United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-00-022
April 2000
Air
HOT Mix ASPHALT PLANTS
E PA KILN DRYER STACK
INSTRUMENTAL METHODS TESTING
ASPHALT PLANT "B"
CARY, NORTH CAROLINA
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HOT MIX ASPHALT PLANTS
KILN DRYER STACK
INSTRUMENTAL METHODS TESTING
Asphalt Plant "B"
Gary, 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. A revised draft report was submitted under Work Assignment 2-10.
Mr. Michael Toney is the EPA 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. Mr. Michael Toney was also the WAM
for the previous work assignments. Dr. Thomas Geyer was the MRI WAL for Work
Assignments No. 4-24 and 2-10 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 (351 pages) with six sections and five appendices.
MIDWEST RESEARCH INSTITUTE
Hosenfeld
Program Manager
Approved:
Jeff Shular
Director, Environmental Engineering Department
April 2000
111
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TABLE OF CONTENTS
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 3-4
3.3 METHOD 25A RESULTS 3-4
3.4 FTIR RESULTS 3-5
3.5 ANALYTE SPIKE RESULTS 3-6
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 Samples 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 4-8
4.4.2 EPA Reference Spectra 4-9
4.5 FTIR SYSTEM 4-12
4.6 CONTINUOUS EMISSIONS MONITORING FOR TOTAL
HYDROCARBONS (THC) 4-12
4.6.1 Total Hydrocarbon Sampling Procedures 4-13
4.6.2 Hydrocarbon Emission Calculations 4-13
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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 B-2
B-2 FTIR FIELD DATA RECORDS B-3
B-3 FTIR FLOW AND TEMPERATURE READINGS B-4
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 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
APPENDIX E - PROCESS DATA E-l
LIST OF FIGURES
Figure 2-1. Baghouse inlet 2-2
Figure 2-2. Baghouse outlet (stack) 2-3
Figure 4-1. Sampling system schematic 4-2
VI
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TABLE OF CONTENTS (CONTINUED)
LIST OF TABLES
TABLE 1-1. SUMMARY OF FTIR RESULTS FOR WET SAMPLES AT PLANT B .... 1-4
TABLE 1-2. SUMMARY OF FTIR RESULTS FOR CONDENSER SAMPLES
AT PLANT B 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 2-5
TABLE 3-1. PLANT B FTIR AND 25A TEST SCHEDULE 3-2
TABLE 3-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS 3-5
TABLE 3-3. SPIKE RESULTS IN WET SAMPLES COLLECTED AT THE
BAGHOUSE INLET 3-8
TABLE 3-4. SPIKE RESULTS IN WET SAMPLES AT THE BAGHOUSE OUTLET ... 3-8
TABLE 3-5. COMPARISON OF EPA REFERENCE SPECTRA TO SPECTRUM OF
TOLUENE CYLINDER STANDARD 3-10
TABLE 4-1. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA 4-1CT
TABLE 4-2. PROGRAM INPUT FOR ANALYSIS, CTS SPECTRA,
AND PATH LENGTH DETERMINATION 4-11
TABLE 4-3. RESULTS OF PATH LENGTH DETERMINATION 4-11
TABLE B-1. FTIR RESULTS OF WET SAMPLES FROM THE BAGHOUSE OUTLET
AT PLANT "B" B-5
TABLE B-2. FTIR RESULTS OF WET SAMPLES FROM THE BAGHOUSE OUTLET
AT PLANT "B" B-13
TABLE B-3. FTIR RESULTS OF DRY SAMPLES FROM THE BAGHOUSE OUTLET
AT PLANT "B" B-22
TABLE B-4. FTIR RESULTS OF DRY SAMPLES FROM THE BAGHOUSE OUTLET
AT PLANT "B" B-29
vn
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Vlll
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1.0 INTRODUCTION,
1.1 BACKGROUND
The Emission Measurement Center (EMC) issued work assignment 4-24 to 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 performed in August 1997 under work
assignment 4-24, on EPA Contract No. 68-D2-0165. A draft report was prepared under work
assignment, 2-08, under EPA Contract No. 68-W6-0048. A revised report was prepared under
work assignment 2-10, EPA Contract No. 68-D-98-027. The process description and data in
Appendix E was prepared by ECR Incorporated and was included in this report without MRI
review.
The purpose of this project was to perform an emissions test on the inlet and outlet of a
baghouse that controls emissions from the parallel-flow rotary dryer process used at the Asphalt
Plant B facility in Gary, North Carolina. MRI used EPA Fourier transform infrared (FTIR)
Method 3201 and EPA Method 25A. Method 320 is an extractive test method using FTIR
spectroscopy. Method 320 uses quantitative analytical procedures described in the EPA FTIR
Protocol2. Method 25A is a an extractive test method using a Flame lonization Analyzer (FIA).
The results were used to characterize and quantify hazardous air pollutant (HAP) emissions and
the performance of the control unit for maximum achievable control technology (MACT)
standard development for this industry.
1.2 PROJECT SUMMARY
Asphalt paving materials are produced by drying and mixing various amounts of raw (and
sometimes recycled) materials with asphalt cement in a rotary drum dryer. The product is then
conveyed to heated storage silos before loading into trucks for distribution. The dryer emissions
are drawn through a knockout box, for primary particulate control, and then a baghouse before
being emitted to the atmosphere. Testing was conducted at the inlet and outlet of the baghouse to
determine the measurable emissions released.
1-1
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Three 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 and 2 were conducted during production using reclaimed asphalt pavement (RAP).
Run 3 was conducted during production using non-RAP containing material.
The FTIR samples were collected by alternately sampling the baghouse inlet and stack
using a single instrument, and the 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) is presented in Table 1-1. FTIR results for samples
collected on a cold/dry basis (i.e., stack gas passed through a condenser to remove moisture) are
summarized in Table 1-2. 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.
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 is provided with this report.
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 FTIR spectra show evidence of aliphatic hydrocarbon compounds in the emissions.
Hexane and 2,2,4-trimethlypentane (isooctane) are the only HAP spectra in the EPA library that
meet this description. Therefore, in the draft analysis results, the hydrocarbon emissions were
principally represented by "hexane." Since then, MRI has measured reference spectra of some
additional non-HAP hydrocarbon compounds. These new hydrocarbon reference spectra were
used in revised analyses of the sample spectra. In the revised results, the hydrocarbon mixture is
principally represented by n-heptane with contributions from 1-pentene and 2-methyl-2-butene.
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
1-2
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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
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 Ba
Untreated (wet) Samples
Toluene
Hexane
Ethylene
Methane
Sulfur Dioxide
Carbon Monoxide
Formaldehyde
Heptane
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
12.6
1.811
0.118
11.2
0.917
0.034
10.9
3.6
0.53
125.1
18.0
1.17
2.19
0.337
0.0236
7.75
3.987
0.9296
4.34
1.562
0.2550
Outlet
10.70
1.653
0.12
11.40
1.00
0.04
6.50
2.29
0.36
125.60
19.30
1.34
1.00
0.16
0.01
8.10
4.46
1.11
6.90
2.65
0.46
Run 2
Inlet
6.9
3.2
0.68
8.01
1.131
0.072
10.2
0.824
0.030
14.4
4.64
0.68
18.4
2.6
0.17
10.7
5.381
1.2312
Outlet
0.6
0.3
0.06
7.6
1.159
0.080
9.6
0.833
0.033
15.7
5.4
0.85
56.1
8.48
0.58
6.8
3.672
0.9011
4.8
1.804
0.3099
Run 3
Inlet
6.6
3.18
0.69
13.3
1.944
0.129
10.5
0.875
0.033
16.0
5.3
0.81
163.5
23.9
1.59
5.3
0.84
0.059
6.7
3.49
0.827
0.7
0.26
0.043
0.2
0.07
0.012
Outlet
7.5
3.9
0.90
13.9
2.173
0.154
10.8
0.962
0.039
17.7
6.3
1.02
194.7
30.3
2.14
4.46
0.75
0.057
4.41
2.46
0.621
2.89
1.13
0.199
The two locations
Tables B-l to B-4
were sampled sequentially. Sampling times for each condition are shown in Table 3-1 and in
. Blank spaces indicate a "non-detect."
1-4
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TABLE 1-2. SUMMARY OF FTIR RESULTS FOR CONDENSER SAMPLES AT PLANT Ba
Condenser Samples
Toluene
Hexane
Ethylene
Methane
Sulfur Dioxide
Carbon Monoxide
Formaldehyde
3-Methylpentane
Isooctane
Heptane
1-Pentene
2-Methyl-2-butene
n-Pentane
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
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
Run 1
Inlet
NDb
ND
1.74
0.18
0.008
1.9
0,11
0.0029
18.8
4.36
0.46
62.3
6.3
0.29
ND
ND
ND
8.20
2.986
0.4930
ND
ND
ND
Outlet
ND
ND
ND
2.0
0.12
0.0034
18.2
4.51
0.51
42.5
4.6
0.23
ND
ND
ND
7.5
2.914
0.5125
ND
ND
ND
Run 2
Inlet
ND
ND
1.77
0.18
0.008
2.4
0.14
0.0037
26.3
6.13
0.65
57.7
5.9
0.27
ND
ND
0.3
0.136
0.0256
8.1
2.968
0.4923
0.2
0.055
0.0064
ND
ND
Outlet
ND
ND
2.26
0.25
0.012
2.6
0.16
0.0045
23.8
5.93
0.67
98.7
10.7
0.53
ND
ND
ND
7.7
3.018
0.5332
ND
ND
ND
Run 3
Inlet
ND
ND
ND
2.0
0.14
0.0043
10.7
2.9
0.36
40.4
4.81
0.26
3.9
0.50
0.029
1.0
0.38
0.063
ND
ND
ND
0.1
0.02
0.003
4.5
1.37
0.190
Outlet
ND
ND
ND
2.1
0.15
0.0047
7.1
2.0
0.26
48.1
5.99
0.34
ND
1.78
0.68
0.118
ND
2.03
0.90
0.182
0.12
0.04
0.005
ND
ND
a The two locations were sampled sequentially (not simultaneously) with the FTIR instrument. Hot/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.
b ND = not detected in this run.
1-5
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TABLE 1-3. SUMMARY OF HYDROCARBON EMISSIONS RESULTS
Test Data3
Run Number
Date
1
27-Aug-98
2
28-Aug-98
Average0
3
29-Aug-98
Baghouse Inlet
Gaseous Concentrations
THC Concentration (ppm propane)
THCb Concentration, ppmc (wet basis)
THC Concentration, ppmc (dry basis)
Emissions Data
THC Emission Rate, Ib/hr"
THC Emission Rate, kg/hr
85.8
257.4
363.5
15.9
7.2
61.9
184.1
253.9
11.1
5.0
73.6
220.7
308.7
13.5
6.1
46.1
138.2
170.1
8.7
3.9
Baghouse Outlet ( Stack)
Gaseous Concentrations
THC Concentration (ppm propane)
THC Concentration, ppmc (wet basis)
THC Concentration, ppmc (dry basis)
Emissions Data
THC Emission Rate, Ib/hr
THC Emission Rate, kg/hr
38.3
114.9
162.6
7.6
3.4
43.6
130.7
181.5
8.5
3.8
40.9
122.8
172.1
8.0
3.6
35.7
107.2
134.3
7.2
3.2
a Method 25A results and run averages are presented in Appendix A-l. Run Times are in Table 3-1.
h THC = Total hydrocarbons.
c The results of the first 2 runs were averaged because the process was using reclaimed asphalt pavement (RAP).
During Run 3 the process was using non-RAP material.
J See equations 5 & 6 in Section 4.6.2 for emission rate calculations.
1-6
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1.3 PROJECT PERSONNEL
The EPA test program was administered by the EMC. The Test Request was initiated by
the Minerals and Inorganic Chemicals Group of the ESD. Some key project personnel are listed
in Table 1-4.
TABLE 1-4. PROJECT PERSONNEL
Organization and Title
Plant B Services, Manager
Plant B Manager/Supervisor
U.S. EPA, EMC
Work Assignment Manager
Work Assignment 4-24
Work Assignment 2-08
U. S. EPA
Minerals & Inorganic
Chemicals Group
MRI
Work Assignment Leader
Work Assignment 3-02
MRI
Work Assignment Leader
Work Assignment 4-24
Work Assignment 2-10
Task Leader, Work Assignment 2-
08, Task 2
MRI
Program Manager
Work Assignment Leader
Work Assignment 2-08
Name
Gene Mills
Don Schell
Michael L. Toney
Mary Johnson
Scott Klamm
Thomas J. Geyer
John Hosenfeld
Phone Number
(704) 394-8354
(919)851-1376
(919) 541-5247
(919)541-5247
(818)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 from the same trailer
position.
2.2.1 Baghouse Inlet Duct
The inlet location was a circular duct with a diameter of 541/2 inches (in.). Testing was
conducted in the vertical segment of the duct downstream of the manual method ports. FTIR and
Method 25A testing was conducted in a 4-in. diameter test port that was installed upstream of the
manual test ports.
2.2.2 Baghouse Outlet (Stack)
The outlet location was a rectangular stack 49% in. wide and 33 in. deep. Six ports, used
for the manual sampling, were arranged horizontally in a line about 24 in. upstream of the stack
exit. Another 4-in. port was installed 3 feet upstream of the manual sampling ports and was used
for the FTIR and Method 25A sampling.
2.3 VOLUMETRIC FLOW
Table 2-1 summarizes the gas composition and exhaust gas 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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EXHAUST
GAS FLOW
Q
MANUAL
SAMPLING
PORTS
Q
INLET SAMPLE LOCATION
to
i
to
FTIR&
METHOD 25A
TEST PORT
o
BAGHOUSE
Figure 2-1. Baghouse inlet.
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49 3/4"
MANUAL METHOD
TEST PORTS
-O--G--O--O--O--O--
33"
24"
FTIR&
METHOD 25A
TEST PORT
o
HANDRAIL
STACK SAMPLING LOCATION
Figure 2-2. Baghouse outlet (stack).
DRAWING NOT TO SCALE
2-3
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2-4
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TABLE 2-1. SOURCE GAS COMPOSITION AND FLOW SUMMARY
Test Dataa
Run Number
Date
1
27-Aug-98
2
28-Aug-98
3
29-Aug-98
Baghouse Inlet
Oxygen, %
Carbon Dioxide, %
Moisture Content, %
Gas Stream Velocity, fps"
Volumetric Flow Rate, dscfnf
14.0
4.9
29.2
49.6
23,334
13.1
5.2
27.5
49.1
23,446
15.2
4.0
18.8
49.8
27,252
Baghouse Outlet ( Stack)
Oxygen, %
Carbon Dioxide, %
Moisture Content, %
Gas Stream Velocity, fps
Volumetric Flow Rate, dscfm
15.0
4.0
29.4
74.3
24,868
13.6
4.9
28.0
74.1
24,978
16.3
3.0
20.2
74.5
28,526
Raw gas composition and velocity data are in Appendix A-3. The values reported are averages of the values
reported from Methods 23 and 29. The raw data in Appendix A-3 was provided by Pacific Environmental
Services (PES).
h fps = feet per second.
c dscfm = dry standard cubic feet per minute.
2-5
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3.0 RESULTS
3.1 TEST SCHEDULE
The test program at Asphalt Plant B was completed from August 27 to August 29, 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,
and in the same periods as the manual sampling conducted by PES, but was not exactly
simultaneous.
3-1
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TABLE 3-1. PLANT B FTIR AND 25A TEST SCHEDULE
Date
8/27/97
8/28/97
FTIR
INLET
Wet
932-1002
1104- 1127 (spike)
1220-1247
1448-1518
818-841 (spike)
923-945
1318-1345
Dry
1333- 1400
1042-1109
1202-1232
OUTLET
Wet
1020-1045 (spike)
1148-1213
732-805 (spike)
954-1027
Dry
1258-1323
1427-1443
1129-1153
1241-1310
1353-1354
1409-1430
THC (25A)
Inlet and Outlet
940-1516
744-1431
Plant Down Times'1
1002-1007
*
1140-1146
1402-1412
901-909
1110-1128
1355-1407
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TABLE 3-1. (CONTINUED)
Date
8/29/97
FTIR
INLET
Wet
759-840 (spike)
927-959
1056-1120
1407-1414
Dry
1207-1210,
1223-1239"
OUTLET
Wet
848-921 (spike)
1005-1045
1329-1359
Dry^
1130-1200
THC (25 A)
Inlet and Outlet
816-1412
Plant Down Times"
i
1212-1221
1242-1323
U)
U) " From EC/R Report in Appendix E.
b The FTIR outlet valve was closed so this represents a single static sample.
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3.2 FIELD TEST PROBLEMS AND CHANGES
Typically, a glass wool plug is inserted at the inlet of the sample probe as a pre-filter.
The paniculate at the baghouse inlet was high enough to quickly clog the pre-filter. Therefore,
an additional Balston filter was installed at the probe inlet. With this arrangement it was possible
to sample for extended periods at the inlet location.
The outlet valve of the FTIR cell was closed for a period during Run 3 so that the inlet
sample was not flowing through the cell (spectra 18290075 to 18290093). For part of this period
the process was not operating, but these are, in effect, spectra of a single sample.
During the Run 2 post-run vacuum leak check a leak was observed in the inlet sampling
system. It is not known what if any leak was present at the sampling pressure. The leak probably
occurred about 4 hours into the run when the inlet Balston filter was replaced during process
down time. The Method 25A passed the post-run calibration so this may have had little effect on
the results.
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
(about 30 percent by volume). The use of the condenser was approved by the EPA observer at
the test site. The condenser was used for portions of all three test runs. 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.
3.3 METHOD 25A RESULTS
Table 3-1 summarizes 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 total hydrocarbon (THC) emissions for all three runs include fairly stable
concentrations with a few spikes occurring during the test periods. The trend data for Runs 1
and 2 are very similar with a stable THC concentration throughout the run with intermittent
3-4
-------
spikes. Run 3 is slightly different because there is a substantial baseline concentration shift at
about 1000 and then at 1215 the concentration becomes fairly unstable. Graphical presentation
of the THC trend can be found in Appendix A. Without accounting for process variations during
the testing periods, no absolute determinations can be made about the data.
Table 3-2 shows the minimum, maximum, and average THC concentrations for each run.
The one-minute average THC concentrations range from as low as 12.9 ppmc at the stack during
Run 3, to as high as 1444 ppmc, during Run 2. This does not mean that the highest spike was
1444 ppmc, but that the highest one minute average was 1444 ppmc. THC emission trends
similar to Runs 1, 2, and 3 are what would normally be found at this type of facility.
TABLE 3-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS
Date
Minimum
ppma
ppmcb
Minimum
ppm
ppmc
Average
ppm
ppmc
Baghouse inlet
08/27/97
08/28/97
08/29/97
34.2
22.6
5.4
102.6
67.8
16.2
176.9
481.3
271.9
530.7
1444
815.7
85.8
61.4
46.1
257.4
184.2
138.3
Baghouse stack
08/27/97
08/28/97
08/29/97
22.4
19.2
4.3
67.2
57.6
12.9
88.6
89.0
97.6
265.8
267.0
292.8
38.3
43.6
35.7
114.9
130.8
107.1
"ppm - as propane
hppmc - ppm as carbon
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. Calibration QA results are included in
Appendix A.
3.4 FITR RESULTS
The FITR spectra show evidence of aliphatic hydrocarbon compounds in the emissions.
Hexane and 2,2,4-trimethlypentane (isooctane) are the only HAP spectra in the EPA library that
3-5
-------
meet this description. Therefore, in the draft analysis results, the hydrocarbon emissions were
principally represented by "hexane." Since then, MRI has measured reference spectra of some
additional non-HAP hydrocarbon compounds. These new hydrocarbon reference spectra were
used in revised analyses of the sample spectra. In the revised results, the hydrocarbon mixture is
principally represented by n-heptane with contributions from 1-pentene and 2-methyl-2-butene.
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 results are
presented graphically after Table B-4. 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. 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 do not include the
samples where toluene was spiked from a cylinder in the gas stream and the unspiked
concentration was zero-
Some samples in all three test runs 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 about 30 percent by volume. See Section 1.2 for additional explanation of how
condenser can affect the results.
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 can be
lower in the dried samples.
3.5 ANALYTE SPIKE RESULTS
An ethylene gas standard (Runs 1 and 3) and a toluene gas standard (Run 2) were used
for analyte spiking experiments for quality control evaluation. Preferably, a spike standard
combines the analyte and the tracer gas in the same cylinder, but the SF6 and the analytes were
contained in separate cylinders. Therefore, the two components (SF6 and toluene or SF6 and
ethylene) were spiked sequentially: the flue gas was spiked with SF6 until three samples were
measured, then the flue gas was spiked with the analyte (toluene or ethylene).
The analyte spike results are presented in Tables 3-3 and 3-4. Samples were spiked with
a measured flow of analyte vapor during each run and at each location. The SF6 tracer gas spike
3-6
-------
was used to determine the spike dilution factor. A description of the spike procedure is given in
Section 4.3.1.
The calculated spike recoveries were within 70 to 100 percent except for the Run 2
toluene spike results at the outlet. The calculated toluene spike concentrations were similar to
those measured in the inlet results. But the outlet unspiked toluene concentration was zero.
Since the emissions were variable, it may be that the outlet spiked samples contained a
contribution from the process emissions. The process contribution may have dropped below
detectible levels when the unspiked samples were collected. There was some disagreement
between the toluene reference spectra in the EPA spectral library and the spectrum of the toluene
cylinder standard measured on-site at Asphalt Plant B. Tables 3-3 and 3-4 present the toluene
recoveries obtained using the EPA library toluene spectra. Using the spectrum of the toluene
cylinder standard in the analysis gives toluene spike recoveries about 40 percent lower.
3-7
-------
TABLE 3-3. SPIKE RESULTS IN WET SAMPLES COLLECTED AT THE BAGHOUSE INLET
Run
1
(ethylene)'
2
(toluene)0
3
(ethylene)e
Average Concentration
Spike Unspike Calca
23.2 3.5 19.7
43.8 15.4 28.4
28.4 5.7 22.8
Average SF6 Concentration
Spike Unspike SF6 (calc)u DFb
0.878 0.000 0.878 4.4
0.859 0.000 0.859 4.5
0.780 0.000 0.780 5.0
Calc - Cexp
Cc^ AJ % Recovery
22.8 -3.1 86.5
26.7 1.7 106.2
20.2 2.4 112.0
11 Calc and SF6(calc) are equal to the difference between the spiked and unspiked concentrations tor the analyte and SF6, respectively.
b DF is the dilution factor in equation 4.
11 Ccxp is shown in equation 5.
J A is equal to the difference, Calc - Ccxp.
' Runs 1 and 3 spike gas was 101 ppm ethylene in air. Run 2 spike gas was 121 ppm Toluene standard.
OO
TABLE 3-4. SPIKE RESULTS IN WET SAMPLES AT THE BAGHOUSE OUTLET
Run
1
(ethylene)'
2
(toluene)"
3
(ethylene)'
Average Concentration
Spike Unspike Calc"
23.2 6.8 16.4
43.1 * 0.0 43.1
35.3 17.7 17.6
Average SF6 Concentration
Spike Unspike SF6 (calc)" DFb
0.758 0.000 0.758 5.1
0.787 0.000 0.787 4.9
0.793 0.000 0.793 4.9
Calc - Cexp
CMpc Ad % Recovery
19.7 -3.3 83.3
24.5 18.6 176.0
24.7 -7.1 71.2
° Calc and SF6(calc) are equal to the difference between the spiked and unspiked concentrations for the analyte and SF6, respectively.
b DF is the dilution factor in equation 4.
c Ccxp is shown in equation 5.
d A is equal to the difference, Calc - Cexp
' Runs 1 and 3 spike gas was 101 ppm ethylene in air. Run 2 spike gas was 121 ppm Toluene standard.
-------
Table 3-5 presents measured band areas of the EPA toluene reference spectra (deresolved
to 1.0 cm"1) and the spectrum of the toluene cylinder standard measured at the Asphalt Plant B
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 more than
40 percent. This observed difference predicts that, if the spectra of the toluene cylinder standard
is used in the analysis rather than the EPA library spectra, then the resulting toluene spike
recovery is more than 40 percent lower.
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 acquired 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 3-5.
This type of discrepancy is compound specific, and the information in Table 3-5 does not"
affect the results for any of the other compounds detected. In fact, the deresolved calibration
transfer standard (CTS) (ethylene calibration) spectra give a path length result (Section 4) 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"' toluene spectra are nearly equal to the band areas in the deresolved 1.0 cm"1
versions of these spectra.
A similar disagreement between reference and standard spectra has been observed at least
once previously.4 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.
3-9
-------
UJ
i
o
TABLE 3-5. COMPARISON OF EPA REFERENCE SPECTRA TO SPECTRUM OF TOLUENE CYLINDER STANDARD
Toluene Spectra
153a4ara(lcm')
153a4arc (1cm'1)
L530828a
Source
EPA library
EPA library
Plant B
Band Area
23.4
4.3
24.2
Frequency
Region (cm"1)
3160.8-2650.1
Spectra comparison
based on band areas
Ratio (Ra)
5.4
1.0
5.5
= l/Ra
0.184
1.000
0.181
Comparison of spectra based on
standard concentrations a
(ppm-m)/K
4.94
1.04
2.84
Ratio (Re)
4.8
1.0
2.7
= l/Rc
0.210
1.000
0.365
" The comparison of the ratio based on concentrations to the ratio based on band area is equal to 49 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
assessment, 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:
• two sample probe assemblies
• two sample lines and pumps
• 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
paniculate 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 efficiency at 0.1 ,um. 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
Data Storage & Analysis FTIR Spectrometer
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 lengths. The pumps are heated, single-headed diaphragm pumps manufactured
by either KNF Neuberger or Air Dimensions. These pumps are capable of sampling 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 particulate 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.
Also included on the cart is 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 baghouse through their
respective sample probes and transported to the gas distribution manifold. Inside the manifold
the gas passed through separate secondary particulate 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; 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 Samples
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 opened 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 all three test runs. 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
4-4
-------
depends on the sampling rate (Rs in LPM), the cell volume (Vcel, in L) and the analyte's chemical
and physical properties.' Therefore,
v
T/~I cell
TC = -*r (1)
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 101 ppm ethylene standard during
Runs 1 and 3 and a toluene (121 ppm in air) standard during Run 2.
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 assurance 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, then this procedure can be used to perform
a Method 301 validation.3 No validation was performed 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 to 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
4-5
-------
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 analytes (either 121 ppm toluene in air or 101 ppm ethylene in air) and the
tracer gas (3.89 ppm SF6 in nitrogen) were in separate cylinders. The tracer gas and the analyte
were spiked in sequence. First, SF6 was spiked into the flue gas. Three samples spiked with SF6
were measured. Second, the flue gas was spiked with the analyte using the same flow rate that
was used for the SF6 spike. Three analyte spiked samples were then measured. This procedure
works best if the sample flow rate is constant during the spike period.
The spike dilution factor, DF, is determined by comparing the measured SF6
concentration in the spiked samples, SF6(spjke), to the SF6 concentration in an undiluted sample
direct from the SF6 cylinder standard, SF6(direct).
DF =
SF
J 6(spike)
where:
DF = the spike dilution factor in Section 9.2.2 of Method 320.
The calculated 100 percent recovery of the analyte spike is analogous to the expected
concentration in Section 9.2.2 of Method 320. In this case:
where:
Cexp = the expected analyte concentration in the spiked samples (100 percent
exp
recovery).
Analyte(direct) = the concentration of the cylinder standard. In this test the analyte was either
toluene or ethylene.
DF = from equation 2.
4-6
-------
4.3.2 Analysis of Spiked Results
The analyte and SF6 concentrations used in the evaluation of the spike recoveries in
Tables 3-3 and 3-4 were taken directly from the sample analyses reported in Tables Bl to B4.
The concentrations in the spiked samples included a contribution from the spike gas and from
analyte present in the flue gas. The component of the analyte concentration attributed to the
spike was determined by subtracting the average of the unspiked samples from the measured
concentration in each spiked sample ("spiked - unspiked" in Tables 3-3 and 3-4). The percent
recoveries were the ratios of the differences, spiked - unspiked, divided by, 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 4-1.5 The computer
program used mathematical techniques based on a K-matrix analysis.6
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. The
results from this second analytical run are summarized in Tables 1-1 and 1-2 and reported in
Appendix B.
The same program used for the analysis also 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 Isigma
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 4.
s
Ccalc (4)
4-7
-------
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 770 mm Hg.
No correction factor for the pressure was applied to the analytical results.
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, Ls, 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 field test. The calculated average cell path
length resulting from this analysis and the variation among the sample CTS over the 3 days of
testing, are reported in Table 4-2.
4.4.1 Computer Program Input
Table 4-1 presents a summary of the reference spectra input for the computer program
used to initially analyze the sample spectra. In the revised analyses, the undetected compounds
were removed and reference spectra of hydrocarbons 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. Only the hydrocarbons that were detected are shown in Tables 1-1, 1-2,
and B-l to B-4. 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 using Section K.2.2 of the EPA FTIR protocol. The program analyzed
4-8
-------
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 Ls in equation 4.
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). The original sample and background
interferograms were truncated to the first 16,384 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 1.0 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.
4-9
-------
TABLE 4-1. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA
Compound name
Water Hot/wet
Condenser
Carbon monoxide
Sulfur dioxide
Carbon dioxide
Formaldehyde
Benzene
Methane
Methyl bromide
Toluene
Methyl chloride
Methyl chloroform
1 , 1 -dichloroethane
1,3-butadiene
Carbon tetrachloride
Chlorobenzene
Cumene
Ethyl benzene
Hexane
Methylene chloride
Propionaldehyde
Styrene
1 , 1 ,2,2-tetrachloroethane
p-Xylene
o-Xylene
m-Xylene
Isooctane
Ethylene
SF6
Ammonia
File name
194jsub,
194fsub
co20829a
198clbsi
193clbsc
087clasa
015a4ara
196clbsd
106a4asb
153a4arc
107a4asa
108a4asc
086b4asa
023a4asc
029a4ase
037a4arc
046a4asc
077a4arb
095a4asd
1 17a4asa
140b4anc
147a4asb
150b4asb
173a4asa
1 7 1 a4asa
172a4arh
165a4asc
CTS0827a
Sf6_002
174clasc
Analytical
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
ISCb
100b
167.1
89.5
415b
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 cm'1
2,035.6
789.3
2,650.1
b Indicates an arbitrary concentration was used for the interferant.
4-10
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TABLE 4-2. PROGRAM INPUT FOR ANALYSIS, CTS SPECTRA,
AND PATH LENGTH DETERMINATION
Compound name
Ethylene3
Ethylene
File name
cts0814b.spc
cts0814c.spc
ASC
1.007
1.007
ISC
1.014
0.999
% Difference
0.7349
0.7350
a This spectrum was used in the analysis of the Plant B CTS spectra.
TABLE 4-3. RESULTS OF PATH LENGTH DETERMINATION
CTS spectra
20.1 ppm Ethylene
cts0827A
cts0827B
cts0828A
cts0828B
cts0829A
cts0829B
Average Path Length (M)
Standard Deviation
Path length calculations
Meters
9.08
9.00
9.06
9.19
9.08
9.23
9.11
0.088
Delta3
-0.02
-0.11
-0.05
0.09
-0.03
0.12
% Delta
-0.27
-1.19
-0.53
0.96
-0.33
1.37
The difference between the calculated and average values.
4-11
-------
4.5 FTIR SYSTEM
A KVB/Analect RFX-40 spectrometer was used to collect all of the data in this field test.
The gas cell was a variable path (D-22H) gas cell from Infrared Analysis, Inc. The cell was
equipped with a 3-zone insulated heating jacket assembled by MRI. The path length of the cell
was set at 20 laser passes and measured to be about 9.11 meters using the CTS reference and
sample spectra. The interior cell walls were 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 1.0 cm"1.
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
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 B
with two exceptions. Section 7.2 of Method 25A specifies an analyzer drift determination hourly
during the test period, but 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 determinations 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.
4-12
-------
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 boih locations by using of 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.
• THC Analyzer- The THC concentration is measured using a flame ionization
detector (FID). MRI used two J.U.M. Model VE-7 analyzers. The THC
analyzers were operated on the zero to 1000 ppm range throughout the test
period. The fuel for the FID is 40% hydrogen and 60% helium mixture.
• 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.
• 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 is presented as THC emissions in Table 1-3. To do this the THC
emission data was first converted to an as carbon basis using Equation 5, and then the THC
emission rate was calculated using Equation 7.
4-13
-------
where:
Cc = organic concentration as carbon, ppmv.
Cmeas = organic concentration as measured, ppmv.
K = carbon equivalent correction factor, 3 for propane.
The emission rate was calculated using Equation 6.
cr
—— x MW x Q ,, x 60
i T-V •, ^5%tQ
E . ws
™C " 385.3 x 106
where:
Ej-HC = THC mass emission rate, Ib/hr.
Bws = moisture fraction.
MW = molecular weight of Carbon, 12 Ib/lb-mole.
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.
4-14
-------
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 on site 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. FTIR spectra were
continuously monitored to ensure that there was no deviation in the spectral baseline greater than
±5 percent (-0.02 < absorbance < +0.02). When a deviation greater than ±5 percent did occur,
sampling was interrupted and a new background spectrum was collected. The run was then
resumed until completed or until it was necessary to collect another background spectrum.
5.2 FTIR SPECTRA
For a detailed description of QA/QC procedures relating to data collection and analysis,
refer to the "Protocol For Applying FTER Spectrometry in Emission Testing."2
A spectrum of the CTS was recorded at the beginning and end of each test day. A leak
check of the FTIR cell was also performed according to the procedures in references 1 and 2.
The CTS gas was 101 ppm ethylene in air. The CTS spectrum provided a check on the operating
conditions of the FTIR instrumentation, e.g., spectral resolution and cell path length. Ambient
pressure was recorded whenever a CTS spectrum was collected. The CTS spectra were
compared to CTS spectra in the EPA library. This comparison is used to quantify differences
between the library spectra and the field spectra so library spectra of FLAP'S can be used in the
quantitative analysis.
Two copies of all interferograms, processed backgrounds, sample spectra, and the CTS
were stored on separate computer disks. Additional copies of sample and CTS absorbance
spectra were also be stored for data analysis. Sample absorbance spectra can be regenerated from
the raw interferograms, if necessary.
The compact disk enclosed with this report contains one complete copy of all of the FTIR
data recorded at the Plant B field test. The data are organized into directories whose titles
5-2
-------
identify the contents. The continuous data are in directories identified by the date on which the
spectra were recorded. The directory titles "BKG," "CIS,", "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 directory "residuals"
contains the residual spectra. 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 of the system.
Calibration criteria for Method 25A 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 check before each test run; and
2. Final Zero and Span calibrations 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. "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.
5. "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.
6. "Computer-Assisted Quantitative Infrared Spectroscopy," Gregory L. McClure (ed.),
ASTM Special Publication 934 (ASTM), 1987.
