United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-99-033
September 1999
Air
FTIR AND METHOD 25A EMISSIONS TEST
E PA AT AN INTEGRATED IRON AND STEEL
MANUFACTURING PLANT
Indiana Harbor Works of LTV Steel
Company, Inc.
East Chicago, Indiana
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EMISSIONS TEST
AT AN INTEGRATED IRON AND STEEL MANUFACTURING PLANT
Indiana Harbor Works of LTV Steel Company, Inc.
East Chicago, Indiana
Prepared for
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Emission Measurement Center (MD-19)
Research Triangle Park, North Carolina 27711
Michael L. Ciolek
Work Assignment Manager
EPA Contract No. 68-D-98-027
Work Assignment 2-12
MRI Project No. 104951-1-012-04
September, 1999
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11
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PREFACE
This draft report was prepared by Midwest Research Institute (MRI) for the U. S.
Environmental Protection Agency (EPA) under EPA Contract No. 68-D-98-027, Work
Assignment No. 2-12. Mr. Michael Ciolek 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. 4-20 and a draft report was
submitted under EPA Contract No. 68-W6-0048, Work Assignment No. 2-08. Mr. Michael
Ciolek was the EPA WAM for the Emission Measurement Center (EMC) under Work
Assignment 4-20 and Mr. Michael Toney was the WAM under Work Assignment No. 2-08.
Mr. John Hosenfeld was the MRI WAL under Work Assignment 2-08 and Dr. Thomas Geyer
was the MRI task leader for Work Assignment 2-08, task 11.
This report presents the procedures, schedule, and test results for an emissions test
performed at LTV Steel Company in East Chicago, Indiana. The emissions test used Fourier
transform infrared (FTIR) sampling procedures to measure hazardous air pollutants (HAP's) and
other pollutants and Method 25A to measure hydrocarbon species.
This report consists of one volume (416 pages) with seven sections and four appendices.
Midwest Research Institute
g John Hosenfeld
Program Manager
Approved:
Jeff Shular
Director, Environmental Engineering Department
September 30,1999
111
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IV
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TABLE OF CONTENTS
1.0 INTRODUCTION M
1.1 BACKGROUND 1-1
1.2 PROJECT SUMMARY 1-1
1.3 PROJECT PERSONNEL 1.3
2.0 LTV STEEL'S SINTER PLANT 2-1
2.1 OVERVIEW 2-1
2.2 PROCESS DESCRIPTION 2-1
2.3 EMISSION CONTROL EQUIPMENT 2-5
2.4 MONITORING RESULTS DURING THE TESTS 2-6
2.5 ANALYSIS OF MONITORING AND TEST RESULTS 2-8
3.0 TEST LOCATIONS .'..' 3-1
3.1 KINPACTOR SCRUBBER OUTLET - STACK 3-1
3.2 KINPACTOR SCRUBBER INLET - DUCT 3-1
3.3 VOLUMETRIC FLOW 3-1
4.0 RESULTS 4-1
4.1 TEST SCHEDULE 4-1
4.2 FIELD TEST PROBLEMS AND CHANGES 4-1
4.3 METHOD 25A RESULTS 4-2
4.4 FTIR RESULTS 4-3
4.5 ANALYTE SPIKE RESULTS 4-4
4.6 SCREENING RESULTS 4-8
5.0 TEST PROCEDURES 5-1
5.1 SAMPLING SYSTEM DESCRIPTION 5-1
5.2 SAMPLING PROCEDURES 5-3
5.3 FTIR SAMPLING PROCEDURES 5-3
5.3.1 Batch Samples 5-3
5.3.2 Continuous Sampling 5-3
5.4 ANALYTE SPIKING 5-4
5.4.1 Analyte Spiking Procedures 5-4
5.4.2 Analysis of Spiked Results 5-5
5.5 ANALYTICAL PROCEDURES 5-5
5.5.1 Computer Program Input 5-7
5.5.2 EPA Reference Spectra 5-7
5.6 FTTR SYSTEM 5-7
5.7 CONTINUOUS EMISSIONS MONITORING FOR THC 5-9
5.7.1 THC Sampling Procedures 5-9
5.7.2 Hydrocarbon Emission Calculations 5-10
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TABLE OF CONTENTS (CONTINUED)
Page
6.0 SUMMARY OF QA/QC PROCEDURES 6-1
6.1 SAMPLING AND TEST CONDITIONS 6-1
6.2 FTIR SPECTRA 6-2
6.3 METHOD 25A 6-3
6.3.1 Initial Checks 6-3
6.3.2 Daily Checks 6-3
7.0 REFERENCES 7-1
APPENDIX A - METHOD 25A AND VOLUMETRIC FLOW DATA A-l
A-l METHOD 25A RESULTS A-2
A-2 METHOD 25A CALIBRATION AND QA CHECK DATA A-3
A-3 VOLUMETRIC FLOW DATA A-4
APPENDIX B - FTIR DATA B-l
B-l FTIR FIELD DATA RECORDS B-2
B-2 FTIR FLOW AND TEMPERATURE READINGS B-29
B-3 FTIR RESULTS B-37
B-4 HYDROCARBON REFERENCE SPECTRA B-75
APPENDIX C - EQUIPMENT CALIBRATION CERTIFICATES C-l
C-l CALIBRATION GAS CERTIFICATES C-2
C-2 ENVIRONICS MASS FLOW METER CALIBRATIONS C-3
APPENDIX D - TEST METHODS AND HC1 VALIDATION PAPER D-l
D-l EPA METHOD 320 D-2
D-2 EPA FTIR PROTOCOL D-3
D-3 EPA METHOD 25A D-4
D-4 EPA DRAFT METHOD 205 D-5
D-5 HC1 VALIDATION PAPER D-6
VI
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TABLE OF CONTENTS (CONTINUED)
LIST OF FIGURES
Figure 2-1. Schematic of material flow in the sinter plant 2-3
Figure 3-1. Test locations 3-2
Figure 4-1.. Example residual spectra 4-11
Figure 5-1. Extractive sampling system 5-2
LIST OF TABLES
'age
TABLE 1-1. SUMMARY OF FTIR RESULTS 1-4
TABLE 1-2. SUMMARY OF HYDROCARBON EMISSIONS RESULTS 1-5
TABLE 1-3. PROJECT PERSONNEL 1-6
TABLE 2-1. SUMMARY OF SINTER MIX (FEED) COMPONENTS 2-2
TABLE 2-2. SUMMARY OF SINTER COMPOSITION 2-5
TABLE 2-3. TYPICAL SCRUBBER PARAMETERS 2-6
TABLE 2-4. PROCESS PARAMETER VALUES DURING THE TESTS 2-7
TABLE 2-5. CONTROL DEVICE OPERATING PARAMETERS DURING THE TESTS . 2-8
TABLE2-6. SUMMARY OF RESULTS FOR EACH TEST RUN ...2-9
TABLE 2-7 SUMMARY OF RESULTS FOR PM AND HAP METALS 2-12
TABLE 2-8 SUMMARY OF RESULTS FOR PAHS 2-13
TABLE 2-9. SUMMARY OF RESULTS FOR DIOXINS AND FURANS 2-14
TABLE 3-1. SOURCE GAS COMPOSITION AND FLOW SUMMARY 3-3
TABLE 4-1. TEST SCHEDULE AT LTV STEEL COMPANY INDIANA
HARBOR WORKS 4-1
TABLE 4-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS 4-3
TABLE 4-3. SUMMARY OF SPIKE RESULTS 4-5
TABLE 4-4. COMPARISON OF EPA TOLUENE REFERENCE SPECTRA
TO SPECTRA OF TOLUENE CYLINDER STANDARD3 4-7
TABLE 4-5. SUMMARY OF ESTIMATED UNCERTAINTIES FOR UNDETECTED
TARGET ANALYTES AT LTV STEEL 4-9
TABLE 4-6. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA 4-10
TABLE 5-1. PROGRAM INPUT FOR ANALYSIS AND CTS SPECTRA AND PATH
LENGTH DETERMINATION (CTSLTV.MCP) 5-8
TABLE 5-2. RESULTS OF PATH LENGTH DETERMINATION 5-8
VII
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1.0 INTRODUCTION
1.1 BACKGROUND
The Emission Measurement Center (EMC) of the U. S. EPA directed MRI to conduct
emissions testing at iron and steel manufacturing facilities, specifically on sintering processes.
The test request for this industry was initiated from the Metals Group of the Emission Standards
Division (ESD) and Source Characterization Group of the Emission Monitoring and Analysis
Division (EMAD), both in the Office of Air Quality Planning and Standards (OAQPS). The test
program was performed in June, 1997 under Work assignment No. 4-20, under EPA Contract
No. 68-D2-0165. This draft report was prepared under Work Assignment No. 2-08, under
Contract 68-W6-0048.
Initially, the project included two field tests: (1) a screening test with FTIR Method 320
to evaluate the data for detected HAP's, and (2) a separate MIR emissions test at the same site
after additional preparation based on the screening results. The emissions test was to include
performance of the Method 301 spiking procedure with method validation for any detected
HAP's. Immediately prior to the test EPA altered the Scope of Work for this project to include
only one test for HAP screening and emissions measurements. No validation testing was
performed.
The testing was performed on the sintering process at the Indiana Harbor Works of LTV
Steel Company, Inc., in East Chicago, Indiana using EPA Draft FTIR Method 3201 and EPA
Method 25A. Method 320 is an extractive test method based on FTIR spectroscopy, which uses
quantitative analytical procedures described in the EPA FTIR Protocol. Data will be used to
quantify and characterize HAP emissions and the performance of the control unit for MACT
standard development for this industry.
1.2 PROJECT SUMMARY
The sintering process is used to agglomerate fine raw materials into a product suitable for
charging into a blast furnace. It is a potentially significant source of HAP emissions, including
both metal and organic compounds. The principal emission point at a sinter plant is the exhaust
from the sintering machine windboxes. Emission controls for the Indiana Harbor Works Sinter
Plant include an American Air Filter designed, double throat Kinpactor scrubber for the windbox
emissions and a Zurn designed venturi scrubber for sinter breaker emissions. Testing was
1-1
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conducted at the stack (outlet) and an inlet location to the Kinpactor scrubber for windbox
emissions to determine the measurable emissions released during the sintering process.
Three test runs were conducted by MRI at each location over a 3 day period concurrently
with manual method testing conducted by Eastern Research Group, Inc. (ERG). The FTIR
samples were collected by alternating sampling between the Kinpactor scrubber inlet and stack,
while the Method 25A testing was continuous at both locations. A summary of the FTIR and
total hydrocarbon (THC) results is presented in Tables 1-1 and 1-2, respectively. The FTIR
screening results for target analytes and other HAP's, which were not detected, is presented in
Table 4-5.
In the draft report submitted i: : 998, some of the heavier hydrocarbon emissions were
represented by hexane in the FTIR re cs. Since the draft report was submitted, MRI has
measured laboratory reference spectra of additional non-HAP hydrocarbon compounds.
Including the new spectra in the revised analysis improved the toluene and hexane
measurements. Four new compounds were detected: n-heptane, 1-pentene, 2-methyl-2-butene,
and n-pentane. As a result, hexane was not detected and the inlet toluene concentrations are
slightly lower compared to the draft report results. Documentation of the new reference spectra
is provided in Appendix B.
The EPA Method 320 uses an extractive sampling procedure. A probe, pump, and heated
line are used to transport sample from the test port to a gas manifold in a trailer that contains the
FTIR equipment. Infrared spectra of a series of samples are recorded. Quantitative analysis of
the spectra was performed after the FTIR data collection was completed. All spectral data and
results were saved on computer media. A compact disk containing all FTIR data is provided
with this report.
The EPA Method 25A also uses an extractive sampling procedure. The same sample
transport system was used for both the FTIR and THC testing. Volume concentration data and
results obtained from the samples were recorded and saved on computer media and reviewed
after the test was completed.
1-2
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1.3 PROJECT PERSONNEL
The EPA test program was administered by EMC. The Test Request was initiated by the
Metals Group of the ESD and the Source Characterization Group of the EMAD, both in OAQPS.
Some key project personnel are listed in Table 1-3.
1-3
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TABLE 1-1. SUMMARY OF FTIR RESULTS
Compound
Toluene ppm
Ib/hr
rlexane ppm
Ib/hr
Ethylene ppm
Ib/hr
VIethane ppm
Ib/hr
Sulfur Dioxide ppm
Ib/hr
Carbon Monoxide ppm
Ib/hr
Ammonia ppm
Ib/hr
Formaldehyde ppm
Ib/hr
n-Heptane ppm
Ib/hr
1 -Pentene ppm
Ib/hr
2-Methyl-2-Butene ppm
Ib/hr
n-Pentane ppm
Ib/hr
Scrubber Inlet
Run 1
6/25/97
4.25
16.19
ND
3.96
4.60
18.1
12.0
93.6
247.9
828
959
4.58
3.22
6.03
7.49
2.92
12.12
6.55
19.01
0.06
0.17
ND
Run 2
6/26/97
5.75
21.34
ND
4.76
5.37
20.1
12.9
79.0
203.7
847
955
8.21 .
5.63
4.27
5.16
3.86
15.57
4.72
13.32
0.14
0.40
ND
Run 3
6/27/97
0.17
0.66
ND
3.40
4.08
16.2
11. 1
83.3
227.7
848
1014
7.27
5.29
3.02
3.88
4.37
18.70
2.01
6.02
1.53
4.65
ND
Scrubber Outlet (Stack)
Run 1
6/25/97
1.72
7.41
ND
4.43
5.80
15.8
11.8
24.8
74.1
807
1056
0.44
0.35
7.26
10.19
0.46
2.16
11.21
36.72
ND
0.27
0.92
Run 2
6/26/97
1.67
7.21
ND
6.13
8.03
17.7
13.3
11.8
35.3
815
1066
2.08
1.66
2.85
4.01
2.20
10.28
6.59
21.60
ND
ND
Run 3
6/27/97
0.09
0.37
ND
6.00
7.79
13.9
10.3
10.0
29.6
854
1106
1.70
1.34
2.27
3.15
1.79
8.30
6.26
20.31
ND
ND
1-4
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TABLE 1-2. SUMMARY OF HYDROCARBON EMISSIONS RESULTS
Test data
Run No.
Date
Time
Scrubber inlet
Gaseous concentrations (carbon equiv.)
THC concentration, ppm (wet basis)
Methane concentration, ppm (wet
basis)
Emissions data (carbon equiv.)
THC emission rate, Ib/hr
Total gaseous nonmethane organic
carbon emission rate, Ib/hr
Scrubber outlet (stack)
Gaseous concentrations (carbon equiv.)
