KANSAS CITY
PROJECT #: 05-97263-002
P0#: 026075
ITEM #: 05023822 4A
DATE: 6/03/96
MO 64110
CYLINDER #: A7853 |
FILL PRESSURE: 2000 PSI
ANALYTICAL ACCURACY: + /- 2%
PRODUCT EXPIRATION: 6/03/1997
BLEND TYPE : CERTIFIED iJtASTER GAS
COMPONENT
SULFUR HBXAFLUORIDB-
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(MOLES)
4.
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4.01
PPM
BALANCE
CERTIFIED MASTER GAS
-------
C-8
-------
01 .'05/98
16:38
88 0320
SCOTT
Scott Specialty Gases, Inc.
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
PO BOX 310
PA 18949-0310
CERTIFICATE
0 F
Fax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
PO#014952
425 VOLKER BLVD
KANSAS CITY
MO 64110
PROJECT #: 01-59176-001
P0#: 014952
ITEM #: 01021912 2AL
DATE: 7/20/94
CYLINDER #: ALM020008
BLEND TYPE : ACUBLEND MASTER GAS
COMPONENT
ETHYLENE
AIR
ANALYTICAL ACCURACY:
REQUESTED GAS
CONC MOLES
ANALYSIS
(MOLES1
100.
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BAL
101.
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iVICH
i-MfeMONi-.CA SAN BERNARDINO, CA UONGMONT, CO TROY. Ml CHICAGO. IL SAflNlA, ONTARIO AVON LAKE, OH HOUSTON.ru
BATON ROUSE. LA MARIETTA.
-------
C-10
-------
Scott Specialty Gases
bftlpped
From:
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
\
CERTIFICATE
PO BOX 310
PA 18949-0310
0 F
Fax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
GARY NC 27511
PROJECT #: 01-08674-002
P0#: A035678
ITEM #: 01021912 2AL
DATE: 9/22/98
CYLINDER #: ALM020008
FILL PRESSURE: 400 PSIG
ANALYTICAL ACCURACY: +\-2%
BLEND TYPE
COMPONENT
ETHYLENE
AIR
ACUBLEND MASTER GAS
REQUESTED GAS
CONC MOLES
ANALYSIS
(MOLES)
100 .
PPM
BALANCE
101.
PPM
BALANCE
ANALYST:
C-ll
-------
C-12
-------
C-2 ENVIRON1CS MASS FLOW METER CALIBRATIONS
C-13
-------
C-14
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf ft: 1, Description: AIR , Size: 10000. SCCM, K-factcr: 1.0
SERIAL *
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceable
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of £1? ( C) and a pressure of 29.92 in.Hg (760Torr )
5
10
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Calibration data was last saved on
Verified by:
Friday 03 January 97
at 16 :22:00
Date :
C-15
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 2, Description: AIR
SERIAL
Size: 10000, SCCM, K-factor: 1.0
This flow controller was calibrated using
Primary Flow Standard Calibration System.
dry air at a temperature of &Z,F ( C) and
5 %
10 *
20 %
30 %
40 *
50 *
50 %
70 *
80 %
90 *
100%
Set F
500.0
1000 .0
2000 .0
3000 .0
4000.0
5000.0
6000 .0
7000.0
8000 .0
9000.0
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CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
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a Sierra Cal Bench(TM), a traceable
This calibration is referenced to
a pressure of 29.92 in.Hg (760Torr )
True Flew
510.51 CCM
1021 .4 CCM
2046
3074
4103
5136
6156
7182
8203
9219
.9
.8
.8
.6
.8
.5
.3
.5
10233
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last saved on
Friday 03 January 97
at 17:09:00
Verified by:._
e: / - J - 97
C-16
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 3, Description: AIR
SERIAL
Size: 1000.0 SCCM, K-faccor: 1.0
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceable
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of gWF ( _ C ) and a pressure of 23.92 in.Hg ( 760Torr )
True Flew
5 9s
10 *
20 %
30 *
40 X
50 *
50 %
70 *
80 *
90 *
100*
Set F
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300.0
400. 0
500.0
600.0
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900 .0
1000 .0
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CCM
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50 .
101
204
306
408
510
611
713
816
913
515
.84
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.67
.82
.43
.44
.59
.61
.19
1021 .3
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last saved on
Friday 03 January 97
at 17:55:00
Verified by:.
Data: /
C-17
-------
ENYIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf *
Description: AIR
Size: 100.0
SCCM, K-factor: 1.0
This flaw controller was calibrated using a Sierra Cal BenchCTM), a traceable
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of jZf ( C) and a pressure of 29.92 in.Hg (760Torr)
5 X
10 X
20 X
30 X
40 X
50 X
60 X
70 X
80 X
90 X
100X
Set F
5 .0
10.0
20 .0
30 .0
40.0
50 .0
50 .0
70.0
80.0
90 .0
100.0
1 ow
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
True F:
5 .236
10.
20.
30.
40.
50.
60 .
70 .
80.
91 .
101
269
434
524
606
636
683
779
917
035
.12
Low
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last savod on
Friday 03 January 9'
at 19:11 : 00
Verified by:
Date :_/
- 97
C-18
-------
APPENDIX D
TEST METHODS AND HC1 VALIDATION PAPER
-------
-------
D-l EPA METHOD 320
D-l
-------
D-2
-------
Appendix A of part 63 is amended by adding, in numerical
order, Methods 320 and 321 to read as follows:
Appendix A to Part 63-Test Methods
*****
TEST METHOD 320
MEASUREMENT OF VAPOI PHASE ORGANIC AND INORGANIC EMISSIONS
BY EXTRACTIVE FOURIER TRANSFORM INFRARED (FTII) SPECTROSCOPY
1.0 Introduction.
Persons unfamiliar with basic elements of FTIR
spectroscopy should not attempt to use this method. This
method describes sampling and analytical procedures for
extractive emission measurements using Fourier transform
infrared (FTIR) spectroscopy. Detailed analytical
procedures for interpreting infrared spectra are described
in the "Protocol for the Use of Extractive Fourier Transform
Infrared (FTIR) Spectrometry in Analyses of Gaseous
Emissions from Stationary Sources," hereafter referred to as
the "Protocol." Definitions no.t' given in this method are
given in appendix A of the Protocol. References to specific
sections in the Protocol are made throughout this Method.
For additional information refer to references 1 and 2, and
other EPA reports, which describe the use of FTIR
spectrometry in specific field measurement applications and
validation tests. The sampling procedure described here is
D-3
-------
extractive. Flue gas is extracted through a heated gas
transport and handling system. For some sources, sample
conditioning systems may be applicable. Some examples are
given in this method. Note: sample conditioning systems
may be used providing the method validation requirements in
Sections 9.2 and 13.0 of this method are met.
1.1 Scope and Applicability.
1.1.1 Analytes. Analytes include hazardous air pollutants
(HAPs) for which EPA reference spectra have been developed.
Other compounds can also be measured with this method if
reference spectra are prepared according.to section 4.6 of
the protocol.
1.1.2 Applicability. This method applies to the analysis
of vapor phase organic or inorganic compounds which absorb
energy in the mid-infrared spectral region, about 400 to
4000 cm"1 (25 to 2.5 um). This method is used to determine
compound-specific concentrations in a multi-component vapor
phase sample, which is contained in a closed-path gas cell.
Spectra of samples are collected using double beam infrared
absorption spectroscopy. A computer program is used to
analyze spectra and report compound concentrations.
1.2 Method Range and Sensitivity. Analytical range and
sensitivity depend on the frequency-dependent analyte
absorptivity, instrument configuration, data collection
parameters, and gas stream composition. Instrument factors
D-4
-------
include: (a) spectral resolution, (b) interferometer signal
averaging time, (c) detector sensitivity 'and response, and
(d) absorption path length.
1.2.1 For any optical configuration the analytical range is
between the absorbance values of about .01 (infrared
transmittance relative to the background = 0.98) and 1.0 (T
= 0.1). (For absorbance > 1.0 the relation between
absorbance and concentration may not be linear.)
1.2.2 The concentrations associated with this absorbance
range depend primarily on the cell path length and the
sample temperature. An analyte absorbance greater than 1.0,
can be lowered by decreasing the optical path length.
Analyte absorbance increases with a longer path length.
Analyte detection also depends on the presence of other
species exhibiting absorbance in the same analytical region.
Additionally, the estimated lower absorbance (A) limit (A =
0.01) depends on the root mean square deviation (RMSD) noise
in the analytical region.
1.2.3 The concentration range of this method is determined
by the choice of optical configuration.
1.2.3.1 The absorbance for a given concentration can be
decreased by decreasing the path length or by diluting the
sample. There is no practical upper limit to the
measurement range.
1.2.3.2 The analyte absorbance for a given concentration
D-5
-------
may be increased by increasing the cell path length or (to
some extent) using a higher resolution. Both modifications
also cause a corresponding increased absorbance for all
compounds in the sample, and a decrease in the signal
throughput. For this reason the practical lower detection
range (quantitation limit) usually depends on sample
characteristics such as moisture content of the gas, the
presence of other interferants, and losses in the sampling
system.
1.3 Sensitivity. The limit of sensitivity for an optical
configuration and integration time is determined using
appendix D of the Protocol: Minimum Analyte Uncertainty,
(MAU). The MAU depends on the RMSD noise in an analytical
region, and on the absorptivity of the analyte in the same
region.
1.4 Data Quality. Data quality shall be determined by
executing Protocol pre-test procedures in appendices B to H
of the protocol and post-test procedures in appendices I and
J of the protocol.
1.4.1 Measurement objectives shall be established by the
choice of detection limit (DLL) and analytical uncertainty
(AUi) for each analyte.
1.4.2 An instrumental configuration shall be selected. An
estimate of gas composition shall be made based on previous
test data, data from a similar source or information
D-6
-------
gathered in a pre-test site survey. Spectral interferants
shall be identified using the selected DLi and AUt and band
areas from reference spectra and interferant spectra. The
baseline noise of the system shall be measured in each
analytical region to determine the MAU of the instrument
configuration for each analyte and interferant (MIUJ .
1.4.3 Data quality for the application shall be determined,
in part, by measuring the RMS (root mean square) noise level
in each analytical spectral region (appendix C of the
Protocol). The EMS noise is defined as the RMSD of the
absorbance values in an analytical region from the mean
absorbance value in the region.
1.4.4 The MAU is the minimum analyte concentration for
which the AU; can be maintained; if the measured analyte
concentration is less than MAUif then data quality are
unacceptable.
2.0 Summary of Method.
2.1 Principle. References 4 through 7 provide background
material on infrared spectroscopy and quantitative analysis.
A summary is given in this section.
2.1.1 Infrared absorption spectroscopy is performed by
directing an infrared beam through a sample to a detector.
The frequency-dependent infrared absorbance of the sample is
measured by comparing this detector signal (single beam
spectrum) to a signal obtained without a sample in the beam
D-7
-------
path (background).
2.1.2 Most molecules absorb infrared radiation and the
absorbance occurs in a characteristic and reproducible
pattern. The infrared spectrum measures fundamental
molecular properties and a compound can be identified from
its infrared spectrum alone.
2.1.3 Within constraints, there is a linear relationship
between infrared absorption and compound concentration. If
this frequency dependent relationship (absorptivity) is
known (measured), it can be used to determine compound
concentration in a sample mixture.
2.1.4 Absorptivity is measured by preparing, in the
laboratory, standard samples of compounds at known
concentrations and measuring the FTIR "reference spectra" of
these standard samples. These "reference spectra" are then
used in sample analysis: (1) compounds are detected by
matching sample absorbance bands with bands in reference
spectra, and (2) concentrations are measured by comparing
sample band intensities with reference band intensities.
2.1.5 This method is self-validating provided that the
results meet the performance requirement of the QA spike in
sections 8.6.2 and 9.0 of this method, and results from a
previous method validation study support the use of this
method in the application.
2.2 Sampling and Analysis. In extractive sampling a probe
D-8
-------
assembly and pump are used to extract gas from the exhaust
of the affected source and transport the sample to the FTIR
gas cell. Typically, the sampling apparatus is similar to
that used for single-component continuous emission monitor
(GEM) measurements.
2.2.1 The digitized infrared spectrum of the sample in the
FTIR gas cell is measured and stored on a computer.
Absorbance band intensities in the spectrum are related to
sample concentrations by what is commonly referred to as
Beer's Law.
A. = at b c. (1)
where:
AL = absorbance at a given frequency of the ith sample
component.
at = absorption coefficient (absorptivity) of the ith
sample component.
b = path length of the cell.
GJ. = concentration of the ith sample component.
2.2.2 Analyte spiking is used for quality assurance (QA).
In this procedure (section 8.6.2 of this method) an analyte
is spiked into the gas stream at the back end of the sample
probe. Analyte concentrations in the spiked samples are
compared to analyte concentrations in unspiked samples.
D-9
-------
Since the concentration of the spike is known, this
procedure can be used to determine if the sampling system is
removing the spiked analyte(s) from the sample stream.
2.3 Reference Spectra Availability. Reference spectra of
over 100 HAPs are available in the EPA FTIR spectral library
on the EMTIC (Emission Measurement Technical Information
Center) computer bulletin board service and at internet
address http://info.amold.af.mil/epa/welcome.htm.
Reference spectra for HAPs, or other analytes, may also be
prepared according to section 4.6 of the Protocol.
2.4 Operator Requirements. The FTIR analyst shall be
trained in setting up the instrumentation, verifying the
instrument is functioning properly, and performing routine
maintenance. The analyst must evaluate the initial sample
spectra to determine if the sample matrix is consistent with
pre-test assumptions and if the instrument configuration is
suitable. The analyst must be able to modify the instrument
configuration, if necessary.
2.4.1 The spectral analysis shall be supervised by someone
familiar with EPA FTIR Protocol procedures.
2.4.2 A technician trained in instrumental test methods is
qualified to install and operate the sampling system. This
includes installing the probe and heated line assembly,
operating the analyte spike system, and performing moisture
and flow measurements.
D-10
-------
3.0 Definitions.
See appendix A of the Protocol for definitions relating
to infrared spectroscopy. Additional definitions are given
in sections 3.1 through 3.29.
3.1 Analyte. A compound that this method is used to
measure. The term "target analyte" is also used. This
method is multi-component and a number of analytes can be
targeted for a test.
3.2 Reference Spectrum. Infrared spectrum of an analyte
prepared under controlled, documented, and reproducible
laboratory conditions according to procedures in section 4.6
of the Protocol. A library of reference spectra is used to
measure analytes in gas samples.
3.3 Standard Spectrum. A spectrum that has been prepared
from a reference spectrum through a (documented)
mathematical operation. A common example is de-resolving of
reference spectra to lower-resolution standard spectra
(Protocol, appendix K to the addendum of this method).
Standard spectra, prepared by approved, and documented,
procedures can be used as reference spectra for analysis.
3.4 Concentration. In this method concentration is
expressed as a molar concentration, in ppm-meters, or in
(ppm-meters)/K, where K is the absolute temperature
(Kelvin). The latter units allow the direct comparison of
concentrations from systems using different optical
D-ll
-------
configurations or sampling temperatures.
3.5 Interferant. A compound in the sample matrix whose
infrared spectrum overlaps with part of an analyte spectrum.
The most accurate analyte measurements are achieved when
reference spectra of interferants are used in the
quantitative analysis with the analyte reference spectra.
The presence of an interferant can increase the analytical
uncertainty in the measured analyte concentration.
3.6 Gas Cell. A gas containment cell that can be
evacuated. It is equipped with the optical components to
pass the infrared beam through the sample to the detector.
Important cell features include: path length (or range if
variable), temperature range, materials of construction, and
total gas volume.
3.7 Sampling System. Equipment used to extract the sample
from the test location and transport the sample gas to the
FTIR analyzer. This includes sample conditioning systems.
3.8 Sample Analysis. The process of interpreting the
infrared spectra to obtain sample analyte concentrations.
This process is usually automated using a software routine
employing a classical least squares (els), partial least
squares (pis), or K- or P- matrix method.
3.9 One hundred percent line. A double beam transmittance
spectrum obtained by combining two background single beam
spectra. Ideally, this line is equal to 100 percent
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transmittance (or zero absorbance) at every frequency in the
spectrum. Practically, a zero absorbance line is used to
measure the baseline noise in the spectrum.
3.10 Background Deviation. A deviation from 100 percent
transmittance in any region of the 100 percent line.
Deviations greater than ± 5 percent in an analytical region
are unacceptable (absorbance of 0.021 to -0.022). Such
deviations indicate a change in the instrument throughput
relative to the background single beam.
3.11 Batch Sampling. A procedure where spectra of
discreet, static samples are collected. The gas cell is
filled with sample and the cell is isolated. The spectrum
is collected. Finally, the cell is evacuated to prepare for
the next sample.
3.12 Continuous Sampling. A procedure where spectra are
collected while sample gas is flowing through the cell at a
measured rate.
3.13 Sampling resolution. The spectral resolution used to
collect sample spectra.
3.14 Truncation. Limiting the number of interferogram data
points by deleting points farthest from the center burst
(zero path difference, ZPD).
3.15 Zero filling. The addition of points to the
interferogram. The position of each added point is
interpolated from neighboring real data points. Zero
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filling adds no information to the interferogram, but
affects line shapes in the absorbance spectrum (and possibly
analytical results).
3.16 Reference CTS. Calibration Transfer Standard spectra
that were collected with reference spectra.
3.17 CTS Standard. CTS spectrum produced by applying a de-
resolution procedure to a reference CTS.
3.18 Test CTS. CTS spectra collected at the sampling
resolution using the same optical configuration as for
sample spectra. Test spectra help verify the resolution,
temperature and path length of the FTIR system.
3.19 RMSD. Root Mean Square Difference, defined in EPA
FTIR Protocol, appendix A.
3.20 Sensitivity. The noise-limited compound-dependent
detection limit for the FTIR system configuration. This is
estimated by the MAU. It depends on the RMSD in an
analytical region of a zero absorbance line.
3.21 Quantitation Limit. The lower limit of detection for
the FTIR system configuration in the sample spectra. This
is estimated by mathematically subtracting scaled reference
spectra of analytes and interferences from sample spectra,
then measuring the RMSD in an analytical region of the
subtracted spectrum. Since the noise in subtracted sample
spectra may be much greater than in a zero absorbance
spectrum, the quantitation limit is generally much higher
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than the sensitivity. Removing spectral interferences from
the sample or improving the spectral subtraction can lower
the quantitation limit toward (but not below) the
sensitivity.
3.22 Independent Sample. A unique volume of sample gas;
there is no mixing of gas between two consecutive
independent samples. In continuous sampling two independent
samples are separated by at least 5 cell volumes. The
interval between independent measurements depends on the
cell volume and the sample flow rate (through the cell) .
3.23 Measurement. A single spectrum of flue gas contained
in the FTIR cell.
3.24 Run. A run consists of a series of measurements. At
a minimum a run includes 8 independent measurements spaced
over 1 hour.
3.25 Validation. Validation of FTIR measurements is
described in sections 13.0 through 13.4 of this method.
Validation is used to verify the test procedures for
measuring specific analytes at a source. Validation
provides proof that the method works under certain test
conditions.
3.26 Validation Run. A validation run consists of at least
24 measurements of independent samples. Half of the samples
are spiked and half are not spiked. The length of the run
is determined by the interval between independent samples.
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3.27 Screening. Screening is used when there is little or
no available information about a source. The purpose of
screening is to determine what analytes are emitted and to
obtain information about important sample characteristics
such as moisture, temperature, and interferences. Screening
results are semi-quantitative (estimated concentrations) or
qualitative (identification only). Various optical and
sampling configurations may be used. Sample conditioning
systems may be evaluated for their effectiveness in removing
interferences. It is unnecessary to perform a complete run
under any set of sampling conditions. Spiking is not
necessary, but spiking can be a useful screening tool for
evaluating the sampling system, especially if a reactive or
soluble analyte is used for the spike.
3.28 Emissions Test. An FTIR emissions test is performed
according specific sampling and analytical procedures.
These procedures, for the target analytes and the source,
are based on previous screening and validation results.
Emission results are quantitative. A QA spike (sections
8.6.2 and 9.2 of this method) is performed under each set of
sampling conditions using a representative analyte. Flow,
gas temperature and diluent data are recorded concurrently
with the FTIR measurements to provide mass emission rates
for detected compounds.
3.29 Surrogate. A surrogate is a compound that is used in
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a QA spike procedure (section 8.6.2 of this method) to
represent other compounds. The chemical and physical
properties of a surrogate shall be similar to the compounds
it is chosen to represent. Under given sampling conditions,
usually a single sampling factor is of primary concern for
measuring the target analytes: for example, the surrogate
spike results can be representative for analytes that are
more reactive, more soluble, have a lower absorptivity, or
have a lower vapor pressure than the surrogate itself.
4.0 Interferences.
Interferences are divided into two classifications:
analytical and sampling.
4.1 Analytical Interferences. An analytical interference
is a spectral feature that complicates (in extreme cases may
prevent) the analysis of an analyte. Analytical
interferences are classified as background or spectral
interference.
4.1.1 Background Interference. This results from a change
in throughput relative to the single beam background. It is
corrected by collecting a new background and proceeding with
the test. In severe instances the cause must be identified
and corrected. Potential causes include: (1) deposits on
reflective surfaces or transmitting windows, (2) changes in
detector sensitivity, (3) a change in the infrared source
output, or (4) failure in the instrument electronics. In
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routine sampling throughput may degrade over several hours.
Periodically a new background must be collected, but no
other corrective action will be required.
4.1.2 Spectral Interference. This results from the
presence of interfering compound(s) (interferant) in the
sample. Interferant spectral features overlap analyte
spectral features. Any compound with an infrared spectrum,
including analytes, can potentially be an interferant. The
Protocol measures absorbance band overlap in each analytical
region to determine if potential interferants shall be
classified as known interferants (FTIR Protocol, section 4.9
and appendix B). Water vapor and C02 are common spectral
interferants. Both of these compounds have strong infrared
spectra and are present in many sample matrices at high
concentrations relative to analytes. The extent of
interference depends on the (I) interferant concentration,
(2) analyte concentration, and (3) the degree of band
overlap. Choosing an alternate analytical region can
minimize or avoid the spectral interference. For example,
C02 interferes with the analysis of the 670 cm"1 benzene
band. However, benzene can also be measured near 3000 cm"1
(with less sensitivity).