7. 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 VOLUMETRIC FLOW DATA
-------
-------
A-l METHOD 25A RESULTS
A-l
-------
A-2
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
8:36
8:37
8:38
8:39
8:40
8:41
THC Inlet
(ppm)
75.2
77.3
80.2
79.6
76.8
77.8
78.4
80.0
82.8
76.9
76.9
74.6
73.7
74.9
77.6
80.5
Plant Problem
84.1
80.7
81.2
82.2
83.1
83.6
84.2
85.4
91.2
93.5
96.6
95.1
90.3
87.4
82.4
78.5
THC Inlet
(ppmc)
225.6
231.9
240.6
238.8
230.4
233.4
235.2
240.0
248.4
230.7
230.7
223.8
221.1
224.7
232.8
241.5
252.3
242.1
243.6
246.6
249.3
250.8
252.6
256.2
273.6
280.5
289.8
285.3
270.9
262.2
247.2
235.5
THC Outlet
(ppm)
45.4
46.5
47.0
45.5
43.3
42.5
42.4
42.3
44.1 .
40.4
39.8
38.4
37.5
37.9
38.7
39.8
38.1
36.0
36.8
38.0
38.5
39.1
39.4
39.7
42.8
44.7
45.9
45.5
42.9
40.9
39.4
36.9
THC Outlet
(ppmc)
136.2
139.5
141
136.5
129.9
127.5
127.2
126.9
132.3
121.2
119.4
115.2
112.5
113.7
116.1
119.4
114.3
108
110.4
114
115.5
117.3
118.2
119.1
128.4
134.1
137.7
136.5
128.7
122.7
118.2
110.7
Run1, Page 1 of 11
A-3
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick '
Time
(24 hr)
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)
75.6
74.6
75.5
76.6
75.9
79.8
83.4
86.4
89.5
88.3
87.3
87.6
83.2
84.8
87.0
90.6
94.2
96.2
98.3
94.8
90.5
86.2
82.6
85.2
85.3
86.1
87.0
87.0
88.3
88.2
85.9
88.5
94.2
97.3
91.8
83.9
79.2
77.4
78.7
80.8
77.6
78.3
THC Inlet
(ppmc)
226.8
223.8
226.5
229.8
227.7
239.4
250.2
259.2
268.5
264.9
261.9
262.8
249.6
254.4
261.0
271.8
282.6
288.6
294.9
284.4
271.5
258.6
247.8
255.6
255.9
258.3
261.0
261.0
264.9
264.6
257.7
265.5
282.6
291.9
275.4
251.7
237.6
232.2
236.1
242.4
232.8
234.9
THC Outlet
(ppm)
35.3
34.8
34.7
35.5
35.4
36.6
37.8
39.2
40.9
40.7
40.2
39.9
38.5
38.0
38.8
40.3
42.4
43.1
44.1
42.7
40.1
37.9
35.8
36.3
36.8
37.0
37.6
37.8
38.3
38.8
37.4
38.3
40.5
42.5
40.3
36.2
33.7
32.8
33.4
33.9
33.1
33.2
THC Outlet
(ppmc)
105.9
104.4
104.1
106.5
106.2
109.8
113.4
117.6
122.7
122.1
120.6
119.7
115.5
114
116.4
120.9
127.2
129.3
132.3
128.1
120.3
113.7
107.4
108.9
110.4
111
112.8
113.4
114.9
116.4
112.2
114.9
121.5
127.5
120.9
108.6
101.1
98.4
100.2
101.7
99.3
99.6
A-4
Run1, Page 2 of 11
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
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
THC Inlet
(ppm)
76.4
76.4
78.9
80.3
80.9
80.4
81.4
84.2
86.4
82.6
81.6
83.6
85.0
86.3
78.0
Inlet Spike
80.0
78.4
77.3
74.9
75.4
77.6
80.3
81.4
82.6
83.2
82.6
81.4
Plant Problem
THC Inlet
(Ppmc)
229.2
229.2
236.7
240.9
242.7
241.2
244.2
252.6
259.2
247.8
244.8
250.8
255.0
258.9
234.0
240.0
235.2
231.9
224.7
226.2
232.8
240.9
244.2
247.8
249.6
247.8
244.2
THC Outlet
(ppm)
32.8
32.2
33.6
34.2
34.5
34.0
34.2
35.0
36.2
34.7
32.7
33.7
33.9
34.5
35.0
35.4
35.5
35.6
36.2
36.8
37.7
37.8
37.1
36.5
35.6
34.8
35.0
34.2
32.9
31.8
31.4
32.4
33.2
33.5
34.3
34.6
34.1
33.3
THC Outlet
(ppmc)
98.4
96.6
100.8
102.6
103.5
102
102.6
105
108.6
104.1
98.1
101.1
101.7
103.5
105
106.2
106.5
106.8
108.6
110.4
113.1
113.4
111.3
109.5
106.8
104.4
105
102.6
98.7
95.4
94.2
97.2
99.6
100.5
102.9
103.8
102.3
99.9
Run1, Page3 of 11
A-5
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
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
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
THC Inlet
(ppm)
86.9
86.6
86.2
86.8
87.3
87.9
83.9
86.1
92.9
95.4
94.8
94.1
92.5
91.3
93.2
93.2
94.4
93.4
93.2
91.2
89.8
88.2
86.2
83.4
81.4
76.8
72.7
74.1
74.0
75.0
75.9
76.5
78.0
79.7
78.5
75.5
THC Inlet
(ppmc)
260.7
259.8
258.6
260.4
261.9
263.7
251.7
258.3
278.7
286.2
284.4
282.3
277.5
273.9
279.6
279.6
283.2
280.2
279.6
273.6
269.4
264.6
258.6
250.2
244.2
230.4
218.1
222.3
222.0
225.0
227.7
229.5
234.0
239.1
235.5
226.5
THC Outlet
(ppm)
31.3
27.3
27.4
27.7
28.0
27.7
26.4
26.4
28.6
29.3
29.3
28.6
28.1
27.4
28.2
28.2
Outlet Spike
THC Outlet
(ppmc)
93.9
81.9
82.2
83.1
84
83.1
79.2
79.2
85.8
87.9
87.9
85.8
84.3
82.2
84.6
84.6
Run1, Page 4 of 11
A-6
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
10:48
10:49
10:50
10:51
1 0.52
10:53
10:54
10:55
10:56
10:57
10:58
10:59
11:00
11:01
11:02
11:03
11:04
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
11:24
11:25
11:26
11:27
11:28
11:29
THC Inlet
(ppm)
74.8
96.1
71.8
70.8
69.2
67.5
66.5
65.3
65.2
66.0
66.9
66.1
63.5
65.1
66.3
66.8
67.2
68.4
68.2
66.9
64.7
64.1
64.9
64.6
59.1
42.3
42.1
41.0
39.7
39.1
39.5
40.4
40.8
41.0
41.3
41.4
41.6
42.3
42.0
41.1
40.5
43.8
THC Inlet
(ppmc)
224.4
288.3
215.4
212.4
207.6
202.5
199.5
195.9
195.6
198.0
200.7
198.3
190.5
195.3
198.9
200.4
201.6
205.2
204.6
200.7
194.1
192.3
194.7
193.8
177.3
126.9
126.3
123.0
119.1
117.3
118.5
121.2
122.4
123.0
123.9
124.2
124.8
126.9
126.0
123.3
121.5
131.4
THC Outlet
(ppm)
26.7
26.3
27.1
28.1
28.1
27.7
28.0
27.5
27.8
29.0
30.2
30.2
28.1
29.2
30.6
31.1
31.2
32.3
32.3
31.4
29.6
29.2
30.3
30.1
30.1
30.3
30.4
30.2
28.5
28.2
28.6
29.4
30.4
31.0
31.2
31.7
31.7
32.5
32.4
31.4
30.6
32.1
THC Outlet
(ppmc)
80.1
78.9
81.3
84.3
84.3
83.1
84
82.5
83.4
87
90.6
90.6
84.3
87.6
91.8
93.3
93.6
96.9
96.9
94.2
88.8
87.6
90.9
90.3
90.3
90.9
91.2
90.6
85.5
84.6
85.8
88.2
91.2
93
93.6
95.1
95.1
97.5
97.2
94.2
91.8
96.3
Run1, Page 5 of 11
A-7
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
11:30
11:31
11:32
11:33
1 1 :34
11:35
11:36
11:37
11:38
11:39
11:40
11:41
11:42
11:43
1 1 :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)
50.3
63.1
69.9
71.8
70.3
69.0
67.8
68.4
74.1
77.3
Plant Problem
86.9
83.3
83.6
86.1
89.6
87.6
86.9
87.4
88.7
88.8
85.7
81.8
80.8
81.5
81.2
80.9
82.7
82.2
78.7
76.5
75.0
78.8
79.3
THC Inlet
(ppmc)
150.9
189.3
209.7
215.4
210.9
207.0
203.4
205.2
222.3
231.9
260.7
249.9
250.8
258.3
268.8
262.8
260.7
262.2
266.1
266.4
257.1
245.4
242.4
244.5
243.6
242.7
248.1
246.6
236.1
229.5
225.0
236.4
237.9
THC Outlet
(ppm)
32.9
33.2
32.5
32.0
30.7
29.2
28.4
28.2
30.1
31.3
32.1
30.9
31.8
32.4
34.0
33.1
32.7
32.6
33.1
32.8
32.0
30.5
29.8
30.1
30.1
29.9
30.7
30.9
29.5
28.5
28.1
28.9
29.3
THC Outlet
(ppmc)
98.7
99.6
97.5
96
92.1
87.6
85.2
84.6
90.3
93.9
96.3
92.7
95.4
97.2
102
99.3
98.1
97.8
99.3
98.4
96
91.5
89.4
90.3
90.3
89.7
92.1
92.7
88.5
85.5
84.3
86.7
87.9
Run1, Page 6 of 11
A-8
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
THC Inlet
(ppm)
77,5
75.5
73.6
75.0
72.1
74.7
80.1
83.6
84.0
82.5
81.3
77.7
75.4
73.0
69.2
72.7
76.1
75.8
76.0
76.9
76.4
75.0
74.1
71.0
68.7
68.8
70.5
73.1
75.7
78.6
80.9
75.3
71.3
69.1
66.9
66.2
65.8
66.4
66.3
65.5
64.3
64.6
THC Inlet
(ppmc)
232.5
226.5
220.8
225.0
216.3
224.1
240.3
250.8
252.0
247.5
243.9
233.1
226.2
219.0
207.6
218.1
228.3
227.4
228.0
230.7
229.2
225.0
222.3
213.0
206.1
206.4
211.5
219.3
227.1
235.8
242.7
225.9
213.9
207.3
200.7
198.6
197.4
199.2
198.9
196.5
192.9
193.8
THC Outlet
(ppm)
28.8
28.4
27.7
28.1
27.1
27.6
29.8
31.4
31.8
31.3
30.9
29.4
28.2
27.7
26.3
26.8
28.7
28.5
28.7
28.8
29.0
28.5
28.0
27.0
25.8
25.6
26.2
27.2
28.4
29.5
30.2
28.7
26.8
25.9
24.7
24.5
24.4
24.6
24.6
24.3
23.9
23.5
THC Outlet
(ppmc)
86.4
85.2
83.1
84.3
81.3
82.8
89.4
94.2
95.4
93.9
92.7
88.2
84.6
83.1
78.9
80.4
86.1
85.5
86.1
86.4
87
85.5
84
81
77.4
76.8
78.6
81.6
85.2
88.5
90.6
86.1
80.4
77.7
74.1
73.5
73.2
73.8
73.8
72.9
71.7
70.5
Run1, Page 7 of 11
A-9
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
12:54
12:55
12:56
12:57
12:58
12:59
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
THC Inlet
(ppm)
64.9
70.9
75.7
77.6
76.2
75.0
73.8
71.3
71.2
67.0
66.0
67.6
68.7
70.0
71.2
72.2
72.6
72.4
71.2
67.6
64.0
65.0
65.0
62.9
61.1
61.4
61.8
63.6
65.1
65.1
64.6
64.2
65.1
72.5
81.5
83.1
81.4
81.8
81.5
84.6
87.1
89.1
THC Inlet
(ppmc)
194.7
212.7
227.1
232.8
228.6
225.0
221.4
213.9
213.6
201.0
198.0
202.8
206.1
210.0
213.6
216.6
217.8
217.2
213.6
202.8
192.0
195.0
195.0
188.7
183.3
184.2
185.4
190.8
195.3
195.3
193.8
192.6
195.3
217.5
244.5
249.3
244.2
245.4
244.5
253.8
261.3
267.3
THC Outlet
(ppm)
23.9
25.5
27.9
28.8
28.5
28.0
27.4
26.4
26.3
24.5 -
24.2
24.7
25.1
25.5
26.4
26.8
27.0
27.0
26.6
25.2
23.7
23.8
24.0
23.2
22.5
22.4
22.6
23.4
24.3
24.2
23.7
23.8
23.7
26.5
30.3
31.6
30.8
30.6
30.1
31.0
32.4
33.0
THC Outlet
(ppmc)
71.7
76.5
83.7
86.4
85.5
84
82.2
79.2
78.9
73.5
72.6
74.1
75.3
76.5
79.2
80.4
81
81
79.8
75.6
71.1
71.4
72
69.6
67.5
67.2
67.8
70.2
72.9
72.6
71.1
71.4
71.1
79.5
90.9
94.8
92.4
91.8
90.3
93
97.2
99
A-10
Run1, PageS of 11
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
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
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
THC Inlet
(ppm)
90.4
89.4
88.1
86.0
84.1
82.0
81.9
84.1
84.8
86.3
86.9
85.9
85.4
84.6
83.2
81.5
81.2
84.5
86.0
86.0
86.1
87.7
88.9
87.1
86.1
80.7
80.3
Plant Problem
85.2
80.8
80.3
78.5
77.5
THC Inlet
(ppmc)
271.2
268.2
264.3
258.0
252.3
246.0
245.7
252.3
254.4
258.9
260.7
257.7
256.2
253.8
249.6
244.5
243.6
253.5
258.0
258.0
258.3
263.1
266.7
261.3
258.3
242.1
240.9
255.6
242.4
240.9
235.5
232.5
THC Outlet
(ppm)
33.5
33.1
32.3
31.4
30.6
29.6
29.4
30.6
30.9
31.5
31.9
31.4
31.2
31.1
30.3
29.8
29.5
30.6
31.2
31.3
31.1
31.8
32.1
31.4
31.0
29.1
27.7
28.1
26.9
27.3
27.4
27.1
THC Outlet
(ppmc)
100.5
99.3
96.9
94.2
91.8
88.8
88.2
91.8
92.7
94.5
95.7
94.2
93.6
93.3
90.9
89.4
88.5
91.8
93.6
93.9
93.3
95.4
96.3
94.2
93
87.3
83.1
84.3
80.7
81.9
82.2
81.3
Run1, Page 9 of 11
A-ll
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
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
THC Inlet
(ppm)
77.8
80.0
82.5
82.4
80.9
81.0
80.2
79.2
78.8
79.0
84.1
104.0
163.1
176.9
176.4
174.1
171.0
168.6
149.1
141.6
147.4
145.3
149.7
145.7
147.5
146.4
148.7
147.7
143.8
142.9
138.4
138.3
136.7
133.8
132.9
133.9
132.2
136.8
138.4
140.1
139.5
137.0
THC Inlet
(ppmc)
233.4
240.0
247.5
247.2
242.7
243.0
240.6
237.6
236.4
237.0
252.3
312.0
489.3
530.7
529.2
522.3
513.0
505.8
447.3
424.8
442.2
435.9
449.1
437.1
442.5
439.2
446.1
443.1
431.4
428.7
415.2
414.9
410.1
401.4
398.7
401.7
396.6
410.4
415.2
420.3
418.5
411.0
THC Outlet
(ppm)
27.6
28.3
29.6
29.8
29.3
28.8
28.8
28.4
28,2
28.1
29.9
35.4
62.6
70.1
71.5
71.6
71.5
71.6
65.5
62.6
66.7
67.8
71.5
72.0
74.4
75.4
78.5
79.9
79.6
80.6
80.2
80.2
81.1
80.2
80.8
81.5
81.0
83.4
84.3
85.2
85.0
82.8
THC Outlet
(ppmc)
82.8
84.9
88.8
89.4
87.9
86.4
86.4
85.2
84.6
84.3
89.7
106.2
187.8
210.3
214.5
214.8
214.5
214.8
196.5
187.8
200.1
203.4
214.5
216
223.2
226.2
235.5
239.7
238.8
241.8
240.6
240.6
243.3
240.6
242.4
244.5
243
250.2
252.9
255.6
255
248.4
Run1, Page 10 of 11
A-12
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
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
Minimum=
Maximum=
Average=
THC Inlet
(ppm)
139.8
138.5
140.3
140.6
139.7
139.6
141.5
145.4
144.7
146.5
146.3
152.1
158.2
152.6
153.4
155.8
154.2
150.6
151.0
105.9
41.6
34.2
34.2
176.9
85.8
THC Inlet
(ppmc)
419.4
415.5
420.9
421.8
419.1
418.8
424.5
436.2
434.1
439.5
438.9
456.3
474.6
457.8
460.2
467.4
462.6
451.8
453.0
317.7
124.8
102.6
102.6
530.7
257.4
THC Outlet
(ppm)
83.5
82.2
82.8
82.5
81.4
81.1
80.6
82.9
82.6
83.2 -
82.5
84.9
88.3
86.9
87.0
88.6
88.5
86.0
86.1
86.2
84.6
81.9
22.4
88.6
38.3
THC Outlet
(ppmc)
250.5
246.6
248.4
247.5
244.2
243.3
241.8
248.7
247.8
249.6
247.5
254.7
264.9
260.7
261
265.8
265.5
258
258.3
258.6
253.8
245.7
67.2
265.8
114.9
A-13
Run1, Page 11 of 11
-------
Run 1
Date: 8/27/97
Project No: 3804-24-04-03
Operator: Gulick
600.0
E 500.0 --
a.
^ 400.0 --
'5 300.0 4-
g 200.0 +
100.0 I
0.0
o
o
Inlet Run 1
k^
00,00000000000
Time
300
1 250
a
^200 +
o
'•£ 150 -k
| 100 --
U 50 "
0
o
o
oo
Outlet Run 1
oooooooo
OO ON CTv o' o' •—• —' CN
Time
Run1
A-14
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
7:44
7:45
7:46
7:47
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
THC Inlet
(ppm)
69.9
61.3
60.6
61.2
61.3
62.2
63.9
66.1
67.1
68.1
67.2
68.5
67.9
68.2
69.1
68.2
67.8
68.1
68.0
67.9
68.3
66.7
66.0
67.3
67.4
67.3
66.5
65.6
69.4
98.8
99.9
98.8
97.5
96.0
95.4
93.8
93.2
93.4
93.3
THC Inlet
(ppmc)
209.7
183.9
181.8
183.6
183.9
186.6
191.7
198.3
201.3
204.3
201.6
205.5
203.7
204.6
207.3
204.6
203.4
204.3
204.0
203.7
204.9
200.1
198.0
201.9
202.2
201.9
199.5
196.8
208.2
296.4
299.7
296.4
292.5
288.0
286.2
281.4
279.6
280.2
279.9
THC Outlet
(ppm)
51.1
43.9
42.9
43.8
44.3
44.6
46.5
48.1
49.2
50.6
62.1
Outlet Spike
57.0
56.3
55.8
53.9
52.4
53.1
51.1
49.7
48.8
47.6
46.8
46.4
46.8
THC Outlet
(ppmc)
153.3
131.7
128.7
131.4
132.9
133.8
139.5
144.3
147.6
151.8
186.3
171
168.9
167.4
161.7
157.2
159.3
153.3
149.1
146.4
142.8
140.4
139.2
140.4
Run2, Page 1 of 11
A-15
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator Gulick "
Time
(24 hr)
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
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
THC Inlet
(ppm)
94.5
94.5
95.9
93.4
78.8
46.2
47.2
48.1
47.1
45.7
44.3
45.1
45.3
43.3
39.9
40.4
43.1
46.4
47.5
48.9
50.0
59.3
63.9
64.8
64.9
63.6
63.0
63.8
65.8
68.6
70.3
72.0
73.2
73.5
72.5
67.5
53.6
52.2
54.1
Plant Problem
THC Inlet
(ppmc)
283.5
283.5
287.7
280.2
236.4
138.6
141.6
144.3
141.3
137.1
132.9
135.3
135.9
129.9
119.7
121.2
129.3
139.2
142.5
146.7
150.0
177.9
191.7
194.4
194.7
190.8
189.0
191.4
197.4
205.8
210.9
216.0
219.6
220.5
217.5
202.5
160.8
156.6
162.3
THC Outlet
(ppm)
48.6
48.2
49.9
48.1
46.5
47.3
48.3
49.5
48.8
47.3
46.0
46.2
46.5
46.1
41.7
41.6
44.4
47.8
49.7
50.3
51.8
54.0
56.7
57.2
57.2
54.5
54.9
54.9
56.7
59.0
60.7
62.0
63.0
63.4
62.4
60.5
47.6
45.0
45.6
THC Outlet
(ppmc)
145.8
144.6
149.7
144.3
139.5
141.9
144.9
148.5
146.4
141.9
138
138.6
139.5
138.3
125.1
124.8
133.2
143.4
149.1
150.9
155.4
162
170.1
171.6
171.6
163.5
164.7
164.7
170.1
177
182.1
186
189
190.2
187.2
181.5
142.8
135
136.8
Run2, Page 2 of 11
A-16
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator Gulick
Time
(24 hr)
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
THC Inlet
(ppm)
40.9
51.6
69.2
51.9
48.5
54.2
57.4
60.9
60.3
62.1
61.1
60.2
59.8
59.8
59.5
58.9
59.1
58.1
57.5
58.4
59.7
53.9
50.4
48.9
50.6
52.0
53.6
54.7
55.1
55.1
54.3
53.6
55.5
59.4
53.8
54.1
55.1
THC Inlet
(ppmc)
122.7
154.8
207.6
155.7
145.5
162.6
172.2
182.7
180.9
186.3
183.3
180.6
179.4
179.4
178.5
176.7
177.3
174.3
172.5
175.2
179.1
161.7
151.2
146.7
151.8
156.0
160.8
164.1
165.3
165.3
162.9
160.8
166.5
178.2
161.4
162.3
165.3
THC Outlet
(ppm)
36.2
30.6
61.1
43.6
39.2
43.2
46.9
49.8
50.2
51.7
51.2
50.1
49.6
49.8
49.2
49.0
49.0
48.4
47.9
48.5
49.8
46.7
40.9
41.3
41.1
42.5
43.5
44.4
44.7
44.8
43.9
43.2
43.8
48.4
43.9
43.6
44.4
THC Outlet
(ppmc)
108.6
91.8
183.3
130.8
117.6
129.6
140.7
149.4
150.6
155.1
153.6
150.3
148.8
149.4
147.6
147
147
145.2
143.7
145.5
149.4
140.1
122.7
123.9
123.3
127.5
130.5
133.2
134.1
134.4
131.7
129.6
131.4
145.2
131.7
130.8
133.2
Run2, Page 3 of 11
A-17
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
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
10:16
10:17
10:18
10:19
10:20
10:21
10:22
THC Inlet
(ppm)
56.4
57.4
57.8
59.4
60.5
61.6
58.0
54.2
55.9
57.2
58.6
58.6
58.4
58.5
58.6
57.9
54.2
50.2
54.1
56.9
58.3
58.5
57.9
58.2
57.8
58.0
54.2
52.9
55.2
56.2
56.9
58.3
59.5
59.3
55.1
45.1
48.2
49.7
48.0
47.8
THC Inlet
(ppmc)
169.2
172.2
173.4
178.2
181.5
184.8
174.0
162.6
167.7
171.6
175.8
175.8
175.2
175.5
175.8
173.7
162.6
150.6
162.3
170.7
174.9
175.5
173.7
174.6
173.4
174.0
162.6
158.7
165.6
168.6
170.7
174.9
178.5
177.9
165.3
135.3
144.6
149.1
144.0
143.4
THC Outlet
(ppm)
45.1
46.5
47.0
47.9
48.9
49.7
47.8
43.2
44.2
45.5
46.9
46.9
46.8
46.8
47.0
46.4
44.8
40.5
43.0
46.4
47.4
47.4
46.5
47.1
46.6
46.4
44.5
42.2
44.3
45.5
46.0
46.8
47.8
48.0
45.3
36.8
37.8
39.9
38.2
38.1
THC Outlet
(ppmc)
135.3
139.5
141
143.7
146.7
149.1
143.4
129.6
132.6
136.5
140.7
140.7
140.4
140.4
141
139.2
134.4
121.5
129
139.2
142.2
142.2
139.5
141.3
139.8
139.2
133.5
126.6
132.9
136.5
138
140.4
143.4
144
135.9
110.4
113.4
119.7
114.6
114.3
Run2, Page 4 of 11
A-18
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
11:00
11:01
11:02
THC Inlet
(ppm)
47.4
48.4
50.8
51.9
48.9
54.4
59.4
56.6
55.2
56.5
57.1
59.1
61.8
61.5
63.3
63.7
64.8
65.5
58.5
56.4
58.3
59.8
61.6
55.3
54.4
61.4
60.3
57.1
52.6
50.4
53.8
56.0
59.0
56.7
55.2
58.1
54.7
52.4
50.7
50.9
THC Inlet
(ppmc)
142.2
145.2
152.4
155.7
146.7
163.2
178.2
169.8
165.6
169.5
171.3
177.3
185.4
184.5
189.9
191.1
194.4
196.5
175.5
169.2
174.9
179.4
184.8
165.9
163.2
184.2
180.9
171.3
157.8
151.2
161.4
168.0
177.0
170.1
165.6
174.3
164.1
157.2
152.1
152.7
THC Outlet
(ppm)
37.4
38.0
40.1
41.7
38.9
41.9
46.5
45.9
43.7
45.1
46.3
47.5
49.6
49.7
51.3
51.2
52.3
52.6
47.8
44.1
45.9
47.2
48.7
45.1
42.1
48.5
48.4
45.7
42.1
39.9
42.1
44.1
46.4
45.9
43.6
47.6
43.7
41.3
39.5
39.6
THC Outlet
(ppmc)
112.2
114
120.3
125.1
116.7
125.7
139.5
137.7
131.1
135.3
138.9
142.5
148.8
149.1
153.9
153.6
156.9
157.8
143.4
132.3
137.7
141.6
146.1
135.3
126.3
145.5
145.2
137.1
126.3
119.7
126.3
132.3
139.2
137.7
130.8
142.8
131.1
123.9
118.5
118.8
Run2, Page 5 of 11
A-19
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
11:03
11:04
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
11:24
11:25
11:26
11:27
11:28
11:29
1 1 :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
THC Inlet
(ppm)
44.0
41.7
43.9
44.9
42.3
41.9
43.0
43.9
44.8
Plant Problem
54.4
22.6
56.9
60.8
42.4
33.7
32.9
33.3
34.1
36.0
38.0
40.6
46.9
54.5
60.5
62.8
61.6
64.0
61.2
67.2
68.6
67.2
66.0
THC Inlet
(ppmc)
132.0
125.1
131.7
134.7
126.9
125.7
129.0
131.7
134.4
163.2
67.8
170.7
182.4
127.2
101.1
98.7
99.9
102.3
108.0
114.0
121.8
140.7
163.5
181.5
188.4
184.8
192.0
183.6
201.6
205.8
201.6
198.0
THC Outlet
(ppm)
35.0
32.2
33.4
34.7
32.9
31.9
32.8
33.3
33.9
87.0
19.2
32.4
47.8
31.9
24.7
23.3
23.5
24.4
25.3
27.0
29.0
32.9
39.0
44.5
46.5
46.7
49.0
46.4
50.3
52.4
51.8
50.5
THC Outlet
(ppmc)
105
96.6
100.2
104.1
98.7
95.7
98.4
99.9
101.7
261
57.6
97.2
143.4
95.7
74.1
69.9
70.5
73.2
75.9
81
87
98.7
117
133.5
139.5
140.1
147
139.2
150.9
157.2
155.4
151.5
Run2, Page 6 of 11
A-20
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator Gulick
Time
(24 hr)
11:43
11:44
11:45
11:46
1 1 .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
12:12
12:13
12:14
12:15
12:16
12:17
12:18
12:19
12:20
12:21
12:22
THC Inlet
(ppm)
67.5
67.5
67.5
68.1
67.8
70.0
69.7
68.0
71.3
71.6
70.8
68.2
57.3
54.1
54.5
53.5
52.9
53.3
60.3
62.8
61.5
58.7
56.4
55.9
53.0
53.5
56.6
55.7
56.0
55.6
57.4
58.9
56.0
51.9
54.3
57.9
57.5
57.2
59.0
60.7
THC Inlet
(ppmc)
202.5
202.5
202.5
204.3
203.4
210.0
209.1
204.0
213.9
214.8
212.4
204.6
171.9
162.3
163.5
160.5
158.7
159.9
180.9
188.4
184.5
176.1
169.2
167.7
159.0
160.5
169.8
167.1
168.0
166.8
172.2
176.7
168.0
155.7
162.9
173.7
172.5
171.6
177.0
182.1
THC Outlet
(ppm)
51.4
51.9
51.7
51.9
52.1
53.1
53.6
51.9
53.8
54.5
53.9
52.6
44.4
40.7
40.5
40.4
39.5
39.5
44.4
47.4
47.3
44.8
42.8
42.7
40.6
39.7
42.7
41.8
42.5
42.5
43.4
44.6
43.5
39.3
40.5
44.1
43.9
44.1
45.5
47.0
THC Outlet
(ppmc)
154.2
155.7
155.1
155.7
156.3
159.3
160.8
155.7
161.4
163.5
161.7
157.8
133.2
122.1
121.5
121.2
118.5
118.5
133.2
142.2
141.9
134.4
128.4
128.1
121.8
119.1
128.1
125.4
127.5
127.5
130.2
133.8
130.5
117.9
121.5
132.3
131.7
132.3
136.5
141
Run2, Page 7 of 11
A-21
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
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
13:00
13:01
13:02
THC Inlet
(ppm)
60.1
58.9
59.1
57.3
57.7
58.9
59.9
63.5
60.6
56.7
54.1
52.5
51.2
50.1
48.2
45.0
43.7
42.4
44.0
45.9
47.1
48.6
46.9
44.8
43.7
42.5
42.5
44.1
43.6
45.5
43.7
39.1
36.5
35.9
34.7
33.8
34.4
35.9
35.6
34.1
THC Inlet
(ppmc)
180.3
176.7
177.3
171.9
173.1
176.7
179.7
190.5
181.8
170.1
162.3
157.5
153.6
150.3
144.6
135.0
131.1
127.2
132.0
137.7
141.3
145.8
140.7
134.4
131.1
127.5
127.5
132.3
130.8
136.5
131.1
117.3
109.5
107.7
104.1
101.4
103.2
107.7
106.8
102.3
THC Outlet
(ppm)
46.9
45.9
45.8
44.2
44.2
45.4
45.9
48.6
48.0
43.9
41.8
40.2
38.9
37.9
36.4
33.9
32.2
31.3
32.0
33.2
34.5
35.5
34.8
32.8
32.2
31.1
30.8
32.0
31.4
32.7
32.1
29.0
26.2
25.4
24.8
24.2
24.2
25.2
25.3
24.1
THC Outlet
(ppmc)
140.7
137.7
137.4
132.6
132.6
136.2
137.7
145.8
144
131.7
125.4
120.6
116.7
113.7
109.2
101.7
96.6
93.9
96
99.6
103.5
106.5
104.4
98.4
96.6
93.3
92.4
96
94.2
98.1
96.3
87
78.6
76.2
74.4
72.6
72.6
75.6
75.9
72.3
Run2, PageS of 11
A-22
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
THC Inlet
(ppm)
36.6
34.7
35.4
36.9
38.0
37.9
36.9
37.0
38.8
40.5
43.8
45.0
45.3
45.5
46.8
48.8
50.1
51.9
52.3
54.3
55.2
57.4
57.0
57.6
58.2
57.6
56.9
55.7
55.5
54.7
55.8
59.0
60.8
62.0
63.3
63.5
61.9
59.9
58.0
56.8
THC Inlet
(ppmc)
109.8
104.1
106.2
110.7
114.0
113.7
110.7
111.0
116.4
121.5
131.4
135.0
135.9
136.5
140.4
146.4
150.3
155.7
156.9
162.9
165.6
172.2
171.0
172.8
174.6
172.8
170.7
167.1
166.5
164.1
167.4
177.0
182.4
186.0
189.9
190.5
185.7
179.7
174.0
170.4
THC Outlet
(ppm)
25.2
24.5
24.7
26.0
27.7
28.1
27.1
27.1
28.2
29.5
32.1
33.1
34.2
34.2
35.6
37.1
38.4
40.0
40.6
41.6
43.2
44.5
45.0
45.0
45.8
45.4
44.3
43.7
43.3
42.7
42.7
45.6
47.5
48.7
49.8
50.3
48.9
47.0
44.7
43.7
THC Outlet
(ppmc)
75.6
73.5
74.1
78
83.1
84.3
81.3
81.3
84.6
88.5
96.3
99.3
102.6
102.6
106.8
111.3
115.2
120
121.8
124.8
129.6
133.5
135
135
137.4
136.2
132.9
131.1
129.9
128.1
128.1
136.8
142.5
146.1
149.4
150.9
146.7
141
134.1
131.1
A-23
Run2, Page 9 of 11
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
13:43
13:44
13:45
13:46
13:47
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
THC Inlet
(ppm)
56.1
56.0
58.2
57.6
55.3
54.3
53.1
53.7
53.2
53.3
52.3
50.4
51.3
108.4
435.9
481.3
381.5
314.6
273.3
245.0
189.9
54.1
45.9
95.5
68.0
56.4
52.1
50.6
49.7
48.9
48.0
48.6
49.2
49.7
52.5
53.2
53.1
52.9
52.5
52.3
THC Inlet
(ppmc)
168.3
168.0
174.6
172.8
165.9
162.9
159.3
161.1
159,6
159.9
156.9
151.2
153.9
325.2
1307.7
1443.9
1144.5
943.8
819.9
735.0
569.7
162.3
137.7
286.5
204.0
169.2
156.3
151.8
149.1
146.7
144.0
145.8
147.6
149.1
157.5
159.6
159.3
158.7
157.5
156.9
THC Outlet
(ppm)
42.9
42.7
43.7
44.1
41.9
40.7
40.4
40.4
40.1
39.5
39.3
37.1
38.2
40.8
45.2
64.9
88.4
77.7
72.9
64.4
89.0
53.8
23.1
67.8
51.6
40.1
35.0
33.9
33.2
32.8
32.4
32.4
33.6
33.8
35.5
36.1
36.4
36.4
36.3
36.1
THC Outlet
(ppmc)
128.7
128.1
131.1
132.3
125.7
122.1
121.2
121.2
120.3
118.5
117.9
111.3
114.6
122.4
135.6
194.7
265.2
233.1
218.7
193.2
267
161.4
69.3
203.4
154.8
120.3
105
101.7
99.6
98.4
97.2
97.2
100.8
101.4
106.5
108.3
109.2
109.2
108.9
108.3
Run2, Page 10 of 11
A-24
-------
Run 2
Date: 8/28/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
14:23
14:24
14:25
14:26
14:27
14:28
14:29
14:30
14:31
Minimum=
Maximum=
Average=
THC Inlet
(ppm)
51.7
51.3
51.8
50.8
49.5
49.3
49.1
49.0
49.4
22.6
481.3
61.4
THC Inlet
(ppmc)
155.1
153.9
155.4
152.4
148.5
147.9
147.3
147.0
148.2
67.8
1443.9
184.1
THC Outlet
(ppm)
36.0
35.5
35.8
35.2
34.0
33.6
34.0
33.6
33.8
19.2
89.0
43.6
THC Outlet
(ppmc)
108
106.5
107.4
105.6
102
100.8
102
100.8
101.4
57.6
267.0
130.7
A-25
Run2, Page 11 of 11
-------
73
c
^
M
Concentration, ppmc
c
7:00
7:30
8:00 -
8:30
9:00
9.30
10:00
10:30
§' 11:00
n
11:30
12:00
12:30
13:00
13:30
14:00
14:30
15:00
o o o o o
3 O 0 O O O
1
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y
%
I
j
X
/
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r
3
(*
f~
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f
pfl
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Concentration, ppmc
c
c
7:00
7:30
8:00 -
8:30 -
9:00
9:30
10:00
10:30
§' 11:00
11:30
12:00
12:30 -
13:00 -
13:30
14:00
14:30
15:00
o o o o o
D O O O O O
3 O O O O O
<-
1
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s
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1
^
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9
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00
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
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
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
THC Inlet
(ppm)
20.7
33.0
31.9
28.4
22.8
20.2
22.1
32.6
38.4
43.2
48.8
53.9
54.3
53.9
53.2
53.9
54.4
53.6
53.6
53.5
53.4
52.3
52.4
53.5
53.4
53.0
67.5
93.9
95.5
95.1
96.4
96.7
94.5
94.9
95.2
93.3
93.9
95.4
94.5
93.3
94.5
THC Inlet
(ppmc)
62.1
99.0
95.7
85.2
68.4
60.6
66.3
97.8
115.2
129.6
146.4
161.7
162.9
161.7
159.6
161.7
163.2
160.8
160.8
160.5
160.2
156.9
157.2
160.5
160.2
159.0
202.5
281.7
286.5
285.3
289.2
290.1
283.5
284.7
285.6
279.9
281.7
286.2
283.5
279.9
283.5
THC Outlet
(ppm)
43.6
47.0
45.9
36.8
27.9
18.5
22.4
38.7
51.9 .
