United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA - 454/R-99-027
July 1999
Air
&EPA
Asphalt Roofing Industry
Fourier Transform Infrared Spectroscopy
Modified Bitumen
U.S. Intec
Port Arthur, Texas
-------
Emissions Test at an Asphaltic Roofing Manufacturer
Test Report
U.S. Intec, Inc.
Port Arthur, Texas
Prepared for
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Emission Measurement Center (MD-19)
Mr. Michael L. Toney
Work Assignment Manager
EPA Contract No.68-D-98-027
Work Assignment 2-11
MRI Project No. 4951-11-04
[KTd^LJ ^^1 July29,1999
-------
PREFACE
This test report was prepared by Midwest Research Institute (MRI) for the U. S.
Environmental Protection Agency (EPA) under EPA Contract No. 68D-98-027, Work
Assignment No. 2-11. Mr. Michael Toney is the EPA Work Assignment Manager (WAM).
Dr. Thomas Geyer is the MRI Work Assignment Leader (WAL). The field test was performed
under EPA Contract No. 68-D2-0165, Work Assignment No. 4-21. A draft report was prepared
under EPA Contract No. 68-W6-0048, Work Assignment No. 2-08. Mr. Toney was also the
WAM for the previous work assignments. Dr. Geyer was the MRI WAL for Work Assignment
No. 4-21 and the Task Leader for Work Assignment No. 2-08. Mr. John Hosenfeld was the MRI
WAL for Work Assignment No. 2-08.
MIDWEST RESEARCH INSTITUTE
Hosenfeld
Program Manager
Approved:
•^leffShular
Director, Environmental Engineering Department
July 29, 1999
111
-------
TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1
1.1 BACKGROUND 1
1.2 PROJECT SUMMARY 1
1.3 KEY PROJECT PERSONNEL 3
2.0 PROCESS DESCRIPTION AND TEST LOCATIONS 4
2.1 PROCESS DESCRIPTION 4
2.2 CONTROL EQUIPMENT DESCRIPTION 4
2.3 SAMPLING AND MONITORING LOCATIONS 7
2.3.1 Thermal Oxidizer Inlet Duct (El) 7
2.3.2 Thermal Oxidizer Outlet Stack (E2) 8
2.3.3 Modified Bitumen Holding Tank Exhaust Outlet E19B (E3) 8
2.3.4 Modified Bitumen Holding Tank Exhaust Outlet E1B (E4) 8
2.3.5 Modified Bitumen Mixing Tank Exhaust Outlet E17B (E5) 10
2.3.6 Modified Bitumen Mixing Tank Exhaust Outlet E2B (E6) 10
2.3.7 Coater Vent Stack E10S (E7) 10
2.3.8 Coater Vent Stack E20S (E8) 11
3.0 RESULTS 12
3.1 SCHEDULE 12
3.2 FIELD TEST PROBLEMS AND CHANGES 12
3.3 FTIR RESULTS 13
3.3.1 Thermal Oxidizer Inlet and Outlet 16
3.3.2 APP and SBS Coaters 16
3.3.3 APP and SBS Mixing Tanks 16
3.3.4 APP and SBS Holding Tanks 16
3.3.5 Results from Spiked Samples 18
3.4 METHOD 25A RESULTS 20
4.0 TEST PROCEDURES 25
4.1 SAMPLING SYSTEM DESCRIPTION 25
4.1.1 Sample System Components 25
4.1.2 Sample Gas Stream Flow 26
4.2 SAMPLING PROCEDURES 26
4.3 FTIR SAMPLES 28
4.3.1 Batch Samples 28
4.3.2 Continuous Sampling 28
4.4 ANALYTE SPIKING 29
4.4.1 Analyte Spiking Procedures 29
4.4.2 Analysis of Spiked Results 30
4.4.3 Determination of Percent Recovery 30
-------
TABLE OF CONTENTS (continued)
4.5 ANALYTICAL PROCEDURES 31
4.5.1 Program Input 32
4.5.2 EPA Reference Spectra 32
4.6 FTIR SYSTEM 34
4.7 CONTINUOUS EMISSIONS MONITORING FOR TOTAL
HYDROCARBONS (THC) 34
4.7.1 Components 35
5.0 SUMMARY OFQA/QC PROCEDURES 36
5.1 SAMPLING AND TEST CONDITIONS 36
5.2 FTIR SPECTRA 37
5.3 METHOD 25A '. 39
5.3.1 Initial Checks :... 39
5.3.2 Daily Checks 39
6.0 REFERENCES 40
APPENDIX A. FIELD DATA SHEETS FOR STACK FLOW MEASUREMENTS
APPENDIX B. THC ANALYZER DATA
APPENDIX C. THC CALIBRATION RECORDS
APPENDK D. FTIR FIELD DATA RECORDS
APPENDIX E. FTIR ANALYTICAL RESULTS
APPENDIX F. EPA METHOD 320 AND EPA FTIR PROTOCOL
VI
-------
LIST OF FIGURES
Page
Figure 1. Modified bitumen operations-U.S. Intec, Inc., Port Arthur, Texas 5
Figure 2. Coater Operations-US. Intec, Inc., Port Arthur, Texas 6
Figure 3. Thermal oxidizer inlet and outlet sampling locations 9
Figure 4. Extractive sampling system 27
LIST OF TABLES
Page
TABLE 1. TEST MATRIX 2
TABLE 2. PROJECT PERSONNEL 3
TABLES. SUMMARY OF FTIR RESULTS AND MASS EMISSIONS RATES... 14
TABLE 4. UNCERTAINTY RESULTS FOR SOME HAP COMPOUNDS
AT THE COATER STACKS 17
TABLES. POSSIBLE DETECTS OF SOME ORGANIC SPECIES 18
TABLE 6. SUMMARY OF ASPHALT ROOFING FTIR P-XYLENE SPIKE
RESULTS 19
TABLE 7. p-XYLENE SPECTRAL BAND AREAS. COMPARISON OF EPA
LIBRARY SPECTRA TO SPECTRA OF P-XYLENE CYLINDER
STANDARD .., 19
TABLES. SUMMARY OF THERMAL OXIDIZER INLET/OUTLET THC
DATA 21
TABLE 9. SUMMARY OF SBS AND APP MIXING AND HOLDING TANK
THC DATA 22
TABLE 10. SUMMARY OF SBS AND APP COATER ROOF STACK THC
DATA 23
TABLE 11. VERSION 1 OF THE PROGRAM INPUT DATA 33
TABLE 12. PROGRAM INPUT FOR ANALYSIS OF CTS SPECTRA AND PATH
LENGTH DETERMINATION 34
TABLE 13. RESULTS OF THE CTS PATH LENGTH DETERMINATION 38
vn
-------
1.0 INTRODUCTION
1.1 BACKGROUND
A "Request for Emissions Testing at Four Asphalt Roofing and Processing Facilities"
was submitted by the U.S. EPA Emission Standards Division (BSD), Minerals and Inorganic
Chemicals Group (MICG) to the Emission Measurement Center (EMC). The Emission
Measurement Center directed Midwest Research Institute (MRI) to conduct emissions testing at
asphalt roofing plants. This report presents results of MRI's FTIR and Method 25A testing
conducted at U. S. Intec in Port Arthur, Texas. The field measurements were performed in
September 1997 under several test conditions for both controlled and uncontrolled emissions.
1.2 PROJECT SUMMARY
The purpose of this test program was to obtain uncontrolled and controlled HAP
emissions data from asphalt roofing and processing plants to support a national emission
standard for hazardous air pollutants. Specifically, the objective was to measure HAPs in several
processes. An additional goal was to measure other compounds that could be detected with the
FTIR system.
Emissions were measured at both the inlet and outlet of the incinerator (thermal oxidizer)
used to control emissions from mixing and holding tanks. Additionally, uncontrolled emissions
from individual mixing and holding tanks and coaters were measured. A total of eight sampling
locations were tested, noted as El through E8 in Table 1. Midwest Research conducted FTIR
testing using EPA Method 320, and hydrocarbon testing using EPA Method 25A. Eastern
Research Group, Inc. (ERG) performed manual methods at the thermal oxidizer inlet and outlet.
Table 1 shows the test matrix and summarizes the tests performed for MRI's portion of the field
testing.
Three test runs were conducted by alternating sampling at the inlet and outlet of the
thermal oxidizer. The sampling time for the FTIR and THC methods (approximately 4 hr per
run) coincided with ERG's manual sampling periods.
Similarly, the two coater vents (roof stacks) for both the SBS and APP product lines were
tested during three separate runs each (approximately 1 hr each). Finally, one test run each
(approximately 1 hr) was conducted on both the holding and mixing tanks for both the APP and
SBS product lines.
1
-------
TABLE 1. TEST MATRIX
Date
9/22
9/23
9/22
9/23
9/26
9/26
9/25
9/25
9/24/97
9/24 &
9/25
Emission
point
El
E2
E3
E4
E5
E6
E7
E8
Description
Holding and Mixing Tank
Collection Header
Holding and Mixing Tank
Collection Header
Modified Bitumen
Holding Tank
Modified Bitumen
Holding Tank
Modified Bitumen
Mixing Tank
Modified Bitumen
Mixing Tank
Coater
Coaler
Sampling location
Thermal Oxidizer Inlet
Thermal Oxidizer
Outlet
Tank Outlet
(SBS Tank 3)
Tank Outlet
(APPTankl)
Tank Outlet
(SBS Tank 11)
Tank Outlet
(APPTankl)
Roof Stack Outlet
(APP)
Roof Stack Outlet
(SBS)
Sample type
THC
All Gaseous HAP
THC
All Gaseous HAP
THC
All Gaseous HAP Flow
THC
All Gaseous HAP Flow
THC
All Gaseous HAP
THC
All Gaseous HAP
THC
All Gaseous HAP
THC
All Gaseous HAP
Sampling
method
Method 25A
FTIR
Method 25A
FTIR
Method 25A
FTIR
Methods 1-2
Method 25A
FTIR
Methods 1-2
Method 25A
FTIR
Method 25A
FTIR
Method 25A
FTIR
Method 25A
FTIR
No. of
test runs
3
3
1
2a
1
1
3
3
Duration
4 hr, performed
simultaneous with
outlet test runs
4 hr, performed
simultaneous with
inlet test runs
Ihr
Ihr
Ihr
Ihr
Ihr
Ihr
ts>
a One test was performed but repeated due to sampling problems, fpr a total of two test runs.
-------
1.3 KEY PROJECT PERSONNEL
A list of the key project personnel, their organization, title, and phone numbers are
presented in Table 2.
TABLE 2. PROJECT PERSONNEL
Organization and Title
Name
Phone No.
U.S. Intec
Project Engineer
Jeff Hughes
(409) 724-7024
U. S. EPA, EMC
Work Assignment Manager
Michael L. Toney
(919) 541-5247
MRI
Work Assignment Leader
Contract No. 68-W6-0048,
Work Assignment No. 2-08
John Hosenfeld
(816)753-7600,ext1336
MRI
Work Assignment Leader
Contract No. 68-D2-0165,
Work Assignment No. 4-21
Contract No. 68D-98-027
Work Assignment 2-11
Thomas J. Geyer
(919) 851-8181, ext 3120
-------
2.0 PROCESS DESCRIPTION AND TEST LOCATIONS
The U.S. Intec facility in Port Arthur, Texas, was selected as a test site representative of
the modified bitumen production process in the asphalt roofing industry. The site uses the
modified bitumen process using atactic polypropylene (APP) or styrene-butadiene-styrene (SBS).
2.1 PROCESS DESCRIPTION
The facility produces rolled roofing products by saturating a polyester substrate and a
fiberglass substrate with modified bitumen in two separate production lines(APP or SBS). A
flow diagram of the process is included in Figures 1 and 2. Sampling points, as noted earlier in
Table 1, are designated as El through E8. Both the APP and SBS substrates enter their
respective production lines through a web unwind stand and then go through a dry looper.
Asphalt is unloaded from tanker trucks into two 100-ton, 350°F asphalt storage tanks. Asphalt
from the storage tanks is distributed to six 10.5-ton, 400°F mixing tanks for the production line
using polyester substrate and two 10.5-ton, 390°F mixing tanks for the production line using
fiberglass substrate. Tanker trucks also unload polymer liquid into two steam-jacket storage
tanks.
Modified bitumen is produced by combining the asphalt with polypropylene and fillers in
the six mixing tanks for the line using polyester substrate. Modified bitumen is produced for the
line using fiberglass substrate by combining asphalt with SBS in one mixing tank and fillers in
the second mixing tank. The modified bitumen in the mixing tanks is transferred to two holding
tanks for the line using polyester substrate and one holding tank for the line using fiberglass
substrate before going to the respective coaters. The coaters are impregnation vats where the
substrates are saturated with the modified bitumen. Once the saturated polyester substrate leaves
the vat, it is coated with granules and talc. The saturated fiberglass substrate is coated with
granules and sand. After both products are cooled, they go through separate finish loopers and
roll winders.
The facility operates 24 hr per day from Monday morning through Friday evening (5 days
per week).
2.2 CONTROL EQUIPMENT DESCRIPTION
Emissions from the holding and mixing tanks for both SBS and APP production lines are
ducted to the thermal oxidizer. The gas stream passes through a booster fan to a cyclone
-------
Stack
Thermal
Oxidizer
Holding
Tank - APP
*—
SBS Mixing
Tank
i
— l
APP Mixing
Tank
i
Figure 1. Modified bitumen operations~U.S. In tec, Inc., Port Arthur, Texas.
-------
o\
Stack W-
Stack
SBS Coater
Roof Line
APP Coater
Figure 2. Coater operations—U.S. Intec, Inc., Port Arthur, Texas.
-------
separator where coarse paniculate matter is removed. The thermal oxidizer operated at a
temperature of 1400°F and a residence time of 0.5 seconds. Gas was moved from the thermal
oxidizer to the slack by an induced draft fan where gas temperatures were approximately 480°F,
at a nominal flow rate of 10,000 acfm (23.6 ft/sec velocity).
Emissions from holding and mixing tanks were not controlled at the locations tested, and
the coalers are not controlled, but vent to the atmosphere. Gas stream temperatures from the
mixing and holding tank outlet ducts ranged from 110° to 316°F at pressures slightly less than
atmospheric pressure. Velocity heads in these ducts were very low and required measurement
with a hot wire anemometer. Gas streams in the coater vent stacks had temperatures of approxi-
mately 90° to 110 °F and pressures above atmospheric pressure (an in of water or more).
Velocity heads in these ducts were approximately 0.60 in of water, or greater.
The water vapor content at all sampling locations except the thermal oxidizer outlet stack
was close to ambient conditions. The water vapor content in the thermal oxidizer outlet stack
was approximately 4 percent to 7 percent by volume.
2.3 SAMPLING AND MONITORING LOCATIONS
Sampling was conducted at a total of 8 different locations, noted previously as locations
El through E8 in Table 1 and Figures 1 and 2. Each of the following sections briefly describes
the sampling locations in greater detail. Sections 2.3.1 and 2.3.2 describe the inlet and outlet
locations for the thermal oxidizer, which is fed via a common duct. Sections 2.3.3 and 2.3.4
describe exhaust ducts from the individual holding tanks which feed into the common duct.
Sections 2.3.5 and 2.3.6 describe exhaust ducts from the individual mixing tanks which feed into
the common duct. Sections 2.3.7 and 2.3.8 describe ve.nt stacks for the coating processes, which
are not part of the thermal oxidizer treatment system.
2.3.1 Thermal Oxidizer Inlet Duct (El)
Thermal oxidizer inlet sampling was conducted in the common manifold (header) which
collects emissions exhausted from the mixing and holding tanks from both production lines. A
schematic drawing of the inlet sampling location is presented in Figure 3. Two 4-in ports
(nipples), 90° apart, were installed in cross-section (CS) 2 of the horizontal, circular, steel duct
for ERG's sampling and velocity traverses. A 3-in port (nipple) was installed in CS1 for the
Method 25A and 320 (FTIR) single-point sampling. Temporary scaffolding for access from the
-------
ground to the location was installed. Approximately 150 ft of sample transfer line from the
trailer was required here.
2.3.2 ThermaTOxidizer Outlet Stack (E2)
Thermal oxidizer outlet sampling was conducted in the stack immediately downstream of
the thermal oxidizer. The outlet sampling location, approximately 30 ft above ground level, is
also presented in Figure 3. The two existing 3-in ports, 90° apart, in CS4 of the circular, steel
stack were replaced with 4-in nipples and were used for ERG's sampling and velocity traverses.
A 3-in port (nipple) was installed in CS3 for the Method 25A and 320 (FTIR) single-point
sampling. Approximately 200 ft of sample transfer line from the trailer was required here.
2.3.3 Modified Bitumen Holding Tank Exhaust Outlet E19B (E3)
This sampling location is in a horizontal run of 10-in diameter steel duct (E19B)
exhausting emissions from SBS production line holding tank No. H3. One 3-in port was
installed on the side of the duct at a location directly over holding tank No. HI. The duct is
approximately 30 ft above the production room floor, just below the roof. The top of the tank is
accessible by stairs from the production room floor and a walkway. Approximately 200 ft of
sample transfer line from the trailer were required here. Only one diameter was traversed for
volumetric flow rate measurements because velocities were very low and stratification across the
gas stream was insignificant. Appendix A contains traverse point information and a sketch of the
sampling port arrangement for this location.
2.3.4 Modified Bitumen Holding Tank Exhaust Outlet E1B CEA)
This sampling location was a vertical section of 8-in diameter black iron pipe (E1B)
exhausting emissions from APP production line holding tank No. HI. The duct was right off the
top of the tank and was accessible from a permanent platform on top of the tank. One 3-in port
was installed on the side of the duct at a location such that the sampling equipment was just
outside of the handrails and supported from an overhead beam. This location was approximately
20 ft above the production room floor and accessible by stairs from the production room floor
and a walkway. Approximately 200 ft of sample transfer line from the trailer were required here.
Again, only one diameter was traversed for volumetric flow rate measurements because
velocities were very low and stratification across the gas stream was insignificant. Appendix A
-------
•v
24ft
(8D)
s^ Row Direction
J__
! PortB
1 1
(J)PortC QportA ^
1 '
i
L 3ft. J
Flow toward
observer
PortB
CS1 for Methods 25A & 320
ortA
36 in. ..D.
CS2 for Methods 5A & 23
x
X
X .
Thermal OxkJizer Inlet Duct (E1)
All ports are nominal 3 or 4-in. pipe nipples. All ports
are 5-6 in. long from outside edge to inside duct wall.
Traverse Point Distance (in.) from Inside Wall
1 1.58
2 5.26
3 10.66
4 25.34
5 30.74
6 34.42
6 ft. (2 D)
Cross-section 4 for Methods 5A & 23 (4-inch ports)
Cross-section 3 for Methods 25A & 320 (3-inch port)
PortC
24 ft. (8 D)
36 in. I.D.
| Port A
Thermal Oxidizer Outlet - Stack (E2)
Port A
Ports
on back side
I
Q
O
N •
\JNMIo
7
ift.
.1.
CS4
CSS
Figure 3. Thermal oxidizer inlet and outlet sampling location.
9
-------
contains traverse point information and a sketch of the sampling port arrangement for this
location.
2.3.5 ModifiedTBitumen Mixing Tank Exhaust Outlet E17B (E5)
This sampling location was a horizontal section of 8-in diameter steel duct (E17B)
exhausting emissions from SBS production line mixing tank No. M7. The duct was
approximately 12 ft above floor level. This floor level was accessible by stairs from the ground
level. One 3-in port was installed on the side of the duct. Approximately 100 ft of sample
transfer line from the trailer was required here. Only one diameter was traversed for volumetric
flow rate measurements because velocities were very low and stratification across the gas stream
was insignificant. Appendix A contains traverse point information and a sketch of the sampling
T
port arrangement for this location.
2.3.6 Modified Bitumen Mixing Tank Exhaust Outlet E2B (E6)
This sampling location was a horizontal section of 8-in diameter steel duct (E2B)
exhausting emissions from APP production line mixing tank No. Ml. The duct was
approximately 10 ft above floor level. This location was above the production room floor and
was accessible by stairs from the production room floor and a walkway. One 3-in port was
installed on the side of the duct. Approximately 200 ft of sample transfer line from the trailer
were required here. Only one diameter was traversed for volumetric flow rate measurements
because velocities were very low and stratification across the gas stream was insignificant.
Appendix A contains traverse point information and a sketch of the sampling port arrangement
for this location.
2.3.7 Coater Vent Stack E10S (E7)
This sampling location was a vertical, 29-in I.D. steel duct or "stack" (E10S) exhausting
emissions from APP coater vat No. L3. The duct was located on the slanted, metal sheet roof
(closest stack to the access ladder up the side of the building). Two 2-in ports, 90° apart, were
about 5 ft above the roof. These ports were replaced with 4-in ports (nipples) for ERG's
sampling and velocity traverses. Another 4-in port was installed 1 ft below and offset 45° from
the other ports for the Method 25A and 320 (FTIR) single-point sampling. Approximately 200 ft
of sample transfer line from the trailer were required here. Appendix A contains traverse point
information and a sketch of the sampling port arrangement for this location.
10
-------
2.3.8 Coater Vent Stack E20S (E8)
This sampling location was a vertical, 29-in I.D. steel duct or "stack" (E20S) exhausting
emissions from-SBS coater vat No. L9. The duct was located approximately 50 ft further up the
roof from location E7. Otherwise, all information described above in Section 3.7 also applies to
this location. Appendix A contains traverse point information and a sketch of the sampling port
arrangement for this location.
11
-------
3.0 RESULTS
3.1 SCHEDULE
Testing of the U.S. Intec, Inc. facility in Port Arthur, Texas, was performed from
September 22-26,1997. Table 1 summarizes the schedule and the specific tests performed.
Sampling logs and notes for the Method 25A (THC) and Method 320 (FTIR) sampling are
contained in Appendix D. The THC and FTIR sampling was performed in coordination with the
manual sampling conducted by ERG.
3.2 FIELD TEST PROBLEMS AND CHANGES
Several deviations from the Test Plan were performed to adapt to field conditions. The
following is a summary of these changes.
1. Difficulties with one of the THC analyzers prevented the simultaneous operation of both
analyzers. Therefore, inlet/Outlet testing of the thermal oxidizer was accomplished by
sampling in alternating 30-min intervals at either location using a single THC analyzer. In
order to provide a parallel data set, the FTIR sampled the same location as the single THC
analyzer, and alternated between locations on the same 30-min schedule.
2. An additional problem with the THC data logging system necessitated manual data logging
during Run 1. For all of the remaining tests a computerized data logger was used.
3. At the request of EPA representatives on site, the 2-hr sampling period for the inlet/outlet
testing of the thermal oxidizer was extended to 4hrs. All three of the thermal oxidizer tests
were 4 hr.
4. Due to sampling error, ambient air was drawn into the sampling system during Run 1 on
the APP Holding Tank 1. This test was repeated and no 25 A analysis of the Run 1 APP
Holding Tank 1 data was performed.
5. During the final test, Run 2 on the APP Holding Tank 1, paniculate buildup in the sampling
lines caused failure of the heated pumps. As a consequence, the FTIR sampling was
changed from continuous spectral collection to batch collection, and was performed
manually. For each batch sample, the cell was flushed twice with dry nitrogen, evacuated,
then filled with sample gas.
6. Absorbance bands were much greater than 1 in the analytical region near 2900 cm"1 in
some spectra from Run 1 at the APP mixing tank and Run 2 at the APP holding tank. At
these locations some spectra of diluted samples were recorded to bring the entire spectrum
on-scale. The dilution procedure involved removing some sample from the gas cell, noting
the sample pressure and then filling the cell with dry nitrogen to ambient pressure. The
spectrum of the static, diluted sample was then recorded. The readings from the Barocell
pressure gauge were used to determine an approximate a dilution ratio. The dilution ratios
were included in the concentration calculations.
7. Samples were spiked in two different ways. For the first day, a blended gas containing both
SF6 and a volatile target compound was not available, requiring two separate gases to be
blended through two mass flow controllers and then spiked into the sample lines. Spiking
after the first day was performed using a single blended gas containing both SF6 and
12
-------
p-xylene as the target volatile organic. Since all locations were spiked with the p-
xylene/SF6 mixture, these results are reported in the spike summary.
8. Because of concern about interference from high CO2 concentrations, the analyte spike of
the p-xylene gas standard was controlled at a flow rate of approximately 2.0 Lpm with a
dilution ratio of about 5:1. Much lower spike flow rates were used at the coater roof stacks.
9. Due to time restrictions in coordinating testing with ongoing plant operations, spiking
during the first four sampling days was performed in duplicate, rather than in triplicate.
Triplicate spiking was performed on the last day.
10. Spectra collected during the last two days occasionally contained especially high
concentrations of hydrocarbon species. Some of the hydrocarbons may have adhered to the
cell walls in subsequent samples, but this had little or no effect on the analytical results.
Some additional nitrogen background spectra were recorded to minimize this effect.
11. A second post-run CTS spectrum was not recorded on 9/22/97. However, the Initial CTS
spectra from 9/22/97 and 9/23/97 past the method criteria. Therefore, the first CTS
spectrum on 9/23 also serves as the post-run CTS for the run on 9/22/97. The average
deviation of all the CTS measurements from their average value was 2.8 percent.
12. The FTIR cell did not pass the vacuum leak check during the field test (leak <4 percent of
cell volume according to the EPA protocol). Gas was sampled continuously, whenever
practical, to avoid diluting the sample When continuous sampling was not practical, the
cell was filled above ambient pressure and the sample spectrum was recorded when the cell
pressure reached equilibrium. A leak would result in a low bias in the reported
concentrations, but the sampling procedures used should have minimized any effect on the
results.
3.3 FITR RESULTS
A summary of the quantitative FTIR results and the average mass emissions rates is given
in Table 3. Complete tables of FTTR results are in Appendix E.
13
-------
TABLE 3. SUMMARY OF FTIR RESULTS AND MASS EMISSIONS RATES
Location
TO Intel
Run 1
Run 2
Run 3
TO Outlet
Runl
Run 2
Run 3
APP Coaler
Runl
SBS Coaler
Runl
APP Mixing Tank
Runl
SBS Mixing Tank
Run 1
APP Holding Tank
Runl
SBS Holding Tank
Run 1
Benzene
ppm Ib/hr kg/hr
65.9 7.4E-02 3.4E-02
Carbonyl sulfidc
ppm Ib/hr kg/hr
0.035 2.7E-03 I.2E-03
0.000 0.000 0.000
0.0054 3.9E-04 1.8E-04
0.000 0.000 0.000
0.000 0.000 0.000
0.000 0.000 0.000
0.74 5. IE-OS 2.3E-05
0.024 9.6E-06 4.4E-06
1.6 I.4E-03 6.3E-04
0.73 2.1E-04 9.4E-05
Methyl chloroform
ppm Ib/hr kg/hr
0.46 2.9E-04 I.3E-04
Elhylidene dichtoride
ppm Ib/hr kg/hr
9.5 I.8E-02 8.3E-03
Melhanol
ppm Ib/hr kg/hr
i
0.14 5.2E-06 24E-06
0.063 2.9E-OS I.3E-05
0.0078 I.2E-06 5.4E-07
Locution
TO Inlet
Run 1
Run 2
Run 3
TOOulkt
Runl
Run 2
Run 3
APP Coaler
Runl
SBS Coaler
Runl
APP Mixing Tank
Runl
SBS Mixing Tank
Runl
APP Holding Tank
Runl
SBS Holding Tank
Run 1
Slyrene
ppm Ib/hr kg/hr •
I.I 5.4E-04 2.4E-04
1.1,2,2-Teirachloroe thane
ppm Ib/hr kg/hr
0.32 2.6E-04 I.2E-04
p-Xylene
ppm Ib/hr kg/hr
021 0.028 0.013
0.000 0.000 0.000
0.052 6.6E-03 3.0E-03
2.0 0.26 0.12
0.000 0.000 0.000
2.8 0.35 0.16
II S.5E-04 2.5E-04
2,2,4-Trimelhylpenlane
ppm Ib/hr kg/hr
0.44 0.064 0.029
0.000 0.000 0.000
0.000 0.000 0.000
0.050 7.IE-03 3.2E-03
0.000 0.000 0.000
0.000 0.000 0.000
Elhylene
ppm to/hi kg/hr
0.000 0.000 0.000
0.0027 9.0E-05 4.1E-05
0.19 6.5E-03 2.9E-03
0.000 0.000 0.000
0.0094 3.2E-04 1.4E-O4
0.016 5.2E-04 2.4E-04
1.5 4.7E-05 2.2E-05
-------
TABLES, (continued)
Locution
TO inlet
Run 1
Rim 2
Run 3
TO Outlet
Runl
Run 2
Run 3
APP Coaler
Run 1
SBS Coaler
Run 1
APP Mixing Tank
Run 1
SBS Mixing Tank
Runl
APP Holding Tank
Run 1
SBS Holding Tank
Runl
Propane
ppm Ib/hr kg/hr
3.5 0.20 0.089
3.5 0.19 0.084
4.2 0.22 0.099
0.48 0.026 0.012
0.24 0.013 5.9E-03
0.35 0.018 8.3E-03
4.6 9.6E-04 4.3E-04
Cumene
ppm Ib/hr kg/hr
1.2 0.18 0.083
5.1 0.74 0.34
61 0.88 0.40
0.08 0.013 5.7E-03
0.08 0.01 1 0.005
0.20 0.028 0.013
Hexane
ppm Ib/hr kg/hr
110 1.19 0.54
11.3 1.17 0.53
11.4 I.J7 0.53
1.5 0.16 0.07
0.85 0.088 0.040
0.45 0.046 0.021
1.5 0.22 0.10
2.0 0.30 0.14
38.4 0.022 9.8E-03
101.6 0.13 0.057
58.2 0.024 0.011
Melhylene chloride
ppm Ib/hr kg/hr
0.36 1.4E-04 6.5E-05
Propionaldehyde
ppm Ib/hr kg/hr
98.7 0.083 0.038
21.9 6.0E-03 2.7E-03
ujcuiion
TOlnlel
Run 1
Run 2
Run 3
TO Outlet
Runl
Run 2
Run 3
APP Coaler
Runl
SBS Coaler
Runl
APP Mixing Tank
Runl
SBS Mixing Tank
Runl
APP Holding Tank
Runl
SBS Holding Tank
Run 1
Methane
ppm Ib/hr kg/hr
3.0 0.061 0.028
3.0 0.058 0.026
4.4 0.083 0.038
0.36 7.2E-03 3.3E-03
0.16 3.0E-03 1.4E-03
0.40 7.7E-03 3.5E-03
3.0 0.083 0.038
3.5 0.097 0.044
4.3 4.5E-04 2.0E-04
14.8 I.1E-03 5.1E-04
Sulfur dioxide
ppm Ib/hr kg/hr
6.6 4.8E-04 2.2E-04
77.0 0.032 0.015
109.6 0.10 0.046
57.4 0.017 7.8E-03
Carbon monoxide | ' Ammonia
ppm Ib/hr kg/hr
11.3 0.40 0.18
0.22 7.4E-03 3.4E-03
4.2 0.14 0.064
1.3 0.043 0.020
0.17 5.6E-03 2.6E-03
0.18 6.2E-03 2.8E-03
13.1 0.64 0.29
14.4 0.70 0.32
58.4 I.9E-03 8.4E-04
9.1 1.7E-03 7.5E-04
143.2 0.058 0.026
118.7 0.016 7.IE-03
ppm Ib/hr kg/hr
4.0 4.4E-04 2.0E-04
10.8 2.7E-03 1.2E-03
16.1 I.3E-03 5.8E-04
Formaldehyde
ppm Ib/hr kg/hr
0.000 0.000 0.000
0.000 0.000 0.000
2.3 0.083 0.038
133.6 0.058 0.026
9.0 1.3E-03 5.8E-04
-------
3.3.1 Thermal Oxidizer Inlet and Outlet
The results for the thermal oxidizer inlet and outlet are presented in Tables E-l and E-2,
respectively. Compound identifications and their concentrations result from a least-squares fit
performed by the analytical program, using the available input data, which determined the best
linear combination from the reference spectra in Section 4.5.1. The infrared absorbance near
3,000 cm"1 is primarily due to non-aromatic organic species. But the presence of cumene is
consistent with the spectra because its strongest absorbance in this region is from the aliphatic
hydrogens not from the aromatic (bonded to the ring) hydrogens. In the C-H stretching region
(near 2,900 cm"1), hexane and trimethylpentane give the best fit of the organic HAPs included in
the analysis.
3.3.2 APP and SBS Coaters
Emissions from the coater roof stacks were much lower compared to the other test
locations. Table 4 presents results of uncertainty calculations for some HAP compounds. The
results for the APP and SBS coater stacks are presented in Tables E-3 and E-4.
3.3.3 APP and SBS Mixing Tanks
Results from the APP and SBS mixing tanks are presented in Tables E-5 and E-6. Both
locations exhibited high organic emissions. Portions of the spectra from the APP mixing tank
were off scale and could not be quantified. Some compounds could not be measured because no
quantitative reference spectra are available. These compounds are not included in Tables E-5
and E-6. These other emissions include propylene and isomers of pentene. These emissions
could be quantified if quantitative reference spectra of each compound were first measured in the
laboratory. The additional reference spectra could then be included in the analytical computer
program. Table 5 shows some additional compounds that may be included in the emissions, but
cannot be measured because there are no quantitative reference spectra available.
3.3.4 APP and SBS Holding Tanks
Results from the APP and SBS holding tanks are presented in Tables E-7 and E-8.
Significant organic emissions, carbonyl sulfide, CO and ammonia were detected at each location.
Some compounds are identified in Tables E-7 and E-8. Additional organic compounds that were
not measured may include propylene and pentene compounds.
16
-------
TABLE 4, UNCERTAINTY RESULTS FOR SOME HAP COMPOUNDS
AT THE COATER STACKS
SAP-name
Benzene
Carbonyl Sulfide
Methyl chloride
Methyl chloroform
1,1-Dichloroethane
Toluene
1,3-Butadiene
Propane
Cumene
Ethyl benzene
Methylene Chloride
Propionaldehyde
Styrene
1 , 1 ,2,2-Tetrachloroethane
p-Xylene
o-Xylene
m-Xylene
2,2,4-Trimethylpentane
Formaldehyde
Uncertainty, ppm
APP coaler
1.191
0.088
4.063
0.081
0.450
3.981
0.350
0.773
1.465
4.280
0.183
0.823
0.595
0.265
0.578
2.252
3.114
0.360
0.572.
SBS coater
0.883
0.066
3.013
0.066
0.367
2.952
0.292
0.574
1.087
3.174
0.149
0.610
0.485
0.216
0.471
1.670
2.309
0.267
0.424
17
-------
TABLES. POSSIBLE DETECTS OF SOME ORGANIC SPECIES
Compound
3-methyl,l-butene
2-methyl,l-pentene
Propylene
Propane
2-pentene
4-methyl,2-pentene
pentane
APP Holding
Tankl
1
2
1
1
1
1
SBS Holding
Tank 3
1
2
1
1
1
1
SBS Mixing
Tankl
1
APP Mixing
Tankl
1
1
1
1
1 - Indicates a possible detect. This list in not exhaustive.
2- Indicates a certain detect.
3.3.5 Results from Spiked Samples
Some samples were spiked with a controlled flow containing a mixture of p-xylene and
SF6. The SF6 was used to determine the spike dilution factor. The SF6 andp-xylene concen-
trations were determined with the same analysis program that was used for the other analyses.
The spike results are summarized in Table 6. Explanations of the calculations are given in the
footnotes to Table 6 and in Section 4.4.
Two spike recoveries are presented in Table 6. The recoveries in column A result from
using the p-xylene reference spectra in the EPA spectral library. Spectra of the p-xylene cylinder
standard disagree with the EPA library spectra by about 25 percent. These spectra give the
recovery results shown in column B of Table 6. In this test the spike recoveries fall within the
requirement of ±30 percent whichever reference data set is used.
The discrepancy between the library spectra and the spectra of the cylinder standard is
illustrated in Table 7. This table compares the integrated absorbance band areas for the spectra
after correction for differences in temperature and pathlength. The same table also compares the
spectra based on their accepted concentrations after correction for differences in temperature and
path length. Ideally the two comparisons would agree. In this case they differ by a bout
25 percent. The results from the analytical program depend on the abosorbance values of the
reference spectra so this discrepancy affects the analytical results. This observation is compound
dependent and nothing can be inferred about the reported results for other compounds.
18
-------
TABLE 6. SUMMARY OF ASPHALT ROOFING FTIR P-XYLENE SPIKE RESULTS
Location
Thermal Oxidizer Inlet
Thermal Oxidizer Outlet
APP Coater
SBSCoater Roof Stack
SBS Mixing Tank 1 1
SBS Holding Tank 3
APP Holding Tank 1
Date
923/97
923/97
923/97
9/24/97
9/24/97
9/25/97
9/25/97
9/26/97
9/26/97
Average p-xylene concentration
Spike Unspike Calc
29.9 0.0 29.9
28.3 0.0 28.3
24.4 0.0 24.4
7.6 0.0 7.6
10.7 0.0 10.7
25.1 0.0 25.1
23.3 0.0 23.3
21.9 3.1 18.8
30.4 0.0 30.4
Average SF^ concentration
Spike Unspike Calc
0.939 0.000 0.939
0.895 0.000 0.895
0.742 0.000 0.742
. 0.259 0.000 0.259
0.324 0.000 0.324
0.823 0.000 0.823
0.856 0.000 0.856
0.618 0.000 0.618
0.975 0.000 0.975
DF
4.3
4.6
5.5
15.7
12.6
5.0
4.8
6.6
4.2
Cexp
23.9
22.8
18.9
6.6
8.2
21.0
21.8
15.7
24.9
A
6.0
5.5
.5-5
1.0
2.5
4.2
1.5
3.0
5.5
% Recovery
A B
125.0 93.3
124.il 92.6
129.1 96:3
115.3 86.0
129.7 96.8
119.9 89.4
107.0 79.8
119.1 88.9
122.1 91.1
"Spike" is the measured concentration of p-xylene or SF^ in the spiked samples. "Unspike" is the measured concentration of p-xylene or SF^ in the unspiked
samples. Calc is the difference, spike - unspike. DF is the dilution factor, 4.08 ppm/SFg(Calc). Cexp is the expected p-xylene concentration (104 ppm/DF).
A is the difference, p-xylene (Calc) - Cexp. The % Recovery of 104 ppm p-xylene standard is relative to the EPA library spectra, column A, relative to
spectra of the p-xylene calibration standard measured while at the Port Arthur test site, column B.
TABLE 7. p-XYLENE SPECTRAL BAND AREAS. COMPARISON OF EPA LIBRARY SPECTRA TO SPECTRA
OF P-XYLENE CYLINDER STANDARD
p-xylene spectra
173a4asa(lcm-l)
173a4asc(lcm-U
Dir03
Dir04
DirOS
Source
EPA library
Port Arthur
Band area
6.5
1.2
3.1
3.3
3.3
Region, cm- 1
818.6 - 769.9
818.6-769.9
Spectra comparison based on
band areas
Ratio (Ra)
5.5
1.0
2.6
2.7
2.8
=l/Ra
0.182
1,000
0.387
0.364
0.364
Comparison of spectra based on standard
concentrations
(ppm-m)/K
5.05
1.00
2.00
2.00
2.00
Ratio (Re)
5.1
1.0
2.0
2.0
2.0
=l/Rc
0.197
1.000
0.500
0.500
0.500
Ra/Rc, %
92.45
100.40
77.5
72.8
72.8
-------
3.4 METHOD 25A RESULTS
THC results as detennined by EPA Method 25A are presented in Tables 8 to 10.
Appendix B contains the raw data and graphical displays of the data versus time.
As shown in Table 8, THC emissions from the outlet of the thermal oxidizer averaged
near 2 ppm as propane (wet). Run 1 emissions were the highest of the three runs, but were
collected by manually logging the data. The Run I manual readings likely introduced a high bias,
since all the readings fell near the extreme low end (zero point) of the instruments scale, 0 to
1,000 ppm as propane. Runs 2 and 3 were electronically logged and are believed to be more
accurate.
The THC concentrations at the inlet to the thermal oxidizer ranged from 60 to 100 ppm as
>
propane (wet), with an average concentration of about 75 ppm. Concentrations were fairly
stable, with an occasional spike of 5 to 10 ppm above the average being observed. Only once
was a spike greater than 10 ppm above the average observed.
Mass emission rates of THC (in carbon equivalents) ranged from 3.1 to 3.5 Ib/hr (Thermal
Oxidizer Inlet) to 0.0043 to 0.0086 Ib/hr (Thermal Oxidizer Outlet). The calculated mass
emission rate of 0.279 Ib/hr for Run 1 of the Thermal Oxidizer Outlet is nearly two orders of
magnitude greater than either Runs 2 or 3, and further reinforces the believed inaccuracy of the
manually logged data. Calculation of combusion efficiency, which is typically >99 percent for
these types of combustion systems, also shows that Run 1 does not agree with Runs 2 and 3, and
falls well below the expected 99 percent.
An examination of THC emissions from the SBS and APP Mixing and Holding Tanks
(Table 9) shows that the APP line had much higher THC concentrations than the SBS line. For all
the mixing and holding tanks tested, APP Mixing Tank 1 had the highest THC concentrations,
and saw levels of 1,250 to 2,100 ppm. The APP Holding Tank 1 was next highest (475 to
875 ppm), followed by the SBS Mixing and Holding tanks, respectively (125 to 300 ppm).