4.2 Sampling System Interferences. These prevent analytes
from reaching the instrument. The analyte spike procedure
is designed to measure sampling system interference, if any.
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4.2.1 Temperature. A temperature that is too low causes
condensation of analytes or water vapor. The materials of
the sampling system and the FTIR gas cell usually set the
upper limit of temperature.
4.2.2 Reactive Species. Anything that reacts with
analytes. Some analytes, like formaldehyde, polymerize at
lower temperatures.
4.2.3 Materials. Poor choice of material for probe, or
sampling line may remove some analytes. For example, HF
reacts with glass components.
4.2.4 Moisture. In addition to being a spectral
interferant, condensed moisture removes soluble compounds.
5.0 Safety.
The hazards of performing this method are those
associated with any stack sampling method and the same
precautions shall be followed. Many HAPs are suspected
carcinogens or present other serious health risks. Exposure
to these compounds should be avoided in all circumstances.
For instructions on the safe handling of any particular
compound, refer to its material safety data sheet. When
using analyte standards, always ensure that gases are
properly vented and that the gas handling system is leak
free. (Always perform a leak check with the system under
maximum vacuum and, again, with the system at greater than
ambient pressure.) Refer to section 8.2 of this method for
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leak check procedures. This method does not address all of
the potential safety risks associated with its use. Anyone
performing this method must follow safety and health
practices consistent with applicable legal requirements and
with prudent practice for each application.
6.0 Equipment and Supplies.
Note: Mention of trade names or specific products does
not constitute endorsement by the Environmental
Protection Agency.
The equipment and supplies are based on the schematic
of a sampling system shown in Figure 1. Either the batch or
continuous sampling procedures may be used with this
sampling system. Alternative sampling configurations may
also be used, provided that the data quality objectives are
met as determined in the post-analysis evaluation. Other
equipment or supplies may be necessary, depending on the
design of the sampling system or the specific target
analytes.
6.1 Sampling Probe. Glass, stainless steel, or other
appropriate material of sufficient length and physical
integrity to sustain heating, prevent adsorption of
analytes, and to transport analytes to the infrared gas
cell. Special materials or configurations may be required
in some applications. For instance, high stack sample
temperatures may require special steel or cooling the probe.
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For very high moisture sources it may be desirable to use a
dilution probe.
6.2 Particulate Filters. A glass wool plug (optional)
inserted at the probe tip (for large particulate removal)
and a filter (required) rated for 99 percent removal
efficiency at 1-micron (e.g., Balston") connected at the
outlet of the heated probe.
6.3 Sampling Line/Heating System. Heated (sufficient to
prevent condensation) stainless steel,
polytetrafluoroethane, or other material inert to the
analytes.
6.4 Gas Distribution Manifold. A heated manifold allowing
the operator to control flows of gas standards and samples
directly to the FTIR system or through sample conditioning
systems. Usually includes heated flow meter, heated valve
for selecting and sending sample to the analyzer, and a by-
pass vent. This is typically constructed of stainless steel
tubing and fittings, and high-temperature valves.
6.5 Stainless Steel Tubing. Type 316, appropriate diameter
(e.g., 3/8 in.) and length for heated connections. Higher
grade stainless may be desirable in some applications.
6.6 Calibration/Analyte Spike Assembly. A three way valve
assembly (or equivalent) to introduce analyte or surrogate
spikes into the sampling system at the outlet of the probe
upstream of the out-of-stack particulate filter and the FTIR
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analytical system.
6.7 Mass Flow Meter (MFM). These are used for measuring
analyte spike flow. The MFM shall be calibrated in the range
of 0 to 5 L/min and be accurate to ± 2 percent (or better)
of the flow meter span.
6.8 Gas Regulators. Appropriate for individual gas
standards.
6.9 Polytetrafluoroethane Tubing. Diameter (e.g., 3/8 in.)
and length suitable to connect cylinder regulators to gas
standard manifold.
6.10 Sample Pump. A leak-free pump (e.g., KNF") , with by-
pass valve, capable of producing a sample flow rate of at
least 10 L/min through 100 ft of sample line. If the pump
is positioned upstream of the distribution manifold and FTIR
system, use a heated pump that is constructed from materials
non-reactive to the analytes. If the pump is located
downstream of the FTIR system, the gas cell sample pressure
will be lower than ambient pressure and it must be recorded
at regular intervals.
6.11 Gas Sample Manifold. Secondary manifold to control
sample flow at the inlet to the FTIR manifold. This is
optional, but includes a by-pass vent and heated rotameter.
6.12 Rotameter. A 0 to 20 L/min rotameter. This meter
need not be calibrated.
6.13 FTIR Analytical System. Spectrometer and detector,
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capable of measuring the analytes to the chosen detection
limit. The system shall include a personal computer with
compatible software allowing automated collection of
spectra.
6.14 FTIR Cell Pump. Required for the batch sampling
technique, capable of evacuating the FTIR cell volume within
2 minutes. The pumping speed shall allow the operator to
obtain 8 sample spectra in 1 hour.
6.15 Absolute Pressure Gauge. Capable of measuring
pressure from 0 to 1000 mmHg to within ± 2.5 mmHg (e.g.,
Baratron") .
6.16 Temperature Gauge. Capable of measuring the cell
temperature to within ± 2°C.
6.17 Sample Conditioning. One option is a condenser
system, which is used for moisture removal. This can be
helpful in the measurement of some analytes. Other sample
conditioning procedures may be devised for the removal of
moisture or other interfering species.
6.17.1 The analyte spike procedure of section 9.2 of this
method, the QA spike procedure of section 8.6.2 of this
method, and the validation procedure of section 13 of this
method demonstrate whether the sample conditioning affects
analyte concentrations. Alternatively, measurements can be
made with two parallel FTIR systems; one measuring
conditioned sample, the other measuring unconditioned
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sample.
6.17.2 Another option is sample dilution. The dilution
factor measurement must be documented and accounted for in
the reported concentrations. An alternative to dilution is
to lower the sensitivity of the FTIR system by decreasing
the cell path length, or to use a short-path cell in
conjunction with a long path cell to measure more than one
concentration range.
7.0 Reagents and Standards.
7.1 Analyte(s) and Tracer Gas. Obtain a certified gas
cylinder mixture containing all of the analyte(s) at
concentrations within ± 2 percent of the emission source
levels (expressed in ppm-meter/K). If practical, the
analyte standard cylinder shall also contain the tracer gas
at a concentration which gives a measurable absorbance at a
dilution factor of at least 10:1. Two ppm SF6 is sufficient
for a path length of 22 meters at 250 °F.
7.2 Calibration Transfer Standard(s). Select the
calibration transfer standards (CTS) according to section
4.5 of the FTIR Protocol. Obtain a National Institute of
Standards and Technology (NIST) traceable gravimetric
standard of the CTS (± 2 percent).
7.3 Reference Spectra. Obtain reference spectra for each
analyte, interferant, surrogate, CTS, and tracer. If EPA
reference spectra are not available, use reference spectra
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prepared according to procedures in section 4.6 of the EPA
FTIR Protocol. '
8.0 Sampling and Analysis Procedure.
Three types of testing can be performed: (1) screening,
(2) emissions test, and (3) validation. Each is defined in
section 3 of this method. Determine the purpose(s) of the
FTIR test. Test requirements include: (a) AUt, DLi, overall
fractional uncertainty, OFUi, maximum expected concentration
(CMAXJ, and t^i for each, (b) potential interferants, (c)
sampling system factors, e.g., minimum absolute cell
pressure, (Pmin), FTIR cell volume (Vss) , estimated sample
absorption pathlength, Ls', estimated sample pressure, Ps' ,
Ts', signal integration time (tss), minimum instrumental
linewidth, MIL, fractional error, and (d) analytical
regions, e.g., m = 1 to M, lower wavenumber position, FLm,
center wavenumber position, FCm/ and upper wavenumber
position, FUm, plus interferants, upper wavenumber position
of the CTS absorption band, FFUm, lower wavenumber position
of the CTS absorption band, FFLm, wavenumber range FNU to
FNL. If necessary, sample and acquire an initial spectrum.
From analysis of this preliminary spectrum determine a
suitable operational path length. Set up the sampling train
as shown in Figure 1 or use an appropriate alternative
configuration. Sections 8.1 through 8.11 of this method
provide guidance on pre-test calculations in the EPA
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protocol, sampling and analytical procedures, and post-test
protocol calculations.
8.1 Pretest Preparations and Evaluations. Using the
procedure in section 4.0 of the FTIR Protocol, determine the
optimum sampling system configuration for measuring the
target analytes. Use available information to make
reasonable assumptions about moisture content and other
interferences.
8.1.1 Analytes. Select the required detection limit (DLJ
and the maximum permissible analytical uncertainty (AUJ for
each analyte (labeled from 1 to i). Estimate, if possible,
the maximum expected concentration for each analyte, CMAXt.
The expected measurement range is fixed by DLi and CMAXi for
each analyte (i).
8.1.2 Potential Interferants. List the potential
interferants. This usually includes water vapor and C02,
but may also include some analytes and other compounds.
8.1.3. Optical Configuration. Choose an optical
configuration that can measure all of the analytes within
the absorbance range of .01 to 1.0 (this may require more
than one path length). Use Protocol sections 4.3 to 4.8 for
guidance in choosing a configuration and measuring CTS.
8.1.4. Fractional Reproducibility Uncertainty (FRUJ . The
FRU is determined for each analyte by comparing CTS spectra
taken before and after the reference spectra were measured.
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The EPA para-xylene reference spectra were collected on
10/31/91 and 11/01/91 with corresponding CTS spectra
"ctslOSla," and "ctsllOlb." The CTS spectra are used to
estimate the reproducibility (FRU) in the system that was
used to collect the references. The FRU must be < AU.
Appendix E of the protocol is used to calculate the FRU from
CTS spectra. Figure 2 plots results for 0.25 cm'1 CTS
spectra in EPA reference library: S3 (ctsllOlb - cts!031a),
and S< [(ctsllOlb + cts!031a)/2]. The RMSD (SRMS) is
calculated in the subtracted baseline, S3, in the
corresponding CTS region from 850 to 1065 cm"1. The area
(BAV) is calculated in the same region of the averaged CTS
spectrum, S4.
8.1.5 Known Interferants. Use appendix B of the EPA FTIR
Protocol.
8.1.6 Calculate the Minimum Analyte Uncertainty, MAU
(section 1.3 of this method discusses MAU and protocol
appendix D gives the MAU procedure). The MAU for each
analyte, i, and each analytical region, m, depends on the
RMS noise.
8.1.7 Analytical Program. See FTIR Protocol, section 4.10.
Prepare computer program based on the chosen analytical
technique. Use as input reference spectra of all target
analytes and expected interferants. Reference spectra of
additional compounds shall also be included in the program
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if their presence (even if transient) in the samples is
considered possible. The program output shall be in ppm (or
ppb) and shall be corrected for differences between the
reference path length, LR, temperature, TR, and pressure, PR,
and the conditions used for collecting the sample spectra.
If sampling is performed at ambient pressure, then any
pressure correction is usually small relative to corrections
for path length and temperature, and may be neglected.
8.2 Leak-check.
8.2.1 Sampling System. A typical FTIR extractive sampling
train is shown in Figure 1. Leak check from the probe tip
to pump outlet as follows: Connect a 0- to 250-mL/min rate
meter (rotameter or bubble meter) to the outlet of the pump.
Close off the inlet to the probe, and record the leak rate.
The leak rate shall be z 200 mL/min.
8.2.2 Analytical System Leak check. Leak check the FTIR
cell under vacuum and under pressure (greater than ambient).
Leak check connecting tubing and inlet manifold under
pressure.
8.2.2.1 For the evacuated sample technique, close the valve
to the FTIR cell, and evacuate the absorption cell to the
minimum absolute pressure Pmln. Close the valve to the pump,
and determine the change in pressure APV after 2 minutes.
8.2.2.2 For both the evacuated sample and purging
techniques, pressurize the system to about 100 mmHg above
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atmospheric pressure. Isolate the pump and determine the
change in pressure APp after 2 minutes.
8.2.2.3 Measure the barometric pressure, Pb in mmHg.
8.2.2.4 Determine the percent leak volume %VL for the
signal integration time tss and for APmax, i.e., the larger of
APV or APP, as follows:
AP
%VL = 50 tss —HZ . (2)
where 50 = 100% divided by the leak-check time of 2 minutes,
8.2.2.5 Leak volumes in excess of 4 percent of the FTIR
system volume Vss are unacceptable.
8.3 Detector Linearity. Once an optical configuration is
chosen, use one of the procedures of sections 8.3.1 through
8.3.3 to verify that the detector response is linear. If
the detector response is not linear, decrease the aperture,
or attenuate the infrared beam. After a change in the
instrument configuration perform a linearity check until it
is demonstrated that the detector response is linear.
8.3.1 Vary the power incident on the detector by modifying
the aperture setting. Measure the background and CTS at
three instrument aperture settings: (1) at the aperture
setting to be used in the testing, (2) at one half this
aperture and (3) at twice the proposed testing aperture.
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Compare the three CTS spectra. CTS band areas shall agree
to within the uncertainty of the cylinder standard and the
RMSD noise in the system. If test aperture is the maximum
aperture, collect CTS spectrum at maximum aperture, then
close the aperture to reduce the IR throughput by half.
Collect a second background and CTS at the smaller aperture
setting and compare the spectra again.
8.3.2 Use neutral density filters to attenuate the infrared
beam. Set up the FTIR system as it will be used in the test
measurements. Collect a CTS spectrum. Use a neutral
density filter to attenuate the infrared beam (either
immediately after the source or the interferometer) to
approximately 1/2 its original intensity. Collect a second
CTS spectrum. Use another filter to attenuate the infrared
beam to approximately 1/4 its original intensity. Collect a
third background and CTS spectrum. Compare the CTS spectra.
CTS band areas shall agree to within the uncertainty of the
cylinder standard and the RMSD noise in the system.
8.3.3 Observe the single beam instrument response in a
frequency region where the detector response is known to be
'zero. Verify that the detector response is "flat" and equal
to zero in these regions.
8.4 Data Storage Requirements. All field test spectra
shall be stored on a computer disk and a second backup copy
must stored on a separate disk. The stored information
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includes sample interferograms, processed absorbance
spectra, background interferograms, CTS sample
interferograms and CTS absorbance spectra. Additionally,
documentation of all sample conditions, instrument settings,
and test records must be recorded on hard copy or on
computer medium. Table 1 gives a sample presentation of
documentation.
8.5 Background Spectrum. Evacuate the gas cell to s 5
mmHg, and fill with dry nitrogen gas to ambient pressure (or
purge the cell with 10 volumes of dry nitrogen). Verify
that no significant amounts of absorbing species (for
example water vapor and C02) are present. Collect a
background spectrum, using a signal averaging period equal
to or greater than the averaging period for the sample
spectra. Assign a unique file name to the background
spectrum. Store two copies of the background interferogram
and processed single-beam spectrum on separate computer
disks (one copy is the back-up).
8.5.1 Interference Spectra. If possible, collect spectra
of known and suspected major interferences using the same
optical system that will be used in the field measurements.
This can be done on-site or earlier. A number of gases,
e.g. C02, S02, CO, NH3, are readily available from cylinder
gas suppliers.
8.5.2 Water vapor spectra can be prepared by the following
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procedure. Fill a sample tube with distilled water.
Evacuate above the sample and remove dissolved gasses by
alternately freezing and thawing the water while evacuating.
Allow water vapor into the FTIR cell, then dilute to
atmospheric pressure with nitrogen or dry air. If
quantitative water spectra are required, follow the
reference spectrum procedure for neat samples (protocol,
section 4.6). Often, interference spectra need not be
quantitative, but for best results the absorbance must be
comparable to the interference absorbance in the sample
spectra.
8.6 Pre-Test Calibrations
8.6.1 Calibration Transfer Standard. Evacuate the gas cell
to $ 5 mmHg absolute pressure, and fill the FTIR cell to
atmospheric pressure with the CTS gas. Alternatively, purge
the cell with 10 cell volumes of CTS gas. (If purge is
used, verify that the CTS concentration in the cell is
stable by collecting two spectra 2 minutes apart as the CTS
gas continues to flow. If the absorbance in the second
spectrum is no greater than in the first, within the
uncertainty of the gas standard, then this can be used as
the CTS spectrum.) Record the spectrum.
8.6.2 QA Spike. This procedure assumes that the method has
been validated for at least some of the target analytes at
the source. For emissions testing perform a QA spike. Use
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a certified standard, if possible, of an analyte, which has
been validated at the source. One analyte standard can
serve as a QA surrogate for other analytes which are less
reactive or less soluble than the standard. Perform the
spike procedure of section 9.2 of this method. Record
spectra of at least three independent (section 3.22 of this
method) spiked samples. Calculate the spiked component of
the analyte concentration. If the average spiked
concentration is within 0.7 to 1.3 times the expected
concentration, then proceed with the testing. If
applicable, apply the correction factor from the Method 301
of this appendix validation test (not the result from the QA
spike).
8.7 Sampling. If analyte concentrations vary rapidly with
time, continuous sampling is preferable using the smallest
cell volume, fastest sampling rate and fastest spectra
collection rate possible. Continuous sampling requires the
least operator intervention even without an automated
sampling system. For continuous monitoring at one location
over long periods, Continuous sampling is preferred. Batch
sampling and continuous static sampling are used for
screening and performing test runs of finite duration.
Either technique is preferred for sampling several locations
in a matter of days. Batch sampling gives reasonably good
time resolution and ensures that each spectrum measures a
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discreet (and unique) sample volume. Continuous static (and
continuous) sampling provide a very stable background over
long periods. Like batch sampling, continuous static
sampling also ensures that each spectrum measures a unique
sample volume. It is essential that the leak check
procedure under vacuum (section 8.2 of this method) is
passed if the batch sampling procedure is used. It is
essential that the leak check procedure under positive
pressure is passed if the continuous static or continuous
sampling procedures are used. The sampling techniques are
described in sections 8.7.1 through 8.7.2 of this method.
8.7.1 Batch Sampling. Evacuate the absorbance cell to
^ 5 mmHg absolute pressure. Fill the cell with exhaust gas
to ambient pressure, isolate the cell, and record the
spectrum. Before taking the next sample, evacuate the cell
until no spectral evidence of sample absorptic. remains.
Repeat this procedure to collect eight spectra ,f separate
samples in 1 hour.
8.7.2 Continuous Static Sampling. Purge the FTIR cell with
10 cell volumes of sample gas. Isolate the cell, collect
the spectrum of the static sample and record the pressure.
Before measuring the next sample, purge the cell with 10
more cell volumes of sample gas.
8.8 Sampling QA and Reporting.
8.8.1 Sample integration times shall be sufficient to
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achieve the required signal-to-noise ratio. Obtain an
absorbance spectrum by filling the cell with N2. Measure
the RMSD in each analytical region in this absorbance
spectrum. Verify that the number of scans used is
sufficient to achieve the target MAU.
8.8.2 Assign a unique file name to each spectrum.
8.8.3 Store two copies of sample interferograms and
processed spectra on separate computer disks.
8.8.4 For each sample spectrum, document the sampling
conditions, the sampling time (while the cell was being
filled), the time the spectrum was recorded, the
instrumental conditions (path length, temperature, pressure,
resolution, signal integration time), and the spectral file
name. Keep a hard copy of these data sheets.
8.9 Signal Transmittance. While sampling, monitor the
signal transmittance. If signal transmittance (relative to
the background) changes by 5 percent or more (absorbance =
-.02 to .02) in any analytical spectral region, obtain a new
background spectrum.
8.10 Post-test CTS. After the sampling run, record another
CTS spectrum.
8.11 Post-test QA.
8.11.1 Inspect the sample spectra immediately after the run
to verify that the gas matrix composition was close to the
expected (assumed) gas matrix.
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34
8.11.2 Verify that the sampling and instrumental parameters
were appropriate for the conditions encountered. For
example, if the moisture is much greater than anticipated,
it may be necessary to use a shorter path length or dilute
the sample.
8.11.3 Compare the pre- and post-test CTS spectra. The
peak absorbance in pre- and post-test CTS must be ± 5
percent of the mean value. See appendix E of the FTIR
Protocol.
9.0 Quality Control.
Use analyte spiking (sections 8.6.2, 9.2 and 13.0 of
this method) to verify that the sampling system can
transport the analytes from the probe to the FTIR system.
9.1 Spike Materials. Use a certified standard (accurate to
± 2 percent) of the target analyte, if one can be obtained.
If a certified standard cannot be obtained, follow the
procedures in section 4.6.2.2 of the FTIR Protocol.
9.2 Spiking Procedure. QA spiking (section 8.6.2 of this
method) is a calibration procedure used before testing. QA
spiking involves following the spike procedure of sections
9.2.1 through 9.2.3 of this method to obtain at least three
spiked samples. The analyte concentrations in the spiked
samples shall be compared to the expected spike
concentration to verify that the sampling/analytical system
is working properly. Usually, when QA spiking is used, the
D-36
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method has already been validated at a similar source for
the analyte in question. The QA spike demonstrates that the
validated sampling/analytical conditions are being
duplicated. If the QA spike fails then the
sampling/analytical system shall be repaired before testing
proceeds. The method validation procedure (section 13.0 of
this method) involves a more extensive use of the analyte
spike procedure of sections 9.2.1 through 9.2.3 of this
method. Spectra of at least 12 independent spiked and 12
independent unspiked samples are recorded. The
concentration results are analyzed statistically to
determine if there is a systematic bias in the method for
measuring a particular analyte. If there is a systematic
bias, within the limits allowed by Method 301 of this
appendix, then a correction factor shall be applied to the
analytical results. If the systematic bias is greater than
the allowed limits, this method is not valid and cannot be
used.