61.2
69.9
82.9
85.6
85.6
86.4
87.8
87.1
85.9
85.2
85.3
85.2
85.1
84.8
84.3
84.5
84.5
97.6
82.5
79.9
79.5
79.3
79.6
78.1
78.0
77.7
76.8
76.7
77.1
76.6
75.6
76.0
THC Outlet
(ppmc)
130.8
141
137.7
110.4
83.7
55.5
67.2
116.1
155.7
183.6
209.7
248.7
256.8
256.8
259.2
263.4
261.3
257.7
255.6
255.9
255.6
255.3
254.4
252.9
253.5
253.5
292.8
247.5
239.7
238.5
237.9
238.8
234.3
234
233.1
230.4
230.1
231.3
229.8
226.8
228
A-27
Run3, Page 1 of 9
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
9:28
9:29
9:30
9:31
9:32
9:33
9:34
9:35
9:36
9:37
9:38
THC Inlet
(ppm)
95.5
95.7
96.7
98.0
97.0
96.6
97.5
96.1
96.3
96.5
95.6
96.4
97.1
95.6
94.0
94.4
94.7
93.8
94.9
96.3
95.0
95.6
94.6
95.6
95.1
95.7
94.9
93.4
94.9
93.4
94.2
94.7
95.0
93.6
93.0
93.5
93.4
93.7
93.6
93.0
92.6
92.5
THC Inlet
(ppmc)
286.5
287.1
290.1
294.0
291.0
289.8
292.5
288.3
288.9
289.5
286.8
289.2
291.3
286.8
282.0
283.2
284.1
281.4
284.7
288.9
285.0
286.8
283.8
286.8
285.3
287.1
284.7
280.2
284.7
280.2
282.6
284.1
285.0
280.8
279.0
280.5
280.2
281.1
280.8
279.0
277.8
277.5
THC Outlet
(ppm)
76.6
76.6
77.4
78.3
77.5
77.2
74.5
67.6
66.8
67.9
67.2
67.5
67.6
67.5
65.5
65.9
66.6
65.6
65.9
66.9
66.2
66.6
66.2
66.5
66.3
70.3
78.3
78.1
78.2
78.1
77.7
78.8
78.6
78.1
76.6
77.2
77.5
77.8
77.4
77.2
77.0
76.2
THC Outlet
(ppmc)
229.8
229.8
232.2
234.9
232.5
231.6
223.5
202.8
200.4
203.7
201.6
202.5
202.8
202.5
196.5
197.7
199.8
196.8
197.7
200.7
198.6
199.8
198.6
199.5
198.9
210.9
234.9
234.3
234.6
234.3
233.1
236.4
235.8
234.3
229.8
231.6
232.5
233.4
232.2
231.6
231
228.6
A-28
Run3, Page 2 of 9
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick .
Time
(24 hr)
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
10:16
10:17
10:18
10:19
10:20
THC Inlet
(ppm)
93.0
92.5
94.2
93.4
94.0
95.4
94.9
94.7
95.4
95.0
94.1
94.7
95.0
95.3
93.8
93.7
95.4
81.3
66.2
62.7
40.4
37.6
37.9
27.5
19.9
20.8
20.8
21.0
22.0
21.9
25.3
26.5
26.7
24.9
24.2
33.7
43.7
45.3
47.0
38.8
22.7
9.0
THC Inlet
(ppmc)
279.0
277.5
282.6
280.2
282.0
286.2
284.7
284.1
286.2
285.0
282.3
284.1
285.0
285.9
281.4
281.1
286.2
243.9
198.6
188.1
121.2
112.8
113.7
82.5
59.7
62.4
62.4
63.0
66.0
65.7
75.9
79.5
80.1
74.7
72.6
101.1
131.1
135.9
141.0
116.4
68.1
27.0
THC Outlet
(ppm)
77.0
76.0
77.0
76.9
76.9
78.4
78.3
78.6
78.5
78.2
77.4
77.5
77.8
78.4
77.1
76.9
78.0
70.6
57.1
53.0
37.2
31.3
31.5
25.3
17.2
17.1
17.7
17.5
18.4
18.1
20.1
21.5
22.0
20.7
19.9
25.1
35.3
36.5
38.8
34.1
20.5
9.2
THC Outlet
(ppmc)
231
228
231
230.7
230.7
235.2
234.9
235.8
235.5
234.6
232.2
232.5
233.4
235.2
231.3
230.7
234
211.8
171.3
159
111.6
93.9
94.5
75.9
51.6
51.3
53.1
52.5
55.2
54.3
60.3
64.5
66
62.1
59.7
75.3
105.9
109.5
116.4
102.3
61.5
27.6
Run3, Page 3 of 9
A-29
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick •
Time
(24 hr)
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
11:00
11:01
11:02
THC Inlet
(ppm)
6.6
7.0
6.7
6.4
6.4
6.4
6.4
6.8
6.9
6.8
6.8
7.1
7.0
7.0
6.9
6.7
6.8
7.0
7.2
7.3
7.3
7.1
7.0
7.1
7.2
6.9
7.1
7.1
6.9
7.0
7.0
7.2
7.1
7.3
7.1
7.0
6.9
6.9
6.6
6.5
6.7
6.6
THC Inlet
(ppmc)
19.8
21.0
20.1
19.2
19.2
19.2
19.2
20.4
20.7
20.4
20.4
21.3
21.0
21.0
20.7
20.1
20.4
21.0
21.6
21.9
21.9
21.3
21.0
21.3
21.6
20.7
21.3
21.3
20.7
21.0
21.0
21.6
21.3
21.9
21.3
21.0
20.7
20.7
19.8
19.5
20.1
19.8
THC Outlet
(ppm)
5.7
5.8
5.7
5.4
5.3
5.8
5.7
5.7
5.6
5.7
5.8
5.9
5.8
5.9
5.9
5.8
5.7
5.8
6.2
6.1
6.2
6.2
5.9
6.1
6.1
5.8
5.9
6.0
6.0
5.9
6.2
6.0
6.1
6.1
6.1
6.0
5.9
5.8
5.7
5.7
5.6
5.7
THC Outlet
(ppmc)
17.1
17.4
17.1
16.2
15.9
17.4
17.1
17.1
16.8
17.1
17.4
17.7
17.4
17.7
17.7
17.4
17.1
17.4
18.6
18.3
18.6
18.6
17.7
18.3
18.3
17.4
17.7
18
18
17.7
18.6
18
18.3
18.3
18.3
18
17.7
17.4
17.1
17.1
16.8
17.1
Run3, Page 4 of 9
A-30
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
11:03
11:04
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
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
THC Inlet
(ppm)
6.9
7.1
6.9
7.0
7.1
6.7
6.8
7.1
6.9
7.0
7.0
7.2
7.0
7.1
6.5
6.3
6.3
6.3
6.5
6.4
6.5
6.2
6.2
6.0
5.9
6.0
6.0
6.0
5.9
5.9
5.9
5.8
6.0
6.0
5.9
5.9
5.9
5.8
5.7
5.9
5.8
5.8
THC Inlet
(ppmc)
20.7
21.3
20.7
21.0
21.3
20.1
20.4
21.3
20.7
21.0
21.0
21.6
21.0
21.3
19.5
18.9
18.9
18.9
19.5
19.2
19.5
18.6
18.6
18.0
17.7
18.0
18.0
18.0
17.7
17.7
17.7
17.4
18.0
18.0
17.7
17.7
17.7
17.4
17.1
17.7
17.4
17.4
THC Outlet
(ppm)
5.7
5.9
5.9
6.0
5.9
6.4
6.2
5.8
6.2
5.6
6.1
6.2
6.3
5.6
5.8
5.4
5.4
5.5
5.5
5.5
5.6
5.4
5.4
5.3
5.2
5.3
5.3
5.3
5.3
5.3
5.3
5.4
5.3
5.3
5.3
5.2
5.1
5.1
5.0
5.3
5.1
5.1
THC Outlet
(ppmc)
17.1
17.7
17.7
18
17.7
19.2
18.6
17.4
18.6
16.8
18.3
18.6
18.9
16.8
17.4
16.2
16.2
16.5
16.5
16.5
16.8
16.2
16.2
15.9
15.6
15.9
15.9
15.9
15.9
15.9
15.9
16.2
15.9
15.9
15.9
15.6
15.3
15.3
15
15.9
15.3
15.3
Run3, Page 5 of 9
A-31
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick •
Time
(24 hr)
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
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
THC Inlet
(ppm)
5.9
5.9
5.9
5.9
5.8
5.7
5.9
5.9
5.9
6.0
6.1
5.8
6.1
6.0
5.8
5.8
6.0
5.9
6.0
6.2
6.0
6.1
6.1
6.0
6.1
6.3
6.3
28.1
139.7
192.9
155.8
122.9
102.4
77.2
20.3
11.4
64.2
35.2
17.5
12.5
10.5
9.7
THC Inlet
(ppmc)
17.7
17.7
17.7
17.7
17.4
17.1
17.7
17.7
17.7
18.0
18.3
17.4
18.3
18.0
17.4
17.4
18.0
17.7
18.0
18.6
18.0
18.3
18.3
18.0
18.3
18.9
18.9
84.3
419.1
578.7
467.4
368.7
307.2
231.6
60.9
34.2
192.6
105.6
52.5
37.5
31.5
29.1
THC Outlet
(ppm)
5.3
5.3
5.2
5.2
5.2
5.1
5.2
5.2
5.4
5.4
5.4
5.2
5.2
5.4
5.2
5.3
5.3
5.4
5.4
5.4
5.4
5.4
5.4
5.4
5.4
5.4
5.5
5.4
8.0
15.9
19.8
20.4
19.6
26.7
19.0
4.6
37.1
26.1
10.8
7.7
6.8
6.6
THC Outlet
(Ppmc)
15.9
15.9
15.6
15.6
15.6
15.3
15.6
15.6
16.2
16.2
16.2
15.6
15.6
16.2
15.6
15.9
15.9
16.2
16.2
16.2
16.2
16.2
16.2
16.2
16.2
16.2
16.5
16.2
24
47.7
59.4
61.2
58.8
80.1
57
13.8
111.3
78.3
32.4
23.1
20.4
19.8
A-32
Run3, Page 6 of 9
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator Gulick
Time
(24 hr)
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
13:00
13:01
13:02
13:03
13:04
13:05
13:06
13:07
13:08
THC Inlet
(ppm)
9.3
9.2
8.7
8.9
13.9
33.0
50.8
57.5
61.7
63.9
64.6
64.9
64.6
64.9
63.5
59.1
105.7
269.3
271.9
212.3
172.8
150.1
129.9
113.5
107.7
91.4
88.0
82.8
74.2
71.3
62.4
59.8
54.2
48.8
48.6
45.3
40.1
39.9
33.8
32.5
30.4
26.7
THC Inlet
(ppmc)
27.9
27.6
26.1
26.7
41.7
99.0
152.4
172.5
185.1
191.7
193.8
194.7
193.8
194.7
190.5
177.3
317.1
807.9
815.7
636.9
518.4
450.3
389.7
340.5
323.1
274.2
264.0
248.4
222.6
213.9
187.2
179.4
162.6
146.4
145.8
135.9
120.3
119.7
101.4
97.5
91.2
80.1
THC Outlet
(ppm)
6.8
6.7
6.9
6.9
9.4
26.5
44.4
53.2
58.4
59.8
60.1
59.8
59.1
59.6
58.7
54.7
50.1
49.4
55.9
55.5
60.4
48.3
53.1
47.3
39.6
38.4
31.3
35.8
35.4
28.1
35.9
37.8
35.6
40.9
34.0
34.6
36.0
31.7
35.1
30.9
30.5
35.2
THC Outlet
(ppmc)
20.4
20.1
20.7
20.7
28.2
79.5
133.2
159.6
175.2
179.4
180.3
179.4
177.3
178.8
176.1
164.1
150.3
148.2
167.7
166.5
181.2
144.9
159.3
141.9
118.8
115.2
93.9
107.4
106.2
84.3
107.7
113.4
106.8
122.7
102
103.8
108
95.1
105.3
92.7
91.5
105.6
Run3, Page 7 of 9
A-33
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick -
Time
(24 hr)
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
THC Inlet
(ppm)
26.6
24.7
25.2
24.7
22.7
22.9
20.7
18.7
18.3
18.9
17.2
16.9
9.3
5.4
13.6
53.0
21.9
25.3
46.0
46.0
44.9
44.2
44.2
44.2
44.0
44.4
44.6
45.2
45.3
45.5
44.7
44.0
43.3
42.1
42.1
42.1
45.6
46.3
47.2
46.2
45.8
45.6
THC Inlet
(ppmc)
79.8
74.1
75.6
74.1
68.1
68.7
62.1
56.1
54.9
56.7
51.6
50.7
27.9
16.2
40.8
159.0
65.7
75.9
138.0
138.0
134.7
132.6
132.6
132.6
132.0
133.2
133.8
135.6
135.9
136.5
134.1
132.0
129.9
126.3
126.3
126.3
136.8
138.9
141.6
138.6
137.4
136.8
THC Outlet
(ppm)
30.0
24.9
21.4
18.8
20.1
17.7
21.6
18.1
18.0
14.7
15.4
14.2
17.5
4.3
11.4
44.8
18.0
16.2
37.8
38.0
36.3
35.7
35.8
35.8
35.9
36.3
36.5
37.1
38.0
38.5
37.8
37.1
36.6
35.6
35.4
35.1
37.7
38.9
39.7
39.0
38.7
38.6
THC Outlet
(ppmc)
90
74.7
64.2
56.4
60.3
53.1
64.8
54.3
54
44.1
46.2
42.6
52.5
12.9
34.2
134.4
54
48.6
113.4
114
108.9
107.1
107.4
107.4
107.7
108.9
109.5
111.3
114
115.5
113.4
111.3
109.8
106.8
106.2
105.3
113.1
116.7
119.1
117
116.1
115.8
Run3, Page 8 of 9
A-34
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick
Time
(24 hr)
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
Minimum=
Maximum=
Average=
THC Inlet
(ppm)
45.8
45.1
44.3
44.7
44.1
44.8
48.3
54.2
53.6
53.2
54.3
54.3
55.0
54.5
54.6
53.7
53.1
53.5
54.3
54.2
52.3
52.0
5.4
271.9
46.1
THC Inlet
(ppmc)
137.4
135.3
132.9
134.1
132.3
134.4
144.9
162.6
160.8
159.6
162.9
162.9
165.0
163.5
163.8
161.1
159.3
160.5
162.9
162.6
156.9
156.0
16.2
815.7
138.2
THC Outlet
(ppm)
39.0
38.5
37.7
37.8
37.7
37.7
40.4
46.4
46.5
45.5
46.5
46.3
46.9
46.6
46.8
46.3
45.3
45.1
46.2
46.6
44.6
44.7
4.3
97.6
35.7
THC Outlet
(ppmc)
117
115.5
113.1
113.4
113.1
113.1
121.2
139.2
139.5
136.5
139.5
138.9
140.7
139.8
140.4
138.9
135.9
135.3
138.6
139.8
133.8
134.1
12.9
292.8
107.2
A-35
Run3, Page 9 of 9
-------
Run 3
Date: 8/29/97
Project No: 3804-24-04-03
Operator: Gulick
a.
a.
s
o
U
900.0
800.0
700.0
600.0
500.0
400.0
300.0
200.0
100.0
0.0
Inlet Run 3
o
p
oei
o
ri
do
ON
O
r-i
ON
O
O
O
O
O
r-i
O
O
o — —
o
rf
Time
300
Outlet Run 3
„ 250
S
a 200 --
*s
.1 150 4-
too --
o 50 +
U
0
oo
o
fp
oo
O
rp
ON'
o
o
O
O
O
O
o
rr
Time
Run3
A-36
-------
A-2 METHOD 25A CALIBRATION AND QC CHECK DATA
A-37
-------
A-38
-------
Calibration Error Determination for 8/27/97
THC 1
Inlet
THC 2
Outlet
Pass/Fail
Cal Gas
Value
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is
Predicted Measured
Value Value
0.0
917.0
512.6 505.0
256.3 247.0
1.4
917.0
513.2 509.0
257.3 251.0
+/- 5% of Calibration Gas
Difference as
% of Cal Gas
0.0
2.1
1.5
3.6
0.1
2.1
0.8
2.5
Calibration Drift determination for 8/27/97
THC 1
Inlet
THC 2
Outlet
Initial
Value
0.0
1.4
Instrument Span for
Pass/Fail Criteria is
Initial
Value
Zero Drift
Final
Value
0.7
3.7
THC 1 and 2 is 1000 ppm
+/- 3% of Instrument Span
Span Drift
Final
Value
Difference as
% of Span
0.1
0.2
Difference as
% of Span
THC 1 917.0
Inlet
THC 2 917.0
Outlet
909.0
928.0
0.8
1.1
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and 2 is 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
A-39
-------
Calibration Error Determination for 8/28/97
Cal Gas Predicted Measured
Value Value Value
THC 1
Inlet
THC 2
Outlet
Pass/Fail
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is
0.4
909.0
508.3 504.0
254.4 248.0
1.8
913.0
511.2 505.0
256.5 248.0
+/- 5% of Calibration Gas
Difference as
% of Cal Gas
0.0
1.2
0.9
2.5
0.2
1.7
1.2
3.3
Calibration Drift determination for 8/28/97
THC 1
Inlet
THC 2
Outlet
Initial
Value
0.4
1.8
Instrument Span for
Pass/Fail Criteria is
Initial
Value
Zero Drift
Final
Value
0.2
2.1
THC 1 and 2 is 1000 ppm
+/- 3% of Instrument Span
Span Drift
Final
Value
Difference as
% of Span
0.0
0.0
Difference as
% of Span
THC 1 909.0
Inlet
THC 2 913.0
Outlet
908.0
915.0
0.1
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 2 is 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
A-40
-------
Calibration Error Determination for 8/29/97
THC 1
Inlet
THC 2
Outlet
Pass/Fail
Cal Gas
Value
0.0
898.0
502.0
251.0
0.0
898.0
502.0
251.0
Criteria is
Predicted Measured Difference as
Value Value % of Cal Gas
0.8
902.0
504.6 505.0
252.7 248.0
0.2
910.0
508.8 506.0
254.5 249.0
+/- 5% of Calibration Gas
0.1
0.4
0.1
1.9
0.0
1.3
0.5
2.2
Calibration Drift determination for 8/29/97
THC 1
Inlet
THC 2
Outlet
Initial
Value
0.8
0.2
Instrument Span for
Pass/Fail Criteria is
Initial
Value
Final
Value
0.9
0.9
THC 1 and 2 is 1000 ppm
+/- 3% of Instrument Span
Final
Value
Zero Drift
Difference as
% of Span
0.0
0.1
Span Drift
Difference as
% of Span
THC 1 902.0
Inlet
THC 2 910.0
Outlet
900.0
916.0
0.2
0.6
Pass/Fail
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Pass
Pass/Fail
Pass
Pass
Instrument Span for THC 1 and 2 is 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
A-41
-------
Response Times
1 32 Seconds
Inlet
THC 2 29 Seconds
Outlet
A-42
-------
A-3 VOLUMETRIC FLOW DATA
A-43
-------
A-44
-------
12 17 97 12:10 O19199410234
PES RTF NC
IgjOLO- 015
Summary of Stack Gaa Parameter* and Test Results
North Carolina
US EPA Teat Method 23 - PCOD / PCDF
Baghousa Inlet
Page 1 of 6
Y
AH
Pb.
vm
Tm
PI»
T.
vte
CO,
Oj
N,
cp
AP1/a
&
Dn
^
Vrna*
Vm<»«
P.
B_
v«^
1-a.
M,
M.
V.
A
Q,
Q.
QXO-O
l
RUNNUMBCR
RUN DATE
RUN TIMe
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. H2O
Barometric Pressure, inches Hg
Sample Volume, ft1
. • * 4. Y * «*IMM «e
Average Mew r em per aura , r*
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 Dp, (in. HjO)"1
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft1
Standard Meier Volume, dscf
Standard Meter Volume, dscm
Stack Pressure, inches Hg
Moisture. % by volume
Moisture (at saturation). % by vokime
Standard Water Vapor Volume, fr1
Dry Mole Fraction
Molecular Weight (d.b.), to/fc-mole
Molecular Weight (w.b.), fc/fe*mole
Stack Gaa Velocity, ft/s
Stack Area, ft1
Stack Gas Volumetric flow, acfm
Stack Gaa Volumetric flow, dscfm
Stack Gaa Volumetric flow, dscmm
Isokirtttte Sampling Ratio, *
R-M23+1 R-M13-t-2 RWM23-M
anr/TT »n9/91 9/2V97 Average
0940-1227 0909-1429 0919-1413
1.021
1.21
29.60
58.263
96
-1.8
308
510.5
5.2
13.8
81.0
0.84
0.6901
96
0.257
0.00036
56.399
1 597
29.67
29.9
522.4
24.029
0.701
29.38
25.98
49.5
16.20
48,074
22,981
650.7
115.0
.^^^•••^•^i^— >
1.021
0.286
29.60
53.015
96
-18
306
414.9
5.2
13.1
81.7
0.84
0.6756
170
0.194
0.00021
50.886
1.441
29.47
27.7
512.8
19.529
0.723
29.36
26.21
48.3
16.20
46,957
23,027
652.1
102.6
1.021
0.396
29.60
83.709
93
-1.8
290
393.0
4.0
15.2
80.8
0,84
0.7133
240
0.194
0.00021
80.735
2286
29.47
18.6
403.1
18.499
0.814
29.25
2715
49.6
16.20
48,211
27,178
769.6
97.7
•i^«— ^— ««™
1.021
0.631
29.67
64.996
95
-1 80
301
439.5
4.8
14.0
81.2
0.84
0.6930
169
0.215
0.00026
62.673
1 775
29.53
25.4
479.4
20.686
0.746
29.33
26.45
49.1
16.20
47,747
24,395
690.8
105.1
aneBB^BBBMB**"""""
A-45
-------
12 17 97
12: LO
©L91994L0234
PES RTF NC
OL5
Summary of Stack Gaa Parameters and Test Results
US EPA EMC Asphalt Concrete Emissions Testing
US EPA Teat Method 29 • Multiple Metals
Baghouse Inlet
Page 1 of 4
Y
AH
Pbar
vm
Tm
P.ude
T.
V,,.
COj
O2
N2
CP
Ap1/Z
0
Dn
^
vm(rw)rf
vj on
Qm
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B**«i)
vwlM
1-B«
Md
M,
V.
A
Q.
Qtcfm
Qtanm
I
RUN NUMBER
RUN DATE
RUN rate
MEASURED DATA
Meter Box Correction Factor
Avg Meter Orifice Pressure, in. HSO
Barometric Pressure, inches Kg
Sample Volume, ft3
Average Meter Temperature, *F
Stack Static Pressure, inches H3O
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/Z
Sample Run Duration, minutes
Nozzle Diameter, inches
CALCULATED DATA
Nozzle Area, ft2
Standard Meter Volume, ft1
Standard Meter Volume, m1
Average Sampling Rate, dscfm
Stack Pressure, Inches Hg
Moisture. % by volume
Moisture (at saturation), % by volume
Standard Water Vapor Volume, ft1
Dry Mole Fraction
Molecular Weight (d.b ), tvt-mo*e
Molecular Weight (w.b.), fefefnole
Stack Gaa Velocity, ft/a
Stack Area, ft2
Slack Gas Volumetric flow, ecfm
Stack Gee Volumetric flow, dscfm
Stack Gaa Volumetric flow, dscmm
Isoklnetlc Sampling Ratio, %
R-M29+1 R-M29+2 R-M29+3
8/27/97 S/28/97 S/29/97
-1000-~1i(» 1019-1427 0919-1403
1.016
1.24
29.80
52.232
101
-1.8
304
422.5
46
14.2
81.2
0.84
0.6972
87
0.256
0.000357
49.883
. 1.413
0.573
29.67
28.5
491.9
19.887
0.715
29.30
26.08
49.7
16.20
48.345
23,687
671
1097
1.016
0.298
29.60
64.379
102
-1.8
309
485.0
5.2
13.1
81.7
0.84
0.6977
200
0.194
0.000205
60.783
1.721
0.304
29.47
27.3
532.3
22.329
0.727
29.36
26.26
49.9
16.20
48,535
23,865
676
100.5
1.018
0.400
29.60
85.398
96
-1.8
289
403.9
4.0
15.2
80.3
0.84
0.7185
240
0.196
0.000210
81.522
2.308
0.340
29.47
18.9
395.0
19.012
0.811
29.25
27.12
49.9
16.20
48,550
27,325
774
96.1
Average
1 016
0-47
29.87
67.336
100
-1,80
300
437.1
4.6
14.2
81.2
084
0.7045
176
0215
0.000257
64.063
1.814
0.406
29.53
249
473.1
20.576
0.751
29.30
26.49
49.9
16.20
48.477
24,959
707
102.1
BBBBBBeieie*""***1*""1*1'
A-46
-------
BA£
LN
StefcftA
Pofttt No.
1
2
3
4
§
S
•?
a
9
10
11
12
DWancaFrom
1.0S
3.38
§,90
ass
12.S
17.S
322
if,S
41.2
44.1
46.7
49,0
A-47
-------
12 17 97 12:11 Ql9 1994 10234
PES RTF NC
013 / 0 15
Summary of Stack Gas Parameters and Test Results
Gary, North Carolina
US EPA Test Method 23 - PCDD / PCDF
Baghouse Outlet
Page 1 of 6
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
y Meter Box Correction Factor
AH Avg Meter Orifice Pressure, in. H2O
Pbv Barometric Pressure, inches Hg
Vm Sampled .TO, ft3
!„ Average Meier Temperature, "F
P.trtc Stack Static Pressure, inches H,O
T, Average Stack Temperature, "F
Vt Condensate Collected, ml
CO2 Carbon Dioxide content. % by volume
O2 Oxygen content, % by volume
N2 Nitrogen content, % by volume
Cp Pitot Tube Coefficient
ap1/z Average Square Root Dp, (in. HjO)"2
9 Sample Run Duration, minutes
Dn Nozzle Diameter, Inches
CALCULATED DATA
A^ Nozzle Area, ft2
V,,,,^ Standard Meter Volume, dscf
Vivtw Standard Meter Volume, dscm
P. Stack Pressure, inches Hg
BM Moisture, % by volume
BV^H,, Moisture (at saturation), % by volume
V^ Standard Water Vapor Volume, ft1
1-8*. Dry Mole Fraction
Md Molecular Weight (d.b.), Ib/to-mote
M, Molecular Weight (w.b.), Ib/to-mole
V. Stack Gas Velocity, ft/s
A Stack Area, ft*
Q. Stack Gas Volumetric flow, acfm
Q, Stack Gas Volumetric flow, dsdm
Qxorifn) Stack Gas Volumetric flow, dscmm
1 Isoktnetic Sampling Ratio, %
R-M23-O-1
0940-1519
0.982
3.04
29.80
226.829
111
-1.5
283
2083.3
4.0
15.0
81.0
0.84
1 0260
240
0.256
0.00036
206.781
5.855
29.69
32.2
359.8
98.061
0.678
29.24
25.62
72.8
11 23
49.075
23,450
664.0
1155
R-M23-O-2
8/28/97
0749-1229
0.982
2.69
29.60
208.171
97
-1.4
287
1620.9
4.9
13.6
815
0.84
1.0561
240
0256
0.00036
192.849
5.461
29.50
28.3
380.0
76.296
0.717
29.33
26.12
74.7
11.23
50,303
25,122
711.4
100.5
R-M23-O-3
a/29017
0809-1239
0.982
2.86
29.60
226.098
96
-1.3
266
10874
3.0
16.3
80.7
0.84
1 0760
240
0.251
0.00034
209.298
5.927
29.50
19.6
282.9
51 184
0804
29.13
26.94
74.0
11.23
49,832
28,612
810.2
99.6
Average
0.982
2.87
29 s?
220,:-5c
".:;
-1.40
279_
1597.2
4.0
15.0
81.1
0.84
1.0527
240
0254
0.00035
202.976
5.748
29.56
26.7
3409
75.180
0.733
2923
26.23
738
11.23
49,737
25,728
728.5
105.2
A-48
-------
12/17-97
12: 11
O19199410234
PES RTF NC
0 14 • 0 15
Summary of Stack Gas Parameters and Test Results
US EPA EMC Asphalt Concrete Emissions Testing
US EPA Test Method 29 • Multiple Metals
Baghouse Outlet
Page 1 of 4
RUN NUMBER
RUN DATE
RUN TIME
MEASURED DATA
y Meter Box Correction Factor
AH Avg Meter Orifice Pressure, in. H,O
PU*. Barometric Pressure, inches Hg
Vm Sample Volume, ft3
Tm Average Meter Temperature, *F
Pjtitie Stack Static Pressure, inches H2O
T, Average Stack Temperature, *F
Vie Condensate Collected, ml
CO2 Carbon Dioxide content, % by volume
O2 Oxygen content, % by volume
N2 Nitrogen content % by volume
Cp Pitot Tube Coefficient
Ap"2 Average Square Root Ap, (in. H2O)1/Z
9 Sample Run Duration, minutes
Dn Nozzle Diameter, inches
CALCULATED DATA
An Nozzle Area, ft2
Vm(iw) a Standard Meter Volume, ft3
Vm(sW) em Standard Meter Volume, mj
Qm Average Sampling Rat*, dscfm
P, Stack Pressure, inches Hg
BW, Moisture, % by volume
BW*W) Moisture (at saturation), % by volume
V^M Standard Water Vapor Volume, ft3
1-B*. Dry Mole Fraction
Md Molecular Weight (d.b. ), b/Rrmole
M, Molecular Weight (w.b.), fc/fcfnole
V, Stack Gas Velocity, ft/s
A Stack Area, ft2
Q, Stack Gas Volumetric flow, acfm
Q, a^ Stack Gas Volumetric flow, dscfm
Q, cmm Stack Gas Volumetric flow, dscmm
1 Isokinet'c Sampling Ratio. %
R-M29-O-1
«/27/97
0940-1518
0.965
2.96
29.80
237.264
109
-0.42
289
1632.0
4.0
15.0
81.0
084
1.0773
240
0.252
0.000346
213.024
6.032
0.888
29.77
26.5
393.7
76.818
0.735
2924
2626
75.7
11.23
51,035
26,285
744
109.5
R-M29-O-2
S/24/97
0746-1339
0965
2.14
29.60
200.329
97
-0.4
292
1484.6
49
13.6
815
0.84
10386
240
0.252
0.000346
182.236
5.160
0.759
29.57
27.7
411.7
69.880
0.723
2933
26.19
73.5
11.23
49,516
24,833
703
99.2
R-M29-O-3
4/2*97
0809-1239
0965
2.80
29.60
227.318
100
-0.42
274
1147.1
3.0
16.3
80.7
0.84
1 .0852
240
0.252
0.000346
205.914
5.831
0.858
29.57
20.8
310.4
53.994
0.792
29.13
26.82
75.0
11.23
50,521
28,440
805
97.8
Average
0.965
263
29.67
221.636
102
-0.41
285
1421.2
40
150
81.1
0 84
1.0670
240
0252
0.000346
200.391
5.674
0835
2964
250
371 9
66897
0.750
2923
26.42
747
11 23
50,357
26,520
751
102.2
A-49
-------
PES IIP VC
c
c
c
c
3
c
c
r M""
t 9
.......
r
' • . *
,
<*l •« i »
...-..,
__„,,.
'"1
.__..„„„
41
v-
,v£
•A
Section B
1
i
3
4
tnrtda
4,13
12.4
20.S
A-50
-------
APPENDIX B
FTIR DATA
-------
-------
B-1FTIR RESULTS
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.
Spiked samples are printed in bold type. Some samples were spiked with ethylene during Runs 1
and 3 and with toluene during Run 2. Additionally, some samples during each run were spiked
with 3.89 SF6. The SF6-spiked samples were analyzed to determine the spike dilution ratio for
each corresponding set of analyte-spiked samples. The field test documentation identifies the file
names with the spiked analyte and the spike flow rate.
Some results measured during process down times are shown in the tables, but these results were
not included in the run averages. Results from spiked samples are included in the run averages
and the dilution from the spike gas has been accounted for.
The results are reported as ppm concentrations with estimated uncertainties, also in ppm,
indicated by the symbol "A" in the column heading.
All of the FTIR results are presented graphically following Table B-4.