In terms of THC mass emissions (in carbon equivalents), the APP line was also
significantly greater than the SBS line. Due to the high concentration at a relatively high flowrate,
APP Holding Tank 1 emissions were the greatest by nearly an order of magnitude (0.4 Ib/hr).
APP Mixing Tank 1, on the other hand, had a quite low flowrate, but with the highest THC
20
-------
TABLE 8. SUMMARY OF THERMAL OXIDIZER INLET/OUTLET THC DATA
Test data
Location
Run No.
Date
Time
Stack Gas Data8
Moisture content, %
Volumetric flow rate, dscfm
THC Concentrations
(as propane)
Maximum, ppm wet
Minimum, ppm wet
Average, ppm wet
Average, ppm dry
(as methane)
Average, ppm dry
Emissions Data
Average THC emission rate,
Ib/hr carbon equivalent
Average THC emission rate
(kg/hr carbon equivalent)
Control efficiency, %
Inlet to thermal oxidizer
1
9/22/97
1450-1926
2.8
7,867
100.0
60.0
73.0
75.1
225.3
3.31
1.51
NA
2
9/23/97
1015-1440
3.5
7,427
91.7
60.9
72.3
74.9
224.8
3.12
1.42
NA
3
9/23/97
1710-2140
3.3
7,387
92.9
71.5
81.5
84.3
252.8
3.49
1.59
NA
Average
-
-
3.2
7,560
94.9
64.1
75.6
78.1
234.3
3.31
1.50
NA
Outlet from thermal oxidizer
1
9/22/97
1450-1926
4.6
7,535
10.0C
5.0C
6.3C
6.6C
19.8C
0.279C
0.1 27C
91.58C
2
9/23/97
1015-1440
4.9
7,336
1.1
0.0
0.1
0.1
0.3
0.00432
0.00197
99.86
3
9/23/97
1710-2140
4.7
7,329
1.4
0.0
0.2
0.2
0.6
0.00862
0.00392
99.75
Average
i -
- '. .
4.7
7,400
4.2
1.7
2.2
2.3
6.9
0.0958
0.0435
97.11
aStack gas data gathered by ERG.
bAverage of PM and D/F trains.
cData taken from manual readings of instrument at extreme low end (zero point) of scale. Accuracy is questionable.
NA = Not applicable.
-------
TABLE 9. SUMMARY OF SBS AND APP MIXING AND HOLDING TANK THC DATA
Test data
Location
Run No.
Date
Time
Stack Gas Data
Oxygen, %
Carbon dioxide, %
Moisture content, %
Gas stream velocity, fps
Volumetric flow rate, dscfm
THC Concentrations
(as propane)
Maximum, ppm wet
Minimum, ppm wet
Average, ppm wet
Average, ppm dry
(as methane)
Average, ppm dry
Emissions Data
Average THC emission rate (Ib/hr
carbon equivalent)
Average THC emission rate
(kg/hr carbon equivalent)
SBS Mixing Tank 1 1
1
9/25/97
1800-1859
20.9
0.0
2.8
2.8
40.9
227
126
146
150
451
0.0344
0.0157
SBS Holding Tank 3
1
9/26/97
1115-1214
20.9
0.0
3.1
1.0
29.3
319
168
217
224
672.
0.0368
0.0167
APP Mixing Tank 1
1
9/25/97
1420-1520
20.9
0.0
3.4
0.45
7.05
2,177
1,253
1,687
1.746
5.239
0.0690
0.0314
APP Holding Tank 1
2
9/26/97,
1634-1641
20.9
0.0
3.3
6.6
89.9
874
473
766
792
2,376
0.399
0.181
NJ
-------
TABLE 10. SUMMARY OF SBS AND APP COATER ROOF STACK THC DATA
Test data
Location
Run No.
Date
Time
Stack Gas Data3
Moisture content, %
Volumetric flow rate, dscfm
THC Concentrations
(as propane)
Maximum, ppm wet
Minimum, ppm wet
Average, ppm wet
Average, ppm dry
(as methane)
Average, ppm dry
Emissions Data
Average THC emission rate
(Ib/hr carbon equivalent)
Average THC emission rate
(kg/hr carbon equivalent)
SBS Coater Roof Stack
1
9/24/97
1443-1538
2.9
10,816
27.1
10.9
17.8
18.3
55.0
1.11
0.505
2
9/25/97
0922-1026
2.0
11,614
6.1
4.1
4.5
4.6
13.8
0.299
0.136
3
9/25/97
1040-.1144
2.0
11,401
5.4
3.9
4.5
4.6
13.8
0.293
0.133
Average
-
-
2.3
11,277
12.9
6.3
8.9
9.1
27.4
0.578
0.263
APP Coater Roof Stack
1
9/24/97
1335-1430
3.3
10,879
14.8
10.4
11.7
12.1
36.3
0.738
0.335
2
9/24/97
1510-1615
3.4
11.070
25.5
2.4
12.3
12.7
38.2
0.790
0.359
3
9/24/97
1631-1735
2.9
11,197
10.3
4.0
8.3
8.5
25.6
0.537
0.244
Average
('
-
3.2
11,049
16.9
5.6
10.8
11.1
33.4
0.689
0.313
U>
1 Stack gas data gathered by ERG
-------
concentrations still produced the second-highest emission rate (0.069 Ib/hr). The SBS mixing and
holding tanks showed the lowest emissions at 0.034 and 0.037 Ib/hr, respectively.
As shown in Table 10, the SBS and APP coater roof stacks tested both had average THC
concentrations near 10 ppm. Both processes experienced some spikes of up to about 25 ppm and
also saw minimum concentrations fall below 5 ppm. Emission rates for the APP Coater Roof
Stack ranged from 0.54 to 0.79 Ib/hr. For the SBS Coater Roof Stack, emissions ranged from
0.29 to 1.1 Ib/hr. Run 1 emissions were three to four times greater than those observed in Runs 2
and 3, which showed essentially similar trends.
24
-------
4.0 TEST PROCEDURES
The procedures used for this field test are described in EPA Method 320 for using FTIR
spectroscopy taLmeasure HAP, the EPA Protocol for extractive FTIR testing at industrial point
sources and EPA Method 25A for total gaseous organics. The objectives of the field test were to
use the FTIR method to measure emissions from the processes, screen for HAP using the EPA
FTIR reference spectrum library, and analyze the spectra for compounds not in the EPA library.
Concentrations were reported for compounds that could be measured with FTIR reference
spectra. Additionally, manual measurements of gas temperature, gas velocities, moisture, CO2,
and O2 by ERG and MRI were used to calculate the mass emissions rates.
Midwest Research Institute used the extractive sampling system shown in Figure 4 to
transport sample gas from the test ports to the FTIR instrument and the THC analyzer.
4.1 SAMPLING SYSTEM DESCRIPTION
4.1.1 Sample System Components
The sampling system consists of three separate components:
1. Two sample probe assemblies;
2. Two sample lines and pumps; and
3. A gas distribution manifold cart.
All wetted surfaces of the system are made of unreactive materials, Teflon®, stainless
steel, or glass and are maintained at temperatures at or above 300° F to prevent condensation.
The sample probe assembly consists of the sample probe, a prefilter, a primary particulate
filter, and an electronically actuated spike valve. The sample probe is a standard heated probe
assembly with a pitot tube and thermocouple. The prefilter is a threaded piece of tubing loaded
with glass wool attached to the end of sample probe. The primary filter is a Balston particulate
filter with a 99 percent removal efficience at 0.1 fj.m. The actuated spike valve is controlled by a
radio transmitter connected to a switch on the sample manifold cart. All sample probe assembly
components are attached to or enclosed in an insulated metal box.
The sample lines are standard heated sample lines with three 3/8-in. Teflon tubes in 10,25,
50, and 100 foot (ft) lengths. The pumps are heated, single-headed diaphragm pumps
manufactured by either KNF Neuberger or Air Dimensions.. These pumps can sample at rates up
25
-------
to 20 liters per minute (Lpm) depending on the pressure drop created by the components installed
upstream.
The gas~3istribution manifold was specially constructed for FUR sampling by MRI. It is
built onto a cart that can be operated inside the MRI mobile lab or in an alternate location, if
necessary. The manifold consists of a secondary paniculate filter, control valves, rotameters, back
pressure regulators and gauges, and a mass flow controller. The manifold can control two sample
gas stream inputs, eight calibration gases, and has three individual outputs for analyzers. Also on
the cart are a computer work station and controls for the spike valves and mass flow controller.
4.1.2 Sample Gas Stream Flow
Exhaust gas was withdrawn through the sample probe and transported to the gas
distribution manifold. Inside the manifold the gas passed through separate secondary paniculate
filters. Downstream of the secondary filters, part of each sample gas stream was directed to
separate THC analyzers; one to measure the inlet concentration and another to measure the outlet
concentration. Part of the remaining sample gas from each stream was either sent to the FTIR
instrument for analysis or exhausted with the remaining portion of the gas stream being sampled
(i.e., when the inlet sample was analyzed the stack sample was exhausted and vice versa). This
was accomplished by rotating the gas selection valves to allow the appropriate sample gas to pass
the instrument inlet port. The gas flow to the instruments was regulated by needle valves on
rotameters at the manifold outlets.
4.2 SAMPLING PROCEDURES
Sampling was conducted at all sampling locations using either one of two identical, but
separate, sample systems which were both connected to the main manifold (Figure 4). A single
FTIR instrument and one THC analyzer were used to sample all locations. The 4-way valves on
the outlets of the common manifold could be used to select sample from either location at any
given time. For several of the tests, sampling was performed using both sample lines, with the
FTIR and THC alternating between locations every 30 minutes. Sample flow to each instrument
was controlled by the use of the rotameter needle valves.
26
-------
VMtt
V«n»
m
NJ
-J
Ma Stomp 4 Andy** FT\RSpKttm** HutodCtl
Sonpto Trarahr Un» (HMtod Bundh) tl
Swnpto Tramfw Lkw (HMtod Bund*)«
Figure 4. Extractive sampling system.
-------
FTIR SAMPLES
Sampling was conducted using either batch or the continuous sampling procedures,
described belowT All data were collected according to the Method 320 sampling procedure, which
is described below.
4.2.1 Batch Samples
In this procedure, the 4-way valve on the manifold outlet was turned to divert a portion of
the sample flow to the FTIR cell. A positive flow to the main manifold outlet vent was
maintained as the cell was filled to just above ambient pressure. The cell inlet valve was then
closed to isolate the sample, the cell outlet valve was open to vent the cell to ambient pressure, the
spectrum of the static sample was recorded, and then'the cell was evacuated for the next sample.
This procedure was repeated to collect as many samples as possible during the test run.
Batch sampling has the advantage that every sample is unique from the other samples. The
time resolution of the measurements is limited by the interval required to pressurize the cell, and
record the spectrum. All of the spiked samples and all of the samples for Run 2 APP Holding
Tank 1 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 kept open 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. The cell volume was about 7 L.
The FTIR instrument was automated to record spectra of the flowing sample about every
2 min. The automated analytical program was revised after the test was completed and all of the
spectra were reanalyzed to measure the pollutants of interest.
This procedure with automated data collection was used for all of the unspiked testing.
Because spectra were collected continuously as the sample flowed through the cell, there was
mixing between consecutive samples. The interval between independent measurements (and the
time resolution) depends on the sample flow rate (through the cell), and the cell volume. The
following explanation is taken from Draft Performance Specification 15, which is for FTIR
GEMS.
28
-------
The Time Constant, TC, is the period for one cell volume to flow through the cell. The
TC determines the minimum interval for complete removal of an analyte from the cell volume. It
depends on the-sampling rate (Rs in LPM), the cell volume (Vcell in L) and the analyte's chemical
and physical properties.
- (1)
Ks
Performance Specification 15 defines 5 * TC as the minimum interval between
independent samples.
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
Since there was little information available about HAP emissions from this source, there
was no plan for validating specific HAPs at this test. MRI conducted spiking for QA purposes
with using a cylinder standard of 104 ppmp-xylene and 4 ppm SF6 in nitrogen.
4.3.1 Analyte Spiking Procedures
The infrared spectrum is ideally suited for analyzing and evaluating spiked samples
because many compounds have very 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
The spike procedure follows Sections 9.2 and 13 of EPA draft Method 320. 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 will comprise
about 1/10 or less of the spiked sample. The expected concentration of the spiked component is
determined using a tracer gas, SF6. The SF6 concentration in the direct sample divided by the SF6
concentration in the spiked sample(s) is used as the spike dilution factor (DF). The analyte
29
-------
standard concentration divided by DF gives the expected value of the spiked analyte
concentration.
For all testing activities on September 22, 1997, MRI generated spike gas by blending two
gas streams through two separate mass flow controllers. One gas stream contained toluene and
one contained SF6. Because of this two controller approach, these spikes are likely less reliable
than those performed on subsequent days. [Final spectral analysis will prove/disprove this.]
For testing on September 23 through September 26, MRI performed spiking by flowing a
gas blend of SF6 and p-xylene through a single mass flow controller. Because of the relatively
low concentration available and low absorbance of p-xylene, spike flows were set to 1 to 2 Lpm,
or approximately 1/6 to 1/3 of the total sample flow-. The spike recovery results are presented in
Table 6 in Section 3.
4.3.2 Analysis of Spiked Results
The statistical procedures in Section 6.3 of EPA Method 301 were followed to analyze the
spiked and unspiked results. The application of these procedures to FTIR test data is described in
Section 13 of EPA Method 320. This involved evaluating the measurement precision,
determining any systematic bias in the results, and calculating a correction factor that can be
applied to the results when the validated method is used.
4.3.3 Determination of Percent Recovery
The expected concentration of the spiked component was determined using the tracer gas,
SF6. In the following discussion the "direct" measurement refers to the measured concentration in
a spectrum of a sample taken directly from the spike cylinder mixture.
The dilution factor, DF, was determined by the ratio of the measured SF6 concentration in
the direct measurement of the spike mixture, SF6(direct), to the measured SF6 concentration in the
spiked samples, SF6(spike).
op
DF = 6(direct) (2)
The direct measurement of the analyte concentration in the spike mixture divided by DF gives the
expected concentration for a 100 percent recovery of the analyte spike, Cexp.
30
-------
Analyte
'exp ~
where: —
Analyte(direct) = The concentration of p-xylene in from the cylinder standard.
The actual spike recoveries in Table 6 represent the percent differences between the measured
analyte concentrations in the spiked samples and Cexp.
% Recovery = CexP " Calc x 100 „.
Cexp v '
where "Calc" is equal to the differences between the measured analyte concentrations in spiked
and unspiked samples.
4.4 ANALYTICAL PROCEDURES
Analytical procedures in the EPA FTIR Protocol2 were followed for this test, and
programs were prepared prior to the field test for use in analyzing the data on site. The programs
employ automated routines to analyze the spectra using mathematical techniques based on a
K-matrix analysis to determine analyte concentrations and an estimated uncertainty for each
measurement.5"7 After the field test the input data (reference spectra) were modified based on the
real appearance of the sample spectra. The subtracted residual baseline spectra were analyzed to
estimate uncertainties in the reported concentrations.
Calculated concentrations in sample spectra were corrected for differences in absorption
path length and temperature between the reference and sample spectra by
where:
Ccorr = concentration, corrected for path length and temperature
Ccalc = concentration, initial calculation (output of the analytical program designed for the
compound)
L,. = conference spectrum path length
Ls = sample spectrum path length
31
-------
Ts = absolute temperature of the sample gas, K
Tr = absolute gas temperature of reference spectrum sample, K
4.4.1 Program Input
Several versions of program input data were used in analyzing the Port Arthur spectra.
Some of the spectra were qualitative and so concentrations of these compounds are not presented
in the results tables. Table 11 summarizes the quantitative version of program input reference
data. This information was used to calculate the reported concentration results. A second
qualitative version of the program input was used to gain insight into other compounds in the
emissions. Results from the second version were used to compile the information summarized in
Table 5.
Table 12 summarizes the input data used to evalutate the ethylene CTS spectra. This CTS
analysis was used 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 to 1.0 cm"1 in the same way as the toluene reference spectra using Section
K.2.2 of the EPA FTIR.protocol. The program analyzed the main two ethylene bands centered
near 2,989 and 949 cm"1. Table 12 summarizes the results of the CTS analysis. The cell path
length from this analysis was used as Ls in equation 5.
4.4.2 EPA Reference Spectra
The quantitative reference spectra used in the analysis were taken from the EPA reference
spectrum library (http://134.67.104.12/html/emtic/ftir2.htm). 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 agreed with those used to collect the sample spectra. The deresolved
1.0 cm"1 single beam spectra were combined with their deresolved single beam background
spectra and converted to absorbance. This same procedure was used to prepare spectral standards
for the HAP's and other compounds included in the preliminary analysis.
For qualitative analysis some spectra from the Hanst spectral library (Infrared Analysis,
Inc.) were used.
32
-------
TABLE 11. VERSION 1 OF THE PROGRAM INPUT DATA
Compound name
Water
Carbon monoxide
Sulfur dioxide
Carbon dioxide
Formaldehyde
Benzene
Methane
Carbonyl sulfide
Toluene
Methyl chloride
Methyl chloroform
1,1-dichloroethane
1,3 -butadiene
Methanol
Propane3
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
194csub
co20829a
198clbsi
194b4a_b
087b4anb
015a4ara
196clbsd
030a4ase
153a4arc
107a4asa
108a4asc
086b4asa
023a4asc
104a4ase
prophan
046a4asc
077a4arb
095a4asd
1 17a4asa
140b4anc
147a4asb
150b4asb
173a4asa
171a4asa
172a4arh
165a4asc
C0926c
Sf6_002
174clasc
Region No.
1,2,3
1
2
1,2,3
3
3
3
1
3
3
2
2
2
2
3
3
3
3
2
3
2
2
2
3
2
3
2
2
2
ISC
* = arbitrary
100*
167.1
90.3
850
100
496.6
16.09
19.5
103.0
501.4
98.8
499.1
98.4
20.1
39.3
96.3
515.5
101.6
498.5
99.4
550.7
493.0
488.2
497.5
497.8
101.4
20.1
1.0029
10.0
Reference
Meters T (K)
22 394
22 394
11.2 373
11.25 373
3 298
22 394
3 298
3 298
3 298
3 298
2.25 373
3 298
3 298
3 298
3 298
3 298
3 298
3 298
2.25 373
3 298
2.25 373
3 298
3 298
3 298
3 298
7.46 388
22 394
20 388
aFrom Infrared Analysis library.
33
-------
TABLE 11. (continued)
Region No.
1
2
3
Upper cm- 1
2142.0
1275.0
3160.8
Lower cm- 1
2035.6
789.3
2650.1
TABLE 12. PROGRAM INPUT FOR ANALYSIS OF CTS SPECTRA AND PATH
LENGTH DETERMINATION
Compound name
Ethylenea
Ethylene
File name
cts0814b.spc
cts0814c.spc
ASC
1.007
1.007
ISC
1.014
0.999
% Difference
0.7349
0.7350
aThis spectrum was used in the analysis of the Port Arthur CTS spectra
4.5 FTIR SYSTEM
The FTIR system used in this field test was a KVB/Analect RFX-40 interferometer. The
gas cell is a heated variable path (D-22H) gas cell from Infrared Analysis, Inc. The path length of
36 laser passes was used for measurement at both locations. The inside of the cell walls have
been treated with a Teflon® coating to minimize potential analyte losses. A mercury/cadmium/
telluride (MCT) liquid nitrogen detector was used. Spectra was collected at 1.0 cm"1, the highest
resolution of the RFX-40 system. The cell was maintained at 240°F throughout the test series.
The optical path length was measured by shining a He/Ne laser into the cell and adjusting
the mirror tilt until the desired number of passes was obtained. The path length in meters was
then calculated by comparing calibration transfer standard (CTS, ethylene in nitrogen) spectra
measured in the field to CTS spectra in the EPA reference spectrum library. Section 5.2 (QA/QC
procedures) shows results of these calculations.
4.6 CONTINUOUS EMISSIONS MONITORING FOR TOTAL HYDROCARBONS (THC)
The THC sampling was conducted continuously by taking a split of the gas used for the
FTIR sampling. Sample gas was directed to the THC analyzer through a separate set of
rotameters and control valves. A summary of the specific procedures used is given below.
34
-------
4.6.1 Components
A brief description of each system component follows.
1. THCAnalyzer—The THC concentration is measured using a flame ionization detector
(FID). MRI used two J.U.M. Model VE-7 instruments. The THC analyzers were operated on the
zero to 100 ppm and 1,000 ppm ranges throughout the test period. The fuel for the FID is
40 percent hydrogen and 60 percent helium mixture.
2. Data Acquisition System—MRI uses LABTECH notebook (Windows version), which
is an integrated system that provides data acquisition, monitoring and control. The system
normally writes data to a disk in the background while performing foreground tasks or displaying
data in real time. This system runs on a Pentium computer with a 700- megabyte hard drive and
expanded memory.
3. Calibration Gases—Calibration gases were prepared from an EPA Protocol 1 cylinder
of propane using an Environics Model 2020 gas dilution system which complies with the
requirements of EPA Method 205. High, Medium and Low standards gases were generated to
perform analyzer calibration checks.
The calibration gases were generated from 5,278 ppm propane in nitrogen standard. The
raw data are reported in ppm as propane.
35
-------
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,
except for Run 2 on the APP Holding Tank 1, for which batch collection was necessary.
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
36
-------
• 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 min before a
sampling run started or after changing to a different test location. FTIR spectra were monitored in
an effort to limit deviations in the spectral baseline to no greater than ±5 percent (-0.02
-------
TABLE 13. RESULTS OF THE CTS PATH LENGTH DETERMINATION
CTS spectra
104.4 ppm Ethylene
C0922A
C0923A
C0923B
C0923C b
C0923D b
C0923E
C0923F
C0924A
C0924B
C0924C
C0924D
C0925A
C0925B
C0925C
C0925D
C0926A
C0926B
C0926C
C0926D
Average path length (M)
Standard deviation
Path length calculations
Meters
7.47
7.66
7.82
6.87
6.86
7.33
7.31
7.59
7.63
7.35
7.33
7.58
7.76
7.36
7.31
7.81
7.80
7.49
7.49
7.53
0.188
Delta3
-0.07
0.13
0.28
-0.66
-0.67
-0.21
-0.22
0.05
0.10
-0.18
-0.21
0.05
0.23
-0.18
-0.23
0.27
0.26
-0.05
-0.04
% Delta
-0.87
1.68
3.76
-8.76
-8.90
-2.75
-2.92
0.73
1.27
-2.44
-2.78
0.67
3.01
-2.34
-3.00
3.63
3.52
-0.63
-0.54
aThe difference between the calculated and average values.
bSpectra CO923C and CO923D were not included in the average because
they deviated by more than 5 percent from the average. Spectra A, B, E, and
F meet the Method 320 requirement for September 23,1997.
38
-------
were also stored for data analysis. Sample absorbance spectra can be regenerated from the raw
interferograms, if necessary.
To measure HAPs 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;
3. Response time of the system; and
4. Calibration criterion for Method 25 A is ±5 percent of calibration gas value.
5.3.2 Daily Checks
The following checks were made for each test run.
1. Zero/Span calibration and Linearity check prior to 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.
39
-------
6.0 REFERENCES
1. Test Method 320 (Draft) "Measurement of Vapor Phase Organic and Inorganic Emissions by
Extractive Courier Transform Infrared (FTIR) Spectroscopy," EPA Contract No. 68-D2-0165,
Work Assignment 3-08, September, 1996.
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. "Computer-Assisted Quantitative Infrared Spectroscopy," Gregory L. McClure (ed.), ASTM
Special Publication 934 (ASTM), 1987.
4. "Multivariate Least-Squares Methods Applied to the Quantitative Spectral Analysis of
Multicomponent Mixtures," Applied Spectroscopy, 39(10), 73-84,1985.
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. "Method 25 A—Determination of Total Gaseous Organic Concentration Using a Flame
lonization Analyzer," 40 CFR 60, Appendix A.
40
-------
APPENDIX A
FIELD DATA SHEETS FOR STACK FLOW MEASUREMENTS
-------
40 CFR 60. APPENDIX A, METHOD 2* - GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE
DATA ENTRY AND SUMMARY OF RESULTS
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc.. Port Arthur, Texas
Sampling Location: APP Line - Modified Bitumen Mixing Tank M1 Outlet Vent E2B (E6)
Run No. 1
Date: 09/25/97
Type S Rot Tube No. 8-2-96-5 Temperature Meter No. Y-3917 Barometer No.
Pilot Tube Coefficient (Cp): 0.84 Elevation Change** from Barometer Location to Sampling Location:
Thermocouple No. 8-2-96-5T Cross Sectional Area of the Duct at Sampling Location:
Carbon Dioxide Concentration By Volume. Dry Basis: 0.0 % Gas Mol. Weight. Dry Basis (Md):
Oxygen Concentration By Volume. Dry Basis: 20.9%
FIRST TRAVERSE - START OF RUN SECOND TRAVERSE - END OF RUN
X-4029
20 feet
0.328 ft>
28.965 Ib/lb-mote
Start Time: 1310 Stop Time: 1350
Barometric Pressure at Barometer Location: 29.94 In. Hg
Barometric Pressure at Sampling Location: 29.92 In. Hg
Velocity Head at Centroid: 0.00 in. w.c.
Total Pressure at Centroid: -0.10 In. w.c.
Static Pressure: -0.100 In. w.c.
Absolute Pressure In Duct (Ps): 29.91 In. Hg
Dry Bulb Temperature: 107 *F
Wet Bulb Temperature: 86 'F
Water Vapor Concentration By Volume: 3.42 %
Gat Mol. Weight, Wet Basis (Ms): 28.590 Ib/lb-mote
Traverse
Point
Number
1
2
3
4
5
6
7
8
Velocity
Head,
(detta-p).
inches w.c.
NR
NR
NR
NR
NR
NR
NR
NR
Gas
Stream
Temp.,
(Is). -F
175
175
175
175
175
175
175
175
Velocity.
-------
40 CFR 60. APPENDIX A, METHOD 2* - GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE
DATA ENTRY AND SUMMARY OF RESULTS
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc.. Port Arthur. Texas
Sampling Location: SBS Una - Modified Bttumen Mixing Tank M11 Outlet Vent (E5)
Run No. 1
Date: 09/25/97
Type S Pilot Tube No. 8-2-96-5 Temperature Meter No. Y-3917 Barometer No. X-4029
Pilot Tube Coefficient (Cp): 0.84 Elevation Change" from Barometer Location to Sampling Location: 20 feet
Thermocouple No. 8-2-96-5T Cross Sectional Area of the Duct at Sampling Location: 0.328 ff
Carbon Dioxide Concentration By Volume. Dry Basis: 0.0% Gat Mol. Weight. Dry Baste (Md): 28.965 Ib/lb-mole
Oxygen Concentration By Volume, Dry Basis: 20.9%
SECOND TRAVERSE - END OF RUN
Start Time: 1930 Stop Time: 2000
Barometric Pressure at Barometer Location: 29.91 In. Hg
Barometric Pressure at Sampling Location: 29.89 In. Hg
Velocity Head at Centrold: 0.00 In. w.c.
Total Pressure at Centrold: -0.01 In. w.c.
Static Pressure: -0.010 In. w.c.
Absolute Pressure In Duct (Ps): 29.89 in. Hg
Dry Bulb Temperature: 94 "F
Wet Bulb Temperature: 79 *F
Water Vapor Concentration By Volume: 2.79 %
Gas Mol Weight. Wet Basis (Ms): 28.659 Ib/lb-mole
Barometi
Barome
Wat
FIRST TRAVERSE • START OF RUN
Start Time: Stop Tims:
ric Pressure at Barometer Location: in. Hg
trie Pressure at Sampling Location: In. Hg
Velocity Head at Centrold: In. w.c.
Total Pressure at Centrold: In. w.c.
Static Pressure: In. w.c.
Absolute Pressure In Duct (Ps): In. Hg
Dry Bulb Temperature: *F
Wet Bulb Temperature: *F
er Vapor Concentration By Volume: %
Gas Mol. Weight. Wet Baste (Ms): to/lb-moto
Traverse
Point
Number
1
2
3
4
5
6
7
8
Velocity
Head.
(delta-p).
inches w.c.
Gas
Stream
Temp-.
fts). *F
Velocity,
-------
40 CFR 60. APPENDIX A, METHOD V • GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE
DATA ENTRY AND SUMMARY OF RESULTS
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec. Inc.. Port Arthur, Texas
Sampling Location: APP Line - Modified Bitumen Holding Tank H1 Outlet Vent E1B (E4)
Run No. 1
Date: 09/26/97
Type SPitot Tube No. 8-2-96-5 Temperature Meter No. Y-3917 Barometer No.
Pitot Tube Coefficient (Cp): 0.84 Elevation Change" from Barometer Location to Sampling Location:
Thermocouple No. 8-2-96-5T Cross Sectional Area of the Duct at Sampling Location:
Carbon Dioxide Concentration By Volume, Dry Basis: 0.0 % Gas Mol. Weight. Dry Baste (Md):
Oxygen Concentration By Volume. Dry Basis: 20.9%
FIRST TRAVERSE - START OF RUN SECOND TRAVERSE - END OF RUN
X-4029
16 feet
0.349ft*
28.965 Ib/lb-mole
Start Time: 1250 Stop Time:
Barometric Pressure at Barometer Location:
Barometric Pressure at Sampling Location:
Velocity Head at Centrold:
Total Pressure at Centrold:
Static Pressure:
Absolute Pressure in Duct (Ps):
Dry Bulb Temperature:
Wet Bulb Temperature:
Water Vapor Concentration By Volume:
Gas Mol. Weight, Wet Baste (Ms):
1315
29.98 in. Hg
29.96 in. Hg
0.01 In. w.c.
-0 04 In. w.c.
-0 047 in. w.c.
29.96 In. Hg
129'F
90 'F
3.32%
28.602 Ih/lb-mole
Start Time: 1828
Stop Time: 1844
Traverse
Point
Number
1
2
3
4
5
6
Velocity
Head.
(detta-p).
inches w.c.
NR
NR
NR
NR
NR
NR
Gas
Stream
Temp..
(to). -F
327
327
327
327
327
327
Velocity.
(vs).
ft/min
320
375
410
430
445
390
Rotation
Angle
a
NR
NR
NR
NR
NR
NR
Barometric Pressure at Barometer Location: 29.97 In. Hg
Barometric Pressure at Sampling Location: 29.95 in. Hg
Velocity Head at CentroW: 0.01 in. w.c.
Total Pressure at Cent/old: -0.04 In. w.c.
Static Pressure: -0.047 in. w.c.
Absolute Pressure In Duct (Ps): 29.95 In. Hg
Dry Bulb Temperature: 125 *F
Wet Bulb Temperature: 89 *F
Water Vapor Concentration By Volume: 3.28 %
Gas Md. Weight. Wet Basis (Ms): 28.605 Ib/lb-mole
Average Rotation Angle:
Average Velocity:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
NR
395 ft/min
138acfm
92.6 scfm
89.5 dscfm
2.54 dry std. mVmin.
Traverse
Point
Number
1
2
3
4
5
6
Velocity
Head.
(delta-p).
inches w.c.
NR
NR
NR
NR
NR
NR
Gas
Stream
Temp.,
(UO. -F
316
316
316
316
316
316
Velocity.
(vs).
ft/min
340
363
395
420
435
400
RESULTS FOR RUN
Average Volumetric Flow Rate:
Average Volumetric Flow Rate:
Deviation of the flow rate after the
run from the one before the run:
5.391 dry std. fP/hr.
152.7 dry std. m'/hr.
-0.7
COMMENTS: No readings (NR) were obtained with a Type S
pitot tube because of the very low flow rate. Absence of
cyclonic flow could not be determined, and a hot wire
anemometer was used to measure velocity and total
pressure (with pitot tube).
Average Velocity:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
392 ft/min
137acfm
93.2 scfm
90.2 dscfm
2.55 dry std. mVmin. yield correct results.)
40 CFR 60. Appendix A. Method 3 is used for the
determination of dry molecular weight, and ASTM
Method £337-84(1996) Is used for determination of
moisture content.
Positive values for locations above the barometer and
negative values for locations below the barometer are
entered here. (Computations reverse the signs to
M2TSWBDB.WK4 09/18/97 (rev. M2TSE4R1.WK4 10/02/97 04:09 PM)
-------
40 CFR 60. APPENDIX A. METHOD 2* - GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE
DATA ENTRY AND SUMMARY OF RESULTS
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec. Inc., Port Arthur. Texas
Sampling Location: SBS Line - Modified Bitumen Holding Tank H3 Outlet Vent E19B (E3)
Run No. 1
Date: 09/26/97
Type SPitot Tube No. 8-2-96-5 Temperature Meter No. Y-3917 Barometer No.
Pilot Tube Coefficient (Cp): Q.84 Elevation Change" from Barometer Location to Sampling Location:
Thermocouple No. 8-2-96-5T Cross Sectional Area of the Duct at Sampling Location:
CartxxiDtoxide Concentration By Volume, Dry Basis: 0.0% Gas Mol. Weight. Dry Baste (Md):
Oxygen Concentration By Volume. Dry Basis: 20.9%
FIRST TRAVERSE-START OF RUN SECOND TRAVERSE - END OF RUN
X-4029
24 feet
0.532 ff
28.965 Ib/lb-mole
Start Time: 1030
Stop Time: 1100
Barometric Pressure at Barometer Location: 29.99 in. Hg
Barometric Pressure at Sampling Location: 29.97 In. Hg
Velocity Head at Centrold: 0.00 In. w.c.
Total Pressure at Centrold: -0.02 In. w.c.
Static Pressure: -0.020 In. w.c.
Absolute Pressure In Duct (Ps): 29.96 In. Hg
Dry Bulb Temperature: 93 *F
Wet Bulb Temperature: 82'F
Water Vapor Concentration By Volume: 3.27 %
Gas Mol. Weight. Wet Baste (Ms): 28.606 to/lb-moto
Traverse
Point
Number
1
2
3
4
Velocity
Head.
(deUa-p).
Inches w.c.
NR
NR
NR
NR
Gas
Stream
Temp.,
fts). 'F
132
132
132
132
*
Velocity,
(vs).
ft/min
275
290
295
278
Rotation
Angle
a
NR
NR
NR
NR
Start Time: 1345 Stop Time: 1405
Barometric Pressure at Barometer Location: 29.98 In. Hg
Barometric Pressure at Sampling Location: 29.96 in. Hg
Velocity Head at Centrold: 0.00 In. w.c.
Total Pressure at Centrold: -O.06 in. w.c.
Static Pressure: -0.060 In. w.c.
Absolute Pressure in Duct (Ps): 29.95 In. Hg
Dry Bulb Temperature: 97'F
Wet Bulb Temperature: 81 *F
Water Vapor Concentration By Volume: 2.97 %
Gas Mol. Weight. Wet Basis (Ms): 28.639 Ib/lb-mole
Traverse
Point
Number
1
2
3
4
Velocity
Head.
(detta-p).
inches w.c.
NR
NR
NR
NR
Gas
Stream
Temp..
(ts). -F
117
117
117
117
Velocity.
(vs).
ft/min
58
64
65
61
RESULTS FOR RUM
Average Volumetric Flow Rate:
Average Volumetric Flow Rate:
Deviation of the flow rate after the
run from the one before the run:
1,758 dry std. fP/hr.
49.79 dry std. m'/hr.
NA
Average Rotation Angle:
Average Velocity:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Row Rate:
Volumetric Flow Rate:
NR
285 ft/min
151 acfm
135 scfm
131 dscfm
3.70 dry std. nvVmin.
Average Velocity:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
Volumetric Flow Rate:
62.0 ft/min
33.0 acfm
30.2 scfm
29.3 dscfm
0.830 dry std. m'/min.
COMMENTS: No readings (NR) were obtained with a Type S
pilot tube because of the very low flow rate. Absence of
cyclonic flow could not be determined, and a hot wire
anemometer was used to measure velocity and total
pressure (with pttot tube).
Results from the first traverse are not representative
of normal operating conditions. An access door at the
top of the tank In the outlet vent breech was open during
the traverse. TNs was discovered shortly after FTIR
and THC sampling started. The door was closed and
FTIR and THC sampling was restarted. Because of
time constraints, the first traverse was not repeated.
• 40 CFR 60, Appendix A, Method 3 is used for the
determination of dry molecular weight, and ASTM
Method £337-84(1996) is used for determination of
moisture content.
** Positive values for locations above the barometer and
negative values for locations below the barometer are
entered here. (Computations reverse the signs to
yield correct results.)
-------
40 CFR 60, APPENDIX A, METHOD 2* -
GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE FIELD DATA SHEET
MRI Project No. 3804.21.04.03 Run No. /
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas Date:
Sampling Location: APR Line - Modified Bitumen Mixing Tank M1 Outlet E2B (E6)
Operator(s): f-el
Temperature Meter No'
Thermocouple No.
Barometer No.
09-
Type S Prtot Tube No.
Pitot Tube Coefficient (CB):
Hot-wire Anemometer No.
Elevation Change** from Barometer Location to Sampling Location:
Cross Sectional Area of Duct at Sampling Location:
Carbon Dioxide Concentration By Volume, Dry Basis:
Oxygen Concentration By Volume, Dry Basis:
ffo
feet
ft3
a. a
FIRST TRAVERSE - START OF RUN
Start Time: S3'O Stop Time:.
SECOND TRAVERSE - END OF RUN
Barometric Pressure (PbJ at Barometer Location:
Velocity Head (Ap) at Centroid of Duct:
Start Time:
O,C6
Total Pressure (P) at Centroid of Duct: . •".
Dry Bulb Temperature: _
.in- Hg
, in. H2C
. in. H2C
°F
Leak Checks - Initial:
Wet Bulb Temperature:
Final:
Pb«:
Ap:
P:
Dry Bulb Temperature:
Stop Time: SWO
#9.93 in. Hg
. in. H20
in. H20
°F
0.CO
-O./O
sot
LceXJ
°F Wet Bulb Temperature:
Initial:
Final: Me
Traverse
Point Number
/
^?
3
4
g~
t,
7
X
Velocity -Head,
/ A-I :_ LJ r\
/9f&»*
#f
S*4T
Z&
«&
30
30 .
3)
Gas Stream
Temp, (g, °F
/7f
/7S"
/7f
J7S"
/?£'
ST!?
/Tjf
;?£'
Rotation
Angle, a
/*x
st
Traverse
Point Number
/
ft
3
«A
&•
&
7
^%
^3
w^ft&'^rt
#/ £&*»»
#3
#t>
Z<*
#(*
#9
3?*
J2-
Gas Stream
Temp, (t,}, °F
/7£
/^
/*7^
S7&
S7&
S7&
J76
S7&
• 40 CFR 60, Appendix A, Method 3 is used for the determination of dry gas molecular weight, and ASTM Method £337-84(1996) is used for
the determination of moisture content.
* * Enter positive values for locations above barometer and negative values for locations below barometer.
Comments:
M2TSWB08.WPO S
-------
40 CFR 60, APPENDIX A, METHOD 2* -
GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE FIELD DATA SHEET
MRI Project No. 3804.21.04.03 Run No /
Client/Source: U.S..EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas Date:
Sampling Location: SBS Line - Modified Bitumen Mixing Tank MX Outlet£*?6 (E5)
Operator(s):
#
3
•7
£
Velocity Wea*,
frj* TTG^WW
x^T?
J6>7
/7J
S8V.
tfo
/^5"
Gas Stream
Temp. (t.). °F
0Z3
f&J
«?X3
3X3
ff#3
Z&3
#&3
3&3
• 40 CFR 60, Appendix A, Method 3 is used for the determination of dry gas molecular weight, and ASTM Method £337-84(1996) is used for
the determination of moisture content.
* * Enter positive values for locations above barometer and negative values for locations below barometer.
Comments:
M2TSWBOB.WPO S«pt«tnlMr 18. 1997 (rw. M2TSES.WPO S«pt«nb«f 18. 1997)
-------
40 CFR 60, APPENDIX A, METHOD 2* -
GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE FIELD DATA SHEET
MRI Project No. 3804.21.04.03 Run No. _^
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas Date:
Sampling Location: APPLJne - Modified Bitumen Holding Tank H1 Outlet E1B (E4)
Operator(s): J> Svsr**ri^ 0. ~T&9Jo*'df
Type S Pilot Tube No. Jt'?-9t-£~ Temperature Meter No.
Thermocouple No.
-m~ 9-7
Pitot Tube Coefficient (C.
Hot-wire Anemometer No.
Barometer No.
Elevation Change** from Barometer Location to Sampling Location:
Cross Sectional Area of Duct at Sampling Location:
Carbon Dioxide Concentration By Volume, Dry Basis:
Oxygen Concentration By Volume, Dry Basis:
6.349
feet
ft3
FIRST TRAVERSE - START OF RUN
Start Time: J2&O Stop Time:
SECOND TRAVERSE • END OF RUN
Barometric Pressure (PbJ at Barometer Location:
Velocity Head (Ap) at Centroid of Duct:
Total Pressure (P) at Centroid of Duct:
Dry Bulb Temperature:
Wet Bulb Temperature:
39.9*
o,e>j
-e.c»J
90
in. Hi
in. H
in. H2O
°F
°F
Leak Checks - Initial:
Lc*JtS
Final:
Traverse
Point Number
/
2
3
*J
£*
&
Velocity Jdeectr
3#t>W»ia
3T&
Wt>
V3D
M£"
390
Gas Stream
Temp, (t,), °F
327
337
3*7
337
327
327
Rotation
Angle, a
A/A
V
Start Time: tf£$ Stop Tima: /^W
P,™: #9.97 in. Ha
AD: 0V i-e&J<3 Final: Afo L&»kS
Traverse
Point Number
/
ft
?