9.2.1 Introduce the spike/tracer gas at a constant flow
rate of ^ 10 percent of the total sample flow, when
possible. (Note: Use the rotameter at the end of the
sampling train to estimate the required spike/tracer gas
flow rate.) Use a flow device, e.g., mass flow meter (± 2
percent), to monitor the spike flow rate. Record the spike
flow rate every 10 minutes.
D-37
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9.2.2 Determine the response time (RT) of the system by
continuously collecting spectra of the spiked effluent until
the spectrum of the spiked component is constant for 5
minutes. The RT is the interval from the first measurement
until the spike becomes constant. Wait for twice the
duration of the RT, then collect spectra of two independent
spiked gas samples. Duplicate analyses of the spiked
concentration shall be within 5 percent of the mean of the
two measurements.
9.2.3 Calculate the dilution ratio using the tracer gas as
follows :
SF
DF = — S2E£ (3)
where :
CS = DF*Spikedir + Unspike(l-DF) (4)
DF = Dilution factor of the spike gas; this value
shall be *10.
SFfiidir) = SF6 (or tracer gas) concentration measured
directly in undiluted spike gas.
SFs,3plc) = Diluted SF6 (or tracer gas) concentration
measured in a spiked sample.
D-38
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Spikedir = Concentration of the analyte in the spike
standard measured by filling the FTIR cell
directly.
CS = Expected concentration of the spiked samples,
Unspike = Native concentration of analytes in unspiked
samples
10.0 Calibration and Standardization.
10.1 Signal-to-Noise Ratio (S/N). The RMSD in the noise
must be less than one tenth of the minimum analyte peak
absorbance in each analytical region. For example if the
minimum peak absorbance is 0.01 at the required DL, then
RMSD measured over the entire analytical region must be
< 0.001.
10.2 Absorbance Path length. Verify the absorbance path
length by comparing reference CTS spectra to test CTS
spectra. See appendix E of the FTIR Protocol.
10.3 Instrument Resolution. Measure the line width of
appropriate test CTS band(s) to verify instrument
resolution. Alternatively, compare CTS spectra to a
reference CTS spectrum, if available, measured at the
nominal resolution.
10.4 Apodization Function. In transforming the sample
interferograms to absorbance spectra use the same
D-39
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38
apodization function that was used in transforming the
reference spectra.
10.5 FTIR Cell Volume. Evacuate the cell to s 5 mmHg .
Measure the initial absolute temperature (Tt) and absolute
pressure (PJ . Connect a wet test meter (or a calibrated
dry gas meter), and slowly draw room air into the cell.
Measure the meter volume (VJ , meter absolute temperature
(Tm) , and meter absolute pressure (PJ; and the cell final
absolute temperature (Tf) and absolute pressure (Pf) .
Calculate the FTIR cell volume Vss, including that of the
connecting tubing, as follows:
v m
777 rrt
SS
(5)
11.0 Data Analysis and Calculations.
Analyte concentrations shall be measured using
reference spectra from the EPA FTIR spectral library. When
EPA library spectra are not available, the procedures in
section 4.6 of the Protocol shall be followed to prepare
reference spectra of all the target analytes.
11.1 Spectral De-resolution. Reference spectra can be
converted to lower resolution standard spectra (section 3.3
D-40
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of this method) by truncating the original reference sample
and background interferograms. Appendix K of the FTIR
Protocol gives specific deresolution procedures. Deresolved
spectra shall be transformed using the same apodization
function and level of zero filling as the sample spectra.
Additionally, pre-test FTIR protocol calculations (e.g.,
FRU, MAU, FCU) shall be performed using the de-resolved
standard spectra.
11.2 Data Analysis. Various analytical programs are
available for relating sample absorbance to a concentration
standard. Calculated concentrations shall be verified by
analyzing residual baselines after mathematically
subtracting scaled reference spectra from the sample
spectra. A full description of the data analysis and
calculations is contained in the FTIR Protocol (sections
4.0, 5.0, 6.0 and appendices). Correct the calculated
concentrations in the sample spectra for differences in
absorption path length and temperature between the reference
and sample spectra using equation 6,
c.
corr
"calc
where:
CCorr = Concentration, corrected for path length.
Ccalc = Concentration,, initial calculation (output of the
analytical program designed for the compound).
D-41
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Lr = Reference spectra path length.
L, = Sample spectra path length.
Ts = Absolute temperature of the sample gas, K.
Tr = Absolute gas temperature of reference spectra, K.
P3 = Sample cell pressure.
Pr = Reference spectrum sample pressure.
12.0 Method Performance.
12.1 Spectral Quality. Refer to the FTIR Protocol
appendices for analytical requirements, evaluation of data
quality, and analysis of uncertainty.
12.2 Sampling QA/QC. The analyte spike procedure of
section 9 of this method, the QA spike of section 8.6.2 of
this method, and the validation procedure of section 13 of
this method are used to evaluate the performance of the
sampling system and to quantify sampling system effects, if
any, on the measured concentrations. This method is self-
validating provided that the results meet the performance
requirement of the QA spike in sections 9.0 and 8.6.2 of
this method and results from a previous method validation
study support the use of this method in the application.
Several factors can contribute to uncertainty in the
measurement of spiked samples. Factors which can be
controlled to provide better accuracy in the spiking
procedure are listed in sections 12.2.1 through 12.2.4 of
this method.
D-42
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12.2.1 Flow meter. An accurate mass flow meter is accurate
to ± 1 percent of its span. If a flow of 1 L/min is
monitored with such a MFM, which is calibrated in the range
of 0-5 L/min, the flow measurement has an uncertainty of 5
percent. This may be improved by re-calibrating the meter
at the specific flow rate to be used.
12.2.2 Calibration gas. Usually the calibration standard
is certified to within ± 2 percent. With reactive analytes,
such as HCl, the certified accuracy in a commercially
available standard may be no better than ± 5 percent.
12.2.3 Temperature. Temperature measurements of the cell
shall be quite accurate. If practical, it is preferable to
measure sample temperature directly, by inserting a
thermocouple into the cell chamber instead of monitoring the
cell outer wall temperature.
12.2.4 Pressure. Accuracy depends on the accuracy of the
barometer, but fluctuations in pressure throughout a day may
be as much as 2.5 percent due to weather variations.
13.0 Method Validation Procedure.
This validation procedure, which is based on EPA Method
301 (40 CFR part 63, appendix A), may be used to validate
this method for the analytes in a gas matrix. Validation at
one source may also apply to another type of source, if it
can be shown that the exhaust gas characteristics are
similar at both sources.
D-43
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13.1 Section 5.3 of Method 301 (40 CFR part 63, appendix
A), the Analyte Spike procedure, is used with these
modifications. The statistical analysis of the results
follows section 6.3 of EPA Method 301. Section 3 of this
method defines terms that are not defined in Method 301.
13.1.1 The analyte spike is performed dynamically. This
means the spike flow is continuous and constant as spiked
samples are measured.
13.1.2 The spike gas is introduced at the back of the
sample probe.
13.1.3 Spiked effluent is carried through all sampling
components downstream of the probe.
13.1.4 A single FTIR system (or more) may be used to
collect and analyze spectra (not quadruplicate integrated
sampling trains).
13.1.5 All of the validation measurements are performed
sequentially in a single "run" (section 3.26 of this
method).
13.1.6 The measurements analyzed statistically are each
independent (section 3.22 of this method).
13.1.7 A validation data set can consist of more than 12
spiked and 12 unspiked measurements.
13.2 Batch Sampling. The procedure in sections 13.2.1
through 13.2.2 may be used for stable processes. If process
emissions are highly variable, the procedure in section
D-44
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13.2.3 shall be used.
13.2.1 With a single FTIR instrument and sampling system,
begin by collecting spectra of two unspiked samples.
Introduce the spike flow into the sampling system and allow
10 cell volumes to purge the sampling system and FTIR cell.
Collect spectra of two spiked samples. Turn off the spike
and allow 10 cell volumes of unspiked sample to purge the
FTIR cell. Repeat this procedure until the 24 (or more)
samples are collected.
13.2.2 In batch sampling, collect spectra of 24 distinct
samples. (Each distinct sample consists of filling the cell
to ambient pressure after the cell has been evacuated.)
13.2.3 Alternatively, a separate probe assembly, line, and
sample pump can be used for spiked sample. Verify and
document that sampling conditions are the same in both the
spiked and the unspiked sampling systems. This can be done
by wrapping both sample lines in the same heated bundle.
Keep the same flow rate in both sample lines. Measure
samples in sequence in pairs. After two spiked samples are
measured, evacuate the FTIR cell, and turn the manifold
valve so that spiked sample flows to the FTIR cell. Allow
the connecting line from the manifold to the FTIR cell to
purge thoroughly (the time depends on the line length and
flow rate). Collect a pair of spiked samples. Repeat the
procedure until at least 24 measurements are completed.
D-45
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13.3 Simultaneous Measurements With Two FTIR Systems. If
unspiked effluent concentrations of the target analyte(s)
vary significantly with time, it may be desirable to perform
synchronized measurements of spiked and unspiked sample.
Use two FTIR systems, each with its own cell and sampling
system to perform simultaneous spiked and unspiked
measurements. The optical configurations shall be similar,
if possible. The sampling configurations shall be the same.
One sampling system and FTIR analyzer shall be used to
measure spiked effluent. The other sampling system and FTIR
analyzer shall be used to measure unspiked flue gas. Both
systems shall use the same sampling procedure (i.e., batch
or continuous) .
13.3.1 If batch sampling is used, synchronize the cell
evacuation, cell filling, and collection of spectra. Fill
both cells at the same rate (in cell volumes per unit time).
13.3.2 If continuous sampling is used, adjust the sample
flow through each gas cell so that the same number of cell
volumes pass through each cell in a given time (i.e. TCt =
TC2) .
13.4 Statistical Treatment. The statistical procedure of
EPA Method 301 of this appendix, section 6.3 is used to
evaluate the bias and precision. For FTIR testing a
validation "run" is defined as spectra of 24 independent
samples, 12 of which are spiked with the analyte(s) and 12
D-46
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of which are not spiked.
13.4.1 Bias. Determine the bias (defined by EPA Method 301
of this appendix, section 6.3.2) using equation 7:
= Sm - CS (7)
m
where :
B = Bias at spike level.
Sm = Mean concentration of the analyte spiked
samples .
CS = Expected concentration of the spiked samples.
13.4.2 Correction Factor. Use section 6.3.2.2 of Method
301 of this appendix to evaluate the statistical
significance of the bias. If it is determined that the bias
is significant, then use section 6.3.3 of Method 301 to
calculate a correction factor (CF) . Analytical results of
the test method are multiplied by the correction factor, if
0.7 5 CF 5 1.3. If is determined that the bias is
significant and CF > ± 30 percent, then the test method is
considered to "not valid."
13.4.3 If measurements do not pass validation, evaluate the
sampling system, instrument configuration, and analytical
system to determine if improper set-up or a malfunction was
the cause. If so, repair the system and repeat the
validation.
D-47
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14.0 Pollution Prevention.
The extracted sample gas is vented outside the
enclosure containing the FTIR system and gas manifold after
the analysis. In typical method applications the vented
sample volume is a small fraction of the source volumetric
flow and its composition is identical to that emitted from
the source. When analyte spiking is used, spiked pollutants
are vented with the extracted sample gas. Approximately 1.6
x 10"" to 3.2 x ICr4 Ibs of a single HAP may be vented to the
atmosphere in a typical validation run of 3 hours. (This
assumes a molar mass of 50 to 100 g, spike rate of 1.0
L/min, and a standard concentration of 100 ppm). Minimize
emissions by keeping the spike flow off when not in use.
15.0 Waste Management.
Small volumes of laboratory gas standards can be vented
through a laboratory hood. Neat samples must be packed and
disposed according to applicable regulations. Surplus
materials may be returned to supplier for disposal.
16.0 References.
1. "Field Validation Test Using Fourier Transform Infrared
(FTIR) Spectrometry To Measure Formaldehyde, Phenol and
Methanol at a Wool Fiberglass Production Facility." Draft.
U.S. Environmental Protection Agency Report, EPA Contract
No. 68D20163, Work Assignment 1-32, September 1994.
2. "FTIR Method Validation at a Coal-Fired Boiler".
D-48
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Prepared for U.S. Environmental Protection Agency, Research
Triangle Park, NC. Publication No.: EPA-454/R95-004, NTIS
No.: PB95-193199. July, 1993.
3. "Method 301 - Field Validation of Pollutant Measurement
Methods from Various Waste Media," 40 CFR part 63, appendix
A.
4. "Molecular Vibrations; The Theory of Infrared and Raman
Vibrational Spectra," E. Bright Wilson, J. C. Decius, and P.
C. Cross, Dover Publications, Inc., 1980. For a less
intensive treatment of molecular rotational-vibrational
spectra see, for example, "Physical Chemistry," G. M.
Barrow, chapters 12, 13, and 14, McGraw Hill, Inc., 1979.
5. "Fourier Transform Infrared Spectrometry," Peter R.
Griffiths and James de Haseth, Chemical Analysis, 83, 16-
25, (1986), P. J. Elving, J. D. Winefordner and I. M.
Kolthoff (ed.J, John Wiley and Sons.
6. "Computer-Assisted Quantitative Infrared Spectroscopy,"
Gregory L. McClure (ed.), ASTM Special Publication 934
(ASTM), 1987.
7. "Multivariate Least-Squares Methods Applied to the
Quantitative Spectral Analysis of Multicomponent Mixtures,"
Applied Spectroscopy, 39(10), 73-84, 1985.
D-49
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Table 1. EXAMPLE PRESENTATION OF SAMPLING DOCUMENTATION.
Suple Tiae
Spectral File HUM
Background Flic Hue
Suple conditioning
frocess coadltloa
d
t
O
Suple Tl«e
Spectnw File
Interferograa
•esoUtioa
Scans
ApodlzatlM
Cala
CTS Spectrui
-------
Probe «1
Probe Box
f ' """"" I-
To J' 'I'
»*1l lj.
Stack
Van! 2
Vend
• Vent »2
Proba*2
Balaton •
Finer
Sample Line #2
Pump #2
Balslon
£
±JL
• • -J- - ' Sample Line #1
Spike Line
ample Gas Delivery Manaold piker
» Toggle
r**-| Vaive
PunT"! ^g9-
Calibration Gas Line
MascFlow Calfcration Gas ManHold
Malar j
i-HJH-J
I
To Calibration
Gas Cylinders
Figure 1. Extractive FTIR sampling system.
-------
.8-
.6-
.4-
0
FRU = SRMS(FU-FL)/BAV
SRMS = .00147
BAV = 3.662
FM = FRU = .086
p-xylene
1050
1000
i i
950 900
Wavenumbers
850
r
800
T
750
Figure 2. Fractional Reproducibility. Top: average of cts!031a and
ctsllOlb. Bottom: Reference spectrum of p-xylene.
-------
D-2 EPA FTIR PROTOCOL
D-53
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D-54
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™™ ?OR TH* USS °P BXTOACTIVB FOURIER TRANSFORM
INFRARED (FTIR) SPBCTROMBTRY FOR THE ANALYSES OF GASEOUS
EMISSIONS FROM STATIONARY SOURCES
INTRODUCTION
The purpose of this document is to set general guidelines
for the use of modern FTIR spectroscopic methods for the analysis
of gas samples extracted from the effluent of stationary emission
sources. This document outlines techniques for developing and
evaluating such methods and sets basic requirements for reporting
and quality assurance procedures.
1.0 NOMENCLATURE
1.1 Appendix A lists definitions of the symbols and terms
used in this Protocol, many of which have been taken directly
from American Society for Testing and Materials (ASTM)
publication E 131-90a, entitled "Terminology Relating to
Molecular Spectroscopy."
1.2 Except in the case of background spectra or where
otherwise noted, the term "spectrum1 refers to a double-beam
spectrum in units of absorbance vs. wavenumber (cm"1).
1.3 The term "Study* in this document refers to a
publication that has been subjected to EPA- or peer-review.
2.0 APPLICABILITY AND ANALYTICAL PRINCIPLE
2.1 Applicability. This Protocol applies to the
determination of compound-specific concentrations in single- and
multiple-component gas phase samples using double-beam absorption
spectroscopy in the mid-infrared band. It does not specifically
address other FTIR applications, such as single-beam
spectroscopy, analysis of open-path (non-enclosed) samples, and
continuous measurement techniques. If multiple spectrometers,
absorption cells, or instrumental linewidths are used in such
analyses, each distinct operational configuration of the system
must be evaluated separately according to this Protocol.
2.2 Analytical Principle.
2.2.1 In the mid-infrared band, most molecules exhibit
characteristic gas phase absorption spectra that may be recorded
by FTIR systems. Such systems consist of a source of mid-
infrared radiation, an interferometer, an enclosed sample cell of
known absorption pathlength, an infrared detector, optical
elements for the transfer of infrared radiation between
components, and gas flow control and measurement components.
Adjunct and integral computer systems are used for controlling
the instrument, processing the signal, and for performing both
Fourier transforms and quantitative analyses of spectral data.
D-55
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2.2.2 ihe absorption spectra of pure gases and of nnxtu —s
of gases are described by a linear absorbance theory referred~-0
as Beer's Law. Using this law, modern FTIR systems use
computerized analytical programs to quantify compounds by
comparing the absorption spectra of known (reference) gas samples
to the absorption spectrum of the sample gas. Some standard
mathematical techniques used for comparisons are classical least
squares, inverse least squares, cross-correlation, factor
analysis, and partial least squares. Reference A describes
several of these techniques, as well as additional techniques
such as differentiation methods, linear baseline corrections, and
non-linear absorbance corrections.
3.0 OSNBBAL PRINCIPLES OF PROTOCOL RSQUIRBMBNTS
The characteristics that distinguish FTIR systems from gas
analyzers used in instrumental gas analysis methods (e.g.,
EPA Methods 6C and 7E) are: (1) Computers are necessary to
obtain and analyze data; (2) chemical concentrations can be
quantified using previously recorded infrared reference spectra;
and (3) analytical assumptions and results, including possible
effects of interfering compounds, can be evaluated after the
quantitative analysis. The following general principles and
requirements of this Protocol are based on these characteristics.
3.1 Veriflability and Reproducibility of Results. Store
all data and document data analysis techniques sufficient to
allow an independent agent to reproduce the analytical results
from the raw interferometric data.
3.2 Transfer of Reference Spectra. To determine whether
reference spectra recorded under one set of conditions (e.g.,
optical bench, instrumental linewidth, absorption pathlength,
detector performance, pressure, and temperature) can be used to
analyze sample spectra taken under a different set of conditions,
quantitatively compare "calibration transfer standards" (CTS) and
reference spectra as described in this Protocol. (Note,: The CTS
may, but need not, include analytes of interest). To effect
this, record the absorption spectra of the CTS (a) immediately
before and immediately after recording reference spectra and
(b) immediately after recording sample spectra.
3.3 Evaluation of FTIR Analyses. The applicability,
accuracy, and precision of FTIR measurements are influenced by a
number of interrelated factors, which may be divided into two
classes:
3.3.1 Sample-Independent Factors. Examples are system
configuration and performance (e.g., detector sensitivity and
infrared source output), quality and applicability of reference
absorption spectra, and type of mathematical analyses of the
spectra. These factors define the fundamental limitations of
FTIR measurements for a given system configuration. These
limitations may be estimated from evaluations of the system
before samples are available. For example, the detection limit
for the absorbing compound under a given set of conditions may be
D-56
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estimated from the system noise level and the strena-h of
o A T" 1.1_ f"' 11 ] fl >•• A Hi«/-\ to ' w s& • k *^ outdiyuii ^> L
3.3.2 Sample-Dependent Factors. Examples are soectrai
interferants (e.g., water vapor and C02) or the overlap of
^posits ofref^ ?' diffe«nt Compounds and contaStSion
deposits on reflective surfaces or transmitting windows To
maximize the effectiveness of the mathematical t2chni™es used in
ia"! »£S!y:i3' id«*ificatidn of interferants U Slndarf "
i? ? P) and analyS1S of samples (includes effects of other
i ? err°rs) are necessary. Thus, the Protocol requires
-analysis calculation of measurement concentration
uncertainties for- the detection of these potential sources of
measurement error. ouu.n_e3 uc
4.0 PR*-TEST PREPARATIONS AMD EVALUATIONS
Before testing, demonstrate the suitability of FTIR
spectrometry for the desired application according to the
procedures of this section.
4.1 Identify Test Requirements. Identify and record the
test requirements described below in 4.1.1 through 4.1.5. These
values set the desired or required goals of the proposed'
analysis; the description of methods for determining whether
these goals are actually met during the analysis comprises the
majority of this Protocol.
4.1.1 Analytes (specific chemical species) of interest.
Label the analytes from i = 1 to I.
4.1.2 Analytical uncertainty limit (AUj) . The AUt is the
maximum permissible fractional uncertainty of analysis for the
i'h analyte concentration, expressed as a fraction of the analyte
concentration in the sample.
4.1,3 Required detection limit for each analyte (DL^ ppm) .
The detection limit is the lowest concentration of an analyte for
which its overall fractional uncertainty (OFUJ is required to be
less than its analytical uncertainty limit (AUt) .
4.1.4 Maximum expected concentration of each analyte
ppm) .
4.2 Identify Potential Interferants. Considering the
chemistry of the process or results of previous Studies, identify
potential interferants, i.e., the major effluent constituents and
any relatively minor effluent constituents that possess either
strong absorption characteristics or strong structural
similarities to any analyte of interest. Label them 1 through
N^, where the subscript "j" pertains to potential interferants.
Estimate the concentrations of these compounds in the effluent
(CPOTj, ppm) .