THC concentration, ppm (wet basis)
Methane concentration, ppm (wet
basis)
Emissions data (carbon equiv.)
THC emission rate, Ib/hr
Total gaseous nonmethane organic
carbon emission rate, Ib/hr
1
25-Jun-97
0927-1701
120.6
18.5
59.9
50.6
80.7
16.3
45.2
36.1
2
26-Jun-97
0953-1536
111.9
20.4
54.7
44.2
81.0
18.0
45.4
35.3
3
27-Jun-97
0835-1346
89.4
16.5
45.8
37.4
73.8
14.1
41.0
33.2
Average
107.3
18.5
53.3
44.1
78.5
16.1
43.9
34.9
1-5
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TABLE 1-3. PROJECT PERSONNEL
Organization and title
LTV Steel Company, Inc.
Indiana Harbor Works
Area Manager, Environmental Services
LTV Steel Company, Inc.
Indiana Harbor Works
General Supervisor, Sinter Plant & Ore Dock
U.S. EPA, EMC
Work Assignment Manager
Work Assignment 4-20
U. S. EPA, EMC
Work Assignment Manager
Work Assignment 2-08 •
MRI
Work Assignment Leader
Work Assignment 4-20
MRI
Work Assignment Leader
Work Assignment 2-08
Name
Michael J. Thomas
Claude Harris, Jr.
Michael K. Ciolek
Michael L. Toney
Thomas J. Geyer
John Hosenfeld
Phone No.
(219)391-2840
(219)391-3765
(919) 541-4921
(919)541-5247
(919)851-8181
Ext. 3120
(816)753-7600
Ext. 1336
1-6
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2.0 LTV STEEL'S SINTER PLANT
The material in Section 2 was prepared by Eastern Research Group (ERG) and provided
to MRI by EMC. It is included in the report without MRI review.
2.1 OVERVIEW
The primary purpose of the sinter plant is to recover the iron value from waste materials
generated at iron and steel plants by converting the materials to a product that can be used in the
blast furnace (as burden material). Many of these wastes have little or no value otherwise and
would require disposal if they could not be recycled by this process. A secondary purpose of the
sinter plant is to incorporate blast furnace flux into the sinter rather than charging it separately
into the furnace. Limestone wastes are converted to lime on the sinter grate, and the lime is used
as a fluxing agent in the blast furnace. The raw material feed (sinter mix) consists of iron ore
fines, chips from iron ore pellets, fine limestone, slag from the steelmaking furnace, scale from
the steel rolling mill, residue from air and water pollution control equipment (blast furnace flue
dust and filter cake), coke breeze (undersize coke that cannot be used in the blast furnace), and
steel reverts.
There are currently nine sinter plants in operation in the U.S. A total of five of these
plants use scrubbers to control emissions from the sinter plant windbox, and four use a baghouse.
The sinter plant at LTV Steel in East Chicago, IN, was chosen for testing to evaluate hazardous
air pollutants and emission control performance associated with sinter plants that use scrubbers.
2.2 PROCESS DESCRIPTION
LTV Steel's sinter plant at their Indiana Harbor Works was constructed in 1959 and is a
part of the integrated iron and steel plant that also includes blast furnaces, basic oxygen furnaces
(BOFs), ladle metallurgy, continuous casting, rolling mills, and galvanizing lines. The sinter
plant has a maximum rated capacity of 5,280 tons per day (tpd) and operates 24 hours per day,
7 days a week. Typically, the plant produces 3,800 tpd and operates 24 hours per day for about
310 days per year. The sinter machine is 8 feet (ft) wide and 168 ft long. The major processing
steps in the sinter plant include preparation of the sinter mix (feed material), sintering, discharge
end operations (crushing and screening), and cooling of the sinter product. Figure 2-1 is a
simplified schematic of the sintering process.
2-1
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The typical feed composition of the sinter mix during the emission tests is shown in
Table 2-1.
TABLE 2-1. SUMMARY OF SINTER MIX (FEED) COMPONENTS
Feed material
Pellet chips (ore)
Mill scale
Limestone
Flue dust
Coke breeze
BOF slag
Fines
NMT blend
Filter cake
Percent of total for the day
Test 1 (6/25/97)
41.1
13.2
16.6
2.7
0.8
9.1
7.4
3.8
5.3
Test 2 (6/26/97)
40.9
14.3
15.9
3.0
0.8
9.1
8.2
3.2
4.6
Test 3 (6/27/97)
41.3
14.4
15.8
3.0
0.9
8.9
7.6
4.2
3.9
The raw materials are fed from 10 storage bins by a table feeder onto a moving belt. This
raw feed is mixed in a pug mill, where water is added to create the desired consistency in the
mix. A "hearth layer" of material, which is undersize sinter material that is recycled from the
screening operation, is first deposited on the grate bars of the sinter pallets, and then the feed mix
is added to a depth of about 14 inches (in.).
The sinter feed passes through an ignition furnace that is 12 ft long. The furnace has
nine side burners fueled by natural gas that ignite the surface of the sinter feed. The sinter pallets
move continually through the ignition furnace at about 90 to 100 in. per minute (min) over
21 vacuum chambers called "windboxes."
2-2
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Clean BF recycle water
UJ
Service water
Clean BF
recycle
water
Breaker end
Venturi
scrubber
Raw materials
(pellet chips, mill scale,
coke breeze, flue dust
BOF slag, filter cake, water
limestone)
Sinter to blast
furnace or
storage
Figure 2-1. Schematic of material flow in the sinter plant.
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A vacuum is created in the windbox by a 3,000 horsepower (hp) fan that draws heat through the
sinter bed and creates the fused "sintered" product.
The red hot sinter from the furnace continues to be transported on the pallets to the
breaker, where it is crushed, screened, and discharged to a rotary cooler. Three fans are used to
create a forced draft to cool the hot sinter product. In addition, water sprays are used to cool the
sinter and to suppress surface dust. The sinter is removed from the bottom of the cooler with a
plow that deposits the cooled material onto a conveyor belt. The sinter is then conveyed over a
double-deck screen and subsequently deposited into a storage bin. An ore car is used to transport
the finished product to the blast furnace. Sinter material that passes through the screens ("fines")
is returned to the sinter process for use as the hearth layer or for addition to the sinter mix.
Several operating parameters are monitored and controlled to ensure proper operation of
the sinter machine. These parameters include the feed rate of each of the ten feed bins, the sinter
furnace temperature, the temperature profile through the various windboxes, draft on the
windboxes, speed of the grate, and percent water in the feed. The oil in the sinter feed, which
comes primarily from rolling mill scale, is limited to 0.2 percent. During the testing, the coke
feed rate appeared to be the parameter that was most often adjusted in order to control
temperatures. To maintain the proper chemistry in the blast furnace, an important quality control
parameter that is monitored and graphed on a control chart is the percent excess base:
(%CaO+%MgO) - (%SiO2 + %A12O3)
The sinter composition for the 3 tests days is summarized in Table 2-2 and shows that the percent
excess base ranged from 13.6 to 13.7 compared to a target of 14.0.
2-4
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TABLE 2-2. SUMMARY OF SINTER COMPOSITION
Component
Fe
Si02
A1203
CaO
MgO
Excess base
Percent of total
Test 1 (6/25/97)
52.8
4.5
0.59
16.7
2.0
13.6
Test 2 (6/26/97)
52.7
4.6
0.65
16.8
2.1
13.7
Test 3 (6/27/97)
52.9
4.4
0.66
16.6
2.1
13.6
2.3 EMISSION CONTROL EQUIPMENT
Emissions are generated in the process as sinter dust and combustion products and are
discharged through the grates and windboxes to a common collector main. Coarse dust particles
settle out of the air stream in the collector main and are discharged through flapper valves to a
conveyor belt. This conveyor also receives the returns from a series of hoppers that collect any
particles that fall under the sinter machine. This material is returned by conveyor to the sinter
mix feed for recycle to the process. The exhaust then passes through a battery of cyclones and a
series of chambers (originally designed for an electrostatic precipitator that is no longer used).
The cyclones and chambers remove dust particles, which are also deposited onto a conveyor
(through air actuated valves) for recycle to the process. The exhaust is moved by a 6,000 hp fan
to the primary control device, which is a double-throat Kinpactor scrubber designed by American
Air Filter. The parameters associated with the scrubber that are monitored include the pressure
drop across the scrubber, flow rate of water to the scrubber, exhaust fan draft and amperage, and
the scrubber water blowdown rate.
Typical operating conditions associated with the scrubber are summarized in Table 2-3.
2-5
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TABLE 2-3. TYPICAL SCRUBBER PARAMETERS
Parameter
Liquid/gas ratio
Water flow rate
Gas flow rate
Pressure drop
pH of scrubber water
Inlet temperature
Outlet temperature
Slowdown rate
Typical value
14gal/l,000acfm
3,100gal/min
265,000 scfm
38 to 46 in. of water
8
235°to270°F
120°F
240 gal/min
A scrubber is also used to control emissions from the discharge end (i.e., breaker,
screens). The discharge end scrubber was not evaluated as part of this test program.
Current State regulations limit particulate matter to 0.02 gr/dscf and 20 percent opacity
(6-min average) for both scrubbers. In addition, the windbox scrubber is limited to a mass rate of
49.7 pounds per hour (Ib/hr) and the discharge end scrubber is limited to 18.05 Ib/hr.
2.4 MONITORING RESULTS DURING THE TESTS
The operating parameters associated with the process and control device were recorded at
15-minute intervals throughout each test day. The process parameters that were monitored
included the feed rate from each of the 10 bins that were used in the sinter mix, the temperatures
and the fan draft for the windboxes, percent water in the feed, sinter machine speed, and the
sinter production rate. The emission control device parameters that were monitored included the
pressure drop across the scrubber, the water flow rate, blowdown rate, fan draft, and fan amps.
Tables 2-4 and 2-5 present a summary of the range of values for these parameters for each test
period.
The process and control device appeared to be stable throughout the 3 test days;
consequently, sampling was conducted under normal and representative conditions. The feed
rates of mill scale and other materials were typical of the historical rates in recent years that had
been reported by the plant. In addition, the oil content of the mill scale was typical (target is
0.2 percent, maximum) with an average of 0.21 percent oil (a range of 0.17 to 0.24 percent)
2-6
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TABLE 2-4. PROCESS PARAMETER VALUES DURING THE TESTS
Parameter
Test 1 (6/25/97)
Test 2 (6/26/97)
Test 3 (6/27/97)
Feed rate (tph):
Mill scale
BOF slag/filter cake
Fines
Pellet chips
Pellet fines-- blend
Limestone
Cold fines
Coke breeze
Flue dust
BOF slag fines
25.2(24.8-25.5)
16.7(16.1- 17.9)
16.7(16.1 - 17.6)
77.4(75.9-78.8)
9.5 (8.5 - 10.2)
27.2 (26.9 - 27.7)
19.6(17.6-21.4)
1.7(1.5- 1.9)
5.9(5.8-6.0)
7.9(7.6-8.2)
25.2 (24.9 - 25.5)
16.9(15.9-18.2)
16.4(15.9- 18.0)
77.7 (76.2 - 79.0)
10.7(10.1- 11.4)
27.5 (26.8 - 27.8)
17.2(15.2- 19.5)
1.2(0.9- 1.5)
5.9(5.8-6.0)
9.3(9.4- 10.1)
25.2(24.8-25.6)
16.9(15.5- 17.9)
16.7(15.3-18.0)
77.6 (76.5 - 79.5)
12.3(11.3-13.6)
27.7 (27.4 - 28.8)
17.8(16.8-23.2)
0.7(0.34- 1.1)
5.9(5.8-6.0)
10.0(9.8-10.1)
Other parameters:
Percent water
Grate speed
Windbox 20 temperature (°F)
Windbox draft (in. water)
Feed rate (tph)
Sinter production (tph)
6.7 - 7.5
70-76
453 - 656
13.6- 17.4
205-210
155-158
6.5 - 7.4
70-76
474 - 659
13.3- 18.2
201-212
153-161
7.2 - 8.2
70 - 82
334-571
14.2- 18.2
209 - 213
159-161
2-7
-------
TABLE 2-5. CONTROL DEVICE OPERATING PARAMETERS DURING THE TESTS
Parameter
Pressure drop (in. water)
Water flow (gal/min)
Blowdown (gal/min)
Fan amps
Fan draft (in. water)
Type of water
Test 1 (6/25/97)
38.4-46.6
3.040 - 3,085
236 - 239
663-695
3.1-5.8
service (lake)
Test 2 (6/26/97)
39.4 - 46.3
3,080-3.130
242 - 246
685 - 700
3.2-5.8
Test 3 (6/27/97)
39.8-47.0
3,080-3,110
241-244
700 - 730
3.8-5.1
recycled blast furnace
based on the analysis of 5 samples. An examination of the monitoring data showed that the
average pressure drop across the scrubber was 43.1, 42.8, and 42.4 in. of water for the 3 test days.
The coke rate seemed to be the most variable parameter during the tests because adjustments
were made frequently to change the sintering temperature. The coke rate for the 3 tests averaged
1.7, 1.15, and 0.67 tph; consequently, the emission test results may provide some insight into the
effect of coke rate on emissions. The windbox temperatures also varied somewhat during the
tests. Using Windbox 20 as an example, the average temperatures during the 3 tests were 538°,
567°, and 443 °F.
2.5 ANALYSIS OF MONITORING AND TEST RESULTS
Table 2-6 summarizes the emission results for each run along with selected parameters
that were monitored during the test. Only a few comparisons can be made because the process
operated stably and consistently during the 3 test runs. One difference is that the coke (fuel) rate
during Run 3 was only 39 percent of the rate during Run 1 and only 58 percent of the rate during
Run 2. The lower fuel rate during Run 3 is reflected in the lower windbox temperature during
Run 3, which was about 100°F lower than in the previous 2 runs. The pollutants most likely to
be affected by the change in combustion conditions are dioxins, furans, and PAHs. During
Run 3, the emission rates for all of these compounds were lower than in the previous 2 runs.