B-3
-------
B-4
-------
TABLE B-l. FTIR RESULT OF WET SAMPLES FROM THE BAGHOUSE INLET AT PLANT "B"
Date
8/27/97
Run 1
Time
9:52
9:53
9:55
9:57
9:58
10:00
10:02
11:04
11:10
11:19
11:27
12:20
12:22
12:23
12:25
12:26
12:29
12:31
12:32
12:34
12:36
12:37
12:39
12:41
12:42
12:45
12:47
14:48
14:49
14:52
14:54
14:55
14:57
14:59
15:00
15:02
15:04
15:05
File Name
18270001
18270002
18270003
18270004
18270005
18270006
18270007
REINS103
REINS104
REINS105
REINS106
18270030
18270031
18270032
18270033
18270034
18270035
18270036
18270037
18270038
18270039
18270040
18270041
18270042
18270043
18270044
18270045
18270098
18270099
18270100
18270101
18270102
18270103
18270104
18270105
18270106
18270107
18270108
Toll
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ene
A
13.6
14.2
14.5
14.6
14.8
14.7
14.7
7.1
7.1
6.9
6.6
10.7
11.5
11.7
11.6
11.8
11.9
11.9
11.8
11.7
11.5
11.5
11.4
11.3
11.3
11.7
11.7
7.6
7.5
7.4
7.5
7.5
7.5
7.4
7.3
7.3
7.2
7.3
Hex
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ane
A
68.9
72.0
73.6
74.1
74.9
74.5
74.5
36.0
36.1
34.7
33.4
54.3
58.2
59.1
59.0
59.9
60.1
60.1
59.9
59.0
58.4
58.1
57.6
57.1
57.1
59.2
59.3
38.6
38.0
37.7
38.0
38.0
37.8
37.3
37.1
36.7
36.7
36.7
Ethy
ppm
8.3
8.9
10.1
10.4
10.6
10.5
10.5
23.2
23J
3.5
3.5
6.1
7.3
7.6
7.7
8.0
8.1
8.0
7.9
7.7
7.6
7.5
7.3
7.1
7.2
7.9
7.9
19.2
18.9
18.6
18.5
18.4
18.7
18.9
18.9
19.1
19.4
19.5
lene
A
4.0
4.8
8.9
8.9
8.9
8.9
8.9
1.8
1.8
1.9
1.9
2.8
3.2
3.3
3.3
3.9
3.6
3.6
3.5
3.4
3.3
3.2
3.2
3.1
3.2
4.2
3.6
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.9
1.9
1.9
S
ppm
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.875
0.880
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
o.ooo
0.000
0.000
0.000
0.000
F6
A
0.113
0.137
0.252
0.251
0.251
0.251
0.251
0.050
0.050
0.048
0.047
0.077
0.089
0.094
0.094
0.110
0.102
0.102
0.098
0.096
0.092
0.091
0.090
0.089
0.091
0.118
0.102
0.056
0.055
0.054
0.055
0.055
0.054
0.054
0.054
0.053
0.053
0.053
Met)
ppm
11.8
12.3
12.4
12.6
12.8
12.7
12.7
6.0
6.0
63
6.1
9.1
9.7
9.7
9.7
9.8
9.8
9.9
9.8
9.7
9.6
9.5
9.3
9.4
9.5
9.7
9.7
12.1
12.0
11.8
11.8
11.9
11.9
11.9
11.9
, 11.9
12.0
12.1
lane
A
4.2
4.3
4.4
4.5
4.5
4.5
4.5
2.2
2.2
2.1
2.0
3.3
3.5
3.6
3.5
3.6
3.6
3.6
3.6
3.6
3.5
3.5
3.5
3.4
3.4
3.6
3.6
2.3
2.3
2.3
2.3
2.3
2.3
2.2
2.2
2.2
2.2
2.2
Sulfur I
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
20.6
20.6
21.2
22.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
16.5
16.6
16.8
16.7
16.8
17.4
17.4
17.7
18.1
18.3
18.7
Dioxide
A
19.7
23.8
43.9
43.7
43.7
43.8
43.8
8.7
8.7
8.5
8.2
13.5
15.6
16.4
16.4
19.3
17.8
17.9
17.2
16.7
16.1
15.8
15.6
15.5
15.8
20.6
17.8
9.7
9.6
9.5
9.5
9.6
9.4
9.4
9.3
9.2
9.2
9.2
Carbon \
ppm
36.4
0.0
0.0
0.0
0.0
0.0
43.0
22J
22.5
29.8
25.2
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
291.8
291.4
291.2
289.3
288.6
290.8
292.8
292.9
295.2
297.8
299.0
lonoxide
A
33.5
34.7
35.0
35.3
35.6
35.5
35.6
18.7
18.7
18.2
17.5
26.7
28.1
28.5
28.5
28.7
28.9
28.8
28.7
28.3
28.1
28.1
27.9
27.6
27.5
28.3
28.4
24.9
24.6
24.5
24.6
24.6
24.5
24.3
24.3
24.2
24.2
24.3
Forma)
ppm
0.0
0.0
0.0
0.0
do
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
4.7
4.6
4.6
4.5
4.4
4.6
4.8
4.9
5.1
5.3
5.4
dehyde
A
6.1
6.4
6.6
6.6
6.7
6.6
6.6
3.2
3.2
3.1
3.0
4.8
5.2
5.3
5.3
5.3
5.4
5.4
5.3
5.3
5.2
5.2
5.1
5.1
5.1
5.3
5.3
3.4
3.3
3.3
3.3
3.3
3.3
3.3
3.2
3.2
3.2
3.2
-------
TABLE B-l. Continued, Plant "B" Wet Inlet Results
Date
8/27/97
Run 1
Time
15:08
15:10
15:11
15:13
15:15
15:16
15:18
File Name
18270109
18270110
18270111
18270112
18270113
18270114
18270115
Average — >
Toll
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
icne
A
7.2
7.1
7.1
6.9
6.9
6.8
6.8
Hex
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ane
A
36.3
36.2
35.9
35.1
34.7
34.2
34.2
Ethy
ppm
19.7
19.9
20.2
20.9
20.8
20.8
20.3
12.6
lene
A
1.9
1.9
1.9
1.9
1.8
1.8
1.8
Si
ppm
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
"6
A
0.052
0.052
0.052
0.051
0.051
0.050
0.050
0.096
Metl
ppm
12.2
12.3
12.4
12.6
12.4
12.3
12.2
11.2
iane
A
2.2
2.2
2.2
2.1
2.1
2.1
2.1
Sulfur 1
ppm
19.2
19.5
20.3
21.3
22.1
22.6
22.8
10.9
Dioxide
A
9.1
9.1
9.0
8.9
8.8
8.6
8.7
Carbon \
ppm
301.5
302.8
305.1
310.4
311.0
312.3
309.6
125.1
fonoxide
A
24.1
24.1
24.0
23.8
23.7
23.4
23.4
Formal
ppm
5.7
5.8
6.2
6.8
6.9
7.1 .
7.0
2.2
dehyde
A
3.2
3.2
3.1
3.1
3.0
3.0
3.0
Date
8/28/97
Run 2
Time
8:18
8:24
8:34
8:41
9:23
9:24
9:26
9:28
9:29
9:32
9:34
9:35
9:37
9:39
9:40
9:42
9:44
9:45
13:18
13:20
13:21
13:23
13:25
13:26
13:28
13:29
13:32
File Name
REINS201
REINS202
REINS203
REINS204
18280001
18280002
18280003
18280004
18280005
18280006
18280007
18280008
18280009
18280010
18280011
18280012
18280013
18280014
18280115
18280116
18280117
18280118
18280119
18280120
18280121
18280122
18280123
Toll
ppm
43.6
43.9
0.0
0.0
0.0
15.2
16.1
15.6
16.5
17.0
16.8
17.1
16.9
17.2
16.9
16.2
16.8
17.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ene
A
6.9
7.6
10.4
10.8
10.9
8.2
8.4
8.4
8.6
8.7
8.7
8.7
8.8
8.8
8.7
8.7
8.7
8.8
9.4
9.2
9.2
9.2
9.2
9.3
9.4
9.4
9.5
Hex
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ane
A
49.9
553
52.6
54.9
55.1
59.3
61.1
60.8
62.3
63.1
62.9
63.1
63.8
63.6
63.3
62.8
63.3
64.1
47.6
46.7
46.6
46.4
46.4
47.0
47.7
47.8
48.1
Ethy
ppm
4.0
4.6
5.9
6.1
7.2
7.4
7.9
7.9
8.6
8.9
8.7
8.7
9.0
8.8
8.9
8.7
9.0
10.3
7.3
7.0
6.9
6.8
6.9
7.1
7.2
7.3
7.4
lene
A
2.5
2.7
2.9
3.0
2.9
3.3
3.6
3.5
6.4
5.3
4.0
4.0
5.5
4.0
4.5
4.2
6.8
9.0
2.7
2.7
2.6
2.6
2.6
2.7
2.7
2.7
2.8
SI
ppm
0.000
0.000
0.868
0.850
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
R6
A
0.068
0.077
0.072
0.077
0.080
0.093
0.101
0.099
0.180
0.151
0.114
0.112
0.154
0.113
0.127
0.119
0.192
0.253
0.075
0.073
0.071
0.071
0.070
0.073
0.073
0.074
0.077
Metl
ppm
8.8
9.8
8.7
9.1
10.1
10.7
11.1
10.9
11.1
11.2
11.1
11.0
11.2
11.1
11.1
11.2
11.2
11.4
8.2
8.1
8.1
8.1
8.1
8.2
8.3
8.2
8.2
iane
A
3.0
33
3.2
3.3
3.3
3.6
3.7
3.7
3.7
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.9
2.9
2.8
2.8
2.8
2.8
2.8
2.9
2.9
2.9
Sulfur 1
ppm
15.1
0.0
17.2
15.9
20.3
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
23.0
24.0
24.2
24.9
24.7
24.2
23.5
23.2
23.4
Dioxide
A
11.9
13.5
12.6
13.4
13.9
16.1
17.5
17.3
31.4
26.3
19.8
19.5
26.9
19.7
22.1
20.7
33.5
44.1
13.0
12.7
12.4
12.4
12.3
12.7
12.7
12.9
13.4
Carbon N
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
32.1
31.0
29.3
28.3
32.4
40.6
43.0
39.4
42.5
Monoxide
A
25.0
27.0
26.1
26.8
27.3
28.8
29.4
29.2
29.7
29.9
29.9
29.9
30.2
30.1
29.9
29.6
29.8
30.2
23.7
23.3
23.1
23.0
23.1
23.4
23.7
23.7
23.8
Formal
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
00
if.U
0.0
0.0
0.0
0.0
0.0
0.0
0.0
dehyde
A
4.4
4.9
4.7
4.9
4.9
5.3
5.4
5.4
5.6
5.6
. 5.6
5.6
5.7
5.7
5.6
5.6
5.6
5.7
4.2
4.2
4.1
4.1
4.1
4.2
4.3
4.3
4.3
DO
ON
-------
TABLE B-l. Continued, Plant "B" Wet Inlet Results
Date
8/28/97
Run 2
Time
13:34
13:35
13:37
13:39
13:40
13:42
13:44
13:45
File Name
18280124
18280125
18280126
18280127
18280128
18280129
18280130
18280131
Average — >
Toll
pptn
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
6.9
ene
A
9.2
9.1
9.2
9.4
9.5
9.6
9.7
9.8
Hex
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ane
A
46.7
46.3
46.7
47.6
48.2
48.6
49.3
49.4
Ethy
ppm
7.1
7.1
7.2
7.4
7.5
7.7
7.9
7.9
8.0
lene
A
2.6
2.6
2.7
2.7
2.8
2.8
3.0
2.9
Si
ppm
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
?6
A
0.072
0.071
0.072
0.074
0.076
0.076
0.082
0.079
0.101
Met!
ppm
8.0
8.0
8.1
8.1
8.2
8.2
8.3
8.4
10.2
iane
A
2.8
2.8
2.8
2.9
2.9
2.9
3.0
3.0
Sulfar I
ppm
25.0
25.4
25.1
23.3
22.2
21.2
20.7
19.9
14.4
Dioxide
A
12.5
12.3
12.6
12.8
13.2
13.3
14.4
13.7
Carbon N
ppm
43.9
44.2
39.7
38.7
43.2
39.8
37.0
38.2
18.4
lonoxide
A
23.4
23.1
23.2
23.5
23.7
23.9
24.1
24.2
Formal
ppm
0.0
0.0
0.0
0.0
0.0
0.0 .
0.0
0.0
0.0
dehyde
A
4.2
4.1
4.2
4.2
4.3
4.3
4.4
4.4
Date
8/29/97
Run 3
Time
7:59
8:07
8:15
8:28
8:34
8:40
9:27
9:33
9:34
9:36
9:38
9:39
9:41
9:43
9:44
9:46
9:49
9:50
9:52
9:54
9:55
9:57
9:59
10:56
10:58
10:59
File Name
REINS301
REINS302
REINS303
REINS304
REINS305
REINS306
REINU307
18290001
18290002
18290003
18290004
18290005
18290006
18290007
18290008
18290009
18290010
18290011
18290012
18290013
18290014
18290015
18290016
18290039
18290040
18290041
Toll
ppm
0.0
5.8
0.0
15.7
7.8
7.9
14.9
15.5
15.6
15.8
15.6
15.6
15.6
15.6
15.7
15.7
15.5
15.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ene
A
5.5
3.9
5.6
3.0
2.9
2.9
4.6
4.7
4.8
4.8
4.8
4.8
4.7
4.7
4.7
4.6
4.6
4.6
6.5
6.5
6.6
7.2
7.6
10.3
10.2
10.1
Hex
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
ane
A
27.9
28.2
28.6
21.0
20.8
20.9
32.8
34.1
34.5
34.3
34.4
34.3
34.1
33.8
33.6
33.4
33.4
33.2
33.1
33.1
33.6
36.4
38.5
52.2
51.7
51.3
Ethy
ppm
3J
7.1
6.8
28.8
28.2
28.1
21.0
20.9
20.9
20.9
20.8
20.8
20.9
20.9
21.0
21.1
21.1
20.9
20.9
21.0
21.3
21.1
19.0
6.4
6.4
6.5
lene
A
1.6
1.6
1.6
1.1
1.1
1.1
1.7
.8
.8
.8
.8
.8
.8
.7
.7
.7
.7
.7
.7
.7
.7
.9
2.0
2.7
2.7
2.7
s:
ppm
0.762
0.791
0.787
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
36
A
0.040
0.040
0.041
0.031
0.030
0.030
0.046
0.048
0.048
0.048
0.048
0.048
0.048
0.048
0.047
0.047
0.047
0.047
0.047
0.047
0.048
0.051
0.054
0.077
0.077
0.075
Met]
ppm
5.9
7.0
6.9
8.6
7.5
7.4
13.3
13.5
13.6
13.6
13.5
13.5
13.5
13.5
13.5
13.5
13.5
13.4
13.1
13.1
13.8
14.1
13.3
8.7
8.6
8.5
iane
A
1.6
1.7
1.7
1J
1.2
U
2.0
2.
2.
2.
2.
2.
2.
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.2
2.3
3.1
3.1
3.1
Sulrur I
ppm
12.6
9.7
8.1
19.8
18.0
17J
28.1
27.5
27.1
27.0
26.7
26.8
27.0
26.9
27.2
27.4
27.4
27.6
27.6
27.9
27.3
25.2
22.8
0.0
0.0
0.0
Dioxide
A
6.9
7.0
7.1
5J
5J
5J
8.1
8.4
8.5
8.4
8.4
8.4
8.4
8.3
8.3
8.2
8.2
8.2
8.2
8.2
8.3
8.9
9.4
13.5
13.4
13.1
Carbon N
ppm
71.5
147.8
137.2
187J
172.8
170.5
273.3
270.9
270.6
270.7
269.9
270.1
270.6
270.5
272.0
272.8
273.6
273.0
273.2
273.1
277.5
284.5
274.1
0.0
0.0
0,0
lonoxide
A
15.2
16.9
16.8
14.5
14.0
14.0
22.1
23.0
23.2
23.1
23.1
23.1
23.0
22.9
22.8
22.7
22.7
22.6
22.6
22.6
23.0
24.5
25.2
25.7
25.4
25.3
Formal
ppm
0.0
2.9
0.0
5.7
5.5
5.3
10.4
10.2
10.2
10.3
10.2
10.2
10.3
10.3
10.5
10.5
10.6
10.5
9.3
9.3
9.1
8.1
6.2
0.0
0.0
0.0
dehyde
A
2.5
2.5
2.5
1.9
1.8
1.8
2.9
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
2.9
2.9
2.9
2.9
2.9
2.9
3.2
3.4
4.7
4.6
4.6
-------
TABLE B-l. Continued, Plant "B" Wet Inlet Results
Date
8/29/97
Run 3
Time
11:01
11:03
11:04
1:06
1:09
1:10
1:12
1:14
1:15
1:17
1:19
11:20
14:07
14:09
14:11
14:12
14:14
File Name
18290042
18290043
18290044
18290045
18290046
18290047
18290048
18290049
18290050
18290051
18290052
18290053
18290132
18290133
18290134
18290135
18290136
Average — >
Toluene
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
12.1
12.1
12.0
11.9
11.6
6.6
A
10.0
9.8
9.7
9.7
9.6
9.6
9.6
9.6
9.5
9.6
9.7
9.6
4.3
4.3
4.3
4.3
4.2
Hexane
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
A
50.8
49.7
49.3
49.1
48.9
48.9
48.6
48.4
48.1
48.8
49.3
48.8
31.2
31.1
30.8
30.5
30.4
Ethylene
ppm
6.4
6.2
6.1
6.0
6.0
6.1
6.0
6.0
5.9
6.3
6.4
6.4
19.7
19.8
19.5
18.6
17.9
13.3
A
2.6
2.6
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.6
2.5
1.7
1.7
1.7
1.7
1.6
SF6
ppm
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
A
0.074
0.073
0.071
0.071
0.071
0.071
0.070
0.071
0.070
0.072
0.073
0.072
0.046
0.046
0.046
0.045
0.045
0.058
Methane
ppm
8.2
8.0
8.1
8.1
7.9
7.9
7.8
7.8
7.7
7.7
7.9
7.8
12.0
11.9
11.9
11.5
11.2
10.5
A
3.1
3.0
3.0
3.0
2.9
2.9
2.9
2.9
2.9
2.9
3.0
2.9
1.9
1.9
1.9
1.8
1.8
Sulfur Dioxide
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
27.0
27.5
28.3
29.3
29.8
16.0
A
12.9
12.6
12.4
12.4
12.3
12.3
12.2
12.3
12.1
12.5
12.7
12.5
8.1
8.0
8.0
7.9
7.9
Carbon Monoxide
ppm
0.0
26.3
26.5
25.6
0.0
0.0
25.4
0.0
0.0
0.0
0.0
0.0
282.6
282.7
280.4
272.4
267.3
163.5
A
25.2
24.8
24.7
24.5
24.3
24.4
24.3
24.4
24.0
24.2
24.5
24.3
21.0
21.0
20.7
20.4
20.3
Formaldehyde
ppm
0.0
0.0
0.0
0.0
0.0
0.0 .
0.0
0.0
0.0
0.0
0.0
0.0
9.2
9.3
9.2
8.8
8.4
5.3
A
4.5
4.4
4.4
4.4
4.4
4.4
4.3
4.3
4.3
4.3
4.4
4.3
2.8
2.7
2.7
2.7
2.7
03
I
oo
-------
TABLE B-l. Continued, Additonal hydrocarbon results in Wet Inlet Samples.
Date
8/27/97
Run 1
8/27/97
Run 1
Time
9:52
9:53
9:55
9:57
9:58
10:00
10:02
11:04
11:10
11:19
11:27
12:20
12:22
12:23
12:25
12:26
12:29
12:31
12:32
12:34
12:36
12:37
12:39
12:41
12:42
12:45
12:47
14:48
14:49
14:52
14:54
14:55
14:57
14:59
15:00
15:02
15:04
15:05
15:08
15:10
File Name
18270001
18270002
18270003
18270004
18270005
18270006
18270007
REINS103
REINS104
REINS105
REINS106
18270030
18270031
18270032
18270033
18270034
18270035
18270036
18270037
18270038
18270039
18270040
18270041
18270042
18270043
18270044
18270045
18270098
18270099
18270100
18270101
18270102
18270103
18270104
18270105
18270106
18270107
18270108
18270109
18270110
Hep
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
9.9
9.5
9.2
8.6
7.8
8.2
8.5
8.8
8.8
8.4
7.9
8.1
8.8
9.3
8.6
7.8
13.2
12.0
11.3
10.9
10.8
11.1
11.4
11.3
11.3
11.3
11.2
11.4
11.7
tane
A
29.8
31.1
31.8
32.0
32.4
32.2
32.2
15.5
15.6
15.0
14.4
0.8
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
0.6
1-Per
ppm
21.2
21.2
20.9
22.0
23.1
23.8
23.9
11.4
10.7
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
itene
A
2.8
2.9
3.0
3.0
3.0
3.0
3.0
1.5
1.5
17.4
16.8
5.7
6.1
6.2
6.1
6.2
6.3
6.3
6.2
6.1
6.1
6.1
6.0
5.9
5.9
6.2
6.2
5.7
5.6
5.6
5.6
5.6
5.6
5.5
5.5
5.4
5.4
5.4
5.4
5.4
2-Methyl
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
-2-butene
A
21.8
22.8
23.3
23.5
23.7
23.6
23.6
11.4
11.4
11.0
10.6
17.2
18.4
18.7
18.7
19.0
19.0
19.0
19.0
18.7
18.5
18.4
18.3
18.1
18.1
18.7
18.8
12.2
12.0
11.9
12.0
12.1
12.0
11.8
11.8
11.6
11.6
11.6
11.5
11.5
B-9
-------
TABLE B-l. Continued, Additional hydrocarbon results in Wet Inlet Samples.
Date
Time
15:11
15:13
15:15
15:16
15:18
File Name
18270111
18270112
18270113
18270114
18270115
Average — >
Hep
ppm
11.9
12.3
12.4
12.6
12.5
7.8
tane
A
0.6
0.5
0.5
0.5
0.5
1-Per
ppm
0.0
0.0
0.0
0.0
0.0
4.3
itene
A
5.3
5.2
5.1
5.8
5.8
2-Methyl
ppm
0.0
0.0
0.0
0.0
0.0
0.0
•2-butene
A
11.4
11.1
11.0
3.3
3.3
Date
8/28/97
Run 2
Time
8:18
8:24
8:34
8:41
9:23
9:24
9:26
9:28
9:29
9:32
9:34
9:35
9:37
9:39
9:40
9:42
9:44
9:45
13:18
13:20
13:21
13:23
13:25
13:26
13:28
13:29
13:32
13:34
13:35
13:37
13:39
File Name
REINS201
REINS202
REINS203
REINS204
18280001
18280002
18280003
18280004
18280005
18280006
18280007
18280008
18280009
18280010
18280011
18280012
18280013
18280014
18280115
18280116
18280117
18280118
18280119
18280120
18280121
18280122
18280123
18280124
18280125
18280126
18280127
Hep
ppm
10.1
10.0
10.4
8.7
10.8
11.0
11.6
9.8
9.3
9.8
10.4
10.7
10.7
11.5
11.1
10.9
11.4
11.8
7.1
7.8
8.2
8.8
9.3
9.2
9.2
9.0
8.7
9.0
9.8
10.2
10.2
tane
A
0.8
0.9
0.8
0.8
0.8
0.9
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
1-Pei
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
nene
A
5.2
5.8
5.S
5.7
5.7
6.2
6.4
6.3
6.5
6.6
6.5
6.6
6.7
6.6
6.6
6.5
6.6
6.7
5.0
4.9
4.9
4.8
6.8
4.9
5.0
5.0
5.0
6.9
6.8
6.9
7.0
2-Methyl
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
•2-butene
A
15.8
17.5
16.7
17.4
17.5
18.8
19.3
19.3
19.7
20.0
19.9
20.0
20.2
20.2
20.1
19.9
20.1
20.3
15.1
14.8
14.7
14.7
14.7
14.9
15.1
15.1
15.2
14.8
14.7
14.8
15.1
B-10
-------
TABLE B-l. Continued, Additional hydrocarbon results in Wet Inlet Samples.
Date
8/28/97
Run 2
Time
13:40
13:42
13:44
13:45
File Name
18280128
18280129
18280130
18280131
Average — >
Heptane
ppm
9.7
9.1
8.6
9.0
10.7
A
0.7
0.8
0.8
0.8
1-Pentene
ppm
0.0
0.0
0.0
0.0
0.0
A
7.1
7.2
5.1
7.3
2-Methyl-2-butene
ppm
0.0
0.0
0.0
0.0
0.0
A
15.3
15.4
15.6
15.7
Date
8/29/97
Run 3
Time
7:59
8:07
8:15
8:28
8:34
8:40
9:27
9:33
9:34
9:36
9:38
9:39
9:41
9:43
9:44
9:46
9:49
9:50
9:52
9:54
9:55
9:57
9:59
10:56
10:58
10:59
11:01
11:03
11:04
11:06
11:09
11:10
11:12
11:14
11:15
File Name
REINS301
REINS302
REINS303
REINS304
REINS305
REINS306
REINU307
18290001
18290002
18290003
18290004
18290005
18290006
18290007
18290008
18290009
18290010
18290011
18290012
18290013
18290014
18290015
18290016
18290039
18290040
18290041
18290042
18290043
18290044
18290045
18290046
18290047
18290048
18290049
18290050
Hep
ppm
0.0
0.0
0.0
0.0
6.1
63
14.7
14.9
15.0
15.2
15.2
15.3
15.4
15.5
15.7
15.9
15.9
15.9
15.0
15.1
16.1
13.2
10.1
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
tane
A
12.0
12.2
12.4
9.1
0.3
0.3
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
0.5
1.0
1.0
0.5
0.6
0.6
22.6
22.3
22.1
21.9
21.5
21.3
21.2
21.1
21.1
21.0
20.9
20.8
1-Per
ppm
0.0
3.8
2.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
itene
A
14.0
1.2
1.1
10.5
10.4
10.5
3.4
3.6
3.6
3.6
3.6
3.6
3.6
3.5
3.5
3.9
3.9
3.8
3.8
3.8
3.5
3.8
4.0
2.1
2.1
2.1
2.1
2.0
2.0
2.0
2.0
2.0
2.0
2.0
1.9
2-Methyl
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
4.4
4.3
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
2-butene
A
8.8
8.9
9.1
6.6
6.6
6.6
10.4
10.8
10.9
10.9
10.9
10.9
10.8
10.7
10.6
3.4
3.4
3.4
2.8
2.8
10.7
11.5
12.2
16.5
16.4
16.2
16.1
15.7
15.6
15.6
15.5
15.5
15.4
15.3
15.2
B-ll
-------
TABLE B-1. Continued, Additional hydrocarbon results in Wet Inlet Samples.
Date
8/29/97
Run 3
Time
11:17
11:19
11:20
14:07
14:09
14:11
14:12
14:14
File Name
18290051
18290052
18290053
18290132
18290133
18290134
18290135
18290136
Average — >
Hep
ppm
0.0
0.0
0.0
4.7
4.6
4.8
5.1
5.1
6.7
tane
A
21.1
21.3
21.1
1.3
1.2
1.2
1.2
2.7
1-Pei
ppm
0.0
0.0
0.0
5.1
5.1
4.9
4.5
4.2
0.7
uene
A
2.0
2.0
2.0
3.3
3.2
3.2
3.2
14.6
2-Methyl
ppm
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.2
-2-butene
A
15.5
15.6
15.5
9.9
9.9
9.8
9.7
6.7
B-12
-------
TABLE B-2. FTIR RESULTS FROM WET SAMPLES AT THE PLANT "B" BAGHOUSE OUTLET
Date
8/27/97
Run 1
Time
10:20
10:25
10:34
10:40
10:45
11:45
11:46
11:48
11:50
11:51
11:53
11:54
11:57
11:59
12:00
12:02
12:04
12:05
12:07
12:09
12:10
12:13
14:27
14:29
14:30
14:32
14:34
14:36
14:38
14:40
14:41
14:43
File Name
REOUS102
REODS103
REOUS104
REOUS105
REOUS106
18270011
18270012
18270013
18270014
18270015
18270016
18270017
18270018
18270019
18270020
18270021
18270022
18270023
18270024
18270025
18270026
18270027
18270088
18270089
18270090
18270091
18270092
18270093
18270094
18270095
18270096
18270097
Average — >
Toluene
ppm A
11.5
11J
11J
11J
10.9
8.8
5.4
6.8
9.9
11.1
11.4
11.4
11.5
11.5
11.5
11.4
11.6
11.6
11.6
11.4
11.3
11.4
10.2
10.1
8.9
7.6
7.2
7.2
7.6
7.5
7.4
7.4
Hexane
ppm A
58.4
57.0
57.0
57.4
55.1
44.5
27.2
34.6
50.3
56.2
57.5
57.6
58.3
58.0
58.0
57.7
58.8
58.7
58.5
57.9
57.0
57.6
51.7
51.2
45.0
38.6
36.7
36.7
38.3
37.9
37.5
37.3
Ethylene
ppm A
6.9 3.2
6.8 3.1
23.2 2.8
23.5 2.8
23.0 2.7
4.7 2.2
2.0 1.4
4.7 1.7
6.3 2.5
6.4 2.9
6.6 3.0
6.8 3.1
7.0 3.1
6.9 3.1
6.9 3.0
6.9 3.0
7.2 3.1
7.3 3.2
7.3 3.1
7.1 3.1
6.8 3.0
7.0 3.0
7.6 2.9
7.5 2.8
11.9 2.3
17.9 2.0
19.0 1.9
19.2 1.9
18.8 2.0
19.1 2.0
19.3 2.0
19.2 2.0
10.7
SF6
ppm A
0.756 0.081
0.760 0.079
0.079
0.080
0.077
0.061
0.039
0.047
0.069
0.082
0.086
0.086
0.087
0.087
0.086
0.085
0.088
0.089
0.088
0.087
0.084
0.086
0.082
0.079
0.065
0.055
0.053
0.053
0.055
0.055
0.054
0.054
0.072
Methane
ppm A
10.5 3.5
10.2 3.4
9.6 3.4
9.6 3.5
93 3.3
9.0 2.7
6.2 1.6
7.7 2.0
9.0 3.0
9.6 3.4
9.8 3.5
9.8 3.5
9.8 3.5
9.7 3.5
9.7 3.5
9.7 3.5
9.8 3.5
9.8 3.5
9.7 3.5
9.4 3.5
9.3 3.5
9.4 3.5
8.4 3.1
8.3 3.1
9.9 2.7
11.7 2.3
12.0 2.2
12.2 2.2
12.2 2.3
12.3 2.3
12.4 2.3
12.3 2.2
11.4
SO2
ppm A
16.2 14.2
15J 13.7
13.9
14.0
13.4
14.9 10.6
15.7 6.8
18.0 8.3
15.0 12.1
14.3
15.0
15.0
15.1
15.1
15.0
14.8
15.4
15.6
15.3
15.1
14.7
14.9
14.3
13.8
11.4
13.4 9.6
14.0 9.2
13.5 9.2
13.4 9.6
15.5 9.5
17.8 9.4
18.9 9.3
6.5
CO
ppm A
70.0 29.5
45.5 28.5
30.6 28.2
29.2 28.3
27.9 27.3
36.6 23.0
32.8 14.5
108.8 19.3
101.4 26.5
85.5 28.4
72.7 28.9
61.5 28.7
56.5 29.0
60.3 28.9
60.3 28.9
58.2 28.7
57.1 29.0
57.7 29.0
58.8 28.9
60.7 28.7
52.0 28.2
52.2 28.5
1 14.8 26.7
140.7 26.8
197.2 25.4
256.1 24.0
267.9 23.6
271.4 23.6
278.4 24.5
288.0 24.6
291.8 24.5
292.2 24.4
125.6
Formaldehyde
ppm A
5.2
5.1
5.1
5.1
4.9
1
4.0
2.4
3.1
4.5
5.0
5.1
5.1
5.2
5.2
5.2
5.1
5.2
5.2
5.2
5.2
5.1
5.1
4.6
4.6
4.0.