D-57
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4.3 Select and Evaluate the Sampling System. Consid»ri-a
the source, e.g., temperature and pressure profiles, moistur*
content, analyte characteristics, and participate concentration)
select the equipment for extracting gas samples. Recommended are
a participate filter, heating system to maintain sample
temperature above the dew point for all sample constituents at
all points within the sampling system (including the filter) and
sample conditioning system (e.g., coolers, water-permeable
membranes that remove water or other compounds from the sample
and dilution devices) to remove spectral interferants or to
protect the sampling and analytical components. Determine the
minimum absolute sample system pressure (Pmin, mmHg) and the
infrared absorption cell volume (Vsg, liter) . Select the
techniques and/or equipment for the measurement of sample
pressures and temperatures.
4.4 Select Spectroscopic System. Select a spectroscopic
configuration for the application.- Approximate the absorption
pathlength (Ls' , meter), sample pressure (Ps', kPa), absolute
sample temperature Ts', and signal integration period (tsg,
seconds) for the analysis. Specify the nominal minimum
instrumental linewidth (MIL) of the system. Verify that the
fractional error at the approximate values Ps' and Ts' is less
than one half the smallest value AU4 (see Section 4.1.2) .
4.5 Select Calibration Transfer Standards (CTS's). Select
CTS's that meet the criteria listed in Sections 4.5.1, 4.5.2, and
4.5.3.
Note: it may be necessary to choose preliminary analytical
regions (see Section 4.7), identify the minimum analyte
linewidths, or estimate the system noise level (see
Section 4.12) before selecting the CTS. More than one
compound may be needed to meet the criteria; if so, obtain
separate cylinders for each compound.
4.5.1 The central wavenumber position of each analytical
region lies within 25 percent of the wavenumber position of at
least one CTS absorption band.
.«
4.5-.2 The absorption bands in 4.5.1 exhibit peak
absorbances greater than ten times the value RMSEST (see
Section 4.12) but less than 1.5 absorbance units.
4.5.3 At least one absorption CTS band within the operating
range of the FTIR instrument has an instrument-independent
linewidth no greater than the narrowest analyte absorption band;
perform and document measurements or cite Studies to determine
analyte and CTS compound linewidths.
4.5.4 For each analytical region, specify the upper and
lower wavenumber positions (FFUm and FFL,, respectively) that
bracket the CTS absorption band or bands for the associated
analytical region. Specify the wavenumber range, FNU to FNL,
containing the absorption band that rr.eecs the criterion of
Section 4.5.3 .
D-58
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4 5.5 Associate, whenever possible, a single set of CT3 a as
cylinders with a set of reference spectra. Replacement CTS gas
cylinders shall contain the same compounds at concentrations
within 5 percent of that of the original CTS cylinders; the
entire absorption spectra (not individual spectral segments) of
the replacement gas shall be scaled by a factor between 0.95 and
1.05 to match the original CTS spectra.
4.6 Prepare Reference Spectra.
NOES: Reference spectra are available in a permanent soft
copy from the EPA spectral library on the EMTIC (Emission
Measurement Technical Information Center) computer bulletin
board; they may be used if applicable.
4.6.1 Select the reference absorption pathlength (LR) of the
4.6.2 Obtain or prepare a set of chemical standards for
each analyte, potential and known spectral interferants, and CTS.
Select the concentrations of the chemical standards to correspond
to the top of the desired range.
4.6.2.1 Commercially-Prepared Chemical Standards. Chemical
standards for many compounds may be obtained from independent
sources, such as a specialty gas manufacturer, chemical company,
or commercial laboratory. These standards (accurate to within
±2 percent) shall be prepared according to EPA Protocol 1 (see
Reference D) or shall be traceable to NIST standards. Obtain
from the supplier an estimate of the stability of the analyte
concentration; obtain and follow all the supplier's
recommendations for recertifying the analyte concentration.
4.6.2.2 Self-Prepared Chemical Standards. Chemical
standards may be prepared as follows: Dilute certified
commercially prepared chemical gases or pure analytes with ultra-
pure carrier (UPC) grade nitrogen according to the barometric and
volumetric techniques generally described in Reference A,
Section A4.6.
4.6'.3 Record a set of the absorption spectra of the CTS
{Rl}, then a set of the reference spectra at two or more
concentrations in duplicate over the desired range (the top of
the range must be less than 10 times that of the bottom),
followed by a second set of CTS spectra {R2}. (If self-prepared
standards are used, see Section 4.6.5 before disposing of any of
the standards.) The maximum accepted standard concentration-
pathlength product (ASCPP) for each compound shall be higher than
the maximum estimated concentration-pathlength products for both
analytes and known interferants in the effluent gas. For each
analyte, the minimum ASCPP shall be no greater than ten times the
concentration-pathlength product of that analyte at its required
detection limit.
4.6.4 Permanently store the background and interferograms
in digitized form. Document details of the mathematical process
for generating the spectra from these interferograms. Record the
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sample pressure (PR), sample temperature (TR) , reference
absorption pathlength (LR), and interferogram signal integration
period (t3R) . Signal integration periods for the background
interferograms shall be >t3R. Values of Pa, LR, and tsT shall not
deviate by more than ±1 percent from the time of recording fRl)
to that of recording {R2}. y
4.6.5 If self-prepared chemical standards are employed and
spectra of only two concentrations are recorded for one or more
compounds, verify the accuracy of the dilution technique by
analyzing the prepared standards for those compounds with a
secondary (non-FTIR) technique as follows:
4.6.5.1 Record the response of the secondary technique to
each of the four standards prepared.
4.6.5.2 Perform a linear regression of the response values
(dependant variable) versus the accepted standard concentration
(ASC) values (independent variable), with the regression
constrained to pass through the zero-response, zero ASC point.
4.6.5.3 Calculate the average fractional difference between
the actual response values and the regression-predicted values
(those calculated from the regression line using the four ASC
values as the independent variable).
4.6.5.4 If the average fractional difference value
calculated in Section 4.6.5.3 is larger for any compound than the
corresponding AUt, the dilution technique is not sufficiently
accurate and the reference spectra prepared are not valid for the
analysis.
4.7 Select Analytical Regions. Using the general
considerations in Section 7 of Reference A and the spectral
characteristics of the analytes and interferants, select the
analytical regions for the application. Label them m = 1 to M.
Specify the lower, center and upper wavenumber positions of each
analytical region (FL,, FCm, and FUm, respectively). Specify the
analytes and interferants which exhibit absorption in each
region.,
4.8 Determine Fractional Reproducibility Uncertainties.
Using Appendix E, calculate the fractional reproducibility
uncertainty for each analyte (FRU^ from a comparison of {Rl} and
{R2}. If FRUt > AUt for any analyte, the reference spectra
generated in Section 4.6 are not valid for the application.
4.9 Identify Known Interferants. Using Appendix B,
determine which potential interferant affects the analyte
concentration determinations. If it does, relabel the potential
interferant as "known* interferant, and designate these compounds
from k = 1 to K. Appendix B also provides criteria for
determining whether the selected analytical regions are suitable.
4.10 Prepare Computerized Analytical Programs.
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4.10.1 Choose or devise mathematical techniques (e g
classical least squares, inverse least squares, cross-
correlation, and factor analysis) based on Equation 4 of
Reference A that are appropriate for analyzing spectral data by
comparison with reference spectra.
4.10.2 Following the general recommendations of Reference
A, prepare a computer program or set of programs that analyzes
all the analytes and known interferants, based on the selected
analytical regions (4.7) and the prepared reference spectra
(4.6). Specify the baseline correction technique (e.g.,
determining the slope and intercept of a linear baseline
contribution in each analytical region) for each analytical
region, including all relevant wavenumber positions.
4.10.3 Use programs that provide as output [at the
reference absorption pathlength (LR) , reference gas temperature
(TR) , and reference gas pressure (PR)] the analyte
concentrations, the known interferant concentrations, and the
baseline slope and intercept values. If the sample absorption
pathlength (Ls) , sample gas temperature (Tg) or sample gas
pressure (Ps) during the actual sample analyses differ from L,,
TR, and Pp< use a program or set of programs that applies
multiplicative corrections to the derived concentrations to
account for these variations, and that provides as output both
the corrected and uncorrected values. Include in the report of
the analysis (see Section 7.0) the details of any transformations
applied to the original reference spectra (e.g.,
differentiation), in such a fashion that all analytical results
may be verified by an independent agent from the reference
spectra and data spectra alone.
4.11 Determine the Fractional Calibration Uncertainty.
Calculate the fractional calibration uncertainty for each analyte
(FCU^ according to Appendix F, and compare these values to the
fractional uncertainty limits (AUt; see Section 4.1). If
FCUL > AUj) , either the reference spectra or analytical programs
for that analyte are unsuitable.
4.1-2 Verify System Configuration Suitability. Using
Appendix C, measure or obtain estimates of the noise level
(RMSgsT'' absorbance) of the FTIR system; alternatively, construct
the complete spectrometer system and determine the values RMS^
using Appendix G. Estimate the minimum measurement uncertainty
for each analyte (MAUt, ppm) and known interf erant (MIUk, ppm)
using Appendix D. Verify that (a) MAUt < (AUt) (DLt) , FRUL < AUL,
and FCUt < AUt for each analyte and that (b) the CTS chosen meets
the requirements listed in Section 4.5.
5.0 SAMPLING AND ANALYSIS PROCBDUR1
5.1 Analysis System Assembly and Leak-Test. Assemble the
analysis system. Allow sufficient time for all system components
to reach the desired temperature. Then determine the leak-rate
(LR) and leak volume (VL) , where V, = LR t.s. Leak volumes shall
be s4 percent of Vss.
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3.2 Verify Instrumental Performance. Measure the ncn se
level of the -system in each analytical region using the procedure
of Appendix G. if any noise level is higher than that estimated""
for the system in Section 4.12, repeat the calculations of
Appendix D and verify that the requirements of Section 4.12 are
met; if they are not, adjust or repair the instrument and repeat
this section.
5.3 Determine the Sample Absorption Pathlength. Record a
background spectrum. Then, fill the absorption cell with CTS at
the pressure PR and record a set of CTS spectra {R3}. Store the
background and unsealed CTS single beam interferograms and
spectra. Using Appendix H, calculate the sample absorption
pathlength (Lg) for each analytical region. The values Ls shall
not differ from the approximated sample pathlength Ls' (see
Section 4.4) by more than 5 percent.
5.4 Record Sample Spectrum. Connect the sample line to the
source. Either evacuate the absorption cell to an absolute
pressure below 5 mmHg before extracting a sample from the
effluent stream into the absorption cell, or pump at least ten
cell volumes of sample through the cell before obtaining a
sample. Record the sample pressure Ps. Generate the absorbance
spectrum of the sample. Store the background and sample single
beam interferograms, and document the process by which the
absorbance spectra are generated from these data. (If necessary,
apply the spectral transformations developed in Section 5.6.2).
The resulting sample spectrum is referred to below as Ss.
Mote: Multiple sample spectra may be recorded according to
the procedures of Section 5.4 before performing Sections 5.5
and 5.6.
5.5 Quantify Analyte Concentrations. Calculate the
unsealed analyte concentrations RUAt and unsealed interferant
concentrations RUIK using the programs developed in Section 4.
To correct for pathlength and pressure variations between the
reference and sample spectra, calculate the scaling factor
RLPS = (LRPRTS> / (LSPSTR) • Calculate the final analyte and
interferant concentrations RSAt = R^RUAj and RSI* = RLPSRUIfc.
5.5 Determine Fractional Analysis Uncertainty. Fill the
absorption cell with CTS at the pressure Ps. Record a set of CTS
spectra {R4}. Store the background and CTS single beam
interferograms. Using Appendix H, calculate the fractional
analysis uncertainty (FAU) for each analytical region. If the
FAU indicated for any analytical region is larger than the
required accuracy requirements determined in Section 4.1, then
comparisons to previously recorded reference spectra are invalid
in that analytical region, and the analyst shall perform one or
both of the following procedures:
5.6.1 Perform instrumental checks and adjust the instrument
to restore its performance to acceptable levels. If adjustments
are made, repeat Sections 5.3, 5.4 (except for the recording of a
sample spectrum), and 5.5 to demonstrate that acceptable
uncertainties are obtained in all analytical regions.
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5.6.2 Apply appropriate mathematical transformations (e g
frequency shifting, zero-filling, apodization, smoothing) to'the
spectra (or to the interferograms upon which the spectra are
based) generated during the performance of the procedures of
Section 5.3. Document these transformations and their
reproducibility. Do not apply multiplicative scaling of the
spectra, or any set of transformations that is mathematically
equivalent to multiplicative scaling. Different transformations
may be applied to different analytical regions. Frequency shifts
shall be smaller than one-half the minimum instrumental
linewidth, and must be applied to all spectral data points in an
analytical region. The mathematical transformations may be
retained for the analysis if they are also applied to the
appropriate analytical regions of all sample spectra recorded,
and if all original s-ample spectra are digitally stored. Repeat
Sections 5.3, 5.4 (except the recording of a sample spectrum),
and 5.5 to demonstrate that these transformations lead to
acceptable calculated concentration uncertainties in all
analytical regions.
6.0 POST-ANALYSIS EVALUATIONS
Estimate the overall accuracy of the analyses performed in
Section 5 as follows:
6.1 Qualitatively Confirm the Assumed Matrix. Examine each
analytical region of the sample spectrum for spectral evidence of
unexpected or unidentified interferants. If found, identify the
interfering compounds (see Reference C for guidance) and add them
to the list of known interferants. Repeat the procedures of
Section 4 to include the interferants in the uncertainty
calculations and analysis procedures. Verify that the MAU and
FCU values do not increase beyond acceptable levels for the
application requirements. Re-calculate the analyte
concentrations (Section 5.5) in the affected analytical regions.
6.2 Quantitatively Evaluate Fractional Model Uncertainty
(FMU) . Perform the procedures of either Section 6.2.1 or 6.2.2:
6.2--. 1 Using Appendix I, determine the fractional model
error (FMU) for each analyte.
6.2.2 Provide statistically determined uncertainties FMU
for each analyte which are equivalent to two standard deviations
at the 95% confidence level. Such determinations, if employed,
must be based on mathematical examinations of the pertinent
sample spectra (not the reference spectra alone). Include in the
report of the analysis (see Section 7.0) a complete description
of the determination of the concentration uncertainties.
6.3 Estimate Overall Concentration Uncertainty (OCU).
Using Appendix J, determine the overall concentration uncertainty
(OCU) for each analyte. If the OCU is larger than the required
accuracy for any analyte, repeat Sections 4 and 6.
7.0 REPORTING RSQUIRBMBNTS
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[Documentation pertaining to virtually all the procedures of
Section* 4, 5, and 6 will be required. Software copies of
reference spectra and sample spectra will be retained for some
minimum time following the actual testing.]
D-64
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8.0 REFERENCES
A) Standard Practices for General Techniques of Infrared
Quantitative Analysis (American Society for Testing and
Materials, Designation E 168-88).
B) The Coblentz Society Specifications for Evaluation of
Research Quality Analytical Infrared Reference Spectra
(Class II); Anal. Chemistry il, 945A (1975); Appl.
Sp«ctro«copy AAA. pp. 211-215, 1990.
C) Standard Practices for General Techniques for Qualitative
Infrared Analysis, American Society for Testing and
Materials, Designation E 1252-88.
D) "Traceability Protocol for Establishing True Concentrations
of Gases Used for Calibration and Audits of Continuous
Emissions Monitors (Protocol Number 1)," June 1978, Quality
Assurance Handbook for Air Pollution Measurement Systems,
Volume III, Stationary Source Specific Methods, EPA-600/4-
77-027b, August 1977.
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D-66
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APPENDIX A
DEFINITIONS OF TERMS AND SYMBOLS
A.I Definition* of T«ra«
absorption band - a contiguous wavenumber region of a spectrum
(equivalently, a contiguous set of absorbance spectrum data
points) in which the absorbance passes through a maximum or
a series of maxima.
absorption pathlangth - in a spectrophotometer, the distance,
measured in the direction of propagation of the beam of
radiant energy, between the surface of the specimen on which
the radiant energy is incident and the surface of the
specimen from which it is emergent.
analytical region - a contiguous wavenumber region (equivalently,
a contiguous set of absorbance spectrum data points) used in'
the quantitative analysis for one or more analyte.
Note: The quantitative result for a single analyte may be
based on data from more than one analytical region.'
apodization - modification of the ILS function by multiplying the
interferogram by a weighing function whose magnitude varies
with retardation.
background apectrum - the single beam spectrum obtained with all
system components without sample present.
ba»«lin« - any line drawn on an absorption spectrum to establish
a reference point that represents a function of the radiant
power incident on a sample at a given wavelength.
B««r»'« law - the direct proportionality of the absorbance of a
compound in a homogeneous sample to its concentration.
calibration transfer •tandard (CTS) ga« - a gas standard of a
compound used to achieve and/or demonstrate suitable
quantitative agreement between sample spectra and the
reference spectra; see Section 4.5.1.
compound - a substance possessing a distinct, unique molecular
structure.
concentration (c) - the quantity of a compound contained in a
unit quantity of sample. The unit "ppm" (number, or mole,
basis) is recommended.
concentration-pathlength product - the mathematical product of
concentration of the species and absorption pathlength. For
reference spectra, this is a known quantity; for sample
spectra, it is the quantity directly determined from Beer's
law. The units "centimeters-ppm" or "meters-ppm" are
recommended.
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derivative absorption.spectrum - a plot of rate of change of
absorbance or of any function of absorbance with respect -
wavelength or any function of wavelength.
double beam spectrum - a transmission or absorbance spectrum
derived by dividing the sample single beam spectrum by the
background spectrum.
The term "double-beam- is used elsewhere to denote a
spectrum in which the sample and background interferograms
are collected simultaneously along physically distinct
absorption paths. Here, the term denotes a spectrum in
which the sample and background interferograms are collected
at different times along the same absorption path.
fast Fourier transform (FFT) - a method of speeding up the
computation of a discrete FT by factoring the data into
sparse matrices containing mostly zeros.
flyback - interferometer motion during which no data are
recorded.
Fourier transform (FT) - the mathematical process for converting
an amplitude-time spectrum to an amplitude-frequency
spectrum, or vice versa.
Fourier transform infrared (FTIR) spectrometer - an analytical
system that employs a source of mid-infrared radiation, an
interferometer, an enclosed sample cell of known absorption
pathlength, an infrared detector, optical elements that
transfer infrared radiation between components, and a
computer system. The time-domain detector response
(interferogram) is processed by a Fourier transform to yield
a representation of the detector response vs. infrared
frequency.
Mote: When FTIR spectrometers are interfaced with other
instruments, a slash should be used to denote the interface;
e.g-v, GC/FTIR; HPCL/FTIR, and the use of FTIR should be
explicit; i.e., FTIR not IR.
frequency, r - the number of cycles per unit time.
infrared - the portion of the electromagnetic spectrum containing
wavelengths from approximately 0.78 to 800 microns.
interf erogram, I (a) - record of the modulated component of the
interference signal measured as a function of retardation by
the detector.
interferometer - device that divides a beam of radiant energy
into two or more paths, generate an optical path difference
between the beams, and recombines them in order to produce
repetitive interference maxima and minima as the optical
retardation is varied.
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lin«width - the full width at half maximum of an absorption ca--
in units of wavenumbers (cm"1) .
mid-infrarad - the region of the electromagnetic spectrum from
approximately 400 to 5000 cm"1.
pathlength - see "absorption pathlength."
reference «pectra - absorption spectra of gases with known
chemical•compositions, recorded at a known absorption
pathlength, which are used in the quantitative analysis of
gas samples.
retardation, o - optical path difference between two beams in an
interferometer; also known as "optical path difference" or
"optical retardation."
•can - digital representation of the detector output obtained
during one complete motion of the interferometer's moving
assembly or assemblies.
•caling - application of a multiplicative factor to the
absorbance values in a spectrum.
•ingle b«am •pectrua - Fourier-transformed interferogram,
representing the detector response vs. wavenumber.
Motet The term "single-beam* is used elsewhere to denote
any spectrum in which the sample and background
interferograms are recorded on the same physical absorption
path; such usage differentiates such spectra from those
generated using interferograms recorded along two physically
distinct absorption paths (see "double-beam spectrum"
above). Here, the term applies (for example) to the two
spectra used directly in the calculation of transmission and
absorbance spectra of a sample.
standard reference aaterial - a reference material, the
composition or properties of which are certified by a
recognized standardizing agency or group.
Nofe: The equivalent ISO term is "certified reference
material.•
tranmaittance, T - the ratio of radiant power transmitted by the
sample to the radiant power incident on the sample.
Estimated in FTIR spectroscopy by forming the ratio of the
single-beam sample and background spectra.
wavenuaber, v - the number of waves per unit length.
Mote: The usual unit of wavenumber is the reciprocal
centimeter, cm"1. The wavenumber is the reciprocal of the
wavelength, A, when X is expressed in centimeters.
zero-filling - the addition of zero-valued points to the end of a
measured interferogram.
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MQJ^: Performing the FT of a zero-filled interf erogram
results -in correctly interpolated points in the computed
spectrum. f^cu.
A. 2 Definitions of Mathematical Symbols
A, absorbance - the logarithm to the base 10 of the reciprocal of
the transmittance (T) .
A = loglo - = -log10T
(1)
- band area of the ich analyte in the m^ analytical
region, at the concentration (CLt) corresponding to the
product of its required detection limit (DLJ and analytical
uncertainty limit (AUJ .
- average absorbance of the ith analyte in the mth
analytical region, at the concentration (CLj) corresponding
to the product of its required detection limit (DLt) and
analytical uncertainty limit
ASC, accepted standard concentration - the concentration value
assigned to a chemical standard.
ASCPP, accepted standard concentration-pathlength product - for
a chemical standard, the product of the ASC and the sample
absorption pathlength. The units "centimeters-ppm* or
" meter s-ppm" are recommended.
AUt/ analytical uncertainty limit - the maximum permissible
fractional uncertainty of analysis for the ictl analyte
concentration, expressed as a fraction of the analyte
concentration determined in the analysis.