V
g"
&
Velocity Jtoa4>
^**>-ft?!.ji
3&>3
^J f^P
^J^9t^
0
Gas Stream
Temp, (t,), °F
&J(*
3}b
3Jt*
3JL
3J(*
3Jb
' 40 CFR 60, Appendix A, Method 3 is used for th« determination of dry gas molecular weight, and ASTM Method 6337-84(1996) is used for
the determination of moisture content.
* * Enter positive values for locations above barometer and negative values for locations below barometer.
Comments:
M2TSWB08.WPO Saptvnlw 18. 1997 (r«v. M2TSE4.WPO S«t»«nMr 18, 1997)
-------
40 CFR 60, APPENDIX A, METHOD 2* -
GAS STREAM VELOCITY AND VOLUMETRIC FLOW RATE FIELD DATA SHEET
MRI Project No. 3804.21.04.03 Run No. /
Client/Source: U.S. EPA-EMC / U.S..Intec, Inc., Port Arthur, Texas Date:
Sampling Location: SBS Line - Modified Bitumen Holding Tank H3 Outlet E19B (E3)
Operator(s): J> £t/^srry*f &*'7&a.fo**£/
Temperature Meter No.
Thermocouple No.
Barometer No.
Type S..Fjtot Tube No.
Pitot Tube Coefficient (Cp):
Hot-wire Anemometer No.
Elevation Change** from Barometer Location to Sampling Location:
Cross Sectional Area of Duct at Sampling Location:
Carbon Dioxide Concentration By Volume, Dry Basis:
Oxygen Concentration By Volume, Dry Basis:
v-
0.0
feet
ft3
%
FIRST TRAVERSE - START OF RUN
Start Time: S03o Stop Time:
SECOND TRAVERSE - END OF RUN
Barometric Pressure (?„„} at Barometer Location:
Velocity Head (Ap) at Centroid of Duct:
Total Pressure (P) at Centroid of Duct:
Dry Bulb Temperature:
Wet Bulb Temperature:
Leak Checks - Initial: S/bL£**J Final: A^o
O.OO
Traverse
Point Number
/
^
3
*
Velocity-Head,
/Ant ;« u n
JiyjWm;*
**t>
29 in. H7O
P: -6.0b in. H,O
°F Dry Bulb Temperature: 9*7 °F
"F Wet Bulb Temperature: 9i °F .
Initial: /fjJ-tz*
i
i
Traverse
Point Number
/
;?
7
*t
\
*t
^kj*y
4/
Gas Stream
Temp, (t,), °F
W7
st?
SJ*7
SS"7
• 40 CFR 60, Appendix A, Method 3 is used for the determination of dry gas molecular weight, and ASTM Method £337-84(1996) is used for
the determination of moisture content.
* * Enter positive values for locations above barometer and negative values for locations below barometer.
•*/>**• o*
Comments:
-fro So* /»/• tt**/*J fS
M2TSWBOB.WPO
>•"$ &*
18. 1997(r«v.
M2TSE3.WPO S«ptimlMr 18. 1997)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No.
Client/Source:
Sampling Location:
Date:
Measured by
3804.21.04.03
U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Thermal Oxidizer Inlet Duct (E1)
09/22/97
J. Surman
Port-A
Port- B
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
Traverse
Point
1
2
3
4
5
6
Percent of
Duct Diameter
from Wall to
Traverse Point
4.4%
14.6%
29.6%
70.4%
85.4%
95.6%
Distance from
Reference
Point to
Traverse Point,
inches
4.81
8.49
13.83
28.42
33.76
37.44
39.000 inches
3.250 inches
35.750 inches
39.000 inches
3.250 inches
35.750 inches
288 inches, (
72 inches, (
12
12
35.75 inches
6
3.25 inches
6.971 ft3
8.1 D)
2.0 D)
Port A
Port B
(Port for
FTIR/THC
upstream
from this
port)
Compass Direction
West
Horizontal Duct - Flow Away From Observer
Comments: Note that the sampling location for FTIR and THC is 35 inches upstream from this
cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E1.WK4 09/29/97 10:14 AM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No.
Client/Source:
3804.21.04.03
_ U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: Thermal Oxidizer Outlet - Stack (E2)
Date: 09/22/97
Measured by J. Surman
Port - South
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Port-West
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
Traverse
Point
1
2
3
4
5
6
7
8
9
10
11
12
Percent of
Duct Diameter
from Wall to
Traverse Point
2.8%
6.7%
11.8%
17.7%
25.0%
35.6%
64.4%
75.0%
82.3%
88.2%
93.3%
97.2%
Distance from
Reference
Point to
Traverse Point,
inches
4.25
5.64
7.47
9.59
12.19
15.96
26.29
30.06
32.66
34.78
36.61
38.00
Port for
FTIR/THC
39.000 inches
3.250 inches
35.750 inches
39.000 inches
3.250 inches
35.750 inches
162 inches, (
42 inches, (
16
24
35.75 inches
12
3.25 inches
6.971 ft3
4.5 D)
1.2 D)
Port South
Port West
Compass Direction
West
Vertical Duct - Top View
Comments: Note that the sampling location for FTIR and THC is 76 inches below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E2.WK4 09/29/97 10:28 AM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: SBS Line - Modified Bitumen Holding Tank H3 Outlet E19B (E3)
Date: 09/22/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
12.625 inches
2.750 inches
9.875 inches
192 inches, ( 19.4 D)
96 inches, ( 9.7 D)
8
8
9.88 inches
4
2.75 inches
0.532 ft?
Traverse
Point
1
2
3
4
Percent of
Duct Diameter
from Wall to
Traverse Point
6.7%
25.0%
75.0% '
93.3%
Distance from
Reference
Point to
Traverse Point,
inches
3.41
5.22
10.16
11.96
Port
Compass Direction
South
Horizontal Duct - Flow Away From Observer
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Row measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E3.WK4 09/29/97 10:11AM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: APP Line - Modified Bitumen Holding Tank H1 Outlet E1B (E4)
Date: 09/22/97
Measured by J. Surman
Inside of far waU to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
10.500 inches
2.500 inches
8.000 inches
52 inches, (
20 inches, (
12
16
8.00 inches
6
2.50 inches
0.349 ft3
6.5 D)
2.5 D)
Traverse
Point
1
2
3
4
5
6
Percent of
Duct Diameter
from Wall to
Traverse Point
6.3%
14.6%
29.6%
70.4%
85.4%
93.8%
Distance from
Reference
Point to
Traverse Point,
inches
3.00
3.67
4.87
8.13
9.33
10.00
Port
Compass Direction
Northwest
Vertical Duct - Top View
Comments: Note that the FT1R and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Row measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E4.WK4 09/29/97 10:12 AM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: SBS Line - Modified Bitumen Mixing Tank M11 Outlet (E5)
Date: 09/22/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for paniculate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
10.250 inches
2.500 inches
7.750 inches
18 inches, (
20 inches, (
16
24
7.75 inches
8
2.50 inches
0.328 fP
2.3 D)
2.6 D)
Traverse
Point
1
2
3
4
5
6
7
8
Percent of
Duct Diameter
from Wall to
Traverse Point
6.5%
10.5%
19.4%
32.3%
67.7%
80.6%
89.5%
93.5%
Distance from
Reference
Point to
Traverse Point,
inches
3.00
3.31
4.00
5.00
7.75
8.75
9.44
9.75
Port
Compass Direction
East
Horizontal Duct - Flow Away From Observer
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
configuration and accessibility do not provide adequate measurement conditions.
Flow measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E5.WK4 09/29/97 10:13 AM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
ClientfSource: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: APP Line - Modified Bitumen Mbdng Tank M1 Outlet E2B (E6)
Date: 09/22/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for participate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct:
Cross sectional area of sampling location:
10.500 inches
2.750 inches
7.750 inches
44 inches, (
27 inches, (
16
20
7.75 inches
8
2.75 inches
0.328 ft3
5.7 D)
3.5 D)
Traverse
Point
1
2
3
4
5
6
7
8
Percent of
Duct Diameter
from Wall to
Traverse Point
6.5%
10.5%
19.4%
32.3%
67.7%
80.6%
89.5%
93.5%
Distance from
Reference
Point to
Traverse Point,
inches
3.25
3.56
4.25
5.25
8.00
9.00
9.69
10.00
Port
Compass Direction
Southwest
Horizontal Duct - Flow Away From Observer
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Flow measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E6.WK4 09/29/97 10:13 AM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No.
Client/Source:
Sampling Location:
Date:
Measured by
3804.21.04.03
U.S. EPA-EMC /.U.S. Intec, Inc., Port Arthur, Texas
Coater Vent E1 OS for APP Line (E7)
09/23/97
J. Surman
Port-East
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Port- South
Inside of far wall to outside reference point (distance LJ):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (LJ - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for participate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
Traverse
Point
1
2
3
4
5
6
7
8
9
10
Percent of
Duct Diameter
from Wall to
Traverse Point
3.4%
8.2%
14.6%
22.6%
34.2%
65.8%
77.4%
85.4%
91.8%
96.6%
Distance from
Reference
Point to
Traverse Point,
inches
4.25
5.62
7.50
9.81
13.16
22.34
25.69
28.00
29.88
31.25
32.125 inches
3.250 inches
28.875 inches
32.375 inches
3.250 inches
29.125 inches
166 inches, (
54 inches, (
16
20
29.00 inches
10
3.25 inches
4.587 fP
5.7 D)
1.9 D)
Port East
Port South
Port for FTIR/THC
Compass Direction
South
Vertical Duct - Top View
Comments: Note that the sampling location for FTIR and THC is 11 inches below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E7.WK4 09/29/97 10:23 AM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: Coater Vent E20S for SBS Line (E8)
Date: 09/23/97
Measured by J. Surman
Port- East
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Port - South
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
32.125 inches
3.250 inches
28.875 inches
32.375 inches
3.250 inches
29.125 inches
176 inches, (
65 inches, (
12
16
29.00 inches
8
3.25 inches
4.587 ff
6.1 D)
2.2 D)
Traverse
Point
1
2
3
4
5
6
7
8
Percent of
Duct Diameter
from Wail to
Traverse Point
3.4%
10.5%
19.4%
32.3%
67.7%
80.6%
89.5%
96.6%
Distance from
Reference
Point to
Traverse Point,
inches
4.25
6.29
8.87
12.62
22.88
26.63
29.21
31.25
Port East
Port South
Port for FTIR/THC
Compass Direction
South
Vertical Duct -Top View
Comments: Note that the sampling location for FT1R and THC is 14 inches below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E8.WK4 09/29/97 10:20 AM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No.
Client/Source:
Sampling Location:
Date:
Measured by
3804.21.04.03
U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Thermal Oxidizer Inlet Duct (E1)
09/20/97
J. Surman
Port-A
Port- B
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (U - Lo):
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticufate) traverses:
Minimum number of points for participate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter
Length of port fronyeference point to inside surface of duct
Cross sectional area of sampling location:
Traverse
Point
1
2
3
4
5
6
Percent of
Duct Diameter
from Wall to
Traverse Point
4.4%
14.6%
29.6%
70.4%
85.4%
95.6%
Distance from
Reference
Point to
Traverse Point,
inches
7.57
11.27
16.65
3T.35
36.73
40.43
0*3
42.000 inches
6.000 inches
36.000 inches
42.000 inches
6.000 inches
36.000 inches
288 inches, (
72 inches, (
12
12
36.00 inches
6
6.00 inches
7.069 ft? £,
,
Port A
Port B
Compass Direction
SW
Horizontal Duct - Flow Away From Observer
Comments: Note that the sampling location for FTIR and THC is 3^e6t upstream from this cross
section.
M1CIRCD.WK4 09/15/97 (rav.M1E1.WK4 09/17/97 12:09 PM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Sfiurce: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: Thermal Oxidizer Outlet - Stack (E2)
Date: 09/20/97
Measured by J. Surman
Port - SW
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Port- NW
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for paniculate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
42.000 inches
6.000 inches
36.000 inches
42.000 inches
6.000 inches
36.000 inches
260 inches,
80 inches,
39, o
nches
ft3
Traverse
Point
1
2
3
4
5
6
Percent of
Duct Diameter
from Wall to
Traverse Point
4.4%
14.6%
29.6%
70.4%
85.4%
95.6%
Distance from
Reference
Point to
Traverse Point,
inches
7.57
11.27
16.65
31.35
36.73
40.43
Port
^
*fr
Vertical Duct - Top View
Comments: Note that the sampling location for FTIR and THC fe 12 ipbhes below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E2.WK4 09/17/97 12:10PM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: SBS Line - Modified Bitumen Holding Tank H3 Outlet E19B (E3)
Date: 09/24/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for particulate traverses:
Inside diameter of the duct:
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
16.000 inches
6.000 inches
10.000 inches
100 inches, ( IfcO D)
75 inches, ( -*5 D ) 9(t
8 1,7
8
ULOe-inches 9. Iff"
4
Traverse
Point
1
2
3
4
Percent of
Duct Diameter
from Wall to
Traverse Point
6.7%
25.0%
75.0%
93.3%
Distance from
Reference
Point to
Traverse Point,
inches
6.67
8.50
13.50
15.33
Port
Compass Direction
Horizontal Duct - Flow Away From Observer
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Row measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E3.WK4 09/17/97 12:10PM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: APR Line - Modified Bitumen Holding Tank H1 Outlet E1B (E4)
Date: 09/24/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for paniculate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
14.000 inches
6.000 inches
8.000 inches
54 inches, ( _&#D) 5&
16 inches, (
12
16
8.00 inches
6
<*«» inches
0.349 fP
Traverse
Point
1
2
3
4
5
6
Percent of
Duct Diameter
from Wall to
Traverse Point
6.3%
. 14.6%
29.6%
70.4%
85.4%
93.8%
Distance from
Reference
Point to
Traverse Point,
inches
6.50
7.17
8.37
11.63
12.83
13.50
3,oo
U1
•a?
9,1$
433
j6&>
Port
Compass Direction
Vertical Duct - Top View
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Row measurements are made before and after pollutant sampling through the
single port. One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E4.WK4 09/17/97 12:10PM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03 ^
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: SBS Line - Modified Bitumen Mixing Tank M* Outte(E17a(E5)
Date: 09/24/97 *.
Measured by J. Surman ''
—
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for paniculate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
14.000 inches
6.000 inches
8.000 inches
30 inches, (
16 inches, (
16
24
D )
D)
^
/$
00
Traverse
Point
1
2
3
4
5
6
7
8
Percent of
Duct Diameter
from Wall to
Traverse Point
6.3%
10.5%
19.4%
32.3%
67.7%
80.6%
89.5%
93.8%
Distance from
Reference
Point to
Traverse Point,
inches
6.50
6.84
7.55
8.59
11.41
12.45
13.16
13.50
$,#>
3,3)
WO
•SifG
7.7?
y)/&
(V |J ^
Port
Compass Direction
Horizontal Duct - Flow Away From Observer
Comments: Note that the FTIR and THC sampling is conducted in this cross section. Duct
configuration and accessibility do not provide adequate measurement conditions.
Row measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E5.WK4 09/17/97 12:11 PM)
-------
40 CFR 60, APPENDIX A, METHODS 1 and 1A -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: APP Line - Modified Bitumen Mixing Tank M1 Outlet E2B (E6)
Date: 09/24/97
Measured by J. Surman
Inside of far wall to outside reference point (distance Li): 14.000 inches
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonpartculate) traverses:
Minimum number of points for participate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
6.000 inches
8.000 inches
50 inches, ( &k D )
20 inches, ( -26. D )
8.00 inches
XV
•free-inches
Traverse
Point
1
2
3
4
5
6
r
Percent of
Duct Diameter
from Wall to
Traverse Point
6.3%
14.6%
29.6%
70.4%
85.4%
93.8%
Distance from
Reference
Point to
Traverse Point,
inches
6.50
7.17
8.37
11.63
12.83
13.50
3.3?
3.31.
V»*5~
.5.«5"
9,aO
Vtf
J6.CC
\
Port
Compass Direction
South
Horizontal Duct - Row Away From Observer
Comments: Note that the FT1R and THC sampling is conducted in this cross section. Duct
location and accessibility do not provide adequate measurement conditions.
Flow measurements are made before and after pollutant sampling through the
single port One traverse is used because flow rate is very low and velocity
variation across the duct is not significant enough to affect representativeness
of the measurements.
M1CIRCD.WK4 09/15/97 (rev. M1E6.WK4 09/17/97 12:11 PM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: Coater Vent E1 OS for APP Line (E7)
Date: 09/25/97
Measured by J. Surman
Port- NE
Port- SE
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for participate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct:
Cross sectional area of sampling location:
Traverse
Point
1
2
3
4
5
6
7
8
9
i"
Percent of
Duct Diameter
from Wall to
Traverse Point
3.4%
6.7%
11.8%
17.7%
25.0%
35.6%
64.4%
75.0%
82.3%
88.2%
93.3%
96.6%
Distance from
Reference
, Point to
Traverse Point,
inches
... 7.00
V7.94
9.43
11.14
13.25
16.31
24.69
27.75
29.86
31.57
33.06
34.00
35.000 inches
6.000 inches
29.000 inches
35.000 inches
6.000 inches
29.000 inches
110 inches, (
102 inches, (
16 v
29.00 inches
XT JO
4.587 fl?
Port NE
Port SE
Compass Direction
SE
Vertical Duct - Top View
Comments: Note that the sampling location for FTIR and THC is 12 inches below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E7.WK4 09/17/97 12:11 PM)
-------
40 CFR 60, APPENDIX A, METHOD 1 -
LOCATION OF TRAVERSE POINTS IN A CIRCULAR DUCT
MRI Project No. 3804.21.04.03.
Client/Source: U.S. EPA-EMC / U.S. Intec, Inc., Port Arthur, Texas
Sampling Location: Coater Vent E20S for SBS Line (E8)
Date: 09/25/97
Measured by J. Surman
Port- NE
Inside of far wall to outside reference point (distance Li): 35.000 inches
Inside of near wall to outside reference point (distance Lo): 6.000 inches
Duct inside diameter (Li - Lo): 29.000 inches
Port- SE
Inside of far wall to outside reference point (distance Li):
Inside of near wall to outside reference point (distance Lo):
Duct inside diameter (Li - Lo):
Nearest flow disturbance upstream from ports:
Nearest flow disturbance downstream from ports:
Minimum number of points for velocity (nonparticulate) traverses:
Minimum number of points for paniculate traverses:
Inside diameter of the duct
Number of traverse points to be used on a diameter:
Length of port from reference point to inside surface of duct
Cross sectional area of sampling location:
35.000 inches 32
6.000 inches
29.000 inches
110 inches, (
102 inches, (
29.00 inches
-&00" inches
4.587 «•
Traverse
Point
1
2
3
4
5
6
7
ci>
9
10
11
12
'
Percent of
Duct Diameter
from Wall to
Traverse Point
3.4%
6.7%
11.8%
17.7%
25.0%
35.6%
64.4%
75.0%
82.3%
88.2%
93.3%
96.6%
Distance from
Reference
Point to
Traverse Point,
inches
- 7.00
7.94
9.43
11.14
13.25
16.31
24.69
27.75
29.86
31.57
33.06
- 34.00
j
*
4,^
b-2-9
$&7
t <4 {f 2/
fit**
y.b-tf''
&.*>
y.jty
Port
Port SE
Compass Direction
SE
Vertical Duct - Top View
Comments: Note that the sampling location for FTIR and THC is 12 inches below (upstream
from) this cross section.
M1CIRCD.WK4 09/15/97 (rev. M1E8.WK4 09/17/97 12:12PM)
-------
PROJECT NO.
PLANT;
FTIR FIELD DATA FORM
Sampling Location Data
r
INLET
SAMPLE
TIME
/o
DELTA P
IN. 1120
O.dj
O.OJ
O.O/
0.0)
o -o/
O.oi
GO/
O^L
O.OI
O,q/
O.o/
n.oi
O.OI
STACK
TEMP.
9V
TO
^
PROBE
TEMP.
30;
302
3 00
Joo
Jo/
302.
FILTER
TEMP.
503
30 /
3o?
303
-30S-
3oc/
303
"30£~
JOT
DATE:
BAROMETRIC:
OPERATOR:
OUTLET
SAMPLE
TIME
1 /
M
if
DELTA P
IN. II2O
o./r
o-/
-------
PROJECT NO.
PLANT;
0" '
FTIR FIELD DATA FORM
Sampling Location Data
DATE:
INLET
SAMPLE
TIME
/03O
SO;
DELTA P
IN. H2O
0-0 /
O.o|
0,0 1
o-o/
O.Of
O-C/j
O.o
O,o»
STACK
TEMP.
s
PROBE
TEMP.
30V
loo
see
50 /
30/
FILTER
TEMP.
303
3C/?
^00
3o/
BAROMETRIC;
OPERATOR:
OUTLET
SAMPLE
TIME
10
tlOo
DELTA P
IN. II2O
o,/r
STACK
TEMP.
M-
PROBE
TEMP.
FILTER
TEMP.
509
305"
3-05
JO?
301/
MIDWEST RESEARCH INSTITUTE
My Documenls/FTIRFORM/FieldaUl.XLS
09-15-97
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Location Data
INLET
SAMPLE
TIME
10
•805^
DELTA P
IN. II2O
0,01
0.01
l.O/
o.oi
^3t
o.oi
0,01
0,01
STACK
TEMP.
90
w-
air
PROBE
TEMP.
303
3QZ.
302,
303
FILTER
TEMP.
303
3
Sfr
(30^
303
303
30,3
300
DATE:
BAROMETRIC;
OPERATOR:
OUTLET
SAMPLE
TIME
r/o
**'
DELTA P
IN. 1120
a/5-
n.
rr.
, /r
0,1$
STACK
TEMP.
2
V
VAf
PROBE
TEMP.
-3CV
503
^99
FILTER
TEMP.
30V
i.
MIDWEST RESEARCH INSTITUTE
My DocumenlVKTIRFORM/Ficldalal.XLS
09-15-97
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Location Data
SAMPLE
TIME
f
INLET-
DELTA P
IN. II2O
0
0.11
0.7O
o.o
0,09
Q.7 d
STACK
TEMP.
/or
o
fr
W
/osr
O
PROBE
TEMP.
3o/
300
Soo
e?-/
300*
-30 /
30
•30/
FILTER
TEMP.
SCO
2-99
Sot
3 or"
So
DATE:
BAROMETRIC:
OPERATOR:
OUTLET-
SAMPLE
TIME
/rvr o.
DELTA P
IN. 1I2O
0.63
n^L
0^3
o,
O.61
0
met
STACK
TEMP.
_£y_
J^L
H*
/a/
PROBE
TEMP.
FILTER
TEMP.
3 cxs/
3oj
<**.
. ^"
MIDWEST RESEARCH INSTITUTE
My Dociimcnts/FTIRFORM/FicldaUl.XLS
09-J 3-97
-------
PROJECT NO.
PLANT; ().£
FTIR FIELD DATA FORM
Sampling Location Data
DATE:
BAROMETRIC:
OPERATOR:
'INLET SV85 i
SAMPLE
TIME
O7ZO
0?30
1030
10 qo
(OSt)
/ICW
4i
3o
\ltfn
DELTA P
IN. H2O
o.^r?
0.65
STACK
TEMP.
4i
»
FILTE
TEMP.
soy
MIDWEST RESEARCH INSTITUTE
My Documents/FTlRFORM/Fieldala 1 .XLS
09-15-97
-------
PROJECTS.
PLANT: OS
-03
FTIR FIELD DATA FORM
Sampling Location Data
DATE:
BAROMETRIC
OPERATOR:
INLET
SAMPLE
TIME
/?°q
DELTA P
IN. H20
STACK
TEMP.
2/2_
2/4
PROBE
TEMP.
3X30
302
309
-300
7W //
FILLER
TEMP.
3 co
3 05
OUTLET
SAMPLE
TIME
DELTA P
IN. UIO
STACK
TEMP.
PROBE
TEMP.
FILTER
TEMP.
MIDWEST RESEARCH INSTITUTE
My Documenls/FTIRFORM/Fieldalal.XLS
09-15-97
-------
PROJECT NO.
FTIR FIELD DATA FORM
Sampling Location Data
BAROMETRIC;
PLANT;
DATE:
^Iftn*) OPERATOR: J^/*** tJ* tZob*
1 f
OUTLET j
SAMPLE
TIME
'
DELTA P
IN. II2O
STACK
TEMP.
PROBE
TEMP.
FILTER
TEMP.
'
1
v4r
MIDWEST RESEARCH INSTITUTE
My Documenls/FTIRFORM/Fieldatal.XLS
09-15-97
-------
PROJECT NO.
PLANT:
-?/~ 0^-03
FTIR FIELD DATA FORM
Sampling Location Data
DATE:
INLET
SAMPLE
TIME
/20
DELTA P
IN. H20
o,/e
0,0^
o.oo
STACK
TEMP.
/O
Jo4
las1-
PROBE
TEMP.
3C8
301
FILTER
TEMP.
/J«K
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
DELTA P
IN. H2O
Q&t-
o.vy
6r
t?.oy
€W-
OUTLETjilyy*
STACK
TEMP.
^5^-
-*52-
PROBE
TEMP.
W
3oV
301
FILTER
TEMP.
-3oy
MIDWliST RESEARCH INSTITUTE
My Documcnls/I-TIKFORM/Ficldatal XLS
09-15-97
-------
APPENDIX B
THC ANALYZER DATA
-------
Run1 TO Chart 1
Run 1 Thermal Oxidizer Inlet/Outlet
100
90
80
70
60
50
u
JE 40
30
20
10
• i ;>'.:-: :;r:!:', ?:::;;:.!.'-.i^:!:ii\:';i::n!n.. :>•tirii!:.:::;J-; tiriSi^riJiiW'1!^'-.' ;':,:;ii:!:r,;!s''il;:;i:i :i;|H!ih^rF!loJll!fi!;iliE|M-,!i;:!!^:!it:;:p^- ^M
;'..;:: •;:'.;:-M:.!'.',!U!;V:MI;^i;Jf!i;1i;fi!;!!i:ii!i:::-Hi-,r i^h ^rirnljj^
-Inlet
-Outlet!
1450
1520
1550
1620
1650 1720
Time (24-hr clock)
1800
1830
1900
Page 1
-------
A Chart 1
Run 2 Thermal Oxidizer Inlet/Outlet I
1015
1045
1115
1145
1215 1245
Time (24-hr clock)
1315
1345
1415
-------
A Chart 2
100
90
80
70
60
o
O
50
40
30
20
10
Run 3 Thermal Oxidizer Inlet/Outlet!
j%!»HM yfe'W'^:''•!
".'ilffi-^, iHj yifff tti J v'i',1" r',k," ;'
".^jHiujH jftifr/i il!l ^'', • •'-; :.
i i i , !«i i'< i • '••! ~ !< ,,-1• " , - >
in,11
1710
1740
1810
1840
1910 1940
Time (24-hr)
2010
2040
2110
-Outlet
-Inlet
2140
Pagel
-------
A Chart 1
Run 1 APP Coater Roof Stack
16
14
12
10
I
\ 8
o
1335 1340 1345 1350 1355 1400 1405
Time (24-hr clock)
1410
1415
1420
1425
1430
Pagel
-------
A Chart 1
Run 2 APP Coater Roof Stack I
30
25
20
15
o
10
1510 1515 1520 1525 1530 1535 1540 1545
Time (24-hr clock)
1550 1555 1600 1605 1610 1615
Page 1
-------
A Chart 1
Run 3 APP Coater Roof Stack
1631
1636 1641 1646 1651
1656 1701 1706
Time (24-hr)
1711 1716
1721
1726 1731
Pagel
-------
A Chart 1
Run 1 SBS Coater Roof Stack!
30
25
20
7 15
o
10
1443 1448 1453 1458 1503 1508 1513
Time (24-hr clock)
1518
1523
1528
1533
1538
Pagel
-------
A Chart 1
Run 2 SBS Coatar Roof Stack!
O 3
922
927 932
937
942
947
952 957
Time (24-hr)
1002 1007 1012 1017 1022
Pagel
-------
A Chart 1
Run 3 SBS Coater Roof Stack
1040 1045 1050 1055
1100 1105 1110 1115
Time (24-hr clock)
1120
1125 1130 1135 1140
Page 1
-------
A Chart 1
2500
APP Mixing Tank 11
1420 1425 1430 1435 1440 1445 1450 1455
Time (24-hr clock)
1500 1505
1510 1515
1520
Pagel
-------
A Chart 1
[SBS Mixing Tank 111
250
200
150
3
u
jE 100
50
1800 1805 1810 1815
1820 1825 1830 1835
Time (24-hr clock)
1840
1845 1850
1855
Pagel
-------
A Chart 1
SBS Holding Tank 3\
350
300
250
i
200
u
U 150
100
50
1115 1120
1125 1130 1135 1140 1145 1150
Time (24-hr clock)
1155
1200
1205
1210
Page 1
-------
A Chart 1
APP Holding Tank 11
900
600
700
600
I
s 50°
d
c
U 400
U
300
200
100
1634
1635
1636
1637 1638
Time (24-hr clock)
1639
1640
1641
Page 1
-------
U.S. Intec
Run 1 Themal Oxidizer
Date 9/22/97
Operator Gulick
Time THC THC
(24 hr) Inlet Outlet
(ppm) (ppm)
Inlet Outlet
1450 10
1451 10
1452 10
1453 10
1454 10
1455 10
1456 10
1457 10
1458 10
1459 10
1500 10
1501 10 ,
1502 10
1503 10
1504 10
1505 10
1506 10
1507 10
1508 10
1509 10
1510 10
1511 10
1512 10
1513 10
1514 10
1515 10
1516 10
1517 9
1518 9
1519 10
1520 60
1521 65
1522 65
1523 65
1524 70
1525 70
1526 75
1527 75
1528 80
-------
1529
1530
1531
1532
1533
1534
1535
1536
1537
1538
1539
1540
1541
1542
1543
1544
1545
1546
1547
1548
1549
1550
1551
1552
1553
1554
1555
1556
1557
1558
1559
1600
1601
1602
1603
1604
1605
1606
1607
1608
1609
1610
1611
1612
1613
1614
1615
1616
90
100
90
80
75
80
80
80
80
80
80
75
75
75
75
75
75
70
70
70
70
9
9
9
9
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
-------
1617
1618
1619
1620
1621
1622
1623
1624
1625
1626
1627
1628
1629
1630
1631
1632
1633
1634
1635
1636
1637
1638
1639
1640
1641
1642
1643
1644
1645
1646
1647
1648
1649
1650
1651
1652
1653
1654
1655
1656
1657
1658
1659
1700
1701
1702
1703
1704
60
60
60
60
60
65
65
65
65
65
65
65
65
65
65
65
65
65
65
65
70
70
70
70
70
70
70
70
70
70
5
5
5
5
5
5
5
5
5
5
5
5
5
5
-------
1705
1706
1707
1708
1709
1710
1711
1712
1713
1714
1715
1716
1717
1718
1719
1720
1721
1722
1723
1724
1725
1726
1727
1728
1729
1730
1731
1732
1733
1734
1735
1736
1737
1738
1739
1740
1741
1742
1743
1744
1745
1746
1747
1748
1749
1800
1801
1802
90
90
85
80
80
80
80
80
80
80
80
75
70
70
70
70
70
70
70
70
70
70
75
75
75
5
5
5
-------
1803
1804
1805
1806
1807
1808
1809
1810
1811
1812
1813
1814
1815
1816
1817
1818
1819
1820
1821
1822
1823
1824
1825
1826
1827
1828
1829
1830
1831
1832
1833
1834
1835
1836
1837
1838
1839
1840
1841
1842
1843
1844
1845
1846
1847
1848
1849
1850
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
75
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
-------
1851
1852
1853
1854
1855
1856
1857
1858
1859
1900
1901
1902
1903
1904
1905
1906
1907
1908
1909
1910
1911
1912
1913
1914
1915
1916
1917
1918
1919
1920
1921
1922
1923
1924
1925
1926
75
75
75
75
75
5
5
5
5
5
5
5
5.
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
1 THC Cone. (w«t ppm) |
100
80
60
40
20
0
14
«, ' 1
Run 1 Thermal Oxidizer Inlet/Outlet)
Av \j
*\
Inlet I
Outlet!
50 1520 1550 1620 1650 1720 1800 1830 1900
Tim* (24-hr clock)
-------
U.S. Intec
Run 2 Themal Oxidizer
Date 9/23/97
Operator Gulick
Time
(24 hr)
Time (24-hr)
1015
1016
1017
1018
1019
1020
1021
1022
1023
1024
1025
1026
1027
1028
1029
1030
1031
1032
1033
1034
1035
1036
1037
1038
1039
1040
1041
1042
1043
1044
1045
1046
1047
1048
1049
1050
1051
1052
THC
Outlet
(ppm)
Outlet
0.1
0.1
0.2
0.0
0.0
0.1
0.1
0.0
0.1
0.0
0.1
0.0
0.1
0.1
0.1 .
0.1
0.0
0.1
0.2
0.1
0.0
0.1
0.0
0.1
0.0
0.1
0.1
0.1
0.1
0.1
THC
Inlet
(ppm)
Inlet
87.8
90.8
91.7
90.8
88.7
89.3
87.3
90.3
-------
1053
1054
1055
1056
1057
1058
1059
1100
1101
1102
1103
1104
1105
1106
1107
1108
1109
1110
1111
1112
1113
1114
1115
1116
1117
1118
1119
1120
1121
1122
1123
1124
1125
1126
1127
1128
1129
1130
1131
1132
1133
1134
1135
1136
1137
1138
1139
1140
1.1
0.6
0.5
0.4
0.2
0.2
0.3
0.2
0.2
0.1
0.1
0.1
0.0
0.1
0.1
0.1
0.1
0.0
0.1
0.0
0.0
0.0
0.1
0.1
0.0
0.0
0.0
88.4
89.1
89.8
88.3
89.9
91.7
90.3
89.8
88.1
86.5
85.5
87.1
84.1
84.0
86.5
86.2
89.7
86.4
86.3
87.1
-------
1141 0.0
1142 0.0
1143 0.1
1144 0.0
1145 -0.1
1146 0.0
1147 63.7
1148 65.1
1149 64.4
1150 66.9
1151 64.6
1152 66.7
1153 64.7
1154 64.8
1155 65.6
1156 65.8
1157 66.9
1158 65.9
1159 65.3
1200 63.6
1201 65.0
1202 65.0
1203 65.9
1204 66.4
1205 67.4
1206 67.3
1207 67.5
1208 67.6
1209 69.0
1210 68.5
1211 69.2
1212 69.4
1213 69.6
1214 Port Change
1215
1216
1217
1218
1219
1220
1221
1222
1223
1224
1225
1226
1227
1228
-------
1229
1230
1231
1232
1233
1234
1235
1236
1237
1238 "
1239
1240 Offline
1241
1242
1243
1244
1245
1246
1247
1248
1249
1250
1251 60.9
1252 62.5
1253 62.2
1254 62.0
1255 62.3
1256 61.2
1257 61.5
1258 65.1
1259 62.8
1300 62.6
1301 61.1
1302 62.4
1303 61.8
1304 65.0
1305 64.3
1306 64.4
1307 65.5
1308 65.7
1309 65.8
1310 65.2
1311 66.6
1312 67.4
1313 67.2
1314 67.5
1315 67.9
1316 68.3
-------
1317
1318
1319
1320
1321
1322
1323
1324
1325
1326
1327
1328
1329
1330
1331
1332
1333
1334
1335
1336
1337
1338
1339
1340
1341
1342
1343
1344
1345
1346
1347
1348
1349
1350
1351
1352
1353
1354
1355
1356
1357
1358
1359
1400
1401
1402
1403
1404
1.0
0.5
0.3
0.2
0.1
0.1
0.1
0.2
0.1
0.1
0.1
0.0
0.0
0.0
0.0
0.0
-0.1
-0.1
-0.1
0.0
-0.1
0.0
-0.1
-0.1
0.0
0.0
-0.1
-0.1
-0.2
0.0
-0.1
69.8
70.7
80.1
77.3
74.4
73.1
73.0
73.6
73.1
73.6
73.8
79.4
74.3
74.3
73.2
74.6
74.4
-------
1405
1406
1407
1408
1409
1410
1411
1412
1413
1414
1415
1416
1417
1418
1419
1420
1421
1422
1423
1424
1425
1426
1427
1428
1429
1430
1431
1432
1433
1434
1435
1436
1437
1438
1439
1440
,M
I
«!
j
\
(.
0.0
-0.1
0.0
-0.2
-0.1
75.2
76.0
73.9
75.0
74.1
74.9
73.1
72.7
71.
70.
71.
70.
69.
68.
5
9
0
0
5
9
67.2
67.
7
68.4
67.
67.
67.
64.
65.
66.
6
7
3
9
3
0
64.2
63.
63.
62.
62.
62.
5
3
3
2
5
63.2
Run 2 Thermal Oxidlzer Inlet/Outlet)
- inn n
[ 80.0 -" '*^to"
i 60.0 •
i 40.0 ~
' 'irt A. "
i ^U.U •
r in n
. _^ juu , - ^
Outlet 1
Inlet 1
-
1015 1045 1115 1145 1215 1245 1315 1345 1415
Tim* (24-hr clock)
-------
U.S. Intec
Run 3 Thermal Oxidizer
Date: 9/23/97
Operator: Gulick
Time
(24 hr)
1710
1711
1712
1713
1714
1715
1716
1717
1718
1719
1720
1721
1722
1723
1724
1725
1726
1727
1728
1729
1730
1731
1732
1733
1734
1735
1736
1737
1738
1739
1740
1741
1742
1743
1744
1745
1746
1747
1748
THC Outlet THC Inlet
(ppm) (ppm)
Outlet Inlet
81.3
81.0
79.4
80.9
82.1
83.3
82.6
84.1
83.7
85.7
86.3
87.2
87.4
87.0
89.7
89.8
88.7
89.5
89.0
88.9
88.5
90.1
91.4
92.3
91.6
89.6
91.7
91.4
92.9
91.6
0.9
0.6
0.3
0.3
0.3
0.2
0.2
0.2
0.2
-------
1749
1750
1751
1752
1753
1754
1755
1756
1757
1758
1759
1800
1801
1802
1803
1804
1805
1806
1807
1808
1809
1810
1811
1812
1813
1814
1815
1816
1817
1818
1819
1820
1821
1822
1823
1824
1825
1826
1827
1828
1829
1830
1831
1832
1833
1834
1835
1836
0.2
0.1
0.1
o;i
0.1
0.1
0.2
0.2
0.1
0.1
0.1
0.1
0.1
0.2
0.1
0.1
0.1
0.1
0.0
0.1
0.2
88.8
86.3
85.8
84.8
83.4
82.7
83.5
81.5
82.1
81.8
79.3
79.0
79.3
78.7
80.4
79.6
82.0
81.8
82.3
83.5
82.2
83.0
82.8
8.1.1
82.1
81.0
82.0
-------
1837
1838
1839
1840
1841
1842
1843
1844
1845
1846
1847
1848
1849
1850
1851
1852
1853
1854
1855
1856
1857
1858
1859
1900
1901
1902
1903
1904
1905
1906
1907
1908
1909
1910
1911
1912
1913
1914
1915
1916
1917
1918
1919
1920
1921
1922
1923
1924
82.1
82.0
80.9
•10
0.5
0.4
0.3
0.2
0.2
0.0
0.1
0.1
0.1
0.1
0.2
0.2
0.2
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.2
0.0
0.1
0.1
0.0
0.1
0.1
0.1
0.1
0.1
Port Change
n
n
n
n
n
n
it
it
n
ii
n
ii
H
-------
1925
1926
1927
1928
1929
1930
1931
1932
1933
1934
1935
1936
1937
1938
1939
1940
1941
1942
1943
1944
1945
1946
1947
1948
1949
1950
1951
1952
1953
1954
1955
1956
1957
1958
1959
2000
2001
2002
2003
2004
2005
2006
2007
2008
2009
2010
2011
2012
82.8
84.8
84.3
85.4
85.2
86.4
86.2
87.6
89.0
90.8
90.1
89.3
87.4
85.7
85.2
82.9
81.3
80.4
79.2
79.6
79.8
80.1
78.8
77.4
77.1
76.9
76.7
77.9
78.0
77.6
79.2
79.3
80.4
80.4
80.0
1.4
0.7
0.5
0.4
-------
2013
2014
2015
2016
2017
2018
2019
2020
2021
2022
2023
2024
2025
2026
2027
2028
2029
2030
2031
2032
2033
2034
2035
2036
2037
2038
2039
2040
2041
2042
2043
2044
2045
2046
2047
2048
2049
2050
2051
2052
2053
2054
2055
2056
2057
2058
2059
2100
0.3
0.3
0.2
0!2
0.3
0.2
0.1
0.2
0.1
0.2
0.1
0.2
0.1
0.1
0.2
0.1
0.1
0.1
0.2
0.0
0.1
0.1
0.0
0.0
0.1
0.1
73.9
75.7
76.6
75.8
76.0
75.4
75.2
74.9
75.1
75.3
76.1
75.2
74.3
74.2
75.5
74.9
75.6
74.1
73.0
74.5
76.1
75.4
-------
2101
2102
2103
2104
2105
2106
2107
2108
2109
2110
2111
2112
2113
2114
2115
2116
2117
2118
2119
2120
2121
2122
2123
2124
2125
2126
2127
2128
2129
2130
2131
2132
2133
2134
2135
2136
2137
2138
2139
2140
0.6
0.6
0.4
0.3
0.2
0.2
0.3
0.2
0.2
0.1
0.1
0.2
0.2
0.2
0.1
0.1
0.1
0.0
0.1
0.1
0.0
0.1
0.1
0.2
0.1
0.1
0.0
0.1
73.7
73.4
73.9
73.1
74.5
73.6
73.6
75.1
76.3
75.4
71.5
81.4
-------
..-. •• ^ ••• I
1710 1740 1810 1840 1910 1940 2010 2040 2110 2140
-------
U.S. Intec
Run 1 - APR Outlet Vent (T1)
Date: 9/24/97
Operator Gulick
Time
(24 hr)
1335
1336
1337
1338
1339
1340
1341
1342
1343
1344
1345
1346
1347
1348
1349
1350
1351
1352
1353
1354
1355
1356
1357
1358
1359
1400
1401
1402
1403
1404
1405
1406
1407
1408
1409
1410
1411
1412
1413
1414
APP-T1
(ppm)
13.7
13.3
13.5
13.4
12.2
12.6
12.7
13.5
12.5
11.4
10.6
10.6
10.4
14.8
12.9
11.2
11.2
11.5
11.1
11.7
12.2
12.0
11.6
11.8
12.0
11.2
10.9
10.8
10.6
10.9
10.8
10.7
10.7
11.7
11.9
10.9
10.5
11.1
10.8
11.8
-------
1415
1416
1417
1418
1419
1420
1421
1422
1423
1424
1425
1426
1427
1428
1429
1430
lii
^ 8
o 6
O .