The highest emissions of paniculate matter and lead occurred during Run 3. The cause is
not conclusive, but some of the possible factors affecting this, perhaps in combination, were that
Run 3 had the highest sinter feed and production rate and the lowest average pressure drop across
the scrubber. In addition, Table 2-4 indicates that Run 3 had a higher feed rate of fines (pellet
fines and EOF slag fines) than that recorded during the previous 2 runs. Service water was used
2-8
-------
TABLE 2-6. SUMMARY OF RESULTS FOR EACH TEST RUN
Parameter
PMa - inlet
PM - outlet
PM efficiency
Lead - inlet
Lead - outlet
Lead efficiency
HAP metals - in
HAP metals - out
Metals efficiency
D/F congeners
D/FTEQC
Total D/F41
7PAHse
16PAHs
TOTAL PAHs
Sinter feed
Sinter production
Scrubber A p
Windbox 20 temperature
Coke feed
Units
Ib/hr
Ib/hr
percent
Ib/hr
Ib/hr
percent
Ib/hr
Ib/hr
percent
Mg/hr
Mg/hr
Mg/hr
g/hr
g/hr
g/hr
tons/hr
tons/hr
in. water
oF
tons/hr
Runl
419
34
92
4.1
3.7
9.8
4.5
3.8
16
810
93
5,650
1.9
69
83
208
156
43.1
538
1.7
Run 2
479
38
92
4.0
3.6
10
4.5
3.7
18
768
91
5,380
2.0
78
92
208
159
42.8
567
1.2
Run 3
550
43
92
4.4
3.8
14
4.9
. 3.9
20
694
79
4,820
1.4
61
73
211
160
42.4
443
0.7
Average
483
38
92
4.2
3.7
12
4.6
3.8
17
757
88
5,280
1.7
69
83
209
158
42.8
516
1.2
a PM = paniculate matter
_)/F congeners are those dioxins and furans that have a toxicity equivalent factor relative to 2,3,7,8-TCDD.
c D/F TEQ is the toxicity equivalent expressed relative to 2,3,7,8-TCDD.
Total D/F are all dioxins and furans that were reported.
e PAH = polycyclic aromatic hydrocarbons.
in the scrubber during Run 1 and recycled blast furnace water was used during Runs 2 and 3.
There is no obvious difference in emissions that can be clearly attributed to the type of scrubber
water.
The major metal HAP that was found was lead, which accounted for over 97 percent of
the total metal HAP emissions. Discussions with the plant and examination of data from the
analysis of blast furnace fines and sludge indicated that a likely source of the lead emissions was
2-9
-------
from this fine material recycled from the blast furnace. Data in the literature showed that the lead
content of blast furnace dust and sludge was generally in the range of 0.01 to 0.1 percent. At a
typical feed rate for the dust and sludge of 28,000 Ib/hr (14 tons per hour [tph]), these materials
would introduce 2.8 to 28 Ib/hr of lead into the process, which could easily account for the lead
that was found entering the scrubber (4.2 Ib/hr). In addition, the small particle size of these
pollution control residues from the blast furnace may increase the probability that they become
airborne, and the volatility of lead and some lead compounds from combustion processes may
tend to increase the concentration of lead in the windbox emissions.
Another interesting result is the very low emission rate of dioxins, relative to what had
been reported from testing at German sinter plants. For example, the German study reported
concentrations of 23 to 68 ng TEQ/m from their initial studies and a range of 5 to 10 ng
TEQ/m for plants that optimized and improved their operation. The results for this sinter plant
was much lower with an average concentration of 0.19 ng TEQ/m . On the basis of sinter
production, the Germans reported emission levels in the range of 10 to 100 /ug/Mg of sinter
compared to a measured level of 0.6 yug/Mg of sinter for this plant. The LTV sinter plant had
emissions of dioxins and furans that were on the order of 10 to 100 times less than that reported
for German sinter plants.
The dioxin results are not unexpected because there are basic differences between the
operation of LTV's sinter plant and the German plants. The German study attributed the
formation of dioxin to the presence of chlorinated organics, primarily in cutting oils, that were in
the waste materials fed to the sintering process. In addition, they stated that the use of
electrostatic precipitators contributed to recombination and formation of dioxin. In contrast, the
LTV plant has eliminated the purchase and use of chlorinated organics in their facility as part of a
voluntary program of pollution prevention, and any new chemical purchases must be approved by
the environmental department. Their rolling mill oils (lubricants and hydraulic fluids) do not
contain chlorinated compounds. In addition, routine analysis of waste materials going to the
sinter plant have not detected chlorinated solvent. Finally, the LTV plant does not use an
electrostatic precipitator. Consequently, dioxin rates at LTV that are much lower than those
reported by German sinter plants appear to be reasonable and explainable.
2-10
-------
Table 2-7 through 2-9 presents a summary of the annual emissions and the emission
factors derived from this test.
2-11
-------
TABLE 2-7 SUMMARY OF RESULTS FOR PM AND HAP METALS
Pollutant
Paniculate
matter
Ml
Pollutant:
HAP metals
Mercury
Arsenic
Beryllium
Cadmium
Cobalt
Chromium
Manganese
Nickel
Lead
Antimony
Selenium
Total HAP
metals
Concentration (gr/dscf)
Inlet
0.23
^m
Concentrator
Inlet
0.96
4.3
0.054
20
0.30
24
400
23
4,500
2.6
13
5,000
Outlet
0.017
••
i (Aig/DSCM)
Outlet
1.5
1.1
0.052
17
0.050
5.2
17
22
3,700
1.6
8.7
3,800
Emission rate (Ib/hr)
Inlet
483
^m
Emission
Inlet
0.41
1.8
0.023
8.4
0.18
9.9
171
9.8
1,900
1.1
5.5
2,100
Outlet
38
••
rate (g/hr)
Outlet
0.69
0.50
0.023
7.8
0.023
2.4
7.9
9.9
1,690
0.75
4.0
1,700
Efficiency
(%)
92
••
Efficiency
(%)
0
. 73
0
7.4
87
76
95
0
11
32
28
18
Annual rate (tpy)a
Inlet
1,800
••
Annual
Inlet
3.3 x 10'3
1.5x 10'2
1.9x 10'4
6.9 x 10'2
1.5x 10'3
8.1 x 10"2
1.4
8.0 x 10'2
16
9.0 x 10'3
4.5 x 10"2
17
Outlet
142
^m
rate (tpy)
Outlet
5.7 x ID'3
4.1 x 10~3
1.9x 10'4
6.4 x 10'2
1.9x 1Q-4
I.9x 10"2
6.4 x 10'2
8.1 x 10'2
1.4 x 10+1
6.1 x 10'3
3.2 x 10'2
1.4 x 10+l
Emission factor (Ib/t sinter)
Inlet
3.1
••i
Emission factor
Inlet
5.7 x 10"6
2.5 x 10'5
3.2 x 10'7
1.2x 10'4
2.5 x 10'6
1.4x 10'4
2.4 x 10'3
1.4 x 10-4
2.7 x 10'2
l.5x 10'5
7.7 x 10'5
2.9 x 10"2
Outlet
0.24
••
(Ib/t sinter)
Outlet
9.7 x 10'6
7.0 x 10'6
3.3 x 1Q-7
1.1 x,10'4
3.3 x 10'7
3.3x 1Q-5
I.I x IQ-4
1.4 x 10"4
2.4 x IO"2
1. Ox 10'5
5.5 x IO'5
2.4 x 10'2
a Based on operation for 24 hours per day for 310 days per year.
-------
TABLE 2-8 SUMMARY OF RESULTS FOR PAHS
Pollutant: PAHs3
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-cd)pyrene
Dibenzo(a,h)anthracene
Total 7 PAHs
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(g.h,l)perylene
Total 16 PAHs
2-Methylnaphthalene
2-Chloronaphthalene
Benzo(e)pyrene
Perylene
Total - all PAHs
Concentration
(Mg/DSCM)
0.53
1.3
1.2
0.22
0.23
0.26
0.097
3.9
78
7.6
3.5
5.4
43
1.8
6.9
3.0
0.36
153
29
0.039
0.76
0.058
183
Emission rate
(g/hr)
0.24
0.60
0.54
0.10
0.11
0.12
0.044
1.7
35
3.4
1.6
2.4
19
0.81
3.1
1.4
0.16
69
13
0.018
0.30
0.026
83
Annual emissions
tpy
0.0019
0.0049
0.0044
0.00082
0.00086
0.00096
0.00036
0.014
0.29
0.028
0.013
0.020
0.16
0.0067
0.026
0.011
0.0013
0.57
0.11
0.00015
0.0028
0.00022
0.68
Ib/ton sinter
3.3 x 10' 6
8.4 x 10'6
7.5 x 10'6
1.4x 10'6
1.5x 10'6
1.6x 10'6
6.1 x 10'7
2.4 x 10'5
4.9 x, 10"4
4.8 x 10'5
2.2 x 10'5
3.4 x 10'5
2.7 x 10"4
1.1 x 10'5
4.3 x 10'5
1.9x 10'5
2.2 x 10'6
9.7 x 10'4
l.SxlO'4
2.5 x 10'7
4.8 x 10'6
3.7 x 10'7
1.2 x 10°
a PAH = polycyclic aromatic hydrocarbons.
*> Based on operation for 24 hours per day for 310 days per year.
2-13
-------
TABLE 2-9. SUMMARY OF RESULTS FOR DIOXINS AND FURANS
Pollutant
D/FTEQb
D/F Congeners0
D/F Totald
Concentration
(ng/DSCM)
0.19
1.7
11.7
Emission rate Og/hr)
88
757
5,280
Annual emissions3
g/yr
0.66
5.6
39
Ib/ton sinter
1.2xlO'9
l.lx 10'8
7.4 x 10'8
a Based on operation for 24 hours per day for 310 days per year.
b D/F TEQ is the toxicity equivalent expressed relative to 2,3,7,8-TCDD.
c D/F congeners are those dioxins and furans that have a toxicity equivalent factor relative to 2,3,7,8-TCDD.
Total D/F are all dioxins and furans that were reported.
2-14
-------
3.0 TEST LOCATIONS
Figure 3-1 is a schematic showing an overview of the test site with a view of both
locations. The exhaust gas at the outlet stack and scrubber inlet were analyzed from the same
trailer position.
3.1 KINPACTOR SCRUBBER OUTLET - STACK
The test platform and test ports on the 150-ft stack were located at 125 ft above ground
level. Access to the stack platform was provided by a spiral staircase around the exterior of the
scrubber structure to a narrow platform and catwalk about half way up. A permanent caged
ladder in three sections provided access from the catwalk to the stack test platform. The platform
was 2 ft wide around the entire circumference of the stack. There were four 4-in. test ports 90°
apart that were used for testing.
3.2 KINPACTOR SCRUBBER INLET - DUCT
Access to the scrubber inlet location was provided by scaffolding that had been
constructed for this test. The sample port used by MRI was located approximately 20 ft above
ground level and in a plane parallel and upstream of the manual test ports.
3.3 VOLUMETRIC FLOW
Table 3-1 summarizes the gas composition and flow data provided by ERG. ERG
provided volumetric flow rates, moisture content, gas molecular weight, etc., as part of their
manual testing; therefore, MRI did not conduct these tests.
3-1
-------
N)
x-~x
FLOW TO ATMOSPHERE
KINPACTOR
SCRUBBER
3.000 hp FAN
Figure 3-1. Test locations.
-------
TABLE 3-1. SOURCE GAS COMPOSITION AND FLOW SUMMARY
Test data
Run No.
Date
Scrubber inlet
Oxygen, %
Carbon dioxide, %
Moisture content, %
Gas Stream velocity, fpm
Volumetric flow rate, dscfm
Scrubber outlet (Stack)2
Oxygen, %
Carbon dioxide, %
Moisture content, %
Gas Stream velocity, fpm
Volumetric flow rate, dscfm
1
25-Jun-97
19.0
2.5
6.6
6236
248,105
17.5
3.5
11.0
2961
266,998
2
26-Jun-97
18.8
3.3
6.8
6058
241,027
17.5
3.7
11.1
2959
266,783
3
27-Jun-97
18.8
3.3
6.8
6182
255,583
18.2
3.4
10.5
2916
266,178
aData presented in this section is the average of the dioxin and multi-metals tests.
3-3
-------
4.0 RESULTS
4.1 TEST SCHEDULE
The test program at LTV Steel was completed from June 23 to June 27, 1997. Table 4-1
summarizes the sampling schedule. A complete record of all THC and FTIR sampling is in
Appendices A and B. The FTIR and THC sampling was coordinated with the manual sampling
conducted by ERG. Table 3-1 summarizes the gas composition and flow data provided by ERG.
TABLE 4-1. TEST SCHEDULE AT LTV STEEL COMPANY INDIANA HARBOR WORKS
Date
6/23/97
6/24/97
6/25/97
6/26/97
6/27/97
Task
Arrive on site and setup at inlet and outlet.
Completed set up and recorded spectra of preliminary samples.
14:00- 16:45
Test Run 1. FTIR and Method 25 A in conjunction with manual
methods by ERG.
8:37-18:05
Test Run 2. FTIR and Method 25A in conjunction with manual
methods by ERG.
9: 10 -17:20
Test Run 3. FTIR and Method 25A in conjunction with manual
methods by ERG.
8:43 - 13:45
Packed equipment and departed site
Location a
Scrubber inlet and
outlet.
al_ocation descriptions are in Section 2.
4.2 FIELD TEST PROBLEMS AND CHANGES
The flue gas at LTV contained concentrations of both water vapor and carbon dioxide
(CO2> high enough to cause interference in the FTIR frequency regions used in the sample
analyses. Toluene vapor was used for the analyte quality assurance spiking. The CO2 spectrum
interfered with the strongest toluene infrared band near 730 cm"1 so the weaker toluene
absorbance, in the analytical region 2,850 to 3,100 cm"1 range, was used for the analysis. The
presence of other aliphatic (nonaromatic species such as methane and hexane) hydrocarbon
species also contributed to the total infrared absorbance in the 2,850 to 3,100 cm" analytical
region.
During testing the sample flow rate was not constant, particularly at the inlet. The flow
continuously dropped due to particulate clogging of the pre-filter at the inlet probe tip. It was
4-1
-------
necessary to periodically replace the fiberglass pre-filter, twice during runs one and two and once
during run three, to restore the sample flow. The inconsistent sample flow rate may have had
some effect on the spike recovery results (this is discussed further in Section 4.5). The flow drop
during a typical spiking period (about 30 min) was not too severe.
The sampling procedure maintained continuous flow to two hydrocarbon analyzers, one
analyzer for each location. One FTIR instrument was used to sample the two locations
alternately and the FTIR cell was evacuated before switching locations. Opening a sample line to
the evacuated cell caused a temporary pressure drop in that sample line, which caused a
temporary loss of flow to the hydrocarbon analyzer and a corresponding decrease in the THC
analyzer response. These events are noted in the Method 25A results. This problem was
discovered early in the testing so MRI modified the sampling system configuration to minimize
the effects. The affected hydrocarbon data (denoted with *** in the field data) were not included
in the run averages. After this test program MRI installed back pressure regulators on the
manifold vents to eliminate this problem.
The inlet probe was temporarily out of the stack each time the pre-filter was replaced.