AVT. - average estimated total absorbance in the m analytical
region.
CKWN,, - estimated concentration of the Ic'" known interf erant.
<"MAyi - estimated maximum concentration of the ich analyte.
CPOT, - estimated concentration of the jch potential interferant.
DLlf required detection limit - for the ich analyte, the lowest
concentration of the analyte for which its overall
fractional uncertainty (OFUJ is required to be less than the
analytical uncertainty limit (AU.) .
FCm - center wavenumber position of the mch analytical region.
, fractional analytical uncertainty - calculated uncertainty
in the measured concentration of the ich analyte because of
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errors in the mathematical comparison of referenc<=> and
sample spectra.
, fractional calibration uncertainty - calculated uncertai-ty
in Che measured concentration of the i'-h analyte because of'
errors in Beer's law modeling of the reference spectra
concentrations.
FFL. - lower wavenumber position of the CTS absorption band
associated with the mch analytical region.
FFU. - upper wavenumber position of the CTS absorption band
associated with the mch analytical region.
FL. - lower wavenumber position of the mch analytical region.
FMDlf fractional nodal uncertainty - calculated uncertainty in
the measured concentration of the ich analyte because of
errors in the absorption model employed.
- lower wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands.
- upper wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands.
FRUt, fractional reproducibility uncertainty - calculated
uncertainty in the measured concentration of the ich analyte
because of errors in the reproducibility of spectra from the
FTIR system.
FUm - upper wavenumber position of the mch analytical region.
IAIja - band area of the jch potential interferant in the mch
analytical region, at its expected concentration (CPOT,) .
lAV^ - average absorbance of the ich analyte in the mch analytical
region, at its expected concentration (CPOT,) .
ISCt „ k, indicated standard concentration - the concentration
from the computerized analytical program for a single-
compound reference spectrum for the ich analyte or kctl known
interferant.
kPa - kilo-Pascal (see Pascal).
L,' - estimated sample absorption pathlength.
LJ - reference absorption pathlength.
L, - actual sample absorption pathlength.
i - mean of the MAULn over the appropriate analytical regions.
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MAUlm, minimum analyte uncertainty - the calculated minimum
concentration for which the analytical uncertainty Umi-
'^ ^Vh measurement of the i''n analyte, based on spectral
data in the m analytical region, can be maintained.
j - mean of the MIUJm over the appropriate analytical regions.
, minimum interferant uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
CPOTV/20 in the measurement of the jch interferant, based on
spectral data in the mch analytical region, can be
maintained.
MIL, minimum instrumental linewidth - the minimum linewidth from
the FTIR system, in wavenumbers.
The MIL of a system may be determined by observing an
absorption band known (through higher resolution
examinations) to be narrower than indicated by the system.
The MIL is fundamentally limited by the retardation of the
interferometer, but is also affected by other operational
parameters (e.g., the choice of apodization).
Mt - number of analytes.
Mj - number of potential interferants.
Hfc - number of known interferants.
- the number of scans averaged to obtain an interferogram.
i - the overall fractional uncertainty in an analyte
concentration determined in the analysis (OFUi = MAXfFRU^,
FCUL, FAUt, FMUt}) .
Paacal (Pa) - metric unit of static pressure, equal to one Newton
per square meter; one atmosphere is equal to 101,325 Pa;
1/760 atmosphere (one Torr, or one millimeter Hg) is equal
to 133.322 Pa.
P«ta - minimum pressure of the sampling system during the sampling
procedure.
Pf' - estimated sample pressure.
P, - reference pressure.
P, - actual sample pressure.
RMSM - measured noise level of the FTIR system in the mctl
analytical region.
RMSD, root mean iquare difference - a measure of accuracy
determined by the following equation:
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-^SD = J ~ E
\ I n / . , :
e2
where:
n = the number of observations for which the accuracy is
determined.
et = the difference between a measured value of a property
and its mean value over the n observations.
The RMSD value "between a set of n contiguous
absorbance values (At) and the mean of the values" (A.) is
defined as
RMSD =
\
- the (calculated) final concentration of the ich analyte.
RSI* - the (calculated) final concentration of the kch known
interferant.
fc.cmm' «can tiaa - time used to acquire a single scan, not
including flyback.
t,, sign*! integration period - the period of time over which an
interferogram is averaged by addition and scaling of
individual scans. In terms of the number of scans Nscan and
scan time tscan, ts = NSCan
tn - signal integration period used in recording reference
spectra.
tM - signal integration period used in recording sample spectra.
T, - absolute temperature of gases used in recording reference
spectra.
T, - absolute temperature of sample gas as sample spectra are
recorded.
TP, Throughput - manufacturer's estimate of the fraction of the
total infrared power transmitted by the absorption cell and
transfer optics from the interferometer to the detector.
VM - volume of the infrared absorption cell, including parts of
attached tubing.
wtk - weight used to average over analytical regions k for
quantities related to the analyte i; see Appendix D.
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Mote that some terms are missing, e.g., BAV^, OCU, RMS5,, Su'3:
SIC , SAC, , S-
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APPENDIX B
IDENTIFYING SPECTRAL INTERFERANTS
B . 1 G«n«ral
B.I.I Assume a fixed absorption pathlength equal to the
lS Lie
B.I. 2 Use band area calculations to compare the relative
absorption strengths of the analytes and potential interferants
In the m analytical region (FLm to FUm) , use either rectangular'
or trapezoidal approximations to determine the band areas
described below (see Reference A, Sections A. 3.1 through A.3.3);
document any baseline corrections applied to the spectra.
B.I. 3 Use the average total absorbance of the analytes and
potential interferants in each analytical region to determine
whether the analytical region is suitable for analyte
concentration determinations.
The average absorbance in an analytical region is the
band area divided by the width of the analytical region in
wavenumbers . The average total absorbance in an analytical
region is the sum of the average absorbances of all analytes
and potential interferants.
B.2 Calculation*
B.2.1 Prepare spectral representations of each analyte at
the concentration CLL = (DLt) (AU^) , where DLt is the required
detection limit and AUt is the maximum permissible analytical
uncertainty. For the m" analytical region, calculate the band
area (AAIim) and average absorbance (AAVLm) from these scaled
analyte spectra.
B.2. 2 Prepare spectral representations of each potential
interferant at its expected concentration (CPOT3) . For the m"h
analytical region, calculate the band area (IAIjm) and average
absorba'nce (IAVJB) from these scaled potential interferant
spectra.
B.2. 3 Repeat the calculation for each analytical region,
and record the band area results in matrix form as indicated in
Figure B.I.
B.2. 4 If the band area of any potential interferant in an
analytical region is greater than the one-half the band area of
any analyte (i.e., IAIjn > 0.5 AAI,m for any pair ij and any m) ,
classify the potential interferant as known interferant. Label
the known interferants k = 1 to K. Record the results in matrix
form as indicated in Figure B.2.
B.2. 5 Calculate the average total absorbance (AVTJ for each
analytical region and record the values in the last row of the
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matrix described in Figure B.2. Any analytical region wher=>
AVTm >2 . 0 is -unsuitable .
FIGURE B.I Presentation of Potential Interferant Calculations
Analytical Regions
1 .... M
Analyte Labels
AAIU . . . AAIIK
I AAIn . . . AAIIM
Potential Interferant
Labels
1 IAIn . . . IAI1M
IAI
J:
FIGURE B.2 Presentation of Known Interferant Calculations
Analytical Regions
I .... M
Analyte Labels
AAIU . ' . . . AAIIM
I - AAIn .... AAIIH
Known Interferant
Labels
1 IAI,, .... IAI,
K IAI., . . . .IAI
Total Average
Absorbance AVT, AVTN
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APPENDIX C
ESTIMATING NOISE LEVELS
C . 1 General
C.I.I The root-mean-square (RMS) noise level is the
standard measure of noise in this Protocol. The RMS noise level
of a contiguous segment of a spectrum is defined as the RMS
difference (RMSD) between the absorbance values which form the
segment and the mean value of that segment (see Appendix A)
C.I. 2 The RMS noise value in double-beam absorbance
spectra is assumed to be inversely proportional to: (a) the
square root of the signal integration period of the sample single
beam spectra from which it. is formed, and (b) to the total
infrared power transmitted through- the interferometer and
absorption cell.
C.I. 3 Practically, the assumption of. C.I. 2 allow the RMS
noise level of a complete system to be estimated from the
following four quantities:
(a) RMS^, - the noise level of the system (in absorbance
units), without the absorption cell and transfer optics,
under those conditions necessary to yield the specified
minimum instrumental linewidth. e.g., Jacquinot stop
size.
(b) t^ ~ t^le manufacturer's signal integration time used to
determine
(c) tss - the signal integration time for the analyses.
(d) TP - the manufacturer's estimate of the fraction of the
total infrared power transmitted by the absorption cell
and transfer optics from the interferometer to the
detector.
C.2 Calculation*
C.2.1 Obtain the values of RMS^, t^, and TP from the
manufacturers of the equipment, or determine the noise level by
direct measurements with the completely constructed system
proposed in Section 4.
C.2. 2 Calculate the noise value of the system (RMSEST) as
follows :
RMSEST = RMS^ TP
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APPENDIX 0
ESTIMATING MINIMUM CONCENTRATION MEASUREMENT
UNCERTAINTIES (MAU and MIU)
D.1 6«n«r«l
Estimate the minimum concentration measurement uncertainties
for the i=h analyte (MAUt) and jch interferant (MIU:) based on the
spectral data in the mch analytical region by comparing the
analyte band area in the analytical region (AAIim) and estimating
or measuring the noise level of the system (RMSEST or RMSg,,) .
Note: For a single analytical region, the MAU or MIU value
is the concentration of the analyte or interferant for which
the band area is equal to the product of the analytical
region width (in wavenumbers) and the noise level of the
system (in absorbance units). If data from more than one
analytical region is used in the determination of an analyte
concentration, the MAU or MIU is the mean of the separate
MAU or MIU values calculated for each analytical region.
D.2 Calculation*
D.2.1 For each analytical region, set RMS = RMSg,, if
measured (Appendix G) , or set RMS = RMSE3T if estimated (Appendix
C) .
D.2.2 For each analyte associated with the analytical
region, calculate
D.2.3 If only the mth analytical region is used to calculate
the concentration of the ich analyte, set MAUt = MAUim.
D 2 4 If a number of analytical regions are used to
calculate the concentration of the ich analyte, set MAUt equal to
the weighted mean of the appropriate MAU,m values calculated
above; the weight for each term in the mean is equal to the
fraction of the total wavenumber range used for the calculation
represented by each analytical region. Mathematically, if the
set of analytical regions employed is (m'}, then the MAU for each
analytical region is
D-79
-------
MAU = W.. MAU .
1 £-*• -< .*
Ke {m'}
where the weight Wilt is defined for each term in the sum as
Wi* = ( ^K * FL* ) I £ H--«p -"pJJ (7)
»* (m'>
D.2.5 Repeat Sections D.2.1 through D.2.4 to calculate the
analogous values MIUj for the interferants j = 1 to J. Replace
the value (AUi) (DLJ in the'above equations with CPOTj/20;. replace
the value AAIia in the above equations with IAIjm.
D-80
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APPENDIX B
DETERMINING FRACTIONAL REPRODUCIBILITY UNCERTAINTIES iFRU)
B.1 General
To estimate the reproducibility of the spectroscopic results
of the system, compare the CTS spectra recorded before and after
preparing the reference spectra. Compare the difference between
the spectra to their average band area. Perform the calculation
for each analytical region on the portions of the CTS spectra
associated with that analytical region.
B.2 Calculation*
E.2.1 The CTS spectra (Rl) consist of N spectra, denoted by
Su, i=l, N. Similarly, the CTS spectra {R2} consist of N
spectra, denoted by S2i, i=l, N. Each Ski is the spectrum of a
single compound, where i denotes the compound and k denotes
the set {Rk} of which Sxi is a member. Form the spectra S,
according to S3i = S2i-Su for each i. Form the spectra S4
according to S4i = [S2i+Su]/2 for each i.
E.2.2 Each analytical region m is associated with'a portion
of the CTS spectra S2i and Sn, for a particular i, with lower and
upper wavenumber limits FFLm and FFUm, respectively.
E.2.3 For each m and the associated i, calculate the band
area of S4i in the wavenumber range FFUm to FFI^. Follow the
guidelines of Section B.I.2 for this band area calculation.
Denote the result by BAVm.
E.2.4 For each m and the associated i, calculate the RMSD
of S.JL between the absorbance values and their mean in the
wavenumber range FFUm to FFLra. Denote the result by SRMSm.
E.2.5 For each analytical region m, calculate the quantity
FM. = SRMSJFFTVFFLJ/BAV,
E.2. 6 If only the mch analytical region is used to calculate
the concentration of the ich analyte, set FRU; =
E.2.7 If a number Pi of analytical regions are used to
calculate the concentration of the ich analyte, set FRUi equal to
the weighted mean of the appropriate F^ values calculated above.
Mathematically, if the set of analytical regions employed is
{m1}, then
L
FRU; = ^ WlleFMk (8)
where the Wilf are calculated as described in Appendix D.
ilt
D-81
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D-82
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APPENDIX F
DETERMINING FRACTIONAL CALIBRATION UNCERTAINTIES (FCU)
F.1 General
F.I.I The concentrations yielded by the computerized
analytical program applied to each single-compound reference
spectrum are defined as the indicated standard concentrations
(ISC's). The ISC values for a single compound spectrum should
ideally equal the accepted standard concentration (ASC) for one
analyte or interferant, and should ideally be zero for all other
compounds. Variations from these results are caused by errors in
the ASC values, variations from the Beer's law (or modified
Beer's law) model used to determine the concentrations, and noise
in the spectra. When the first two effects dominate, the
systematic nature of the errors is often apparent; take steps to
correct them.
F.I.2 When the calibration error appears non-systematic,
apply the following method to estimate the fractional calibration
uncertainty (FCU) for each compound. The FCU is defined as the
mean fractional error between the ASC and the ISC for all
reference spectra with non-zero ASC for that compound. The FCU
for each compound shall be less than the required fractional
uncertainty specified in Section 4.1.
F.I.3 The computerized analytical programs shall also be
required to yield acceptably low concentrations for compounds
with ISC=0 when applied to the reference spectra. The limits
chosen in this Protocol are that the ISC of each reference
spectrum for each analyte or interferant shall not exceed that
compound's minimum measurement uncertainty (MAU or MIU) .
F.2 Calculation*
F.2.1 Apply each analytical program to each reference
spectrum. Prepare a similar table as that in Figure F.I to
present, the ISC and ASC values for each analyte and interferant
in each- reference spectrum. Maintain the order of reference file
names and compounds employed in preparing Figure F.I.
F.2.2 For all reference spectra in Figure F.I, verify that
the absolute value of the ISC's are less than the compound's MAU
(for analytes) or MIU (for interferants).
F.2.3 For each analyte reference spectrum, calculate the
quantity (ASC-ISC)/ASC. For each analyte, calculate the mean of
these values (the FCU, for the ich analyte) over all reference
spectra. Prepare a similar table as that in Figure F.2 to
present the FCUi and analytical uncertainty limit (AUt) for each
analyte.
D-83
-------
FIGURE F. 1
Presentation of Accepted Standard Concentrations (ASC's)
and Indicated Standard Concentrations (ISCs)
GOfflgXKUKi
None
Reference
$j&0c$r$}xik
^So^B luA^H^fe:
> FOKS^tSOK
;> ASC
1; (m*&
ISCCppro)
:: ; Asatyta • "• teerferants
•• J^Wf *«*»*(»**•*«*»«•«*'*««,. J*JS*» *K* *•(*••* »K* M(* « Ji
FIGURE F.2
Presentation of Fractional Calibration Uncertainties (FCU's)
and Analytical Uncertainties (AU's)
Name
D-84
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APPENDIX Q
MEASURING NOISE LEVELS
0.1 G«n«r*l
The root-mean-square (RMS) noise level is the standard
measure of noise. The RMS noise level of a contiguous segment of
a spectrum is the RMSD between the absorbance values that form
the segment and the mean value of the segment (see Appendix A).
Q.2 Calculations
G.2.1 Evacuate the absorption cell or fill it with UPC
grade nitrogen at approximately one atmosphere total pressure.
G.2.2 Record two single beam spectra of signal integration
period tss.
G.2.3 Form the double beam absorption spectrum from these
two single beam spectra, and calculate the noise level RMS,,, in
the M analytical regions.
D-85
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D-86
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APPENDIX H
DETERMINING SAMPLE ABSORPTION PATHLENGTH ( L ) AND
FRACTIONAL ANALYTICAL UNCERTAINTY
H . 1 General
Reference spectra recorded at absorption pathlength (L.), gas
pressure (PR), and gas absolute temperature (Ts) may be used to
determine analyte concentrations in samples whose spectra are
recorded at conditions different from that of the reference
spectra, i.e., at absorption pathlength (Ls) , absolute
temperature (Ts) , and pressure (Ps) . . Appendix H describes the
calculations for estimating the fractional uncertainty (FAU) of
this practice. It also describes the calculations for
determining the sample absorption pathlength from comparison of
CTS spectra, and for preparing spectra for further instrumental
and procedural checks .
H.I.I Before sampling, determine the sample absorption
pathlength using least squares analysis. Determine the ratio
LS/LR fay comparing the spectral sets {Rl} and {R3}, which are
recorded using the same CTS at Ls and LR, and Ts and TR, but both
at PR.
H.I. 2 Determine the fractional analysis uncertainty (FAU)
for each analyte by comparing a scaled CTS spectral set, recorded
at Ls, Ts, and Ps, to the CTS reference spectra of the same gas,
recorded at LB, TR, and PR. Perform the quantitative comparison
after recording the sample spectra, based on band areas of the
spectra in the CTS absorbance band associated with each analyte.
H.2 Calculation*
H.2.1 Absorption Pathlength Determination. Perform and
document separate linear baseline corrections to each analytical
region in the spectral sets {Rl} and {R3}. Form a one-
dimensional array A, containing the absorbance values from all
segments of {Rl} that are associated with the analytical regions;
the members of the array are A^, i = 1, n. Form a similar one-
dimensional array A, from the absorbance values in the spectral
set {R3}; the members of the array are A^, i = 1, n. Based on
the model A, = rA,, + I, determine the least-squares estimate of
r', the value of r which minimizes the square error la.
Calculate the sample absorption pathlength Ls = r ' (TS/TR) LR.
H.2. 2 Fractional Analysis Uncertainty. Perform and
document separate linear baseline corrections to each analytical
region in the spectral sets {Rl} and {R4}. Form the arrays Ag
and AR as described in Section H.2.1, using values from {Rl} to
form AR, and values from {R4} to form Ag . Calculate the values
D-87
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NRMSE =
1=1
*"-I-NL; b;
(9)
and
IAAV -
A-* T \\T\\T
\ 1 - / I ij. I t r_
(10)
The fractional analytical uncertainty is defined as
FAU =
NRMS,
IA
(11)
AV
D-88
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APPENDIX I
DETERMINING FRACTIONAL MODEL UNCERTAINTIES (FMU)
I . 1 General
To prepare analytical programs for FTIR analyses, the sample
constituents must first be assumed; the calculations in this
appendix, based upon a simulation of the sample spectrum, verify
the appropriateness of these assumptions. The simulated spectra
consist of the sum of single compound reference spectra scaled to
represent their contributions to the sample absorbance spectrum;
scaling factors are based on the indicated standard
concentrations (ISC) and measured (sample) analyte and
interferant concentrations, the sample and reference absorption
pathlengths, and the sample and reference gas pressures. No
band-shape correction for differences in the temperature of the
sample and reference spectra gases is made; such errors are
included in the FMU estimate. The actual and simulated sample
spectra are quantitatively compared to determine the fractional
model uncertainty; this comparison uses the reference spectra
band areas and residuals in the difference spectrum formed from
the actual and simulated sample spectra.
I. 2 Calculation*
1.2.1 For each analyte (with scaled concentration RSAt),
select a reference spectrum SAt with indicated standard
concentration ISCL. Calculate the scaling factors
m LL1_
1 Ts LR PR ISC,
and form the spectra SACi by scaling each SAt by the factor RAt .
I 2 -.2 For each interferant, select a reference spectrum SI*
with indicated standard concentration ISC,. Calculate the
scaling' factors
RT - * S S * (13)
* Ts LR PR ISC,
and form the spectra SIC, by scaling each SI, by the factor RI,.
1.2.3 For each analytical region, determine by visual
inspection which of the spectra SAC, «d SIC, exhibit ab3ortan«
bands within the analytical region. Subtract each spectrum SAC,
and SIC, exhibiting absorbance from the sample spectrum S, tc ,
form the soectrum SUB,. To save analysis time and to avoid trie
n^oducticTofTnwanUd noise into the subtract ed spectr^ it
is recommended that the calculation be made (1) only for those
D-89
-------
spectral data points within the analytical regions, and (2) for
each analytical region separately using the original spectrum 3-.
1.2.4 For each analytical region m, calculate the RMSD of
SUBS between the absorbance values and their mean in the region
FFUm to FFLm. Denote the result by RMSSra.
1.2.5 For each analyte i, calculate the quantity
FM =
RMSSm ( FFU - FFL \ AU, DL .
= ' '
AAI
for each analytical region associated with the analyte.
1.2.6 If only the meh analytical region is used to calculate
the concentration of the ieh analyte, set FMU^FM,,.
1.2.7 If a number of analytical regions are used to
calculate the concentration of the ieh analyte, set FMt equal to
the weighted mean of the appropriate FM,, values calculated above.
Mathematically, if the set of analytical regions employed is
{m1}, then
,
(m'}
FMU, = £ Wu FM
te« (m'}
where Wix. is calculated as described in Appendix D.