0 *
1:
11.9
10.6
10.6
11.4
11.9
11.1
12.0
13.7
11.3
10.7
11.5
12.0
11.2
12.0
11.7
12.0
..
•
•
'-
535 1340 1345
APP Coater Roof Stack |
f\. '' A"
^
1350 1355 1400 1405 1410 1415 1420 1425 1430
Time (24-hr clock)
-------
U.S. Intec
Run 2 - App Outlet Vent (T1)
Date: 9/24/97
Operator Gulick
Time
(24 hr)
1510
1511
1512
1513
1514
1515
1516
1517
1518
1519
1520
1521
1522
1523
1524
1525
1526
1527
1528
1529
1530
1531
1532
1533
1534
1535
1536
1537
1538
1539
1540
1541
1542
1543
1544
1545
1546
1547
1548
1549
APP-T1
(ppm)
10.1
11.8
12.6
11.1
7.2
9.3
11.6
11.9
7.2
6.1
5.2
4.7
2.4
20.5
2.5
25.5
18.5
17.0
18.0
15.7
14.7
14.0
13.4
14.4
14.7
14.2
13.7
14.1
15.5
15.3
14.0
13.9
13.2
13.4
14.6
14.8
13.0
12.8
13.3
12.6
-------
1550
1551
1552
1553
1554
1555
1556
1557
1558
1559
1600
1601
1602
1603
1604
1605
1606
1607
1608
1609
1610
1611
1612
1613
1614
1615
OU
"S 25
?1S
J 10
X 5
P
1!
12.5
11.9
11.5
13.1
12.2
12.0
12.4
12.6
11.3
11.6
11.0
12.0
12.0
11.4
12.1
10.6
10.7
11.8
11.0
11.3
11.8
10.9
11.1
11.0
10.4
11.0
Run 2 APP Coater Roof Stack |
- ,i . ' - - - _ . . _.
; • :--.-'"..' ' --------- - - , - : _ U|,|i,_
^S|te^^_ .-';-;?- ^
^\^y^fe¥ H|K; ""'^ **/"*— *N- ^-^>^^->_i^
•"j-'u^ V»^~" — V-"1 --"^ |J 11-" -"''"-. - - - ~ -' '
»€^~-C-~"?>v^jp if"1" '"" i " ' ''
S-T:?-r3r- - >R t- - - -» - ,
510 1515 1520 1525 1530 1535 1540 1545 1550 1555 1600 1605 1610 1615
Time (24-hr clock)
-------
U.S. Intec
Run 3 - APR Outlet Vent (T1)
Date: 9/24/97
Operator Gulick
Time
(24 hr)
1631
1632
1633
1634
1635
1636
1637
1638
1639
1640
1641
1642
1643
1644
1645
1646
1647
1648
1649
1650
1651
1652
1653
1654
1655
1656
1657
1658
1659
1700
1701
1702
1703
1704
1705
1706
1707
1708
1709
1710
APP-T1
(ppm)
10.0
10.3
8.9
9.0
9.3
8.8
10.1
9.5
9.1
9.0
9.6
10.0
8.9
8.9
9.8
10.2
. 9.0
8.9
8.9
9.1
8.9
8.5
9.6
9.3
8.8
8.9
8.7
8.6
9.3
9.5
9.4
9.4
8.9
8.5
8.8
8.6
8.3
8.0
7.7
7.5
-------
17V
171:
171C
171<
171!
17K
1711
17U
1715
172(
172'
172;
172:
172<
172!
172(
172'
172J
1721
173(
173'
173J
173:
173-
173!
1 10
« 8
7 6
o 4
K
I
)
J
•
J
r
3
)
}
I
I
3
I
•
3
7
3
3
3
1
2
3
*
5
A
-
-
c."
331
7.8
8.3
8.4
8.3
7.9
7.9
8.5
8.3
7.9
7.7
8.0
8.1
8.5
8.6
8.5
8.3
8.5
6.1
5.3
5.0
4.8
4.7
4.4
4.0
4.2
Run 3 APP Coater Roof Stack)
yv ^*\« /^
^s*^x^ • ^*^ ^^^ Y
• \^"
_ L - . • .
-.- - 1 ' • ' .
1638 1641 1646 1651 1656 1701 1706 1711 1716 1721 1726 1731
Time (24-hr)
-------
U.S. Intec
Run 1 - SBS Outlet Vent (T2)
Date: 9/24/97
Operator Gulick
Time SBS - T2
(24 hr) (ppm)
1443
1444
1445
1446
1447
1448
1449
1450
1451
1452
1453
1454
1455
1456
1457
1458
1459
1500
1501
1502
1503
1504
1505
1506
1507
1508
1509
1510
1511
1512
1513
1514
18.6
18.3
18.2
18.2
17.9
17.7
17.6
17.5
17.2
17.0
17.0
16.7
16.6
16.0
16.4
16.5
16.1
15.7
15.4
15.8
15.5
15.5
15.5
15.2
15.1
15.7
15.7
15.7
15.7
15.7
15.7
15.7
-------
1515
1516
1517
1516
151S
152C
1521
1522
1523
1524
152£
152€
1527
152£
152$
153C
1531
1532
1532
153^
153J
153€
1537
153*
I25
a
3 20
7 15
J 10
o
f
H
I 1
i 1
1
I 1
I 1
> 1
1
! 2
I 2
I 2
> 1
J 2
r 2
J 2
) 2
) 2
2
> 2
) 2
L 2
> 1
J 1
' 1
J 1
.
• .
t,t
r' "
»—
143 1448 1
5.7
5.7
0.9
2:1
3.7
5.2
4.8
.6.0
I5.7
!0.8
7.6
!0.6
12.1
I3.6
!6.1
17.1
!5.8
I4.0
!2.4
>0.8
9.5
8.3
7.1
6.3
Run 1 SBS Coater Roof Stack |
r\--/\'-
/ \ s ^\r
- J V \
^ :, - \^r
~ - I
..
453 1458 1503 1508 1513 1518 1523 1528 1533 1538
Tim* (24-hr clock)
-------
U.S. Intec
Run 2 - SBS Outlet Vent (T2)
Date: 9/25/97
Operator Gulick
Time
(24 hr)
922
923
924
925
926
927
928
929
930
931
932
933
934
935
936
937
938
939
940
941
942
943
944
945
946
947
948
949
950
951
952
953
954
955
956
957
958
959
1000
1001
SBS - T2
(ppm)
4.2
4.3
4.4
4.3
4.4
4.4
4.3
4.4
4.4
4.3
4.3
4.3
4.3
4.3
4.6
4.5
4.4
4.4
4.4
4.3
4.3
4.2
4.4
. 4.3
4.2
4.2
4.3
4.4
4.2
4.2
4.3
4.4
4.5
4.4
4.1
4.1
4.2
4.1
4.8
4.6
-------
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
1015
1016
1017
1018
1019
102Q
1021
1022
1023
1024
1025
1026
7
/
H
fa
0 2
0
JC i
9
4
4
4
4
5
4
4
4
4
4
4
6
5
4
4
4
4
4
4
4
4
5
4
4
4
* *
•!~
i^sT \ j..~
IZ-_t.. - j--_.
*•=£-•:. 1" -"• "!,">'
£ ^ ." -" ;.L
22 927 932
.6
6
.6
.6
.4
.5
.4
.6
.7
.5
.5
.1
.3
.8
.5
.7
.8
.6
.4
.3
.4
.3
.8
.3
.4
Run 2 SBS Coater Roof Stack |
L
'"* L^-^j^^A^A.
' iy-"" "'
i.~~* ' '
J! "jj _" '
•,"« • I I i > 1 1 •
937 942 947 952 957 1002 1007 1012 1017 1022
Tim* (24-hr)
-------
U.S. Intec
Run 3 - SBS Outlet Vent (T2)
Date: 9/25/97
Operator: Gulick
Time
(24 hr)
1040
1041
1042
1043
1044
1045
1046
1047
1048
1049
1050
1051
1052
1053
1054
1055
1056
1057
1058
1059
1100
1101
1102
1103
1104
1105
1106
1107
1108
1109
1110
1111
1112
1113
1114
1115
1116
1117
1118
1119
SBS-T2
(ppm)
4.3
4.6
4.6
4.5
4.4
4.6
4.4
4.2
4.4
4.5
4.3
4.0
4.4
4.2
3.9
3.9
4.1
4.2
4.2
4.2
4.2
5.4
4.5
4.3
4.2
4.5
4.7
4.3
4.2
4.2
5.2
4.5
4.3
4.2
4.2
4.3
4.4
4.4
5.0
4.6
-------
1120
1121
1122
1123
1124
1125
1128
1127
1128
1129
1130
1131
1132
1133
1134
1135
1136
1137
1138
1139
114Q
1141
1142
1143
1144
J«
1C
4.5
4.5
4.5
4.8
4.8
4.7
4.9
5.3
4.7
4.4
4.3
4.5
4.7
4.5
4.4
4.8
4.4
4.3
4.3
4.7
4.5
4.2
4.3
4.4
I 4.4
Run 3 SBS Coater Roof Stack |
^^ut^M^
£k r 1{ -~. - T~ ;" " """' -
tfe4V:--^'
MO 1045 1050 1055 1100 1105 1110 1115 1120 1125 1130 1135 1140
Tlii»(24.hr clock)
-------
U.S. Intec
Mixing Tank #1
Date: 9/25/97
Operator Gulick
Time Tank #1
THC
(24 hr) (ppm)
1420 1253
1421 1270
1422 1290
1423 1309
1424 1312
1425 1307
1426 1351
1427 1368
1428 1370
1429 1352
1430 1372
1431 1413
1432 1430
1433 1425
1434 1453
1435 1503
1436 1531
1437 1536
1438 1534
1439 1567
1440 1606
1441 1616
1442 1630
1443 1621
1444 1654
1445 1649
144* 1644
1447 1671
1448 1683
1449 1706
1450 1702
1451 1687
1452 1688
1453 1763
1454 1756
1455 1766
1456 1809
1457 1828
1458 1837
-------
1459
1500
1501
1502
1503
1504
1505
1506
1507
1508
1509
1510
1511
1512
1513
1514
1515
1516
1517
1518
1519
1520
1829
1887
1931
1859
1849
1867
1846
1849
1859
1845
1846
1855
1840
1893
1962
1986
2030
2072
2125
2117
2119
2177
APP Mixing Tank 1 [
2500
2000
150°
1000
500
1420 1425 1430 1435 1440 1445 1450 1455 1500 1505 1510 1515 1520
Tim* (24-hr clock)
-------
U.S. Intec
Mixing Tank #11
Date: 9/25/97
Operator Gulick
Time
(24 hr)
1800
1801
1802
1803
1804
1805
1806
1807
1808
1809
1810
1811
1812
1813
1814
1815
1816
1817
1818
1819
1820
1821
1822
1823
1824
1825
1826
1827
1828
1829
1830
1831
1832
1833
1834
1835
1836
1837
1838
Tank #11
THC
(ppm)
227
219
211
207
196
191
170
140
142
165
167
166
162
163
157
. 155
154
154
151
148
147
146
144
142
140
138
138
134
132
134
131
132
133
135
133
132
130
132
130
-------
1839
1840
1841
1842
1843
1844
1845
1846
1847
1848
1849
1850
1851
1852
1853
1854
1855
1856
1857
1858
1859
| 200
a
§ 100
o
| 50
127
129
128
129
127
126
128
127
126
128
132
133
131
130
133
130
131
133
131
132
133
SBS Mixing Tank 11 1
^X-^y . -. -.v
'" ' _ si" i ' r, -
1800 1805 1810 1815 1820 1825 1830 1835 1840 1845 1850 1855
Time (24-hr clock)
-------
U.S. Intec
SBS Holding Tank #3
Date: 9/26/97
Operator: Gulick
Time Tank #3
THC
(24 hr) (ppm)
1115
1116
1117
1118
1119
1120
1121
1122
1123
1124
1125
1126
1127
1128
1129
1130
1131
1132
1133
1134
1135
1136
1137
1138
1139
1140
1141
1142
1143
1144
1145
1146
1147
1148
1149
1150
1151
1152
1153
315
319
313
302
306
302
294
280
279
273
272
266
254
255
245
245
243
238
234
220
223
224
220
216
215
210
210
199
195
202
200
198
197
197
193
194
182
186
189
-------
1154
1155
1156
1157
1158
1159
1200
1201
1202
1203
1204
1205
1206
1207
1208
1209
1210
1211
1212
1213
1214
187
186
184
179
183
182
182
177
179
178
172
174
176
172
177
168
170
174
174
175
175
I
350
300
250
200
150
100
50
SBS Holding Tank 31
1115 1120 1125 1130 1135 1140 1145 1150 1155 1200 1205 1210
Tim* (24-hr clock)
-------
U.S. Intec
APP Holding Tank #1
Date: 9/26/97
Operator: Gulick
Time
(24 hr)
1634
1635
1636
1637
1638
1639
1640
1641
900
3W
1 800
| 700
teoo
500
y 400
3 300
0 200
H 100
Tank*
THC
(ppm)
473
683
771
810
849
874
874
791
X^ '-•---
•
1634 1635
1
APP Holding Tank 1 1
ff*~^
.'
^
1636 1637 1638 1639 1640 1641
Time (24-hr clock)
-------
APPENDIX C
THC CALIBRATION RECORDS
-------
Run 1 Thermal Oxidizer 9/22/97
Calibration Error Determination
Cal Gas Predicted Measured
Value Value Value
THC1
0.0
898.0
502.0
251.0
503.1
251.6
0.0
900.0
500.0
255.0
Difference as
% of Cal Gas
0.0
0.2
0.6
1.4
Pass/Fail
Pass
Pass
Pass
Pass
Pass/Fail Criteria is +/- 5% of Calibration Gas
Calibration Drift Determination
Zero Drift
Initial
Value
THC1 0.0
Final
Value
0.0
Difference as
% of Span
0.0
Pass/Fail
Pass
Instrument Span for THC 1 and 2 is 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 900.0
Final
Value
890.0
Span Drift
Difference as
% of Span
1.0
Pass/Fail
Pass
Instrument Span for THC 1 and 2 is 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
THC1
Run 2 Thermal Oxidizer 9/23/97
Calibration Error Determination
CalGas Predicted Measured
Value Value Value
0.0
90.4
50.3
30.1
50.3
30.4
0.8
89.7
49.9
29.4
Pass/Fail Criteria is +/- 5% of Calibration Gas
Difference as
% of Cal Gas
0.1
0.8
0.7
3.3
Calibration Drift Determination
Zero Drift
Pass/Fail
Pass
Pass
Pass
Pass
Initial
Value
THC 1 0.8
Final
Value
0.4
Difference as
% of Span
0.4
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 89.7
Final
Value
90.1
Span Drift
Difference as
% of Span
0.4
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
SUMMARY OUTPUT
Regression Statistics
Multiple R 1
R Square 1
Adjusted R : 65535
Standard Er 0
Observation 2
ANOVA
df SS
Regression 1 3952
Residual 0 8E-28
Total 1 3952
Coefficients idard E
MS F nificance F
3952 0 #####
65535
t Stat P-valueiwer 95iper 95ver 95. oer 95. C
Intercept 0.8 0 65535 ##### 0.8 0.8 0.8 0.8
X Variable 1 0.9834071 0 65535 ##### 0.983 0.983 0.983 0.983
-------
Run 3 Thermal Oxidizer 9/23/97
Calibration Error Determination
Cal Gas Predicted Measured
Value Value Value
THC 1
0.0.
90.4
50.3
30.1
50.4
30.4
0.6
90.1
50.1
30.1
Pass/Fail Criteria is +/- 5% of Calibration Gas
Difference as
% of Cal Gas
0.1
0.3
0.6
1.0
Calibration Drift Determination
Zero Drift
Pass/Fail
Pass
Pass
Pass
Pass
Initial
Value
THC 1 0.6
Final
Value
0.7
Difference as
% of Span
0.1
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 90.1
Final
Value
90.0
Span Drift
Difference as
% of Span
0.1
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
Run 1- SBS Outlet Vent 9/24/97
Calibration Error Determination
THC1
Cat Gas Predicted Measured
Value Value Value
0.0
90.4
50.3
30.1
50.0
29.9
0.0
90.9
49.4
29.1
Difference as
% of Cal Gas
0.0
0.6
1.2
2.8
Pass/Fail Criteria is +/- 5% of Calibration Gas
Calibration Drift Determination
THC1
Initial
Value
0.0
Zero Drift
Final
Value
0.1
Difference as
% of Span
0.1
Pass/Fall
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Instrument Span for THC 1 is 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Span Drift
Initial
Value
THC 1 90.9
Final
Value
90.3
Difference as
% of Span
0.6
Pass/Fall
Pass
Instrument Span for THC 1 is 100 ppm
Pass/Fail Criteria is W- 3% of Instrument Span
-------
Runs 2 and 3 SBS Outlet Vent (T2) 9/24/97
Calibration Error Determination
Cat Gas Predicted Measured
Value Value Value
Difference as
% of Cal Gas
Pass/Fail
THC1
0.0
90.4
50.3
30.1
50.9
30.5
0.2
91.3
49.4
29.1
0.0
1.0
2.9
4.7
Pass
Pass
Pass
Pass
Pass/Fail Criteria is +/• 5% of Calibration Gas
Calibration Drift Determination
Zero Drift
Initial
Value
THC 1 0.2
Final
Value
0.4
Difference as
% of Span
0.2
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC1 91.3
Final
Value
90.2
Span Drift
Difference as
% of Span
1.1
Pass/Fail
Pass
Instrument Span for THC 1 100 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
SUMMARY OUTPUT
Regression
Multiple R
R Square
Adjusted R :
Standard Er
Observation
ANOVA
Regression
Residual
Total
Statistics
1
1
65535
0
2
df
1
0
1
SS
4150
2E-28
4150
Coefficients idard B
Intercept
X Variable 1
0.2
1.0077434
0
0
MS
4150
65535
tStat
65535
65535
F nificance F
0 #####
P-value>wer 95jper 95ver 95. t
##### 0.2 0.2 0.2
##### 1.008 1.008 1.008
3er95.C
0.2
1.008
1%
-------
Mixing Tank #1 9/25/97
Calibration Error Determination
CalGas Predicted Measured
Value Value Value
THC1
Difference as
% of Cal Gas
0.0
5003.0
2504.0
1002.0
2502.4
1004.2
4.8
4995.0
2509.0
1005.0
0.0
0.2
0.3
0.1
Pass/Fail
Pass
Pass
Pass
Pass
Pass/Fail Criteria is +/- 5% of Calibration Gas
Calibration Drift Determination
Zero Drift
Initial
Value
THC 1 4.9
Final
Value
9.7
Difference as
% of Span
0.5
Pass/Fail
Pass
Instrument Span for THC 1 10000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 4990.0
Final
Value
5014.0
Span Drift
Difference as
% of Span
0.2
Pass/Fail
Pass
Instrument Span for THC 1 10000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
SUMMARY OUTPUT
Regression Statistics
Multiple R
R Square
Adjusted R:
Standard Er
Observation
ANOVA
1
1
65535
0
2
Regression
Residual
Total
df SS MS
1j»j*j*j«j* JAJAJAJAJA
TrTrTtTrTr rrrftfttir
0 2E-25 65535
F nificar
0 Iffltili
E t Stat °-yalu&wer Sfnper 95ver 95, (per 95. 0%
0 65535 "mm .......... 478 .......... 48 ........... 4™8 ........... 4T8~
0 65535 ##### 0.997 0.997 0.997 0.997
ntecept 4.8
X Variable 1 0.9974415
-------
Mixing Tank # 11 9/25/97
Calibration Error Determination
Cal Gas Predicted Measured
Value Value Value
THC1
Difference as
% of Cal Gas
0.0
898.0
502.0
251.0
503.4
252.6
1.9
899.0
491.0
255.0
0.0
0.1
2.5
0.9
Pass/Fail
Pass
Pass
Pass
Pass
Pass/Fail Criteria is +/- 5% of Calibration Gas
Calibration Drift Determination
Zero Drift
Initial
Value
THC1 1.9
Final
Value
0.5
Difference as
% of Span
0.1
Pass/Fail
Pass
Instrument Span for THC 1 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 899.0
Final
Value
896.0
Span Drift
Difference as
% of Span
0.3
Pass/Fail
Pass
Instrument Span for THC 1 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
SUMMARY OUTPUT
Statistics
Multiple R
R Square
Adjusted R :
Standard Er
Observation
>>X'XOflW}*>>>x*K'>»wwfl*»9»»>w«w>>»X'5^
ANOVA
Regression
Residual
^^^^^^^S^L^^^^
,_^^^
1
1
65535
0
2
CWMWWWWWWWWWOW
df SS MS F nificance F
4 J&JUUU& JU4J4J4J4 f^ JXJAJJ^AJA
0 2E-26 65535
1 //////////
^efficients idard E t Staf °-valuewer 95?per 95ver 95.ioer 95. C
Intercept19o65535w191919l9
X Variable 1 0.9989978 0 65535 ##### 0.999 0.999 0.999 0.999
-------
SBS Holding Tank # 3 9/26/97
Calibration Error Determination
THC1
Cal Gas
Value
0.0
898.0
502.0 506.5
251.0 253.2
Measured
Value
0.0
906.0
496.0
248.0
Pass/Fail Criteria is +/- 5% of Calibration Gas
Difference as
% of Cal Gas
0.0
0.9
2.1
2.1
Initial
Value
THC 1 0.0
Calibration Drift Determination
Final
Value
0.5
Zero Drift
Difference as
% of Span
0.1
Pass/Fail
Pass
Pass
Pass
Pass
Pass/Fail
Pass
Instrument Span for THC 1 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
Initial
Value
THC 1 906.0
Final
Value
904.0
Span Drift
Difference as
% of Span
0.2
Pass/Fail
Pass
Instrument Span for THC 1 1000 ppm
Pass/Fail Criteria is +/- 3% of Instrument Span
-------
SUMMARY OUTPUT
MutipeR1
R Square 1
Adjusted R 65535
Standard Er 0
Observatior 2
ANOVA
df SS MS F ?.^?anceF
r\oyrw55ion I fwwww^ #wwww^ \
Residual 0 1E-26 65535
Total 1 mm
Coefficjents jdartEt Stat_°-yaluewer 95^ger d5ver95. oer 95.0%
IrrtercepT 0 b"65535 "mm 0™ """6 "" "0 ™o"
X Variable 1 1.0089087 0 65535 W### 1.009 1.009 1.009 1.009
-------
APPENDIX D
FTIR FIELD DATA RECORDS
-------
TABLED-1. SUMMARY OF FTIR SPECTRAL FILES
Date
9/22
9/23
9/23
Tune
1450-1520
1520-1550
1550-1620
1620-1650
1650-1720
1720-1755
1755-1829
1829-1857
1857-1928
1009-1045
1045-1115
1115-1145
1145-1215
1215-1230
1305-1335
1335-1412
1412-1442
1442-1447
1710-1740
1740-1810
1810-1840
1840-1918
1940-2010
2010-2040
2040-2110
2110-2141
Run No. & Location
Run 1 T.O. Outlet
Run 1 T.O. Inlet
Run 1 T.O. Outlet
Run 1 T.O. Inlet
Run 1 T.O. Outlet
Run 1 T.O. Inlet
Run 1 T.O. Outlet
Run 1 T.O. Inlet
Run 1 T.O. Outlet
Run 2 T.O. Outlet
Run 2 T.O. Inlet
Run 2 T.O. Outlet
Run 2 T.O. Inlet
Run 2 T.O. Outlet
Run 2 T.O. Inlet
Run 2 T.O. Outlet
Run 2 T.O. Inlet
Run 2 T.O. Outlet
Run 3 T.O. Inlet
Run 3 T.O. Outlet
Run 3 T.O. Inlet
Run 3 T.O. Outlet
Run 3 T.O. Inlet
Run 3 T.O. Outlet
Run 3 T.O. Inlet
Run 3 T.O. Outlet
Spectral Files
19220035-19220052
19220053-19220068
19220069-19220080
19220081-19220097
19220098-19220100
19220101-19220104
19220105-19220123
19220124-19220139
19220140-19220158
19230006-19230024
19230025-19230041
19230042-19230060
19230061-19230075
19230076-19230078
19230079-19230095
19230096-19230117
19230118-19230134
19230134-19230138
19230140-19230157
19230158-19230173
19230174-19230191
19230192-19230208
19230209-19230226
19230227-19230243
19230244-19230261
19230262-19230277
Notes
Computer error. Automated
collection of files not working
correctly.
Port change from 1230 to 1305.
Port change from 1918 to 1940.
D-l
-------
TABLE D-l. SUMMARY OF FTIR SPECTRAL FILES (continued)
Date
9/24
9/25
9/26
Time
1318-1437
1437-1510
1510-1610
1610-1739
0921-1026
1040-1144
1404-1520
1801-1902
1115-1216
1331-1431
1707-1808
Run No. & Location
Run 1, APP Coater
Roof Stack
Runl, SBS Coater
Roof Stack
Run 2, APP Coater
Roof Stack
Run 3, APP Coater
Roof Stack
Run 2, SBS Coater
Roof Stack
Run 3, SBS Coater
Roof Stack
Run 1, APP Mixing
Tankl
Run 1, SBS Mixing
Tank 11
Run 1, SBS Holding
Tank 3
Run l.APP Holding
Tankl
Run 2, APP Holding
Tankl
(repeat test)
Spectral Files
19240001-19240044
19240045-19240063
19240064-19240097
19240098-19240147
19250003-19250039
19250045-19250083
19250097-19250139
19250146-19250178
19260007-19260040
19260043-19260075
APP01-APP07
Notes
Test repeated. Spectra were analyzed.
Computer error. Samples collected
manually in batch mode. Samples
APP03 and APP04 are dilutions of
APP02.
D-2
-------
PROJECT NO.
PLANT:
FTIR HELD DATA FORM
Background and Calibration Spectra
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
PRESSURE
BKG
APOD
NOTES
5*0
s
01 5 o
2--5D
ho
A/^AA.
015V
loo
710
8
0751*
foo
l.o
Tie
&
A/AM.
tt&uteji
loo
/-o
TSO
Stro
Z-Vo
lie
fao
en
ho
C-
MIDWEST RESEARCH INSTITUTE
My Documcnis/FnRFORM/Field»u2.XLS
09-15-97
-------
PROJECT NO.
PLANT: P
FTIR FIELD DATA FORM
Background and Calibration Spectra
DATE: 7 A//? 7
BAROMETRIC;
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
PRESSURE
BKG
APOD
NOTES
\'0
~7~>o
c: of i'/
C/3T
fro
A<
-770
lottf
loo
NBA
100
770
loo
T-J
7o
Iz/l*
TTJf
IJY'J
•£
.r'
oO
MIDWEST RESEARCH INSTITUTE
My Docummt!/FT!RK>RM/Fieldau2.XLS
09-15-97
-------
PROJECT NO.
FTIR HELD DATA FORM
Background and Calibration Spectra
BAROMETRIC;
PLANT:
DATE;
OPERATOR:
. f. ?
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-1)
CELL
TEMP(F)
PRESSURE
BKG
APOO
NOTES
h 042-5 A.
A/i.
OS6I
L $ ««y
M'
/J
775"
ft 00
tltfl
'
OO
1,0
I7W
•e/vf
f/l.
loo
,o
•1X9
C(**^
IX'* t S^
•ft
CTS
loo
1.0
•7-70
(00
li
A-
MIDWEST RESEARCH INSTITUTE
My Documenls/rTIRFORM/Reld»u2.XLS
09-15-97
-------
FTIR FIELD DATA FORM
Background and Calibration Spectra
PROJECT NO.
PLANT; PCS
DATE:
BAROMETRIC:.
OPERATOR: J
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
PRESSURE
BKG
APOD
NOTES
A/5H
CIS r
/oo
-770
•770
Ml,
C75 /
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(Background and cc/jbratfan spectra.;
DATE:
9/22/23
BAROMETRIC:
OPERATOR:
GMP/SK
SAMPLE
TIME
8:30
9:25
9/23/97
7:30
7:35
7:50
7:56
10:00
15:34
15:42
16:10
22:15
22:18
FILE
NAME
BO922A
B0922B
BO923A
BO923B
CO923A
CO923B
19230001
CO923C
C0923D
B0923C
C0923E
CO923F
PATH
Inlet/Outlet
N2 Background
N2 Background
N2 Background (Actidently not saved)
CIS w/104.4 ppm ethytene
Dup. CTS w/104.4 ppm elhylene
NUMBER
SCANS
500
500
250
500
100
100
N2 blanks collected as pan of continuous batch (run) for possible back
CTS w/104.4 ppm elhylene
Dup. CTS w/104.4 ppm elhylene
N2 Background
CTS post test 2 104.4 ppm
CTS post lest 2 104.4 ppm
100
100
500
100
100
RES
-------
PROJECT NO. 4701-08-ff
PLANT: Port Arthur
FTIR FIELD DATA FORM
(Background and calibration tpoctra.)
DATE: 9/24/97
BAROMETRIC:
OPERATOR:
29.85
Klamm
SAMPLE
TIME
10:48
10:56
10:59
18:12
18:14
18:16
18:49
18:52
19:06
FILE
NAME
bo924a
co924a
co924b
INSP07
INSP08
INSP09
CO924c
CO924D
FINN2
PATH
N2 background - purge flow
Ethylcne CTS @ 104 ppm
Duplicate of co924a
spike of APP line (Line 1)
MFC #2c 1.0 Ipm (SF6 + cthylene)
Dup. (same as above)
Trip, (same as above)
CTS post test (stopped flow)
CTS duplicate
Final N2 blank - possible background
stored in "Others" file
NUMBER
SCANS
500
100
100
100
100
100
100
100
100
too
RES
(c—I)
CELL
TEMP(F)
240
240
240
240
240
240
240
240
240
240
PRESSURE
770
770
770
770
770
770
770
770
770
770
BKG
A
A
A
A
A
A
A
A
A
APOD
NBM
NBM
NBM
NBM
NBM
NBM
NBM
NBM
NBM
NBM
NOTES
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 9/25/97
BAROMETRIC:
OPERATOR:
29.9J
SAMPLE
TIME
8:38
8:51
8:57
13:00
17:58
19:52
19:56
FILE
NAME
bo925a
co925a
co925b
N201
19250144-0145
C0925C
CO925D
PATH
N2 background
CTS initial (stopped flow)
Duplicate of CO925a (stopped flow)
N2 blanks collected as "Monitor"
w/cell purge - very clean
N2 blanks at beginning of test collected in
"Monitor" mode (contains residual 2900 peak)
Final CTS
Duplicate CTS
NUMBER
SCANS
500
100
100
100
too
100
100
RES
(oo-l)
1
1
1
1
1
1
1
CELL
TEMP(F)
240
240
240
240
240
240
240
PRESSURE
770
770
775
775
770
770
770
BKC
A
A
A
A
A
A
APOD
NBM
NBM
NBM
NBM
NBM
NBM
NBM
NOTES
purge flow
N2 purge
N2 purge
stopped flow
slopped flow
-------
PROJECT NO.
PLANT: Port Arthur
4701-08-05
FTIR FIELD DATA FORM
(Background and calibration spectra.)
DATE: 9Q6/97
BAROMETRIC:
OPERATOR:
fClamm
SAMPLE
TIME
9:25
9:37
9:41
11:05
13:29
16:41
18:19
18:24
18:46
18.48
FILE
NAME
b0926a
c9026a
co926b
19260001-0002
19260041-0042
19260084-85
c0926c
c0926d
PT03
PT04
PATH
N2 background - purge flow
CTS initial
Duplicate
N2 blanks
N2 blanks
N2 blanks
CTS final - purge flow
Duplicate CTS
N2 blank
N2 blank
NUMBER
SCANS
500
100
100
100
100
RES
(«••!)
1
1
1
1
1
CELL
TEMP(F)
240
240
240
240
240
PRESSURE
770
770
770
770
770
BKG
A
A
A
A
APOD
NBM
NBM
NBM
NBM
NBM
NOTES
-------
FTIR FIELD DATA FORM
Sampling Data
PROJECT NO.
PLANT:
OPERATOR:
DATE:
: f [
BAROMETRIC:
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMPOS
SPIKED/
UNSPIKED
SAMPLE
CONO.
SAMPLE
FLOW
CELL
PRESS.
BKt;
-II
I 00
(A
/w
II 3
7
loo
JDO
/oo
Ao
£.0
7/to
6
/oo
l.o
~78o
6
loo
L
?#>
6
-&*•
Ao
7fo
1*0
- fr^f fa*
too
6
/-so
3-c
(4
111*00*1
/aO
/oO
a
'•F**
-7-7S"
/32J
U
it
S
iuflcL
/oC
U
6
ml,
Z '0
s
'Jttffff*
MIIIWIiST RKSIr.ARC:il INSTITUTE
* ir •/
My Ducumenis/FnKTORM/Ficl
-------
FTIR FIELD DATA FORM
Sampling Data
PROJECT NO.
PLANT:
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK START:
LEAK CHECK END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
CELL
PRESS.
BKG
/do
1,0
OUfSfl
net
to*
oo
3 00
77^
loo
(.0
$0-0
Ir*-
MIUWLST RESEARCH INSTITUTE
My Documenis/FnRFORM/Hel
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Data
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cro-l)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
CELL
PRESS,
BKli
looo
14230001
//
U*
/oo
l-o
A/* ifi^mf.
Utt,
1001
300
(,.
/J
Joo
(..0
A
too
ho
fo.O
770
£>
U
(y -
77o
/DO
ho
Wo
6
ov
C4L,
fitrtvTlflbvl a, «>& fVt *•*
loo
B
leo
,*
770
e>
GO 5
loo
ho
K
77o
6
ho
Stt&L-
tt/O
6
/V/2-
2- //
loo
ho
u
6
hO
u
(f
lO
110
ho
u.
(0-O
no
/DO
/-o
Mo
s
/5?3
I'O
Wo
6
MIDWI-ST RJ-SliAKCII INSTITUTE
My Documenii/FTIKFORM/Ficldau3.XLS
09 -15-97
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Data
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION /NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
CONO.
SAMPLE
FLOW
CELL
PRESS.
BKG
HlO
tf&ONa
3r(rnlt*-
to/0
(L,
Mo
loo
t/o
7?o
rtlo
[oo
,0
n MQ 1*12*
too
Wo
il/sr
our^/7
loo
loO
ho
J
la.O
(o o
6 '
0
/JO
10
•770
/Oo
i-0
17 o
Wo
u
-no
2110
1 fo
/•
ZYo
u
6 ^<
77o
422
U
100
V P
770
4
I'O
1-/0
c
MIDWI-ST KI-SHARCII INSI1TUTE
My Documcnls/FnRFORM/Field«u3.XLS
09 1597
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Data
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
SPIKED/
UNSPIKEO
SAMPLE
COND.
SAMPLE
FLOW
CELL
PRESS.
BKG
\W0oot
foo
U
6-0
A/J7
1 &
U
1 ~)O
if to
[00
1,0
2-Vo
t> ,Ct
77^
"7
.&
S
7
A
±
01
(MKflO
c /. o
i
MIIWI3T RI-SHARCII INSTlTim-
My Duaunrals/FnRH)RM/Fieldau3.XLS
-15-97
-------
PROJECT NO.
PLANT:
OPERATOR:
FT1R FIELD DATA FORM
Sampling Data
DATE:
BAROMETRIC:
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-1)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
CELL
PRESS.
BKG
oi/s
£.0
01 1/
-77^
Xf
100
Ac
/-«*:
0*1
/<*>
ill'l
JPO
Lo
2,^0
77<
t'O
5
Thlp
to
A
(a st)
5/ttt:
fgp A.
<,o
^-
Prttt
100
/*»»»
/ o
X-
MIDWEST RESEARCH INSTITUTE
My Doouticnli/FnRK)RM/BeW«u3.XLS
09-15-97
-------
FTIR FIELD DATA FORM
Sampling Data
PROJECT NO.
PLANT:
-2 /
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK-START;
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES.
(cro-1)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
CONO.
SAMPLE
FLOW
CELL
PRESS.
BKG
T/5S
;O
u
M.
(0,0
A
tap
b-0
77o
tfvro
10. O
u.o
770
A
{ • L
LOO
(,,3
77.?
/f
MIDWKST RESEARCH INSTITUTE
My O>cumenis/FnRTORM/Ficl
-------
FT1R FIELD DATA FORM
Sampling Data
PROJECT NO.
PLANT:
OPERATOR:
DATE:
BAROMETRIC:
LEAK CHECK START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMPOO
SPIKED/
UNSP1KED
SAMPLE
COND.
SAMPLE
FLOW
CELL
PRESS.
BKG
i rx+r
loo
M.
/OO
• o
U
Srxoc
STVP
[Zljo
t.
loo
I-*
14
7\
1331
U
77
*'
/
Uc
60 &
ritit-.
loo
(a ,O
77^-
xV
-4°
U
I ArPP
100
\.o
u
I7o7
i-Vo
14
o
77o
/Vo
U
MIDWEST RESEARCH INSTITUTE
My Daciunenli/FnRFORM/FiddMa3.XLS
09-15-97
-------
PROJECT NO.
PLANT:
FTIR FIELD DATA FORM
Sampling Data
OPERATOR:
DATE:
BAROMETRIC: :
LEAK CHECK-START:
LEAK CHECK-END:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION /NOTES
NUMBER
SCANS
RES
(cm-l)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
CONI).
SAMPLE
FLOW
CELL
PRESS.
BK(;
fyk.
1
{ff
A-
MfC
lov
I'O
trv*
?TD*
MIDWI^T RESEARCH INSTITUTE
My Docum«ii
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(FTIR Svrvlliy Out*)
DATE: 9122/97
BAROMETRIC:
OPERATOR:
29.98
Klama
SAMPLE
TIME
10:11
10:53
11:29
11:34
11:39
11:43
11:53
12:05
12:11
12:20
12:25
12:35
14:50
15:20
15:50
16:20
16:50
17:20
17:48
17:55
18:29
18:57
19:56
19:59
20:18
20:21
FILE
NAME
SPSF60I
SPSF602
SPTOL01
SPTOL02
DKTOL01
OUTUN01
OUTUN02
OUTSPOI
OUTSP02
INLUN01
19220035
19220053
19220069
19220081
19220098
19220101
19220105
19220124
19220140
DIR01
DK02
OUTSP03
OUTSP04
INSPOI
INSP02
PATH
Surt ambient 777? monitor
Manual spike tests/ambient
Spike loul flow - 6.0 Ipm (4.08ppm SF6 @ 2.0)
Duplicate (time as above)
rokieae 60.6 ppm @ 2.0 Ipm
Duplicate (same as above)
toluene direct to cell 60.6 ppm
Outlet untpikcd sample
Quite! unspiked sample
Spiked outlet W/SF6 @ 2.0 Ipm
Spiked outlet wAohieoe 60.6 ppm @ 2.0 Ipm
Inlet unspiked sample
"Sampler (Outlet) - First one
(Stan of Test)
"Sampler (Inlet) - Alternate location
Outlet
Inlet
Outlet
Inlet (Batch files not working)
Back on-line (out of memory)
Switch to outlet
Switch to inlet ("Sampk2")
Switch to outlet ("Samptel ")
Direct to call MFC#10 7 <§> 2 0
60.6 toluene 4.08 ppm SF6, 104 ppm p-xylenc
Duplicate of DIR01
(also use as direct to cell for outlets)
Outlet spike MFC «1 @ 10.9
Duplicate (same as above)
Inlet spike MFC ffl @ 1 1 .3
Duplicate of INSPOI
NUMBEB
SCANS
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
BES
(eavll
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
300
SPIKED/
UNSPIKEU
U
S
S
S
S
U
U
U
S
S
U
U
U
U
U
U
U
U
U
U
S
S
S
S
S
SAMPLE
COND.