This operation did not affect the FTIR results because the pre-filter was always replaced when
the FTIR system was sampling the outlet. The inlet hydrocarbon data for these periods were
logged, but not included in the run averages.
Space was limited on the platform at the outlet location so that it was necessary to change
the MRI outlet sampling port during one of the manual method port changes for each run. This
port change did not affect the FTIR results because it was done while the FTIR system was
sampling at the inlet location. However, the hydrocarbon data were still logged; these data are
noted in the results and were not included in the run averages. The port changes caused the loss
of 20, 30, and 26 min of THC data during runs 1, 2, and 3, respectively.
4.3 METHOD 25A RESULTS
Table 1-2 summarizes the Method 25 A THC results at both the inlet and outlet. The
mass emission data is presented as both THC and total gaseous nonmethane organic carbon
(T<~ VMOC). The TGNMO was calculated using the procedures outlined in Section 5.7.2 of this
report using methane concentrations from the FTIR analysis.
4-2
-------
The THC emissions varied greatly with each test run and peaks in the THC concentration
occurred at several points during each run. The inlet concentrations varied greater than the outlet
concentrations as would be expected after a scrubber. No determinations can be made about the
THC concentration variations without taking into account the process and scrubber operational
conditions for the time period during each run. Table 4-2 shows the minimum and maximum
THC concentrations for each test run.
TABLE 4-2. MINIMUM AND MAXIMUM THC CONCENTRATIONS
Run No.
ppmc
Minimum
Maximum
Average
Scrubber inlet
1
2
3
77.1
53.1
54.6
172.5
•160.8
141
120.6
111.9
89.4
Scrubber outlet (stack)
I
2
3
67.2
56.7
54
108.6
117.9
95.1
80.7
81.0
73.8
The complete Method 25A results are included in Appendix A. The concentrations
presented were measured by MRI, the mass emissions data, presented in Section 1.2, were
calculated using volumetric flow results provided by ERG. The pre- and post-run calibrations
and QA checks met the Method 25A criteria in all cases. Calibration QA results are included in
Appendix A.
4.4 FTIR RESULTS
A summary of the FUR results is presented in Table 1-1. Complete FTIR results at the
inlet and outlet are presented in Tables B-l and B-2, respectively. The infrared spectra showed
evidence of water vapor, CO2, carbon monoxide (CO), methane, formaldehyde, sulfur dioxide
(SO2), toluene, ethylene, hydrocarbon, and ammonia. New reference spectra of nine
hydrocarbon compounds were used in the revised analysis results. The new reference spectra
were measured in the laboratory and helped provide more accurate measurements of the HAPs
hexane and toluene. A description of the analytical procedures used to prepare the FTIR results
4-3
-------
is given in Section 4.5. The mass emission rates were calculated using flow data provided by
ERG. Mass emission calculations for toluene include only the results from unspiked samples.
The inlet and outlet concentrations are similar for methane, hexane, and ethylene.
Concentrations of formaldehyde (runs 2 and 3), ammonia, and SC>2 were reduced by the scrubber
control device (approximately 67, 91, and 76 percent removal, respectively).
4.5 ANALYTE SPIKE RESULTS
A toluene gas standard was used for analyte spiking experiments for quality assurance
only. Preferably, a spike standard combines the analyte and the tracer gas in the same cylinder,
but the SFg and toluene were contained in two separate cylinders. Therefore, the spiking
sequence was; first the sample was spiked with the SFg (or toluene) and, second, the sample was
spiked with the toluene (or SF^). This procedure was followed because it was not possible to
obtain a mixture with both components in time to perform this test.
The spiked concentrations are summarized in Table B-3 and the analyte spike results are
presented in Table 4-3. Samples were spiked with a measured amount of toluene vapor at the
start and completion of each run at each location. A standard of SFg tracer gas was also spiked
into the gas stream to determine the spike dilution factor. A description of the spike procedure is
given in Section 4.4.1.
In most cases the calculated spike recoveries were greater than 130 percent, which is
above the range allowed by Method 301 for a validation correction factor (between 70 and
130 percent). This does not reflect on the accuracy of the emissions results in Tables B-1 and
B-2. The residual spectra (Figure 4-1), which show no significant (or negative) remaining
absorbances, indicate that the computer program correctly measured the absorbances from the
interfering species and the analytes.
Three factors contributed to the high recoveries; two are minor and one is major. These
factors are discussed in order of increasing importance. One minor factor is that the total sample
flow rate varied some during the sampling periods, but the variation was not large during any
spiking period. This factor was only potentially significant at the inlet, where the initial
4-4
-------
TABLE 4-3. SUMMARY OF SPIKE RESULTS
Scrubber Inlet
Run
1
2
3
Toluene
Average
Spike
26.5
33.8
33.1
49.6
37.7
56.5
Unspike
0
1.2
4.4
4.9
4.2
0
Tol(calc)
spike -
unspike
26.5
32.7
28.7
44.7
33.5
56.5
SF6
Average
Spike
0.548
0.666
0.658
1.022
0.745
1.211
Unspike
0.000
0.000
0.000
0.000
0.000
0.000
spike -
unspike
0.548
0.666
0.658
1.022
0.745
1.211
DF
7.3
6.0
6.1
3.9
5.4
3.3
Cexp
16.5
20.1
19.9
30.8
22.5
36.5
Library spectra3
% Recovery
160
163
145
145
149
155
Standard spectra
% Recovery
101
103
91.3
91.3
93.8
97.6
Scrubber Outlet (Stack)
Run
1
2
3
Toluene
Average
Spike
23.5
27.2
28.3
29.0
28.6
.25.2
Unspike
0
0
0
1.4
0
0
Tol(calc)
spike -
unspike
23.5
27.2
28.3
27.6
28.6
25.2
SF6
Average
Spike
0.474
0.512
0.563
0.572
0.539
0.472
Unspike
0.000
0.000
0.000
0.000
0.000
0.000
spike -
unspike
0.474
0.512
0.563
0.572
0.539
0.472
DF
8.5
7.8
7.1
7.0
7.4
8.5
Cexp
14.3
15.4
17.0
17.3
16.3
14.2
Library spectraa
% Recovery
164
176
166
160
176
177
Standard spectra
% Recovery
103
111
105
101
111
111
aThese recoveries were obtained using EPA library reference spectra for toluene.
''These were obtained using spectra of the toluene cylinder standard measured on site.
-------
paniculate filter was periodically replaced, however the spike recoveries were highest in the
outlet samples. The second minor, but more significant factor relates to the determination of the
unspiked toluene concentration in the spiked samples. Because the spiked samples were
measured sequentially and because there was a variable unspiked toluene concentration, there is
an undetermined uncertainty in the calculation of "spike minus unspike."
The spike recoveries were about 100 percent compared to the toluene spike standard.
However, compared to the library toluene reference spectra, the recoveries seem high. The
library spectra and the spectra of the toluene cylinder standard differ by about 37 percent. The
two sets of spectra are compared in Table 4-4. This observation does not effect the spike
recovery results, but it may have implications for the use of the toluene library reference spectra,
and this may warrant further investigation. A similar, but smaller, effect was observed
previously.4
4-6
-------
TABLE 4-4. COMPARISON OF EPA TOLUENE REFERENCE SPECTRA TO SPECTRA OF
TOLUENE CYLINDER STANDARD3
Toluene spectra
1 53a4ara
153a4arc
1530624b
1530624a
Source
EPA lib
EPA lib
LTV test
LTV test
Band area
23.4
4.4
33.4
33.6
Region (cm-1)
3160.8-2650.1
Spectra comparison using the
band areas
Ratio (Ra)
5.4
1.0
7.7
7.7
= l/Ra
0.186
1.000
0.130
0.130
Comparison of spectra using standard
concentrations
(ppm-m)/K
4.94
1.04
5.80
5.80
Ratio (Rb)
4.8
1.0
5.6
5.6
= l/Rb
0.210
1.000
0.179
0.179
a The relevant comparison is R|/Ra About 72 percent lower calculated spike concentrations are obtained using the cylinder standard spectra, 1530624a,b,
instead of the library reference spectra.
-------
4.6 SCREENING RESULTS
Estimated uncertainties for the HAP screening analysis are reported in Table 4-5. The
spectra were analyzed for the potential analytes listed in the original test request and for other,
principally hydrocarbon, species, which are in the EPA library of FTIR reference spectra or were
measured in the laboratory after completion of the test. The procedure for estimating the
uncertainties is described in Section 5.5. The compounds for which the spectra were screened
and the analytical region(s) for each compound are given in Table 4-6. The reported
uncertainties can be interpreted as the practical measurement limits imposed by the sampling
conditions. The method of calculating uncertainties was identical to that used for the compounds
reported in Tables B-l and B-2 and depends on the noise in the residuals (Figure 4-1).
4-8
-------
TABLE 4-5. SUMMARY OF ESTIMATED UNCERTAINTIES FOR UNDETECTED TARGET ANALYTES AT LTV STEEL
Compound
Benzene (ch)
Methyl bromide (fp)
Methyl Chloride (ch)
Methyl chloroform (fp)
1 , 1 -Dichloroethane (ch)
l,3-Butadiene(fp)
Carbon tetrachloride (fp)
Chlorobenzene (fp)
Cumene (ch)
Ethylbenzene (ch)
Methylene chloride (fp)
Propionaldehyde (ch)
Styrene (fp)
1 , 1 ,2,2-Tetrachloroethane (fp)
p-Xylene (ch)
o-Xylene (ch)
m-Xylene (ch)
Isooctane (ch)
Run 1
Inlet uncertainty
2.1
7.2
5.1
0.7
6.1
0.8
0.13
2.3
2.1
5.1
1.3
11
1.7
0.59
3.9
4.1
9.4
0.50
Outlet uncertainty
2.7
9.9
7.2
0.9
9.3
1.2
0.20
3.0
2.9
7.6
1.8
1.7
2.4
0.87
5.9
5.6
12.1
0.67
Run 2
Inlet uncertainty
1.8
7.5
4.5
0.7
5.4
0.8
0.13
2.4
1.8
4.5
1.4
1.0
1.7
0.61
3.4
3.6
8.3
0.44
Outlet uncertainty
2.9
10.8
7.6
1.0-
9.7
1.3
0.22
3.2
3.0
8.0
1.9
1.8
2.7
0.95
6.2
5.9
12.7
0.70
Run 3
Inlet uncertainty
1.8
7.0.
4.4
0.7
5.2
0.7
0.12
2.2
1.8
4.4
1.3
1.0
1.6
0.57
3.3
3.5
8.1
0.42
Outlet uncertainty
3.3
13.4
8.7
1.2
11.2
1.6
0.28
4.0
3.5
9.2
2.2
2.1
3.3
1.2
7.1
6.8
14.7
081
Analytical Region
(ch)-2,650.1 -3,160.8cm
(fp)- 789.3- 1275.0cm-'
Procedure for estimating uncertanties is described in Section 4.5.3
-------
TABLE 4-6. PROGRAM INPUT FOR ANALYSIS OF SAMPLE SPECTRA
Compound name
Water
Carbon monoxide
Sulfur dioxide
Carbon dioxide
Formaldehyde
Benzene
Methane
Methyl bromide
Toluene
Methyl chloride
Methyl chloroform
1.1-dichloroe thane
1 ,3 -butadiene
Carbon tetrachloride
Chlorobenzene
Cumene
Ethyl benzene
Methylene chloride
Propionaldehyde
Styrene
1 , 1 ,2,2-tetrachloroethane
p-Xylene
o-Xylene
m-Xylene
Ethylene
SF6
Ammonia
Hexane
butane
n-heptane
pentane
1 -pentene
2 -methyl- 1-pemene
2-methyl-2butene
2-methyl-2-pentene
Isooctane
T .vwthulrw-nl'an^'
File name
194hsub
co20829a
I98clbsi
co2ascal
087clasa
015a4ara
196clbsd
106a4asb
153a4arc
107a4asa
108a4asc
086b4asa
023a4asc
029a4ase
037a4arc
046a4asc
077a4arb
117a4asa
140b4anc
147a4asb
150b4asb
173a4asa
17U4asa
172a4arh
CTS0626b
Sf6_002
174clasc
0950709a
bur0715a
hep0716a
pen0715a
Ipe0712a
2mlp716a
2m2b716a
2m2p713a
16507 15a
3mo0713a
Region No.
1.2.3
1
2
1.2.3
3
3
3
2
3
3
2
2
2
2
2
3
3
2
3
2
2
2
3
2
2
2
2
3
3
3
3
3
3
3
3
3
3
ISC (* indicates
arbitrary)
100*
167.1
90.3
415*
4.436
496.6
16.09
485.3
103.0
501.4
98.8
499.1
98.4
20.1
502.9
96.3
515.5
498.5
99.4
550.7
493.0
488.2
497.5
497.8
20.1
1.0029
10.0
46.9
100.0
49.97
49.99
50.1
50.08
50.04
51.4
50.3
50.0
Reference
Meters
22
22
22
3
22
3
3
3
3
2.25
3
3
3
3
3
3
2.25
3
2.25
3
3
3
18.9
22
20
10.3
11.25
10.3
10.3
10.3
10.3
10.3
10.3
10.3
10.3
T (K)
394
394
394
298
394
298
298
298
298
373
298
298
298
298
298
298
373
298
373
298
298
298
394
394
388
399
397.8
398.3
397.9
399
398.2
398.2
398.6
398.3
398.5
Region No.
1
2
3
Upper cm- 1
2.142.0
1,275.0
3,160.8
Lower cm- 1
2.035.6
789.3
2.650.1
4-10
-------
-.05-
3100
3000
2900
Wavenumbers
2800
2700
Top trace, "inls4012" post run sample spiked with toluene; bottom traces, (overlaid) subtracted residual spectra from
samples "inls4001" to "mls4012."
Figure 4-1. Example residual spectra.
-------
5.0 TEST PROCEDURES
The procedures followed in this field test are described in EPA Method 320 for using
FTIR spectroscopy to measure HAP's, the EPA Protocol for extractive FTIR testing at industrial
point sources and EPA Method 25A for measuring total gaseous organics. The objectives of the
field test were to use the FTIR method to measure emissions from the processes, screen for
HAP's in the EPA FTIR reference spectrum library, conduct analyte spiking for quality
assurance, and analyze the spectra for compounds not in the EPA library. Additionally, manual
measurements of gas temperature, gas velocities, moisture, CC^, and C>2 by ERG were used to
calculate the mass emissions rates.
The extractive sampling system shown in Figure 5-1 was used to transport sample gas
from the test ports to the FTIR instrument and the THC analyzer.