D-90
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APPENDIX J
DETERMINING OVERALL CONCENTRATION UNCERTAINTIES (OCU)
The calculations in previous sections and appendices
estimate the measurement uncertainties for various FTIR
measurements. The lowest possible overall concentration
uncertainty (OCU) for an analyte is its MAU value, which is an
estimate of the absolute concentration uncertainty when spectral
noise dominates the measurement error. However, if the product
of the largest fractional concentration uncertainty (FRU, FCU,
FAU, or FMU) and the measured concentration of an analyte exceeds
the MAU for the analyte, then the OCU is this product. In
mathematical terms, set OFUi = MAX{FRUt, FCU^, FAUt, FMUJ and OCU,
MAU^}.
D-91
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D-92
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APPENDIX K
SPECTRAL DE-RESOLUTION PROCEDURES
K.1 Central.
High resolution reference spectra can be converted into
lower resolution standard spectra for use in quantitative
analysis of sample spectra. This is accomplished by truncating
the number of data points in the original reference sample and
background interferograms.
De-resolved spectra must meet the following requirements to
be used in quantitative analysis.
(a) The resolution must match the instrument sampling
resolution. This is verified by comparing a de-resolved CTS
spectrum to a CTS spectrum measured on the sampling instrument.
(b) The Fourier transformation of truncated interferograms
(and their conversion to absorbance spectra) is performed using
the same apodization function (and other mathematical
corrections) used in converting the sample • interferograms into
absorbance spectra.
X.2 Procedure*
This section details three alternative procedures using two
different commercially available software packages. A similar
procedures using another software packages is acceptable if it is
based on truncation of the original reference interferograms and
the results are verified by Section K.3.
K.2.1 KVB/Analect Software Procedure - The following
example converts a 0.25 cm"1 100 ppm ethylene spectrum (cts0305a)
to 1 cm"1 resolution. The 0.25 cm"1 CTS spectrum was collected
during the EPA reference spectrum program on March 5, 1992. The
original data (in this example) are in KVB/Analect FX-70 format.
(i) d«coap ct«0305m.mif,0305dr«»,1,16384,1
"decomp" converts cts0305a to an ASCII file with name
0305dres. The resulting ASCII interferogram file is truncated to
16384 data points. Convert background interferogram
(bkg0305a.aif) to ASCII in the same way.
(ii) compel* 0305dr««,0305dr«».aif,l
"Compose" transforms truncated interferograms back to spectral
format.
(iii) IO2SP 0305dr«fl.aif,0305dr«».d«f,3,l,low cm' ,hiffh cm
"IG2SP" converts interferogram to a single beam spectrum
using Norton-Beer medium apodization, 3, and no zero filling, 1.
D-93
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De-resoived incerferograms should be transformed using -H- 3a-e
apodization-and zero filling that will be used to colle<-- same1«
spectra. Choose the desired low and high frequencies, in cm"'
Transform the background interferogram in the same way.
(iv) DVDR 0305dr««.dBf,bkg0305a.dBf,0305dr««.dlf
"DVDR" ratios the transformed sample spectrum against the
background.
(v) XBSB 0305dr««.dlf,0305dr««.dlf
"ABSB" converts the spectrum to absorbance.
The resolution of the resulting spectrum should be verified
by comparison to a CTS spectrum collected at the nominal
resolution. Refer to Section K.3.
K.2.2 Alternate KYB/Analect Procedure — In either DOS
(FX-70) or Windows version (FX-80) use the "Extract" command
directly on the interferogram.
(i) EXTRACT CTS0305«.«if,0305dr«».aif,l, 16384
"Extract" truncates the interferogram to data points from to
16384 (or number of data points for desired nominal resolution).
Truncate background interferogram in the same way.
(ii) Complete steps (iii) to (v) in Section K.2.1.
K.2.3 Grams™ Software Procedure - Grams™ is a software
package that displays and manipulates spectra from a variety of
instrument manufacturers. This procedure assumes familiarity
with basic functions of Grams™.
This procedure is specifically for using Grams to truncate
and transform reference interferograms that have been imported
into Grams from the KVB/Analect format. Table K-l shows data
files and parameter values that are used in the following
procedure.
The choice of all parameters in the ICOMPUTE.AB call of step
3 below should be fixed to the shown values, with the exception
of the 'Apodization* parameter. This parameter should be set
(for both background and sample single beam conversions) to the
type of apodization function chosen for the de-resolved spectral
library.
D-94
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TABLE K-l. GRAMS DATA FILES AND DE-RESOLUTION PARAMETERS.
Deiired Nominal Spectral
Resolution (cm*1)
0.25
0.50
1.0
2.0
Data File Nam*
Z00250.sav
Z00500 .sav
Z01000 .sav
Z02000 .sav
Parameter "N"
Value
65537
32769
16385
8193
(i) Import using "File/Import" the desired *.aif file. Clear
all open data slots.
(ii) Open the resulting *.spc interferogram as file #1.
(iii) Xflip - If the x-axis is increasing from left to rigrht,
and the ZPD burst appears near the left end of the trace, omit
this step.
In the -Arithmetic/Calc' menu item input box, type the text
below. Perform the calculation by clicking on -OK' (once only),
and, when the calculation is complete, click the -Continue'
button to proceed to step (iv) . Note the comment in step (iii)
regarding the trace orientation.
xflip:#S«#S(#0,#lf)+50
(iv) Run ICOMFUTS.AB from 'Arithmetic/Do Program- menu.
Ignore the -subscripting error,' if it occurs.
The following menu choices should be made before execution
of the program (refer to Table K-l for the correct choice of
First: M Last: 0 Type: Single Beam
Zero Fill: Nona Apodization: (as desired)
Pharsing: User
Points: 1024 Interpolation: Linear Phase:
Calculate
(v) As in step (iii), in the -Arithmetic/Calc- menu item
enter and then run the following commands (refer to Table 1 for
appropriate -FILM,' which may be in a directory other than
•c:\mdgrams.')
aetffo 7898.8805, 0 : loadspc "c:\mdgra«s\ FIL1" : #2»#s+#2
?vi) Use -Page UP- to activate file #2, and then use the
-File/Save As- menu item with an appropriate file name to save
the result.
D-95
-------
K.3 Verification of New Resolution
K.3,1 Obtain interferograms of reference sample and
background spectra. Truncate interferograms and convert to
absorbance spectra of desired nominal resolution.
K.3.2 Document the apodization function, the level of zero
filling, the number of data points, and the nominal resolution of
the resulting de-resolved absorbance spectra. Use the identical
apodization and level of zero filling when collecting sample
spectra.
K.3. 3 Perform the same de-resolution procedure on CTS
interferograms that correspond with the reference spectra
(reference CTS) to obtain de-resolved CTS standard spectra (CTS
standards). Collect CTS spectra using the sampling resolution
and the FTIR system to be used for the field measurements (test
CTS). If practical, use the same pathlength, temperature, and
standard concentration that were used for the reference CTS.
Verify, by the following procedure that CTS linewidths and
intensities are the same for the CTS standards and the test CTS.
K.3.4 After applying necessary temperature and pathlength
corrections (document these corrections), subtract the CTS
standard from the test CTS spectrum. Measure the RMSD in the
resulting subtracted spectrum in the analytical region(s) of the
CTS band(s). Use the following equation to compare this RMSD to
the test CTS band area. The ratio in equation 7 must be no
greater than 5 percent (0.05).
RMSS x n(FFU. - FFL.)
i i i- * .05 (16)
CTS-t«tt
RMSS=RMSD in the ieh analytical region in subtracted result, test
CTS minus CTS standard.
n=number of data points per cm"1. Exclude zero filled points.
i &=The upper and lower limits (cm"1), respectively, of the
FFL- analytical region.
A.aJc.CTS=band area in the ich analytical region of the test CTS.
D-96
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D-3 EPA METHOD 25A
D-97
-------
D-98
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METEOR
METEOR 25A-DETERMINATION OF TOTAL GASEOUS ORGANIC
CONCENTRATION USING A FLAME IONIZATION ANALYZER
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total gaseous
organic concentration of vapors consisting primarily of alkanes, alkenes, and/or
arenes (aromatic hydrocarbons) . The concentration is expressed in terms of
propane (or other appropriate organic calibration gas) or in terms of carbon.
1.2 Principle. A gas sample is extracted from the source through a heated
sample line, if necessary, and glass fiber filter to a flame ionization analyzer
(FIA). Results are reported as volume concentration equivalents of the
calibration gas or as carbon equivalents.
2. Definitions
2.1 Measurement Systens. The total equipment required for the determination
of the gas concentration. The system consists of the following major subsystems:
2.1.1 Sanple Interface. That portion of the system that is used for one or more
of the following: sample acquisition, sample transportation, sample
conditioning, or protection of the analyzer from the effects of the stack
effluent.
2.1.2 Organic Analyzer. That portion of the system that senses organic
concentration and generates an output proportional to the gas concentration.
2.2 Span Value. The upper limit of a gas concentration measurement range that
is specified for affected source categories in the applicable part of the
regulations. The span value is established in the applicable regulation and is
usually 1.5 to 2.5 times the applicable emission limit. If no span value is
provided, use a span value equivalent to 1.5 to 2.5 times the expected
concentration. For convenience, the span value should correspond to 100 percent
of the recorder scale.
2.3 Calibration Gas. A known concentration of a gas in an appropriate diluent
gas.
2.4 Zero Drift. The difference in the measurement system response to a zero
level calibration gas before ar.:: after a stated period of operation during which
no unscheduled maintenance, repair, or adjustment took place.
2.5 Calibration drift. The difference in the measurement system response to
a midlevel calibration gas before and after a stated period of operation during
which no unscheduled maintenance, repair or adjustment took place.
2.6 Response Tine. The time interval from a step change in pollutant
Prepared by Emission Measurenent Rrancb EMTIC TM-25A
Technical Support Division, OAQPS, EPA June 23, 1993
D-99
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EMTIC TM-25A EMTIC NSPS TEST METHOD
concentration at the inlet to the emission measurement system to the time at
which 95 percent of the corresponding final value is reached as displayed on the
recorder.
2.7 Calibration Error. The difference between the gas concentration indicated
by the measurement system and the known concentration of the calibration gas.
3. Apparatus.
A schematic of an acceptable measurement system is shown in Figure 25A-1.
The essential components of the measurement system are described below:
3.1 Organic Concentration Analyzer. A flame ionization analyzer (FIA) capable
of meeting or exceeding the specifications in this method.
3.2 Sanple Probe. Stainless steel, or equivalent, three-hole rake type.
Sample holes shall be 4 mm in diameter or smaller and located at 16.7, 50, and
83.3 percent of the equivalent stack diameter. Alternatively, a single opening
probe may be used so that a gas sample is collected from the centrally located
10 percent area of the stack cross-section.
3.3 Sanple Line. Stainless steel or Teflon * tubing to transport the sample
gas to the analyzer. The sample line should be heated, if necessary, to prevent
condensation in the line.
3.4 Calibration Valve Assenbly. A three way valve assembly to direct the zero
and calibration gases to the analyzers is recommended. Other methods, such as
quick-connect lines, to route calibration gas to the analyzers are applicable.
3.5 Particulate Filter. An in-stack or an out-of-stack glass fiber filter is
recommended if exhaust gas particulate loading is significant. An out-of-stack
filter should be heated to prevent any condensation.
* Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
3.6 Recorder. A strip-chart recorder, analog computer, or digital recorder for
recording measurement data. The minimum data recording requirement is one
measurement value per minute, Note: This method is often applied in highly
explosive areas. Caution and care should be exercised in choice of equipment and
installation.
4. Calibration and Other Gases.
Gases used for calibrations, fuel, and combustion air (if required) are
contained in compressed gas cylinders. Preparation of calibration gases shall
be done according to the procedure in Protocol No. 1, listed in Citation 2 of
Bibliography. Additionally, the manufacturer of the cylinder should provide a
recommended shelf life for each calibration gas cylinder over which the
concentration does not change more than ±2 percent from the certified value. For
calibration gas values not generally available (i.e., organics between 1 and 10
percent by volume), alternative methods for preparing calibration gas mixtures,
such as dilution systems, may be used with prior approval of the Administrator.
Calibration gases usually consist of propane in air or nitrogen and are
determined in terms of the span value. Organic compounds other than propane can
D-100
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EMTIC TM-25A . EMTIC NSPS TEST METHOD
be used following the above guidelines and making the appropriate corrections for
response factor.
4.1 Fuel. A 4O percent H2/60 percent N2 gas mixture is recommended to avoid
an oxygen synergism effect that reportedly occurs when oxygen concentration
varies significantly from a mean value.
4.2 Zero Gas. High purity air with less than 0.1 parts per million by volume
(ppmv) of organic material (propane or carbon equivalent) or less than 0.1
percent of the span value, whichever is greater.
4.3 Low-level Calibration Gas. An organic calibration gas with a concentration
equivalent to 25 to 35 percent of the applicable span value.
4.4 Hid-level Calibration Gas. An organic calibration gas with a concentration
equivalent to 45 to 55 percent of the applicable span value.
4.5 Higk-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 80 to 90 percent of the applicable span value.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than ±3 percent of the span value.
5.2 Calibration Drift. Less than ±3 percent of span value.
5.3 Calibration Error. Less than ±5 percent of the calibration gas value.
6. Pretest Preparations
6.1 Selection of Sampling Site. The location of the sampling site is generally
specified by the applicable regulation or purpose of the test; i.e., exhaust
stack, inlet line, etc. The sample port shall be located at least 1.5 meters or
2 equivalent diameters upstream of the gas discharge to the atmosphere.
6.2 Location of Sample Probe. Install the sample probe so that the probe is
centrally located in the stack, pipe, or duct and is sealed tightly at the stack
port connection.
6.3 Measurement System Preparation. Prior to the emission test, assemble the
measurement system following the manufacturer's written instructions in preparing
the sample interface and the organic analyzer. Make the system operable.
FIA equipment can be calibrated for almost any range of total organics
concentrations. For high concentrations of organics (>1.0 percent by volume as
propane) modifications to most commonly available analyzers are necessary. One
accepted method of equipment modification is to decrease the size of the sample
to the analyzer through the use of a smaller diameter sample capillary. Direct
and continuous measurement of organic concentration is a necessary consideration
when determining any modification design.
6.4 Calibration Error Test. Immediately prior to the test series, (within 2
hours of the start of the test) introduce zero gas and high-level calibration gas
at the calibration valve assembly. Adjust the analyzer output to the appropriate
levels, if necessary. Calculate the predicted response for the low-level and
D-101
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EMTIC TM-25A EMTIC NSPS TEST METHOD
mid-level gases based on a linear response line between the zero and high-level
responses. Then introduce low-level and mid-level calibration gases successively
to the measurement system. Record the analyzer responses for low-level and mid-
level calibration gases and determine the differences between the measurement
system responses and the predicted responses. These differences must be less
than 5 percent of the respective calibration gas value. If not, the measurement
system is not acceptable and must be replaced or repaired prior to testing. No
adjustments to the measurement system shall be conducted after the calibration
and before the drift check (Section 7.3). If adjustments are necessary before
the completion of the test series, perform the drift checks prior to the required
adjustments and repeat the calibration following the adjustments. If multiple
electronic ranges are to be used, each additional range must be checked with a
mid-level calibration gas to verify the multiplication factor.
6.5 Response Tiae Test. Introduce Zero gas into the measurement system at the
calibration valve assembly. When the system output has stabilized, switch
quickly to the high-level calibration gas. Record the time from the
concentration change to the measurement system response equivalent to 95 percent
of the step change. Repeat the test three times and average the results.
7. Emission Measurement Test Procedure
7.1 Organic Measurement. Begin sampling at the start of the test period,
recording time and any required process information as appropriate. In
particular, note on the recording chart periods of process interruption or cyclic
operation.
7.2 Drift Determination. Immediately following the completion of the test
period and hourly during the test period, reintroduce the zero and mid-level
calibration gases, one at a time, to the measurement system at the calibration
valve assembly. (Make no adjustments to the measurement system until after both
the zero and calibration drift checks are made.) Record the analyzer response.
If the drift values exceed the specified limits, invalidate the test results
preceding the check and repeat the test following corrections to the measurement
system. Alternatively, recalibrate the test measurement system as in Section 6.4
and report the results using both sets of calibration data (i.e., data determined
prior to the test period and data determined following the test period) .
8. Organic Concentration calculations
Determine the average organic concentration in terms of ppmv as propane or
other calibration gas. The average shall be determined by the integration of the
output recording over the period specified in the applicable regulation. If
results are required in terms of ppmv as carbon, adjust measured concentrations
using Equation 25A-1.
*q. 25A-1
Where:
C = organic concentration as carbon, ppmv.
Organic concentration as measured, ppmv.
= Carbon equivalent correction factor.
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EMTIC TM-25A
K
K
K
K
EMTIC NSPS TEST METHOD
2 for ethane.
3 for propane.
4 for butane.
Appropriate response factor for other organic
calibration
gases.
9. libliography
1. Measurement of Volatile Organic Compounds-Guideline Series. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-450/2-78-041. June 1978. p. 46-54.
2. Traceability Protocol for Establishing True Concentrations of Gases
Used for Calibration and Audits of Continuous Source Emission
Monitors (Protocol No. 1). U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory. Research Triangle
Park, NC. June 1978.
3. Gasoline Vapor Emission Laboratory Evaluation-Part 2. U.S.
Environmental Protection Agency, Office of Air Quality Planning and
Standards. Research Triangle Park, NC. EMB Report No. 75-GAS-6.
August 1975.
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EMTIC TM-25A
EMTIC NSPS TEST METHOD
ProtM
Haatod
Sampta
Lirw
CXJ
Organic
Analyz«r
and
Recorder
Calibration
Valve
Pump
Stack
Figure 25A-1. Organic Concentration Measurement System.
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D-4 EPA DRAFT METHOD 205
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EMISSION MEASU1EMENT TECHNICAL INFORMATION CENTE1
TEST METHOM
DRAFT—DO NOT CITE OR QUOTE
The EPA proposes to amend Title 40, Chapter I, Part 51 of the Code of
Federal Regulations as follows:
1. The authority citation for Part 51 continues to read as follows-
Authority: Section 110 of the Clean Air Act as amended. 42 U.S.C. 7410.
2. Appendix M, Table of Contents is amended by adding an entry to read as
follows:
Method 205—Verification of Gas Dilution Systems for Field Instrument
Calibrations
3. By adding Method 205 to read as follows:
Method 205 - Verification of Gas •ilutioa Systems
for Field iMstraeat Calibrations
1. INTROiOCTION
1.1 Applicability. A gas dilution system can provide known values of
calibration gases through controlled dilution of high-level calibration gases
with an appropriate dilution gas. The instrumental test methods in 40 CFR Part
60 — e.g., Methods 3A, 6C, 7E, 10, 15, 16, 20, 25A and 25B -- require on-site,
multi-point calibration using gases of known concentrations. A gas dilution
system that produces known low-level calibration gases from high-level
calibration gases, with a degree of confidence similar to that for Protocol1
gases, may be used for compliance tests in lieu of multiple calibration gases
when the gas dilution system is demonstrated to meet the requirements of this
method. The Administrator may also use a gas dilution system in order to produce
a wide range of Cylinder Gas Audit concentrations when conducting performance
specifications according to Appendix F, 40 CFR Part 60. As long as the
acceptance criteria of this method are met, this method is applicable to gas
dilution systems using any type of dilution technology, not solely the ones
mentioned in this method.
1.2 Priaciple. The gas dilution system shall be evaluated on one analyzer once
during each field test. A precalibrated analyzer is chosen, at the discretion
of the source owner or operator, to demonstrate that the gas dilution system
produces predictable gas concentrations spanning a range of concentrations.
After meeting the requirements of this method, the remaining analyzers may be
calibrated with the dilution system in accordance to the requirements of the
applicable method for the duration of the field test. In Methods 15 and 16, 40
CFR Part 60, Appendix A, reactive compounds may be lost in the gas dilution
system. Also, in Methods 25A and 25B, 40 CFR Part 60, Appendix A, calibration
with target compounds other than propane is allowed. In these cases, a
laboratory evaluation is required once per year in order to assure the
Administrator that the system will dilute these reactive gases without
significant loss. Note: The laboratory evaluation is required only if the
source owner or operator plans to utilize the dilution system to prepare gases
mentioned above as being reactive.
2. SPECIFICATIONS
2.1 Gas •ilatioa Systea. The gas dilution system shall produce calibration
gases whose measured values are within ±2 percent of the predicted values. The
predicted values are calculated based on the certified concentration of the
supply gas (Protocol gases, when available, are recommended for their accuracy)
and the gas flow rates (or dilution ratios) through the gas dilution system.
Prepared by Eaisaioa Measu-eaeat Braacb EMTIC TM-205
Technical Support Division, OAQPS, EPA
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EMTIC TM-205 EMTIC NESHAP TEST METHOD
injection shall differ by more than ±2 percent from the average instrument
response for that dilution. 3.2.5 For each level of dilution, calculate the
difference between the average concentration output recorded by the analyzer and
the predicted concentration calculated in Section 3.2.2. The average
concentration output from the analyzer- shall be within ±2 percent of the
predicted value.
3.2.6 Introduce the mid-level supply gas directly into the analyzer, bypassing
the gas dilution system. Repeat the procedure twice more, for a total of three
mid-level supply gas injections. Calculate the average analyzer output
concentration for the mid-level supply gas. The difference between the certified
concentration of the mid-level supply gas and the average instrument response
shall be within +2 percent.
3.3 If the gas dilution system meets the criteria listed in Section 3.2, the gas
dilution system may be used throughout that field test. If the gas dilution
system fails any of the criteria listed in Section 3.2, and the tester corrects
the problem with the gas dilution system, the procedure in Section 3.2 must be
repeated in its entirety and all the criteria in Section 3.2 must be met in order
for the gas dilution system to be utilized in the test.
4. REFERENCES
1. "EPA Traceability Protocol for Assay and Certification of Gaseous
Calibration Standards," EPA-600/R93/224, Revised September 1993.