AMB
AMB
AMB
AMB
AMB
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
direct cell
direct cell
mbient+spil
mbicnl+spik
mbient+spik
SAMPLE
PLOW
51pm
6 1pm
61pm
61pm
61pm
61pm
61pm
61pm
61pm
61pm
5.51pm
61pm
61pm
61pm
61pm
61pm
61pm
61pm
61pm
stopped
slopped
9
6
6
CELL
PRESS
770
780
780
780
780
780
780
780
780
780
780
780
780
780
780
780
775
775
775
775
765
765
775
775
775
BUG
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
B
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(FTIft Sampling Dmto)
DATE:
9/23/97
BAROMETRIC: 29.92
OPERATOR: Klamm
SAMPLE
TIME
10:00
10:09
10:45
11:15
11:45
12:15
12.30
12:34
12:49
12:50
13:05
13:35
14:12
14:42
14:47
15:11
15:13
FILE
NAME
19230001
19230006
19230025
19230042
19230061
19230076
DIR03
DIR04
OUTSP05
OUTSP06
19230079
19230096
19230118
19230135
19230138
INSP03
INSP04
PATH
N2 blank before lest siait
possible use as BKGRD or coniamineni check
Switch to sample 1 (outlet)
Switch to sample 2 (inlet)
Switch to sample 1 (outlet)
Switch to sample 2 (inlet)
Switch to sample 1 (outlet)
direct to cell, p-xylene 104ppm + SF6 4 ppm
Duplicate of DIR03
Outlet spiked @ 2.0 MFC #2
Duplicate of OUTSP05
Sample of inlet (SAMP62)
Switch to sample 1 (outlet)
Switch to sample 2 (inlet)
Switch to sample 1 (outlet)
Switch to sample 2 (inlet)
Inlet spike MFC #2@ 2.0
4.0 ppm SF6. 104 ppm xylene
Duplicate of INSP03
NUMBER
SCANS
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
RES
(OB-1)
1
1
CELL
TEMP(F)
300
300
300
300
240
240
240
240
240
240
240
240
240
240
240
240
240
SPIKED/
UNSPIKED
U
U
U
U
U
U
S(puie)
S(pure)
S
s
U
U
U
U
U
s
s
SAMPLE
CONO.
N2 purge
stack
stack
stack
stack
stack
cal
cal
stack
stack
stack
slack
slack
stack
stack
slack
stack
SAMPLE
FLOW
7
6
6
6
6
6
stop flow
stop flow
6
6
6
6
6
6
6
6
6
CELL
PRESS
775
775
770
770
770
770
760
760
770
770
770
770
770
770
770
780
780
BKG
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(FT1R Sampling Dat*)
DATE: 9/23/97
BAROMETRIC:
OPERATOR:
29.92
SAMPLE
TIME
17:10
17:40
18:10
18:40
19:18
19:21
19:33
19:40
20:10
20:40
21:10
21:59
22:01
FILE
NAME
19230140
19230158
19230174
19230192
OUTSP07
OUTSP08
OUTSP09
19230209
19230227
19230244
19230262
1NSP05
1NSP06
PATH
Begin new lest line 2 (inlet)
Switch to line 1 (outlet^)
Switch lo line 2 (inlet)
Switch lo fine 1 (outlet)
Spike on outlet MFC *2@ 2.0
SF6 4 ppm lylene 104ppm
Duplicate of OUTSP07
Duplicate of OUTSP07
Restan test line 2 (inlet)
Switch to line 1 (outlet)
Switch to line 2 (inlet)
Switch to line 1 (inlet)
Spike inlet, MFC «2 @ 2.0, 4ppm SF6,
104 ppmxylene •
Duplicate of INSP05
NUMBER
SCANS
100
100
100
100
100
100
100
100
100
100
100
100
100
RES
(«-!>
1
1
1
CELL
TEMP(F)
240
240
240
240
240
240
240
240
240
240
240
240
240
SPIKED/
UNSPIKED
U
U
U
U
s
s
s
U
U
U
U
s
.
s
SAMPLE
COND.
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
SAMPLE
FLOW
6
6
6
6
6
6
6
6
6
6
6
3
3
CELL
PRESS
775
770
770
770
770
770
770
770
770
770
770
770
770
8KG
C
C
C
C
C
C
C
C
C
C
C
C
C
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(FTIR Sampling Data)
DATE: 9JMI97
BAROMETRIC: 29.85
OPERATOR: Klamtn
SAMPLE
TIME
13:18
14:37
15:10
17:39
18:12
18:14
18:16
18:29
18:31
18:33
FILE
NAME
19240001
19240045
19240064
19240147
INSP07
INSP08
INSP09
OUTSP10
OUTSP11
OUTSP12
PATH
Line 1 - APP
Switch to Line2-SBS
Switch to Line2 - APP
Run tests 1,2,3 continuous each hour
End of test
Spike of App(Lincl ) MFC @ 1.0 1pm
Spike of App(Linel) MFC @ 1.0 Ipm
Spike of App(Line 1 ) MFC @ 1 .0 1pm
Spike of SBS(Line2) MFC @ 1.0 1pm
Dup (same as above)
Spike of SBS(Line2) MFC @ 1.0 1pm
NUMBER
SCANS
100
100
100
100
100
too
100
100
100
RES
(OB-1)
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
240
240
240
240
240
240
240
240
240
SPIKED/
UNSP1KED
U
U
U
U
U
U
U
U
U
SAMPLE
COND.
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
SAMPLE
FLOW
6
6
6
6
6
6
6
6
6
CELL
PRESS
770
770
770
770
770
770
770
770
770
BUG
A
A
A
A
A
A
A
A
A
-------
PROJECT NO. 4701-08-05
PLANT: Porl Arthur
FTIR FIELD DATA FORM
(FTIR Svnptotg Datf)
DATE:
>/2S/»7
BAROMETRIC: 29.93
OPERATOR: Klamrn
SAMPLE
TIME
9.18
9:21
10.26
10:40
11:44
12:26
12:29
12:32
13:00
13:05
14:04
14.20
15:20
15:49
15:51
15:53
15:58
16:57
16.59
17:19
17:58
18:01
19:02
19:20
19:22
19:24
19:41
19:44
19:46
20:04
PILE
NAME
19250001
19250003
19250039
19250045
19250083
SBSSP01
SBSSP02
SBSSP03
N20I
19250089-%
19250097
19250139
19250141
19250142
19250143
PT01
DIROS
DIR06
ETSP01
19250144-145
19250146
19250
T11SP01
T11SP02
T11SP03
T1SP01
T1SP02
TISP03
PT02
ran
hi! prior u> lest - possible background
Switch to Line2(SBS) - test
Continue monitoring - end lest
Suit lest - continue monitoring
End test - stop monitoring
ipike of SBS(Line2) post lest
MFC *2 @ 2.0 Ipm (SF6 & xylene)
Dup. MFC «2 @ 2.0 Ipm (SF6 & xylene)
Trip. Dup MFC #2 <2> 2.0 Ipm (SF6 & xylene)
N2 blank - stored in OTHERS
very clean background between leil
On line "monitor" unkl app (Linel)
On line "monitor" lankl app (Linel)
Start lest coincident w/THC
End test
Pegged with compound 2900d
Spikes of line 1 MFC#2 <3 2.0 (SF6 & xylene)
Spikes of line 1 MFC«2 @ 2.0 (SF6 & xylene)
Spikes of line 1 MFC«2 2.0 (SF6 & xylene)
Post test of Unk 1- no dilution
(may contain some spike gas)
Cal (spike) direct to cell
Dup Cal (spike) direct to cell
Ethytene spike 2.0 Ipm MFC #2
Tank 11 post test N2 Wank
online •monitor' Tank 1 1 (Line 2)
End test
Spike MFC #2 2.0 Ipm (SF6 & xylene)
line 2 Spike MFC #2 @ 2.0 lorn (SF6 & xylene)
Spike MFC #2 2.0 Ipm (SF6 & lylenc)
Tl spike (2nd try) W/SF6 + xylene MFC @ 21pm
Tl spike (2nd try) w/SF6 + xylene MFC @ 21pm
Tl spike (2nd try) w/SF6 + xylene MFC 21pm
Post lest N2 blank - Background
NUMBER
SCANS
100
100
100
100
100
100
100
100
100
100
100
100
too
100
100
100
100
100
100
100
100
100
100
100
100
RES
(OM-1)
1
1
1
1
1
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
SPIKED/
UNSPIKED
u
u
u
u
u
s
s
s
u
u
u
s
s
s
u
u
u
u
s
s
s
s
s
s
SAMPLE
COND.
N2 purge
STACK
STACK
STACK
STACK
STACK
STACK
STACK
N2 purge
Ambient
STACK
STACK
STACK
STACK
STACK
CAL
N2 blank
STACK
STACK
STACK
STACK
Ambient
Ambient
Ambient
N2 blank
SAMPLE
FLOW
6
6
6
6
6
6
6
6
3
6
6
6
6
6
6
slop flow
6
6
6
6
6
6
6
6
6
CELL
PRESS
770
775
775
775
775
775
775
775
760
770
770
770
770
770
760
770
770
770
770
770
770
770
770
770
BUG
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
-------
PROJECT NO. 4701-08-05
PLANT: Port Arthur
FTIR FIELD DATA FORM
(FTIH SempUng D**)
DATE:
9/26/91
BAROMETRIC:
OPERATOR: Kiamra
SAMPLE
TIME
11:05
11:07
11:15
12:16
12:40
12:45
12:47
13:29
13:31
14:19
14:20
14:31
14:38
14:52
15:05
16.41
16:45
17:07
17:16
17:19
17:24
17:46
17:55
18:00
18:04
18:06
18:08
18:46
18:48
FILE
NAME
19260001-0002
19260003
19260007
19260040
T3SP01
T3SP02
T3SP03
19260041-42
19260043
19260069
19260070
19260075
19260076
19260083
T1SP04
19260084 85
19260086
APPOI
APP02
APP03
APP04
APP05
APPSP01
APPSP02
APPSP03
APP06
APP07
PT03
PT04
PATH
N2 blanks <3> nan of lea
SBS unk 3 (Line 2)
Switch to Line 2 (SBS unk 3)
Tank doted - was ambient before
Slop lest
Spike Line 2 (SBS unk 3) SF6+xy lene MFC @2.0
Spike Line 2 (SBS unk 3) SF6+xylene MFC @2.0
Spike Line 2 (SBS unk 3) SF6+xylene MFC @2.0
N2 blanks prior to leu
Suit test APP Tank 1 (Line 1)
Spike (TAQ w/6000 ppm propane
Leak check - sample no good
End lest
Restart lest
End test
Spike MFC #2 @ 2.01pm
(SF6 + xylene) - N2 good
N2 blanks prior to retest
Online Unk 1 APP
Manual collection Unk 1 APP
Manual collection lank 1 APP appears lo be saturated daoclor
Dilution of APP02 (- 250 mmHg)
Dilution of APP03 (serial dilution)
Manual collection
Spike of APP tank line
MFC * 2 @ 2.0 SF6 + lylene
Dup (same as above)
Trip (same as above)
Online spike cut off (may contain residual)
Online spike cut off (may contain residual)
Post ieslN2 blank
DupofPT03
NUMBEB
SCANS
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
too
100
100
100
100
100
100
100
100
100
100
RES
((•-I)
i
1
CELL
TEMP(F)
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
240
SPIKED/
UNSPIKED
N2 blank
STACK
U
U
S
S
S
U
U
U
U
U
U
U
S
U
U
U
U
U
U
U
S
S
S
U
SAMPLE
COND.
Ambient
STACK
STACK
STACK
STACK
STACK
N2 purge
STACK
STACK
STACK
STACK
STACK
STACK
STACK
N2
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
STACK
N2 blank
SAMPLE
FLOW
6
6
6
6
6
6
6
4
6
6
6
6
6
6
6
6
4
4
4
4
4
6
6
6
6
4
CELL
Pit ESS
770
770
770
770
770
770
770
770
770
770
770
770
770
770
770
770
760
770
770
770
770
770
770
770
770
770
BKC
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
-------
APPENDIX E
FTIR ANALYTICAL RESULTS
-------
TABLE E-l. FTIR RESULTS AT THE THERMAL OXIDIZER INLET
Dale
9/22/97
9/22/97
Run!
Average — >
Time
11:39
14:21
14:23
14:25
14:27
14:28
14:30
14:32
14:34
14:35
14:37
14:39
14:41
14:43
14:44
14:46
14:48
15:19
15:21
15:23
15:24
15:26
15:28
15:30
15:31
15:33
15:35
15:37
15:38
15:40
15:42
15:44
15:45
15:47
16:47
16:48
16:50
16:52
17:27
17:29
17:31
17:33
17:34
17:36
17:38
17:40
17:41
17:43
17:45
17:47
17:49
17:50
17:52
17:54
File name
INLUNOI
19220053
19220054
19220055
19220056
19220057
19220058
19220059
19220060
I922O06I
19220062
19220063
19220064
19220065
19220066
19220067
19220068
19220081
19220082
19220083
I9220U84
19220085
19220086
19220087
19220088
19220089
19220090
I9220O9I
19220092
19220093
19220094
19220095
19220096
19220097
19220101
19220102
19220103
I9220IO4
19220124
19220125
19220126
19220127
19220128
19220129
19220130
19220131
19220132
19220133
19220134
19220135
19220136
19220137
19220138
19220139
Cartonyl sulfide
ppm Uncertainly
0.080
0.127
0.097
0.187 0.0*5
0.186 0.011
0.190 0.080
0.228 0.011
0.264 0.083
0.241 0.083
0.216 0.081
0.191 0080
0.169 0.079
0.080
0.080
0.080
0.079
0.078
0.128
0.121
0.090
0.076
0.072
0.069
O.069
0.071
0.072
0.072
0.073
0.074
0.074
0.075
0.076
0.076
0.078
0.077
0077
0.077
0.077
0.128
0.118
O.089
0.079
0.075
0.073
0.072
0.072
0.072
0.072
0.073
0.074
0.074
0.074
0.074
0.075
0.035 0.082
Propane
ppm Uncertainly
0.369
1.017
3.591 0.416
4.212 0.419
1.582 0.411
1.749 0.409
2.279 0.418
3.146 0.530
2.805 0.529
2.406 0.422
2.209 0.417
1.957 0.414
1.804 0.414
1.754 0.411
1.730 0.411
1.665 0.411
1.673 0.407
1.039
0.999
3.321 0.409
4.431 0.366
4.882 0.353
4.661 0.372
4.809 0.373
4.872 0.376
4.946 0.380
5.033 0.383
5.O82 0.386
5.O93 0.389
5.128 0.393
5.185 0.398
5.212 0.401
5.267 0.404
5.302 0.409
4.144 0.586
4.328 0.586
4.472 0.589
4.543 0.589
1.078
1.018
4.818 0.428
5.579 0.426
4.379 0.589
4.265 0.584
4.229 0.583
4.164 0.586
4.171 0.588
4.234 0.589
4.508 0.593
4.459 0.5%
4.321 0.5%
4.254 0.598
4.238 0.598
4.275 0.599
3.531 0.522
Cumene
ppm Uncertainly
6.786 0.419
1.927
1.612
1.501
5.235 0.487
5.508 0.485
5.754 0.495
1.554
1.543
5.893 0.499
5.864 0.493
5.972 0.490
6.037 0.491
5.978 0.487
5.988 0.487
5.997 0.486
5.949 0.483
1.969
1.892
1.557
1.3%
1.345
1.330
1.334
1.343
1.355
1.364
1.378
1.386
1.400
1.418
1.429
1.443
1.459
1.466
1.468
1.480
1.480
2.O42
1.929
1.624
1.517
1.468
1.450
1.444
1.447
1.452
1.452
1.466
1.475
1.475
1.477
1.477
1.480
1211 1.300
Hsiane
ppm Uncertainly
3.574 0.438
0.984
6.063 0.582
8.703 0.554
8.558 0.502
9.472 0.500
11.543 0.511
17.172 0.554
16.306 0.552
13.133 0.515
12.263 0.509
11.465 0.506
10.883 0.506
10.393 0.502
10.076 0.502
9.761 0.502
9.559 0.498
1.005
0.966
6.171 0.572
9.103 0.512
10.264 0.494
10.842 0.491
11.270 0.493
11.430 0.497
11.527 0.501
11.602 0.505
11.699 0.510
11.643 0.513
11.686 0.518
11.754 0.525
11.700 0.529
11.759 0.534
II.8O9 0.539
13.742 0.544
14.398 0.543
15.499 0.546
16.021 0.546
1.043
2.482 0.702
9.326 0.599
12.500 0.562
13.910 0.547
14.162 0.542
14.208 0.541
14.131 0.543
14.142 0.546
14.137 0.546
14.314 0.550
14.284 0.553
14.065 0.553
13.953 0.554
13.923 0.555
13.900 0.556
10.994 0.569
p-Xyteas
ppm Uncertainly
0.537
3.9O9 1.159
0.774
0.595
0.552
0.539 '
0.547
0.568
0.562
0.552
0.545
0.543
O.54I
0.536
0.533
0.531
0.518
3.535 1.249
3.810 1.192
0.786
0.563
0.508
0.492
0.490
0.488
0.491
0.493
0.495
0.501
0.507
0.513
0.521
0.524
0.531
0.530
0.532
0.537
0.533
1.474
1.264
0.735
0.578
0.533
0.517
0.506
0.501
0.501
0.505
0.508
0.512
0.517
0.522
0.523
0.524
0.212 0.609
2.2.4-
Trenrl'hfrraianr
ppm Uncertainly
0.343
0.474
0.3%
0.369
0.361
0.360
0.369
1.807 0.285
1.815 0.284
0.315
0.311
0.365
0.364
0.361
0.361
0.360
0.357
0.484
0.465
0.383
0.343
0.331
0.327
0.328
0.330
0.333
0.335
0.339
0.341
0.344
0.349
0.351
0.355
0.359
1.100 0.288
I.I 18 0.288
1.157 0.289
1.175 0.289
0.502
0.474
0.399
0.373
1.1)99 0.289
1.209 0.287
1.244 0.286
1.2% 0.288
1.345 0.289
1.335 0.289
1.303 0.291
1.289 0.293
1.293 0.293
1.286 0.293
.277 0.294
.268 0.294
0.442 0.343
Elhyfcac
ppm Uncertainly
0.058
0.145
0.084
0.064
0.060
0.058
0.059
0.061
0.061
0.060
0.059
0.059
0.058
0.058
0.058
0.057
0.056
0.159
0.149
0.085
0.061
0.055
0.053
0.053
0.053
0.053
0.053
0.054
0.054
0.055
0.055
0.056
0.057
0.057
0.057
0.058
O.O58
0.058
0.159
0.137
0.079
0.063
0.058
0.056
0.055
0.054
0.054
0.055
0.055
0.055
0.056
0.056
0.057
O.057
0.067
Mci&iac
ppm Uncertainly
2.818 0.383
0.526
2.578 0.441
3.366 0.416
3.722 0.400
3.707 0399
4.063 0.407
4.381 0.429
4.116 0.427
3.922 0.411
3.713 0.406
3.546 0.403
3.411 0403
3.338 0.400
3.296 0.400
3.266 0.400
3.256 0397
0.544
0.523
2.205 0.433
3.010 0.388
3.255 0.374
3.368 0.370
3.424 0.371
3.459 0.374
3.477 0.377
3.474 0.380
3.437 0.384
3.425 0.386
3.431 0.390
3.432 0.395
3.404 0.398
3.387 0.402
3.372 0.406
3.082 0.406
3.262 0.406
3.283 0.408
3.222 0.408
0.564
0.533
2.570 0.454
3.281 0423
3.288 0.409
3.193 0.405
3.073 0.404
3.093 0.406
3.103 0.408
3.030 0.408
3.550 0.411
3.350 0.413
.077 0.413
.015 0.414
.031 0.415
.974 0.415
.014 0.417
CO
ppm Uncertainly
3.697
5.859
12.971 4.223
13.743 3.741
13.823 3.599
14.541 3.549
16.163 3.600
17.128 3.681
16.428 3.656
15.831 3.585
15.170 3.536
14.390 3.509
12.660 3.485
12.191 3.459
11.803 3.463
11.709 3.454
11.679 3.411
5.921
5.619
12.904 3.925
13.035 3.292
13.286 3.117
13.582 3.055
13.681 3.061
13.868 3.095
13.834 3.129
13.706 3.150
13.506 3.176
13.285 3.198
13.101 3.232
12.875 3.262
12.735 3.282
13.138 3.322
I3.O43 3.366
10.847 3.309
11.379 3.313
11.535 3.328
11.394 3.316
5.932
5.478
2.155 3.874
1.243 3.404
0.680 3.228
0.417 3.138
0.150 3.101
0.128 3.098
9.964 3.119
9.821 3.132
0.741 3.167
0.564 3.186
0.142 3.197
9.917 3.207
9.9*5 3.221
9.950 • 3.225
1.336 3.585
FanaikJeiyite
ppm Uncertainly
0.545
0.753
0.630
0.586
0.574
0.572
0.586
0:607
0.603
0.591
0.583
O.579
0.578
0.574
0.573
0.572
0.567
0.769
0.739
0.608
0.545
0.525
0.519
0.521
0.525
0.529
0.533
0.538
0.541
0.547
0.554
0.558
0.564
0.570
0.572
0.573
0.578
0.578
0.798
0.753
0.634
0.593
0.573
0.566
0.564
0.565
0.567
0.567
0.573
0.576
0.576
0.577
0.577
0.578
0.588
-------
TABLE E-l. (continued)
Dale
9/13191
Run 2
Time
9:43
:47
9:49
9:51
9:53
9:54
9:56
9:58
oao
0:01
003
0:05
0:07
0:09
10:10
10:12
10:14
10:49
10:51
10:53
10:55
10:56
10:58
II:OU
11:02
11:03
11:05
11:07
11:09
11:11
11:12
11:14
12:05
12:06
12:08
12:10
12:12
12:13
12:15
12:17
12:19
12:21
12:22
12:24
12:26
12:28
12:29
12:31
12:33
13:14
13:11
13:17
13:19
13:21
13:23
13:24
13:26
13:28
13:30
13:31
13:33
13-35
:uename
9230025
9230026
9230027
9230028
9230029
9230030
9230031
9230032
9230033
9230)34
9230035
9230)36
19230037
9230038
19230039
19230040
19230041
19230061
19230062
19230063
19230064
19230065
19230066
19230067
19230068
1 9230069
1 92311070
19230071
19230072
19230073
19231)074
192311075
19230079
19230080
I9230U8I
19230082
19230083
19230084
19230085
19230086
19230087
19230088
19230089
19230090
19230091
19230092
19230093
19230094
19230095
19230118
I9230H9
19230120
19230121
19230122
19230123
19230124
19230125
19230126
19230127
19230128
19230129
19230130
Cutiooyl uiVkJc
ppui Uoccfuunly
0.131
0.121
a 103
0.093
O.OW
0.092
0.092
0.093
0.093
0.094
0.094
0.094
0.092
0.092
0.092
0.093
0.093
0.114
0.096
0.090
0.088
0.087
0.087
0.087
0.087
O.U88
0.089
0.088
0.089
0.089
0.08V
0.089
0.084
0.084
0.084
0.085
0.085
0.085
0.084
0.084
0.084
0.084
0.084
0.085
0.085
0.084
0.084
0.084
0.084
0.112
0.095
0.09O
0.088
0.088
0.087
0.088
0.088
0.088
0.088
0.089
0090
(1 OK9
Propane
ppm Uncertainly
1.143
3.337 0.488
2.670 0.422
2.157 0.460
2.966 0.454
2.960 0.454
2.959 0.456
2.965 0.459
3.020 0.462
2.985 0.465
2.780 0.464
2.680 0.462
2.365 0.458
2.430 0.456
2.441 0.458
2.306 0.459
2.444 0.458
3.803 0.463
5.275 0.419
3.854 0.470
3.838 0.462
3.749 0.458
3.720 0.460
3.717 0.460
3.512 0.463
3.372 0.467
3.384 0.471
3.435 0.474
3.423 0.476
3.433 0.476
3.465 0.475"
3.490 0.476
3.727 0.452
3.818 0.454
3.917 O.457
3.890 0.461
3.878 0.463
3.856 0.464
3.834 0.464
3.763 0.464
3.709 0.463
3.735 0.464
4.158 0.467
3.930 0.468
3.784 0.470
3.750 0.470
3.802 0470
3.924 0.471
3.731 0.473
3.943 0.475
3.809 0.511
3.999 0.497
4.045 0.493
3.986 0.489
3.942 0.487
3.897 0.487
3.908 0.487
3.834 0.487
3.920 0.487
3.965 0.489
3.874 0.494
3 75(1 0 492
Cumene
ppm Uncertainty
2.165
1.894
7.160 0.560
8.276 0.545
8.532 0.537
8.642 0.537
8.789 0.540
8.816 0.543
8.851 0.547
8.882 0.551
8.880 0.549
8.802 0.548
8.628 0.543
8.549 0.540
8.661 0.343
8.692 0.344
8.689 0.343
1.787
1.589
4.216 0.543
4.514 0.534
4.626 0.530
4.762 0.532
4.859 0.533
4.930 0.536
5.036 0.540
5.204 0.545
5.306 0.548
5.359 0.550
5.385 0.550
5.453 O.550
5.555 0.551
3.832 0.523
3.854 0.526
3.921 0.529
4.022 0.533
4.169 0.535
4.225 0.536
4.294 0.537
4.428 0.536
4.593 0.536
4.781 0.536
4.984 0.540
5.117 0.542
5.133 0.543
5.121 0.544
5.052 0.543
5.084 0.545
5.163 0.347
1.796
4.080 0.591
4.843 0.575
5.130 0.570
5.193 0.566
5.152 0.563
5.042 0.563
4.897 0.563
4.782 0.563
4.669 0.563
4.546 0.566
4.410 0.571
4271 0569
Heune
ppm Unceruimy
1.103
5.416 0.683
10.362 0.582
12.633 0.562
13.216 0.554
13.351 0.554
13.384 0.557
13.355 0.560
13.394 0.364
13.271 0.368
12.806 0.367
12.376 0.565
12.199 0.560
12.047 0.557
12.208 0.560
12.592 0.561
12.685 0.560
6.819 0.630
10.573 0.586
10.963 0.566
11.274 0.557
11.188 0.552
11.185 0.554
11.279 0.555
10.866 0.558
10.481 0.563
10.381 0.568
10.392 0.571
10.413 0.574
10.485 0.573
10.660 0.573
10.849 0.574
11.068 0.545
11.144 0.348
11.392 0.551
11.479 0.555
11.521 0.558
11.528 0.559
11.671 0.560
11.753 0.559
11.866 0.558
12.047 0.559
13.330 0.563
13.216 0.565
12.839 0.566
12.724 0.367
12.807 0.566
13.239 0.568
13.021 0.570
7.455 0.665
10.727 0.616
11.684 0.599
11.977 0.394
11.996 0.590
11.880 0.587
11.738 0.587
11.637 0.587
11.460 0.587
11.512 0.586
11.564 0.590
11.414 0.595
11.082 0593
p-Xyfcne
ppm Uncertainty
1.614
1.160
0.761
0.668
0.643
0.637
0.641
0.645
0.651
0.657
0.656
0.653
0.644
0.640
0.641
0.642
0.639
0.941
0.687
0.624
0.604
0.597
0.598
0.5%
0.598
0.602
0.610
0.611
0.61 1 •
0.610
0.609
0.610
0.574
0.576
0.582
0.590
0.590
0.590
0585
0.582
0.578
0.576
0.585
0.586
0.582
0.583
0.583
0.586
0.588
0.945
0.687
0.628
0.616
0.605
0.399 .
0.600
0.597
0.398
0.600
0.606
0.614
0610
2.2.4-
Trim»^lllpMll>n»
ppm Unceruimy
0.532
0.466
0.414
0.400
0.394
0.394
0.3%
0.399
0.402
0.405
0.403
0.401
0.398
0.395
0.397
0.398
0.397
0.439
0.391
0.376
0.369
0.365
0.366
0.366
0.368
0.371
0.374
0.376
0.378
0.377
0.377
0.377
0.357
0.359
0.362
0.365
0.366
0.367
0.367
0.366
0.363
0.366
0.369
0.370
0.370
0.371
0.371
0.373
0.374
0.442
0.402
0.390
0.386
0.383
0.381
0381
0.381
0.380
0.380
0.383
0.387
0385
Ethyfcne
ppm Uncertainty
0.174
0.125
0.082
0.072
0.183 0.070
0.069
0.069
0.070
0.070
0.071
0.071
0.071
0.070
0.069
0.069
0.069
0.069
0.102
0.074
0.067
0.065
0.064
0.065
0.064
0.065
0.065
0.066
0.066
0.066
0.066
0.066
0.066
0.062
0.062
0.063
0.064
0.064
0.064
0.063
0.063
0.062
0.062
0.063
0.063
0.063
0.063
0.063
0.063
0.064
0.102
0.074
0.068.
0.067
0.065
0.065
0065
0.065
0.065
0065
0.065
O.O66
0066
Methane
ppm Uncertainty
0.398
1.606 0.517
2.771 0.464
3.075 0.448
3.101 0.442
3.174 0.442
3.284 0.444
3.415 0.447
3.577 0.450
3.666 0.453
3.624 0.452
3.580 0.450
3.427 0.446
3.316 0.444
3.413 0.446
3.525 0.447
3.225 0.446
1.986 0.492
2.854 0.444
3.201 0.421
3.180 0.414
3.093 0.410
3.061 0.412
2.993 0.412
2.991 0.415
3.006 0.418
3.014 0.422
3.054 0.424
3.125 0.426
3.066 0.426
3.074 O.426
2.986 0.427
3.647 0.405
3.605 0.407
3.525 0.410
3.473 0.413
3.419 0.415
3.378 0.415
3.366 0.416
3.313 0.415
3.267 0.415
3.257 0415
3.289 0.418
3.222 0.420
3.192 0.421
3.182 0.421
3.247 0.421
3.244 0.422
3.181 0.424
1.804 0.304
2.691 0.458
2.831 0.445
2.825 0.441
2.789 0.438
.772 0.436
.759 0.436
.737 0.436
.730 0.436
.849 0.436
.877 0.438
.831 0.442
805 O440
CO
ppm Uncertainty
6.991
5.923
4.773
4.408
4.274
4.247
4.279
4.306
4.323
4.360
4.339
4.331
4.277
4.259
4.279
4.283
4.281
5.290
4.435
4.168
4.069
4.026
4.040
4.018
4.034
4.057
4.100
4.094
4.114
4.099
4.102
4.116
3.870
3.878
3.891
3.921
3.927
3.922
3.909
3.902
3.885
3.887
3.904
3.921
3.924
3.664
7.565 3.636
7.510 3.663
3.656
5.200
4.395
4.148
4.080
4.053
4.041
4.055
4.067
4.069
4.072
4.113
4.164
4.124
Formaldehyde
ppm Uncertain!*
0.846
0.740
0.659
0.636
0.626
0.626'
0.629
0.633
0.638
0.643
0.640
0.638
0.632
0.628
0.631
0.632
0.630
0.698
0.620
0.597
0.587
0.581
0.582
0.582
0.585
0.589
0.594
0.397
0.600
0.599
0.599
0.600
0.568
0.571
0.575
0.579
0.582
0.583
0.584
0.582
0.581
0.581
0.587
0.588
0.589
0.589
0.590
0.592
0.594
0.702
0.639
0.619
0.613
0.609
0.606
0.605
0605
0.604
0.604
0.609
0.615
0.611
m
-------
TABLE E-l. (continued)
Date
Average — >
Time
13:37
13:39
13:40
13:42
13:411
13:51
14:12
14:14
File name
1 9230131
19230132
19230133
19230134
19230138
19230139
INSF03
INSF04
Carbonyl iulfide
ppm Uncertainly
0.088
0.08*
u.ou
0.018
0.103
0.093
M71
0.070
0091
Propane
porn Uncertainly
3.691 0.48V
3.621 0.488
3.32) 0.488
3.517 0.489
4.489 U.453
3603 0.503
4.09* O.J7»
1.52* 0.381
3.508 0.480
Cumcne
ppm Uncenaimy
4.212 0.566
4.115 0.565
4.095 0.564
4.021 0.565
1.688
3977 0.582
1.347
0.502
5.136 0.661
Heune
ppm Uncertainly
10.804 0.590
10.602 0.589
10.402 0.588
10.326 0.58V
8.899 0.634
10.38V 0.6117
13.277 0.512
13.067 0.516
1 1.284 0.584
p-Xylene
ppm Uncertainly
0.604
0.601
0598
0.601
0.745
0.626
29.809 0.535
30.025 0.52*
0.648
2,2,4-
Trimpi hlpMi am*
ppm Uncertainly
0.382
0.381
0.380
0.381
0415
0392
0.331
0.332
0.387
Elhylene
ppm Uncenaimy
0.065
0.065
0.065
0.065
0.081
0068
0.344 0.0*8
0.339 0.0*8
0.003 0.070
Melhane
ppm Uncertainty
2.722 0.438
2.607 0.437
2.562 0.437
2.582 0.438
2.070 O.480
2.560 0.451
3.63H 0.390
3.52* OJW
2.995 0.438
CO
ppm Uncertainly
4.087
4.068
4.061
4.07V
4.761
4.301
16.390 3.0*7
10.640 3.043
0.222 4.206
Formaldehyde
ppm Uncertainty
0.608
0.605
0.604
0.605
0659
0.623
0.52*
0.527
0.614
m
-------
TABLE E-l. (continued)
Due
9/23/97
Rua 3
'ime
6:10
6:11
6:13
6:1]
6:17
6:18
6:20
6:22
6:24
6:25
6:27
6:29
6:31
6:33
6:34
6:36
6:38
6:40
7:10
7:12
7:13
17:15
7:17
7:19
17:20
17:22
17:24
17:26
17:28
17:29
17:31
17:33
17:35
17:36
17:38
17:40
18:39
18:41
18:43
18:44
18:46
18:48
18:30
18:51
18:53
18:5)
18:57
18:59
19:00
19:02
19:04
19:06
19:07
19:09
19:41
19:43
19:45
19:46
19:48
19:50
19:52
19-54
File name
9230140
9230141
9230142
9230143
9230144
9230145
9230146
9230147
9230148
9230149
9230150
9230151
9230152
92301)3
9230154
9230155
9230156
9230157
9230174
19230175
19230176
19230177
19230178
9230179
19230180
19230181
19230182
19230183
19230184
19230185
19230186
19230187
19230188
19230189
19230-190
19230191
19230209
19230210
19230211
19230212
19230213
19230214
19230215
19230216
19230217
19230218
I92WI9
19230220
19230221
19230222
19230223
19230224
19230225
19230226
19230244
19230245
19230246
19230247
19230248
19230249
19230250
19230251
CarfaonyliuUide
ppm Uncenaimy
0.07S
0.0*2
(LOIS
0.086
0.0*7
0.0*7
0088
0.088
0.089
0.089
0.090
0.090
0.090
0.090
0.196 0.091
0.196 0.091
0.091
0.090
0.142
0.118
0.094
0.088
0.087
0.087
0.087
0.087
0.087
0.087
0.088
0093
0.096
0.097
0.097
0.095
0.094
0.093
0.088
O.O88
O.O87
0.0X9
0.092
0.093
0.090
0.088
0.086
0.085
0.084
0.084
0.083
0.083
0.083
0.084
0.084
0.084
0.114
0091
0.083
0.081
0.080
0.080
0.080
0 080
Propane
ppm Uncenaimy
3.629 0.411
3.753 0.448
3.663 0.459
3.621 0.463
3.618 0.469
3.603 0.471
3.671 0.473
3.793 0.477
4.003 0.478
4.371 0.479
4.464 0.483
4.348 0.484
4.237 0.483
4.3S9 0.484
4.716 0.494
4.784 0.49)
4.S84 0.491
4.587 0.491
1.105
2.900 0.413
3.291 0.477
3.615 0.469
3.540 0.466
3.468 0.467
3.390 0.468
3.368 0.467
3.198 0.464
3.049 0.464
3.336 0.470-
3.757 0.485
4.029 0.496
4.187 0.502
4.334 0499
4.286 0.494
4.568 0.491
4.470 O.488
4.784 0.4S8
5.211 0.465
5.370 0.464
5.744 0.474
6.110 0.489
5.931 0.486
5.580 0.476
5.259 0.464
4.998 0.455
4.894 0.448
4.833 0.446
4.794 0.444
4.624 O.441
4.621 0.440
4.612 0.441
4.648 0.443
4.712 0.446
4.779 0.448
3.285 0.446
3.266 0.441
3.998 0.428
4.155 0.424
4.167 0.423
4.227 0422
4.252 0.422
4 175 0421
Ciunene
ppm Uncertainty
6.177 0.551
6.602 0.570
6.916 0.584
7.024 0.589
7.187 0.596
7.288 0600
7.282 0.602
7.274 0.607
7.093 0.608
6.691 0.610
6.926 0.649
6.867 0.650
6.955 0.649
6.902 0.649
6.843 0.664
6.772 0.665
6.841 0.659
6.971 0.660
2.093
1.848
5.929 0.607
6.655 0.597
6.859 0.593
6.962 0.594
6.959 0.595
6.918 0.593
7.010 0.591
7.165 0.591
7.111 0.598
6.944 0.617
6801 0631
6.832 0.639
6.787 0.635
6.861 0.628
6.800 0.625
6.823 0.621
6.215 0.582
6.337 0.591
6.300 0.590
6.197 0.603
6.084 0.621
6.113 0.618
6.153 0.605
6.178 0.591
6.152 0.579
6.IO9 0.570
6.107 0.567
6.126 0.564
6.152 0.561
6.152 0.560
6.162 0.561
6.156 0.564
6.218 0.568
6.231 0.570
1.764
4.853 0.566
5.442 0.549
5.758 0.544
5.8O8 0.543
5.817 0.541
5.795 0.541
5767 0541
Heune
ppm Uncertainly
11.532 0.507
12.520 0.537
12.531 0.550
12.336 0.555
12.477 0.562
12.520 0.565
12.513 0.567
12.731 0.572
13009 0.573
13.622 0.574
13.809 0.596
13.892 0.598
13.776 0.5%
13.865 0.597
14.260 0.610
14.407 0.611
14.328 0.606
14.409 0.606
1.068
5.039 0.621
11.495 0.571
12.512 0.562
12.337 0.559
12.071 0.560
11.912 0.560
11.602 0.559
11.326 0.556
10.988 0.556
10.895 0.563
11.154 0.582
11.255 0.594
11.355 0.602
11.211 0.598
11.004 0.591
10.960 0.589
10.929 0.584
10.989 0.548
11.988 0.557
12.470 0.556
13.071 0.568
13.493 0.585
13.303 0.582
12.909 0.570
12.421 0.556
11.885 0.545
11.474 0.537
11.198 0.534
10.880 0.531
10.634 0.528
10.574 0.527
10.665 0.528
10.883 0.531
11.212 0.535
11.410 0.537
3.6% 0.626
8.240 0.526
10.176 0.510
10.853 0.506
11.073 0.505
11.171 0503
11.259 0503
11247 0503
p-Xylene
ppm Uncertainly
0.493
0.539
0.553
0.556
0.563
0.565
0.568
0.574
0.581
0.585
0.589
0.591
0.589
0.589
0.604
0.604
0.592
0.588
3.763 1.340
1.028
0.645
0.584
0.571
0.564
0.564
0.561
0.561
0.562
0.574
0.606
0.628
0.639
0.635
0.623
O.6I7
0.607
0.593
0.592
0.587
0.599
0.622
0.622
0.607
0.590
0.579
0.575
0.572
0.568
0.565
0.564
0.564
0.562
0.564
0.564
1.067
0.674
0.582
0.557
0.549
0.548
0.544
0541
2.2.4-
Trimcthlpciuane
ppm Uncertainly
0.350
0.383
0.392
0.3%
0.400
0.402
0.404
0.407
0.408
0.409
0.412
0.413
0.411
0.412
0.421
0.422
0.418
0.418
0.515
0.454
0.410
0.401
0.398
0.399
0.400
0399
0.397
0.397
0.402
0.416
0.425
• 0.431
0.429
0.423
0.421
0.418
0.394
0.399
0.398
0.407
0.419
0.417
0.408
0.398
0.391
0.385
0.383
0.381
0.379
0.378
0.379
0.381
0.383
0.385
0.434
0.385
0.372
0.367
0.366
0.364
0.364
0364
Elhyfene
ppm Uncertainly
0.144 0.053
0.159 0.057
0.164 0.059
0.161 0.059
0.163 0.060
0.165 0.060
0.166 0.060
0.167 0.061
0.175 0.062
0.177 0.062
0.180 0.062
0.186 0.063
0.178 0.062
0.179 0.062
0.183 0.064
0.183 0.064
0.176 0.063
0.175 0.062
0.168
0.286 0.102
0.201 0.068
0.174 0.062
0.171 0.061
0.170 0.060
0.171 0.060
0.168 0.060
0.166 0.060
0.171 0.050
0.186 0.061
0.199 0.064
0.208 0.066
0.209 O.O67
0.201 0.067
0.202 0.066
0.207 0.065
0.210 0.064
0.448 0.063
0.267 0.063
0.219 0.063
0.214 0.064
0.222 0.066
0.221 0.066
0.212 0.065
0.208 0.063
0.203 0.062
0.207 0.062
0.208 0.061
0.207 0.061
0.205 0.061
0.2O9 0060
0.207 0.061
0.204 0.060
0.201 0.060
a 198 O.O6I
0.115
0.226 0.071
0.208 0.063
0.206 O.O60
0.207 0.059
0.206 O.O59
0.202 0.059
0.205 O.O59
Methane
ppm Uncertainly
4.429 0.394
4.767 0.423
4.748 0.434
4.795 0.437
4.611 0.442
4.507 0.445
4.585 0.447
4.737 0.450
4.958 0.451
5.304 0.452
5.272 0.464
5.186 0.465
5.186 0.464
5.489 0.464
5.774 0.474
5.810 0.475
5.653 0.471
5.628 0.471
0.578
2.476 0.4%
4.373 0.450
4.743 0443
4.582 0.440
4.579 0.441
4.639 0.441
4.604 0.440
4.374 0.438
4.374 0.438
4.805 0.443
5.147 0.458
5.469 0.468
5.458 0.474
4.738 0.471
4.403 0.466
4.511 0.464
4.971 0.460
4.215 0.432
4.395 0.439
4.4% 0.438
4.857 0.448
5.090 0.461
4.941 , 0.459
4.634 ' 0.449
4.449 0.438
4.294 0.430
4.190 0.423
4.068 0.421
3.963 0.419
3.878 0.416
3.862 0.415
3.920 0.416
4.048 0.418
4.192 0.421
4.177 0.423
2.085 0.473
3.311 0.420
3.605 0.407
3.640 0.403
3.644 0.403
.836 0.401
.934 0.401
935 0 401
CO
ppm Uoccruini)
6.S64 3.254
3.816
3.930
3.96}
4.009
4.031
4.057
3.821
3.845
8.619 3.878
8.651 3.897
8.507 3.900
8:131 3.898
8.349 3.915
9.926 4.031
10.821 4.037
9.700 3961
9.500 3.929
6.576
5.477
10.437 4.054
9.480 3.817
8.420 3.757
7.517 3.753
3.762
3.757
7.647 3.752
7.675 3.753
7.921 3.816.