5.1 SAMPLING SYSTEM DESCRIPTION
Flue gas was extracted through a 4-ft stainless steel probe and transported to the gas
distribution manifold through heated, insulated, 3/8-in. OD Teflon® sample line. A KNF
Neuberger heated head sample pump (Model NO35 ST.l II) was used to pull sample through the
line at 10 to 15 liters per minute (Lpm). A Balston paniculate filter (holder Model Number
30-25, filter element Model Number 100-25-BH, 99 percent removal efficiency at 0.1 f^m) was
connected in-line at the outlet of the sample probe. Temperature controllers monitored and
regulated the sample line temperature at about 350°F.
Inside the FTIR trailer, the outlet of the sample pump was connected to the heated
stainless steel gas manifold. Immediately inside the manifold the sample stream passed through
a secondary paniculate filter. The manifold contained 3/8-in. stainless steel tubing, three
four-way valves and heated radiometers (0 to 20 Lpm) to allow the operator to control sample
flow to the FTIR cell and THC analyzer. The three manifold outlets were used to supply sample
to the FTIR gas cell and to two THC analyzers. Heated 1/4-in. OD, 20-ft long Teflon® lines
connected the manifold outlet to the inlet of the FTIR gas cell and the THC analyzers. The
manifold was maintained at about 300°F.
5-1
-------
Vent
Vent
Vent*2 <
Ventfl
NJ
Data Storage A Analyil* FOR Spectrometer Heated CeD
Heated Probe Box *1
Heated Probe *1
J-WeyV«t»
^BtUxAHM
Bundlet are 50-300+ fi. long.
Sample Urn
CaHxaUon Qa» / Spfce Une
Sample Trantfer Line (Heated Bundle) *1
Heated Probe Box 12
Heated Probe Hi
Bundle! are 50-300+ A. long.
Sample Une
Calibration OM/Spike Line
Sample Transfer Une (Heated Bundle) *2
Calibration Standard!
Figure 5-1. Extractive sampling system.
-------
5.2 SAMPLING PROCEDURES
Sampling was conducted at both the scrubber inlet duct and the process stack. The two
locations were sampled using two separate sampling systems which were both connected to the
main manifold (Figure 5-1). A single FTIR instrument and two THC analyzers were used to
sample both locations. The four-way valves on the outlets of the common manifold could be
used to select sample from either location. The FTIR instrument was used to sample each
location alternately, while the two THC analyzers were used to sample both locations
simultaneously. Sample flow to each instrument was controlled by the use of the rotameter
needle valves.
5.3 FTIR SAMPLING PROCEDURES
Figure 5-1 shows a schematic of the FTIR instrument and connections to the sample
distribution manifold.
Sampling was conducted using either the batch or the continuous sampling procedures.
All data were collected according to Method 320 sampling procedures, which are described
below.
5.3.1 Batch Samples
In this procedure, the four-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 Run 1.
Batch sampling has the advantage that every sample is independent. The time resolution
of the measurements is limited by the interval required to pressurize the cell, and record the
spectrum, for this test the time resolution was 4 to 5 min. All of the spiked samples and all of the
samples in Run 1 were collected using this procedure.
5.3.2 Continuous Sampling
The cell was filled as in the batch sampling procedure, but the cell inlet and outlet valves
were then opened to keep gas continuously flowing through the cell. The inlet and outlet flows
5-3
-------
were regulated to keep the sample at ambient pressure. The flow through the cell was maintained
at about 5 Lpm (about 0.7 cell volumes per min). The cell volume was about 7 liters (L).
The FTIR instrument was automated to record spectra of the flowing sample about every
2 min. The analytical program was revised after the field tests and the spectra were analyzed to
prepare the results reported in Section 4.
This procedure with automated data collection was used for all of the unspiked testing
during Runs 2 and 3. 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) depended on the sample flow rate (through the cell), and
the cell volume. The following explanation is taken from Performance Specification 15 for FTIR
CEMS.
'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 (^g in Lpm), the cell volume (^ejj in L) and the analyte's chemical
and physical properties.'
= ~jT (1)
s
Performance Specification 15 defines 5 * TC as the minimum interval between independent
samples. In this test 5 *TC was about 7 minutes.
A stainless steel tube ran from the cell inlet connection point to the front of the cell. The
outlet vent was at the back of the cell so that the flowing sample passed through the greatest
portion of the cell volume.
5.4 ANALYTE SPIKING
Since no information about possible HAP emissions or flue gas composition was
available for this source prior to the test, there was no plan for validating specific HAP's at this
screening test. MRI conducted limited spiking for quality control (QC) purposes using a toluene
(121 ppm in air) standard.
5.4.1 Analvte Spiking Procedures
The infrared spectrum is ideally suited for analyzing and evaluating spiked samples
because many compounds have very distinct infrared spectra.
5-4
-------
The reason for analyte spiking is to provide a QC 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. No validation was performed at this field test.
The spike procedure follows Sections 9.2 and 13 of EPA draft Method 320 in
Appendix D. In this procedure a gas standard is measured directly in the cell. This direct
measurement is then compared to measurements of the analyte in spiked samples. Ideally, the
spike comprises about 1/1-0 or less of the spiked sample. The actual dilution ratio depends on the
sample flow rate and the spike gas flow rate. The expected concentration of the spiked
component is determined using a tracer gas, SFg. The SFg concentration in the direct sample
divided by the SFg concentration in the spiked sample(s) is used as the spike dilution factor (DF).
The analyte standard concentration divided by DF gives the "expected" value (100 percent) of the
spiked analyte recovery.
5.4.2 Analysis of Spiked Results
The toluene and SF/r concentrations used in the evaluation of the spike recoveries in
Table 4-3 were taken directly from the sample analyses reported in Tables B-l and B-2. The
concentrations in the spiked samples included a contribution from the spike gas and from any
analyte present in the flue gas. The component of the spike recovery in the spiked samples was
determined by subtracting the average of the unspiked samples from the measured (average)
concentration in each spiked sample (spiked - unspiked). The percent recovery was determined
by comparing the spiked - unspiked concentration to the calculated 100 percent recovery
determined in Section 5.4.1.
5.5 ANALYTICAL PROCEDURES
Analytical procedures in the EPA FTIR Protocol2 were followed for this test. A
computer program was prepared with reference spectra shown in Table 4-6. The computer
program^ used mathematical techniques based on a K-matrix analysis.
Initially, the spectra were reviewed visually to determined appropriate input for the
computer program. Next an analysis was run on all of the sample spectra using all of the
reference spectra listed in Table 4-6. The estimated uncertainty results for the undetected species
5-5
-------
were reported in Table 4-4. Finally, the undetected compounds were removed from the analysis
and the spectra were analyzed again using reference spectra only for the detected compounds.
The results from this second analytical run are summarized in Table 1-1 and reported in
Tables B-l and B-2. The revised analysis for this report included reference spectra of n-heptane,
1-pentene, 2-methyl-2-butene, n-pentane, 2-methyl-2-pentene, 3-methylpentane, butane, and
2-methyl-l-pentene.
The same program that performed the analysis calculated the residual spectra (the
difference between the observed and least squares fit absorbance values). Three residuals, one
for each of the three analytical regions, were calculated for each sample spectrum. All of the
residuals were stored electronically and are included.with the electronic copy of the sample data
provided with this report. Finally the computer program calculated the standard l*sigma
uncertainty for each analytical result, but the reported uncertainties are equal to 4*sigma.
The concentrations were corrected for differences in absorption path length and
temperature between the reference and sample spectra using equation 2.
T.
C
con
L
T.
(2)
where:
^Corr = Concentration, corrected for path length and temperature.
CCa|c = Concentration, initial calculation (output of the analytical program designed for the
compound).
Lj. = Reference spectrum path length.
Lg = Sample spectrum path length.
TS = Absolute temperature of the sample gas, K.
Tr = Absolute gas temperature of reference spectrum sample, K.
The sample path length was estimated by measuring the number of laser passes through
the infrared gas cell. These measurements were recorded in the data records. The actual sample
path length, LS was calculated by comparing the sample CTS spectra to CTS spectra in the EPA
FTIR reference spectrum library. The reference CTS were used as input for a K-matrix analysis.
The calculated cell path length and the variation among the sample CTS over 3 days of testing,
are reported in Table 5-2.
5-6
-------
5.5.1 Computer Program Input
Table 4-6 presents a summary of the reference spectra input for the computer program
used to screen the sample spectra. Table 5-1 summarizes the program input used to analyze the
CTS spectra recorded at the field test. The CTS spectra were analyzed as an independent
determination of the cell path length. To analyze the CTS spectra, MRI used 0.25 cm-1 spectra
"cts0814b" and "cts0814c." These reference CTS spectra were recorded on the same dates as the
toluene reference spectra used in the analysis. These spectra were deresolved in the same way as
the toluene reference spectra using Section K.2.2 of the EPA FTIR protocol. The program
analyzed the main two ethylene bands centered near 2,989 and 949 cm'1. Table 5-2 summarizes
the results of the CTS analysis. The cell path length from this analysis was used as Ls in
equation 2.
5.5.2 EPA Reference Spectra
The toluene spectra used in the MRI analysis were taken from the EPA reference
spectrum library (http://www.epa.gov/ttn/emc/ftir.html). The original sample and background
interferograms were truncated to the first 16,384 data points. The new interferograms were then
Fourier transformed using Norton-Beer medium apodization and no zero filling. The
transformation parameters were chosen to agree with those used to collect the sample absorbance
spectra. The new 1cm'1 toluene single beam spectra were combined with their deresolved single
beam background spectra and converted to absorbance. This procedure was used to prepared
spectral standards for toluene and other HAP's that were included in the analysis.
5.6 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.
5-7
-------
TABLE 5-1. PROGRAM INPUT FOR ANALYSIS AND CTS SPECTRA AND PATH
LENGTH DETERMINATION (CTSLTV.MCP)a
Compound name
Ethylene
Ethylene
File name
cts0814b.asd
cts0814c.asd
ASCb
1.007
1.007
ISCb
1.014
0.999
% Difference
0.69
0.79
aSample CTS spectra were analyzed from 1107 to 843 cm"1 and from 2992 to 2984cm'
ASC = accepted concentration. ISC = calculated concentration.
TABLE 5-2. RESULTS OF PATH LENGTH DETERMINATION
CTS spectra
20.01 ppm Ethylene
CTS0623A , .
CTS0624A
CTS0624B
CTS0625A
CTS0625B
CTS0626A
CTS0626B
CTS0627A
CTS0627B
CTS0627C
Average Path Length (M)
Standard Deviation
Path length calculations
Meters
18.75
18.22
18.09
18.30
18.07
18.79
17.96
18.07
18.25
18.44
18.3
0.287
Aa
0.46
-0.07
-0.20
0.01
-0.22
0.50
-0.33
-0.22
-0.04
0.15
%Aa
2.48
-0.37
-1.09
0.07
-1.20
2.69
-1.86
-1.19
-0.22
0.84
= calculated path length in meters minus the average path length.
5-8
-------
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 achieved. The number of passes was
recorded on the field data sheets in Appendix B. The path length in meters was determined by
comparing calibration transfer standard (CTS, ethylene in nitrogen) spectra measured in the field
to CTS spectra in the EPA reference spectrum library. Figure 5-1 instrument were integrated
with the sampling system.
5.7 CONTINUOUS EMISSIONS MONITORING FOR THC
The guidelines set forth in Method 25A were used for sampling at LTV Steel with one
exception. Section 7.2 of Method 25A specifies an analyzer drift determination hourly during the
test period, this instruction was not followed.
The drift determination was not completed as specified to keep the FTIR and THC
sampling synchronized as closely as possible. Drift checks would have involved THC and FTIR
off-line periods of about 10 min per hour. Experience with the analyzers MRI was using
indicates they are capable of stable operation over extended periods when the analyzers are
operated in a climate controlled environment.
5.7.1 THC Sampling Procedures
The THC sampling was conducted continuously from both locations by the use of two
separate analyzers. The same sample systems used for the FTIR sampling were used for the THC
sampling. Sample gas was directed to the analyzers through a separate set of rotameters and
control valves. Each test run was conducted from the start to the end of the manual test runs
completed by ERG. A summary of specific procedures used is given below.
A brief description of each system component follows.
1. THC Analyzer- The THC concentration is measured using a flame ionization detector
(FID). MRI used a J.U.M. Model VE-7 and a Ratfisch Model RS-55CA. The THC analyzers
were operated on the zero to 100 ppm range throughout the test period. The fuel for the FTD 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. The averaging period set for this test was 1 min.
5-9
-------
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 is reported in ppm as propane, but is converted to an
as carbon basis for reporting.
5.7.2 Hydrocarbon Emission Calculations
The hydrocarbon data is presented as both THC and TGNMO emissions in Table 1-2. To
do this the THC emission data was first converted to an as carbon basis using equation 3 and then
the THC emission rate was calculated using Equation 5.
CC=KCmeas (3)
where:
Cc = Organic concentration as carbon, ppmv.
Cmeas = Organic concentration as measured, ppmv.
K = Carbon equivalent correction factor, 3 for propane.
The TGNMO concentration was calculated by subtracting the methane concentration
measured by the FTIR from Cc (equation 4). The emission rate was then calculated using
Equation 5.
(4)
where:
CTGNMO = Total gaseous nonmethane organic concentration, ppmv
CCH4 = Methane concentration in gas stream, ppmv.
C
x MW x CL. x 60
(1-BWS) s'd (5)
fcroNMom^ 385.3 x 106
where:
ETGNMO/THC = TGNMO or THC mass emission rate, Ib/hr
Bws = moisture fraction in gas stream
5-10
-------
MW = Molecular Weight of Carbon, 12 Ib/lb-mole
Qstd = Volumetric Flowrate corrected to standard conditions, dscfm
60 = Conversion to hours, min/hr
385.3 = Molar Volume, ft3/mole at standard conditions
106 = Conversion for decimal fraction to ppm
5-11
-------
6.0 SUMMARY OF QA7QC PROCEDURES
6.1 SAMPLING AND TEST CONDITIONS
Before the test sample lines were checked for leaks and cleaned by purging with moist air
(250°F). Following this, the lines were checked for contamination using dry nitrogen. This is
done by heating the sampling lines to 250°F and purging with dry nitrogen. The FTIR cell was
filled with some of the purging nitrogen and the spectrum of this sample was collected. This
single beam spectrum was converted to absorbance using a spectral background of pure nitrogen
(99.9 percent) taken directly from a cylinder. The lines were checked again on site before
sampling, after each change of location, and after spiking.
During sampling spectra of at least 10 different samples were collected during each hour
(five at each of two locations).