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D-5 HC1 VALIDATION PAPER
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D-110
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For Presentation at the Air & Waste Management Association's 90th Annual iMeeting
& Exhibition, June 8-13,1997, Toronto, Ontario, Canada
97-MP74.05
Validation of EPA FTIR Method For Measuring HC1
Thomas J. Geyer
Midwest Research Institute, Suite 350,401 Harrison Oaks Boulevard, Gary, North Carolina 27513
Grant M. Plummer
Rtio Squared, 703 Ninth Street, Suite 183, Durham, North Carolina 27705
Introduction
In 1997 EPA is preparing to publish a sampling method (Draft Method 320)1 based on the use of Fourier
transform infrared (FOR) spectroscopy to measure emissions of hazardous air pollutants (HAPs). This
method establishes sampling procedures for measuring HAPs and employs analytical procedures in the
EPA FTIR Protocol.2
In 1996 EPA conducted a field test at a source with HC1 emissions. The test goal was to use the FTIR
Draft Method 320 to measure vapor phase pollutants at this source. Measurements were conducted on
the inlet and outlet of a control device. Hydrogen chloride (HC1) was a target pollutant for this source
and, for this reason, some samples were spiked from a cylinder containing a standard concentration of
103 ppm HC1. Results of HC1 measurements are presented along with a Method 3013 statistical analysis
of spiked and unspiked samples, and a comparison of results obtained using EPA reference spectra and
results obtained using spectra of the HO gas standard to measure the sample concentrations.
Experimental
The source tested in this project was a coal burning process with a relatively low moisture content (3 to
4% by volume). Flue gas temperatures were between 400 and 500°F. The principal components of the
gas stream were water vapor, CO:, SOz, and NO.
Sampling System
The sampling system is depicted in Figure 1. The sample was extracted through a 4-ft long, 0.5-in
diameter stainless steel probe. Sample was transported through heated 3/8-in Teflon line using a KNF
Neuberger heated head sample pump (Model NO35 ST. 1II). A Balston paniculate filter (holder Model
Number 30-25, filter element Model Number 100-25-BH, 99 percent removal efficiency at 0.1 ^m) was
connected in-line at the outlet of the sample probe. The sample line was heat wrapped and insulated.
Temperature controllers were used to monitor and regulate the sample line temperature at about 350° F.
The stainless steel manifold contained 3/8-in tubing, rotameters and 4-way valves to monitor and control
the sample flow to the FTIR gas cell. The manifold temperature was maintained between 300 to 310°F.
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97-MP74.05
The FTIR system included an Analect instruments Model RFX-40 interferometer equipped with a broad
band MCT detector. Samples were contained in an Infrared Analysis Model D22H variable path gas cell.
The cell temperature was maintained at 250°F.
Sampling Procedure
A series of discreet batch samples was collected by filling the cell above ambient pressure and closing the
inlet valve to isolate the sample. An outlet valve was briefly opened to vent the sample to ambient
pressure. The spectrum of the static sample was recorded. Then the cell was evacuated for the next
sample. Each spectrum consisted of 50 co-added scans. The minimum time between consecutive
samples was about 2 minutes. Inlet and outlet runs were conducted at the same time: the two location
were sampled alternately with the one FTIR system. The minimum time between consecutive
measurements was about 3 to 5 minutes.
Path Length Determinations
Two path lengths were used in this test The cell was adjusted to 40 beam passes for the first two test
runs and reduced to 20 beam passes for a third test run. The number of beam passes was measured by
shining a He/Ne laser through the optical path and observing the number of laser spots on the field
minor. The path lengths in meters were determined by comparing CTS EPA reference spectra to the
CTS spectra collected at each path length.
Absorption path lengths were determined from a comparison of the field test CTS spectra and EPA
library CTS spectra of ethylene (CzrU). For high temperature spectra, the EPA library interferograms
ctsOl 15a.aif and bkgOl 15a.aif were de-resolved to the appropriate spectral resolution (either 1 or 2 cm"1)
according to the procedures of reference 2 (Appendix K). The same procedure was used to generate
low-temperature spectra from the original interferometric data in the EPA library files cts0829a.aif and
bkg0829a.aif. The resulting files were used in least squares fits to the appropriate field CTS spectra (see
reference 2, Appendix H) in two regions (the FP, or "fingerprint" region from 790 to 1139 cm"' and the
CH, or "CH-stretch region" from 2760 to 3326 cm'1). The fit results for each region, test, and set of test
sampling conditions were averaged. They and their average uncertainties are presented in Table 1. The
CH values were used in analytical region 4 where HC1 was measured.
Analyte Spiking
Draft Method 3201 contains a procedure for spiking the flue gas with one or more of the target analytes.
The spike procedure closely follows Section 6.3 of reference 3. The primary purpose of analyte spiking
is to provide a quality assurance check on the sampling system to determine if analyte losses occur in
transport to the analyzer. A second purpose is to test the analytical program to verify that the analyte(s)
can be measured in the sample matrix. If at least 12 (independent) spiked and 12 (independent) unspiked
samples are measured then a Method 301 statistical analysis can be performed on the results to "validate"
the method.
Figure 1 shows the sampling configuration used for the analyte spike. This procedure is described in
detail elsewhere1. In this test, a measured flow of the gas standard was preheated to the sample line
temperature before being introduced into the extracted flue gas at the back of the probe. The spiked
sample then passed through all of the sample components to the gas cell where the spectrum was
recorded. A series of unspiked samples was measured, the spike was turned on and then a complete
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97-MP74.05
series of spiked samples was measured. The spike then was turned off to make additional unspiked
measurements. Ideally, the spike comprises 1/10 or less of the sample mixture. The dilution is estimated
by comparing the spike flow to the total flow, but the actual dilution is determined measuring a tracer
(SF6) concentration in the spiked samples and comparing that to tracer concentration in the undiluted gas
standard.1
Usually the tracer is spiked with the analyte standard. In this test the SF6 standard and HC1 standard
were contained in separate cylinders so the SF6 was spiked first, then the HC1 was spiked, and finally the
SF6 was spiked again. The total sample flow stayed constant during the entire sampling period. The
spike flow was also held constant to insure that the dilution ratio was the same when the SF6 was spiked
as when the HC1 was spiked.
Quantitative Analysis
FTIk analysis is performed in two steps: (1) collecting spectra of samples, and (2) analyzing the spectra
to determine concentrations of detected compounds. The quantitative analysis step usually is performed
with an automated program that relates sample absorbance intensities to absorbance intensities at known
concentrations in reference spectra.2 The Protocol2 describes procedures for preparing reference spectra
and Method 3201 requires the analyst to use reference spectra prepared with the Protocol procedures. To
date, the only existing set of reference spectra for HC1 and most Clean Air Act HAPs is in the EPA FTIR
spectral library (http:/Anfo.arnold.af.mil/cpa/welcome.htm).
The Calibration Transfer Standard2 is the key requirement in using reference spectra for quantitative
analysis. CTS spectra help the analyst characterize differences in resolution, path length, temperature,
and sample pressure between the instrument system used to collect reference spectra and the system used
to collect the sample spectra. Table 1 illustrates how the CTS spectra were used to determine the optical
path lengths for the system used in this test The HC1 reference spectra were de-resolved in the same way
as the CTS reference spectra before they were used in the quantitative analysis.
References 4 through 8 comprise a thorough description of one technique for analyzing FTIR absorbance
spectra. Two different analytical routines were used in this study. The first was prepared by Rho
Squared using the programming language ARRAY BASIC™ (GRAMS,™ Version 3.02, Galactic
Industries Corporation, Salem, New Hampshire). The "classical least squares" (CLS) or "K-Matrix"
technique and the associated computer program "4FIT" are described in Reference 9. The terminology
and basic analytical approach employed in this work are described in the "EPA FTIR Protocol"
(Reference 2). The second routine used the K-matrix analytical program "Multicomp" version 6.0
(Analect Instruments).
The two analyses were performed independently by different analysts and then compared without
modification.
Reference Spectra
The program "4FTT" used as input EPA FTIR library spectra of HC1 de-resolved to 1 cm'1 and
normalized for absolute temperature, concentration, and absorption path length. The resulting files were
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97-MP74.05
averaged to provide a "-reduced absorptivity" (see Reference 9), which was stored in the spectral file
O97.alf and employed in all subsequent HC1 analyses. The HC1 analysis was applied to the de-resolved
EPA library HC1 spectra to determine the fractional calibration uncertainty (FCU) which is presented in
Table 2.
During the test MRI recorded spectra of samples taken directly from an HC1 cylinder standard (103 ppm
HC1 in nitrogen, ± 5% accuracy from Scott Specialty Gases). Four independent HC1 "calibration" spectra
were measured at each of the two instrument configurations used to collect the data presented in Figures
2 and 3. The Fractional Calibration Uncertainty for each set of four spectra and the analytical region for
the "Multicomp" analysis is presented in Table 2.
Even though the two sets of results are identified by the program names "4FTT" and "Mulitcomp," it is
important to note that the "Multicomp" results were reproduced by the program "4FTT" when the HC1
calibration spectra were used as input for "4FTT." Therefore, any differences in the analyses are not
attributable to the programs, but to the use of different input spectra.
Results
HCI Concentrations
Table 3 summarizes results from the three test runs at the two locations. The agreement between the
"4FTT" and the "Multicomp" analyses is very good except for the third run. This run was conducted after
the path length had been decreased from 40 to 20 laser passes.
The two comparisons plotted in Figures 2 and 3 are indicated in Table 3. The Run 2 outlet results
(Figure 2) are typical of those obtained for the Run 2 inlet results recorded on the same day and the Run
1 inlet and outlet results recorded a day earlier. The close agreement was typical also for two data sets
collected at another field test in one test run. For 3 of the 6 data sets presented in Table 3, the results
obtained with program "4F1T," using de-resolved EPA library reference spectra and the CTS-derived
absorption path lengths, are nearly identical (within the 4 a uncertainty) to those obtained using
"Multicomp," which employed the field HCI calibration standard spectra without an explicit absorption
path length determination. The average percent difference of the Run 2 inlet results was slightly higher
than the 4a uncertainty, but this percent difference corresponded to an average difference of 1.7 ppm.
The error bars in Figures 2 and 3 correspond to the 4a statistical uncertainties in the "4FTT" HCI
concentrations.
Method 301 Analysis
Tables 4 and 5 present the results of the method 301 statistical analysis of the spiked and unspiked
"4FTT" and "Multicomp" Run 3 outlet results, respectively. Note that the nearly constant difference of
about 19 percent in the two analyses has almost no effect on the Method 301 statistical analyses, which
indicate no significant bias in the HCI measurements. This is because the statistical treatment analyzes
differences between spiked and unspiked measurements and compares the differences to an expected
value of the spike. Since the same offset is apparent in the "Multicomp" analysis of both the spiked and
unspiked results, the calculated bias is not affected.
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97-MP74.05
This is another indication that the difference in the "4FIT" and "Multicomp" run 3 results is not due to a
measurement or analytical error. It is likely due either to an anomaly in the Run 3 path length
determination for the CH stretch region or to an error associated with using the HC1 "calibration spectra
as input for the "Multicomp" program. As stated above, the "4FIT" program reproduced the
"Multicomp" results when using the HC1 "calibration" spectra as input
Discussion
The uncertainties for the four data sets in Runs 1 and 2 are approximately equal to the small differences
between the "4FIT" and "Multicomp" results. The excellent agreement of the two analyses is noteworthy
for several reasons. HC1 is notoriously difficult both in terms of sampling and data analysis, due
(respectively) to the compound's high chemical reactivity and the details of the infrared spectrum which
make the analysis susceptible to instrument resolution errors. The results also provide a direct
comparison between two fundamentally different analytical approaches, one relying on in situ calibration
of the instrument using actual calibration gas standards, and the other using the calibration transfer
concept.
This comparison is somewhat clouded by the results depicted in Figure 3, which show the HC1
concentration determined during Run 3 at the outlet These are also typical of the results for another data
set recorded on the same day at the inlet Unlike the Runs 1 and 2 data, the Run 3 data indicate a
statistically meaningful difference of approximately 18% between the "4FIT" and "Multicomp" results.
We stress that this difference is not attributable to errors in the computer programs, which produced
reliable results in these and many independent test cases. Rather, the difference seems be related to an
anomaly in the absorption path length determinations presented in Table 1. Note that the CTS-derived
absorption path length for (nominally) 20 passes, corresponding to the Run 3 data, are 10.2 meters 14.3
meters for the CH-stretch and "fingerprint" (FP) analytical regions. The difference between the CH and
FP results is much larger for this particular day of testing than on the other two test days, represented in
the table by the 16- and 40- pass results. (It is also anomalous with respect to results obtained using the
same instrument in another field test completed within nine days of the testing addressed here.)
Moreover, were the average of the CH and FP region values (12.2 meters) used for the HC1
concentration values rather than the CH region value of 10.2 meters, the level of agreement between the
two sets of analytical results for the Run 3 data would be comparable to that of the Run 1 and 2 data
discussed immediately above.
We have attempted to determine the cause of this difference by considering of a number of possible
operational and instrumental problems. However, no single systematic effect seems sufficient Because
consistent path length determinations were carried out both before and after the HC1 measurements in
question, a sudden change in instrument performance must be ruled out Gas pressure and dilution
effects cannot cause the type of wavenumber-dependent effects observed in the CTS spectra; subsequent
laboratory measurements of CjH* indicated that temperature variations, like pressure and dilution effects,
would lead to path length errors in the same direction for the CH and FP regions. Because the same EPA
CTS ethylene spectra were used in all the path length determinations and led to excellent statistical results
in all cases, potential data processing errors in the deresoluton procedure are also insufficient to explain
D-115
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97-MP74.05
the anomalous results. However, we note that the observed 18% discrepancy still allows high confidence
in the data and the infrared technique, and the discrepancy is obvious mainly because of the overall high
quality of the data set and statistical results.
Conclusions
The evaluation presented in this paper demonstrates that the EPA FTIR Protocol analytical procedures
based on the use of laboratory reference spectra to determine analyte concentrations in sample spectra
give excellent, and verifiable, results. This is true even for HC1, which is difficult to sample, and even
when the reference spectra are deresolved to match the sample spectra.
Two independent analyses using different programs and different spectral input data were performed on 6
FTIR data sets collected at a site with HC1 emissions. The alternate analyses produced nearly identical
results in 4 of the data sets. In two of the data sets the agreement was also good, but the average
discrepancy of about 18 percent between results produced by the alternate analyses was larger than the
average measurement uncertainty of about 5.5 percent. A preliminary evaluation of this discrepancy has
not determined the exact cause, but it is probably attributable to an anomaly in the measurement of the
absorption path length for the one test run.
These results also demonstrate the need for careful instrument performance checks and preparation of
library reference spectra. Strict QA/QC standard procedures are required to produce accurate
measurements. The Method 301 validation results showed no significant bias in the FTIR measurements
of HC1 at this test, but the validation procedure cannot reveal a constant offset "error" that is applied
equally to both spiked and unspiked samples.
Acknowledgments
The field test discussed in this paper was funded by the Emission Measurement Center of the United
States Environmental Protection Agency.
References
1) Draft Method 320, "Measurement of Vapor Phase Organic and Inorganic Emissions by Extractive
Fourier Transform Infrared (FTIR) Spectroscopy," EPA Contract No. 68-D2-0165, Work Assignment
3-08, July, 1996.
2) "Protocol For The Use of FTIR Spectrometry to Perform Extractive Emissions Testing at
Industrial Sources," EPA Contract No. 68-D2-0165, Work Assignment 3-12, EMTIC Bulletin Board,
September, 1996.
3) "Method 301 - Field Validation of Pollutant Measurement Methods from Various Waste Media," 40
CFR Part 63, Appendix A.
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4. D.M. Haaland and R.G. Easterling, "Improved Sensitivity of Infrared Spectroscopy by the Application
of Least Squares Methods," Appl. Soectrosc. 34(5):539-548 (1980).
5. D.M. Haaland and R.G. Easterling, "Application of New Least-Squares Methods for the Quantitative
Infrared Analysis of Multicomoonent Samples." Appl. Spectrosc. 36(6):665-673 (1982).
6. D.M. Haaland, R.G. Easterling and D.A. Vopicka, "Multivariate Least-Squares Methods Applied to
the Quantitative Spectral Analysis of Multicomponent Samples," Appl. Soectrosc. 39(l):73-84 (1985).
7. W.C. Hamilton, Statistics in Physical Science. Ronald Press Co., New York, 1964, Chapter 4.
8. P.R. Griffiths and J.A. DeHaseth, Fourier Transform Infrared Spectroscopv. John Wiley and Sons,
New York, 1986, ISBN 0-471-09902-3.
9. G. M. Plummet and W. K. Reagen, "An Examination of a Least Squares Fit FTIR Spectral Analysis
Method," Air and Waste Management Association. Paper Number 96-WA65.03, Nashville, 1996.
10. T. J. Geyer, "Method 301 Validation of Fourier Transform Infrared (FTIR) spectroscopy
For Measuring Formaldehyde and Carbonyl Sulfide," Air and Waste Management Association. Paper
Number. 96-RA110.03, Nashville, 1996.
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Table 1. Pathlength Determination Results.
97-MP74.05
CTS Conditions
# Passes Temp (K)
16 293
Run 3 (Figure 3)
Run2 (Figure 2)
20 293
20 393
40 293
40 393
CH region
Result (m) % uncert.
6.5 2.9
11.0 2.6
10.2 2.5
19.2 5.5
20.2 2.6
•"• «— • *m*mmmmm mmmm mmmm.
FP region
Result (m) % uncert.
6.7 1.3
11.3 1.6
14.3 2.2
20.0 1.8
23.4 1.6
Table 2. Fractional Calibration Uncertainties (FCU in Reference 2) For the Two Quantitative Analyses.
Compound
HC1 "4fit"
HC1 "Mcomp"
Run 2*
Run 3*
FCU(%)
4.6
1.05
3.14
Analytical Region (cm'1)
2747 - 2848
2569-2871
* Spectra of four samples from the cylinder standard (103 ppm HC1 in nitrogen) were used in the
"Mcomp" analysis. The spectra were measured at the same instrument configuration used in each run.
Table 3. Summary of results comparisons in 4 runs (8 data sets).
Data Set
Run 1 Inlet
Run 1 Outlet
Run 2 Inlet
Run 2 Outlet (Figure 2)
Run 3 Inlet
Run 3 Outlet (Figure 3)
Average "4FTF'
Results
HCI ppm % 4 * o '
43.3 3.9
34.5 4.1
14.8 7.7
48.0 4.5
62.5 5.6
58.0 5.5
Average "Multicomp"
Result
HCI ppm
42.1
32.9
13.1
46.4
50.9
47.3
% Difference '
2.9
4.4
11.8*
3.2
18.6
18.4
No. of Results 3
36
30
16
33
41
52
1 - Average percent uncertainty in the 4FTT results.
2 - Equals (4FIT-Multicomp)/4FIT.
3 - Equals the number of spectra included in the average. Results from condenser and ambient air
samples were not included in the averages.
4 - Flow restriction during this run may have caused HCI losses resulting in lower measured
concentrations for this run. An average difference of 1.7 ppm corresponded to a relatively large percent
difference of 11.8 % on the smaller average concentration for this run.
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Table 4. Method 301 statistical analysis of "4FIT" HC1 results in Figure 3.
97-MP74.05
Run Average =
Statistical
Results
Unspiked
HClppm
SD =
F =
RSD=
Bias =
t =
di (dO2
2.093
0.491
3.7
-0.088
0.12
HC1 ppm
62.14 *
SD =
SD— "
Exp Cone =
Spiked
di
4.74
1.466
1.807
5.05
1.02
(d,)2
25.784
* Represents the average result in 12 unspiked or spiked samples. Statistical variables are described in
Section 6.3 of EPA Method 301.3 Procedure for determining spiked dilution factor and expected
concentration, Exp Cone, is described in reference 10.
Table 5. Summary of Method 301 statistical analysis of "Multicomp" results in Figure 3.
Unspiked
Run Average =
Statistical
Results
HG ppm
45.88 *
SD =
F =
RSD»
Bias s
t =
d , (d i)2
8.62 34.242
1.689
0.628
3.7
•0.070
0.11
Spiked
HC1 ppm
50.86 *
SD =
SDpoo,ed =
Exp Cone =
CF =
di
3.51
1.338
1.524
5.05
1.01
(di)2
21.496
* Represents the average result in 12 unspiked or spiked samples. Statistical variables are described in
Section 6.3 of EPA Method 301.3 Procedure for determining spiked dilution factor and expected
concentration, Exp Cone, is described in reference 10.
D-H9
-------
Figure 1. Extractive sampling system.
to
o
Uiihcalcd Lliu:
Healed Line
4-
o
L/l
-------
APPENDIX E
PROCESS DESCRIPTION
-------
-------
This process description was prepared by EC/R Incorporated and was provided to MR1 by
the Emission Measurement Center. The process description was included in this report without
review by MRI.
E-l
-------
E-2
-------
PROCESS DESCRIPTION FOR CLAYTON FACILITY
Facility Description
The ^ Construction Asphalt Concrete Production
Facility in Clayton, North Carolina, has been in operation since
1989. It is a counter flow, continuous drum mix process. The
dryer/mixer is an ASTEC double-barrel drum, a variation of the
drum mixer, with a rated capacity of 400 tons per hour. The
plant has the capability of producing up to 15 asphalt mix types,
with or without the use of reclaimed asphalt pavement (RAP)
Asphalt concrete, called "hot mix asphalt"(HMA) by the
industry, is a mixture of well-graded, high quality virgin
aggregate that is heated and mixed with liquid asphalt cement to
produce paving material. The characteristics of the asphalt
concrete are determined by the relative amounts and types of
aggregate (and RAP) used. In the asphalt reclamation process,
old asphalt pavement is removed from the road surface,
transported to the plant, and crushed and screened to the
appropriate size for further processing.