8.419 4.032
8.605 4.174
9.070 4.237
8.658 4.197
4.1 II
4.341
4.289
10.367 3.823
10.399 3.798
10.277 3.771
10.550 3.879
10.769 4.051
10.198 4.028
9.381 3.916
8.916 3.799
8.454 3.714
7.8% 3.667
7.634 3.637
3.614
3.835
3.833
3.847
3.618
8.143 3.628
8.274 3.638
5.278
4.201
3.850
3.738
3.706
3.7O5
3.687
3687
Formaldehyde
ppm Uncertainly
3.209 0.536
3.421 0.587
3.456 0.601
3.435 0.607
3.460 0614
3.475 0.617
3.551 0.620
3.634 0.625
3.684 0.626
3.682 0.628
3.719 0.630
3.6% 0.632
3.641 0.630
3.605 0.631
3.585 0.645
3.609 0.646
3.575 0.641
3.698 0.641
0.817
0.722
2.614 0.624
3.177 0.615
3.295 0.611
3.294 0.61 1
3.228 0.612
3.183 0.611
3.136 0.6O8
3.158 0.608
3.O93 0.615
2.991 0.636
2.862 0.650
2.835 0.658
2.779 0.654
2.803 0.646
2.753 0.643
2.745 0.639
2.408 0.599
2.780 0.609
2.874 0.608
2.905 0.621
2.828 0.640
2.775 0.636
2.676 0.623
2.627 0.608
2.589 0.5%
.517 0.587
.484 0.584
.450 0.581
.365 0.577
.347 0.576
.336 0.577
.375 0.580
.414 0.585
.429 0.587
0.689
0.612
0.591
0.583
0.581
0.579
0.579
0.578
m
-------
TABLE E-l. (continued)
Dale
Average — >
Time
19:55
19:57
19:59
20:01
20:02
20:04
20:06
20:08
20:09
20:11
21:00
21:02
Filename
19230252
19230253
19230254
19230255
19230256
19230257
19230258
19230259
19230260
19230261
INSP65
INS POt
Cartx>nyl sulfide
ppm Uncertainly
0.079
0.079
0.079
0.079
0.079
0079
0.079
0.078
0.078
0.079
O.M2
0.0*1
0.005 0.088
Prupane
open Uncertainly
4.181 0.420
4.124 0.419
3.932 0.416
4.127 0.418
4.203 0.419
4.147 0.418
4.027 0.417
3.985 0.417
3.730 0.415
3.855 0.419
3.975 o.3s«
3.897 OJI1
4.166 0.466
Ciunene
ppm Uncenainiy
5.738 0.539
5.785 0.538
5.821 0.534
5.792 0.532
5.828 0.533
S.838 0.531
5.875 0.530
5.885 0.530
5.889 0.533
5.903 0.538
3.675 0.451
3.692 0.451
6 ISO 0.642
Hexane
ppm Uncertainly
11.200 0.501
11.123 0.500
10.956 0.496
10.687 0.501
10.739 0.502
10.626 0500
10.558 0.499
10.604 0.499
10.945 0.496
11.148 0.501)
10.303 0.475
10.368 0.477
11.449 0.560
p-Xylene
ppm Uncertainty
0.543
0.54J
0.543
0.543
0.542
0.542
0.539
O.538
0.534
0.539
28.074 0.465
28.557 0.467
O.O52 0.600
2.2.4-
TrimethlpenuiK
ppm Uncertainly
0.362
0.362
O.359
0.360
0.360
0.359
0359
0.359
0.359
0.362
OJ18
0.31*
0.396
Elhyfcnc
ppm Uncertainly
0.202 0.059
0.203 0.059
0.206 0.059
0.209 0.059
0.210 0.059
0.203 0.059
0.202 0.059
0.199 0.058
0.199 0.058
0199 O.O59
0.3*5 0.057
0.365 0.057
0.194 0.064
Methane
ppm Uncenainiy
4.046 0.399
4.274 0.399
3.968 0.396
4.049 0.394
4.099 0.395
3.825 0.394
3.662 0.393
3.582 0.393
3.451 0.395
3.721 0.399
3.532 8.374
3.591 0.375
4.361 0.437
CO
ppm Uncertainly
3.668
3.664
3.655
3.642
3.643
3.635
3.639
3.626
3.618
3.647
10.708 2.664
10.875 2.686
4.221 3.920
Furroakfehytlc
ppm Uncertainly
0.576
0.575
0.571
1.873 0.547
1.863 .0.548
1.855 0.547
1.883 0.546
1.872 0.546
0.570
0.575
0.505
0.507
2.328 0.610
m
-------
TABLE E-2. FTIR RESULTS FROM THE THERMAL OXIDIZER OUTLET
Dale Tune File name
11/22/97 11:10 OUTDNO1
H/22W7 11:14 OUTUNU2
SI/22/97 11:25 OUTSP01
IW22/97 11:31 OUTSP02
OT2/97 13:50 19220035
9/22/97 13:51 19220036
9/22/97 13:53 19220037
W32AT7 13:5) 19220038
W22/97 13:57 19220039
W22/97 13:58 19220040
D/22/97 14 «) 19220041
D/22/97 14:02 192201)42
9/22/V7 I4:O4 19220043
9/22/97 14:05 19220044
W22/V7 14:07 I9220O45
»/22»7 14:09 19220046
OT2/97 14:11 19220047
a/22/97 14:13 19220048
H/22/97 14:14 19220049
a/22/97 14:16 19220050
9/22/97 14:18 19220051
9/22/97 14:20 19220052
9/22/V7 14:50 I9220U69
9/22/97 15:00 I9220U70
9/22/97 15:01 19220071
9/22/97 15:03 19220072
9/22/97 15:05 19220073
9/22/97 15:07 19220074
9/22/97 15:08 19220075
9/22/97 15:10 19220076
9/22/97 15:12 19220077
9/22/97 15:14 19220078
!W22/97 15:15 19220079
W22/97 15:17 19220080
9/22/97 15:49 19220098
9/22/97 15:51 192200*9
9/22/97 15:52 19220100
9/22/97 16:54 19220105
9/22/97 16:56 19220106
9/22/97 16:57 19220107
9/22/V7 16:59 19220108
9/22/97 17:01 19220109
9/22/97 17:03 192201 10
9/22/97 17:04 192201 II
9/22/97 17:06 192201 12
9/22/97 17:08 192201 13
9/22/97 17:10 19220114
9/22/97 17:11 19220115
9/22/97 17:13 192201 16
9/22/97 17:15 19220117
9/22/-I/ i' !? I-I.V201I8
9/2i- .Ml'19
Carbonyl sulfide
ppm Uncertainly
0.086
0.116
MT4
MT3
a 137
a 141
0.141
a 140
a 140
a 139
0.139
0139
0.139
0.138
0.137
0.136
0.135
0.135
0.134
0.134
0.135
0.135
0.078
0.133
0.133
0.132
0133
0.134
0.134
0.133
0.133
0.133
0.133
0.132
0.078
0.084
0.114
0.076
0.077
0.103
0119
0.125
0.127
0.128
0.129
0.130
0.129
0.129
0.128
0.128
0.128
O.I 28
Propane
ppm Uncertainly
0.778
0.937
0,312
MT9
1.063
1.092
1.099
1.092
1095
1.091
1.092
1.094
1.087
1.078
1.066
1.060
1.058
1.058
1.057
I.O6I
1.064
1.066
1.721 0.408
1.073
1.074
1.073
1.076
1.082
1.079
1.075
1.072
1.074
I.O79
1.070
5.308 0.412
5.198 0.405
0.976
4.324 0.586
4.185 0.592
3.255 0.461
1.013
1.047
1.063
1.071
1.076
1.086
1.085
1.083
1.081
1.081
1.080
1 079
Cumene
ppm Uncertainly
1.474
1.774
1.311
1.286
2.014
2.069
2.082
2.070
2.075
2.067
2.069
2.073
2.059
2.041
2.019
2.008
2.005
2.004
2.002
2.010
2.015
2.019
6.005 0.484
2033
2.035
2.033
2.038
2.050
2.044
2.037
2.032
2.034
2.043
2.027
1.473
1.545
• 1.849
1.468
1.484
1.745
1.919
1.984
2.014
2.029
2.038
2.058
2.056
2.052
2.048
2.048
2.046
2.043
Heune
ppm Uncertainly
0.752
0.906
O.tt»
0.657
1.028
1.056
1.063
1.056
1.0)9
1.055
1.056
1.058
1.051
1.042
1.031
1.025
1.023
1.023
1.022
1.026
1.028
1.031
9.451 0.499
1.038
1.039
1.038
1.040
1.047
1.043
1.040
1.037
1.038
1.043
1.035
11.770 0.544
10.205 0.566
4.847 0.669
15.532 0.543
14.599 0.549
6.340 0.645
2.453 0.697
1.013
1.028
1.036
1040
1.050
I.O49
1.047
I.O45
1.045
1.044
1043
p-Xyfcne
ppm Unceruimy
3.216 0.594
3.879 0.986
2XOM . 0.522
Ull 0.53J
3.649 1.263
3.735 1.296
3.848 1.307
3.877 1.306
3.826 1.31 1
3.930 1.312
3.933 1.310
3.903 1.309
3.837 1.301
3.772 1.294
3.669 1.284
3.669 1.280
3.626 1.275
3.690 1.283
3.736 1.283
3.745 1.288
3.759 1.289
3.811 1.291
0.506
4.291 1.288
3.798 1.280
3.784 1.275
3.758 1.278
3.808 1.278
3.671 1.274
3.676 1.269
3.655 1.266
3.620 1.264
3.624 1.265
3.582 1.262
0.531
0.583
1.082
0.526
0.533
0.956
1.289
1.397
1.440
1.456
1.466
1.482
1.477
3.953 1.273
3.961 1.267
3.931 1.265
3.974 1.266
3 888 1 260
2.2.4-
TrimeUiylpenune
ppm Unceruimy
'0.362
0.436
•J21
OJU
0.495
0.509
0.512
0.509
0.510
0.508
0.509
0.510
0.506
0.502
0.496
0.493
0.493
0.493
0.492
0.494
0.495
0.496
0.358
0.500
0500
0.500
0.501
0.5O4
0.503
0.501
0.499
0.500
0.502
0.498
0.362
0.380
0.455
1.198 0.288
1.104 0.291
0.429
0.472
0.488
0.495
0.499
0.501
0.506
0.505
0.504
0.503
0.503
0.503
0.502
Elhytene
ppm Uncertainty
0.069
0.125
0.930 0.0*4
MM
0.161
0.165
0.166
0.166
0.167
0.167
0.167
0.167
0.166
0.165
0.163
0.163
0.162
0.163
0.163
0.164
0.164
0.164
0.055
0.161
0.163
0.162
0.162
O.I62
O.I62
0.161
0.161
0.161
0.161
0.160
0.057
0.063
0.117
0.057
0.058
0.103
0.139
0.151
0.156
0.157
0.158
0.160
0.160
0.159
0.159
0.158
0.158
0.158
Methane
ppm Uncertainly
2.439 0.400
1.493 0.478
2,9*9 OJM
2,773 «L35»
0.556
0.572
0.575
0.572
0573
0.571
0.572
0.573
0.569
0.564
0.558
0.555
0.554
0.554
0.553
0.555
0.557
0.558
3.344 0.398
0.562
0.562
0.562
0.563
0.566
0.565
0.563
0.561
0.562
0.564
0.560
3.369 0.409
3.024 0.429
1.390 0.522
3.132 0.406
3.005 0.411
1.508 0.488
0.530
0.548
0.557
0.561
0.563
0.569
0.568
0.567
0.566
0.566
0.565
0565
CO
ppm Uncertainty
3.962
5.359
24.100 3.215
IUM 3.130
6.354
6.503
6.524
6.470
6.473
6.439
6.436
6.452
6.419
6.366
6.329
6.293
6.245
6.238
6.214
6.220
6.229
6.225
11.737 3.371
6.162
6.145
6.116
6.132
6.180
6.184
6.172
6.157
6.148
6.165
6.104
12.654 3.407
12.926 3.662
5.266
11.303 3.268
11.415 3.320
9.476 4.689
5.526
5.790
5.885
5.930
5.950
5.996
5.980
5.958
$.929
5.926
5.930
5.931
m
-------
TABLE E-2. (continued)
Due Time File name
9/22/97 17:20 19220120
9/22/97 17:22 19220121
9/22/97 17:24 19220122
9/22/97 17:26 19220123
9/22/97 17:56 19220140
9/22/97 17:57 19220141
9/22/97 17:39 19220142
9/22/97 18:01 19220143
a/22/97 18:03 19220144
9/22/97 18:04 1922014)
9/22/97 18:06 19220146
9/22/97 18:08 19220147
9/22/97 18:10 19220148
9/22/97 18:11 19220149
9/22/97 18:13 19220I5O
mifil 18:15 19220151
9/22/97 18:17 192201)2
W22/97 18:18 192201)3
9/22/97 18:20 192201)4
9/22/97 18:22 192201))
9/22/97 18:24 192201)6
9/22/97 18:2) 192201)7
9/22/97 18:27 19220158
4/22/97 19:08 OUTSP03
9/22/97 19:11 OUTSPO4
Average — >
Carbonyl ailfkle
ppm Uncertainty
0.128
a 128
0.128
0.128
0.07S
0.077
0.10)
0.121
0.126
0.128
0.129
0.130
0.129
0.129
0.129
0.129
0.129
0.129
0.129
0.128
0.128
0.128
0.128
0.068
0.070
0125
Propane
ppm Uncertainty
1.07)
1.074
1.07)
1.079
4.208 0.601
6133 0.40)
0.9)3
I.O43
1.076
1.088
1.0%
1.100
1.098
1.099
1.097
1.097
I.O98
1.098
1.096
1.094
1.092
1.089
1.089
0.764
0.784
0.484 1.008
Cumene
ppm Uncertainly
2.037
2.03)
2.036
2.043
1.483
1516
1.806
1.976
2.037
2.061
2.076
2.084
2.079
2.082
2.079
2.078
2.079
2.080
2.076
2.073
2.069
2.064
2.063
1.448
1.485
0.08) 1.965
Hexane
ppm Uncertainly
1.040
1.039
1.039
I.O43
13.891 0.5)7
12.474 ' 0)66
6.244 0.667
2.149 0.722
1.040
1.0)2
1.060
1.064
1.061
1.063
I.O6I
1.061
1.061
1.062
1.060
1.0)8
1.056
1.053
1.053
0.274
0.28*
1.549 0970
p-Xytne
ppm Uncertainly
1.4))
1.4)3
1.4)0
1.469
0523
0543
0.997
1.300
1.399
1.434
1.4)1
1.466
1.461
1.464
4.01) 1.268
4.002 1.270
4.008 1.269
1.46)
1.462
1.45)
1.449
1.4)0
1.452
1.978 .0.471
6.46V
1.986 1.250
2.2.4-
Tnmclhyipcnune
ppm Uncertainly
0.501
0500
0.5OO
0.502
1.275 0.29)
0.373
0.444
0.486
0501
0.507
0)10
0512
0511
0512
0511
0511
0511
0511
0510
0.509
0.509
0.507
O.)07
0.356
0.365
0.050 0.483
EUiylene
ppm Uncertainly
0.1)7
0.1)7
0.1)7
0.1)9
0.0)7
0.0)9
0.108
0.141
0.1)1
O.I))
0.1)7
0.1)8
0.1)8
0.1)8
0.1)9
0159
0.1)9
0.1)8
0.1)8
0.1)7
0.1)7
0.1)7
0.1)7
0.049
0.051
0.148
Methane
ppm Uncertainly
0.563
0.562
0.562
0.564
2.92) 0.417
2.8)2 0.429
1.334 0520
0.546
0.563
0.569
0.574
0.576
0.574
0.575
0.574
0.574
0.57)
0575
0.)74
0.573
O.J72
0.570
0.570
I.S3S 0.439
1.716 0.464
0365 0.547
CO
ppm Uncertainly
5.930
5.926
5.921
5.941
9.900 3.227
10.202 3.34)
4.877
).608
5846
).932
).979
5995
5.972
5.970
).9S2
5949
).9S9
).9S3
5.949
5.944
5.944
).94I
).»39
3.156
3.243
1.262 5.772
m
-------
TABLE E-2. (continued)
Dale Time File lume
9/23/97 9:12 19230UD6
W23/97 9:14 19230007
9/23/97 9:1) 19230008
OT3/97 9:17 192301)09
9/23/97 9:19 19230010
9/23/97 9:21 I92JOOII
9/23/97 9:22 19230012
9/23/97 9:24 19230013
9/23/97 9:26 19230014
9/23/97 9:28 19230015
W23/97 9:30 I923UUI6
M23/V7 9.31 1923UI17
9/23/97 9:33 19230018
9/23/97 9:35 I92300'I9
W23/97 9:37 19230020
W23W7 9:38 I923O02I
OT3/97 9:40 19230022
a/23/97 9:42 19230023
9/23/97 9:44 19230024
9/23/97 10:16 I923UU42
9/23/97 10:17 19230043
W23/V7 10:19 19230044
9/23/97 10:21 I9230U45
W23/97 10:23 19230046
9/23/97 10:25 19230047
9/23/97 10:26 19230048
9/23/97 10:28 19230049
9/23/97 10:30 19230050
9/23/97 10:32 19230051
W23/97 10:33 19230052
9/23/97 IO:3S 19230053
9/23/97 10:37 19230054
W23/97 10:39 I923OU55
W23/97 10:40 19230056
W23/97 10:42 19230057
W23/V7 10:44 19230058
M/21/97 10:46 19230059
OT3/97 10:48 I923O06O
SV23/97 11:16 19230076'
9/23/97 11:18 19230077
9/23/97 11:19 19230078
9/23/97 11:50 OUTSPOS
9/23/97 11:52 OUTSF06
W23/97 12:35 I923UW6
9/23/97 12:37 19230097
D/23/97 12:38 I923O098
9/23/97 12:40 19230099
9/23/97 12:42 19230100
9/23/97 12:44 19230101
9/23/97 12.45 19230102
OT3/97 12:47 19230103
Carbonyl sulfide
ppm Uoccnumy
0.113
a 142
0.141
0.146
0.148
0.148
0.141
0.148
0.148
0.147
0.147
0.148
0.149
0.148
0.149
0.149
0.150
0.149
0.150
0.114
0.139
0.145
0.146
0.146
0146
0.147
0.147
0.147
O.I4S
0.145
0.145
0.145
0.148
0.151
0.151
0.150
0.154
0.152
0.113
0.138
0.138
O.Otli
0.015
0.084
0.108
0.134
0.142
0.144
0 144
0.145
0 145
Propane
ppm Uncertainly
0.863
1.054
1.086
1.0%
I.IIO
1 113
I.I 17
1 118
I.I 14
1.109
1.105
(III
1 115
1 III
1 119
1.128
1.134
1 131
1.138
4.742 0.461
1.061
1.106
1.120
1.123
1.127
1.129
1.132
1.124
1.112
1.110
1.105
1.105
1.129
1.153
1.154
1.154
1.184
1.180
3.875 0.460
1.069
1.083
0.437
0.416
3.652 0.473
3.810 0.458
1.067
.113
.126
.128
131
.135
Cumene
ppm Uncertainly
1.634
1.997
2.057
2.O75
2.1O4
2.109
2.116
2.118
2.110
2.101
2094
2.104
2.113
2.104
2.121
2.137
2.148
2.143
2.156
1.754
2.009
2.095
2.121
2.127
2.134
2.140
2.144
2.129
2.107
2.103
2.093
2.093
2.139
2.184
2.187
2.187
2.243
2.235
1.749
2.024
2.052
1.554
1.54D
5.213 0.547
1.734
2.021
2.109
2.134
2.137
2.142
2 ISO
He June
ppm Uncertainly
0.834
1.019
1.050
1.059
1.074
1.077
1.080
1.081
1.077
1.072
1.069
1074
1.079
1.074
1.082
1.091
1.097
1.094
1 101
8.697 0.645
3.007 0.709
1.070
1.083
1.086
I.O89
1.092
I.O94
1.087
1.076
1.073
1.069
1.068
1.092
.115
.116
.116
.145
.141
6.890 0.643
2.430 0.720
I.O48
0.306
0.305
12.903 0.570
8.009 0.640
2.774 0.725
1.076
1.089
1.091
1094
1.097
p-Xylene
ppm Unceiuimy
1.192
1.526
1.565
1.584
1.597
1.605
1.608
1.607
1.598
1.588
1.585
1.589
1.590
1.588
1.604
1.602
1.610
1.609
1.614
0.899
1.410
1.537
1.567
1.581
1.582,
1.582
1.588
1.579
1.570
1.560
1.555
1.560
1.578
1.597
1.602
1.601
1.626
1.589
0.903
1.393
1.351
24U71 0.610
24.5X7 0.417
0.586
0.878
1.381
1.512
1.559
1.554
1.561
1 568
2.2.4-
Tnmelhyipeiuanc
ppm Uncertainly
0.402
0.491
0.506
0.510
0.517
0.518
0.520
0.521
0.519
0.516
0.515
0.517
0.519
0.517
0.521
0.525
0.528
0.527
0.530
0.431
0.494
0.515
0.521
0.523
0.525
0.526
0.527
0.523
0.518
0.517
0.515
0.514
0.526
0.537
0.538
0.338
0.551
0.549
0.430
0.498
0504
0.38J
OJ»I
0.373
0.426
0.497
0.518
0.524
0.525
0.527
0.528
Elayfew
ppm UoccfUuniy
0.621 0.111
0.165
0.169
0.171
0.173
0.173
0.174
0.174
0.173
0.172
0.171
0.172
0.172
0.172
0.173
a 173
0.174
0.174
0.174
0.097
0.152
0.166
0.169
0.171
0.171
0.171
0.172
0.171
0.170
0.169
0.168
0.169
0.171
0.173
0.173
0.173
0.176
0.172
0.098
0.151
0.146
0.416 0.076
0.411 0.07*
0.063
0.095
0.149
0.163
0.169
0.168
0.169
0169
Mellune
ppm UocefUinly
0.451
0.552
0.168
0.173
0.581
0.583
0.584
0.585
0.583
0.580
0.578
0.581
0.584
0.581
0.586
0.590
0.593
0.592
0.596
2.075 0.488
0.554
0.579
0.586
0.588
0.590
0.591
0.592
0.588
0.582
0.581
0.578
0.578
0.591
0.603
0.604
0.604
0.620
0.618
1.855 0.487
0.519
0.567
U»3 0.44*
JJ87 0.445
3.090 0.424
1.926 0.485
0.558
0.583
0.589
0.590
O.592
0594
CO
ppm Uncertainly
11.071 1.169
6.150
6.732
6.761
6.829
6.834
6.814
6.869
6.853
6.817
6.811
6.869
6.905
6.863
6.903
6.918
6.943
6.903
6.951
5.270
6.432
6.722
6.759
6.755
6.761
6.784
6.810
6.783
6.730
6.725
6.707
6.695
6.855
6.990
6.973
6.943
7.109
7.047
5.208
6.366
6.406
11.275 3.707
11.293 3.691
3.658
4.995
6.205
6.558
6.673
6.681
6.697
6.717
oo
-------
TABLE E-2. (continued)
Dale Time File name
9/23/97 12:49 19230104
mVfl 12:51 19230105
OT3/97 12:52 19230106
W23/97 12:54 19230107
S/23/97 12:56 I92301O8
W23/W7 12:58 19230109
9/23/97 13:00 192301 10
W23/97 13:01 192301 II
it/23/97 13:03 192301 12
W23/97 13:05 192301 13
SV23/97 13:07 192301 14
It/23/97 13:08 19230115
W23/97 13:10 19230116
W23/97 13:12 192301 17
OT3/97 13:44 19230135
W23/97 13:46 19230136
K/23/97 13:47 19230137
Avenge — >
Cutaunrl sulfrfc
ppm Uncertainly
a 146
a 146
0.146
a 146
0.147
0.146
0.146
0.146
0.146
0.146
0.146
0.146
0.146
0.144
0.118
0.139
U.I 33
0143
Propane
ppm Uncertainly
1.142
1.150
1.154
1.157
1.158
1.152
1.149
1.147.
1.144
1.143
1.142
1.144
1.149
1.138
0.978
1 100
1065
0.244 I.O77
Cumene
ppm Uncertainly
2.163
2.178
2.185
2.193
2.194
2.182
2.178
2.174
2.168
2.164
2.163
2.167
2.177
2.155
1.852
2.084
2.017
0.079 2.075
Hexane
ppm Uncertainly
.104
.112
.115
.119
.120
.114
.112
.110
.107
.105
.104
.106
.III
.100
6.3U8 0.681
2.IU3 0.754
3.243 0.731
0.854 1025
p-Xylene
ppm Uncertainly
1.570
1.582
1.584
1.588
1.589
1.587
1.586
1.585
1.572
1.566
1.568
1.569
1.573
1.544
1.015
1.431
1.294
1.501
2.2.4-
Trimelhylpemane
ppm Uncertainly
0.532
0.535
0.537
0.539
0.539
0.536
0.535
0.534
0.533
0.532
0.532
0.533
0.535
0.530
0.455
0.512
0.496
0.514
Elhylene
ppm Uncertainly
0.170
0.171
0.171
0.172
0.172
0.172
0.171
0.171
0.170
0.169
0.170
0.170
O.I70
0.167
O.I 10
0.155
0.140
0009 0.162
Methane
ppro Uncertainly
0.598
0.602
0.604
0.606
0.6O6
0603
0.602
0.601
0.599
0.598
0.598
0.599
0.601
0.595
1.350 0.531
0.576
0.557
0.156 0.578
CO
ppm Uncertainly
6.748
6.756
6.761
4.776
6.779
6.776
6.767
6.769
. 6.760
6.756
6.758
6.749
6.765
6.657
5.463
6.420
6.164
0168 6.591
m
-------
TABLE E-2. (continued)
Due Time File name
9/23/97 16:41 19230158
9/23/97 16:43 19230159
9/23/V7 |6:45 19230160
9/23/97 16:47 19230161
mvn 16:49 19230162
9/23/97 16:50 19230163
9/23/97 16:52 19230164
9/23/97 16:54 19230165
9/23/97 16:56 19230166
9/23/97 16:57 19230167
9/23/97 16:59 19230168
9/23/97 17:01 19230169
9/23/97 17:03 19230170
9/23/97 17:04 19230171
9/23/W 174)6 19230172
9/23/97 17:08 19230173
9/23/97 17:42 1923WI92
9/23/97 17:43 19230-193
9/23*7 17:45 IWWISK
9/23/97 17:47 19230-195
9/23/97 17:49 19230M96
9/23/97 17:51 I9230'I97
9/23/97 17:52 I92WI98
9/23/97 17:54 I9230'I99
9/23/97 17:56 19230200
9/23/97 17:5)1 19230201
9/23/97 17:59 19230202
9/23/97 18:01 19230203
9/23/97 18:03 I92302O4
9/23/97 18:05 19230205
mvn 18:07 19230206
#23/97 18:08 19230207
9/23/97 18:10 19230208
W23/97 18:19 OUISIW7
9/23/97 18:21 OUTSTM
W.vn 18:34 OUTSm
9/23/97 19:11 19230227
mvn 19:13 19230228
9/23/97 19:15 19230229
9/23/97 19:16 19230230
mvn 19:18 19230231
9/23/97 19:20 19230232
9/23/97 19:22 19230233
mvn 19:23 19230234
9/23/97 19:25 19230235
9/23/97 19:27 19230236
9/23/97 19:29 19230237
9/23/97 19:30 19230238
9/23/97 19:32 19230239
9/2J/97 19:34 19230240
9/23/97 19:36 19230241
Carbunyl sulfide
ppm Uncertainly
0.113
am
am
a 142
0.142
a M3
0.143
a 143
0.143
0.143
0.143
a 143
0.143
0.143
0.142
0.142
0.114
0.138
0.143
0.144
0.144
0.146
0.151
0.150
0.147
0.146
0.145
0.145
0.145
0.144
0.144
a 144
0.144
MM
«.M4
MK>
0.101
0.126
0.134
0.137
0.138
0.138
0.137
0.136
0.136
0.136
0.136
0.136
0.137
0.136
0136
Propane
ppm Uncertainly
4.301 0.410
1306 0.495
1.0%
1.106
1.108
1 112
1 109
1.108
1.106
1.105
1.104
1.105
1.106
1.104
1.102
1 101
2.516 0.469
2.162 0.502
1.113
1 115
1.116
1.132
1.169
1.165
1.148
1.137
1.130
1.123
1.119
1.117
1.115
1 117
I.I 17
•JIM
•Jtt
Wit
3.219 0.431
2.854 0.462
1.040
1.058
1.066
1.066
1.062
1.056
1.052
1.050
1.051
1.049
1.050
1.048
1.043
Cumene
ppm Unceruiniy
1.818
2.026
2.076
2.O96
2.O99
2.107
2.101
2.098
2.095
2.094
2.092
2.092
2.095
2.091
2.088
2.085
4.057 0.657
2.051
2.108
2.112
2.114
2.144
2.215
2.206
2.174
2.154
2.140
2.128
2.121
2.117
2.112
2.116
2.115
1.141
1.519
1.496
4.276 0.604
1.878
1.969
2.005
2.019
2.020
2.012
2.OUI
1.993
1.990
I.99O
1.986
1.990
1.985
1.976
Hcune
ppm Uncertainly
7.698 0.617
1.034
1.060
1.070
1.071
1.075
1.072
1.071
1.069
1.069
1.068
1.068
1.069
1.067
1.066
1.064
5.132 0.610
1.047
1.076
1.078
1.079
1.095
1.131
1.126
II 10
1.099
1.092
1.086
1.082
1.081
1.078
1.080
1.080
«X7M
t.775
0.743
6.603 0.561
0.959
1.005
1.023
1.030
1.031
1.027
1.021
1.017
1.016
1.016
1.014
1.016
1.013
I 009
p-Xylene
ppm Unceruiniy
0.886
3.835 1.209
3.691 1.294
3.801 1.325
3.770 1.332
3.785 1.346
3.737 1.338
3.760 1.339
3.729 1.335
3.706 1.332
3.616 1.326
3.635 1.326
3.623 1.329
3.609 1.328
3.687 1.333
3.714 1.334
0.899
3.797 1.217
3.638 1.309
3.666 1.329
3.651 1.336
3.667 1.359
3.913 1.380
3.948 1.375
3.927 1.364
3.800 1.357
3.722 1.347
3.684 1.341
3.623 1.337
3.604 1.336
3.617 1.336
3642 1.338
3.698 1.341
3J44 1431
1*7* OJJ7
H65
0.785
1.274
3.761 1.252
3.541 1.301
3.621 1.316
3.619 1.325
3.648 1.321
3.593 1.316
3.567 1.311
3.495 1.3 II
I.5O9
1.506
1.509
3.387 1.301
3.415 1.303
2.2,4-
Trimethylpeuane
ppm Uncertainly
0.447
0.498
0.510
0.515
0.516
0.518
0.516
0.516
0.515
0.515
0.514
0.514
0.515
0.514
0.513
0.513
0.449
0.504
0.518
0.519
0.520
0.527
0.544.
0.542
0534
0.529
0.526
0.523
0.521
0.520
0.519
0.520
0.520
-------
TABLE E-2. (continued)
3ale Time File name
9/23/97 1*38 19730242
9/23/97 19:39 19230243
!»/23/97 20:13 19230262
a/23/97 20:15 19230263
9/23/97 20:17 19230264
W23/97 20: Ig I923O265
9/23/V7 2O:20 I923U266
D/23/97 20:22 19230267
9/23/97 20:24 1923026H
9/23/97 20:25 192302*9
K/23/97 20:27 19230270
9/23/97 20:29 19230271
9/23/97 20:31 19230272
W23/97 20:32 19230273
9/23/97 20:34 19230274
9/23/97 20:36 19230275
W23/97 20:38 19230276
9/23/97 20:39 19230277
Average — >
Carbunyl sullkle
ppm UacefUiniy
a 136
0136
0.091
0.119
0.129
0.133
0.134
0.135
0.134
0.134
0.135
0.135
0.135
0.135
O135
0.135
O.I 35
O.I 36
0.137
Propane
ppm Uncertainly
1.044
I.O49
3090 0.401
2.453 0.452
l.OOO
1.023
1.034
1.039
1.041
1042
1.042
1.042
I.O4I
1.039
1.039
1.039
1.039
I.O43
0.347 1.005
Cumene
ppm Uncertainly
1.978
1.987
4.675 0.562
1.787
1.894
1.937
1.960
1.967
1.973
1.974
1.974
1.974
1.972
1.969
1.969
1.969
1.968
1.976
0.197 1.972
Heunc
ppm Uncertainty
1.009
1.014
7.591 0.522
2.520 0.634
0.967
0.989
1.000
I.OO4
1.007
1.007
1.008
1.007
1.007
1.005
1.005
1.005
1.005
I.U08
0.448 1.009
p-Xylcne
ppm Uncertainty
3.457 1.309
3.516 1.314
• 0.668
1.197
1.399
1.471
3.401 1.294
3.482 1.307
3.535 1.309
3.531 1311
3.503 1311
3.453 1.309
3.417 1.307
1.507
1 SOI
I.5O4
1.504
1 511
2.761 1.313
2.2.4-
Trimelhylpealane
ppm Uncertainty
0.486
0.488
0.382
0.439
0.466
0.476
0.482
0.484
0.485
0.485
0.485
0.485
0.485
0.484
0.484
. 0.484
0.484
0.486
0.497
Elhyfcne
ppm Uncertainty
0.164
0.164
0.234 0.069
0.129
0.151
0.159
0.162
0.164
0.164
0.164
0.164
O.I64
0.164
0.163
O.I62
0.163
0.163
0.163
0.016 0.1S9
Methane
npro Uncertainty
0.546
0.549
3.001 0.417
1.755 0.479
1.242 0.507
1.098 0.519
0.541
0.544
0.545
0.545
0.545
0.545
0.545
0.544
0.544
0.544
0.544
0.546
0.401 0.555
CO
ppm Uncertainly
6.274
6.284
4.210
5.486
5.955
6.136
6.204
6.225
.6.218
6.223
6.227
6.249
6.245
6.246
6.254
6.249
6.260
6.278
0.185 6.334
-------
TABLE E-3. RESULTS FROM APP COATINGS ROOF STACKS
Date Time File name
9/24/97 12:20 19240001
12:22 19240002
Run 1 12:23 19240003
12:25 19240004
12:27 19240005
12:29 19240006
12:30 19240007
12:32 19240008
12:34 19240009
12:36 19240010
12:38 19240011
12:39 19240012
12:41 19240013
12:43 19240014
12:45 19240015
12:46 19240016
12:48 19240017
12:50 19240018
12:52 19240019
12:54 19240020
12:55 19240021
12:57 19240022
12:59 19240023
13:01 19240024
13:02 19240025
13:04 19240026
13:06 19240027
13:08 19240028
13:09 19240029
13:11 19240030
13:13 19240031
13:15 19240032
13:17 19240033
13:18 19240034
13:20 19240035
13:22 19240036
13:24 19240037
13:25 19240038
13:27 19240039
13:29 19240040
13:31 19240041
13:33 19240042
Hexane
ppm Uncertainty
0.67
0.72
1.5 0.52
1.6 0.53
1.7 0.53
1.7 0.52
1.7 0.52
1.8 0.52
1.8 0.52
1.9 0.52
1.9 0.51
2.0 0.52
2.0 0.52
2.0 0.52
2.1 0.53
2.1 0.53
1.9 0.53
1.9 0.52 .
2.1 0.53
2.1 0.52
2.0 0.53
2.0 0.53
2.0 0.54
2.1 0.53
2.0 0.53
1.9 0.53
1.8 0.53
1.8 0.54
1.8 0.54
1.9 0.54
1.9 0.54
1.9 0.54
1.9 0.54
2.0 0.54
1.9 0.54
1.9 0.54
1.9 0.55
1.9 0.55
1.8 0.56
1.8 0.56
1.8 0.56
1.9 0.56
Methane
ppm Uncertainty
3.1 0.38
3.2 0.40
3.4 0.41
3.4 0.41
3.4 0.41
3.3 0.41
3.3 0.41
3.4 0.40
3.3 0.40
3.3 0.40
3.2 0.40
3.2 0.40
3.4 0.41
3.4 0.41
3.4 0.41
3.5 0.41
3.5 0.41
3.6 0.41
4.0 0.41
3.7 0.41
3.6 0.41
3.5 0.41
3.6 0.42
3.6 0.41
3.7 0.41
- 3.7 0.41
3.5 0.41
3.4 0.42
3.4 0.42
3.7 0.42
3.8 0.42
' 3.8 0.42
3.7 0.42
3.6 0.42
3.5 0.42
3.5 0.42
3.6 0.43
4.0 0.43
3.8 0.43
3.8 0.44
3.9 0.44
3.8 0.43
Carbon monoxide
ppm Uncertainty
14.0 3.5
13.6 3.8
11.4 3.9
11.5 4.0
11.8 4:0
11.4 3.9
13.0 3.9
13.5 3.9
10.6 3.9
10.9 3.9
11.3 3.9
10.8 4.0
13.3 4.0
13.7 4.0
13.9 4.0
15.9 4.0
18.2 4.0
21.9 3.9
44.3 4.1
28.9 4.0
29.3 4.0
34.7 4.1
43.6 4.2
33.3 4.1
38.0 4.0
39.8 4.0
30.4 3.9
23.4 4.0
20.1 4.0
18.9 4.0
17.9 4.0
16.1 4.0
14.6 4.0
13.5 4.0
13.5 4.0
13.1 4.0
23.2 4.1
56.3 4.2
42.7 4.2
42.5 4.2
53.5 4.3
44.4 4.2
E-12
-------
TABLE E-3. (continued)
Date Time File name
13:34 19240043
13:36 19240044
Average — >
Hexane
ppm Uncertainty
1.9 0.55
1.9 0.55
1.8 0.54
Methane
ppm Uncertainty
3.7 0.43
3.7 0.43
3.5 0.42
Carbon monoxide
ppm Uncertainty
40.6 4.1
38.9 4.1
24.0 4.0
E-13
-------
TABLEE-3. (continued)
Date Time File name
9/24/97 14:11 19240064
14:13 19240065
Run 2 14:15 19240066
14:17 19240067
14:19 19240068
14:20 19240069
14:22 19240070
14:24 19240071
14:26 19240072
14:27 19240073
14:29 19240074
14:31 19240075
14:33 19240076
14:34 19240077
14:36 19240078
14:38 19240079
14:40 19240080
14:42 19240081
14:43 19240082
14:45 19240083
14:47 19240084
14:49 19240085
14:50 19240086
14:52 19240087
14:54 19240088
14:56 19240089
14:57 19240090
14:59 19240091
15:01 19240092
15:03 19240093
15:05 19240094
15:06 19240095
15:0» 19240096
15:10 19240097
Average — >
Hexane
ppm Uncertainty
1.8 0.54
2.0 0.56
2.0 0.56
2.3 0.56
2.4 0.56
2.3 0.56
2.4 0.56
2.6 0.56
2.4 0.57
2.4 0.57
2.4 0.57
2.4 0.57
2.2 0.57
2.1 0.57
2.2 0.56
2.2 0.56
2.2 0.56 .