3.4
5.0 3.2
5.2 3.2
4.5 3.3
4.8 3.3
5.0 3.3
5.1 3.3
1.0
GO
-------
TABLE B-2. Continued. FTIR RESULTS OF WET OUTLET SAMPLES
Date
8/28/97
Run 2
Time
7:32
7:40
7:50
8:00
8:05
9:54
9:55
9:57
9:59
10:00
10:02
10:05
10:06
10:08
10:10
10:11
10:13
10:15
10:16
10:18
10:21
10:22
10:24
10:26
10:27
12:41
12:44
12:45
12:47
12:49
12:50
12:52
12:54
12:55
12:57
13:00
13:01
13:03
13:05
13:06
13:08
13:10
13:53
13:54
File Name
REOUS201
REOUS202
REOUS203
REOUS204
REOUS205
18280016
18280017
18280018
18280019
18280020
18280021
18280022
18280023
18280024
18280025
18280026
18280027
18280028
18280029
18280030
18280031
18280032
18280033
18280034
18280035
18280096
18280097
18280098
18280099
18280100
18280101
18280102
18280103
18280104
18280105
18280106
18280107
18280108
18280109
18280110
18280111
18280112
18280134
18280135
Toluene
ppm A
7.6
7.7
10.1
42.9 7.4
43.4 8.0
12.0
11.8
11.8
11.7
11.6
11.7
11.9
11.9
11.8
11.8
11.7
11.7
11.7
11.7
11.7
11.7
16.1 8.2
16.0 8.3
11.8
11.7
8.2
8.5
8.5
8.7
8.8
8.7
8.7
8.7
8.8
9.0
8.8
8.8
8.7
8.8
8.9
9.0
9.2
9.0
8.9
Hexane
ppm A
38.7
39.1
51.3
53.5
58.1
60.8
59.7
59.6
59.3
58.7
59.1
60.3
60.5
59.9
59.7
59.4
59.2
59.3
59.5
59.4
59.5
59.9
60.2
59.5
59.1
41.8
42.9
43.2
43.9
44.4
44.1
43.9
44.1
44.8
45.4
44.7
44.4
44.1
44.7
45.0
45.7
46.6
45.6
45.0
Ethylene
ppm A
5.8 2.1
4J 2.1
5.8 2.8
5J 2.7
5.7 2.9
7.5 3.6
8.0 3.4
7.2 3.3
7.2 3.3
7.9 3.3
8.0 3.4
7.6 3.4
7.7 3.6
7.5 3.4
7.5 3.3
7.3 3.2
7.4 3.2
7.5 3.4
7.6 3.5
7.5 3.4
7.5 3.3
7.7 3.6
7.9 3.8
7.7 3.7
7.5 3.6
6.4 2.2
6.7 2.3
6.9 2.3
7.5 2.3
8.0 2.4
8.1 2.4
8.2 2.4
8.1 2.4
7.4 2.4
7.5 2.5
7.6 2.4
7.7 2.4
7.8 2.4
7.2 2.4
6.7 2.4
6.7 2.5
6.8 2.5
6.9 2.5
7.0 2.5
SF6
ppm A
0.835 0.053
0.704 0.053
0.822 0.070
0.074
0.082
0.098
0.093
0.092
0.093
0.090
0.093
0.096
0.102
0.096
0.094
0.091
0.091
0.095
0.099
0.097
0.094
0.100
0.106
0.104
0.101
0.060
0.062
0.063
0.064
0.065
0.064
0.065
0.064
0.065
0.067
0.066
0.066
0.065
0.066
0.066
0.067
0.069
0.068
0.068
Methane
ppm A
7.0 2J
8.3 23
8.7 3.1
9.6 3.2
10.4 3.5
11.1 3.7
10.8 3.6
10.8 3.6
10.7 3.6
10.6 3.5
10.6 3.6
10.8 3.6
10.8 3.6
10.7 3.6
10.4 3.6
10.4 3.6
10.3 3.6
10.5 3.6
10.6 3.6
10.5 3.6
10.2 3.6
10.2 3.6
10.2 3.6
10.3 3.6
10.2 3.6
7.5 2.5
7.8 2.6
7.9 2.6
8.3 2.6
8.5 2.7
8.5 2.7
8.6 2.7
8.5 2.7
8.2 2.7
8.3 2.7
8.2 2.7
8.3 2.7
8.2 2.7
8.1 2.7
7.9 2.7
7.9 2.8
7.9 2.8
7.8 2.7
7.8 2.7
S02
ppm A
24.2 9.2
22.1 93
20.5 12.2
14.0 12.9
14.2
38.5 17.2
20.3 16.2
16.1
16.2
17.9 15.7
17.7 16.2
16.7
17.8
16.7
16.4
15.9
15.9
16.6
17.3
16.9
16.4
17.5
18.5
18.1
17.6
23.0 10.5
22.9 10.9
23.0 10.9
20.9 11.2
19.9 11.3
20.1 11.2
20.6 11.3
20.2 11.2
19.5 11.3
18.3 11.7
18.5 11.6
18.6 11.5
19.0 11.3
20.0 11.6
21.0 11.5
20.8 11.7
21.2 12.0
21.5 11.8
21.8 11.8
CO
ppm A
78.0 20.8
33.1 20.0
46.5 26.1
36.6 26.8
30.8 28.4
29.0
28.6
28.5
28.5
28.3
28.4
28.9
28.9
28.7
28.6
28.5
28.4
28.4
28.5
28.5
28.6
28.7
28.6
28.5
28.4
94.3 22.2
97.0 22.7
96.8 22.9
117.3 23.4
126.7 23.8
134.3 23.8
137.8 23.8
134.3 23.8
109.3 23.6
105.2 23.7
112.9 23.6
116.7 23.6
119.7 23.5
90.0 23.2
66.5 23.0
55.3 23.1
32.9 23.2
38.3 22.7
38.0 22.5
Formaldehyde
ppm A
3.4
3.5
4.6
4.8
5.2
5.4
5.3
5.3
5.3
5.2
5.3
5.4
5.4
5.3
5.3
5.3
5.3
•5.3
5.3
5.3
5.3
5.3
5.4
5.3
5.3
3.7
3.8
3.8
3.9
4.0
3.9
3.9
3.9
4.0
4.0
4.0
4.0
3.9
4.0
4.0
4.1
4.1
4.1
4.0
-------
TABLE B-2. Continued. FTIR RESULTS OF WET OUTLET SAMPLES
Date
8/28/97
Run 2
Time
13:56
13:58
13:59
14:01
14:04
14:05
14:09
14:11
14:12
14:14
14:16
14:17
14:20
14:22
14:23
14:25
14:27
14:28
14:30
File Name
18280136
18280137
18280138
18280139
18280140
18280141
18280142
18280143
18280144
18280145
18280146
18280147
18280148
18280149
18280150
18280151
18280152
18280153
18280154
Average — >
Toluene
ppm A
7.5
5.5
4.4
3.4
3.0
2.4
8.8
9.2
9.7
9.7
9.1
9.0
9.0
9.1
9.2
9.3
9.2
9.3
9.3
0.6
Hexane
ppm A
37.7
28.0
22.3
17.4
15.4
12.0
44.8
46.4
48.9
49.3
46.0
45.7
45.5
46.0
46.4
47.2
46.8
46.9
47.1
Ethylene
ppm A
5.4 2.0
3.9 1.5
2.7 1.3
1.8 1.0
1.4 0.9
1.0 0.7
7.1 2.5
7.4 2.7
7.4 2.8
7.6 2.9
7.3 2.6
7.3 2.6
7.3 2.6
7.4 2.6
7.6 2.7
7.7 2.7
7.6 2.7
7.6 2.7
7.6 2.7
7.6
SF6
ppm A
0.055
0.042
0.035
0.028
0.025
0.020
0.068
0.073
0.077
0.079
0.072
0.070
0.071
0.071
0.073
0.075
0.074
0.073
0.074
0.075
Methane
ppm A
6.8 2.3
6.2 1.7
5.9 1.4
5.2 1.1
4.9 1.0
4.2 0.8
8.0 2.7
8.2 2.8
8.4 3.0
8.5 3.0
8.0 2.8
7.9 2.8
7.9 2.7
8.0 2.8
8.0 2.8
8.1 2.9
8.1 2.8
8.0 2.8
8.1 2.8
9.6
S02
ppm A
37.2 9.5
44.5 7.4
36.9 6.1
27.4 4.9
23.0 4.4
16.7 3.5
21.7 11.9
20.3 12.6
19.6 13.4
19.5 13.7
21.0 12.5
21.6 12.2
21.7 12.4
21.0 12.5
20.2 12.8
20.0 13.1
20.0 12.8
19.9 12.8
20.0 13.0
15.7
CO
ppm A
41.8 19.7
46.9 15.3
43.1 12.2
33.1 9.6
28.5 8.4
30.7 6.8
105.8 23.3
86.1 23.6
84.8 24.7
86.3 24.8
74.1 23.2
63.5 23.0
61.5 23.0
61.0 23.1
63.7 23.2
72.7 23.7
73.4 23.5
66.7 23.4
69.6 23.6
56.1
Formaldehyde
ppm A
3.4
2.5
2.0
1.6
1.4
1.1
. 4.0
4.1
4.4
4.4
4.1
4.1
4.1
4.1
4.1
4.2
4.2
4.2
4.2
Date
8/29/97
Run 3
Time
8:48
8:54
9:01
9:08
9:14
9:21
10:05
10:07
10:09
10:10
10:12
10:14
10:15
10:17
10:20
10:21
10:23
10:25
10:26
10:28
10:30
10:31
10:33
File Name
REOUS30I
REOLS302
REOLS303
REOLS304
REOLS305
REOLS306
18290018
18290019
18290020
18290021
18290022
18290023
18290024
18290025
18290026
18290027
18290028
18290029
18290030
18290031
18290032
18290033
18290034
Toluene
ppm A
12.7 4.1
13.0 4.2
13.2 4.0
12.9 4.0
12.7 4.1
12.5 4.0
8.0
7.9
7.8
7.5
7.3
7.3
7.4
7.4
7.9
8.9
9.7
10.2
10.1
10.1
10.0
10.1
10.2
Hexane
ppm A
29.4
30.2
28.8
29.2
29.5
29.1
40.6
40.1
39.5
37.9
37.2
37.2
37.2
37.5
40.0
44.9
49.1
51.4
51.4
51.3
50.9
51.1
51.6
Ethylene
ppm A
35.2 1.5
35.2 1.6
35.4 1.5
17.9 1.7
17.6 1.7
17.6 1.6
9.1 2.1
9.0 2.1
9.2 2.0
9.8 1.9
10.0 1.9
10.0 1.9
12.8 1.9
14.4 1.9
12.9 2.0
9.0 2.3
7.0 2.5
6.7 2.6
6.4 2.6
6.3 2.6
6.2 2.6
6.2 2.6
6.2 2.6
SF6
ppm A
0.042
0.043
0.041
0.784 0.042
0.798 0.042
0.797 0.042
0.057
0.056
0.055
0.053
0.053
0.052
0.052
0.053
0.056
0.062
0.069
0.073
0.074
0.074
0.074
0.074
0.075
Methane
ppm A
11.2 1.8
11.4 .8
11 J .7
11J .8
11.1 .8
11.1 .7
9.3 2.4
9.1 2.4
9.1 2.4
9.2 2.3
9.1 2.2
9.2 2.2
10.7 2.2
11.0 2.3
10.7 2.4
9.3 2.7
8.8 2.9
8.6 3.
8.5 3.
8.4 3.
8.3 ' 3.
8.3 3.
8.4 3.
S02
ppm A
23.5 7.3
23.7 7.5
24.7 7.2
24.5 7J
25.4 7J
26.4 7J
19.2 9.9
19.5 9.8
20.6 9.6
23.1 9.3
24.9 9.2
25.1 9.1
24.9 9.1
24.9 9.2
21.4 9.7
13.5 10.9
12.1
12.8
12.9 -
12.9
12.8
12.9
13.0
CO
ppm A
242.4 19.8
241.7 20.2
243.9 19.6
243.4 19.7
242.9 19.8
243.0 19.7
186.3 24.0
185.8 23.8
191.5 23.6
203.4 23.2
207.4 22.9
206.6 22.9
229.8 23.5
242.7 23.8
222.7 24.5
147.0 25.0
74.3 25.4
35.1 25.7
25.5
25.4
25.3
25.3
25.5
Formaldehyde
ppm A
8.8 2.6
8.6 2.7
8.9 2.5
8.6 2.6
8.4 2.6
8.4 2.6
3.6
3.6
3.5
3.4
3.3
3.3
3.3
3.5 3.3
3.5
4.0
4.4
4.6
4.6
4.6
4.5
4.6
4.6
-------
TABLE B-2. Continued. FTIR RESULTS OF WET OUTLET SAMPLES
Date
8/29/97
Run 3
8/29/97
Run 3
Time
10:36
10:37
10:39
10:40
10:45
12:47
12:49
12:50
12:52
12:54
12:55
12:57
13:00
13:01
13:03
13:05
13:06
13:08
13:10
13:11
13:13
13:16
13:29
13:32
13:33
13:35
13:37
13:38
13:40
13:42
13:43
13:45
13:48
13:49
13:51
13:53
13:54
13:56
13:58
13:59
File Name
18290035
18290036
18290037
18290038
REOUU307
18290095
18290096
18290097
18290098
18290099
18290100
18290101
18290102
18290103
18290104
18290105
18290106
18290107
18290108
18290109
18290110
18290111
18290112
18290113
18290114
18290115
18290116
18290117
18290118
18290119
18290120
18290121
18290122
18290123
18290124
18290125
18290126
18290127
18290128
18290129
Average — >
Toluene
ppm A
10.3
10.4
10.0
9.9
9.9
3.4
2.9
2.5
2.2
2.0
2.0
2.0
2.0
2.0
2.0
.9
.9
.9
.8
.6
.6
.6
12.4 4.6
11.8 4.4
11.8 4.4
11.9 4.4
11.7 4.3
11.9 4.3
11.9 4.3
11.8 4.4
11.7 4.4
11.9 4.4
12.1 4,3
12.1 4.4
12.0 4.4
12.0 4.4
11.8 4.4
11.9 4.4
12.4 4.3
12.9 4.2
7.5
Hexane
ppm A
52.2
52.6
50.5
50.1
50.2
17.4
14.5
12.8
11.3
10.3
10.1
10.0
10.3
10.1
9.9
9.7
9.5
9.4
9.0
8.3
7.9
7.9
32.7
31.6
31.8
31.8
31.1
30.7
30.9
31.4
31.5
31.4
31.2
31.5
31.3
31.4
31.3
31.4
31.0
30.5
Ethylene
ppm A
6.5 2.7
6.4 2.7
6.2 2.6
6.2 2.6
6.3 2.6
7.2 1.1
4.8 0.9
3.7 0.8
2.7 0.7
2.2 0.7
2.1 0.7
2.0 0.7
2.1 0.7
2.1 0.7
.9 0.6
.9 0.6
.7 0.6
.8 0.6
.6 0.6
.3 0.6
.2 0.5
.2 0.5
14.6 1.8
14.3 1.7
14.7 1.7
14.8 1.7
15.0 1.7
15.1 1.7
14.9 1.7
14.8 1.7
14.6 1.7
15.4 1.7
16.2 1.7
16.2 1.7
16.2 1.7
16.1 1.7
16.0 1.7
16.0 1.7
17.3 1.7
18.6 1.7
13.9
SF6
ppm A
0.075
0.076
0.073
0.072
0.073
0.029
0.024
0.022
0.020
0.018
0.018
0.018
0.018
0.018
0.018
0.017
0.017
0.017
0.016
0.016
0.015
0.015
0.048
0.047
0.047
0.047
0.046
0.046
0.046
0.046
0.046
0.046
0.046
0.046
0.046
0.046
0.047
0.046
0.046
0.045
0.045
Methane
ppm A
8.4 3.1
8.5 3.2
8.2 3.0
8.1 3.0
8.1 3.0
6.6 1.1
5.4 0.9
4.8 0.8
4.3 0.7
4.0 0.7
3.9 0.6
3.9 0.6
4.0 0.7
4.0 0.7
3.9 0.6
3.9 0.6
3.8 0.6
3.8 0.6
3.6 0.6
3.4 0.5
3.3 0.5
3.3 0.5
10.2 2.0
10.0 1.9
10.1 1.9
10.2 1.9
10.3 1.9
10.2 1.8
10.2 1.9
10.2 1.9
10.1 1.9
10.4 1.9
10.7 1.9
10.7 1.9
10.7 1.9
10.6 1.9
10.6 1.9
10.7 1.9
11.2 1.9
11.8 1.8
10.8
SO2
ppm A
13.2
13.3
12.6
12.6
12.8
18.2 5.0
15.2 4.2
13.4 3.8
11.2 3.4
10.0 3.2
9.6 3.1
9.5 3.1
9.8 3.2
9.8 3.1
9.4 3.1
9.4 3.0
9.2 3.0
9.3 3.0
8.8 2.9
8.0 2.7
7.7 2.6
7.7 2.6
19.6 8.4
19.6 8.1
19.1 8.2
19.0 8.2
20.2 8.0
21.0 7.9
20.7 8.0
19.7 8.1
18.7 8.1
19.0 8.1
19.3 8.0
19.5 8.1
19.2 8.1
18.6 8.1
18.6 8.1
18.7 8.1
19.0 8.0
21.2 7.9
17.7
CO
ppm A
25.7
26.0
25.1
24.9
24.5
146.8 11.5
110.8 9.3
90.9 8.2
73.7 7.2
62.3 6.6
59.0 6.5
57.7 6.5
60.1 6.6
58.0 6.5
56.1 6.4
54.2 6.2
51.6 6.1
52.1 6.1
47.9 5.8
40.2 5.5
36.8 5.3
36.9 5.3
239.7 20.7
233.2 20.1
235.7 20.3
237.7 20.2
240.8 20.0
241.5 19.8
239.3 19.9
237.4 20.1
236.2 20.1
242.4 20.2
247.8 20,2
247.3 20.3
247.3 20.2
246.3 20.3
246.9 20.2
246.7 20.2
259.6 20.3
273.4 20.4
194.7
Formaldehyde
ppm A
4.6
4.7
4.5
4.5
4.5
1.6 ' 1.5
1.3
1.1
1.0
0.9
0.9
0.9
0.9
0.9
0.9
0.9
0.8
0.8
0.8
0.7
0.7
0.7
5.0 2.9
5.3 2.8
5.7 2.8
5.8 2.8
6.2 2.7
6.4 2.7
6.1 2.7
5.8 2.8
5.7 2.8
6.2 2.8
6.8 2.8
6.7 2.8
6.6 2.8
6.5 2.8
6.5 2.8
6.4 2.8
7.4 2.7
8.4 2.7
4.5
da
-------
TABLE B-2. Continued. Addtional Hydrocarbon Results in Wet Samples From the Plant B Outlet.
Date
8/27/97
Run 1
8/27/97
Run 1
Time
10:20
10:25
10:34
10:40
10:45
11:45
11:46
11:48
11:50
11:51
11:53
11:54
11:57
11:59
12:00
12:02
12:04
12:05
12:07
12:09
12:10
12:13
14:27
14:29
14:30
14:32
14:34
14:36
14:38
14:40
14:41
14:43
Average — >
File Name
REOUS102
REOUS103
REOUS104
REOUS105
REOUS106
18270011
18270012
18270013
18270014
18270015
18270016
18270017
18270018
18270019
18270020
18270021
18270022
18270023
18270024
18270025
18270026
18270027
18270088
18270089
18270090
18270091
18270092
18270093
18270094
18270095
18270096
18270097
Heptane
ppm A
25.2
24.6
24.6
24.8
23.8
22.4 0.7
18.4 0.4
15.0 0.5
11,9 0.8
10.0 0.9
9.8 0.9
9.8 0.9
9.6 0.9
9.6 0.9
9.1 0.9
8.5 0.9
8.3 0.9
8.3 0.9
8.3 0.9
25.0
24.6
24.9
7.2 0.8
7.5 0.8
10.7 0.7
14.7 0.6
15.6 0.6
15.4 0.6
13.6 0.6
13.1 0.6
13.6 0.6
13.9 0.6
8.1
1-Pentene
ppm A
18.1 23
19.0 2.2
17.2 23
13.9 23
15.6 2.2
7.6
13.6
5.8
5.2
5.8
6.0
6.0
6.1
6.0
6.0
6.0
6.1
6.1
6.1
18.5 2.4
18.5 2.3
18.5 2.3
7.6
7.6
6.6
5.7
6.2
3.8
6.5
6.4
3.9
3.9
6.9
2-Methyl-2-butene
ppm A
18.5
18.1
18.1
18.2
17.4
4.8
2.4
3.4
15.9
17.8
18.2
18.3
18.5
18.4
18.4
18.3
18.6
18.6
18.5
18.3
18.1
18.2
16.4
16.2
14.2
12.2
3.6
3.7
3.7
3.7
3.8
3.8
B-17
-------
TABLE B-2. Continued. Addtional Hydrocarbon Results in Wet Outlet Samples
Date
8/28/97
Run 2
8/28/97
Run 2
Time
7:32
7:40
7:50
8:00
8:05
9:54
9:55
9:57
9:59
10:00
10:02
10:05
10:06
10:08
10:10
10:11
10:13
10:15
10:16
10:18
10:21
10:22
10:24
10:26
10:27
12:41
12:44
12:45
12:47
12:49
12:50
12:52
12:54
12:55
12:57
13:00
13:01
13:03
13:05
File Name
REOUS201
REOUS202
REOUS203
REOUS204
REOUS205
18280016
18280017
18280018
18280019
18280020
18280021
18280022
18280023
18280024
18280025
18280026
18280027
18280028
18280029
18280030
18280031
18280032
18280033
18280034
18280035
18280096
18280097
18280098
18280099
18280100
18280101
18280102
18280103
18280104
18280105
18280106
18280107
18280108
18280109
Heptane
ppm A
8.5 0.6
19.5 0.6
10.7 0.8
11.1 0.8
10.S 0.9
13.2 0.9
13.2 0.9
13.2 0.9
12.5 0.9
10.7 0.9
10.8 0.9
10.9 0.9
11.1 0.9
11.0 0.9
10.0 0.9
9.3 0.9
9.7 0.9
10.3 0.9
10.5 0.9
8.3 0.9
25.7
25.9
26.0
25.7
25.5
18.0
18.6
18.6
19.0
19.2
19.1
19.0
19.1
19.3
19.6
19.3
19.2
19.1
19.3
1-Pentene
ppm A
4.0
5.7
5_3
5.6
6.0
6.3
6.2
6.2
6.2
6.1
6.2
6.3
6.3
6.2
6.2
6.2
6.2
6.2
6.2
6.2
18.9 2.4
17.2 2.5
16.6 2.5
18.7 2.4
19.2 2.4
10.7 1.7
11.7 1.7
12.3 1.7
11.1 1.8
10.6 1.8
11.2 1.8
12.2 1.8
11.8 1.8
9.8 1.8
8.7 1.8
8.4 1.8
9.2 1.8
9.0 1.8
9.8 1.8
2-Methyl-2-butene
ppm A
12.2
4.1
16.3
17.0
18.4
19.3
18.9
18.9
18.8
18.6
18.7
19.1
19.2
19.0
18.9
18.8
18.7
18.8
18.9
18.8
18.8
19.0
19.1
18.9
18.7
13.2
13.6
13.7
13.9
14.1
14.0
13.9
14.0
14.2
14.4
14.2
14.1
14.0
14.2
B-18
-------
TABLE B-2. Continued. Addtional Hydrocarbon Results in Wet Outlet Samples
Date
8/28/97
Run 2
Time
13:06
13:08
13:10
13:53
13:54
13:56
13:58
13:59
14:01
14:04
14:05
14:09
14:11
14:12
14:14
14:16
14:17
14:20
14:22
14:23
14:25
14:27
14:28
14:30
File Name
18280110
18280111 .
18280112
18280134
18280135
18280136
18280137
18280138
18280139
18280140
18280141
18280142
18280143
18280144
18280145
18280146
18280147
18280148
18280149
18280150
18280151
18280152
18280153
18280154
Average — >
Heptane
ppm A
19.4
19.7
20.1
7.8 0.7
7.3 0.7
8.3 0.6
14.1 0.4
26.4 0.3
27.0 0.3
28.6 0.2
18.3 0.2
9.6 0.7
7.8 0.7
7.1 0.8
7.0 0.8
7.5 0.7
7.9 0.7
8.1 0.7
7.9 0.7
7.5 0.7
7.3 0.7
7.2 0.7
6.9 0.7
6.7 0.7
6.8
1-Pentene
ppm A
10.9 1.8
11.8 1.9
11.5 1.9
6.7
6.7
5.6
3.4
5.0
8.8
7.7
6.0
4.7
6.9
5.1
5.1
6.8
6.8
6.7
6.8
4.8
7.0
6.9
6.9
7.0
4.8
2-Methyl-2-butene
ppm A
14.3
14.5
14.7
14.4
14.3
12.0
2.9
2.0
1.6
1.5
1.1
14.2
14.7
15.5
15.6
14.6
14.5
14.4
14.6
14.7
15.0
14.8
14.9
14.9
Date
8/29/97
Run 3
8/29/97
Run 3
Time
8:48
8:54
9:01
9:08
9:14
9:21
10:05
10:07
10:09
10:10
10:12
10:14
10:15
File Name
REOUS301
REOUS302
REOUS303
REOUS304
REOUS305
REOUS306
18290018
18290019
18290020
18290021
18290022
18290023
18290024
Heptane
ppm A
11.1 0.5
11.4 0.5
12.1 0.5
12.0 0.5
11.8 0.5
12.1 0.5
17.5
17.3
17.0
16.4
16.1
16.1
16.1
1-Pentene
ppm A
3.1
3.1
3.0
3.0
3.1
3.0
6.0 1.6
4.7 1.6
4.4 1.6
4.8 1.5
5.1 1.5
5.1 1.5
7.7 - 1.4
2-Methyl-2-butene
ppm A
93
9.6
9.1
9.2
9J
9.2
12.9
12.7
12.5
12.0
11.8
11.8
11.8
B-19
-------
TABLE B-2. Continued. Addtional Hydrocarbon Results in Wet Outlet Samples
Date
8/29/97
Run 3
8/29/97
Run 3
8/29/97
Run 3
Time
10:17
10:20
10:21
10:23
10:25
10:26
10:28
10:30
10:31
10:33
10:36
10:37
10:39
10:40
10:45
12:47
12:49
12:50
12:52
12:54
12:55
12:57
13:00
13:01
13:03
13:05
13:06
13:08
13:10
13:11
13:13
13:16
13:29
13:32
13:33
13:35
13:37
13:38
13:40
13:42
13:43
13:45
File Name
18290025
18290026
18290027
18290028
18290029
18290030
18290031
18290032
18290033
18290034
18290035
18290036
18290037
18290038
REOUU307
18290095
18290096
18290097
18290098
18290099
18290100
18290101
18290102
18290103
18290104
18290105
18290106
18290107
18290108
18290109
18290110
18290111
18290112
18290113
18290114
18290115
18290116
18290117
18290118
18290119
18290120
18290121
Heptane
ppm A
16.2
17.3
19.4
21.2
22.2
22.2
22.2
22.0
22.1
22.3
22.5
22.7
21.8
21.7
21.7
17.7 0.3
18.5 0.2
18.2 0.2
15.6 0.2
13.6 0.2
13.4 0.2
13.3 0.2
14.7 0.2
14.7 0.2
14.3 0.2
13.7 0.2
13.0 0.1
13.2 0.1
11.9 0.1
9.1 0.1
7.8 0.1
7.8 0.1
4.1 1.3
4.1 1.3
4.1 1.3
4.3 1.3
4.6 1.2
5.0 1.2
4.9 1.2
4.6 1.3
4.4 1.3
4.3 1.3
1-Pentene
ppm A
10.4 1.5
8.5 1.6
3.3 1.8
2.0
2.1
2.1
2.1
2.1
2.1
2.1
2.1
2.1
2.0
2.0
2.0
8.8
7.3
6.4
5.7
5.2
5.0
5.0
5.2
5.1
5.0
4.9
4.8
4.7
4.5
4.2
4.0
4.0
4.6 3.4
4.2 3.3
4.3 3.3
4.2 3.3
4.0 3.2
3.9 3.2
3.9 3.2
4.0 3.3
4.0 3.3
4.2 3.3
2-Methyl-2-butene
ppm A
11.9
12.7
14.2
15.6
16.3
16.3
16.2
16.1
16.2
16.3
16.5
16.6
16.0
15.9
15.9
1.5
1.3
1.2
1.0
0.9
0.9
0.9
1.0
0.9
0.9
0.9
1.0
0.9
0.9
0.8
0.8
0.8
10.4
10.0
10.1
10.1
9.9
9.7
9.8
9.9
10.0
9.9
B-20
-------
TABLE B-2. Continued. Addtional Hydrocarbon Results in Wet Outlet Samples
Date
8/29/97
Run 3
Time
13:48
13:49
13:51
13:53
13:54
13:56
13:58
13:59
File Name
18290122
18290123
18290124
18290125
18290126
18290127
18290128
18290129
Average — >
Heptane
ppm A
4.6 1.3
4.6 1.3
4.5 1.3
4.4 1.3
4.2 1.3
4.2 1.3
4.6 1.2
5.0 1.2
4.4
1-Pentene
ppm A
4.2 3.3
4.2 3.3
4.2 3.3
4.2 3.3
4.3 3.3
4.2 3.3
4.4 3.2
4.6 3.2
2.9
2-Methyl-2-butene
ppm A
9.9
10.0
9.9
10.0
9.9
9.9
9.8
9.7
B-21
-------
TABLE B-3. FTIR RESULTS OF DRY SAMPLES FROM THE PLANT B BAGHOUSE INLET
Date
8/27/97
Run 1
Time
13:33
13:34
13:36
13:38
13:39
13:41
13:43
13:44
13:48
13:50
13:52
13:53
13:55
13:57
13:58
14:00
Average — >
File Name
18270064
18270065
18270066
18270067
18270068
18270069
18270070
18270071
18270073
18270074
18270075
18270076
18270077
18270078
18270079
18270080
Toluene
ppm A
0.0 2.7
0.0 2.8
0.0 2.8
0.0 3.0
0.0 3.1
0.0 3.1
0.0 3.2
0.0 3.2
0.0 3.2
0.0 3.1
0.0 3.1
0.0 3.1
0.0 3.2
0.0 3.1
0.0 3.1
0.0 3.2
0.0
Hexane
ppm A
0.0 13.5
0.0 14.2
0.0 14.3
0.0 15.0
0.0 15.5
0.0 15.9
0.0 16.2
0.0 16.2
0.0 16.1
0.0 15.9
0.0 15.9
0.0 15.9
0.0 16.0
0.0 15.9
0.0 15.9
0.0 16.0
0.0
Ethylene
ppm A
1.4 0.7
1.5 0.8
1.5 0.8
1.6 0.8
1.7 0.8
1.8 0.8
1.8 0.9
1.8 0.9
1.8 0.9
1.8 0.8
1.9 0.8
1.9 0.9
1.8 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.7
Methane
ppm A
1.9 0.8
1.9 0.9
1.8 0.9
1.9 0.9
1.9 0.9
1.9 1.0
1.9 1.0
1.9 1.0
1.9 1.0
1.8 1.0
1.9 1.0
1.8 1.0
1.9 1.0
1.9 1.0
1.9 1.0
1.9 1.0
1.9
SO2
ppm A
19.7 3.5
20.3 3.6
20.2 3.7
19.9 3.8
18.9 3.9
18.2 4.0
18.1 4.1
18.3 4.1
18.4 4.1
18.3 4.0
18.4 4.0
18.2 4.0
18.1 4.1
18.2 4.0
18.3 4.0
18.5 4.1
18.8
CO
ppm A
80.3 9.9
70.5 10.0
62.6 9.9
60.5 10.2
63.7 10.5
65.9 10.7
65.6 10.8
63.6 10.7
58.0 10.6
56.6 10.4
57.1 10.5
57.6 10.5
59.4 10.5
59.5 10.5
57.5 10.5
57.6 10.5
62.3
Formaldehyde
ppm A
0.0 1.2
0.0 1.3
0.0 1.3
0.0 1.3
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0
dd
Date
8/28/97
Run 2
Time
10:42
10:46
10:47
10:49
File Name
REINU205
18280036
18280037
18280038
Toluene
ppm A
0.0 3.0
0.0 3.3
0.0 3.3
0.0 3.4
Hexane
ppm A
0.0 15.4
0.0 16.7
0.0 16.8
0.0 17.2
Ethylene
ppm A
1.6 0.8
1.7 0.9
1.8 0.9
1.8 0.9
Methane
ppm A
2.8 0.9
2.8 1.0
2.8 1.0
2.8 1.0
SO2
ppm A
28.7 3.8
28.0 4.1
28.1 4.2
27.9 4.2
CO
ppm A
49.5 10.3
53.0 11.1
51.3 11.1
52.1 11.2
Formaldehyde
ppm A
0.0 1.4
0.0 1.5
0.0 1.5
0.0 1.5
-------
TABLE B-3. Continued. Baghouse Inlet Dry Sample Results.
Date
8/28/97
Run 2
Time
10:52
10:53
10:55
10:57
10:58
11:00
11:02
11:03
11:05
11:08
11:09
11:11
12:02
12:03
12:05
12:07
12:08
12:10
12:13
12:14
12:16
12:18
12:19
12:21
12:23
12:24
12:26
File Name
18280039
18280040
18280041
18280042
18280043
18280044
18280045
18280046
18280047
18280048
18280049
18280050
18280076
18280077
18280078
18280079
18280080
18280081
18280082
18280083
18280084
18280085
18280086
18280087
18280088
18280089
18280090
Toluene
ppm A
0.0 3.4
0.0 3.5
0.0 3.5
0.0 3.5
0.0 3.5
0.0 3.5
0.0 3.6
0.0 3.7
0.0 3.7
0.0 3.7
0.0 3.7
0.0 3.7
0.0 3.5
0.0 2.8
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.8
0.0 2.9
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.8
Hexane
ppm A
0.0 17.4
0.0 17.6
0.0 17.5
0.0 17.6
0.0 17.6
0.0 17.9
0.0 18.3
0.0 18.5
0.0 18.6
0.0 18.7
0.0 18.8
0.0 18.8
0.0 17.6
0.0 14.4
0.0 13.7
0.0 13.5
0.0 13.8
0.0 14.2
0.0 14.7
0.0 14.4
0.0 14.3
0.0 14.0
0.0 14.0
0.0 14.0
0.0 14.0
0.0 14.3
0.0 14.4
Ethylene
ppm A
1.8 0.9
1.8 0.9
1.9 0.9
1 .9 0.9
2.0 0.9
2.0 0.9
1.9 0.9
1.9 1.0
2.0 1.0
2.0 1.0
1.9 1.0
2.0 1.0
1.9 0.9
1.6 0.8
1.5 0.7
1.4 0.7
1.5 0.7
1.5 0.8
1.6 0.8
1.6 0.8
1.6 0.8
1.6 0.7
1.6 0.8
1.6 0.7
1.7 0.7
1.7 0.8
1.8 0.8
Methane
ppm A
2.8 1.1
2.7 1.1
2.7 1.1
2.7 1.1
2.8 1.1
2.7 1.1
2.8 1.1
2.7 1.1
2.5 1.1
2.5 1.1
2.5 1.1
2.6 1.1
2.2 1.1
2.2 0.9
2.2 0.8
2.2 0.8
2.1 0.8
2.1 0.9
2.1 0.9
2.1 0.9
2.1 0.9
2.1 0.8
2.0 0.8
2.1 0.8
2.1 0.8
2.1 0.9
2.1 0.9
S02
ppm A
27.5 4.3
27.5 4.3
27.4 4.3
27.7 4.3
26.5 4.3
26.1 4.4
25.7 4.5
25.4 4.5
25.3 4.6
25.3 4.6
25.2 4.6
25.1 4.6
23.6 4.4
25.2 3.7
25.7 3.5
25.9 3.5
26.0 3.5
25.9 3.6
26.0 3.7
26.0 3.7
26.1 3.6
26.4 3.6
26.8 3.6
27.0 3.6
26.2 3.6
25.8 3.6
25.5 3.6
CO
ppm A
53.6 11.3
56.3 11.5
60.8 11.5
62.3 11.5
59.8 11.4
48.4 11.3
39.3 11.4
34.2 11.3
31.4 11.3
30.7 11.4
30.4 11.4
30.5 11.4
60.0 11.2
64.1 10.0
63.4 9.6
61.5 9.5
59.7 9.6
59.5 9.7
61.5 10.0
61.6 9.8
58.2 9.7
59.5 9.5
62.3 9.6
69.0 9.6
74.0 9.7
73.5 9.8
75.0 9.8
Formaldehyde
ppm A
0.0 1.5
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6 '
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.7
0.0 1.7
0.0 1.7
0.0 1.7
0.0 1.6
0.0 1.3
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.3
0.0 1.3
0.0 1.3
0.0 1.3
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.3
0.0 1.3
Cd
to
u>
-------
TABLE B-3. Continued. Baghouse Inlet Dry Sample Results.
Dale
8/28/97
Run 2
Time
12:29
12:30
12:32
File Name
18280091
18280092
18280093
Average— >
Toluene
ppm A
0.0 2.9
0.0 2.9
0.0 2.9
0.0
Hexane
ppm A
0.0 14.5
0.0 14.5
0.0 14.5
0.0
Ethylene
ppm A
1.8 0.8
1.9 0.8
1.9 0.8
1.8
Methane
ppm A
2.1 0.9
2.2 0.9
2.2 0.9
2.4
SO2
ppm A
25.6 3.7
25.7 3.7
25.7 3.7
26.3
CO
ppm A
78.4 9.9
84.9 10.0
92.4 10.2
57.7
Formaldehyde
ppm A
0.0 1.3
0.0 1.3
0.0 1.3
0.0
Date
8/29/97
Run 3
Time
12:07
12:09
12:10
12:13
12:15
12:16
12:18
12:20
12:21
12:23
12:25
12:26
12:29
12:30
12:32
12:34
12:35
12:37
12:39
File Name
18290075
18290076
18290077
18290078
18290079
18290080
18290081
18290082
18290083
18290084
18290085
18290086
18290087
18290088
18290089
18290090
18290091
18290092
18290093
Average — >
Toluene
ppm A
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.4
0.0 2.5
0.0 2.5
0.0 2.5
0.0
Hexane
ppm A
0.0 12.8
0.0 12.7
0.0 12.7
0.0 12.7
0.0 12.6
0.0 12.7
0.0 12.7
0.0 12.7
0.0 12.6
0.0 12.6
0.0 12.6
0.0 12.6
0.0 12.6
0.0 12.5
0.0 12.5
0.0 12.4
0.0 12.5
0.0 12.6
0.0 12.6
0.0
Ethylene
ppm A
1.4 0.7
1.4 0.7
1.3 0.7
1.3 0.7
1.2 0.7
1.2 0.7
1.1 0.7
1.1 0.7
1.1 0.7
1.1 0.7
1.0 0.7
1.0 0.7
0.9 0.7
0.9 0.7
0.9 0.7
0.8 0.7
0.8 0.7
0.7 0.7
0.7 0.7
1.0
Methane
ppm A
2.2 0.8
2.2 0.8
2.2 0.8
2.1 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0 0.8
2.0
S02
ppm A
11.4 3.3
11.4 3.3
11.4 3.3
11.4 3.3
11.3 3.3
11.1 3.3
11.1 3.3
11.0 3.3
10.7 3.3
10.5 3.3
10.5 3.3
10.6 3.2
10.5 3.2
10.3 3.2
10.2 3.2
10.0 3.2
10.1 3.2
9.8 3.2
9.8 3.2
10.7
CO
ppm A
40.0 8.3
40.0 8.2
40.1 8.2
40.1 8.3
40.3 8.2
40.1 8.3
40.1 8.3
40.3 8.3
40.3 8.2
40.5 8,2
40.4 8.3
40.7 8.2
40.6 8.2
40.7 8.2
40.8 8.2
40.9 8.1
40.8 8.2
40.8 8.2
40.9 8.2
40.4
Formaldehyde
ppm A
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
1.4 1.1
2.0 1.1
2.7 1.1
3.3 1.1
3.9 1.1
4.6 1.1
5.2 1.1
5.7 1.1
6.2 1.1
6.8 1.1
7.4 1.1
7.9 1.1
8.4 1.1
9.0 1.1
3.9
CD
-------
TABLE B-3. Continued. Additional Hydrocarbon Results.