Each spectrum was assigned a unique file name and written to the hard disk and a backup
disk under that file name. Each interferogram was also be 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
6-1
-------
• Length of time to measure spectrum
• Time spectrum was collected
• Time and conditions of recorded background spectrum
• Time and conditions of relevant CTS spectra
• Apodization
Hard copy records were also kept of all flue gas measurements, such as sample flow,
temperature, moisture and diluent data.
Effluent was allowed to flow through the entire sampling system for at least 5 minutes
before a sampling run started or after changing to a different test location. FTIR spectra were
continuously monitored to ensure that there was no deviation in the spectral baseline greater than
±5 percent (-0.02 < absorbance <, +0.02). When this condition occurred, sampling was
interrupted and a new background spectrum was collected. The run was then be resumed until
completed or until it was necessary to collect another background spectrum.
6.2 FTIR SPECTRA
For a detailed description of QA/QC procedures relating to data collection and analysis,
refer to the "Protocol For Applying FTIR Spectrometry in Emission Testing".2
A spectrum of the CTS was recorded at the beginning and end of each test day. A leak
check of the FTIR cell was also performed according to the procedures in references 1 and 2.
The CTS gas was 20.1 ppm ethylene in nitrogen. The CTS spectrum provided a check on the
operating conditions of the FTIR instrumentation, e.g., spectral resolution and cell path length.
Ambient pressure were recorded whenever a CTS spectrum was collected. The CTS spectra
were compared to CTS spectra in the EPA library. This comparison is used to quantify
differences between the library spectra and the field spectra so library spectra of HAP's can be
used in the quantitative analysis.
Two copies of all interferograms, processed backgrounds, sample spectra, and the CTS
were stored on separate computer disks. Additional copies of sample and CTS absorbance
spectra were also be stored for data analysis. Sample absorbance spectra can be regenerated from
the raw interferograms, if necessary.
The compact disk enclosed with this report contains one complete copy of all of the FTIR
data recorded at the LTV field test. The data are organized into directories, whose titles identify
6-2
-------
the contents. The data continuously are in directories identified by the date on which the data
were recorded. The directory titles "BKG," "CTS,", "outlet," and "inlet," identify backgrounds,
CTS spectra, and spectra of inlet and outlet samples, respectively. Additional sub-directories
"AIF' and "ASF' identify inferograms and absorbance spectra, respectively. All of the sample
data are in the Analect Instruments software format. The directories "refs" and "residuals"
contain de-resolved reference spectra that were used in the analysis and the residual spectra,
respectively. There are three residual spectra for each sample spectrum, a residual for each
analytical region. The information on the enclosed disk with the data records in Appendix A
meet the reporting requirements of the EPA FTIR Protocol and Method 320.
To measure HAP's detected in the gas stream MRI used spectra from the EPA library,
when available.
6.3 METHOD 25A
6.3.1 Initial Checks
Before starting the first run, the following system checks were performed.
1. Zero and Span check of the analyzer;
2. Analyzer linearity check at intermediate levels; and
3. Response time of the system.
Calibration criteria for Method 25A is ±5 percent of calibration gas value.
6.3.2 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.
6-3
-------
7.0 REFERENCES
1. Test Method 320 (Draft) "Measurement of Vapor Phase Organic and Inorganic Emissions by
Extractive Fourier Transform Infrared (FTIR) Spectroscopy," 40 CFR Part 63,
Appendix A.
2. "Protocol For The Use of FTIR Spectrometry to Perform Extractive Emissions Testing at
Industrial Sources," Revised, EPA Contract No. 68-D2-0165, Work Assignment 3-12,
September, 1996.
3. "Method 301 - Field Validation of Pollutant Measurement Methods from Various Waste
Media," 40 CFR Part 63, Appendix A.
4. "Validation of EPA FTIR Method For Measuring HC1," T. J. Geyer and G. M. Plummer, Ajr
and Waste Management Association Paper Number 97-MP74.05. 1997.
5. "An Examination of a Least Squares Fit FTIR Spectral Analysis Method," G. M. Plummer
and W. K. Reagen, Air and Waste Management Association. Paper Number 96-WA65.03,
1996.
6. "Computer-Assisted Quantitative Infrared Spectroscopy," Gregory L. McClure (ed.), ASTM
Special Publication 934 (ASTM), 1987.
7-1
-------
APPENDIX A
METHOD 25A AND VOLUMETRIC FLOW DATA
A-l
-------
A-l METHOD 25 A RESULTS
A-2
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-204443-01
Operator: Gulick
Time
(24 hour)
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
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
THC 1 (Inlet)
(ppm)
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
37.4
37.3
37.1
37.1
36.9
37.0
37.1
37.5
37.1
37.1
THC 2 (Outlet)
(ppm)
24.5
24.4
24.7
24.6
24.4
24.1
24.2
24.4
24.9
24.7
24.5
24.3
24.3
24.3
24.4
24.4
24.4
24.7
24.8
24.9
25.6
25.9
25.9
26.0
26.0
25.9
26.1
26.1
26.3
26.3
26.2
25.9
25.7
25.8
25.7
25.4
25.3
24.9
24.5
24.4
24.5
24.3
24.5
24.0
24.5
24.1
24.2
RUN 1, Page 1
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-20-04-0341
Operator: Oulick
Time
(24 hour)
1014
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
1053
1054
1055
1056
1057
1058
1059
1100
1101
THC 1 (Inlet)
(ppm)
37.1
37.5
38.0
38.1
38.7
38.8
38.5
38.6
38.6
38.2
38.5
38.9
39.1
40.0
40.3
40.6
41.1
41.2
40.8
40.0
38.7
38.1
37.5
36.8
36.1
35.9
36.1
35.9
35.9
36.3
36.4
35.8
35.5
35.6
36.1
36.2
36.6
37.0
37.3
37.8
37.8
38.0
38.2
38.2
38.4
38.3
38.1
38.3
THC 2 (Outlet)
(ppm)
24.2
24.5
24.9
25.1
25.3
25.7
25.5
25.5
25.7
25.2
25.6
25.9
25.9
26.5
26.7
26.9
27.6
27.7
27.3
26.9
26.4
25.7
25.2
24.8
24.5
24.4
24.3
24.3
24.4
24.7
24.7
24.5
24.4
24.2
24.2
24.4
25.0
25.1
25.3
25.7
25.8
25.9
26.3
26.1
26.3
26.2
26.2
26.1
RUN 1, Page 2
-------
LTV
Run 1
Date: 6/25/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1141
1142
1143
1144
1145
1146
1147
1148
1149
THC 1 (Inlet)
(ppm)
38.4
38.1
37.8
37.5
37.3
37.2
37.1
36.6
34.7
26.0
29.5
33.7
34.2
34.1
***
**»
***
33.8
34.1
***
***
***
34.9
35.3
31.8
***
•**
***
34.5
34.6
34.6
34.7
34.3
34.3
33.8
33.5
33.2
33.3
33.1
33.0
33.2
32.6
32.3
32.0
32.3
34.3
34.1
34.2
THC 2 (Outlet)
(ppm)
26.4
26.3
26.1
25.8
25.5
25.5
25.4
25.3
25.0
24.6
24.3
24.2
24.5
24.3
24.5
24.4
24.4
24.5
24.6
24.7
25.3
25.6
25.5
25.7
25.8
25.6
25.4
25.5
25.5
25.5
25.4
25.4
25.2
25.4
25.5
25.2
25.1
25.5
25.7
24.2
24.9
26.0
25.9
23.3
26.5
27.2
27.5
28.1
RUN 1, Page 3
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1150
1151
1152
1153
1154
1155
1156
1157
1158
1159
1200
1201
1202
1203
1204
1205
1206
1207
1208
1209
1210
1211
1212
1213
1214
1215
1216
1217
1218
1219
1220
1221
1222
1223
1224
1225
1226
1227
1228
1229
1230
1231
1232
1233
1234
1235
1236
1237
THC 1 (Inlet)
(ppm)
34.5
34.4
34.2
33.9
33.9
34.0
34.0
34.4
34.4
34.4
25.7
44.4
46.8
47.8
49.6
50.9
Filter Change
Analyzers off line
49.4
50.5
51.3
52.0
52.3
52.7
53.5
53.5
53.5
54.0
55.0
56.0
56.4
56.9
57.5
56.8
56.7
56.4
56.8
56.6
56.7
57.1
56.8
55.5
54.6
54.1
54.3
53.5
53.4
THC 2 (Outlet)
(ppm)
28.7
29.0
29.2
29.0
29.2
29.4
30.0
30.1
30.4
30.6
31.1
31.6
32.4
32.8
33..1
34.1
Filter Change
Analyzers off line
30.9
31.3
31.8
32.1
32.3
32.3
32.7
32.9
33.1
33.7
34.5
35.2
35.2
35.6
36.0
36.2
35.9
35.5
35.8
35.7
35.4
34.8
32.0
31.6
32.4
32.6
33.3
33.4
33.6
RUN 1, Page 4
-------
LTV
Run 1
Date: 6/25/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1238
1239
1240
1241
1242
1243
1244
1245
1246
1247
1248
1249
1250
1251
1252
1253
1254
1255
1256
1257
1258
1259
1300
1301
1302
1303
1304
1305
1306
1307
1308
1309
1310
1311
1312
1313
1314
1315
1316
1317
1318
1319
1320
1321
1322
1323
1324
1325
THC 1 (Inlet)
(ppm)
52.5
51.6
51.3
51.0
50.1
48.9
47.8
46.9
46.2
45.6
45.1
43.7
42.8
42.4
42.4
»**
42.6
43.3
44.3
***
43.6
44.4
44.0
***
42.5
43.4
***
***
42.9
43.6
43.7
44.0
44.0
44.1
44.4
44.7
45.0
45.2
44.8
45.0
44.6
45.6
45.2
43.5
42.7
41.6
41.0
40.8
THC 2 (Outlet)
(ppm)
33.5
33.2
33.2
33.1
32.7
31.9
31.2
26.2
29.9
29.7
27.6
26.4
27.9
27.7
27.7
28.0
28.2
28.3
28.9
29.1
29.5
29.4
29.3
29.2
29.2
29.2
29.1
29.1
29.4
29.8
29.2
25.9
29.3
28.5
26.6
25.9
30.1
30.8
30.1
30.0
30.7
31.1
30.3
Port Change
Port Change
Port Change
Port Change •
Port Change
RUN 1, Page 5
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1405
1406
1407
1408
1409
1410
1411
1412
1413
THC 1 (Inlet)
(ppm)
41.9
41.0
39.3
38.6
37.9
38.3
38.2
36.6
Filter Change
Fitter Change
Filter Change
Filter Change
Leak Check
Leak Check
43.3
44.0
44.6
44.7
44.1
43.4
43.3
43.1
42.5
42.7
42.9
42.1
41.9
41.7
41.7
40.6
40.4
40.0
39.7
39.4
39.3
39.0
39.4
39.8
40.0
39.5
39.0
38.8
39.0
38.8
39.2
39.3
39.5
39.0
THC 2 (Outlet)
(ppm)
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
Port Change
26.1
26.4
26.7
26.9
27.1
26.8
26.9
26.8
26.7
26.7
26.7
26.4
26.3
26.3
26.1
25.9
25.7
25.2
24.7
24.8
24.8
25.0
25.0
25.9
26.1
25.6
25.5
26.0
26.2
25.8
26.1
26.6
26.4
RUN 1, Page 6
-------
LTV
Run 1
Date: 6/25/97
Project No. : 3802-2044-03-01
Operator: Gulick
Time
(24 hour)
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
1441
1442
1443
1444
1445
1446
1447
1448
1449
1450
1451
1452
1453
1454
1455
1456
1457
1458
1459
1500
1501
THC 1 (Inlet)
(ppm)
37.2
36.7
35.1
38.4
38.6
34.8
36.1
39.2
39.4
39.8
40.1
40.5
41.1
41.5
41.6
40.6
39.1
39.9
40.2
39.7
39.0
38.7
38.3
37.6
36.7
36.3
35.7
35.6
35.8
35.4
34.9
34.8
34.9
34.7
34.4
34.1
34.0
33.5
33.0
32.0
30.2
31.6
32.6
33.3
32.0
32.1
34.0
34.4
THC 2 (Outlet)
(ppm)
26.1
26.5
26.8
27.3
27.5
27.5
27.7
28.4
28.6
28.7
29.3
29.6
30.2
29.4
29.2
28.7
28.3
28.2
28.0
27.6
26.9
26.2
26.2
26.2
25.8
24.9
24.5
24.7
24.9
24.7
23.8
23.8
24.4
24.3
23.6
23.1
23.3
23.2
23.1
22.9
22.8
22.6
22.7
22.8
23.0
23.4
23.8
23.7
RUN 1, Page 7
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-20-04-03-01
Operator: Gulick
Time THC 1 (Inlet) THC 2 (Outlet)
(24 hour) (ppm) (ppm)
1502 34.6 23.7
1503 32.9 23.9
1504 33.5 24.1
1505 34.6 24.3
1506 35.4 24.5
1507 33.6 24.7
1508 33.4 24.8
1509 35.4 24.8
1510 36.0 24.7
1511 36.0 24.4
1512 36.1 24.0
1513 36.2 24.3
1514 36.2 24.6
1515 35.7 24.5
1516 35.5 23.9
1517 THCFIameout 23.7
1518 System Check 24.0
1519 24.0
1520 24.1
1521 23.7
1522 23.8
1523 24.2
1524 24.5
1525 24.4
1526 24.1
1527 24.4
1528 25.1
1529 25.4
1530 25.5
1531 22.4
1532 System Check
1533 THC off fine
1534
1535
1536
1537
1538
1539
1540
1541
1542
1543
1544
1545
1546
1547
1548
1549
RUN 1, Page 8
-------
LTV
Run 1
Date: 6/25/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1617
1618
1619
1620
1621
1622
1623
1624
1625
1626
1627
1628
1629
1630
1631
1632
1633
1634
1635
1636
1637
THC 1 (Inlet)
(ppm)
34.8
34.8
35.6
36.1
36.3
34.6
35.8
37.6
37.7
38.4
36.4
37.7
39.6
40.4
37.9
39.8
42.6
43.5
43.6
44.1
44.9
45.3
45.4
45.6
45.5
45.2
45.3
44.9
THC 2 (Outlet)
(ppm)
24.2
25.2
26.1
26.0
26.1
24.9
24.6
25.7
26.2
25.6
28.0
28.0
28.7
28.9
29.0
27.3
25.5
25.7
25.8
26.0
25.9
25.9
26.2
26.0
26.3
26.6
26.7
27.0
27.1
27.4
27.7
28.1
28.6
28.4
28.5
28.4
28.4
29.3
29.6
29.6
29.3
28.4
28.3
RUN 1, Page 9
-------
LTV
Run 1
Date: 6/25/97
Project No.: 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1638
1639
1640
1641
1642
1643
1644
1645
1646
1647
1648
1649
1650
1651
1652
1653
1654
1655
1656
1657
1658
1659
1700
1701
THC 1 (Inlet)
(ppm)
44.6
43.5
43.4
43.1
42.8
42.7
42.5
42.5
42.3
42.5
42.9
42.8
42.5
42.2
38.0
39.1
41.3
40.6
35.6
39.5
40.5
39.7
39.9
40.5
THC 2 (Outlet)
(ppm)
28.8
28.2
27.6
27.2
27.4
27.7
27.7
26.7
26.8
27.5
27.8
27.4
27.0
26.9
26.8
27.1
27.4
27.4
27.2
27.2
27.1
26.6
26.4
26.7
Minimum3 25.7 22.4
Maximum3 57.5 36.2
Average3 40.2 26.9
*** Sample flow fluctuation due to filling of FTIR cell
Data point not used in average
RUN 1, Page 10
-------
60
THC Concentrations vs. Time (Run 1, 6/25/97)
THC (Inlet) (ppm)
THC (Outlet) (ppm)
50
40
E
o.
a.