2.5 0.56
2.5 0.56
2.3 0.56
2.3 0.56
2.3 0.56
2.2 0.56
2.1 0.56
2.1 0.56
2.0 0.56
2.0 0.56
2.0 0.56
2.0 0.56
1.9 0.55
2.1 0.55
2.0 0.55
1.9 0.55
1.9 0.55
2.2 0.56
Methane
ppm Uncertainty
3.2 0.42
3.3 0.44
3.3 0.44
3.3 0.44
3.4 0.43
3.4 0.44
3.5 0.44
3.7 0.44
3.6 0.44
3.7 0.44
3.5 0.45
3.4 0.45
3.3 0.45
3.2 0.44
3.2 0.44
3.2 0.44
3.2 0.44
3.2 0.44
3.2 0.44
3.2 0.44
3.1 0.44
3.1 0.44
3.1 0.44
3.0 0.44
3.0 0.44
3.0 0.44
3.0 0.44
3.0 0.44
3.1 0.43
3.3 0.43
3.3 0.43
3.3 0.43
3.3 0.43
3.3 0.43
3.3 0.44
Carbon monoxide
ppm Uncertainty
7.4 3.7
23.3 3.9
23.1 4.0
21.9 4.0
24.6 4.0
20.6 4.0
18.4 4.0
29.1 4.1
25.4 4.1
31.6 4.1
26.8 4.0
24.9 4.0
24.9 4.0
21.0 3.9
24.8 3.9
28.8 3.9
29.8 3.9
28.3 3.9
27.5 4.0
25.6 3.9
22.1 3.9
22.5 3.9
26.4 3.9
22.3 3.8
24.1 3.8
21.9 3.8
17.1 3.8
16.3 3.8
17.4 3.7
23.9 3.7
20.3 3.8
17.2 3.9
16.0 3.8
19.5 3.8
22.8 3.9
E-14
-------
TABLEE-3. (continued)
Date Time File name
9/24/97 15:12 19240098
15:13 19240099
Run 3 15:15 19240100
15:17 19240101
15:19 19240102
15:21 19240103
15:22 19240104
15:24 19240105
15:26 19240106
15:28 19240107
15:29 19240108
15:31 19240109
15:33 19240110
15:35 19240111
15:36 19240112
15:38 19240113
15:40 19240114
15:42 19240115
15:44 19240116
15:45 19240117
15:47 19240118
15:49 19240119
15:51 19240120
15:52 19240121
15:54 19240122
15:56 19240123
15:58 19240124
15:59 19240125
16:01 19240126
16:03 19240127
16:05 19240128
16:07 19240129
16:08 19240130
16:10 19240131
16:12 19240132
16:14 19240133
16:15 19240134
16:17 19240135
16:19 19240136
16:21 19240137
16:22 19240138
16:24 19240139
16:26 19240140
Hexane
ppm Uncertainty
1.9 0.56
1.9 0.56
1.8 0.56
1.8 0.56
1.8 0.57
1.9 0.56
2.0 0.56
2.0 0.56
1.8 0.55
1.8 0.55
1.9 0.55
1.8 0.55
1.6 0.55
1.7 0.55
1.6 0.55
1.5 0.54
1.6 0.54 .
1.6 0.54
1.6 0.54
1.7 0.54
1.6 0.54
1.7 0.54
1.6 0.54
1.6 0.54
1.5 0.54
1.5 0.54
1.5 0.54
1.4 0.55
1.4 0.55
1.5 0.55
1.6 0.55
1.5 0.55
1.5 0.55
1.4 0.55
1.3 0.55
1.3 0.55
1.3 0.55
1.3 0.56
1.3 0.56
1.3 0.56
1.3 0.56
1.3 0.56
1.4 0.56
Methane
ppm Uncertainty
3.4 0.44
3.3 0.44
3.4 0.44
3.3 0.44
3.3 0.44
3.4 0.44
3.9 0.44
4.1 0.44
3.8 0.43
3.5 0.43
3.4 0.43
3.2 0.43
3.1 0.43
3.0 0.43
2.8 0.43
2.8 0.42
2.9 0.42
2.8 0.42
2.8 0.42
2.9 0.42
2.8 0.42
2.8 0.42
2.8 0.42
2.7 0.42
2.8 0.42
2.8 0.42
2.7 0.42
2.7 0.43
2.7 0.43
2.7 0.43
2.8 0.43
2.7 0.43
2.7 0.43
2.8 0.43
2.8 0.43
2.7 0.43
2.8 0.43
2.8 0.44
2.7 0.44
2.8 0.44
2.7 0.44
2.7 0.44
2.7 0.44
Carbon monoxide
ppm Uncertainty
23.3 3.8
23.4 3.8
28.2 3.8
26.1 3.8
21.5 3.8
27.8 3.8
23.6 3.8
21.7 3.8
21.6 3.7
19.5 3.7
29.4 3.7
26.6 3.7
20.1 3.6
19.6 3.6
16.2 3.5
12.6 3.5
10.7 3.5
9.6 3.5
9.0 3.4
8.6 3.4
8.1 3.4
8.2 3.4
8.0 3.4
7.8 3.4
7.6 3.4
7.7 3.4
7.9 3.4
7.9 3.4
8.0 3.4
7.9 3.4
8.0 3.4
7.9 3.5
8.0 3.4
8.0 3.4
8.1 3.4
7.9 3.4
8.0 3.4
8.1 3.5
8.1 3.5
8.3 3.5
8.2 3.5
8.3 3.4
8.5 3.5
E-15
-------
TABLE E-3. (continued)
Date Time File name
16:28 19240141
16:30 19240142
16:31 19240143
16:33 19240144
16:35 19240145
16:37 19240146
16:38 19240147
18:12 inspOT
18:14 inspOS
18:16 insp09
Average — >
Hexane
ppm Uncertainty
1.4 0.56
1.4 0.56
1.2 036
0.56
0.57
0.57
0.56
1.5 0.23
1.5 0.23
1.6 0.23
1.5 0.55
Methane
ppm Uncertainty
2.8 0.44
2.7 0.44
2.7 0.44
2.6 0.44
2.9 0.44
2.7 0.44
2.7 0.44
3.2 037
3.6 0.37
3J 0.37
3.0 0.43
Carbon monoxide
ppm Uncertainty
8.4 3.5
8.8 3.5
8.5 3.5
8.1 3.4
8.2 3.4
8.1 3.4
8.2 3.3
21.9 2.8
20.5 2.8
20.2 2.8
13.1 3.5
E-16
-------
TABLE E-4. RESULTS FROM SBS COATER ROOF STACK
Date Time File name
9/24/97 13:38: 19240045
9/24/97 13:40: 19240046
9/24/97 13:41: 19240047
9/24/97 13:43: 19240048
9/24/97 13:45: 19240049
9/24/97 13:47: 19240050
9/24/97 13:48: 19240051
9/24/97 13:50: 19240052
9/24/97 13:52: 19240053
9/24/97 13:54: 19240054
9/24/97 13:56: 19240055
9/24/97 13:57: 19240056
9/24/97 13:59: 19240057
9/24/97 14:1: 19240058
9/24/97 14:3: 19240059
9/24/97 14:4: 19240060
9/24/97 14:6: 19240061
9/24/97 14:8: 19240062
9/24/97 14:10: 19240063
9/25/97 8:25: 19250003
9/25/97 8:27: 19250004
9/25/97 8:29: 19250005
9/25/97 8:31: 19250006
9/25/97 8:32: 19250007
9/25/97 8:34: 19250008
9/25/97 8:36: 19250009
9/25/97 8:38: 19250010
9/25/97 8:40: 19250011
9/25/97 8:41: 19250012
9/25/97 8:43: 19250013
9/25/97 8:45: 19250014
9/25/97 8:47: 19250015
9/25/97 8:48: 19250016
9/25/97 8:50: 19250017
9/25/97 8:52: 19250018
9/25/97 8:54: 19250019
9/25/97 8:56: 19250020
9/25/97 8:57: 19250021
9/25/97 8:59: 19250022
9/25/97 9:1: 19250023
9/25/97 9:3: 19250024
9/25/97 9:4: 19250025
9/25/97 9:6: 19250026
9/25/97 9:8: 19250027
9/25/97 9:10: 19250028
9/25/97 9:11: 19250029
9/25/97 9:13: 19250030
Hexane
ppm Uncertainty
1.9 0.54
1.6 0.52
1.5 0.51
1.4 0.51
1.4 0.52
1.4 0.52
1.3 0.52
1.3 0.52
1.3 0.52
1.4 0.52
1.4 0.51
1.4 0.51
1.4 0.51
1.5 0.51
1.5 0.51
1.4 0.52
1.4 0.52
1.4 0.52
1.4 0.52
1.5 0.16
1.7 0.17
1.8 0.18
1.8 0.18
1.9 0.18
1.9 0.18
1.9 0.18
1.9 0.18
2.0 0.18
2.0 0.18
2.0 0.18
2.0 0.18
2.0 0.18
2.0 0.18
2.0 0.19
2.0 0.19
2.0 0.19
2.0 0.19
2.0 0.19
2.0 0.19
2.0 0.19
2.0 0.19
2. 0.19
2. 0.19
2. 0.19
2. 0.19
2. 0.19
2. 0.20
Methane
ppm Uncertainty
3.6 0.42
3.3 0.40
3.3 0.40
3.4 0.40
3.4 0.40
3.3 0.41
3.2 0.41
3.2 0.41
3.1 0.40
3.0 0.40
3.0 0.40
3.0 0.40
3. 0.40
3. 0.40
3. 0.40
3. 0.40
3. 0.41
. 3. 0.41
3.2 0.41
3.0 0.25
3.5 0.27
3.6 0.28
3.6 0.29
3.6 0.29
3.6 0.29
3.6 0.29
3.6 0.29
3.6 0.29
3.5 0.29
3.5 0.29
3.4 0.29
3.4 0.29
3.6 0.30
3.5 0.30
3.5 0.30
3.3 0.30
3.5 0.31
3.6 0.31
3.4 0.30
3.4 0.30
3.7 0.30
3.8 0.31
3.7 0.31
3.6 0.31
3.6 0.31
3.4 0.31
3.7 0.31
CO
ppm Uncertainty
32.9 4.0
17.2 3.7
8.7 3.6
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
3.8
2.5
6.0 2.6
6.8 2.7
7.9 2.7
8.7 2.7
8.4 2.7
8.3 2.7
8.0 2.7
8.9 2.7
8.7 2.7
7.4 2.7
6.8 2.7
7.4 2.7
8.1 2.7
8.7 2.7
10.0 2.7
8.2 2.6
7.5 2.7
7.1 2.7
6.5 2.6
6.7 2.6
16.3 2.7
17.7 2.7
14.6 2.7
14.2 2.7
22.9 2.7
16.8 2.7
17.6 2.7
E-17
-------
TABLE E-4. (continued)
Date Time File name
9/25/97 9:15: 19250031
9/25/97 9:17: 19250032
9/25/97 9:19: 19250033
9/25/97 9:20: 19250034
9/25/97 9:22: 19250035
9/25/97 9:24: 19250036
9/25/97 9:26: 19250037
9/25/97 9:27: 19250038
9/25/97 9:29: 19250039
9/25/97 9:40: 19250045
9/25/97 9:42: 19250046
9/25/97 9:43: 19250047
9/25/97 9:45: 19250048
9/25/97 9:47: 19250049
9/25/97 9:49: 19250050
9/25/97 9:50: 19250051
9/25/97 9:52: 19250052
9/25/97 9:54: 19250053
9/25/97 9:56: 19250054
9/25/97 9:58: 19250055
9/25/97 9:59: 19250056
9/25/97 10:1: 19250057
9/25/97 10:3: 19250058
9/25/97 10:5: 19250059
9/25/97 10:6: 19250060
9/25/97 10:8: 19250061
9/25/97 10:10: 19250062
9/25/97 10:12: 19250063
9/25/97 10:13: 19250064
9/25/97 10:15: 19250065
9/25/97 10:17: 19250066
9/25/97 10:19: 19250067
9/25/97 10:20: 19250068
9/25/97 10:22: 19250069
9/25/97 10:24: 19250070
9/25/97 10:26: 19250071
9/25/97 10:27: 19250072
9/25/97 10:29: 19250073
9/25/97 10:31: 19250074
9/25/97 10:33: 19250075
9/25/97 10:35: 19250076
9/25/97 10:36: 19250077
9/25/97 10:38: 19250078
9/25/97 10:40: 19250079
9/25/97 10:42: 19250080
9/25/97 10:43: 19250081
9/25/97 10:45: 19250082
Hexane
ppm Uncertainty
2.1 0.20
2.2 0.20
2.2 0.20
2.1 0.20
2.2 0.20
2.1 0.20
2.1 0.20
2.2 0.20
2.1 0.20
2.2 0.20
2.2 0.20
2.2 0.20
2.2 0.20
2.2 0.20
2.2 0.21
2.2 0.21
2.2 0.21
2.2 0.21
2.2 0.21
2.1 0.21
2.2 0.21
2.2 0.21
2.2 0.21
2.2 0.21
2.2 0.21
2.3 0.21
2.2 0.21
2.3 0.21
2.3 0.22
2.3 0.22
2.3 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.5 0.22
2.5 0.22
2.5 0.22
2.5 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
2.4 0.22
Methane
ppm Uncertainty
3.8 0.32
4.4 0.32
4.0 0.32
3.9 0.32
3.8 0.32
3.6 0.32
3.9 0.32
3.8 0.32
3.7 0.32
3.8 0.33
3.7 0.33
3.9 0.33
3.8 0.33
3.7 0.33
3.5 0.33
3.6 0.33
3.6 0.34
3.5 0.34
3.3 0.34
3.3 0.34
3.3 0.34
3.4 0.34
3.8 0.34
3.7 0.34
3.5 0.34
3.7 0.34
3.6 0.34
3.7 0.34
3.6 0.35
3.3 0.35
3.0 0.35
3.2 0.35
3.7 0.35
3.6 0.35
3.5 0.35
3.6 0.35
3.6 0.35
3.7 0.35
3.4 0.35
3.4 0.35
3.6 0.36
3.6 0.36
3.8 0.36
3.5 0.36
3.6 0.36
3.6 0.36
3.4 0.36
CO
ppm Uncertainty
25.1 2.7
46.5 2.9
28.3 2.7
24.2 2.7
19.9 2.7
14.2 2.7
27.3 2.7
27.3 2.7
18.2 2.7
19.6 2.7
20.1 2.7
29.5 2.7
26.1 2.7
17.8 2.7
13.8 2.7
18.3 2.7
15.8 2.7
20.0 2.7
17.2 2.7
11.9 2.6
13.9 2.6
13.7 2.6
30.1 2.7
28.5 2.7
19.3 2.7
23.5 2.7
16.4 2.7
25.4 2.7
22.5 2.7
14.2 2.7
12.4 2.6
14.8 2.7
27.3 2.7
20.2 2.7
15.8 2.7
18.7 2.7
19.4 2.7
33.3 2.8
23.9 2.7
19.3 2.7
19.7 2.7
-23.0 2.7
38.1 2.8
21.3 2.7
21.2 2.7
19.5 2.7
13.7 2.6
E-18
-------
TABLE E-4. (continued)
Date Time File name
9/25/97 10:47: 19250083
9/24/97 18:29: outsplO
9/24/97 18:31: outspll
9/24/97 18:33: outspll
9/25/97 11:26: SBSSP01
9/25/97 11:30: SBSSP02
9/25/97 11:32: SBSSP03
Average — >
Hexane
ppm - Uncertainty
2.4 0.22
1.0 0.46
1.0 0.46
1.1 0.43
2.0 0.21
1.9 0.21
1.9 0.21
2.0 0.26
Methane
ppm Uncertainty
3.4 0.36
3.5 036
3.5 0.36
33 034
4.0 034
3.9 033
3.9 033
3.5 0.34
CO
ppm Uncertainty
21.2 2.6
10.5 2.7
103 2.7
10.4 2.7
31.8 23
28.1 23
21.7 23
14.4 2.9
E-19
-------
TABLE E-5. RESULTS FROM APP MIXING TANK
Date
9/25/97
Time
13:06
13:08
13:09
13:11
13:13
13:15
13:16
13:18
13:20
13:22
13:24
13:25
13:27
13:29
13:31
13:32
13:34
13:36
13:38
13:39
13:41
13:43
13:45
13:47
13:48
13:50
13:52
13:54
13:55
13:57
13:59
14:01
14:02
File name
19250097
19250098
19250099
19250100
19250101
19250102
19250103
19250104
19250105
19250106
19250107
19250108
19250109
192501 10
19250111
192501 12
19250113
19250114
19250115
19250116
19250117
19250118
19250119
19250120
19250121
19250122
19250123
19250124
19250125
19250126
19250127
19250128
19250129
Carbonyl sulfide
ppm Uncertainty
0.53 0.080
0.55 0.081
0.54 0.082
0.55 0.082
0.57 0.083
0.58 0.084
0.58 0.083
0.59 0.083
0.63 0.084
0.63 0.085
0.63 0.085
0.63 0.086
0.64 0.086
0.65 0.086
0.67 0.087
0.66 0.086
0.69 0.087
0.70 0.087
0.73 0.088
0.75 0.089
0.75 0.089
0.78 0.090
0.79 0.091
0.79 0.092
0.79 0.092
0.79 0.092
0.80 0.093
0.80 0.092
0.81 0.092
0.83 0.093
0.85 0.094
0.88 0.094
0.89 0.094
Methanoi
ppm Uncertainty
0.10 0.01
0.10 0.01
0.10 0.01
0.11 0.01
0.11 0.01
0.11 0.01
0.11 0.01
0.12 0.01
0.12 0.01
0.12 0.01
0.12 0.01
0.12 0.01
0.12 0.01
0.13 0.01
0.13 0.01
0.13 0.01
0.13 0.01
0.13 0.01
0.14 0.01
0.14 0.01
0.14 0.01
0.15 0.01
0.15 0.01
0.15 0.01
0.15 0.01
0.15 0.01
0.16 0.01
0.16 0.01
0.16 0.01
0.16 0.01
0.16 0.01
0.17 0.01
0.17 0.01
Ethylene
ppm Uncertainty
1.2 0.3
1.2 0.3
1.2 0.3
1.2 0.3
1.2 0.3
1.2 0.3
1.2 0.3
1.2 0.4
1.3 0.4
1.3 0.4
1.3 0.4
1.3 0.4
1.4 0.4
1.4 0.4
1.4 0.4
1.4 0.4
1.4 0.4
1.4 0.4
1.5 0.4
1.5 0.5
1.5 0.5
1.5 0.5
1.5 0.5
1.5 0.5
1.5 0.5
1.5 0.5
1.6 0.5
1.5 0.5
1.5 0.5
1.5 0.5
1.6 0.5
1.6 0.5
1.6 0.6
Sulfur dioxide
ppm Uncertainty
8.5
8.8
9.0
9.2
9.5
9;7
9.8
10.0
10.4
10.5
10.5
10.7
10.9
11.1
11.3
11.4
11.8
12.0
12.4
12.8
13.0
13.5
13.8
14.0
14.1
14.2
14.4
14.4
14.5
14.9
15.1
15.5
15.7
CO
ppm Uncertainty
40.0 3.5
42.7 3.6
45.9 3.6
49.3 3.6
52.2 3.7
55.2 3.7
55.7 3.7
55.1 3.7
55.5 3.7
56.6 3.7
58.5 3.7
61.0 3.8
62.7 3.8
62.4 3.8
61.1 3.8
60.0 3.8
58.8 3.8
58.6 3.9
59.6 3.9
60.5 3.9
61.9 3.9
64.1 4.0
65.1 4.0
65.6 4.0
67.5 4.
68.5 4.
68.0 4.
66.7 4.
65.0 4.
63.1 4.
61.2 4.
60.1 4.2
59.7 4.2
m
K>
o
-------
TABLEE-5. (continued)
Date
Average — >
Time
14:04
14:06
14:08
14:10
14:11
14:13
14:15
14:17
14:18
14:20
File name
19250130
19250131
19250132
19250133
19250134
19250135
19250136
19250137
19250138
19250139
Carbonyl sulfide
ppm Uncertainty
0.91 0.095
0.90 0.094
0.88 0.093
0.87 0.092
0.85 0.091
0.85 0.091
0.84 0.091
0.89 0.093
0.94 0.094
0.99 0.096
0.74 0.089
Methanol
ppm Uncertainty
0.17 0.01
0.17 0.01
0.17 0.01
0.16 0.01
0.16 0.01
0.16 0.01
0.16 0.01
0.17 0.01
0.17 0.01
0.18 0.01
0.14 0.01
Ethylene
ppm Uncertainty
.6 0.6
!6 0.6
.8 0.6
.8 0.6
.7 0.6
.7 0.6
.7 0.6
.8 0.6
.9 0.6
2.0 0.6
1.49 0.46
Sulfur dioxide
ppm Uncertainty
16.1
16.0
32.3 15.8
33.2 15.7
34.1 15.6
35.2 15.5
35.8 15.4
36.6 16.2
37.4 16.8
38.5 17.6
6.59 12.98
CO
ppm Uncertainty
60.1 4.2
58.5 4.2
56.6 4.1
54.8 4.1
53.6 4.0
52.9 4.0
53.3 4.0
55.5 4.1
57.4 4.1
58.8 4.2
58.35 3.93
m
-------
TABLE E-6. SBS MIXING TANK 11
Date
9/25/97
Time
17:05
17:07
17:09
17:11
17:12
17:14
17:16
17:18
17:20
17:21
17:23
17:25
17:27
17:28
17:30
17:32
17:34
17:35
17:37
17:39
17:41
17:43
17:44
17:46
17:48
17:50
17:51
17:53
17:55
17:57
17:58
18:00
18:02
18:21
18:24
18:26
Average — >
File name
19250146
19250147
19250148
19250149
192501 SO
19250151
19250152
19250153
19250154
19250155
19250156
19250157
19250158
19250159
19250160
19250161
19250162
19250163
19250164
19250165
19250166
19250167
19250168
19250169
19250170
19250171
19250172
19250173
19250174
19250175
19250176
19250177
19250178
T11SP01
T11SP02
T11SP03
Carbonyl sulfide
ppm Uncertainty
0.14 0.06
0.15 0.06
0.12 0.06
0.06
0.06
0.13 0.06
0.13 0.06
0.12 0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.06
0.05
0.05
0.05
0.02 0.06
Hexane
ppm Uncertainty
44.13 0.56
48.75 0.65
46.52 0.63
37.90 0.56
41.08 0.60
43.45 0.64
43.54 0.66
42.74 0.68
41.99 0.70
40.75 0.71
39.25 0.71
38.49 0.71
37.64 0.71
37.04 0.71
36.16 0.70
36.20 0.71
35.97 0.71
35.62 0.70
35.77 0.71
35.21 0.70
35.20 0.70
34.83 0.70
34.60 0.70
34.60 0.69
35.05 0.70
34.81 0.69
35.52 0.70
36.92 0.71
37.41 0.72
37.23 0.71
37.04 0.71
37.30 0.71
37.30 0.71
25.47 0.58
24.56 0.59
24.63 0.60
38.36 0.68
Methane
ppm Uncertainty
4.99 0.51
5.22 0.58
4.83 0.57
3.61 0.51
4.58 0.55
4.93 0.58
4.82 0.60
4.60 0.62
4.52 0.63
4.40 0.64
4.37 0.64
4.24 0.65
4.06 0.65
4.09 0.64
4.08 0.64
4.05 0.64
4.04 0.64
4.06 0.64
4.33 0.64
4.18 0.64
4.08 0.64
4.09 0.64
4.03 0.63
3.97 0.63
4.10 0.63
4.02 0.63
4.02 0.64
4.13 0.65
4.23 0.65
4.19 0.65
4.25 0.64
4.24 0.64
4.18 0.64
3.% 0.53
3.90 0.54
3.94 0.55
4.29 0.62
Sulfur dioxide
ppm Uncertainty
107.49 6.80
118.14 7.38
115.49 7.18
106.55 6.57
101.28 6.25
99.15 6.14
96.13 5.94
91.67 5.66
86.98 5.35
82.33 5.06
77.81 4.78
74.27 4.58
71.84 4.43
70.40 4.35
68.92 4.27
67.88 4.20
66.88 4.15
66.02 4.11
65.35 4.10
65.14 4.08
65.16 4.07
64.73 4.04
64.16 4.00
63.75 4.00
63.77 4.01
63.29 4.00
63.42 3.99
64.50 4.05
64.91 4.10
65.50 4.12
65.52 4.12
66.06 4.16
66.61 4.19
47.74 3.12
46.77 3.08
46.63 3.07
77.0 4.8
CO
ppm Uncertainty
14.44 2.44
11.94 2.67
9.75 2.66
6.27 2.50
7.80 2.64
8.66 2.72
8.61 2.73
8.51 2.72
7.95 2.74
8.19 2.72
8.06 2.71
7.73 2.69
7.28 2.68
7.03 2.68
6.85 2.66
6.75 2.68
6.83 2.68
6.90 2.66
7.22 2.68
7.11 2.66
7.17 2.65
7.24 2.65
7.06 2.63
6.93 2.63
7.24 2.64
7.31 2.63
11.12 2.65
13.57 2.69
10.66 2.69
9.05 2.68
12.01 2.68
18.44 2.69
17.02 2.69
33.49 2.27
32.19 2.27
34.70 2.29
9.1 2.7
Ammonia
ppm Uncertainty
1.31
1.43
1.39
1.27.
2.66 1.26
3.11 1.24
3.34 1.20
3.48 1.14
3.62 1.08
3.74 1.02
3.81 0.97
3.96 0.93
4.06 0.90
4.23 0.88
4.28 0.86
4.31 0.85
4.33 0.84
4.37 0.83
4.57 0.83
4.60 0.82
4.63 0.82
4.69 0.82
4.72 0.81
4.76 0.81
4.98 0.81
5.05 0.81
5.16 0.81
5.47 0.82
5.72 0.83
5.74 0.83
5.80 0.83
6.00 0.84
6.03 0.85
3.96 0.63
3.93 0.62
4.04 0.62
4.0 0.96
frt
K>
to
-------
TABLE E-7. RESULTS FROM APP HOLDING TANK 1
Due Tone filename
mbffl 16:8 APFU1
16:17 APP02
16:21 APP03
l*:25 APfOT
Dilution APPO4
Corrtclfd
16:48 APP05.
17:6 APP06
17:10 APP07
Average — >
Bftwnr
ppm Unceruimy
10.7 X*
ta.y
65.9 2.0
CarbonyliulftJe
ppm Uncertainty
1.9 0.081
1.11 0.090
0.53 0.047
•.11 0.8J3
a?
1.0 0.070
J.5 0.076
2.7 0.084
1.6 O.I
Elhyfcae dichluride
ppm Uncertainly
5.0 1.7
S.4 1.8
2.7 I.I
0.47
8.7 IS
21.7 3.4
22.7 3.5
9.5 l.«
Mclhanul
ppm Unceruimy
0.029 O.OU5
0.035 O.OU5
0.028 O.UU3
0.013 0.001
O.I
0.054 0.004
0.10 0.010
0.11 0.010
O.I 0.0
Heune
ppm Uncertainly
It5 IJ
101.6
101.6 1.3
PrupunaUehyde
ppm Uncertainty
16.0 2,0
VS.7
98.7 2.0
Sulfur HimiHo
ppm Uncertainly
174.2 5.9
169.3 6.1
60.6 3.8
!*.» 1.4
1O4.I
S5.0 5.4
103.5 12.1
IU0.5 12.3
109.6 6.7
CO
ppm Uncertainly
220.5 4.0
219.3 4.0
85.7 2.1
I9J 1.4
118.7
90.9 3.1
132.0 3.4
135.6 3.7
143.2 3.1
Ammonia
ppm Uncertainly
6.3 1.04
6.1 I.I
3.3 0.62
1.7 O3*
10.4
6.4 0.91
20.5 2.0
22.7 2.1
10.8 I.I
FormaMehyde
ppm Unceruimy
21.7 1.5
IJJ6
133.6 1.5
m
to
-------
TABLE E-8. RESULTS FROM SBS HOLDING TANK 3
Date
9/26/97
9/26/97
9/26/97
9/26/97
9126191
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26191
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
Average — >
Time
10:17
10:19
10:20
10:22
10:24
10:26
10:28
10:29
10:31
10:33
10:35
10:36
10:38
10:40
10:42
10:43
10:45
10:47
10:49
10:51
10:52
10:54
10:56
10:58
10:59
11:01
11:03
11:05
11:06
11:08
11:10
11:12
11:14
11:15
11:42
11:46
File name
19260007
19260008
19260009
19260010
19260011
19260012
19260013
19260014
19260015
19260016
19260017
19260018
I92600'19
19260020
19260021
19260022
19260023
19260024
19260025
19260026
19260027
19260028
19260029
19260030
19260031
19260032
19260033
19260034
19260035
19260036
19260037
19260038
19260039
1*260040
T3SP01
T3SP02
Carbonyl sulfide
Uncer-
ppm tainiy
0.8S 0.11
0.96 0.11
0.99 0.11
0.98 0.11
0.95 0.11
0.92 0.11
0.90 0.11
0.87 0.11
0.84 0.11
0.82 0.10
0.80 0.10
0.77 0.10
0.75 0.099
0.74 0.099
0.72 0.098
0.70 0.0%
0.69 0.0%
0.68 0.095
0.67 0.094
0.66 0.094
0.65 0.093
0.63 0.092
0.63 0.092
0.62 0.091
0.61 0.090
0.61 0.089
0.59 0.089
0.59 0.088
0.59 0.088
0.59 0.088
0.58 0.087
0.59 0.087
0.58 0.087
0.58 0.087
0.47 0.072
0.35 0.065
0.73 0.098
Uncer-
ppm lainly
0.0028
0.0025
0.0024
0.0023
0.0022
0.0059 0.0019
0.0062 0.0018
0.0066 0.0018
0.0067 0.0018
0.0068 0.0018
0.0069 0.0018
0.0070 0.0017
0.0072 0.0018
0.0073 0.0018
0.0076 0.0018
0.0076 0.0017
0.0077 0.0018
0.0079 0.0018
0.0078 0.0018
0.0088 0.0019
04082 0.0018
0.0092 0.0019
0.010 0.0019
0.011 0.0019
0.01 1 0.0019
0.01 1 0.0019
0.012 0.0020
0.012 0.0020
0.012 0.0020
0.012 0.0020
0.012 0.0020
0.013 0.0020
0.013 0.0020
0.013 0.0021
0.013 0.0020
0.012 0.0018
0.0078 0.0020
Meihanol
Uncer-
ppm lainty
11.94 0.83
13.42 0.89
13.05 0.91
12.50 0.89
11.31 0.86
10.40 0.85
9.61 0.82
8.73 0.80
7.% 0.78
7.36 0.76
6.81 0.73
6.04 0.71
5.46 0.70
4.97 0.69
4.49 0.68
4.20 0.65
3.51 0.65
3.06 0.64
2.68 0.64
2.3 0.63
2.3 0.61
1.7 0.61
1.4 0.61
1.3 0.59
0.64
0.64
0.63
0.63
0.62
0.62
0.62
0.61
0.61
0.62
0.56
0.59
4.6 0.70
Uncer-
ppm lainly
75.9 1.1
79.8 1.2
80.7 1.2
78.8 1.2
76.1 1.2
74.1 1.2
71.4 1.1
68.9 I.I
66.8 1.1
65.2 1.0
62.6 1.0
60.5 0.98
59.4 0.97
58.3 0.95
57.1 0.93
54.7 0.89
54.2 0.89
53.8 0.89
53.2 0.88
52.5 0.87
50.7 0.84
50.6 0.84
50.3 0.84
49.0 0.82
49.4 0.72
48.8 0.71
48.2 0.70
47.9 0.70
47.2 0.69
46.8 0.69
46.8 0.69
46.4 0.69
46.1 0.69
46.4 0.69
39.9 0.65
39.2 0.69
58.2 0.91
Propane
Uncer-
ppm lainty
23.6 1.8
26.1 1.9
26.9 1.9
26.8 1.9
26.1 1.9
25.8 1.8
25.2 1.8
24.6 1.7
24.2 1.7
23.8 1.6
23.2 1.6
22.6 1.5
22.4 1.5
22.1 1.5
21.8 1.4
21.1 1.4
21.0 1.4
21.0 1.4
.20.9 1.4
20.8 1.3
20.2 .3
20.2 .3
20.2 .3
19.9 .3
20.7
20.5
20.0
19.7
19.5
19.2
19.0
19.0
18.7
18.6 .1
16.2 1.0
11.8 1.1
21.9 1.4
Heianc
Uncer-
ppm lainty
1.25
1.15
1.08
1.02
0.97
2.9 0.82
2.8 0.80
2.6 0.78
2.5 0.78
2.4 0.77
2.3 0.77
2.2 0.76
2.3 0.77
2.2 0.78
2.2 0.78
2.1 0.77
2.0 0.78
1.9 0.79
1.9 0.80
1.7 0.81
1.8 0.81
0.82
1.7 0.83
0.83
0.83
0.84
0.84
0.85
0.85
0.85
0.86
0.87
0.87
0.88
0.84
0.78
1.1 0.86
Propionaldehyde
Uncer-
ppm lainly
0.56
0.51
0.48
0.46
0.43
0.42
0.41
0.40
0.40
0.40
0.40
0.39
0.39
0.40
0.40
0.39
0.39
0.40
0.40
0.41
0.40
0.41
0.41
0.41
0.42
0.42
1.3 0.42
1.3 0.43
1.3 0.43
1.4 0.43
1.4 0.43
1.4 0.44
1.4 0.44
1.5 0.44
2.1 0.37
1.7 0.34
0.32 0.42
Styrene
Uncer-
ppm lainty
1.2
1.1
1.0
0.99
0.95
0.92
0.90
0.88
0.87
0.87
0.86
0.85
0.86
0.86
0.86
0.85
0.85
0.87
0.88
0.89
0.88
0.89
3.5 0.83
3.5 0.83
3.7 0.84
3.8 0.84
2.7 0.93
2.8 0.94
2.7 0.94
2.8 0.95
2.9 0.95
3.0 0.%
.1 0.%
.2 0.98
1.9 0.82
1.9 0.76
.1 0.92
1.1.2.2-
Teuacj;prpeljame
Uocer-
ppm lainty
20.2 0.89
22.0 0.95
22.2 0.97
21.9 0.95
21.0 0.93
20.3 0.91
19.6 0.88
18.8 0.85
18.1 0.83
17.6 0.82
16.9 0.79
16.2 0.77
15.7 0.75
15.3 0.74
14.8 0.73
14.3 0.70
13.9 0.69
13.6 0.69
13.3 0.68
12.9 0.67
12.6 0.65
12.3 0.65
12.0 0.65
11.7 0.64
11.5 0.64
11.3 0.63
11.0 0.62
10.8 0.62
10.6 0.61
10.4 0.61
10.2 0.61
10.1 0.61
9.9 0.61
9.8 0.62
8.0 0.58
6.7 0.62
14.8 0.73
m
-------
TABLE E-8. (continued)
Date
9/26/97
9/26/97
9126m
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
W26/97
9/26/97
9/26/97
9126191
9/76/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9126191
W26/97
9/26/97
9/26/97
9/26/97
9/26/97
9126191
9126191
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
9/26/97
Average — >
Time
10:17
10:19
10:20
10:22
10:24
10:26
10:28
10:29
10:31
10.33
10:35
10:36
10:38
10.40
10:42
10:43
10:45
10.47
10:49
10:51
10:52
10:54
10:56
10:58
10:59
11:01
11:03
11:05
11:06
11:08
11:10
11:12
11:14
11:15
11:42
11:46
File name
19260007
19260008
19260009
19260010
19260011
19260012
19260013
19260014
19260015
19260016
19260017
19260018
I92600'19
19260020
19260021
19260022
19260023
19260024
19260025
19260026
19260027
19260028
19260029
19260030
19260031
19260032
19260033
19260034
19260035
19260036
19260037
19260038
19260039
19260040
T3SPOI
T3SP02
p-Xylene
Uncer-
ppm tainty
46.1 2.9
42.8 2.6
42.0 2.5
38.9 2.3
39.5 2.2
40.2 2.2
41.5 2.1
43.1 2.1
45.2 2.1
47.7 2.1
48.8 2.1
50.0 2.0
52.5 2.0
54.8 2.1
56.7 2.1
56.0 2.0
57.8 2.1
60.5 2.1
62.7 2.1
64.1 2.2
64.0 2.2
65.0 2.2
66.4 2.2
65.9 2.2
67.2 2.2
68.1 2.2
67.7 2.3
68.8 2.3
69.2 2.3
69.7 2.3
70.9 2.3
71.6 2.3
71.8 2.3
73.1 2.4
66.3 2.3
62.8 2.1
57.4 2.2
Methane
Uncer-
ppm lainly
93.4 4.7
105.2 5.0
110.3 5.1
113.4 5.0
114.2 4.9
116.1 4.9
117.0 4.8
117.2 4.7
118.3 4.7
119.6 4.6
119.4 4.6
1 19.0 4.5
120.0 4.4
120.8 4.4
121.2 4.3
120.4 4.3
120.5 4.2
121.4 4.2
121.8 4.
121.9 4.
121.5 4.
121.7 4.
122.5 4.
121.9 4.0
121.6 4.0
122.3 3.9
121.5 3.9
121.5 3.9
121.5 3.9
121.0 3.9
121.3 3.8
122.2 3.8
121.4 3.8
121.8 3.8
109.7 3.2
88.6 2.9
118.7 4.3
Sulfur dioxide
Uncer-
ppm lainly
26.1 0.56
26.9 0.51
27.2 0.48
26.6 0.46
25.6 0.43
24.9 0.42
23.8 0.41
22.8 0.40
21.8 0.40
20.8 0.39
19.6 0.39
18.7 0.39
17.9 0.39
17.1 0.39
16.3 0.40
15.3 0.39
14.8 0.39
14.2 0.40
13.6 0.41
13.1 0.41
12.4 0.41
12.1 0.41
11.6 0.42
II .0 0.42
10.8 0.42
10.3 0.42
10.0 0.43
9.7 0.43
9.2 0.43
8.9 0.43
8.8 0.43
8.4 0.44
8.3 0.44
8.1 0.45
5.1 0.42
5.4 0.39
16.1 0.42
CO
Uncer-
ppm lainly
9.2 1.2
10.1 1.3
10.7 1.3
10.6 1.3
10.4 1.3
10.4 1.2
10.1 1.2
9.9 1.2
9.8 1.1
9.8 I.I
9.4 1.1
9.2 1.0
9.2 1.0
9.2 1.0
9.1 1.00
8.6 0.95
8.6 0.95
8.7 0.94
8.8 0.94
8.7 0.92
8.4 0.90
8.5 0.90
8.6 0.90
8.3 0.87
8.2 0.86
8.2 0.85
8.2 0.85
8.3 0.84
8.2 0.83
8.2 0.83
8.4 0.83
8.3 0.82
8.4 0.82
8.5 0.83
7.3 0.78
6.9 0.83
9.0 1.0
m
-------
APPENDIX F
EPA METHOD 320 AND EPA FTIR PROTOCOL
-------
3. Appendix A of part 63 is amended by adding, in numerical
order,.Methods 320, 321, and 322 to read as follows:
Appendix A to Part 63-Test Methods
*****
(PROPOSED) TEST METHOD 320
MEASUREMENT OF VAPOR PHASE ORGANIC AND INORGANIC EMISSIONS
BY EXTRACTIVE FOURIER TRANSFORM INFRARED (FTIR) 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
extractive. Flue gas is extracted through a heated gas
transport and handling system. For some sources, sample
conditioning systems may be applicable. Some examples are
given in this method. Note: sample conditioning systems
may be used providing the method validation requirements in
Sections 9.2 and 13.0 of this method are met.
1.1 Scope and Applicability.
1.1.1 Analytes. Analytes include hazardous air pollutants
(HAPs) for which EPA reference spectra have been developed.
Other compounds can also be measured with this method if
reference spectra are prepared according to section 4.6 of
the protocol.
1.1.2 Applicability. This method applies to the analysis
of vapor phase organic or inorganic compounds which absorb
energy in the mid-infrared spectral region, about 400 to
4000 cm"1 (25 to 2.5 um). This method is used to determine
compound-specific concentrations in a multi-component vapor
phase sample, which is contained in a closed-path gas cell.
Spectra of samples are collected using double beam infrared
absorption spectroscopy. A computer program is used to
analyze spectra and report compound concentrations.
1.2 Method Range and Sensitivity. Analytical range and
sensitivity depend on the frequency-dependent analyte
absorptivity, instrument configuration, data collection
parameters, and gas stream composition. Instrument factors
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
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 (DLj.) and analytical uncertainty
(AUJ 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
-------
gathered in a pre-test site survey. Spectral interferants
shall be identified using the selected DLj. 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 (MIUX) .
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 AUi can be maintained; if the measured analyte
concentration is less than MAUi_, 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
path (background).
2.1.2 Most molecules absorb infrared radiation and the
absorbance occurs in a characteristic and reproducible
pattern. The infrared spectrum measures fundamental
molecular properties and a compound can be identified from
its infrared spectrum alone.
2.1.3 Within constraints, there is a linear relationship
between infrared absorption and compound concentration. If
this frequency dependent relationship (absorptivity) is
known (measured), it can be used to determine compound
concentration in a sample mixture.
2.1.4 Absorptivity is measured by preparing, in the
laboratory, standard samples of compounds at known
concentrations and measuring the FTIR "reference spectra" of
these standard samples. These "reference spectra" are then
used in sample analysis: (I) 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 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.
-------
2.2 Sampling and Analysis. In extractive sampling a probe
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
(CEM) 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.
where:
Ax = absorbance at a given frequency of the ith sample
component.
at = absorption coefficient (absorptivity) of the ith
sample component.
b = path length of the cell.
cx = 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.
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.arnold.af.mil/epa/welcome.htm.
Reference spectra for HAPs, or other analytes, may also be
prepared according to section 4.6 of the Protocol.
2.4 Operator Requirements. The FTIR analyst shall be
trained in setting up the instrumentation, verifying the
instrument is functioning properly, and performing routine
maintenance. The analyst must evaluate the initial sample
spectra to determine if the sample matrix is consistent with
pre-test assumptions and if the instrument configuration is
suitable. The analyst must be able to modify the instrument
configuration, if necessary.
2.4.1 The spectral analysis shall be supervised by someone
familiar with EPA FTIR Protocol procedures.