Date
8/27/97
Run 1
Time
13:33
13:34
13:36
13:38
13:39
13:41
13:43
13:44
13:48
13:50
13:52
13:53
13:55
13:57
13:58
14:00
File Name
18270064
18270065
18270066
18270067
18270068
18270069
18270070
18270071
18270073
18270074
18270075
18270076
18270077
18270078
18270079
18270080
Average — >
3-Methylpenlane
ppm A
0.0 0.6
0.0 0.6
0.0 1.2
0.0 1.3
0.0 1.3
0.0 1.4
0.0 1.1
0.0 1.1
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0
Isooclane
ppm A
0.0 0.9
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0
Heptane
ppm A
7.9 0.2
8.1 0.2
8.4 0.2
8.6 0.2
8.6 0.2
8.4 0.2
8.1 0.3
8.1 0.3
8.3 0.3
8.2 0.2
8.0 0.2
7.9 0.2
8.0 0.2
8.1 0.2
8.2 0.2
8.2 0.3
8.2
1-Pentene
ppm A
0.0 2.3
0.0 2.4
0.0 3.1
0.0 3.2
0.0 3.3
0.0 3.4
0.0 2.7
0.0 2.7
0.0 3.4
0.0 3.4
0.0 3.4
0.0 3.4
0.0 3.4
0.0 3.4
0.0 3.4
0.0 3.4
0.0
2-Methyl-2-butene
ppm A
0.0 1.3
0.0 1.4
0.0 1.5
0.0 1.5
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0
n-Pentane
ppm A
0.0 13.3
0.0 13.9
0.0 2.7
0.0 2.8
0.0 2.9
0.0 3.0
0.0 15.9
0.0 15.8
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0
Cd
-------
TABLE B-3. Continued. Additional Hydrocarbon Results.
Date
8/28/97
Run 2
8/28/97
Run 2
Time
10:42
10:46
10:47
10:49
10:52
10:53
10:55
10:57
10:58
11:00
11:02
11:03
11:05
11:08
11:09
11:11
12:02
12:03
12:05
12:07
12:08
12:10
12:13
12:14
12:16
12:18
12:19
File Name
REINU205
18280036
18280037
18280038
18280039
18280040
18280041
18280042
18280043
18280044
18280045
18280046
18280047
18280048
18280049
18280050
18280076
18280077
18280078
18280079
18280080
18280081
18280082
18280083
18280084
18280085
18280086
3-Methylpentane
ppm A
0.0 1.3
0.0 1.4
0.0 1.4
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.6
0.0 1.2
0.0 1.2
0.0 1.1
0.0 1.1
0.0 1.1
0.0 1.1
0.0 0.9
0.0 0.9
0.0 1.0
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
Isooctane
ppm A
0.8 0.4
0.8 0.4
0.8 0.4
0.7 0.4
0.7 0.4
0.7 0.4
0.7 0.4
0.7 0.4
0.7 0.4
0.7 0.4
0.8 0.4
0.7 0.4
0.0 1.3
0.0 1.3
0.0 1.3
0.0 1.3
0.0 1.2
0.7 0.3
0.7 0.3
0.7 0.3
0.0 0.9
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 0.9
0.0 0.9
Heptane
ppm A
10.4 0.4
10.7 0.5
10.4 0.5
10.6 0.5
10.3 0.5
9.7 0.5
9.6 0.5
9.6 0.5
9.6 0.5
9.5 0.5
9.1 0.5
8.6 0.5
7.8 0.7
7.4 0.7
8.1 0.3
7.9 0.3
7.7 0.7
7.1 0.4
7.0 0.4
6.7 0.4
7.1 0.2
7.2 0.2
7.2 0.2
7.3 0.2
7.2 0.2
6.8 0.2
6.8 0.2
1 -Pentene
ppm A
0.0 2.3
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.1
0.0 2.1
0.0 2.1
0.0 2.1
0.0 2.1
0.0 2.2
0.0 2.2
0.0 2.2
2.4 1.9
2.5 1.9
0.0 2.8
0.0 2.8
2.4 1.8
0.0 2.5
0.0 2.3
0.0 2.3
0.0 2.3
0.0 2.4
0.0 2.5
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.4
2-Methyl-2-butene
ppm A
0.0 1.3
0.0 1.5
0.0 1.8
0.0 1.8
0.0 1.9
0.0 1.9
0.0 1.9
0.0 1.9
0.0 1.9
0.0 1.9
0.0 2.0
0.0 2.0
0.0 1.9
0.0 5.9
0.0 5.9
0.0 5.9
0.0 1.7
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
n-Pentane
ppm A
0.0 3.8
0.0 4.1
0.0 4.1
0.0 , 4.2
0.0 4.3
0.0 4.3
0.0 4.3
0.0 4.3
0.0 4.3
0.0 4.4
0.0 4.5
0.0 4.5
0.0 3.4
0.0 3.4
0.0 18.4
0.0 18.4
0.0 17.3
0.0 14.1
0.0 13.4
0.0 13.3
0.0 13.5
0.0 13.9
0.0 14.4
0.0 14.1
0.0 14.0
0.0 13.7
0.0 13.7
CO
I
to
-------
TABLE B-3. Continued. Additional Hydrocarbon Results.
Date
8/28/97
Run 2
Time
12:21
12:23
12:24
12:26
12:29
12:30
12:32
File Name
18280087
18280088
18280089
18280090
18280091
18280092
18280093
Average — >
3-Methylpentane
ppm A
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0
Isooctane
ppm A
0.0 0.9
0.0 0.9
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.3
Heptane
ppm A
6.7 0.2
6.7 0.2
6.7 0.2
6.8 0.2
6.9 0.2
7.3 0.2
7.5 0.2
8.1
1-Pentene
ppm A
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.4
0.2
2-Melhyl-2-butene
ppm A
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0
n-Pentane
ppm A
0.0 13.7
0.0 13.7
0.0 14.0
0.0 14.1
0.0 14.2
0.0 14.2
0.0 14.2
0.0
Cd
N>
-J
Date
8/29/97
Run 3
8/29/97
Run 3
Time
12:07
12:09
12:10
12:13
12:15
12:16
12:18
12:20
12:21
12:23
12:25
12:26
12:29
File Name
18290075
18290076
18290077
18290078
18290079
18290080
18290081
18290082
18290083
18290084
18290085
18290086
18290087
3-Methylpentane
ppm A
3.7 0.2
3.9 0.2
4.0 0.2
4.1 0.2
3.9 0.4
0.0 1.0
0.0 1.0
0.0 1.1
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
Isooctane
ppm A
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.8
0.0 0.9
0.0 0.8
0.0 0.8
Heptane
ppm A
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.5
0.0 5.4
0.0 5.4
0.0 5.5
0.0 5.4
0.0 5.4
1-Pentene
ppm A
0.0 2.2
0.0 2.2
0.0 2.2
. 0.0 2:2
0.0 2.2
0.0 2.5
0.0 2.5
0.0 2.6
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
2-Methyl-2-butene
ppm A
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
1.2 0.9
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
n-Pentane
ppm A
0.0 12.5
0.0 12.4
0.0 12.4
0.0 12.4
0.0 12.4
5.1 0.2
5.3 0.2
5.4 0.3
5.6 0.2
5.7 0.2
5.9 0.2
6.0 0.2
6.1 0.2
-------
TABLE B-3. Continued. Additional Hydrocarbon Results.
CO
I
NJ
00
Date
Time
12:30
12:32
12:34
12:35
12:37
12:39
File Name
18290088
18290089
18290090
18290091
18290092
18290093
Average — >
3-Methylpentane
ppm A
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
1.0
Isooctane
ppm A
0.0 0.8
0.0 0.8
0.0 0.8
0.0 0.8
0.0 0.9
0.0 0.8
0.0
Heptane
ppm A
0.0 5.4
0.0 5.4
0.0 5.4
0.0 5.4
0.0 5.4
0.0 5.4
0.0
1-Pentene
ppm A
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.5
0.0
2-Methyl-2-butene
ppm A
0.0 1.2
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.1
n-Pentane
ppm A
6.3 0.2
6.4 0.2
6.6 0.2
6.7 0.2
6.9 0.2
7.0 0.2
4.5
-------
TABLE B-4. FTIR RESULTS OF DRY SAMPLES FROM THE PLANT B BAGHOUSE OUTLET
Date
8/27/97
Run I
Time
12:58
13:01
13:02
13:04
13:06
13:07
13:09
13:10
13:12
13:14
13:16
13:18
13:20
13:21
13:23
File Name
18270047
18270048
18270049
18270050
18270051
18270052
18270053
18270054
18270055
18270056
18270057
18270058
18270059
18270060
18270061
Average — >
Toluene
ppm A
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.8
0.0 2.8
0.0 2.8
0.0 2.9
0.0 2.9
0.0 3.0
0.0 3.0
0.0 3.1
0.0 3.0
0.0
Hexane
ppm A
0.0 13.5
0.0 13.5
0.0 13.6
0.0 13.5
0.0 13.6
0.0 13.8
0.0 14.0
0.0 14.3
0.0 14.4
0.0 14.6
0.0 14.8
0.0 15.0
0.0 15.3
0.0 15.4
0.0 15.4
0.0
Ethylene
ppm A
.2 0.7
.2 0.7
.2 0.7
.2 0.7
.2 0.7
.2 0.7
.3 0.8
.3 0.8
.4 0.8
.4 0.8
.4 0.8
.5 0.8
.5 0.8
.5 0.8
.5 0.8
.3
Methane
ppm A
2.0 0.8
2.0 0.8
2.1 0.8
2.0 0.8
2.0 0.8
1.9 0.8
1.9 0.9
2.0 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.9 0.9
2.0
Sulfur Dioxide
ppm A
18.5 3.5
18.6 3.5
18.4 3.5
18.1 3.5
18.3 3.5
18.3 3.5
18.5 3.6
18.3 3.6
18.1 3.7
17.9 3.7
17.6 3.8
17.8 3.8
17.8 3.9
18.1 3.9
18.6 3.9
18.2
Carbon Monoxide
ppm A
45.5 9.3
46.0 9.4
45.5 9.3
43.9 9.3
42,6 9.3
41.6 9.3
40.5 9.4
40.0 9.5
38.9 9.5
38.5 9.6
38.8 9.7
39.5 9.8
42.7 10.0
45.5 10.1
47.4 10.0
42.5
Formaldehyde
ppm A
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .4
0.0 .4
0.0 .4
0.0
03
to
Dale
8/28/97
Run 2
Time
11:24
11:25
11:27
11:29
11:30
11:32
11:34
11:35
11:37
11:40
11:41
11:43
11:45
11:46
11:48
11:50
11:51
11:53
File Name
18280056
18280057
18280058
18280059
18280060
18280061
18280062
18280063
18280064
18280065
18280066
18280067
18280068
18280069
18280070
18280071
18280072
18280073
Average — >
Toluene
ppm A
0.0 2.1
0.0 2.7
0.0 3.0
0.0 3.2
0.0 3.4
0.0 3.5
0.0 3.6
0.0 3.6
0.0 3.6
0.0 3.7
0.0 3.8
0.0 3.8
0.0 3.9
0.0 3.9
0.0 3.9
0.0 4.0
0.0 4.0
0.0 4.0
0.0
Hexane
ppm A
0.0 10.6
0.0 13.7
0.0 15.2
0.0 16.4
0.0 17.4
0.0 18.0
0.0 18.1
0.0 18.3
0.0 18.4
0.0 18.8
0.0 19.0
0.0 19.4
0.0 19.5
0.0 19.7
0.0 19.9
0.0 20.1
0.0 20.2
0.0 20.1
0.0
Ethylene
ppm A
2.7 0.5
2.9 0.7
2.3 0.8
2.0 0.9
2.0 0.9
2.1 0.9
2.1 0.9
2.2 .0
2.2 .0
2.2 .0
2.2 .0
2.3 .0
2.3 .0
2.2 .0
2.3 .0
2.3 .0
2.3 .1
2.3 .1
2.3
Methane
ppm A
3.4 0.6
3.0 0.8
2.6 0.9
2.5 .0
2.5 1.0
2.4
2.4
2.5
2.4
2.4
2.5
2.5 .2
2.5 .2
2.5 1.2
2.5 .2
2.5 1.2
2.6 1.2
2.6 .2
2.6
Sulfur Dioxide
ppm A
9.7 2.6
18.2 3.4
22.3 3.8
23.9 4.1
24.8 4.3
25.7 4.4
26.7 4.5
27.4 4.5
27.3 4.6
26.7 4.7
26.3 4.7
26.0 4.8
25.3 4.8
24.7 4.9
23.8 4.9
23.4 5.0
23.2 5.0
23.2 5.0
23.8
Carbon Monoxide
ppm A
80.4 7.2
93.6 9.6
86.0 10.5
97.4 11.5
115.3 12.3
108.9 12.5
105.7 12.4
108.7 12.6
108.8 12.6
108.9 12.8
104.7 12.8
104.3 12.9
99.6 12.8
90.6 12.7
91.4 12.8
94.7 13.0
91.2 12.9
85.8 12.8
98.7
Formaldehyde
ppm A
0.0 0.9
0.0
0.0
0,0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
.2
.4
.5
.5
.6
.6
.6
.6
.7
.7
.7
.7
.8
.8
.8
.8
.8
0.0
-------
TABLE B-4. Continued. Results of Dry Outlet Samples.
Date
8/29/97
Run3
8/29/97
Run3
Time
11:30
11:31
11:33
11:35
11:36
11:38
11:41
11:42
11:44
11:46
11:47
11:49
11:50
11:52
11:54
11:56
11:58
12:00
Average — >
File Name
18290056
18290057
18290058
18290059
18290060
18290061
18290062
18290063
18290064
18290065
18290066
18290067
18290068
18290069
18290070
18290071
18290072
18290073
Toluene
ppm A
0.0 3.5
0.0 3.2
0.0 3.1
0.0 3.1
0.0 3.1
0.0 3.0
0.0 3.0
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.8
0.0
Hexane
ppm A
0.0 17.5
0.0 16.2
0.0 15.7
0.0 15.6
0.0 15.4
0.0 15.4
0.0 15.1
0.0 14.9
0.0 14.8
0.0 14.7
0.0 14.7
0.0 14.7
0.0 14.6
0.0 14.5
0.0 14.5
0.0 14.5
0.0 14.5
0.0 14.4
0.0
Ethylene
ppm A
.5 0.9
.5 0.9
.5 0.8
.4 0.8
.5 0.8
.5 0.8
.4 0.8
.4 0.8
.4 0.8
.5 0.8
.5 0.8
.5 0.8
.5 0.8
.5 0.8
.5 0.8
.4 0.8
.4 0.8
.4 0.8
.5
Methane
ppm A
2.1 1.1
2.0 1.0
2.0 1.0
1.9 0.9
1.9 0.9
1.9 0.9
1.9 0.9
1.8 0.9
2.1 0.9
2.2 0.9
2.2 0.9
2.2 0.9
2. 0.9
2. 0.9
2. 0.9
2. 0.9
2. 0.9
2. 0.9
2.
Sulfur Dioxide
ppm A
11.0 4.3
8.3 4.1
7.3 3.9
6.8 3.9
6.5 3.9
6.3 3.9
6.3 3.8
6.4 3.8
6.6 3.7
6.8 3.7
6.9 3.7
6.7 3.7
6.7 3.7
6.8 3.7
7.0 3.7
7.1 3.7
7.2 3.7
7.2 3.7
7.1
Carbon Monoxide
ppm A
49.5 10.6
52.3 10.1
52.7 9.8
52.6 9.7
52.1 9.7
50.9 9.6
48.9 9.5
45.6 9.3
43.6 9.2
42.7 9.2
43.7 9.2
44.7 9.2
46.0 9.2
48.4 9.2
49.0 9.2
47.6 9.1
47.9 9.1
48.4 9.1
48.1
Formaldehyde
ppm A
0.0 1.6
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.4
0.0 1.3
0.0 1.3
0.0 1.3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0
CO
!^J
o
-------
TABLE B-4. Continued. Additional Hydrocarbon Results of Dry Outlet Samples
Date
8/27/97
Run 1
Time
12:58
13:01
13:02
13:04
13:06
13:07
13:09
13:10
13:12
13:14
13:16
13:18
13:20
13:21
13:23
Average — >
File Name
18270047
18270048
18270049
18270050
18270051
18270052
18270053
18270054
18270055
18270056
18270057
18270058
18270059
18270060
18270061
3-Methylpentane
ppm A
0.0 1.2
0.0 0.9
0.0 0.9
0.0 0.6
0.0 0.6
0.0 0.6
0.0 0.6
0.0 0.9
0.0 0.9
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0
Isooctane
ppm A
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 0.9
0.0 1.0
0.0 1.0
0.0 1.0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0
Heptane
ppm A
8.4 0.2
8.5 0.2
8.2 0.2
7.8 0.2
7.4 0.2
7.3 0.2
7.5 0.2
7.7 0.2
7.8 0.2
7.6 0.2
7.2 0.2
7.0 0.2
6.8 0.2
6.7 0.2
6.8 0.2
7.5
1-Pentene
ppm A
0.0 2.9
0.0 2.3
0.0 2.3
0.0 2.3
0.0 2.3
0.0 2.3
0.0 2.4
0.0 2.4
0.0 2.4
0.0 2.5
0.0 2.5
0.0 2.5
0.0 2.6
0.0 2.6
0.0 2.6
0.0
2-Methyl-2-butene
ppm A
0.0 .4
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .4
0.0 .4
0.0 .4
0.0 .4
0.0 .4
0.0 .5
0.0 1.5
0.0 1.5
0.0 1.5
0.0 1.5
0.0
n-Pentane
ppm A
0.0 2.5
0.0 13.3
0.0 13.3
0.0 13.3
0.0 13.3
0.0 13.5
0.0 ,13.7
0.0 14.0
0.0 14.1
0.0 14.3
0.0 14.5
0.0 14.7
0.0 15.0
0.0 15.1
0.0 15.1
0.0
Date
8/28/97
Run 2
8/28/97
Run 2
Time
11:24
11:25
11:27
11:29
11:30
11:32
11:34
11:35
11:37
11:40
11:41
11:43
11:45
11:46
11:48
11:50
11:51
11:53
File Name
18280056
18280057
18280058
18280059
18280060
18280061
18280062
18280063
18280064
18280065
18280066
18280067
18280068
18280069
18280070
18280071
18280072
18280073
Average — >
3-Methylpentane
ppm A
0.0 0.8
0.0 1.
0.0 0.9
0.0 1.0
0.0 1.
0.0 1.
0.0 1.
0.0 1.
0.0 1.
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.2
0.0 1.7
0.0 1.7
0.0 1.7
0.0
Isooctane
ppm A
0.0 0.3
0.0 ' 0.3
0.0 .0
0.0 .1
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .2
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .3
0.0 .4
0.0 .4
0.0 .4
0.0
Heptane
ppm A
9.0 0.2
8.3 0.2
7.3 0.2
6.8 0.3
6.5 0.3
6.5 0.3
6.8 0.3
7.2 0.3
7.4 0.3
7.4 0.3
7.7 0.3
7.5 0.3
7.4 0.3
7.5 0.3
7.9 0.3
8.7 0.3
9.4 0.3
10.0 0.3
7.7
1-Pentene
ppm A
0.0 1.8
0.0 2.3
0.0 2.2
0.0 2.4
0.0 2.6
0.0 2.6
0.0 2.7
0.0 2.7
0.0 2.7
0.0 2.8
0.0 2.8
0.0 2.9
0.0 2.9
0.0 2.9
0.0 2.9
0.0 3.7
0.0 3.7
0.0 2.1
0.0
2-Methyl-2-butene
ppm A
0.0 0.9
0.0 1.5
0.0 4.8
0.0 5.2
0.0 5.5
0.0 5.7
0.0 5.7
0.0 5.8
0.0 5.8
0.0 6.0
0.0 6.0
0.0 6.1
0.0 6.2
0.0 6.2
0.0 6.3
0.0 6.4
0.0 6.4
0.0 2.0
0.0
n-Pentane
ppm A
0.0 10.4
0.0 13.5
0.0 14.9
0.0 16.1
0.0 17.0
0.0 17.6
0.0 17.8
0.0 18.0
0.0 18.0
0.0 18.4
0.0 18.6
0.0 19.0
0.0 19.1
0.0 19.3
0.0 19.5
0.0 3.6
0.0 3.6
0.0 3.7
0.0
ca
U)
-------
TABLE B-4. Continued. Additional Hydrocarbon Results of Dry Outlet Samples
Date
8/29/97
Run 3
8/29/97
Run 3
Time
11:30
11:31
11:33
11:35
11:36
11:38
11:41
11:42
11:44
11:46
11:47
11:49
11:50
11:52
11:54
11:56
11:58
12:00
File Name
18290056
18290057
18290058
18290059
18290060
18290061
18290062
18290063
18290064
18290065
18290066
18290067
18290068
18290069
18290070
18290071
18290072
18290073
Average — >
3-Methylpentane
ppm A
0.0 1.5
0.0 1.4
0.0 0.7
0.0 0.7
0.0 0.7
0.0 1.0
0.0 1.0
0.0 0.7
2.8 0.9
3.5 0.3
3.4 0.3
3.4 0.3
3.3 0.3
3.2 0.3
3.2 0.3
3.1 0.3
3.1 0.3
3.0 0.3
1.8
Isooctane
ppm A
0.0 .2
0.0 .1
0.0 .1
0.0 .1
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 .0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0 1.0
0.0
Heptane
ppm A
5.9 0.3
5.4 0.3
5.0 0.2
4.6 0.2
4.2 0.2
4.0 0.2
3.8 0.2
3.6 0.2
0.0 6.4
0.0 6.3
0.0 6.4
0.0 6.3
0.0 6.3
0.0 6.3
0.0 6.3
0.0 6.3
0.0 6.3
0.0 6.2
2.0
1 -Pentene
ppm A
0.0 3.7
0.0 3.5
0.0 3.3
0.0 3.3
0.0 3.3
0.0 2.6
0.0 2.5
0.0 2.2
2.1 2.0
0.0 2.0
0.0 2.0
0.0 2.0
0.0 2.0
0.0 2.5
0.0 2.0
0.0 2.0
0.0 2.0
0.0 2.0
0.1
2-Methyl-2-butene
ppm A
0.0 .8
0.0 .6
0.0 .6
0.0 .6
0.0 .6
0.0 .5
0.0 .5
0.0 4.7
0.0 4.7
0.0 4.6
0.0 4.7
0.0 4.6
0.0 4.6
0.0 .3
0.0 4.6
0.0 4.6
0.0 4.6
0.0 4.6
0.0
n-Pentane
ppm A
0.0 3.2
0.0 3.0
0.0 2.9
0.0 2.9
0.0 2.9
0.0 15.1
0.0 14.8
0.0 14.6
0.0 14.5
0.0 14.4
0.0 14.4
0.0 14.4
0.0 14.3
0.0 14.2
0.0 14.2
0.0 14.2
0.0 14.2
0.0 14.1
0.0
Cd
u>
K)
-------
The graphs on the following pages show concentration versus time plots of the FTIR results
presented in Tables B-l to B-4. Each graph shows the FTIR results from a single day (Test Run)
and for a single analyte. Runs 1, 2 and 3 occurred on 8/27/97, 8/28/97 and on 8/29/97,
respectively.
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.
B-33
-------
B-34
-------
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
• Toluene inlet
- Toluene (dry) inlet
• Toluene out
- Toluene (dry) outlet
td
45.0
35.0
25.0
15.0
5.0
Spiked Samples
-5.0
7:00
8:00
9:00
10:00
11:00
Time
12:00
13:00
14:00
-------
Baghouse Inlet and Outlet Concentrations vs. Time
Run 3 - 8/29/97
• Toluene inlet
• Toluene (dry) outlet
• Toluene out
• Toluene (dry) inlet
25.0
15.0
co
u>
OS
s
PLH
PH
5.0
-5.0
7:30
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
CO
25.0
20.0 -
15.0
10.0
5.0
0.0
r
Baghouse Inlet and Outlet Concentrations vs. Time
8/27/97
• Ethylene inlet
• Ethylene (dry) inlet
• Ehtylene out
• Ethylene (dry) outlet
-5.0
9:30
10:30
11:30
12:30
Time
13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
• Ethylene inlet
• Ethylene (dry) inlet
• Ethylene out
• Ethylene (dry) outlet
00
11.0
9.0 -
7.0
5.0
3.0
1.0
r
-1.0
7:00
8:00
9:00
10:00
11:00
Time
12:00 13:00
14:00
-------
Baghouse Inlet and Outlet Concentrations vs. Time
Run 3 - 8/29/97
• Ethylene inlet
• Ethylene (dry) inlet
—a— Ethylene out
—X- Ethylene (dry) outlet
35.0
cd
25.0
PL,
PL,
15.0
5.0
-5.0
7:30
8:30 9:30 10:30 11:30 12:30
Time
13:30
-------
CD
15.0
10.0
5.0
r
Baghouse Inlet and Outlet Concentrations vs. Time
8/27/97
• Methane inlet
• Methane (dry) Inlet
Methane out
Methane (dry) outlet
0.0
9:30
10:30
11:30
12:30
Time
13:30
14:30
-------
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
• Methane inlet
• Methane (dry) inlet
Methane out
Methane (dry) outlet
14.0
12.0
10.0
CO
a.
a.
6.0
4.0
2.0
0.0
7:00
8:00
9:00
10:00
11:00
Time
12:00
13:00
14:00
-------
20.0
Baghouse Inlet and Outlet Concentrations vs. Time
Run 3 - 8/29/97
• Methane inlet
• Methane (dry) inlet
Methane out
Methane (dry) outlet
w
A
KJ
15.0
10.0
5.0
0.0
7:30
8:30
9:30
10:30 11:30
Time
12:30
13:30
-------
30.0
Baghouse Inlet and Outlet Concentrations vs. Time
8/27/97
SO2 inlet
SO2 (dry) inlet
SO2 out
• SO2 (dry) outlet
25.0 -
Cd
a,
a.
20.0
15.0
10.0
5.0
0.0
-5.0
9:30
10:30
11:30
12:30
Time
13:30
14:30
-------
I
50.0
45.0
40.0
35.0
30.0
25.0
20.0
15.0
10.0
5.0
0.0
-5.0
7:00
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
• SO2 inlet
• SO2 (dry) inlet
SO2 out
• SO2 (dry) outlet
8:00
9:00
10:00
11:00
Time
12:00
13:00
14:00
-------
CD
ct.
ct.
40.0
35.0
30.0
25.0
20.0
15.0
10.0
5.0
0.0
-5.0
7:30
Baghouse Inlet and Outlet Concentrations vs. Time
Run 3 - 8/29/97
SO2 inlet
SO2 (dry) inlet
SO2 out
SO2 (dry) outlet
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
Baghouse Inlet and Outlet Concentrations vs. Time
8/27/97
CO inlet
CO (dry) inlet
CO out
• CO (dry) outlet
340.0 -
290.0
oo
Pi
Pi
240.0
190.0
140.0
90.0
40.0
-10.0
U
9:30
10:30
11:30
12:30
Time
13:30
14:30
-------
Cd
150.0
130.0
110.0
90.0
70.0
50.0
30.0
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
CO inlet
(dry) inlet
CO out
CO (dry) outlet
10.0 -
-10.0
7:00
8:00
9:00
10:00
11:00
Time
12:00
13:00
14:00
-------
CO
-k".
oo
300
280
260
240
220
200
180
160
140
120
100
80
60
40
20
0
-20
7:30
Baghouse Inlet and Outlet Concentrations vs. Time
8/29/97
•CO inlet
• CO (dry) inlet
CO out
CO (dry) outlet
&B-S-DD D
Jl
8:30
9:30
10:30 11:30
Time
12:30
13:30
-------
10.0
Baghouse Inlet and Outlet Concentrations vs. Time
(Untreated Samples). 8/27/97
• Formaldehyde inlet
• Formaldehyde out
CD
8.0
6.0
4.0
2.0 -
0.0
DD a ao »• • «
-2.0
9:30
10:30
11:30
12:30
Time
13:30
14:30
-------
10.0
8.0
6.0
co g
6, £4.0
O QH
2.0
Baghouse Inlet and Outlet Concentrations vs. Time
Run 2 - 8/28/97
• Formaldehyde inlet
• Formaldehyde out
0.0
7:00 8:00 9:00 10:00 11:00 12:00 13:00 14:00
Time
-------
12.0
Baghouse Inlet and Outlet Concentrations vs. Time
(Untreated Samples). Run 3 - 8/29/97
• Formaldehyde inlet
• Formaldehyde out
03
PH
PH
10.0
8.0
6.0
4.0
2.0
0.0
-2.0
7:30
8:30
9:30
10:30 11:30
Time
12:30
13:30
-------
B-52
-------
TABLE B-5. PLANT B METHOD DETECTION LIMIT ESTIMATES
Compound
Acetaldehyde
Benzene
Carbonyl Sulfide
Methylchloride
Methylchloroform
1,1-dichloroethane
Toluene
1 ,3-butadiene
Methanol
Cumene
Ethylbenzene
Hexane
Methylene chloride
Propionaldehyde
Styrene
1,1,2,2-
Fetrachloroe thane
p-Xylene
3-Xylene
n-Xylene
2,2,4-Trimethylpentane
Formaldehyde
sul
0.19
0.41
0.01
0.61
0.09
0.17
1.27
0.31
0.10
0.23
0.00
0.14
0.25
0.08
0.00
0.08
0.35
0.37
0.79
0.04
0.26
MDL2
(ppm)
0.58
1.24
0.04
1.83
0.28
0.50
3.80
0.93
0.31
0.69
1.89
0.43
0.76
0.24
1.28
0,25
1.04
1.12
2.36
0.12
0.79
1 SU = "Statistical Uncertainty" From Proposed ASTM FTIR Method
2 "Method Detection Limit"
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 absorbances equivalent to the sample spectra, (2) runs the analytical program on
these spectra, (3) calculates the standard deviation ("statistical uncertainty," SU) in the results,
B-53
-------
and (4) multiplies the SU results by 3 to give the "Method Detection Limit" (MDL)
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.
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 test results in Tables B-l 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 =
where;
SU - The "Statistical Uncertainty."
N = The number of spectra analyzed.
C, = The concentration result from the i"1 spectrum. In this procedure the
absolute value of the results was used in equation B-l.
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.
V fr
i i\ 2-~> {
(«-i) i=i
C }2
i CM >
B-54
-------
B-2 FTIR FIELD DATA RECORDS
B-55
-------
B-56
-------
PROJECT NO. 4701-08-02
PLANT: B
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/26-8/27/97
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
13:00
8:11
8:37
15:32
15:37
16:07
FILE
NAME
BKG0827A
CTS0827A
SF61001
CTS0827B
NITCON01
PATH
20 passes
20 passes
20 passes
20 passes
System set up and leak checked
NUMBER
SCANS
RES
(cm 1)
CELL
TEMP (F)
PRESSURE
Am using the largest (3.3mm) Jacquinot stop because 1 get no throughput at the medium (1 .5mm) stop
The 1.5 nun would be better for 1 cm -1 resolution. So there may be some degradation of the resolution.
Path length set at 20 passes through the cell (approximately 10 meters)
Date: 8/27/97
101 ppm ethylene in air ALMO20008
3.89 ppm SF6
101 ppm ethfylene
N2 through wet condenser
100
100
1
1
1
1
115C
115C
115C
115C
766
770
769
767
BKC
A
A
A
APOD
NB/med
NB/med
NOTES
M
to
i
Lft
-------
PROJECT NO.
PLANT: B
4701-08-02
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/28/97
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
7:05
7:10
7:25
7:26
8.57
9:01
9:08
9:11
J
9:18
14:16
14:18
15:02
15:14
FILE
NAME
BKG0828A
CTS0828a
BKG0828B
EVAC2001
NIT2002
BKG0828C
1530828a
CTS0828b
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
N2 through cell at 2 1pm
Ethylene through cell at 2 1pm
good leak check on cell, M25A is on line
SF6 spike to outlet @ 2.01 1pm, 3 89 ppm SF6
NUMBER
SCANS
250
100
Purging w/N2 for new background but there is a lot of moisture
Process down
Kiln Back on
N2 through cell
250
Some residual hydrocarbons came through the line for background
Spectrum of evacuated cell
Nitrogen thru cell at 2 1pm (Cell background)
small amount of residual hydrocarbons
N2 through cell at 2 1pm
toluene 121 ppm
Ethylene at 2.01 1pm
100
100
250
100
100
RES
(cra-l)
1
1
1
1
1
1
1
1
CELL
TEMP (F)
115
115
115
115
115
115
115
115
PRESSURE
772
765
765
23
763
762
760
762
BKG
A
B
B
C
C
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTE'S
GO
00
-------
PROJECT NO.
PLANT: B
4701-08-02
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 8/29/97
BAROMETRIC:
OPERATOR: T. Gever
SAMPLE
TIME
6:43
6:56
7:08
7:46
13:21
14:30
14:40
14:46
FILE
NAME
BKG0829
CTS0829A
NIT3001
BKG0829
BKG0829
BKG0829
SF60829a
CTS0829b
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
N2 through cell
1 0 1 ppm ethylene in air
N2 through cell 3.6 1pm - showing ice band
N2 through cell at 3.9 1pm
N2 through cell at 3.6 1pm
NUMBER
SCANS
250
100/250
100/250
250
250
Did not pass inlet location leak check at the end of the run
Tightened a fitting and then passed the leak check
N2 through cell at 2.01 1pm
SF6 3.89 ppm through cell (2> 2.01 1pm
101 ppm ethylene (2> 2.01 1pm through cell
250
100/250
100/250
RES
(cm 1)
1
1
1
CELL
TEMP(F)
115
115
115
115
115
115
115
115
PRESSURE
761
762
769
770
769
763
764
764
BKG
A
A
D
D
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
td
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
(FT1R Sampling Data)
BAROMETRIC:
DATE:
8/27/97
OPERATOR: T. Gever
SAMPLE
TIME
8:50
9:02
9:43
9:40
9:45
9:55
10:09
10:14
10:16
10:20
10:27- 10:31
10:34
10:37-10:41
10:42- 10.46
10:47
10:54
11:00- 11:04
11:07- 11:10
11:13- 11:16
11:17
11:20/11:15
11:15-11:17
11:23
11:39
11:41
11:46
12:16
FILE
NAME
REINUI01
REOUU10I
18270001
18270007
REOUS102
REOUS103
REOUS104
REOUS105
REOUS106
REINS 102
REfNSlOS
REINS 104
REAINS105
REAINS106
18270008
18270012
18270027
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
inlet sample flowing
outlet sample flowing
SF6 spike on to inlet
Manual runs started
Started inlet sample
NUMBER
SCANS
100
100/250
100/250
100/250
RES
(cm-D
1
1
1
1
Spike not working, start sampling while look at where Spike flow is going
first inlet sample
P=775 torr, process went down
process restarted
Started SF6 spike to outlet
Started fill with outlet,
P = 766 torr
Started fill with outlet sample
Started lOlpptn cthylene spike to outlet
Outlet spiked with cthylene
Outlet spiked with cthylene
101 ppm Ethylene spiked at 2.01 Ipm
10 1 ppm ethylene spiked to inlet @ 2.0 1 Ipm
Inlet spiked with elhylene
Inlet spiked with ethylene
Inlet spiked with ethylene
Switched to SF6 spike @ 2.01 Ipm to inlet
5 minute time shift to match
3.89 ppm SF6 spike at 2.01 Ipm
3.89 ppm SF6 spike at 2.01 1pm
Outlet sample
Process down
Process up
First good sample
Final outlet sample
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100
100
1
1
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
115
115
115
115
115
115
115
115
115
115
115
115
115
115
118
118
SPIKED/
UNSPIKED
UN
UN
SF6
SF6
UN
S
s
S
s
s
s
s
s
s
s
UN
SAMPLE
COND.