In the counter flow continuous double-barrel drum mix
process, virgin aggregate of. various sizes is fed to the drum by
cold feed controls in proportions dictated by the final mix
specifications. Aggregate is delivered by conveyor belt to the
inner drum, entering at the opposite end as the burner (hence,
the descriptor "counter* flow). The aggregate moves towards the
burner within the inner drum and is dried. The hot aggregate
falls to the outer drum through holes at the burner end of the
inner drum. As the hot aggregate moves along the outer drum,
liquid asphalt cement and conditioner (if used) are added. The
liquid asphalt cement and conditioner are delivered to the drum
mixer by a variable flow pump that is electronically linked to
the aggregate feed weigh scales. Recycled dust from the control
system and RAP (if used) are also added into the outer drum. The
resulting asphalt concrete mixture is discharged from the outer
drum and conveyed to storage silos for delivery to trucks.
There are five cold storage bins and three hot mix storage
silos at Clayton facility. The hot mix storage
silo capacity is 200 tons each, for a total of 600 tons. There
are three screens for aggregate sizing and one 52,000 gallon (130
ton) heated asphalt cement storage vessel. The plant uses virgin
and recycled No.2 fuel oil, supplied by Noble Oil Services, Inc.,
for all its process fuel needs. (Recycled fuel assay report is
attached). Virgin fuel oil is used during extremely cold weather
and/or if there is a fuel-related problem with the burner.
Therefore, virgin fuel is usually only used during the winter
months (January/February). The amount of energy needed from the
E-3
-------
fuel for the asphalt production process is 225,600 BTU per ton of
asphalt produced. The hot gas contact time with the aggregate is
approximately I minute, and the process time from the beginning
of the drum to- the coater is approximately 6 minutes.
Clayton facility uses an asphalt cement (AC)
called AC-20, obtained from Citgo of Wilmington, North Carolina.
An anti-strip conditioner, called Perma-Tac (from Arr-Maz), is
sometimes used; antistrip is required for all NC DOT jobs.
(Conditioner MSDS is attached). For particulate matter (PM)
control, the facility uses a fabric filter. The
fabric filter is an ASTEC Pulse-Jet, equipped with 1024 14-ounce
Nomex bags; it is operated with an air-to-cloth ratio of 5.54
feet per minute. The process gas exits the drum and coater and
proceeds into the fabric filter, where it is exhausted through a
stack. As mentioned above, the dust collected by the PM control
devices is recycled to process.
Source Tests
EPA source tests were performed at Clayton
facility on August 19, 20, and 21, 1997. The source testing took
place at the inlet and outlet of the fabric filter. Data were
taken at 15-minute intervals during the entire "test period,'
i.e. the time period when at least one manual and both
instrumental tests were running. According to plant personnel,
the plant was operating under normal conditions during the tests.
Four tests were performed during the three-day test period.
(Two test runs were performed on August 20: one in the morning
and one in the afternoon). The average asphalt concrete
production rates during the four test runs were 171, 276, 240,
and 185 tons per hour (tph), respectively, corresponding to total
production of 735, 1,187, 840, and 778 tons. During the first
three test runs (August 19, August 20 a.m., and August 20 p.m.),
a surface asphalt coating that included RAP was produced; during
the fourth test run (August 21), a surface coating (accounting
for 75 percent of the total asphalt concrete produced) and a
binder coating (accounting for 25 percent of total production)
were produced, both without RAP. Recycled No. 2 fuel oil was
used for fuel in the production process during the tests.
Conditioner was used during the four test runs at a rate of
0.25 percent of the asphalt cement used, for a total of 186, 302,
220, and 200 pounds, respectively, during the four test runs. No
visible emissions were observed by EC/R Inc. personnel during the
source tests.
E-4
-------
Table 1 that follows summarizes the operating conditions
observed during the EPA source test periods at
Clayton facility. Tables 2 and 3 describe the asphalt mixes
produced and the fuel used, respectively, during the tests.
Table 4 describes the specifics of plant operation during the
tests. Appendix A shows all the data recorded during the tests,
along with the results of statistical analyses.
E-5
-------
TABLE 1. PLANT OPERATING CONDITIONS DURING
SOURCE TESTS, AUGUST 19, 20, AND 21, 1997
m
Process Data
Product Type(s)'
Asphalt Concrete
Production Rate,
tph
Average"
Range
Total Produced,
tons
Mix Temperature,
°F
Average"
Range
Raw Material
(Virgin Aggregate)
Use Rate, tph
Average15
Range
Total Used, tons
Test Run / Test Date
Run 1
08/19/97
surface mix,
with RAP
(BCSC, Type
RDS)
171
146-254
735
305
295-315
145
126-213
622
Run 2
08/20/97
(a.m.)
surface mix,
with RAP
(BCSC, Type
RDS)
276
223-302
1,187
312
303-346
236
191-255
1,013
Run 3
08/20/97
(p.m.)
surface mix,
with RAP
(BCSC, Type
RDS)
240
152-254
840
310
299-322
205
138-215
718
Run 4
08/21/97
surface mix,
no RAP (BCSC,
Type HDS) ;
and binder
(BCBC, Type H)
185
150-204
778
308
271-351
176
142-194
740
-------
TABLE 1. (continued)
W
Process Data
RAP
Use rate, tph
Average13
Range
Total Used, tons
Asphalt Cement
Use rate, tph
Average13
Range
Total Used, tons
Conditioner (lb)c
Fabric Filter
Operation13
Temperature, °F
Inlet
Outlet
Pressure Drop,
inches water
Average"
Range
Fuel
Use Rate,d gph
Total Used, gal
Test Run / Test Date
Run 1
08/19/97
18
13-27
76
8.7
7.5-12.6
37
186
193
170
1.8
1.5 - 2.9
214
920
Run 2
OB/20/97
(a.m. )
28
21-32
119
14.0
11.4-15.5
60
302
255
214
3.3
2.1-4.0
410
1,762
Run 3
OB/20/97
(p.m.)
24
17-27
85
12.3
7.8-13.0
43
216
232
195
2.5
1.8-2.9
334
1,168
Run 4
OB/21/97
none
9.2
7.8-10.6
39
200
201
175
1.9
1.8-2.0
280
1,117
-------
TABLE 1. (continued)
w
oo
Process Data
Visible Emissions
Test Run / Test Date
Run 1
08/19/97
none
Run 2
08/20/97
(a.m. )
none
Run 3
08/20/97
(P.m.)
none
Run 4
08/21/97
none
BCSC, Type HDS = bituminous concrete, surface coarse, type high density surface
BCSC, Type RDS = bituminous concrete, surface coarse, type high density surface
with RAP
BCBC, Type H = bituminous concrete, binder coarse (type H)
See Table 2 for more detail on product specifications.
As a straight average of the 15-minute interval data shown in Appendix A.
The amount of conditioner used was calculated as 0.25 percent of the asphalt cement
Fuel use rate was calculated from the total fuel used during the time interval.
-------
TABLE 2.
ASPHALT MIX SPECIFICATIONS
Product
Surface
(BCSC,
Coating
Type HDS)
Surface Coating, with
RAP (BCSC, Type RDS)
Binder
(BCBC, Type H)
Material
78-M
screenings
sand
asphalt cement
conditioner
78-M
dry screenings
natural sand
RAP
asphalt cement total
additional
from RAP
conditioner
78-M
#67
screenings
sand
asphalt cement
conditioner
Amount
50% aggregate
30% aggregate
20% aggregate
5 .2% mix
0.25% cement
43% aggregate
27% aggregate
20% aggregate
10% aggregate
5 . 1% mix
4.6% mix
0.5% mix
0.25% cement
16% aggregate
46% aggregate
20% aggregate
18% aggregate
4.5% mix
0.25% cement
TABLE 3.
FUEL SPECIFICATIONS
Fuel Type
Oil
Characteristics
flash point
lead
sulfur
150°F
28 mg/kg
3590 mg/kg
(0.36%)
Descriptor ( s )
recycled no . 2
diesel fuel
E-9
-------
TABLE 4. SPECIFICS OF PLANT OPERATION DURING
EPA SOURCE TESTS
Parameter
Test Period
Plant Shut
Downs'
(with
approximate
duration)
Plant
Production
Rate Change (s)
Product
Changes
Test Run / Test Date
Run 1
08/19/97
0915-1456
none
1115-1145:
mix rate
slowed from
nominally
250 to 200
tph
1200-1500:
mix rate
slowed from
nominally
200 to 150
tph
none
Run 2
08/20/97
(a.m. )
0822-1240
0930(4
min)
0945-
1245: mix
rate
increased
from
nominally
225 to
300 tph
none
Run 3
08/20/97
(p.m.)
1405-1735
none
1715-
1745: mix
rate
decreased
from
nominally
250 to
150 tph
none
Run 4
08/21/97
0741-1153
none
1030-1200:
mix rate
increased
from
nominally
180 to 200
tph
0730-0815,
0900-0915,
1015-1155:
HDS produced
(600 tons)
0830-0900,
0915-1000,
1155-1200:
binder
produced 195
tons)
Shutdown occured because the RAP feed went down.
E-10
-------
Appendix A: Process Data
Test Run 1
Test Date: August 19, 1997
Total Test Time: 4.3 hrs
Time
0915
1100
1115
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1430
1445
1456
Total**
Mean
St. Dev
Min
Max
Event
*
*
*
Product
Type
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
Asphalt Concrete
Production
Rate
(TPH)
250
254
202
202
200
150
152
149
150
152
150
150
149
147
146
150
151
171
35
146
254
Total
(tons)
735
Asphalt
Temp.
(oF)
315
304
295
311
304
299
306
306
300
300
300
310
301
313
307
305
304
305
5
295
315
Aggregate Use
Rate
(TPH)
213
211
171
170
168
127
126
127
127
128
127
128
127
127
127
128
129
145
29
126
213
Total
(tons)
622
RAP Use
Rate
(TPH)
26
27
22
21
21
15
16
16
15
16
16
15
15
13
15
15
15
18
4
13
27
Total
(tons)
76
Asphalt
Cement Use
Rate
(TPH)
12.5
12.6
10.2
10.0
10.0
7.8
7.5
7.7
7.7
7.6
.7.8
7.6
7.7
7.6
7.5
7.7
7.7
8.7
1.7
7.5
12.6
Total
(tons)
37
Calculated
Conditioner Use
Rate
(TPH)
0.03
0.03
0.03
0.03
0.03
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.004
0.02
0.03
Total
(tons)
0.093
* See Table 4 for a description of these events.
** Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 1
Test Date: August 19, 1997
Total Test Time: 4.3 hrs
Time
0915
1100
1115
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1430
1445
1456
Total**
Mean
St. Dev
Min
Max
Event
*
*
*
Product
Type
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
Fabric Filter
Inlet
Temp.
(oF)
245
240
220
205
205
180
175
185
180
180
185
185
182
180
180
180
170
193
22
170
245
Outlet
Temp.
(oF)
200
200
195
185
180
170
160
160
160
160
160
160
160
160
160
160
160
170
15
160
200
Pressure
Drop
(in. H20)
2.9
2.5
2.5
2.0
2.0
1.8
.5
.5
.8
.5
.5
.5
.7
.5
.5
.5
.5
1.8
0.4
1.5
2.9
Fuel Use
Rate
(GPM)
5
5
5
5
3
3
3
3
3
3
3
3
3
3
3
3
3
3.5
0.9
3.0
5.3
Total
(gal)
80
1693
1817
1855
1911
1994
2036
2092
2136
2192
2234
2274
2336
2388
2441
2489
2533
920
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
* See Table 4 for a description of these events.
"Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 2
Test Date: August 20, 1997 a.m.
Total Test Time: 4.3 hrs
Time
0822
0845
0900
0915
0930
0945
0100
1015
1030
1045
1100
1115
1130
1145
1200
1215
1230
1240
Total**
Mean
St. Dev
Min
Max
Event
*
*
Product
TYDC
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS_J
RDS
RDS
Asphalt Concrete
Production
Rate
(TPH)
225
226
223
225
223
249
298
299
301
300
300
301
302
300
300
300
298
299
276
34
223
302
Total
(tons)
1,187
Asphalt
Temp.
(oF)
306
304
316
306
346
308
312
314
308
314
303
314
309
311
317
307
313
310
312
9
303
346
Aggregate Use
Rate
(TPH)
192
191
192
191
214
213
254
254
255
254
255
253
255
255
254
252
255
253
236
27
191
255
Total
(tons)
1,013
RAP Use
Rate
(TPH)
21
24
22
23
24
25
30
30
30
31
26
32
31
31
30
31
29
30
28
4
21
L 32
Total
(tons)
119
Asphalt
Cement Use
Rate
(TPH)
1.5
1.5
1.5
1.4
1.5
12.7
15.3
15.5
15.3
15.2
15
15
15
15.4
15.3
15
15
15
14.0
.7
11.4
15.5
Total
(tons)
60
Calculated
Conditioner Use
Rate
(TPH)
0.03
0.03
0.03
0.03
0.03
0.03
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.04
0.00
0.03
0.04
Total
(tons)
0.151
w
* See Table 4 for a description of these events.
** Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 2
Test Date: August 20, 1997 a.m.
Total Test Time: 4.3 hrs
w
Time
0822
0845
0900
0915
0930
0945
0100
1015
1030
1045
1100
1115
1130
1145
1200
1215
1230
1240
Total**
Mean
St. Dev
Min
Max
Event
*
*
Product
Type
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
Fabric Filter
Inlet
Temp.
(oF)
230
230
230
235
195
260
270
270
270
271
269
262
270
270
270
265
268
260
255
21
195
271
Outlet
Temp.
(oF)
185
192
190
197
200
205
215
225
230
228
225
220
225
225
230
225
220
220
214
15
185
230
Pressure
Drop
(in. H2O)
2.1
2.6
2.8
2.8
2.1
2.8
3.2
3.1
3.8
3.6
3.5
3.8
4.0
3.8
3.5
3.9
3.8
3.8
3.3
0.6
2.1
4.0
Fuel Use
Rate
(GPM)
5
5
5
5
3
7
7
7
7
7
7
7
7
8
7
7
7
6
6.3
1.2
3.0
8.0
Total
(gal)
324
427
512
592
704
760
869
984
1118
1200
1335
1440
1539
1663
1757
1881
1993
2086
1,762
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
* See Table 4 for a description of these events.
** Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 3
Test Date: August 20, 1997 p.m.
Total Test Time: 3.5 hrs
Time
1405
1415
1430
1445
1500
1515
1530
1545
1600
1615
1630
1645
1700
1715
1735
Total**
Mean
St. Dev
Min
Max
Event
*
Product
Type
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
Asphalt Concrete
Production
Rate
(TPH)
250
251
251
252
245
245
254
250
249
247
252
250
249
205
152
240
26
152
254
Total
(tons)
840
Asphalt
Temp.
(oF)
309
303
312
311
305
320
310
307
307
322
312
316
315
307
299
310
6
299
322
Aggregate Use
Rate
(TPH)
214
211
212
212
212
212
215
213
211
215
214
213
213
172
138
205
21
138
215
Total
(tons)
718
RAP Use
Rate
(TPH)
25
27
27
26
25
22
26
25
24
23
25
24
25
24
17
24
2
17
27
Total
(tons)
85
Asphalt
Cement Use
Rate
(TPH)
12.6
13.0
13.0
13.0
12.8
12.5
12.8
12.9
13.0
12.7
12.6
12.8
12.8
10.5
7.8
12.3
1.3
7.8
13.0
Total
(tons)
43
Calculated
Conditioner Use
Rate
(TPH)
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.03
0.02
0.03
0.003
0.02
0.03
Total
(tons)
0.108
w
* See Table 4 for a description of these events.
** Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 3
Test Date: August 20, 1997 p.m.
Total Test Time: 3.5 hrs
Crt
Time
1405
1415
1430
1445
1500
1515
1530
1545
1600
1615
1630
1645
1700
1715
1735
Total**
Mean
St. Dev
Min
Max
Event
*
Product
Type
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
RDS
Fabric Filter
Inlet
Temp.
(oF)
240
238
232
235
230
240
235
240
245
235
240
240
240
210
180
232
16
180
245
Outlet
Temp.
(oF)
200
200
200
195
195
195
195
195
200
200
200
200
200
190
165
195
9
165
200
Pressure
Drop
(in. H2O)
2.8
2.9
2.5
2.5
2.5
2.8
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.0
1.8
2.5
0.3
1.8
2.9
Fuel Use
Rate
(GPM)
6
5
5
5
5
6
6
5
6
5
6
6
6
5
3
5.3
0.8
3.0
6.0
Total
(gal)
2560
2630
2731
2823
2873
2992
3071
3162
3248
3333
3415
3488
3602
3656
3728
1,168
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
* See Table 4 for a description of these events.
** Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
Test Run 4
Test Date: August 21,1997
Total Test Time: 4.2 hrs
Time
0741
0745
0800
0815
0830
0845
0900
0915
0930
0945
1000
1015
1030
1045
1100
1115
1130
1145
1153
Total**
Mean
St. Dev
Min
Max
Event
*
Product
Type
HDS
HDS
HDS
HDS
Binder
Binder
HDS
Binder
Binder
Binder
Binder
HDS
HDS
HDS
HDS
HDS
HDS
HDS
Binder/ HDS
Asphalt Concrete
Production
Rate
(TPH)
150
179
177
177
178
179
184
179
181
178
177
176
200
200
200
200
200
200
204
185
13
150
204
Total
(tons)
778_j
Asphalt
Temp.
(oF)
315
306
302
335
300
300
351
283
297
319
320
350
271
303
282
310
289
318
297
308
21
271
351
Aggregate Use
Rate
(TPH)
142
169
169
168
171
171
174
167
172
172
171
167
191
190
189
190
191
189
194
176
13
142
194
Total
(tons)
740
RAP Use
Rate
(TPH)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Total
(tons)
0
Asphalt
Cement Use
Rate
(TPH)
7.8
9.2
9.2
9.3
8.1
8.2
9.0
9.1
8.5
8.0
7.8
9.3
10.4
10.6
10.4
10.5
10.3
10.6
8.9
9.2
1.0
7.8
10.6
Total
(tons)
39
Calculated
Conditioner Use
Rate
(TPH)
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.03
0.03
0.03
0.03
0.03
0.03
0.02
0.02
0.00
0.02
0.03
Total
(tons)
0.10
w
* See Table 4 for a description of these events.
"* Because running total data were not available, the run totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
Appendix A: Process Data
w
oo
Test Run 4
Test Date: August 21, 1997
Total Test Time: 4.2 hrs
Time
0741
0745
0800
0815
0830
0845
0900
0915
0930
0945
1000
1015
1030
1045
1100
1115
1130
1145
1153
Total**
Mean
St. Dev
Min
Max
Event
*
Product
Type
HDS
HDS
HDS
HDS
Binder
Binder
HDS
Binder
Binder
Binder
Binder
HDS
HDS
HDS
HDS
HDS
HDS
HDS
Binder/ HDS
Fabric Filter
Inlet
Temp.
(oF)
195
203
203
205
195
200
210
200
195
195
190
192
205
210
205
200
205
210
210
201
6
190
210
Outlet
Temp.
(oF)
168
178
177
178
170
170
180
180
170
175
168
170
170
180
175
180
175
180
180
175
5
168
180
Pressure
Drop
(in. H2O)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.8
2.0
.9
.9
.8
.9
2.0
.9
.8
.9
2.0
1.9
1.9
0.1
1.8
2.0
Fuel Use
Rate
(GPM)
5
4
4
4
4
3
4
3
4
4
4
4
5
5
5
4
4
5
4
4.2
0.6
3.0
5.0
Total
(gal)
146
216
288
363
440
474
560
626
669
743
812
871
932
1004
1063
1133
1208
1285
1323
1,177
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
* See Table 4 for a description of these events.
** Because running total data were not available, the ran totals were calculated from the average of the TPH data multiplied
by the total run time.
-------
. UUb P
SPECIAL:ZED ASSAYS ENVIRONMENTAL
2S/£0 Foater Cr«ighton Drive
Nicshvi 11c , Tennesoee 37204
ANALYTICAL REPORT
Original report and a copy of the chain cf custody wili. follow by mail.
NC/a.l.E Oil, CO. 7680
ATTN: LARRY PRJCE
5617 CLYDE RHYNE DRIVE
3ANFORD, NC 27330
Sample- ID: 861-625 OIL
Project:
Project. Name:
Sampler:
Star« Cercifiration: 3fiv
Lab Number: 57-A.06S425
Date Collected: 7/25/97
Time Collected:
Date Received: 8/ 7/97
Tine Received: 9:00
Sample Type: Oj1
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ftpare Qarx Dll
UrtC Unit Rotor
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4f-4.
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FUNKED XT 150P
359C
1.0
1.0
3.0
1.0
1.0
100.
1.0
1.0
1.0
1.0
1.0
10.0
0.01
5.00
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14:29 K.££0et 601CA
14:29 R-ittSCt
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SA4/S7 9:22 D. Ifco-r
6A*/97 12:37 a. Bui
2146
21.46
3E60
D402 343"J
1010 3465
WJ1KSCB 6920
Report Approvod Byi
Report Data i
Theodore
-------
MATERIAL SAFETY DATA SHEET
Manjftgtnrrr
ARR.MAZ PRODUCTS, LP.
621 SntvclyAveane
Winter Harem, FI J3MO
Phong
941-293-7U4
PRODUCT INFORMATION
HMTS RATING:
Shiin
AD-hcrc LOF (55-00
Amines
Modified Fatty Amidoamine
Health Hazard
Flannnability Hazard
Reactivity Hazard
Notragolsted
2 Moderate
ISligfa
OMimmaJ
PHYSICAL DATA
Salrihillt in 'Vter
»t
Vapor Petwitv fAy «» 1):
Ane
>500'F
Slight
Dark brown liquid
Mild
0.96-0.98
FIRE EXPLOSION,
Poin PM Closed
>300 "F
CO2, foam, or dry chemical
Wear NIOSH/MSHA approved aelf-contained breathing equtpmeni
and protective clothing.
Rev. Date: 11/26796
Z-9061
E-20
------- |