X.X
U
m
H
30
20
10
0
9.00
10:00
11:00
12:00
13:00
14:00
15;00
16:00
17:00
Time
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
953
954
955
956
957
958
959
1000
1001
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
1015
1016
1017
1018
1019
1020
1021
1022
1023
1024
1025
1026
1027
1028
1029
THC 1 (Inlet)
(ppm)
30.6
30.5
31.0
30.5
30.4
30.6
30.9
31.0
30.9
30.5
30.6
30.2
30.1
30.0
29.5
29.3
29.8
30.1
30.0
30.4
30.5
30.7
30.7
30.8
31.0
31.3
30.8
30.7
30.7
30.5
30.1
30.0
30.1
30.2
30.3
30.3
30.4
THC 2 (Outlet)
(ppm)
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
RUN 2, Page 1
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1030
1031
1032
1033
1034
1035
1036
1037
1038
1039
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
THC 1 (Inlet)
(ppm)
30.3
30.2
30.3
30.0
30.0
30.6
30.5
30.3
30.2
30.1
30.3
30.4
30.0
30.6
30.8
30.7
30.6
29.8
29.1
28.8
28.4
28.3
28.2
28.4
26.2
26.6
28.8
29.2
29.8
29.9
30.8
31.0
31.3
31.6
32.0
32.3
32.6
THC 2 (Outlet)
(ppm)
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
24.3
24.6
24.8
24.7
28.9
29.7
25.4
24.4
24.7
24.8
24.9
24.9
25.2
25.4
25.3
RUN 2, Page 2
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
. 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
1141
1142
1143
THC 1 (Inlet)
(ppm)
33.1
33.8
34.2
34.2
34.2
34.4
34.3
33.9
33.5
33.4
32.5
32.2
32.2
32.5
32.6
32.8
33.0
33.2
33.6
33.9
34.1
34.6
35.0
34.9
34.6
35.1
35.2
35,0
35.1
34.9
34.7
34.7
35.0
35.6
36.1
36.7
36.7
THC 2 (Outlet)
(ppm)
25.7
26.8
27.2
27.3
27.2
27.4
27.4
27.1
26.5
26.2
25.6
24.8
25.3
25.6
25.8
25.9
26.3
26.3
26.7
24.9
21.9
18.9
21.1
19.5
19.5
25.0
25.2
25.1
25.1
25.4
26.1
25.1
25.2
25.4
25.8
26.2
26.5
RUN 2, Page 3
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1144
1145
1146
1147
1148
1149
1150
1151
1152
1153
1154
1155
1156
1157
1158
1159
1200
1201
1202
1203
1204
1205
1206
1207
1208
1209
1210
1211
1212
1213
1214
1215
1216
1217
1218
1219
1220
THC 1 (Inlet)
(ppm)
37.1
36.9
37.2
37.3
38.0
38.5
37.9
38.3
38.0
37.9
37.9
37.9
34.6
34.5
38.5
38.2
38.6
38.6
39.4
40.0
40.3
40.1
40.8
40.7
40.1
39.4
39.8
39.5
38.7
37.9
37.4
36.8
36.0
35.9
35.6
34.7
34.8
THC 2 (Outlet)
(ppm)
26.7
26.8
27.0
27.2
27.8
28.5
28.4
28.3
28.2
28.0
28.1
32.8
36.5
37.4
37.9
38.1
38.7
39.3
32.2
29.8
29.1
28.8
29.1
29.3
29.5
29.7
30.2
30.5
30.7
30.5
30.5
30.5
30.7
30.7
30.9
31.2
31.2
RUN 2, Page 4
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time THC 1 (Inlet) THC 2 (Outlet)
(24 hour) (ppm) (ppm)
1221 40.6 31.5
1222 43.8 25.0
1223 44.0 33.6
1224 44.0 38.7
1225 44.4 35.5
1226 17.7 33.9
1227 43.9 33.8
1228 44.8 33.8
1229 43.6 33.7
1230 42.7 33.9
1231 42.9 35.0
1232 42.0 36.2
1233 Analyzers off line Analyzers off line
1234 Filter Change Port Change
1235
1236
1237
1238
1239
1240
1241
1242
1243
1244
1245
1246
1247
1248
1249
1250
1251
1252
1253
1254
1255
1256
1257
RUN 2, Page 5
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1258
1259
1300
1301
1302
1303
1304
1305
1306
1307
1308
1309
1310
1311
1312
1313
1314
1315
1316
1317
1318
1319
1320
1321
1322
1323
1324
1325
1326
1327
1328
1329
1330
1331
1332
1333
1334
THC 1 (Inlet)
(ppm)
51.4
50.6
50.0
52.3
53.0
52.7
52.9
53.6
53.2
51.8
52.4
52.5
52.4
51.9
51.0
50.4
49.9
49.9
49.6
48.8
48.1
47.4
47.0
46.4
46.0
45.7
45.8
45.9
45.5
45.0
44.8
44.4
THC 2 (Outlet)
(ppm)
38.4
38.9
38.6
38.3
27.7
29.9
30.8
31.0
30.4
29.2
29.2
29.2
29.2
28.8
28.5
28.1
27.6
27.5
27.2
26.8
26.3
26.0
25.7
25.6
25.3
25.2
25.3
25.2
25.0
24.8
24.5
24.3
RUN 2, Page 6
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
THC 1 (Inlet)
(ppm)
44.2
43.8
43.4
42.8
42.8
42.6
42.7
42.4
41.9
41.7
41.6
41.6
41.3
40.9
40.5
40.2
39.8
39.8
36.8
32.7
35.5
35.1
37.5
30.7
35.8
36.9
37.6
37.5
36.9
36.7
36.7
35.9
35.8
36.3
36.5
36.4
36.5
THC 2 (Outlet)
(ppm)
24.1
24.0
24.4
27.9
27.8
27.8
27.8
27.9
27.5
27.3
27.5
27.4
27.3
26.9
26.8
26.5
26.2
26.2
26.1
26.2
26.1
25.8
25.7
25.6
25.6
25.4
25.5
25.3
25.1
25.0
25.1
25.0
24.9
25.5
25.4
25.3
25.2
RUN 2, Page 7
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1441
1442
1443
1444
1445
1446
1447
1448
THC 1 (Inlet)
(ppm)
36.8
37.1
37.1
37.1
37.2
37.0
37.7
37.6
37.7
37.3
37.0
36.9
36.7
36.6
36.0
36.0
36.5
36.7
37.8
39.7
40.0
40.3
40.8
41.2
41.4
41.5
41.8
41.9
41.5
41.3
41.6
41.4
41.7
41.9
42.0
42.1
42.5
THC 2 (Outlet)
(ppm)
25.3
25.6
25.6
25.6
25.7
25.7
26.2
26.2
26.2
26.0
25.6
25.6
25.3
25.5
25.1
25.0
24.9
24.7
25.0
24.3
20.6
21.6
22.8
22.6
22.6
22.3
22.3
22.4
22.2
22.0
23.2
23.0
23.2
Analyzer off line
23.9
24.0
23.3
RUN 2, Page 8
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1515
1516
1517
1518
1519
1520
1521
1522
1523
1524
1525
THC 1 (Inlet)
(ppm)
42.2
41.6
41.3
41.1
40.5
40.1
40.0 .
39.6
39.2
39.0
38.9
38.8
38.8
39.3
39.4
39.5
38.9
27.1 A
33.0 A
31.7 A
31.2 A
31.0 A
30.5 A
30.3 A
29.7 A
29.3 A
28.9 A
29.0 A
28.7 A
28.2 A
29.7 A
31.4 A
31.4 A
31.5 A
31.3 A
31.4 A
31.5 A
THC 2 (Outlet)
(ppm)
24.0
26.8
26.7
26.6
26.3
26.1
26.1
26.1
25.8
25.9
25.7
25.8
25.7
26.1
26.3
26.5
26.4
26.5
26.5
26.4
26.2
26.4
26.3
26.4
26.3
26.1
24.7
25.0
25.1
25.2
25.0
25.0
25.1
25.1
25.2
25.2
25.5
RUN 2, Page 9
-------
LTV
Run 2
Date: 6/26/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
1526
1527
1528
1529
1530
1531
1532
1533
1534
1535
1536
Minimum=
Maximum=
THC 1 (Inlet)
(ppm)
31.3 A
31.0 A
30.8 A
30.6 A
30.5 A
30.4 A
30.5 A
30.6 A
30.6 A
32.1 A
37.2
17.7
53.6
THC 2 (Outlet)
(ppm)
25.6
25.5
25.7
25.3
25.4
25.2
25.6
25.9
26.0
26.1
25:2
18.9
39.3
Average= 37.3 27.0
A -Sample flow drop due to filter plugging. Data not used in run average
RUN 2, Page 10
-------
60
THC Concentrations vs. Time (Run 2,6/26/97)
THC (Inlet) (ppm) -a- THC (Outlet) (ppm)
50
40
Q.
Q.
<-^
U
E
30
20
10
0
9:30
10.30
11:30
12:30
13.30
14:30
15:30
Time
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24hour)
835
836
837
838
839
840
841
842
843
844
845
846
847
848
849
850
851
852
853
854
855
856
857
858
859
, 900
901
902
903
904'
905
906
907
908
909
910
911
912
913
914
915
916
917
918
919
920
921
922
923
924
THC 1 (Inlet)
(Ppm)
28.2
27.7
27.3
27.5
27.4
27.1
26.8
26.8
26,9
27.0
27.5
26.8
27.8
28.3
28.1
28.0
28.4
28.2
28.2
28.3
28.3
27.6
27.3
27.8
N 27.9
28.0
28.3
28.0
27.8
27.5
27.4
27.0
26.3
26.6
26.9
26.3
26.1
25.9
25.5
25.0
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
THC 2 (Outlet)
(Ppm)
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
24.1
23.9
24.0
24.2
24.2
24.4
24.2
23.8
23.4
23.2
RUN 3, Page 1
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24hour)
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
1002
1003
1004
1005
1006
1007
1008
1009
1010
1011
1012
1013
1014
THC 1 (Inlet)
(Ppm)
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
20.8
20.6
20.5
20.2
20.0
19.7
19.7
19.6
19.4
18.7
19.0
19.0
18.9
18.6
18.4
18.3
18.2
18.6
18.3
18.2
18.8
26.0
27.5
27.9
27.9
28.1
28.2
28.7
THC 2 (Outlet)
(Ppm)
23.1
23.3
23.1
23.7
23.7
23.7
23.7
23.8
23.7
23.8
23.6
23.7
24.1
24.4
24.5
24.4
24.4
24.5
24.3
24.5
24.4
24.0
18.4
19.6
19.9
19.0
18.8
18.6
18.7
18.7
18.5
18.5
18.4
18.5
18.3
18.2
18.1
18.0
18.0
18.3
18.4
18.7
18.9
21.0
21.8
21.9
21.7
21.7
21.7
21.9
RUN 3, Page 2
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1053
1054
1055
1056
1057
1058
1059
1100
1101
1102
1103
1104
THC 1 (Inlet)
(PPm) .. .
28.4
28.3
28.2
27.8
26.3
***
*-*•*
***
27.8
27.5
27.3
27.3
27.0
26.8
26.8
26.7
26.5
26.6
26.2
26.0
26.6
27.4
28.0
28.2
27.3
27.1
27.3
273
27.0
26.5
26.6
26.8
28.4
299
29.7
29.4
33.8
34.9
Filter Change
38.7
40.2
41.0
41.7
42.2
40.9
36.3
35.1
34.4
34.3
33.4
THC 2 (Outlet)
. (PPm)
22.0
21.7
21.5
23.0
24.9
24.7
24.6
24.5
23.9
23.7
23.6
23.3
23.0
22.6
22.5
22.6
22.4
22.5
22.3
22.5
22.9
23.3
23.9
24.3
24.5
24.6
24.9
25.0
25.0
25.1
25.1
25.4
25.1
25.1
25.1
25.0
25.0
23.7
19.1
21.7
21.8
21.6
21.8
21.7
22.3
24.6
24.6
24.9
25.2
25.2
RUN 3, Page 3
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24 hour)
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
1141
1142
1143
1144
1145
1146
1147
1148
1149
1150
1151
1152
1153
1154
THC 1 (Inlet)
(ppm).
32.9
32.6
***
***
***
***
»**
***
#**
***
29.4
29.6
29.6
29.7
29.0
28.6
28.8
28.5
28.6
28.4
28.1
28.6
28.8
28.9
28.8
28.6
28.1
29.2
29.8
28.8
28.4
27.8
27.2
27.5
28.3
27.9
28.5
30.7
30.9
29.8
30.7
30.6
31.4
30.8
30.8
30.7
31.2
31.0
30.8
31.0
THC 2 (Outlet)
(PPM .