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
SAMPLE
FLOW
3.5 Ipm
51pm
2 Ipm, VTP = 4.9
2 Ipm, VTP = 4.8
41pm
SF6' 3.89 pom (2.01 1pm)
BKG
A
A
A
A
A
SF6 = 2.0 1 1pm, sample flow = 4 1pm
SF6 = 2.01 Ipm, sample 4.0 1pm
101 ppm elhylene at 2.01 1pm
101 ppm elhylene at 2.01 1pm
41pm
4 1pm, spike 2.01 1pm
4 1pm, spike 2.01 Ipm
4 1pm, spike 2.01 Ipm
41pm
4 Ipm
A
A
A
A
ON
O
-------
PROJECT NO. 4701-08-02
PLANT: B
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/27/97
SAMPLE
TIME
12:18
12:48
12:56
13:06
13:30
14:00
14:03
14:10
14:14
14:44
14:46
14:48
15:19
FILE
NAME
18270030
18270045
18270047
18270061
18270064
18270080
18270088
18270097
18270098
18270115
PATH
Inlet sample
final inlet sample
Outlet sample
Final outlet sample
Inlet sample
final inlet sample
Outlet sample
Process down
Process up
NUMBER
SCANS
100
100
100
100
RES
(crn-l)
1
1
1
1
CELL
TEMP(F)
118
115
117
115
SPIKED/
UNSPIKED
u
u
u
u
Cone heater in outlet filter box had shaken loose and filter was at 1 25 F. Reconnected - at 1 43 F.
Last good outlet sample
Started inlet sample
First good inlet spectrum
Last good inlet spectrum
SAMPLE
COND.
H/W
C/D
C/D
H/W
SAMPLE
fLOW
4 Ipm
41pm
4 Ipm
4 Ipm
BKG
•
A
A
A
A
•
Cd
-------
PROJECT ISO. 4701-08-02
PLANT: B
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/28/97
OPERATOR: T. Gtyer
SAMPLE
TIME
7:31
7:37
7:48
7:53
7:59
8.03
8:08
8:16
8:23
• 8:27
8:32
8:41
9:21
9:22
9:48
9:52
10:36
10:41 - 10:45
10:46
11.11
11:11
FILE
NAME
REOUS201
REAOUS202
REAOUS203
REAOUS204
REAOUS205
REA1NS201
REAINS202
REA1NS203
REAINS204
18280001
18280014
18280016
18280035
REINU205
18280036
18280050
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
Outlet spike with SF6
Mike Maret of PES reports approx. 3 1% moisture
Outlet spike with SF6
Outlet spike with SF6
Start toluene spike @ 2.01 1pm
Outlet spike with toluene
Outlet spike with toluene
Start spike toluene at inlet at 2.0 1 Ipm
Inlet spike with toluene
Inlet spike with toluene
Start inlet SF6 spike at 2.0 1 Ipm
Inlet spike SF6
Inlet spike SF6
Start Till, start continuous inlet sample
First inlet spectrum
Last inlet spectrum
First outlet spectrum
I>ast outlet sample
Started inlet sample through condenser
Inlet batch sample
First continuous inlet spectrum
Last inlet sample
Process down, changing Balston filter at inlet probe.
NUMBER
SCANS
100/250
100/250
100/250
100/250
100/250
100
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
RES
(C.-1)
1
1
1
1
1
1
1
1
I
1
1
1
1
1
1
1
CELL
TEMP(F)
115
115
115
118
118
118
115
115
115
115
115
115
115
115
115
115
SPIKED/
UNSFIKED
s
s
s
s
s
s
s
s
s
u
u
u
u
u
u
u
SAMPLE
COND.
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
Cond
Cond
SAMPLE
FLOW
41pm
4 Ipm
4 Ipm
4 Ipm
41pm
4 Ipm
4 1pm
4 Ipm
41pm
5 Ipm
5 Ipm
5 1pm
5 Ipm
41pm
4.5 Ipm
BKG
A-
A
A
A
A
A
A
A
A
B
B
B
B
B
. B
B
Cd
Os
-------
FTIR FIELD DATA FORM
PROJECT NO.
PLANT:
4701-08-02
(FTIR Sampling Data)
DATE: 8/28/97
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
11:13
11:17
11:22
11:23
11:53
12:00
12:03
12:40
13:10
13:15
13:46
13 50
13:55
14:07
14:32
FILE
NAME
18280053
1 8280056
1 8280073
1 8280076
18280093
18280096
18280112
10280115
18280131
1820134
1820135
1820143
1820154
PATH
20 passes
Evacuated Condenser impinger
Start outlet sample through condenser
First outlet spectrum through condenser
Process back up
First outlet sample after process back up
Last outlet spectrum
First inlet sample
Last inlet sample
First outlet sample
last outlet sample
First inlet sample
Last inlet sample
First outlet sample
Process down, last good sample
First sample after process back up
Last outlet sample
NUMBER
SCANS
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
RES
(cm-1)
1
1
1
CELL
TEMP(F)
115
115
115
115
115
115
115
115
115
115
SPIKED/
UNSPIKED
u
u
u
u
u
u
u
u
u
u
SAMPLE
COND.
Cond
Cond
Cond
Cond
H/W
H/W
H/W
H/W
H/W
H/W
SAMPLE
FLOW
41pm
4.51pm
5 1pm
51pm
4 1pm
41pm
51pm
5 1pm
41pm
41pm
BKC
B
B
B
B
B
B
B
B
B
B
.
to
0\
U)
-------
PROJECT NO. 4701-08-02
PLANT: B
FTIR FIELD DATA FORM
(FT1R Sampling Data)
BAROMETRIC:
DATE:
8/29/97
OPERATOR: T. Gever
SAMPLE
TIME
7:54-7:58
8:04-8:08
8:11 -8:14
8:17
8:26
8:33
8:40
8:43
8:45 - 8:48
8:51 -8:55
900-9:03
9:03
9:06-9:10
9:12-9:16
9:18-9:22
9:22
9:24
9:24-9:28
9:32
10:00
10:03
1005
10:41
10:49
10:52
10:20
FILE
NAME
REINS301
REINS302
REINS303
REINS304
REINS305
REINS306
REOUS301
REOUS302
REOUS303
REOUS304
REOUS305
REOUS306
REINU307
18290001
18290016
18290018
18290038
REOUU307
18290049
PATH
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
20 passes
Inlet spiked with SF6 @ 2.01 1pm
P = 769 torr
Inlet spiked with SF6 @ 2.01 Ipm
Inlet spiked with SF6 (a! 2.0 1 1pm
Start inlet ethylene spike at 2 1pm
Inlet ethylene
Inlet ethylene
Inlet ethylene
Ethylene spike on to outlet/ spike off at inlet
Outlet spiked with ethylene
Outlet spiked with ethylene
Outlet spiked with ethylene
started SF6 spike to outlet/ ethylene spike off
Outlet sample spiked with SF6 @ 2.0 1 Ipm
Outlet sample spiked with SF6 & 2.01 1pm
Outlet sample spiked with SF6 @ 2.01 Ipm
SF6 spike off at outlet
go to hot/wet sampling at inlet
inlet sample
first continuous inlet sample
Last inlet sample
Started fill with outlet sample
first good outlet sample
last outlet sample
NUMBER
SCANS
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
100/250
RES
(cm-l)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
Outlet unspiked to verify test hydrocarbon's concentrations have dropped.
Started to fill with inlet sample
inlet sample H/W
100/250
1
CELL
TEMP(F)
114
114
114
114
114
114
115
115
115
115
115
115
115
115
115
115
115
115
the process was changed - this change coincides with the observed drop in TI1C;
hydrocarbon, and CO in FTIR , increase in moisture
SPIKED/
UNSPIKED
S/SF6
S/SF6
S/SF6
S/ethylene
S/ethylene
S/ethylene
S/ethylene
S/ethylene
S/ethylene
S
S
S
U
U
U
U
U
U
SAMPLE
COND.
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
H/W
SAMPLE
FLOW
4 Ipm
4 Ipm
4 1pm
4 1pm
4 1pm
4 Ipm
4 1pm
4 Ipm
4 Ipm
4 Ipm
4 Ipm
4 Ipm
4 Ipm
41pm
4 Ipm
4 Ipm
4 Ipm
41pm
BKC
B
B
B
B
B
B
B
B
B
B
B
B
B
" B
B
B
B
B
B
CD
fc
-------
PROJECT NO. 4701 0802
PLANT: B
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
DATE:
8/29/97
OPERATOR: T. Gever
SAMPLE
TIME
11:23
11:25
11:29
12:00
12:03
12:07
12:11
12:21
12.40
12:42
12.44
12:46
13:16
13:24
13:29
13.31
14:00
14:01
14:07
14:13
FILE
NAME
1829053
1821056
18290073
18290075
18290078
18290082
18290093
18290094
182900111
18290112
18290129
18290132
18290136
PATH
20 passes
20 passes
Last inlet sample
Start outlet through Conditioner
first good outlet sample
Computer clock is about 1 hi slow
last outlet sample
Started filling with inlet sample
Inlet
Process down
Kiln back on line
Last inlet sample
P= 760 torr
NUMBER
SCANS
100/250
100/250
100/250
100/250
Cell inlet valves may have been closed during this period
so samples (0073 - 0093) may not be good
Process down
Started nil with outlet
first outlet spectrum
Last outlet sample, process is still down
Kiln is back on line
Start fill with outlet
first outlet sample
last outlet sample
start fill with inlet
first inlet sample
Last good outlet sample
100/250
100/250
100/250
100/250
100/250
RF.S
(cm-1)
1
1
1
1
1
1
1
1
1
1
CELL
TEMPfJ)
115
115
115
115
115
115
115
115
115
115
SPIKED/
UNSPIKED
U
U
U
U
U
U
U
U
U
U
SAMPLE
COND.
1I/W
Cond
Cond
Condenser
Condenser
H/W
H/W
H/W
H/W
H/W
SAMPLE
FLOW
4 1pm
41pm
41pm
4 !pm
4 1pm
41pm
5 Ipm
51pm
BKC
I
B
B
R
B
B
B
C
C
C
w
b\
-------
B-66
-------
Data Slicci: FTIR Background and Calibration Spectra: EPA Woik Assignment 4
Date
Time
File Name
Path
LocatJorVNolBS
f scans
*P
I// •**•»- KO t*~1fi
^L
(cm-1)
Cell temp (F)
Pressure
BKG
Js^L
3trf
Os
-J
3d ^~
*
Wlt
-------
DalaShcct: PTIR Background and Calibration Spccl/a: EPA Work Assignment 4- .
Date
Time
File Name
Path
LocatiorVNoles
» scans
(cm-1)
JLci_
Cell temp (F)
Pressure
BKG
_Agod
'V^'
-?
m$^
-U-
Cd
Ov
oo
\rl
(00
XO-
7 O
4^-
E
T?*
-------
Datasheet FTIR Background and Calibration Spectra: EPA Work Assignment 4- .
Date
Tims
File Name
Palh
Location/Notes
•scans
Res (cm-1)
Cell temp (F)
Pressure
BKG
t.Q
/ t'j
/ft
//,,
f.o
fJH 3oo (
JL£_
t/t,'
^L Ctf]T@
''
1. 0
H
/L
V
f^TT
< L
~^F—r^~—/T / if) ,
-T\f.\^+^f6/.<-« /.(.q/n's
I. O
U5
o
to
"br
U2_
-------
iiiii Shed: FTJR Samples:
-------
Data Slicci: FTIR Samples:
if
l'A Work Assignment 4- .
Dafr ,
sS|
Sample lime I File name
PaUi
•i£f-
Localion/Noles
^H^E^r:
*scans
Res (cm l)i Cell Tump (F)
f, o
1 ,0
/ / k"
Spk/Unsp
Samle Corid
^a/iiple Flow
BKG
4UX
£7
BTZ
1C
/L
UH>
CO
-V^
^—
Z_o_
n^
JC£L
/o
^
-------
D heel. FTIR Samples:
EPA Work Assignment 4-
(I
Dale
lime
File name
Pa»i
•scans
Res (ctn-1
/ 0
Cell Temp (F)
// 5
Spk/Unsp
Sample Com)
Sample Flow
BKG
.Ao-
J£&_
5"
-A-
-A-
c^z
Jf&^OL
¥
0-5
~B~
C^CL
-------
•scans Res (cm-1
Cell Temp (F)
Spk/Unsp
Sample Good
Sample Flow
BKG
IU-
J £2 Li
V
ti
3Z-
ii^
A
//
1^G_
L .heat: FTIR Samples:
EPA Work Assignment 4-
Dale
Sample time
11 1*7
U)
File name
I&2-2
Pan
nr
Loca don/Notes
-------
2.1
L ,hecl: FT1R Samples:
EPA Work Assignment 4-
Pale
ample bme
fe
File name PaBi
^TAT?
Locabon/Nol
#scans
Res (cm-1
y_£af.£>*
e7K/fc»v^.
t\
>2
1 i
CeM Temp (FJ
Spk/Unsp
Sample Cond
Sample Flow
BKG
I.D
it f
ff
w
^-J-
"775*7?
r ^
U
*-T-yi-T J a ti t J/s
Hf bv-J-H.i'i-i'O ,j fiti ^.'t-^V
y./>^
*^ ^
-------
D ,heet: FTIR Samples:
•2.H
EPA Work Assignment 4- .
-------
D heel: FTIR Samples:
EPA Work Assignment 4-
td
•ia
-I
ample time
File name
r
Locabon/Noles
7^
•scans les (cm-1
Cell Temp (F)
Spk/Unsp
-U-
Sample Cond
Sample Flow
BKG
-------
B-3 FTIR FLOW AND TEMPERATURE READINGS
B-77
-------
B-78
-------
(Y)
9
Q
oo
td
FTIR FIELD DATA FORM
PROJECT NO. 3&o'/ --)<•/ PLANT:
DATE:
BAROMETRIC: "/-7V
INLET
CLOCK
TIME
DELTA P
IN. H2O
STACK
TEMP.
PROBE
TEMP.
PROBE BOX
TEMP.
OUTLET
CLOCK
TIME
DELTA P
IN. H20
Ld-
l.
STACK
TEMP.
PROBE
TEMP.
PROBE BOX
TEMP.
7
OPEP *
FTIRF^^M.XLS
-------
B-80
-------
FTIR FIELD DATA FORM
PROJECT NO. ^c^-2*/ PLANT:
Cd
I
oo
CLOCK
TIME
t&ll
/ / 1 '? •
OPER * Ti
INLET
DELTA P
IN. IUO
G.1\
KJB
STACK
TEMP.
•-n
l -7
PROBE
TEMP.
-^
PROBE BOX
TEMP.
DATE:
CLOCK
TIME
Hz/
FT1RFO«»M.XLS
BAROMETRIC:
OUTLET
DELTA P
IN. 1120
A
/
ft
STACK
TEMP.
PROBE
TEMP.
PROBE BOX
TEMP.
"S-08-97
A'.. ^
-------
(•0
y
. j
.i
FTIR FIELD DATA FORM
PROJECT NO. 3flQl/-^lt/ PLANT:
CLOCK
TIME
T3 U
oo
INLET
DELTA P
IN. H2O
A/
P.G, \
\A
\,A
V
STACK
TEMP.
3/2-
PROBE
TEMP.
PROBE BOX
TEMP.
OPER "OR:
DATE:
BAROMETRIC:
OUTLET
CLOCK
TIME
DELTA P
IN. H2O
STACK
TEMP.
PROBE
TEMP.
PROBK BOX
TEMP.
loct-\
175"
10
4-
"S-08-97
-------
APPENDIX C
EQUIPMENT CALIBRATION CERTIFICATES
-------
-------
C-l CALIBRATION GAS CERTIFICATES
C-l
-------
C-2
-------
• - — -i n til)
GASES
7 99S 6389
1 3
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-------
OCT-16-96 UJED 13:29
EID SPECIOLJV
998 6399
1 3
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01 05-98 16:56 O215 766 0320 SCOTT
Scott Specialty Gases
6141 BASTON ROAD PO BOX 310
From': PLUMSTBADVILLB PA 18949-0310
Phona: 215-766-8861 Fax: 215-766-2070
CERTIFICATE OF ANALYSIS
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: +-1%
FILL PRESSURE: 2000 PSIG
BLEND TYPE : GRAVIMETRIC MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT CONC MQLHS (MOT.RSI
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Scott Specialty Gases
6141 BASTON ROAD PO BOX 310
PLUMSTBADVILLE PA 18949-0310
Phone: 215-766-88S1 Fax: 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH PROJECT #: 01-89796-005
DAVE ALBURTY, X1525 PO#: 029872
425 VOLKSR BLVD ITEM #: 01023912 4AL
DATE: 5/13/97
KANSAS CITY MO 64110
CYLINDER #: ALM057730 ANALYTICAL ACCURACY: +/- 2>
FILL PRESSURE: 2000 PSIO
BLSND TYPE : CERTIFIED MASTER GAS
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Scott Specialty Gases
1290 COMBERMERE STREET
TROY MI 48083
Phone: 248-589-2950
C E R T I P I
GATE OF
Fax: 248-589-2134
ANALYSIS
MIDWEST RESEARCH
MELISSA TUCKER; # 026075
425 VOLKER BLVD
KANSAS CITY
PROJECT #: 05-97268-002
P0#: 026075
ITEM #: 05023822 4A
DATE: 6/03/96
MO 64110
CYLINDER #: A7S53 j
FILL PRESSURE: 2000 PSI
ANALYTICAL ACCURACY: +/- 2%
PRODUCT EXPIRATION: 6/03/1997
BLEND TYPE : CERTIFIED MASTER GAS
COMPONENT
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Scott Specialty Gases, Inc.
Sped 6141 EASTON ROAD PO BOX 310
From: PLUMSTEADVILLE PA 18949-0310
Phone: 215-766-8861 Fax: 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH
PO#014952
425 VOLXER BLVD
KANSAS CITY
MO 64110
PROJECT #: 01-59176-001
PO#: 014952
ITEM f: 01021912 2AL
DATE: 7/20/94
CYLINDER #: ALM020008 ANALYTICAL ACCURACY:
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Scott Specialty Gases
6141 EASTON ROAD
PLUMSTEADVILLE
Phone: 215-766-8861
CERTIFICATE
PA 18949-0310
PO BOX 310
0 F
Fax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC 27511
PROJECT #: 01-08674-002
P0#: A035678
ITEM #: 01021912 2AL
DATE: 9/22/98
CYLINDER #: ALM020008
FILL PRESSURE: 400 PSIG
BLEND TYPE : ACUBLEND MASTER GAS
COMPONENT
ETHYLENE
AIR
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C-9
-------
c-io
-------
C-2 ENVIRONICS MASS FLOW METER CALIBRATIONS
C-ll
-------
C-12
-------
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 A2.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
10000.
1 ow
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
a Sierra Cal Bench(TM), a traceable
This calibration is referenced to
a pressure of 29.92 in.Hg (760Torr )
True F
510 .51
1021 .4
2046 .9
3074 .8
4103 .8
5136.6
6156.8
7182 .5
8203 .3
9219 .5
10233 .
lew
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last saved on
Friday 03 January S7
at 17:09:00
Verified by:.
Date : / - ^ - 11
C-13
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf *
Description: AIR
Size: 100.0
SCCM, K-factor: 1.0
SERIAL
This flow controller was calibrated using
Primary Flow Standard Calibration System.
dry air at a temperature of $JUc ( C) and
5 *
10 %
20 *
30 %
40 %
50 %
60 *
70 %
80 X
90 X
100%
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
a Sierra Cal Bench(TM), a traceable
This calibration is referenced to
a pressure of 29.92 in.Hg (760Torr)
True Flow
5 .
10
20
30
40
50
60
70
80
91
236
.269
.434
.524
.606
.636
.683
.779
.917
.035
101 .12
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last saved on
Friday 03 January 97
at 19 ill :00
Verified by:
Date :_/
- 9?
C-14
-------
AO -7 3
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 1, 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 £iF ( C) and
5
10
20
30
40
50
60
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
10000 .
1 ow
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
a Sierra Cal Bench(TM), a traceable
This calibration is referenced to
a pressure of 29.92 in .Hg (760Torr )
True F
498.79
1009 .0
2029
3053
4088
5121
6143
7178
8206
9224
10252
low
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
Calibration data was last saved on
Friday 03 January 97
at 16:22:00
Verified by:.
Date: /
- 97
C-15
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf #: 3, Description: AIR
SERIAL
Size: 1000.0 SCCM, K-factor: 1.0
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceable
Primary Flow Standard Calibration System. This calibration Ls referenced to
dry air at a temperature of gXF ( _ C) and a pressure of 29.92 in.Hg ( 76.0Torr )
5
10
20
30
40
50 *
50 %
70 *
80 %
90 *
1005t
Set F
5C .0
100.0
200.0
300.0
400.0
5CO.O
600 .0
7CO.O
800.0
900.0
1GOO .0
1 ow
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
CCM
True Flew
50.
101
204
306
408
510
611
713
816
918
515
.84
.84
.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:.
Dat 3: I
.--3.2.
C-16
-------
APPENDIX D
TEST METHODS
-------
-------
D-1 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 VAPOR 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 not' 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 vim). 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 (DLt) 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 DLt 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 RMS 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 AUt can be maintained; if the measured analyte
concentration is less than MAUt, 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 ETIR "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.
At = atb ci (1)
where:
AL = absorbance at a given frequency of the ith sample
component.
aL = absorption coefficient (absorptivity) of the ith
sample component.
b = path length of the cell.
ct = 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 ETIR 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
ETIR 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
D-12
-------
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
D-13
-------
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 ETIR 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
D-14
-------
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 (1) 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 Aaencv.
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 ETIR 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 (MIST) 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, DLt, overall
fractional uncertainty, OFUi, maximum expected concentration
(CMAXJ, and t^ 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 (DLi)
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, CMAXi.
The expected measurement range is fixed by DLi and CMAXj 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
"cts!031a," 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 * 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 Pmin. 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
- 50
*ss
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 GTS 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, GTS sample
interferograms and GTS 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 s 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. I-f 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
s 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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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
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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 s 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.
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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 :
DF = (3)
where :
C5 = DF*Spikedir + Unspike(l-DF) (4)
DF = Dilution factor of the spike gas; this value
shall be *10.
SF6(dir) - SF« (°r tracer gas) concentration measured
directly in undiluted spike gas.
SF6l3plc) = Diluted SF6 (or tracer gas) concentration
measured in a spiked sample.
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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
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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 (TJ 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
(TJ , and meter absolute pressure (Pm); 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
m T-I
\7 m
VSS - 7 i (5)
Tf r,
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 (6)
c
C -
c-
where:
Ccorr = Concentration, corrected for path length.
ccaic = Concentration, initial calculation (output of the
analytical program designed for the compound) .
D-41
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Lr = Reference spectra path length.
Ls = 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.
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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. TCj =
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:
B - S* - CS (7)
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 10~4 to 3.2 x 10"4 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 CF1 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.), 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), 73-34, 1985.
D-49
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Table 1. EXAMPLE PRESENTATION OF SAMPLING DOCUMENTATION.
TlM
Hit
•ackgroud Flic Na
froce««
o
I
o
Suple Ti«
Spectnw Ftl«
iBterfercgraa
•BMUtiiM
Sew
Apadlzatioa
Call
CTS Spcctnui
-------
Colibrolion GM Lma
Mnt F(ow Calfcration Gas Manifold
Motor . 1
rH8> • !*IIIIMMII *
To Catibralion
GasCylindor*
Pump«2
Figure 1. Extractive FTIR sampling system.
-------
o
I
Lft
to
.8-
.6-
.4-
.2
0-
FRU = SRMS(FU-FL)/BAV
SRMS = .00147
BAV = 3.662
FM = FRU = .086
J^V^JtUw^
&
p-xylene
1050
1000
950 900
Wavenumbers
i
850
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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PROTOCOL FOR THE USE OF EXTRACTIVE FOURIER TRANSFORM
INFRARED (FTIR) SPECTROMETRY 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 "spectrum" 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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t.2.2 The absorption spectra of pure gases and o= m-x e~
of gases are described by a linear absorbance theory ref^^'—
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 GENERAL PRINCIPLES OF PROTOCOL REQUIREMENTS
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 Verifiability 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 strength of a
particular absorption band. Similarly, the accuracy of
measurements, may be estimated from the analysis of the refer=r- =
spectra . ~ *~~
3.3.2 Sample-Dependent Factors. Examples are spectral
interferants (e.g., water vapor and CO2) or the overlap of
spectral features of different compounds and contamination
deposits on reflective surfaces or transmitting windows. To
maximize the effectiveness of the mathematical techniques used in
spectral analysis, identification of interferants (a standard
initial step) and analysis of samples (includes effects of other
analytical errors) are necessary. Thus, the Protocol requires
post -analysis calculation of measurement concentration
uncertainties for the detection of these potential sources of
measurement error.
4.0 PR1-T1ST 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 (AUi) . The AUt is the
maximum permissible fractional uncertainty of analysis for the
ich analyte concentration, expressed as a fraction of the analyte
concentration in the sample.
4.1..3 Required detection limit for each analyte (DLt, ppm) .
The detection limit is the lowest concentration of an analyte for
which its overall fractional uncertainty (OFUi) is required to be
less than its analytical uncertainty limit (AUJ .
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
Nj, where the subscript "j" pertains to potential interferants.
Estimate the concentrations of these compounds in the effluent
(CPOT:, ppm) .
D-57
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4.3 Select and Evaluate the Sampling System. C
-he source, e.g., temperature and pressure profiles moist
content analyte characteristics, and particle corcent'atlon)
r^ticulate^r *? *Xt^CC^ gas samples. Recommended are
a particulate filter, heating system to maintain sample
"??P™?n?JeJ^Ve ^e dew ?oint for a11 Cample constituents at
all points within the sampling system (including the filter) and
sample conditioning system (e.g., coolers, water-permeable '
^n?5a?eJ' * re*°ve 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 (PBin, mmHg) and the
infrared absorption cell volume (Vss/ 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 T3', and signal integration period (t
seconds) for the analysis. Specify the nominal minimum "'
instrumental linewidth (MIL) of the system. Verify that the
fractional error at the approximate values Pg' and Ts' is less "
than one half the smallest value AUt (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.
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 (FFU, 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.eets the criterion of
Section 4.5.3.
D-58
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4.3.5 Associate, whenever possible, a single set of --3 gas
cylinders with a set of reference spectra. Replacement CTS gas
cylinders shall contain the same compounds at concentrators
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.
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
cell .
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
D-59
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sample pressure (PS), sample temperature (Ts) , reference
absorption p.athlength (LR), and interferogram signal incegrac—n
period (tSH). Signal integration periods for the background
interferograms shall be >t3R. Values of PR, LR, and tsa shall nor
deviate by more than ±1 percent from the time of recording fRlf
to that of recording {R2}.
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.,
4.9 Determine Fractional Reproducibility Uncertainties.
Using Appendix E, calculate the fractional reproducibility
uncertainty for each analyte (FRUt) from a comparison of {Rl} and
{R2}. If FRUi > 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 (Ts) or sample gas
pressure (Ps) during the actual sample analyses differ from LR,
TR, and PR, 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
(FCUJ according to Appendix F, and compare these values to the
fractional uncertainty limits (AUt; see Section 4.1). If
FCUt > AUt), 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
(RMSgsr/ 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 < AU.,
and FCUi < AUL for each analyte and that (b) the CTS chosen meets
the requirements listed in Section 4.5.
5.0 SAMPLING AND ANALYSIS PROCBDUKX
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. = L, t.3. Leak volumes shall
be s4 percent of Vss.
D-61
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5.2 Verify Instrumental Performance. Measure the noise
level of the-system in each analytical region using the'proced"r=
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 (Ls) 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 = RLpSRUAt and RSI^ = R^RU^.
5.6' 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.
D-62
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5.6.2 Apply appropriate mathematical transformations .'« a
frequency shifting, zero-filling, apodization, smoothing) to"--e
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 sample 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 REQUIREMENTS
D-63
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[Documentation pertaining to virtually all the procedures of
Sections 4, -5, and 6 will be required. Software copies of
reference spectra and sample spectra will be retained for some
minimum tim» 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 41, 945A (1975); Appl.
Sp«ctroicopy 444. 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 D," 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 X
DEFINITIONS OF TERMS AND SYMBOLS
A.I Definitions of Term*
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 pathlength - 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.
Nata*- The quantitative result for a single analyte may be
based on data from more than one analytical region.'
apodiiation - modification of the ILS function by multiplying the
interferogram by a weighing function whose magnitude varies
with retardation.
background spectrum - the single beam spectrum obtained with all
system components without sample present.
baseline - 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.
Beers's law - the direct proportionality of the absorbance of a
compound in a homogeneous sample to its concentration.
calibration transfer standard (CTS) gas - 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; fo.r sample
spectra, it is the quantity directly determined from Beer's
law. The units "centimeters-ppm" or "meters-ppm" are
recommended.
D-67
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derivative absorption spectrum - a plot of rate of change o*=
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 interf erograms
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
( interf erogram) 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.--., GC/FTIR; HPCL/FTIR, and the use of FTIR should be
explicit; i.e., FTIR not IR.
frequency, TT - the number of cycles per unit time.
infrared - the portion of the electromagnetic spectrum containing
wavelengths from approximately 0.78 to 800 microns.
interferooram, I(o) - 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.
D-68
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linewidth - che full width at half maximum of an absorption ~a —
in units of wavenumbers (cm"1) .
mid-infrared '- the region of the electromagnetic spectrum ^r-m
approximately 400 to 5000 cm'1. " ~
pathlangth - see "absorption pathlength."
reference apectra - 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,
-------
Note: Performing the FT o£ a zero-filled interferogram
results in correctly interpolated points in the computed
spectrum. ^
A.2 Definitions of Mathematical Symbols
A, absorbance - the logarithm to the base 10 of the reciprocal of
the transmittance (T).
A = Iog10 - = -log10T
- band area of the ich analyte in the mch analytical
region, at the concentration (CLt) corresponding to the
product of its required detection limit (DLt) and analytical
uncertainty limit (AUL) .
- average absorbance of the icb analyte in the mch
analytical region, at the concentration (CLt) corresponding-
to the product of its required detection limit (DLt) and
analytical uncertainty limit (AUJ .
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
"meters-ppm* are recommended.
AUt, analytical uncertainty limit - the maximum permissible
fractional uncertainty of analysis for the ich analyte
concentration, expressed as a fraction of the analyte
concentration determined in the analysis.
AVT. - average estimated total absorbance in the mch analytical
region.
- estimated concentration of the kch known interferant.
CMAXj - estimated maximum concentration of the i:h analyte.
CPOTj - estimated concentration of the j"1 potential interferant.
DLt, 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,) .
PC. - center wavenumber position of the mch analytical region.
FAUt, fractional analytical uncertainty - calculated uncertainty
in the measured concentration o£ the ich analyte because of
D-70
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errors in the mathematical comparison of reference and
sample spectra.
PCU1V fractional calibration uncertainty - calculated uncertainty
in Che measured concentration of the i:h analyte because of
errors in Beer's law modeling of the reference spectra
concentrations.
pyi«» - lower wavenumber position of the CTS absorption band
associated with the mch analytical region.
FFT7. - upper wavenumber position of the CTS absorption band
associated with the mch analytical region.
FL^ - lower wavenumber position of the mch analytical region.
nfDt, fractional model uncertainty - calculated uncertainty in
the measured concentration of the ich analyte because of
errors in the absorption model employed.
FH,. - lower wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands.
FMj - upper wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands.
FRU1/ 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.
FUB - upper wavenumber position of the mcb analytical region.
IAIjm - 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:) .
isciork» indicated standard concentration - the concentration
from the computerized analytical program for a single-
compound reference spectrum for the i:h analyte or kch known
interferant.
JcPa - kilo-Pascal (see Pascal) .
L,1 - estimated sample absorption pathlength.
L, - reference absorption pathlength.
L, - actual sample absorption pathlength.
MAUt - mean of the MAUini over the appropriate analytical regions.
D-71
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MAUt,, minimum analyte uncertainty - the calculated mil- -nun
concentration for which the analytical uncertainty 1 < m'< -
(AUJ >n the measurement of the i:n analyte, based on spectra^
data in the m~ analytical region, can be maintained.
MIUj - mean of the MIU:m over the appropriate analytical regions.
MIU3m, minimum interferant uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
CPOTV/20 in the measurement of the rh 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.
Hj - number of potential interf erants .
^ - number of known interf erants .
- the number of scans averaged to obtain an interf erogram.
OPUt - the overall fractional uncertainty in an analyte
concentration determined in the analysis (OFU^ = MAX{FRUL,
FCUL, FAUL,
Pascal (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»ia ~ 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 mch
analytical region.
RMSD, root mean «quare difference - a measure of accuracy
determined by the following equation:
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.RMSD =1 £ el
where:
n = the number of observations for which the accuracy is
determined.
eL = 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" (AJ is
defined as
RMSD =
\
U) £>'-*•*'
- the (calculated) final concentration of the ich analyte.
RSI* - the (calculated) final concentration of the kcb known
interferant.
£«»•' «can tiam - time used to acquire a single scan, not
including flyback.
t,, signal 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 = N9cantscaft.
tn - signal integration period used in recording reference
spectra.
tf- - 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.
Vf- - volume of the infrared absorption cell, including parts of
attached tubing.
Wlk - 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, RMS3_, 3U3-,
SIC , SAC , S,
D-74
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APPENDIX B
IDENTIFYING SPECTRAL INTERFERANTS
B . 1 General
B.I.I Assume a fixed absorption pathlength equal to the
value Ls' .
B.I. 2 Use band area calculations to compare the relative
absorption strengths of the analytes and potential interferants .
In the mc 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 Calculations
B.2.1 Prepare spectral representations of each analyte at
the concentration CLt = (DLJ (AUL) , where DL^ is the required
detection limit and AUt is the maximum permissible analytical
uncertainty. For the mch analytical region, calculate the band
area (AAIim) and average absorbance (AAVim) 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 (IAI:m) and average
absorbance (IAVja) 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., IAIJB > 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 (AVTm) 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 where
AVT, >2 . 0 is-unsuitable.