2.4.2 A technician trained in CEM 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.
3.0 Definitions.
See appendix A of the Protocol for definitions relating
to infrared spectroscopy. Additional definitions are given
below.
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). 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
configurations or sampling temperatures.
3.5 Interferant. A compound in the sample matrix whose
infrared spectrum overlaps with part of an analyte spectrum.
The most accurate analyte measurements are achieved when
reference spectra of interferants are used in the
quantitative analysis with the analyte reference spectra.
The presence of an interferant. can increase the analytical
uncertainty in the measured analyte concentration.
3.6 Gas Cell. A gas containment cell that can be
evacuated. It is equipped with the optical components to
pass the infrared beam through the sample to the detector.
Important cell features include: path length (or range if
variable), temperature range, materials of construction, and
total gas volume.
3.7 Sampling System. Equipment used to extract the sample
from the test location and transport the sample gas to the
FTIR analyzer. This includes sample conditioning systems.
3.8 Sample Analysis. The process of interpreting the
infrared spectra to obtain sample analyte concentrations.
This process is usually automated using a software routine
-------
employing a classical least squares (els), partial least
squares (pis), or K- or P- matrix method.
3.9 One hundred percent line. A double beam transmittance
spectrum obtained by combining two background single beam
spectra. Ideally, this line is equal to 100 percent
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
filling adds no information to the interferogram, but
affects line shapes in the absorbance spectrum (and possibly
analytical results).
3.16 Reference CTS. Calibration Transfer Standard spectra
that were collected with reference spectra.
3.17 CTS Standard. CTS spectrum produced by applying a de-
resolution procedure to a reference CTS.
3.18 Test CTS. CTS spectra collected at the sampling
resolution using the same optical configuration as for
sample spectra. Test spectra help verify the resolution,
temperature and path length of the FTIR system.
3.19 RMSD. Root Mean Square Difference, defined in EPA
FTIR Protocol, appendix A.
3.20 Sensitivity. The noise-limited compound-dependent
detection limit for the FTIR system configuration. This is
estimated by the MAU. It depends on the RMSD in an
analytical region of a. zero absorbance line.
3.21 Quantitation Limit. The lower limit of detection for
the FTIR system configuration in the sample spectra. This
-------
is estimated by mathematically subtracting scaled reference
spectra of analytes and interferences from sample spectra,
then measuring the RMSD in an analytical region of the
subtracted spectrum. Since the noise in subtracted sample
spectra may be much greater than in a zero absorbance
spectrum,, the quantitation limit is generally much higher
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.
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
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
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.
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
leak check procedures. This method does not address all of
the potential safety risks associated with its use. Anyone
performing this method must follow safety and health
practices consistent with applicable legal requirements and
with prudent practice for each application.
6.0 Equipment and Supplies.
Note: Mention of trade names or specific products does
not constitute endorsement by the Environmental
Protection Agency.
The equipment and supplies are based on the schematic
of a sampling system shown in Figure 1. Either the batch or
continuous sampling procedures may be used with this
sampling system. Alternative sampling configurations may
also be used, provided that the data quality objectives are
met as determined in the post-analysis evaluation. Other
-------
10
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.
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
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
-------
11
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,
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
sample.
6.17.2 Another option is sample dilution. The dilution
factor measurement must be documented and accounted for in
the reported concentrations. An alternative to dilution is
to lower the sensitivity of the FTIR system by decreasing
the cell path length, or to use a short-path cell in
conjunction with a long path cell to measure more than one
concentration range.
7.0 Reagents and Standards.
7.1 Analyte(s) and Tracer Gas. Obtain a certified gas
cylinder mixture containing all of the analyte(s) at
concentrations within ± 2 percent of the -emission source
levels (expressed in ppm-meter/K). If practical, the
-------
.-.-••-' 12
analyte standard cylinder shall also contain the tracer gas
at a concentration which gives a measurable absorbance at a
dilution factor of at least 10:1. Two ppm SF6 is sufficient
for a path length of 22 meters at 250 °F.
7.2 Calibration Transfer Standard(s). Select the
calibration transfer standards (CTS) according to section
4.5 of the FTIR Protocol. Obtain a National Institute of
Standards and Technology (NIST) traceable gravimetric
standard of the CTS (± 2 percent).
7.3 Reference Spectra. Obtain reference spectra for each
analyte/ interferant, surrogate, CTS, and tracer. If EPA
reference spectra are not available, use reference spectra
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) AUif DLt, overall
fractional uncertainty, OFUif maximum expected concentration
(CMAXi), and tM for each, (b) potential interferants, (c)
sampling system factors, e.g., minimum absolute cell
pressure, (Prain), 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, FCra, 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
protocol, sampling and analytical procedures, and post-test
protocol calculations.
8.1 Pretest Preparations and Evaluations. Using the
procedure in section 4.0 of the FTIR Protocol, determine the
optimum sampling system configuration for measuring the
target analytes. Use available information to make
reasonable assumptions about moisture content and other
interferences.
8.1.1 Analytes. Select the required detection limit (DLJ
and the maximum permissible analytical uncertainty (AUJ for
each analyte (labeled from 1 to i). Estimate, if possible,
the maximum expected concentration for each analyte,
-------
13
The expected measurement range is fixed by DLX and CMAXt 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.
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 S4 [(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
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
-------
- 14
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 Prain. 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
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:
%VL = 50 tss i!=i ' ' (2)
where 50 = 100% divided by the leak-check time of 2 minutes.
8.2.2.5 Leak volumes in excess of 4 percent of the FTIR
system volume Vss are unacceptable.
8.3 Detector Linearity. Once an optical configuration is
chosen, use one of the procedures of sections 8.3.1 through
8.3.3 to verify that the detector response is linear. If
the detector response is not linear, decrease the aperture,
or attenuate the infrared beam. After a change in the
instrument configuration perform a linearity check until it
is demonstrated that the detector response is linear.
8.3.1 Vary the power incident on the detector by modifying
the aperture setting. Measure the background and CTS at
three instrument aperture settings: (I) at the aperture
setting to be used in the testing, (2) at one half this
aperture and (3) at twice the proposed testing aperture.
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.
-------
15
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
includes sample interferograms, processed absorbance
spectra, background interferograms, CTS sample
interferograms and CTS absorbance spectra. Additionally,
documentation of all sample conditions, instrument settings,
and test records must be recorded on hard copy or on
computer medium. Table 1 gives a sample presentation of
documentation.
8.5 Background Spectrum. Evacuate the gas cell to z 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
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
-------
16
reference spectrum procedure for neat samples (protocol,
section. 4.6). Often, interference spectra need not be
quantitative, but for best results the absorbance must be
comparable to the interference absorbance in the sample
spectra.
8.6 Pre-Test Calibrations
8.6.1 Calibration Transfer Standard. Evacuate the gas cell
to £ 5 mmHg absolute pressure, and fill the FTIR cell to
atmospheric pressure with the CTS gas. Alternatively, purge
the cell with 10 cell volumes of CTS gas. (If purge is
used, verify that the CTS concentration in the cell is
stable by collecting two spectra 2 minutes apart as the CTS
gas continues to flow. If the absorbance in the second
spectrum is no greater than in the first, within the
uncertainty of the gas standard, then this can be used as
the CTS spectrum.) Record the spectrum.
8.6.2 QA Spike. This procedure assumes that the method has
been validated for at least some of the target analytes at
the source. For emissions testing perform a QA spike. Use
a certified standard, if possible, of an analyte, which has
been validated at the source. One analyte standard can
serve as a QA surrogate for other analytes which are less
reactive or less soluble than the standard. Perform the
spike procedure of section 9.2 of this method. Record
spectra of at least three independent (section 3.22 of this
method) spiked samples. Calculate the spiked component of
the analyte concentration. If the average spiked
concentration is within 0.7 to 1.3 times the expected
concentration, then proceed with the testing. If
applicable, apply the correction factor from the Method 301
of this appendix validation test (not the result from the QA
spike).
8.7 Sampling. If analyte concentrations vary rapidly with
time, CEM sampling is preferable using the smallest cell
volume, fastest sampling rate and fastest spectra collection
rate possible. CEM sampling requires the least operator
intervention even without an automated sampling system. For
continuous monitoring at one location over long periods, CEM
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 discreet (and unique) sample volume.
Continuous static (and CEM) 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
-------
17
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 GEM 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
z 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 absorption remains.
Repeat this procedure to collect eight spectra of 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
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 CIS. 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.
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,
-------
• - . • 18
it may be necessary to use a shorter path length or dilute
the sample.
8.11.3 Compare the pre- and post-test GTS spectra. The
peak absorbance in pre- and post-test CIS 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 system is working
properly. Usually, when QA spiking is used, the method has
already been validated at a similar source for the analyte
in question. The QA spike demonstrates that the validated
sampling conditions are being duplicated. If the QA spike
fails then the sampling system shall be repaired before
testing proceeds. The method validation procedure (section
13.0 of this method) involves a more extensive use of the
analyte spike procedure of sections 9.2.1 through 9.2.3 of
this method. Spectra of at least 12 independent spiked and
12 independent unspiked samples are recorded. The
concentration results are analyzed statistically to
determine if there is a systematic bias in the method for
measuring a particular analyte. If there is a systematic
bias, within the limits allowed by Method 301 of this
appendix, then a correction factor shall be applied to the
analytical results. If the systematic bias is greater than
the allowed limits, this method is not valid and cannot be
used.
9.2.1 Introduce the spike/tracer gas at a constant flow
rate of * 10 percent of the total sample flow. (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.
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
-------
19
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:
CE1
w = ir1^ (3)
where:
Spike.,,.
cs'-Tsr* <«
DF = Dilution factor of the spike gas; this value
shall be *10.
= SF6 (or tracer gas) concentration measured
directly in undiluted spike gas.
SFs(3Pio = Diluted SF6 (or tracer gas) concentration
measured in a spiked sample.
Spikedir = Concentration of the analyte in the spike
standard measured by filling the FTIR cell
directly.
CS = Expected concentration of the spiked 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.
-------
20
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
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 (Pi) . 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 (TE) and absolute pressure (Pf) .
Calculate the FTIR cell volume Vss, including that of the
connecting tubing, as follows:
v.i
Vss ' — ?-• <»>
Pf Pt
-------
21
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
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
-------
. 22
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 =
where:
= Concentration, corrected for path length.
= Concentration, initial calculation (output of the
analytical program designed for the compound) .
Lr = Reference spectra path length.
L3 = Sample spectra path length.
T3 = Absolute temperature of the sample gas, K.
Tr = Absolute gas temperature of reference spectra, K.
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
-------
23
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.
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 HC1, 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.
-------
24
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.
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).
-------
/ 25
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
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
-------
26
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.
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).
-------
27
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
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=Sm-Mm-CS (7)
where:
B = Bias at spike level.
Sm = Mean concentration of the analyte spiked
samples.
M,, = Mean concentration of the unspiked 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
-------
28
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 * CF s 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.
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.
-------
29
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".
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.
-------
- .. .. 30
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), 73-84, 1985.
-------
31
Table 1. EXAMPLE PRESENTATION OF SAMPLING DOCUMENTATION.
Saaple Tiae
Spectra File Maae
Backgroiud File Hume
Saaple coMUtiiwlag
Process c
Saaple Tiae
SpectniB File
laterfieragraa
•esalMtiiM
Scams
Afo^iutioa
Gala
CTS Spectrua
-------
32
Calfcration Gas Line
Mass Flow Calibfation Gas Manifold
Meter f~ 1
rh® • !*iu ii n i ii »*
To Calibration
Gas Cylinder
Pump«2
Figure 1. Extractive FTIR sampling system.
-------
33
.8-
.6-
.4-
.2
0
FRU = SRMS(FU-FL)/BAV
SRMS = .00147
BAV = 3.662
FM = FRU = .086
p-xylene
1050
1000
i
950
900
Wavenumbers
850
i
800
i
750
Figure 2. Fractional Reproducibility. Top: average of cts!031a and
ctsllOlb. Bottom: Reference spectrum of p-xylene.
-------
PROTOCOL FOR THB USB OF EXTRACTIVE FOURIER TRANSFORM
INFRARED (FTIR) SPBCTROMETRY FOR THB 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.
-------
2.2.2 The absorption spectra of pure gases and of mixtures
of gases are described by a linear absorbance theory referred to
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 Veriflability and Reproducibility of Results. Store
all data and document data analysis techniques sufficient to
allow an independent agent to reproduce the analytical results
from the raw in.terferometric 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
-------
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 reference
spectra.
3.3.2 Sample-Dependent Factors. Examples are spectral
interferants (e.g., water vapor and C02) 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 PRB-TBST 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 (AUt) . 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 (DL^, ppm) .
The detection limit is the lowest concentration of an analyte for
which its overall fractional uncertainty (OFU^ is required to be
less than its analytical uncertainty limit (AUi) .
4.1.4 Maximum expected concentration of each analyte
(CMAXt, ppm) .
4.2 Identify Potential Interferants. Considering the
chemistry of the process or results of previous Studies, identify
potential interferants, i.e., the major effluent constituents and
any relatively minor effluent constituents that possess either
strong absorption characteristics or strong structural
similarities to any analyte of interest. Label them 1 through
N.J, where the subscript "j"- pertains to potential interferants.
Estimate the concentrations of these compounds in the effluent
(CPOT.J, ppm) .
-------
4.3 Select and Evaluate the Sampling System. Considering
the source, e.g., temperature and pressure profiles, moisture
content, analyte characteristics, and particulate concentration),
select the equipment for extracting gas samples. Recommended are
a particulate filter, heating system to maintain sample
temperature above the dew point for all sample constituents at
all points within the sampling system (including the filter), and
sample conditioning system (e.g., coolers, water-permeable
membranes that remove water or other compounds from the sample,
and dilution devices) to remove spectral interferants or to
protect the sampling and analytical components. Determine the
minimum absolute sample system pressure (Pnin, 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 (L3' , meter), sample pressure (P3' , kPa) , absolute
sample temperature Ts', and signal integration period (tss/
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 leas
than one half the smallest value AUi (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.
Mote: It may be necessary to choose preliminary analytical
regions (see Section 4.7), identify the minimum analyte
linewidths, or estimate the system noise level (see
Section 4.12) before selecting the CTS. More than one
compound may be needed to meet the criteria; if so, obtain
separate cylinders for each compound.
4.5.1 The central- wavenumber position of each analytical
region lies within 25 percent of the wavenumber position of at
least one CTS absorption band.
4.5.2 The absorption bands in 4.5.1 exhibit peak
absorbances greater than ten times the value RMSEST (see
Section 4.12) but less than 1.5 absorbance units.
4.5.3 At least one absorption CTS band within the operating
range of the FTIR instrument has an instrument -independent
linewidth no greater than the narrowest analyte absorption band;
perform and document measurements or cite Studies to determine
analyte and CTS compound linewidths.
4.5.4 For each analytical region, specify the upper and
lower wavenumber positions (FFUm and FFLm, 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 meets the criterion of
Section 4.5.3.
-------
4.5.5 Associate, whenever possible, a single set of CTS gas
cylinders with a set of reference spectra. Replacement CTS gas
cylinders shall contain the same compounds at concentrations
within 5 percent of that of the original CTS cylinders; the
entire absorption spectra (not individual spectral segments) of
the replacement gas shall be scaled by a factor between 0.95 and
1.05 to match the original CTS spectra.
4.6 Prepare Reference Spectra.
Note: 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 (L0) 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
-------
sample pressure (PR), sample temperature (TR) , reference
absorption pathlength (LR) , and interferogram signal integration
period (tSR). Signal integration periods for the background
interferograius shall be 2tSR. Values of PR, LR, and tSR shall not
deviate by more than ±1 percent from the time of recording {Rl}
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.
4.8 Determine Fractional Reproducibility Uncertainties.
Using Appendix E, calculate the fractional reproducibility
uncertainty for each analyte (FRUL) from a comparison of {Rl} and
{R2}. If FRUt > AUt for any analyte, the reference spectra
generated in Section 4.6 are not valid for the application.
4.9 Identify Known Interferants. Using Appendix B,
determine which potential interferant affects the analyte
concentration determinations. If it does, relabel the potential
interferant as "known" interferant, and designate these compounds
from k = 1 to K. Appendix B also provides criteria for
determining whether the selected analytical regions are suitable.
4.10 Prepare Computerized Analytical Programs.
-------
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 (PRH 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
(FCUi) according to Appendix F, and compare these values to the
fractional uncertainty limits (AU^- see Section 4.1) . If
FCUt > AUt), either the reference spectra or analytical programs
for that analyte are unsuitable.
4.12 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 interferant (MIUk, ppm)
using Appendix D. Verify that (a) MAUL < (AUt) (DLt) , FRUL < AUi(
and FCUt < AUt for each analyte and that (b) the CTS chosen meets
the requirements listed in Section 4.5.
5.0 SAMPLING AND ANALYSIS PROCEDURE
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
(Lfl) and leak volume (VL) , where VL = LR tss. Leak volumes shall
be s4 percent of Vsg.
-------
5.2 Verify Instrumental Performance. Measure the noise
level of the system in each analytical region using the procedure
of Appendix G. If any noise level is higher than that estimated
for the system in Section 4.12, repeat the calculations of
Appendix D and verify that the requirements of Section 4.12 are
met; if they are not, adjust or repair the instrument and repeat
this section.
5.3 Determine the Sample Absorption Pathlength. Record a
background spectrum. Then, fill the absorption cell with CTS at
the pressure PR and record a set of CTS spectra {R3}. Store the
background and unsealed CTS single beam interferograms and
spectra. Using Appendix H, calculate the sample absorption
pathlength (L3) 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.
Note; Multiple sample spectra may be recorded according to
the procedures of Section 5.4 before performing Sections 5.5
and 5.6.
5.5 Quantify Analyte Concentrations. Calculate the
unsealed analyte concentrations RUAt and unsealed interferant
concentrations RUIK using the programs developed in Section 4.
To correct for pathlength and pressure variations between the
reference and sample spectra, calculate the scaling factor
RLPS = (LRPRTS) / (LSPSTR) . .Calculate the final analyte and
interferant concentrations RSAt = R^RUAi and RSI^ = RLPSRUIk.
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.
-------
5.6.2 Apply appropriate mathematical transformations (e g
frequency shifting, zero-filling, apodization, smoothing) to the
spectra (or to the interferograms upon which the spectra are
based) generated during the performance of the procedures of
Section 5.3. Document these transformations and their
reproducibility. Do not apply multiplicative scaling of the
spectra, or any set of transformations that is mathematically
equivalent to multiplicative scaling. Different transformations
may be applied to different analytical regions. Frequency shifts
shall be smaller than one-half the minimum instrumental
linewidth, and must be applied to all spectral data points in an
analytical region. The mathematical transformations may be
retained for the analysis if they are also applied to the
appropriate analytical regions of all sample spectra recorded,
and if all original 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 BVALUATIONS
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 RSQUIRSMBNTS
-------
-------
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 Al, 945A (1975); Appl.
Spectroscopy 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 1)," June 1978, Quality
Assurance Handbook for Air Pollution Measurement Systems,
Volume III, Stationary Source Specific Methods, EPA-600/4-
77-027b, August 1977.
-------
APPENDIX A
' ' DEFINITIONS OF TERMS AND SYMBOLS
A.. 1 Definition* of Terms
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.
Note; The quantitative result for a single analyte may be
based on data from more than one analytical region.'
apodization - modification of the ILS function by multiplying the
interferogram by a weighing function whose magnitude varies
with retardation.
background 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 (CTSJ 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; for sample
spectra, it is the quantity directly determined from Beer's
law. The units "centimeters-ppm" or "meters-ppm" are
recommended.
-------
derivative absorption spectrum - a plot of rate of change of
absorbance or of any function of absorbance with respect to
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.
Note: The term "double-beam* is used elsewhere to denote a
spectrum in which the sample and background interferograms
are collected simultaneously along physically distinct
absorption paths. Here, the term denotes a spectrum in
which the sample and background interferograms are collected
at different times along the same absorption path.
fast Fourier transform (FFT) - a method of speeding up the
computation of a discrete FT by factoring the data into
sparse matrices containing mostly zeros.
flyback - interferometer motion during which no data are
recorded.
Fourier transform (FT) - the mathematical process for converting
an amplitude-time spectrum to an amplitude-frequency
spectrum, or vice versa.
Fourier transform infrared (FTIR) spectrometer - an analytical
system that employs a source of mid-infrared radiation, an
interferometer, an enclosed sample cell of known absorption
pathlength, an infrared detector, optical elements that
transfer infrared radiation between components, and a
computer system. The time-domain detector response
(interferogram) is processed by a Fourier transform to yield
a representation of the detector response vs. infrared
frequency.
Mote: When FTIR spectrometers are interfaced with other
instruments, a slash should be used to denote the interface;
e.g., GC/FTIR; HPCL/FTIR, and the use of FTIR should be
explicit; i.e., FTIR not IR.
frequency, r - the number of cycles per unit time.
infrared - the portion of the electromagnetic spectrum containing
wavelengths from approximately 0.78 to 800 microns.
interferogram, 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.
-------
linewidth - the full width at half maximum of an absorption band
in units of wavenumbers (cm ).
mid-infrared - the region of the electromagnetic spectrum from
approximately 400 to 5000 cm"1.
pathlength - see "absorption pathlength."
reference spectra - absorption spectra of gases with known
chemical compositions, recorded at a known absorption
pathlength, which are used in the quantitative analysis of
gas samples.
retardation, o - optical path difference between two beams in an
interferometer; also known as "optical path difference" or
"optical retardation." •
scan - digital representation of the detector output obtained
during one complete motion of the interferometer's moving
assembly or assemblies.
scaling - application of a multiplicative factor to the
absorbance values in a spectrum.
single beam spectrum - Fourier-transformed interferogram,
representing the detector response vs. wavenumber.
Note: The term "single-beam" is used elsewhere to denote
any spectrum in which the sample and background
interferograms are recorded on the same physical absorption
path; such usage differentiates such spectra from those
generated using interferograms recorded along two physically
distinct absorption paths (see "double-beam spectrum"
above). Here, the term applies (for example) to the two
spectra used directly in the calculation of transmission and
absorbance spectra of a sample.
standard reference material - a reference material, the
composition or properties of which are certified by a
recognized standardizing agency or group.
Note: The equivalent ISO term is "certified reference
material.•
transmittance/ T - the ratio of radiant power transmitted by the
sample to the radiant power incident on the sample.
Estimated in FTIR spectroscopy by forming the ratio of the
single-beam sample and background spectra.
wavenumber, v - the number of waves per unit length.
Mote: The usual unit of wavenumber is the reciprocal
centimeter, cm"1. The wavenumber is the reciprocal of the
wavelength, X, when X is expressed in centimeters.
zero-filling - the addition of zero-valued points to the end of a
measured interferogram.
-------
U2LS.: Performing the FT of 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 = log,0 - = -log10T
(1)
- band area of the ith analyte in the mth analytical
region, at the concentration (CLt) corresponding to the
product of its required detection limit (DLj) and analytical
uncertainty limit
^ - average absorbance of the ich analyte in the meh
analytical region, at the concentration (CLi) corresponding
to the product of its required detection limit (DLt) and
analytical uncertainty limit
ASC, accepted standard concentration - the concentration value
assigned to a chemical standard.
ASCPP, accepted standard concent rat ion-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.
AVTm - average estimated total absorbance in the mcb analytical
region.
- estimated concentration of the kch known interferant.
- estimated maximum concentration of the ieh analyte.
CPOT, - estimated concentration of the jth potential interferant.
DLt, required detection limit - for the ith analyte, the lowest
concentration of the analyte for which its overall
fractional uncertainty (OFU^ is required to be less than the
analytical uncertainty limit (AUt) .
PC. - center wavenumber position of the mc analytical region.
FAUt, fractional analytical uncertainty - calculated uncertaint:
in the measured concentration of the i analyte because of
-------
errors in the mathematical comparison of reference and
sample spectra.
, fractional calibration uncertainty - calculated uncertainty
in the measured concentration of the ich analyte because of
errors in Beer's law modeling of the reference spectra
concentrations.
FPL, - lower wavenumber position of the CTS absorption band
associated with the mch analytical region.
m - upper wavenumber position of the CTS absorption band
associated with the meh analytical region.
- lower wavenumber position of the mth analytical region.
j, fractional modal uncertainty - calculated uncertainty in
the measured concentration of the ich analyte because of
errors in the absorption model employed.
- lower wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands .
- upper wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands .
FRQt, fractional reproducibility uncertainty - calculated
uncertainty in the measured concentration of the ith analyte
because of errors in the reproducibility of spectra from the
FTIR system.
FUm - upper wavenumber position of the mch analytical region.
j, - band area of the jch potential interferant in the mch
analytical region, at its expected concentration (CPOT^) .
- average absorbance of the ich analyte in the mth analytical
region, at its expected concentration (CPOTj) .
isci or *' indicated standard concentration - the concentration
from the computerized analytical program for a single-
compound reference spectrum for the ich analyte or kch known
interferant .
kPa - kilo-Pascal (see Pascal) .
L,1 - estimated sample absorption pathlength.
L,, - reference absorption pathlength.
L, « actual sample absorption pathlength.
MAU, - mean of the MAUln over the appropriate analytical regions.
-------
MAUlm, minimum analyte uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
(AUt) in the measurement of the ich analyte, based on spectral
data in the mc analytical region, can be maintained.
MIUj - mean of the MIUjm over the appropriate analytical regions.
MIU,., minimum interferant uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
CPOTV/20'in the measurement of the jch interferant, based on
spectral data in the meh analytical region, can be
maintained.
MIL, minimum instrumental linewidth - the minimum linewidth from
the FTIR system, in wavenumbers.
The MIL of a system may be determined by observing an
absorption band known (through -higher resolution
examinations) to be narrower than indicated by the system.
The MIL is fundamentally limited by the retardation of the
interferometer, but is also affected by other operational
parameters (e.g., the choice of apodization) .
Mt - number of analytes.
Mj - number of potential interferants.
^ - number of known interferants.
M „ - the number of scans averaged to obtain an inter ferogram.
OFUt - the overall fractional uncertainty in an analyte
concentration determined in the analysis (OFUi = MAX{FRUi(
FMUt}) .
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»m ~ minimum pressure of the sampling system during the sampling
procedure.
P,' - estimated sample pressure.
Pm - reference pressure.
P, - actual sample pressure.
RMS^ - measured noise level of the FTIR system in the mch
analytical region.
RMSD, root mean square difference - a measure of accuracy
determined by the following equation:
-------
•RMSD. =
>
n
where:
n = the number of observations for which the accuracy is
determined.
et = the difference between a measured value of a property
and its mean value over the n observations.
Note: The RMSD value "between a set of n contiguous
absorbance values (At) and the mean of the values" (A,,) is
defined as
RMSD =
>
- the (calculated) final concentration of the ith analyte.
RSIk - the (calculated) final concentration of the kth known
interferant.
tmi* acan tin* - 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, tg = Nscantscan.
tn - signal integration period used in recording reference
spectra.
t,, - signal integration period used in recording sample spectra.
Tm - absolute temperature of gases used in recording reference
spectra.
T, - absolute temperature of sample gas as sample spectra are
recorded.
TP, Throughput - manufacturer's estimate of the fraction of the
total infrared power transmitted by the absorption cell and
transfer optics from the interferometer to the detector.
VM - volume of the infrared absorption cell, including parts of
attached tubing.
wlk - weight used to average over analytical regions k for
quantities related to the analyte i; see Appendix D.
-------
Note that some terms are missing, e.g., BAVm/ OCU, RMSS , SUB
SIC,, SAC,, Ss
-------
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 me analytical region (FLn to FUJ , 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.
Note,: The average absorbance in an analytical region is the
band area divided by the width of the analytical region in
wavenumbers. The average total absorbance in an analytical
region is the sum of the average absorbances of all analytes
and potential interferants.
B.2 Calculation*
B.2.1 Prepare spectral representations of each analyte at
the concentration CLt = (DLi) (AUt) , where DLj is the required
detection limit and AUt is the maximum permissible analytical
uncertainty. For the mth analytical region, calculate the band
area (AAIi(J and average absorbance (AAVlm) from these scaled
analyte spectra.
B.2.2 Prepare spectral representations of each potential
interferant at its expected concentration (CPOTj) . For the mch
analytical region, calculate the band area (IAIjra) and average
absorbance (IAVjlt) 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 AAIim 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
-------
matrix described in Figure B.2. Any analytical region where
AVTm >2.0 is unsuitable.
FIGURE B.I Presentation of Potential Interferant Calculations
Analytical Regions
1 .... M
Analyte Labels
Potential Interferant
Labels
AAIn . . . AAItM
IAIU . . . IAI1M
IAI
Jt
FIGtJRE B.2 Presentation of Known Interferant Calculations
Analytical Regions
1 .... M
Analyte Labels
1 AAIn .... AAI1M
Known Interferant
Labels
AAIn .... AAIIM
IAIU .... IAI1M
K IAIK1 .... IAI
Total Average
Absorbance AVTt AVT,
H
-------
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.
twAN ~ 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 the
total infrared power transmitted by the absorption cell
and transfer optics from the interferometer to the
detector.
C.2 Calculation*
C.2.1 Obtain the values of RMS^, t^, and TP from the
manufacturers of the equipment, or determine the noise level by
direct measurements with the completely constructed system
proposed in Section 4.
C.2. 2 Calculate the noise value of the system (RMSEST) as
follows:
RMSEST = RMS^ TP
(4)
t
MAN
-------
APPENDIX D
ESTIMATING MINIMUM CONCENTRATION MEASUREMENT
UNCERTAINTIES (MAU and MIU)
D.1 General
Estimate the minimum concentration measurement uncertainties
for the ic analyte (MAUJ and jch interferant (MIU,) based
h' >-*">•» J -ti»v.^i. a_<=j.ati\_ \l-liUj, _____ _
spectral data in the mc analytical region by comparing the
analyte band area in the analytical region (AAIU) 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.3 Calculations
D.2.1 For each analytical region, set RMS = RMS^ if
measured (Appendix G) , or set RMS = RMSEST if estimated (Appendix
C) .
D.2.2 For each analyte associated with the analytical
region, calculate
fFU. - FL.
D.2.3 If only the m analytical region is used to calculate
the concentration of the ich analyte, set MAUt = MAUim.
D.2.4 If a number of analytical regions are used to
calculate the concentration of the ieh analyte, set MAUt eoiaal to
the weighted mean of the appropriate MAULm 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
-------
MAU, = Wu MAU
where the weight Wilt is defined for each term in the sum as
(7)
P6
D.2.5 Repeat Sections D.2.1 through D.2.4 to calculate the
analogous values MIU^ for the interferants j = 1 to J. Replace
the value (AUi) (DLi) in the above equations with CPOTj/20;. replace
the value AAIiffl in the above equations with IAIjra.
-------
APPENDIX B
DETERMINING FRACTIONAL REPRODUCIBILITY 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 Calculations
E.2.1 The CTS spectra {Rl} consist of N spectra, denoted by
Su, i=l, N. Similarly, the CTS spectra {R2} consist of N
spectra, denoted by S2i, i=l, N. Each Ski is the spectrum of a
single compound, where i denotes the compound and k denotes
the set {Rk} of which Sxi is a member. Form the spectra S-,
according to S3i = S2i-Su for each i. Form the spectra S4
according to S4i = [S2i+Su]/2 for each i.
E.2.2 Each analytical region m is associated with a portion
of the CTS spectra S2i and Su, for a particular i, with lower and
upper wavenumber limits FFLm and FFUm, respectively.
E.2.3 For each m and the associated i, calculate the band
area of S4i in the wavenumber range FFUm to FFLm. Follow the
guidelines of Section B.I.2 for this band area calculation.
Denote the result by BAVm.
E.2.4 For each m and the associated i, calculate the RMSD
of S3i between the absorbance values and their mean in the
wavenumber range FFUm to FFLm. Denote the result by SRMSm.
E.2.5 For each analytical region m, calculate the quantity
FM, = SRMSm(FFUm-FFLJ/BAVm
E.2.6 If only the mch analytical region is used to calculate
the concentration of the ich analyte, set FRUt = FM,,.
E.2.7 If a number p^ of analytical regions are used to
calculate the concentration of the ich analyte, set FRUt equal to
the weighted mean of the appropriate FM,, values calculated above.
Mathematically, if the set of analytical regions employed is
{m1}, then
x (8)
*€{«')
FRU, = £ Wu FH
*€{«')
where the Wik are calculated as described in Appendix D.
-------
APPENDIX F
DETERMINING FRACTIONAL CALIBRATION UNCERTAINTIES (FCU)
F. 1 General
F.I.I The concentrations yielded by the computerized
analytical program applied to each single-compound reference
spectrum are defined as the indicated standard concentrations
(ISC's). The ISC values for a single compound spectrum should
ideally equal the accepted standard concentration (ASC) for one
analyte or interferant, and should ideally be zero for all other
compounds. Variations from these results are caused by errors in
the ASC values, variations from the Beer's law (or modified
Beer's law) model used to determine the concentrations, and noise
in the spectra. When the first two effects dominate, the
systematic nature of the errors is often apparent; take steps to
correct them. ' •
F.I.2 When the calibration error appears non-systematic,
apply the following method to estimate the fractional calibration
uncertainty (FCU) for each compound. The FCU is defined as the
mean fractional error between the ASC and the ISC for all
reference spectra with non-zero ASC for that compound. The FCU
for each compound shall be less than the required fractional
uncertainty specified in Section 4.1.
F.I.3 The computerized analytical programs shall also be
required to yield acceptably low concentrations for compounds
with ISC=0 when applied to the reference spectra. The limits
chosen in this Protocol are that the ISC of each reference
spectrum for each analyte or interferant shall not exceed that
compound's minimum measurement uncertainty (MAU or MIU).
F.2 Calculation*
F.2.1 Apply, each analytical program to each reference
spectrum. Prepare a similar table as that in Figure F.I to
present the ISC and ASC values for each analyte and interferant
in each reference spectrum. Maintain the order of reference file
names and compounds employed in preparing Figure F.I.
F.2.2 For all reference spectra in Figure F.I, verify that
the absolute value of the ISC's are less than the compound's MAU
(for analytes) or MIU (for interferants).
F.2.3 For each analyte reference spectrum, calculate the
quantity (ASC-ISC)/ASC. For each analyte, calculate the mean of
these values (the FCUi for the ich analyte) over all reference
spectra. Prepare a similar table as that in Figure F.2 to
present the FCUj and analytical uncertainty limit (AUt) for each
analyte.
-------
FIGURE F.I
Presentation of Accepted Standard Concentrations (ASC's)
and Indicated Standard Concentrations (ISC's)
y. %
Compound
Ntttt*
' -*•• " --
^ Reference %
:: SpectrjHB
FieNanne
,
ASC
(ppat)
, ISC(pfjro)
„
Ar^Byfi$$''' *' T^tfrTrCT-ftitfS
****» *«»•««•*«• •««»* *K* *«* 3^'***'*«* ***** *** •«* «*
FIGURE F.2
Presentation of Fractional Calibration Uncertainties (FCU's)
and Analytical Uncertainties (AU's)
Name
FCU
AH
-------
APPENDIX G
MEASURING NOISE LEVELS
Q.I General
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).
G.2 Calculations
G.2.1 Evacuate the absorption cell or fill it with UPC
grade nitrogen at approximately one atmosphere total pressure.
G.2.2 Record two single beam spectra of signal integration
period tss.
G.2.3 Form the double beam absorption spectrum.from these
two single beam spectra, and calculate the noise level RMSg,, in
the M analytical regions.
-------
APPENDIX H
DETERMINING SAMPLE ABSORPTION PATHLENGTH (Ls) AND
FRACTIONAL ANALYTICAL UNCERTAINTY (FAU)
H.1 General
Reference spectra recorded at absorption pathlength (LR) , gas
pressure (PR) , 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 L3 and LR, and Tg 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 LR, 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 ARi, i = 1, n. Form a similar one-
dimensional array Ag from the absorbance values in the spectral
set {R3}; the members of the array are Asi/ i = 1, n. Based on
the model A, = rA,, + I, determine the least-squares estimate of
r1, the value of r which minimizes the square error Ba.
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 AS
and AR as described in Section H.2.1, using values from {Rl} to
form A^, and values from {R4} to form Ag. Calculate the values
-------
NRMS.. =
*•
«
's; \ "R; v ER
(9)
and
IAAV =
(10)
The fractional analytical uncertainty is defined as
FAU =
NPMS,
IA
(11)
AV
-------
APPENDIX I
DETERMINING FRACTIONAL MODEL UNCERTAINTIES (FMU)
I . 1 General
To prepare analytical programs for FTIR analyses, the sample
constituents must first be assumed; the calculations in this
appendix, based upon a simulation of the sample spectrum, verify
the appropriateness of these assumptions. The simulated spectra
consist of the sum of single compound reference spectra scaled to
represent their contributions to the sample absorbance spectrum;
scaling factors are based on the indicated standard
concentrations (ISC) and measured (sample) analyte and
interferant concentrations, the sample and reference absorption
pathlengths, and the sample and reference gas pressures. No
band-shape correction for differences in the temperature of the
sample and reference spectra gases is made; such errors are
included in the FMU estimate. The actual and simulated sample
spectra are quantitatively compared to determine the fractional
model uncertainty; this comparison uses the reference spectra
band areas and residuals in the difference spectrum formed from
the actual and simulated sample spectra.
1.2 Calculat ions
1.2.1 For each analyte (with scaled concentration
select a reference spectrum SAt with indicated standard
concentration ISCi. Calculate the scaling factors
TR Ls Ps RSA.
RA = R s s - i (12)
1
and form the spectra SACi by scaling each SAt by the factor RAt .
1.2.2 For each interferant, select a reference spectrum SI
with indicated standard concentration ISCk. Calculate the
scaling factors
T_ L, Pg
* s s (13)
PR ISC,
and form the spectra SIC,, by scaling each SI,, by the- factor RIk.
1.2.3 For each analytical region, determine by visual
inspection which of the spectra SACt and SIC* exhibit absorbance
bands within the analytical region. Subtract each spectrum SACt
and SIC,, exhibiting absorbance from the sample spectrum 83 to
form the spectrum SUBS. To save analysis time and to avoid the
introduction of unwanted noise into the subtracted spectrum, it
is recommended that the calculation be made (I) only for those
-------
spectral data points within the analytical regions, and (2) for
each analytical region separately using the original spectrum Ss.
1.2.4 For each analytical region m, calculate the RMSD of
SUBS between the absorbance values and their mean in the region
FFUm to FFL,,. Denote the result by RMSSm.
1.2.5 For each analyte i, calculate the quantity
RMSS/FFU - FFLm)AUt DL(
FM = - ^ - ^ - ^ - i - L- M4)
m AAIiRSAi * '
for each analytical region associated with the analyte.
1.2.6 If only the meh analytical region is used to calculate
the concentration of the ich analyte., set
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
FMU, = £ Wu FM, ' (15)
fce(m')
where Wi)t is calculated as described in Appendix D.
-------
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 = MAXCFRUi, FCUt/ FAUL, FMUJ and OCUt
= MAX{RSAi*OFUi,
-------
APPENDIX K
SPECTRAL DE-RESOLUTION PROCEDURES
K.I General.
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.a 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) decoop ct«0305a.aif,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) coopoae 0305dre«,0305dre».aif ,1
"Compose" transforms truncated interferograms back to spectral
format.
(iii) I02SP 0305dre«.aif,0305drea.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.
-------
De-resolved interferograms should be transformed using the same
apodization and zero filling that will be used to collect sample
spectra. Choose the desired low and high frequencies, in cm"1.
Transform the background interferogram in the same way.
(iv) DVDR 0305dres.dsf,bkg0305a.dflf,0305dres.dlf
"DVDR" ratios the transformed sample spectrum against the
background.
(v) ABSB 0305dre0.dlf,0305dres.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 CTS0305a.aif,0305dre«.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 Grams™ Software Procedure - Grams™ is a software
package that displays and manipulates spectra from a variety of
instrument manufacturers. This procedure assumes familiarity
with basic functions of Grams™.
This procedure is specifically for using Grams to truncate
and transform reference interferograms that have been imported
into Grams from the KVB/Analect format. Table K-l shows data
files and parameter values that are used in the following
procedure.
The choice of all parameters in the ICOMPUTE.AB call of step
3 below should be fixed to the shown values, with the exception
of the "Apodization' parameter. This parameter should be set
(for both background and sample single beam conversions) to the
type of apodization function chosen for the de-resolved spectral
library.
-------
TABLE K-l. GRAMS DATA FILES AND DE-RESOLUTION PARAMETERS.
Desired Nominal Spectral
Resolution (cm'1)
0.25
0.50
1.0
2.0
Data File Name
Z00250.sav
ZOOSOO.sav
ZOlOOO.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 "Arithmetic/Calc* menu item input box, type the text
below. Perform the calculation by clicking on "OK* (once only),
and, when the calculation is complete, click the 'Continue*
button to proceed to step (iv). Note the comment in step (iii)
regarding the trace orientation.
Xflip:#•-*»(#0,»N)+50
(iv) Run ICOMPUTB.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
"N":)
First: N
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 "FILB,• which may be in a directory other than
"c:\mdgrams.")
setffp 7898.8805, 0 : loadspc "c:\mdgrams\ FILB" : #2«#s+#2
(vi) Use "Page Op* to activate file #2, and then use the
"File/Save As* menu item with an appropriate file name to save
the result.
-------
K.3 Verification of New Resolution
K.3.1 -Obtain iriterferograms 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- s .05 (16)
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.
^ &=The upper and lower limits (cm"1) , respectively, of the
FFLt analytical region.
=band area in the ich analytical region of the test CTS.
case-CTS
------- |