FIGURE B.I Presentation of Potential Interferant Calculations
Analytical Regions
1 .... M
Analyte Labels
AAIU . . . AAIIM
I AAITl . • • AAI[M
Potential Interferant
Labels
1 IAIn . . • IAI1M
IAI
J:
FIGURE B.2 Presentation of Known Interferant Calculations
Analytical Regions
1 . . . . M
Analyte Labels
1 AAIU
AAIn .... AAIIM
Known Interferant
Labels
1 IAIn . . . - IAI
1H
IAI,, .... IAI
•Kl '
KM
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^ - the 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 Che
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 :
RMS = RMS TP
EST
(4)
'"
MAN
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D-78
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APPENDIX D
ESTIMATING MINIMUM CONCENTRATION MEASUREMENT
UNCERTAINTIES (MAU and MIU)
o . 1 G«n«ral
Estimate the minimum concentration measurement uncertainties
for the ich analyte (MAUJ 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
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 Calculations
D.2.1 For each analytical region, set RMS = RMS 3, if
measured (Appendix G) , or set RMS = RMSEST if estimated (Appendix
0 .
D.2. 2 For each analyte associated with the analytical
region, calculate
D.2.3 If only the mch analytical region is used to calculate
the concentration of the ich analyte, set MAUL = MAUim.
D.2.4 If a number of analytical regions are used to
calculate the concentration of the ich analyte, set MAU, equal to
the weighted mean of the appropriate MAUim 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 {m1}, then the MAU for each
analytical region is
D-79
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MAUt = W
where the weight Wilt is defined for each term in the sum as
E [FMp-FL
lit
P T (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 CPOT.,/20; replace
the value AAIia in the above equations with IAIjm.
-------
APPENDIX B
DETERMINING FRACTIONAL REPRCDUCIBILITY UNCERTAINTIES (FRU)
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 S2L, 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 Ski is a member. Form the spectra S-,
according to Sn = S2l-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 Sti, for a particular i, with lower and
upper wavenumber limits FFLm and FFU,,, respectively.
E.2.3 For each m and the associated i, calculate the band
area of S4i in the wavenumber range FFUm to FFLm. Follow the
guidelines of Section B.I. 2 for this band area calculation.
Denote the result by
E.2.4 For each m and the associated i, calculate the RMSD
of S3i between the absorbance values and their mean in the
wavenumber range FFU, to FFLm. Denote the result by SRMSm .
E.2.5 For each analytical region m, calculate the quantity
FH. = SRMSm(FFUm-FFLJ/BAV,
E.2.6 If only the mch analytical region is used to calculate
the concentration of the i analyte, set FRUt =
E.2.7 If a number p-t of analytical regions are used to
calculate the concentration of the i;h analyte, set FRUt equal to
the weighted mean of the appropriate F^ values calculated above.
Mathematically, if the set of analytical regions employed is
{m1}, then
FRU, = £ WikFMk
Ice (m' )
where the Wllt are calculated as described in Appendix D.
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D-82
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APPENDIX P
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 Calculations
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 FCUt and analytical uncertainty limit (AUL) for each
analyte.
D-83
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FIGURE F. I
Presentation of Accepted Standard Concentrations (ASCs)
and Indicated Standard Concentrations (ISC's)
Compomxt
Reference
ASC
^^ *'
*«* M(Jt
* ** *K+ MCVM*
FIGURE F.2
Presentation of Fractional Calibration Uncertainties (FCU's)
and Analytical Uncertainties (AU's)
Kane
PCIf
Ail
D-84
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APPENDIX G
MEASURING NOISE LEVELS
Q.I G«n«ral
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 Calculation*
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 RMSg,, in
the M analytical regions.
D-85
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D-86
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APPENDIX H
DETERMINING SAMPLE ABSORPTION PATHLENGTH ( L )
FRACTIONAL ANALYTICAL UNCERTAINTY (FAU)
H . 1 G«n«ral
nr-oC sp!5tra recorded at absorption pathlength (LR), gas
pressure (PH), and gas absolute temperature (TR) 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 by comparing the spectral sets {Rl} and {R3}, which are
recorded using the same CTS at Lg 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 LH, 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 ASl/ i = 1, n. Based on
the model A, = rA,, + B, determine the least-squares estimate of
r', the value of r which minimizes the square error BJ.
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 A-
and A,, as described in Section H.2.1, using values from {Rl} to
form A,,, and values from {R4} to form AS . Calculate the values
D-87
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NRMSE =
N
1*1
-
(9)
and
IAAV = ^ £
T I I T I/O
- - ~
Ts LJ P,
(10)
The fractional analytical uncertainty is defined as
FAU
NRMS,
"IA]
(11)
D-88
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APPENDIX I
DETERMINING FRACTIONAL MODEL UNCERTAINTIES (FMU)
I . 1 G«n«ral
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.
1.2 Calculations
1.2.1 For each analyte (with scaled concentration RSAJ ,
select a reference spectrum SAj with indicated standard
concentration ISCt. Calculate the scaling factors
T. Ls Ps
RA = - - (12)
1 TS LR PR ISC,
and form the spectra SACt by scaling each SA; by the factor RA, .
1.2,. 2 For each interferant, select a reference spectrum SI,,
with indicated standard concentration ISC,. Calculate the
scaling' factors
* Ts LR PR ISC,
and form the spectra SIC, by scaling each SI, by the factor RIk.
I 2.3 For each analytical region, determine by visual
inspection which of the spectra SAC, and SIC, exhibit absorbance
bands within the analytical region. Subtract each spectrum SACt
and SIC, exhibiting absorbance from the sample spectrum Sj to
form the spectrum SUBS. To save analysis time and to avoid the
introduction of unwanted noise into the subtracted spectrum, i.
is recommended that the calculation be made (1) only for those
D-89
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spectral data points within the analytical regions, and ;2) fc--
each analytical region separately using Che original spectrurrTs.
1.2.4 For each analytical region m, calculate the RMSD of
SUB3 between the absorbance values and their mean in the region
FFUm to FFLm. Denote the result by RMSSm.
1.2.5 For each analyte i, calculate the quantity
FM = > ' MA)
m a aT oca »A '
AAIi RSAi
for each analytical region associated with the analyte.
1.2.6 If only the mth analytical region is used to calculate
the concentration of the ich analyte, set FMU^FM,,.
1.2.7 If a number of analytical regions are used to
calculate the concentration of the ich 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
FMUi = E wu FM* (15)
tee(m')
where Wi)t 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{FRU,, FCUL, FAUL, FMUJ and OCU,
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D-92
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APPENDIX K
SPECTRAL DE-RESOLUTION PROCEDURES
K.I G«n«r«l.
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.
K.3 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«0305«.«if,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) conpOM 0305dr««,0305dr««.aif,1
"Compose" transforms truncated interferograms back to spectral
format.
(iii) I02SP 0305dr««.aif,0305dr«».d»f,3,l,low cm'1,high cm'1
"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-resolved incerferograms should be transformed -3--a -'-=> 3 = -=,
apodization- and zero filling that will be used to col1 s^'-""3a-cT«
spectra. Choose the desired low and high frequencies i^ cm*';'"
Transform the background interferogram in the same way
iv)
DVDR 0305dres.dflf,bkg0305a.dsf,0305dre«.dlf
"DVDR" ratios the transformed sample spectrum against the
background.
(v) ABSB 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 KVB/Analect Procedure -- In either DOS
(FX-70) or Windows version (FX-80) use the "Extract" command
directly on the interferogram.
(i) EXTRACT CTS0305«.ai£,0305dr««.aif,1,16384
"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 Grains™ 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.
Deeired -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 right,
and the ZPD burst appears near the left end of the trace, omit
this step.
In the -Aritnmetic/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:«»-«»(*0,«N)+50
(iv) Run ICOMPUT1.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
"M":)
First: M
Zero Fill: None
Phasing: User
Points: 1024
Calculate
Last: 0 Type: Single Beam
Apodization: (as desired)
Interpolation: Linear
Phase:
(v) As in step (iii), in the "Arithmetic/Calc' menu item
enter and then run the following commands (refer to Table 1 for
appropriate 'FILE,- which may be in a directory other than
"c:\mdgrams.•)
•etffp 7898.8805, 0 : loadspc "c: \mdgraM \ FIH" : #2-#s+#2
7vi) Use 'Page Op- to activate file #2, and then use the
-File/Save A«' menu item with an appropriate file name to save
the result.
D-95
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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- 5 .05 (16)
crs-ttst
RMSS=RMSD in the ich analytical region in subtracted result, test
CTS minus CTS standard.
n=number of data points per cm"1. Exclude zero filled points.
FFUt &=The upper and lower limits (cm"1), respectively, of the
FFI/L analytical region.
A, _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
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D-98
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
NSPS TEST METHOD
METHOD 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 Systems. The total equipment required for the determination
of the gas concentration. The system consists of the following major subsystems:
2.1.1 Sample 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 and 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 Measurement Branch 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
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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 40 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 Mid-level Calibration Gas. An organic calibration gas with a concentration
equivalent to 45 to 55 percent of the applicable span value.
4.5 High-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 80 to 90 percent of the applicable span value.
5. Measurement Systen 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 Sanple 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
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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 Tine 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.
E<5' 25A-1
Where:
cc = Organic concentration as carbon, ppmv.
cn>«ai= Organic concentration as measured, ppmv.
K = Carbon equivalent correction factor.
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EMTIC TM-25A EMTIC NSPS TEST METHOD
K = 2 for ethane.
K = 3 for propane.
K = 4 for butane.
K = Appropriate response factor for other organic calibration
gases.
9. Bibliography
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
Probe
Heated
Sample
Line
Calibration
Valve
Pump
Stack
Figure 25A-1. Organic Concentration Measurement System.
D-104
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D-4 EPA DRAFT METHOD 205
D-105
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D-106
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EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
TEST METHOD
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:
I. 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 Dilution Systems
for Field Instrument Calibrations
1. INTRODUCTION
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 Principle. 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 Dilation Systen. 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 Emission Measurement Branch EMTIC TM-205
Technical Support Division, OAQPS, EPA
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EMTIC TM-205 EMTIC NESHAP TEST METHOD
2.1.1 The gas dilution system shall be recalibrated once per calendar year using
NIST-traceable primary flow standards with an uncertainty <0.25 percent. A label
shall be affixed at all times to the gas dilution system listing the date of the
most recent calibration, the due date for the next calibration, and the person
or manufacturer who carried out the calibration. Follow the manufacturer's
instructions for the operation and use of the gas dilution system. A copy of the
manufacturer's instructions for the operation of the instrument, as well as the
most recent recalibration documentation shall be made available for the
Administrator's inspection upon request.
2.1.2 Some manufacturers of mass flow controllers recommend that flow rates
below 10 percent of flow controller capacity be avoided; check for this
recommendation and follow the manufacturer's instructions. One study has
indicated that silicone oil from a positive displacement c ,mp produces an
interference in SO2 analyzers utilizing ultraviolet flue . aence; follow
laboratory procedures similar to those outlined in Section 1 in order to
demonstrate the significance of any resulting effect on instru. - performance.
2.2 High-Level Supply Gas. An EPA Protocol calibration gas is _• -2commended, due
to its accuracy, as the high-level supply gas.
2.3 Mid-Level Supply Gas. An EPA Protocol gas shall be used as an independent
check of the dilution system. The concentration of the mid-level supply gas
shall be within 10 percent of one of the dilution levels tested in Section 3.2.
3. PERFORMANCE TESTS
3.1 Laboratory Evaluation (Optional). If the gas dilution system is to be used
to formulate calibration gases with reactive compounds (Test Methods 15, 16, and
25A/25B (only if using a calibration gas other than propane during the field
test) in 40 CFR Part 60, Appendix A), a laboratory certification must be
conducted once per calendar year for each reactive compound to be diluted. In
the laboratory, carry out the procedures in Section 3.2 on the analyzer required
in each respective test method to be laboratory certified (15, 16, or 25A and 25B
for compounds other than propane) . For each compound in which the gas dilution
system meets the requirements in Section 3.2, the source must provide the
laboratory certification data for the field test and in the test report.
3.2 Field Evaluation (Required). The gas dilution system shall be evaluated at
the test site with an analyzer or monitor chosen by the source owner or operator.
It is recommended that the source owner or operator choose a precalibrated
instrument with a high level of precision and accuracy for the purposes of this
test. This method is not meant to replace the calibration requirements of test
methods. In addition to the requirements in this method, all the calibration
requirements of the applicable test method must also be met.
3.2.1 Prepare the gas dilution system according to the manufacturer's
instructions. Using the high-level supply gas, prepare, at a minimum, two
dilutions within the range of each dilution device utilized in the dilution
system (unless, as in critical orifice systems, each dilution device is used to
make only one dilution; in that case, prepare one dilution for each dilution
device). Dilution device in this method refers to each mass flow controller,
critical orifice, capillary tube, positive displacement pump, or any other device
which is used to achieve gas dilution. 3.2.2 Calculate the predicted
concentration for each of the dilutions based on the flow rates through the gas
dilution system (or the dilution ratios) and the certified concentration of the
high-level supply gas.
3.2.3 Introduce each of the dilutions from Section 3.2.1 into the analyzer or
monitor one at a time and determine the instrument response for each of the
dilutions.
3.2.4 Repeat the procedure in Section 3.2.3 two times, i.e., until three
injections are made at each dilution level. Calculate the average instrument
response for each triplicate injection at each dilution level. No single
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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-110
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For Presentation at the Air & Waste Management Association's 90th Annual Meeting
& 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
Rho 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 (FTIR) 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 HC1 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, COj, SOj, 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 urn) 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
mirror. 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 (CzHO . For high temperature spectra, the EPA library interferograms
ctsOl 15a.aif and bkgOl I5a.aif were de-resolved to the appropriate spectral resolution (either 1 or 2 cm ')
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"1 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 SFS was spiked
as when the HC1 was spiked.
Quantitative Analysis
FTIR 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://lnfo.arnold.af.rruVepa/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 "4FTT" 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 "4FIT" 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 "4FTT," 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 4o 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 4o 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
"4FIT" 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 "4FTT1 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 "4FTr" 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 "4FTT' 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 C2H4 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
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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 FTER 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
FTTR 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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97-MP74.05
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. Soectrosc. 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. Spectrosc. 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 Spectroscopy. John Wiley and Sons,
New York, 1986, ISBN 0-471-09902-3.
9. G. M. Plummcr 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 f K)
16 293
Run 3 (Figure 3)
Run2 (Figure 2)
20 293
20 393
40 293
40 393
"""""""^^""""""""l
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
— — •— — — . __
FP region
Result (m) % uncert.
6.7 1.3
11.3 1.6
14.3 22
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 HCI 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 "4FTT"
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 1
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)/4FTT.
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
Unspiked
Run Average =
Statistical
Results
HC1 ppm
SD =
P —
RSD=
Bias =
t =
d i (d ,)2
9.68 52.561
2.093
0.491
3.7
•0.088
0.12
HC1 ppm
62.14 *
SD =
SDp^.
Exp Cone =
CF =
Spiked
4.74
1.466
1.807
5.05
1.02
(d,)1
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
HC1 ppm
45.88 *
SD =
F =
RSD=
Bias =
t =
d i (d i)2
8.62 34.242
1.689
0.628
3.7
.0.070
0.11
Spiked
HC1 ppm
50.86 *
SD =
SDpooled =
Exp Cone =
CF =
di
3.51
1.338
1.524
5.05
1.01
(d,)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.
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Figure 1. Extractive sampling system.
to
<=>
v«*i n
Healed
Sani|ile Manlluld
Flow meter
Uiiheatiid Lint:
Heated Line:
-------
APPENDIX E
PROCESS DATA
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This process description was prepared by ECR Incorporated and was provided to MRI by
the Emission Measurement Center. The process description was included in this report without
review by MRI.
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E-2
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PROCESS DESCRIPTION FOR CARY (WEST RALEIGH) FACILITY
Facility
The Construction Asphalt Concrete Production Facility in
Gary, North Carolina, has been in operation since 1987. It is a
parallel flow, continuous drum mix process. The dryer/mixer is
an ASTEC drum (8 ft. by 45 ft.), with a rated capacity of 325
tons per hour. The plant has the capability of producing up to
14 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 parallel flow continuous drum mix process, virgin
aggregate of various sizes is fed to the dryer/mixer by cold feed
controls in proportions dictated by the final mix specifications.
Aggregate is delivered by conveyor belt to the dryer section of
the drum, entering at the same end as the burner (hence, the
descriptor "parallel* flow) . The aggregate is heated and dried
by the high temperatures in the dryer and then moves into the
mixer section where it is coated with liquid asphalt cement, and
conditioner (if used). Liquid asphalt cement and conditioner are
delivered to the mixer by a variable flow pump that is
electronically linked to the aggregate feed weigh scales. The
hot aggregate mixture is also combined with RAP (if any) and
recycled dust from the control system. The resulting asphalt
concrete mixture is discharged from the end of the drum mixer and
conveyed to storage silos for delivery to trucks.
There are six cold storage bins and three hot mix storage
silos at the Gary facility. The hot mix storage silo
capacity is 200 tons each, for a total of 600 tons. There are
two screens for aggregate sizing and two 25,000 gallon heated
asphalt cement storage vessels, for a total asphalt cement
capacity of 50,000 gallons (125 tons). The plant usually uses
natural gas for all its process fuel needs; however, during the
source tests No. 2 oil, the back-up fuel, was used in the drum
mixer. The amount of energy needed from the fuel for the asphalt
production process is 300,000 BTU per ton of asphalt produced.
The hot gas contact time, i.e. the time from when the aggregate
enters the dryer to when it exits the coater, is between,
E-3
-------
approximately, 3 Co 4 minutes. Surface mixes are closer to 3
minutes and base mixes are closer to 4 minutes.
The Gary facility uses an asphalt cement (AC) called
AC-20, obtained from Citgo of Wilmington, North Carolina An
anti-strip conditioner, called Ad-Here (from Arr-Maz), is
sometimes used; antistrip is required for all NC DOT jobs.
For particulate matter (PM) control, the facility uses a
knockout box as a primary control and a fabric filter as a
secondary control. The fabric filter is an ASTEC Pulse-Jet,
equipped with 780 14-ounce Nomex bags; it is operated with an
air-to-cloth ratio of approximately 5 feet per minute. The
process gas exits the drum and proceeds through the knockout box
into a 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 Teats
EPA source tests were performed at : Gary facility on-
August 27, 28, and 29, 1997. The source testing took place at
the inlet and outlet of the fabric filter. Process data were
taken at 15-minute intervals during the entire "test period,*
i.e. during 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.
For the three test dates (August 27, 28, and 29, 1997), the
average asphalt concrete production rates per test run were 201,
199, and 163 tons per hour (tph), respectively, corresponding to
total production of 1,039, 1,242, and 839 tons. During the first
two test runs (August 27 and 28), a surface asphalt coating that
included RAP was produced; during the third test run (August 29),
a surface coating (accounting for 73% of the total asphalt
concrete produced) and a binder coating (accounting for 27% of
total production) were produced, both without RAP. A high sulfur
No. 2 fuel oil was used for fuel in the production process during
the tests. No conditioner was used during the tests. No visible
emissions were observed by EC/R Inc. personnel during the source
tests.
Table 1 that follows summarizes the operating conditions
observed during the EPA source test periods at Gary
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-4
-------
TABLE 1. PLANT OPERATING CONDITIONS DURING
AUGUST 27, 28, AND 29, 1997
SOURCE TESTS,
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
Average"
Range
Total Used, tons
RAP
Use rate, tph
Average13
Range
Total Used, tons
Asphalt Cement
Use rate, tons/hr
Average13
Range
Total Used, tons
Conditioner
Test Run / Test Date
Run 1
08/27/97
surface mix,
with RAP
(BCSC RI-2)
201
149-212
1,039
301
290-330
153
113-161
788
36
18-40
197
12.3
9.1-12.9
54
none
Run 2
08/28/97
surface mix,
with RAP
(BCSC RI-2)
199
192-206
1,241
299
284-321
151
145-154
943
36
30-43
235
12.1
11.7-12.6
64
none
Run 3
08/29/97
surface mix,
no RAP
(BCSC 1-2} ;
and binder
(BCBC, Type H)
163
130-195
839
303
286-352
154
122-183
839
none
9.2
6.8-12.1
51
none
(Continued)
E-5
-------
TABLE 1. (continued)
Process Data
Fabric Filter
Operation5
Temperature , °F
Inlet
Outlet
Pressure Drop,
inches water
Average"
Range
Fuel
Use Rate,c gph
Total Used, gal
Visible Emissions
Test Run / Test Date
Run 1
08/27/97
344
271
0.9
0.8-1.2
340
1,906
none
Run 2
08/28/97
343
283
0.9
0.1-1.1
344
2,305
none
Run 3
08/29/97
325
269
1.2
0.5-2.0
266
1,620
none
BCSC, Type 1-2
BCSC, Type RI-2
BCBC, Type H
bituminous concrete, surface
coarse
bituminous concrete, surface
coarse, with RAP
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.
Fuel use rate was calculated from the total fuel used during
the time interval.
E-6
-------
TABLE 2.
ASPHALT MIX SPECIFICATIONS
Product
Material
Amount
Surface Coating
(BCSC, Type 1-2)
78-M
regular screenings
classified screenings
asphalt cement
22% aggregate
34% aggregate
44% aggregate
6.4% mix
Surface Coating, with
RAP (BCSC, Type RI-2)
78-M
screenings
classified screenings
RAP
asphalt cement total
additional
from RAP
17% aggregate
23% aggregate
42% aggregate
18% aggregate
6.4% mix
5.2% mix
0.9% mix
Binder (BCBC, Type H)
78-M
#67
regular screenings
wet screenings
asphalt cement
19% aggregate
48% aggregate
23% aggregate
10% aggregate
4.6% mix
TABLE 3.
FUEL SPECIFICATIONS
Fuel Type
High Sulfur
No. 2 Fuel Oil
Characteristic ( a )
flash point
sulfur
API index
125°F
<500 mg/kg
(0.05%)
33 .2
Descriptor (s)
dyed diesel fuel not
for on-road use
E-7
-------
TABLE 4. SPECIFICS OF PLANT OPERATION DURING EPA SOURCE TESTS AT
Parameter
Test Run / Test Date
Run 1
08/27/97
Run 2
08/28/97
Run 3
OB/29/97
Test Period
0940-1516
0746-1428
0809-1413
Plant Shut Downs*
(with approximate
duration)
1002 (5 min)
1140 (6 min)
1402 (10 min)
0901 (8 min)
1110 (18 min)
1355 (12 min)
1212 (9 min)
1242 (41 min)
Plant Production Rate
Change(s)
W
oo
1430-1515: mix
rate slowed down
from nominally
200 to 150 tph
none
1007-1222: mix rate
increased from
nominally 150 to
200 tph
1237-1422: mix rate
decreased from
nominally 200 to
130 tph
Product Changes
none
none
0807-0822 and 1022-
1422: 1-2 produced
(642 tons)
0837-1007: binder
produced (237 tons)
The shutdown at 1242 during Run 3 was put into effect to avoid overfilling of the
silos with asphalt concrete mix; all other shutdowns were due to aggregate clogging
in the conveyor system.
-------
Appendix A: Process Data
Gary
Test Run 1
Test Date: August 27, 1997
Total Test Time: 5.6 hrs
Time
0940
1000
1015
1030
1045
1100
1115
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1430
1445
1500
1516
Event
*
*
*
*
Product
Type
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
Asphalt Concrete
Production
Rate
(TPH)
210
209
208
209
210
209
208
209
208
211
209
210
211
212
209
207
211
206
211
149
151
149
Total
(tons)
547
600
631
684
736
788
840
892
928
976
1,028
1,080
1,133
,185
,238
,290
,343
,422
,474
,511
,549
1,586
Asphalt
Temp.
(oF)
297
297
309
303
296
310
301
301
320
304
301
296
292
330
292
305
293
290
297
296
292
308
Aggregate Use
Rate
(TPH)
159
159
159
158
159
158
158
158
158
159
159
159
159
160
160
159
161
158
161
113
114
113
Total
(tons)
418
457
481
521
560
600
640
679
707
743
782
822
862
902
942
981
,022
,081
,120
,149
,177
,206
RAP Use
Rate
(TPH)
39
37
37
38
38
39
38
39
37
40
37
38
39
39
37
36
37
35
37
18
28
26
Total
(tons)
102
112
118
128
138
147
157
167
174
183
193
203
213
223
233
243
253
268
278
285
292
299
Asphalt
Cement Use
Rate
(TPH)
12.9
12.7
12.6
12.8
12.7
12.6
12.7
12.7
12.7
12.9
12.8
12.8
12.9
12.9
12.7
12.5
12.9
12.8
12.9
9.2
9.2
9.1
Total
(tons)
28
31
32
35
38
40
43
46
48
50
53
55
58
61
64
66
69
73
76
78
80
82
Calculated
Conditioner 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
Total
(tons)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
w
-------
Appendix A: Process Data
Gary
Test Run 1
Test Date: August 27, 1997
Total Test Time: 5.6 hrs
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Asphalt Concrete
Production
Rate
(TPH)
201
21
149
212
Total
(tons)
1,039
Asphalt
Temp.
(oF)
301
9
290
330
Aggregate Use
Rate
(TPH)
153
16
113
161
Total
(tons)
788
RAP Use
Rate
(TPH)
36
5
18
40
Total
(tons)
197
Asphalt
Cement Use
Rate
(TPH)
12.3
1.2
9.1
12.9
Total
(tons)
54
Calculated
Conditioner Use
Rate
(TPH)
0
0
0
0
Total
(tons)
0
*See Table 4 for a description of these events.
-------
Appendix A: Process Data
Gary
Test Run 1
Test Date: August 27, 1997
Total Test Time: 5.6 hrs
Time
0940
1000
1015
1030
1045
1100
1115
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1430
1445
1500
1516
Event
*
*
*
Product
Type
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
Fabric Filter
Inlet
Temp.
(oF)
345
340
365
350
340
350
350
350
330
350
340
340
340
335
335
350
340
350
330
350
345
350
Outlet
Temp.
(oF)
270
270
270
285
270
270
270
280
235
275
280
270
270
270
270
270
270
260
280
270
275
285
Pressure
Drop
(in. H2O)
0.8
0.8
0.8
0.9
0.9
0.9
0.9
0.9
1.2
1.1
1.0
1.0
1.0
1.0
1.0
0.8
0.8
0.9
1.0
1.0
1.0
1.0
Fuel
Use
(gal)
77564
77656
77719
77815
77911
78003
78113
78201
78260
78375
78448
78577
78648
78749
78837
78923
79020
79154
79258
79325
79404
79470
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
-------
Appendix A: Process Data
Gary
Test Run 1
Test Date: August 27, 1997
Total Test Time: 5.6 hrs
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Fabric Filter
Inlet
Temp.
(oF)
344
8
330
365
Outlet
Temp.
(oF)
271
10
235
285
Pressure
Drop
(in. H20)
0.9
0.1
0.8
1.2
Fuel
Use
(gal)
1,906
Visible
Emissions
*See Table 4 for a description of these events.
W
-------
Appendix A: Process Data
Gary
Test Run 2
Test Date: August 28, 1997
Total Test Time: 6.7 hrs
Time
0746
0800
0815
0830
0845
0900
0915
0930
0945
1000
1015
1030
1045
1100
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1428
Event
*
*
*
Product
Type
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
Asphalt Concrete
Production
Rate
(TPH)
194
193
192
195
197
195
198
206
200
199
198
199
198
204
199
203
201
201
203
198
204
203
202
195
197
198
Total
(tons]
86
116
164
212
261
310
341
390
440
490
540
589
639
689
755
805
856
906
957
1007
1058
1109
1159
1209
1278
1327
Asphalt
Temp.
(oF)
295
298
294
288
299
306
300
285
299
299
299
302
301
297
296
321
307
309
304
303
284
296
305
302
293
302
Aggregate Use
Rate
(TPH)
146
145
147
148
149
149
150
150
151
151
151
151
151
153
152
153
154
152
154
153
154
154
153
152
150
150
Total
(tons)
66
90
126
163
200
237
260
298
336
372
411
449
487
525
575
613
651
689
728
766
805
843
881
920
972
1009
RAP Use
Rate
(TPH)
37
36
34
36
36
34
36
43
37
36
35
36
35
39
35
38
35
37
37
32
38
37
36
30
35
36
Total
(tons)
15
21
30
39
48
57
63
73
82
92
101
110
120
129
142
152
161
171
180
190
200
209
219
228
241
250
Asphalt
Cement Use
Rate
(TPH)
11.7
11.8
11.7
11.7
12.0
12.0
12.1
12.6
12.2
12.1
12.2
12.1
12.2
12.3
12.2
12.2
12.2
12.2
12.3
12.1
12.3
12.3
12.2
12.0
12.0
12.0
Total
(tons)
4
6
8
11
13
16
17
20
22
25
27
30
33
35
38
41
44
46
49
51
54
56
59
62
65
68
Calculated
Conditioner 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
0
0
0
Total
(tons)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
w
-------
Appendix A: Process Data
Gary
Test Run 2
Test Date: August 28, 1997
Total Test Time: 6.7 hrs
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Asphalt Concrete
Production
Rate
(TPH)
199
4
192
206
Total
(tons)
1,241
Asphalt
Temp.
(oF)
299
7
284
321
Aggregate Use
Rate
(TPH)
151
2
145
154
Total
(tons)
943
RAP Use
Rate
(TPH)
36
2 .
30
43
Total
^tonsl
235
Asphalt
Cement Use
Rate
(TPH)
12.1
0.2
11.7
12.6
Total
(tons)
64
Calculated
Conditioner Use
Rate
(TPH)
0
0
0
0
Total
(tons)
0
w
*See Table 4 for a description of these events.
-------
Appendix A: Process Data
Gary
Test Run 2
Test Date: August 28, 1997
Total Test Time: 6.7 hrs
Time
0746
0800
0815
0830
0845
0900
0915
0930
0945
1000
1015
1030
1045
1100
1130
1145
1200
1215
1230
1245
1300
1315
1330
1345
1415
1428
Event
*
*
*
Product
Type
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
RI-2
Fabric Filter
Inlet
Temp.
(oF)
345
340
340
330
340
350
350
330
340
350
350
350
345
350
350
360
350
350
350
340
325
335
335
340
330
340
Outlet
Temp.
(oF)
340
260
270
255
260
270
280
285
285
280
290
285
280
290
280
300
295
290
295
285
275
275
285
290
280
275
Pressure
Drop
(in. H2O)
0.9
0.8
0.9
0.9
0.8
0.9
.0
.0
.0
.0
.0
.0
.0
.0
.1
.0
.0
.0
.0
.0
.0
0.5
0.5
0.5
0.1
0.9
Fuel
Use
(eal)
79777
79861
79947
80048
80118
80224
80284
80374
80485
80570
80655
80763
80854
80943
81068
81170
81261
81364
81461
81529
81611
81692
81776
81864
81978
82082
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
en
-------
Appendix A: Process Data
Gary
Test Run 2
Test Date: August 28, 1997
Total Test Time: 6.7
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Fabric Filter
Inlet
Temp.
(oF)
343
8
325
360
Outlet
Temp.
(oF)
283
16
255
340
Pressure
Drop
(in. H20)
0.9
0.2
0.1
1.1
Fuel
Use
(gal)
2,305
Visible
Emissions
*See Table 4 for a description of these events.
M
ON
-------
Appendix A: Process Data
Gary
Test Run 3
Test Date: August 29, 1997
Total Test Time: 6.1 hrs
Time
0809
0822
0837
0852
0907
0922
0937
0952
1007
1022
1037
1052
1107
1122
1137
1152
1207
1222
1237
1325
1337
1352
1407
1413
Event
*
*
*
Product
Type
1-2
1-2
Binder
Binder
Binder
Binder
Binder
Binder
Binder
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
Asphalt Concrete
Production
Rate
JTPH)
130
160
150
153
154
154
155
155
188
185
194
193
195
194
194
193
194
193
132
130
130
130
131
130
Total
Jtons^_
28 \
66
102
139
175
212
249
285
329
373
419
464
509
555
'600
645
691
709
749
772
788
818
819
867
Asphalt
Temp.
(oF)
344
293
310
296
296
295
296
300
297
300
291
300
302
286
288
289
297
302
334
352
293
292
307
311
Aggregate Use
Rate
iTPHL
122
150
143
146
147
147
148
148
179
177
182
181
183
182
182
181
182
182
124
122
122
122
123
123
Total
(tons)
28
66
102
138
175
212
249
285
329
373
419
464
509
555
600
645
691
709
749
772
788
818
849
867
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
0
Total
{tons]
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
Asphalt
Cement Use
Rate
(TPH)
8.1
9.9
6.8
7.1
7.0
7.0
7.2
7.2
8.7
8.4
12.0
12.0
12.1
12.0
12.0
12.0
12.0
11.8
8.2
8.0
8.0
8.1
8.1
8.1
Total
(tons]
1
4
6
8
9
11
13
15
17
19
22
25
28
31
34
37
40
41
44
45
46
48
50
52
Calculated
Conditioner 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
0
Total
(tons)
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
-------
Appendix A: Process Data
Gary
Test Run 3
Test Date: August 29, 1997
Total Test Time: 6.1 hrs
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Asphalt Concrete
Production
Rate
(TPH)
163
26
130
195
Total
(tons)
839
Asphalt
Temp.
(oF)
303
17
286
352
Aggregate Use
Rate
(TPH)
154
25
122
183
Total
(tons)
839
RAP Use
Rate
(TPH)
0
0
0
0
Total
(tons)
0
Asphalt
Cement Use
Rate
(TPH)
9.2
2.0
6.8
12.1
Total
ftonsl
51
Calculated
Conditioner Use
Rate
(TPH)
0
0
0
0
Total
(tons)
0
w
oo
*See Table 4 for a description of these events.
-------
Appendix A: Process Data
Gary
Test Run 3
Test Date: August 29, 1997
Total Test Time: 6.1 hrs
Time
0809
0822
0837
0852
0907
0922
0937
0952
1007
1022
1037
1052
1107
1122
1137
1152
1207
1222
1237
1325
1337
1352
1407
1413
Event
*
*
*
Product
Type
1-2
1-2
Binder
Binder
Binder
Binder
Binder
Binder
Binder
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-2
Fabric Filter
Inlet
Temp.
(oF)
365
320
335
320
320
320
325
330
320
290
310
320
320
310
310
310
320
310
360
370
320
320
335
335
Outlet
Temp.
(oF)
285
265
285
270
270
270
270
270
270
270
260
260
270
260
260
260
265
250
290
270
260
260
280
280
Pressure
Drop
iiILH2QL
1.0
2.0
1.0
1.2
.2
.1
.1
.1
.0
.0
.2
.5
.3
.2
.2
.2
.5
.9
1.9
0.5
0.5
0.5
1.0
1.0
Fuel
Use
(gal)
83174
83250
83317
83394
83444
83508
83572
83638
83711
83784
83872
83927
84055
84171
84209
84305
84404
84434
84512
84556
84600
84657
84728
84794
Visible
Emissions
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
none
w
Co
-------
Appendix A: Process Data
Gary
Test Run 3
Test Date: August 29, 1997
Total Test Time: 6.1 hrs
Time
Total
Mean
St. Dev
Min
Max
Event
Product
Type
Fabric Filter
Inlet
Temp.
(oF)
325
18
290
370
Outlet
Temp.
(oF)
269
9
250
290
Pressure
Drop
(in. H2O)
1.2
0.4
0.5
2.0
Fuel
Use
(gal)
1,620
Visible
Emissions
*See Table 4 for a description of these events.
------- |