24.6
Port Change
24.4
26.7
26.6
26.2
25.6
24.8
25.2
25.2
25.0
24.9
24.9
24.6
24.2
25.3
25.4
25.3
25.2
25.5
25.8
26.0
25.6
25.3
25.6
RUN 3, Page 4
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24hour)
1155
1156
1157
1158
1159
1200
1201
1202
1203
1204
1205
1206
1207
1208
1209
1210
1211
1212
1213
1214
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
1241
1242
1243
1244
THC 1 (Inlet)
(ppm)
30.6
30.8
30.8
30.5
30.2
30.1
29.7
29.7
29.6
29.0
28.1
28.6
28.5
28.3
28.1
27.6
28.2
27.9
27.8
27.0
***
***
***
**•
**»
*+*
#**
***
***
***
28.0
29.4
30.0
30.6
30.8
30.9
32.0
31.8
31.6
31.1
30.7
30.7
30.9
30.9
30.7
30.0
299
29.3
31.7
33.4
THC 2 (Ou1
(ppm)
26.1
26.0
25.8
25.7
25.5
25.3
25.2
254
25.6
25.6
25.2
25.1
25.2
24.7
24.6
24.5
24.3
24.4
24.4
24.8
25.1
25.5
25.7
25.5
25.4
25.0
24.9
25.0
25.3
25.1
25.0
25.3
25.7
26.2
26.5
26.7
27.1
27.6
27.6
27.6
27.2
27.2
27.3
269
26.9
26.9
26.6
26.5
26.7
26.7
RUN 3, Page 5
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time
(24hour)
1245
1246
1247
1248
1249
1250
1251
1252
1253
1254
1255
1256
1257
1258
1259
1300
1301
1302
1303
1304
1305
1306
1307
1308
1309
1310
1311
1312
1313
1314
1315
1316
1317
1318
1319
1320
1321
1322
1323
1324
1325
1326
1327
1328
1329
1330
1331
1332
1333
1334
THC 1 (Inlet)
(ppm)
33.2
33.0
37.6
38.2
38.1
39.2
38.3
37.9
37.8
37.4
37.0
36.8
36.3
36.6
37.4
38.0
38.4
39.3
40.0
40.6
41.5
42.5
42.8
43.4
44.1
44.7
44.8
47.0
43.5
42.1
42.0
43.0
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
THC 2 (Outlet)
(ppm)
t.T. 17.... ./.
26.6
27.1
26.3
25.6
23.1
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
Outlet Spike
27.7
28.2
28.3
28.2
28.9
28.8
29.1
29.1
292
29.1
29.5
29.5
29.7
29.9
30.3
31.1
31.5
RUN 3, Page 6
-------
LTV
Run 3
Date: 6/27/97
Project No. : 3802-20-04-03-01
Operator: Gulick
Time THC 1 (Inlet) THC 2 (Outlet)
(24 hour)
31.7
31.7
31.3
30.8
30.2
29.3
28.4
27.6
27.1
26.9
26.5
26.7
Minimum= 18.2 18.0
Maximum= 47.0 31.7
Average= 29.8 24.6
*** Sample flow fluctuation due to FTIR cell filling.
Data point not used in average
1335
1336
1337
1338
1339
1340
1341
1342
1343
1344
1345
1346
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
Inlet Spike
RUN 3, Page 7
-------
50
THC Concentrations vs. Time (Run 3,6/27/97)
THC (Inlet) (ppm)
THC (Outlet) (ppm)
40
30
B
a.
o.
•^
U
m
20
10
0
8:00
9:00
10:00
11:00
12:00
13:00
14:00
Time
-------
A-2 METHOD 25A CALIBRATION AND QA CHECK DATA
-------
Calibration Error Determination For 6/25/97
CalGa* Measured Difference as Pass/Fail
Valu« Value %ofCalGas
THC1 0.0 0.2 02 Pass
Inlet 90.4 90.8 0^4 Pass
50.4 50.2 0.4 pass
35-2 35.4 0.6 Pass
THC2 0.0 0.3 0.3 Pass
Outlet 90.4 90.8 0.4 Pass
50.4 50.0 0.8 Pass
35.2 34.5 2.0 pass
Pass/Fail Criteria is +/- 5% of Calferation gas.
Calibration Drift Determination for 6/25/97
Zero Drift
Initial Final Difference as Pass/Fail
Value Value % of Span
THC1 0.2 1.2 1.0 Pass
Inlet
THC2 0.3 -0.4 0.7 Pass
Outlet
Instrument Span for THC 1 and THC 2 is 100 ppov
Pass/Fail Criteria is +/- 3% of Instrument Span.
Span Drift
Initial Final Difference as Pass/Fail
Value) Value % of Span
THC1 90.8 90.2 0.6 Pass
Inlet
THC 2 90.8 91.7 0.9 Pass
Outlet
strument Span for THC 1 and THC 2 is 100 ppm.
Pass/Fa! Criteria is +/- 3% of Instrument Span.
-------
Calibration Error Determination For 6/26/97
CalGas Measured Difference as Pass/ Fail
Value %ofCalGas
THC1 0.0 0.1 0.1 Pass
In'et 90.4 91.2 0.9 Pass
50.4 49.8 1.2 Pass
35.2 34.3 2.6 Pass
THC2 0.0 0.2 0.2 Pass
Outlet 90.4 91.3 1.0 Pass
50.4 50.0 0.8 Pass
35.2 34.3 2.6 Pass
Pass/Fay Criteria is +/- 5% of Calfcration gas.
Calibration Drift Determination for 6/26/97
Zero Drift
Initial Final Difference as Pass/Fail
Value Value % of Span
THC1 0.1 -1.0 1.1 Pass
Inlet
THC2 0.2 0.6 0.4 Pass
Outlet
Instrument Span for THC 1 and THC 2 is 100 ppm.
Pass/Fail Criteria is +/- 3% of Instrument Span.
Span Drift
Initial Final Difference ae Pass/Fail
Value Value % of Span
THC1 91.2 88.4 2.8 Pass
Inlet
THC 2 91.3 91.0 0.3 Pass
Outlet
strument Span for THC 1 and THC 2 is 100 ppm.
Pass/Fail Criteria is +/- 3% of Instrument Span.
-------
Calibration Error Determination For 6/27/97
Cal Ga* Measured Difference as Pass) Fail
Value value % of Cal Gas
THC1 0.0 0.1 0.1 pass
Inlet 90.4 91.0 0.7 Pass
50.4 50.5 0.2 Pass
35.2 35.0 0.6 Pass
THC2 0.0 0.2 0.2 Pass
Outlet 90.4 91.6 1.3 Pass
50.4 50.8 0.8 Pass
35.2 35.2 0.0 Pass
Pass/Fail Criteria is +/- 5% of Calfcration gas.
Calibration Drift Determination for 6/27/97
Zero Drift
Initial Final Difference as Pass/Fail
Value Value % of Span
THC1 0.1 2.4 2.3 Pass
Inlet
THC2 0.2 0.9 0.7 Pass
Outlet
Instrument Span for THC 1 and THC 2 is 100 pom.
Pass/Fail Criteria » +/- 3% of Instrument Span.
Span Drift
Initial Final Difference as Pass/Fail
Value Value % of Span
THC1 91.0 90.2 0.8 Pass
Inlet
THC 2 91.6 91.1 0.5 Pass
Outlet
istrument Span for THC 1 and THC 2 is 100 ppm.
Pass/Fan Criteria is +/- 3% of Instrument Span.
-------
Response Times
20
-------
A-3 VOLUMETRIC FLOW DATA
-------
A-3 VOLUMETRIC FLOW DATA
-------
-97
auiiuy.
Date:
.ocatlon:
lun Number
Sample Type:
iiv tasiuitcago
e/26/97
Outlet
1
Dloxin
btal Sampling Time (min)
Corrected Barometric Pressure (In Hg)
Absolute Stack Pressure (In H2O)
Stack Static Pressure (In H2O)
Average Stack Temperature (*F)
Stack Area (aq in)
Actual Meter Volume (eu ft)
Average Meter Pressure (Hi H2O)
Average Meter Temperature (*F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
5ry Gas Meter Factor
Nozzle Diameter (in)
Pltot Constant
Average Sampling Rate (dscfm)
Standard Metered Volume (dscf)
Standard Metered Volume (dscm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity (fpm)
Stack Gas Velocity (mpm)
Volumetric Flow Rate (acfrn)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dacfm)
Volumetric Flow Rate (decmm)
Percent Isokinette
Percent Excess Air
Concentration (g/dscm)
Concentration (kg/hr)
Concentration (ppmv)
Emissions (Ib/hr)
240.0
29.18
29.31
1.80
117.46
16286.02
160.748
0.81
93.02
388.80
3.5
17.5
79.0
0.9960
0.217
0.84
0.622
149.293
4.228
10.94
0.891
29.26
28.03
2908.67
886.56
328962.48
9316.22
262438.55
7432.26
104.38
519.01
0.00
0.00
0,00
0.00
-------
5EN
'ESN S£5c.-RC:-i 'jRCUPMO- 3-3"
3:17PM
acility.
Date:
.ocation:
Run Number.
Sample Type:
LTV East bhicago
6/26/97
Outlet
2
Dtexin
Total Sampling Time (mln)
(Directed Barometric Preaaura (in Hg)
Absolute Stack Praaaure (in H2O)
Stack Static Praaaure (In H20)
Average Stack Temperature (T)
Stack Area (aq In)
Actual Meter Volume (cu ft)
Average Meter Pressure (in H2O)
Average Meter Temperature (*F)
Moisture Coflected (g)
arbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Mrtrogen Concentration (%V)
Dry Oaa Meter Factor
Nozzle Diameter (In)
Prtot Constant
Average Sampling Rate (decfm)
Standard Metered Volume (dacf)
Standard Metered Volume (dscm)
Stack Moisture (HV)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gaa Velocity (fpm)
Stack Gaa Velocity (mpm)
Volumetric Flow Rate (acfrn)
Volumetric Flow Rate (scmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (decmm)
Percent laokinetic
Percent Excess Air
Concentration (g/dacm)
Concentration (kg/hr)
Concentration (ppmv)
flb/hr)
240.0
29.35
29.36
0.18
117.33
16286.02
158.400
0.81
88.17
394,70
3.5
17.5
79.0
0.9960
0.217
0.84
0.623
149.562
4.236
11.07
0.689
29.26
28.01
2932.41
893.80
331647.78
9392.26
264711.06
7496.62
103.67
519.01
0.00
0.00
0.00
0.00
-------
3 30
acilky:
Date:
ocation:
Run Number
Sample Type:
LTV East Chicago
8/27/97
Outlet
3
Dkudn
Total Sampling Time (min)
Directed Barometric Preaeure (in Hg)
Absolute Stack Pressure (In H2O)
Stack Static Preaaure (In H2O)
Average Stack Temperature (*F)
Stack Area (aq In)
Actual Meter Volume (cu ft)
Average Meter Preaaure (In H2O)
Average Meter Temperature (*F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gaa Meter Factor
Nozzle Diameter (in)
Pttot Constant
Average Sampling Rate (dscfm)
Standard Metered Volume (dacf)
Standard Metered Volume (dsem)
Stack Molature (%V)
Mole Fraction Dry Stack Gaa
Dry Molecular Weight
Wet Molecular Weight
Stack Gaa Velocity (fpm)
Stack Gaa Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Row Rate (acmm)
Volumetric Flow Rate (dacfrn)
Volumetric Flow Rate (dtcmm)
Percent laoklnette
Percent Exceaa Air
Concentration (g/dacm)
Concentration (kg/hr)
Concentration (ppmv)
Emissions (Ib/hr)
240.0
29.40
29.41
0.18
115.29
18288.02
183.075
0.83
98.60
388.20
3.5
17.5
79.0
0.9980
0.217
0.84
0.831
151.351
4.288
10.29
0.897
29.28
28.10
2985.93
904.02
335439.29
9499.84
271494.08
7888.71
102.29
519.01
0.00
0.00
0.00
0.00
-------
^•z^-j-t-'.':-
3 3 w ' ' ' j „ „ .,
Facility:
BQIS,
.ocatlon:
Number.
Sample Type
Outlet
1
Multi metal*
Total Sampling Time (mln)
orrected Barometric Pressure (in Hg)
Absolute Stack Pressure (In H2O)
Stack Static Pressure (in M2O)
Average Stack Temperature (*F)
Stack Area (sq In)
Actual Meter Volume (cu ft)
Average Meter Pressure (In H2O)
Average Meter Temperature (*F)
Moisture Collected (g)
arbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Nozzle Diameter (In)
Pttot Constant
Average Sampling Rate (dscfm)
Standard Metered Volume (dacf)
Standard Metered Volume (dscm)
Stack Moisture (%V)
Mole Fraction Dry Stack Oaa
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity (fpm)
Stack Gas Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmrn)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dacmm)
Percent laoklnette
Percent Excess Air
Concentration (g/daem)
Concentration (kg/hr)
Concentration (ppmv)
Emissions Hb/hh
240.0
29.18
29.31
1.80
117.50
16288.02
168.707
0.83
92.17
404.40
3.5
17.8
79.0
0.9840
0.217
0.84
0.640
153.538
4.348
11.06
0.890
29.26
28.02
3013.70
918.58
340841.62
9652.63
271558.40
7690.53
103.74
519.01
0.00
0.00
0.00
0.00
-------
acil
Data:
.ocation:
Run Number:
Sample Type:
LTVEasfShi
6/26/97
Outlet
2
Multlmetaia
Total Sampling Time (min)
Corrected Barometric Preeaure (In Hg)
Abaolute Stack Preaaure (in H2O)
Stack Static Preaaure (In H2O)
Average Stack Temperature (*F)
Stack Area (aq In)
Actual Meter Volume (cu tt)
Average Meter Preaaure (In H2O)
Average Meter Temperature (*F)
Moiature Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Qaa Meter Factor
Nozzle Diameter (in)
Pitot Conatant
Average Sampling Rate (dacfm)
Standard Metered Volume (dacf)
Standard Metered Volume (dacm)
Stack Moiature (%V)
Mole Fraction Dry Stack Qaa
Dry Molecular Weight
Wet Molecular Weight
Stack Gaa Velocity (fpm)
Stack Gaa Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dacfm)
Volumetric Flow Rate (dacmm)
Percent laokinetto
Percent Exceaa Air
Concentration (g/dacm)
Concentration (kg/hr)
Concentration (ppmv)
Emlaaiona (Ib/brt
240.0
29.35
29.36
0.18
117.83
16286.02
157.579
0.83
91.94
390.00
3.8
17.4
78.9
0.9640
0.217
0.84
0.608
146.035
4.136
11.18
0.888
29.30
28.03
2984.84
909.78
337576.99
9560.18
268654.67
7613.96
99.66
506.97
0.00
0.00
0.00
0.00
-------
5c,\T
i = 5 £..
3?M
3' 3 5"";; 5:; s'
acii
Date:
Location:
Run Number
Sample Type:
LTV East Chicago
6/27/97
Outiec
3
Muffl metals
Total Sampling Time (mln)
Corrected Barometric Pressure (In Hg)
Absolute Stack Pressure (In H2O)
Stack Static Pressure (In H2O)
Average Stack Temperature (*F)
Stack Area (sq In)
Actual Meter Volume (cu ft)
Average Meter Pressure (In H2O)
(Average Meter Temperature (*F)
(Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Oas Meter Factor
Nozzle Diameter (In)
Pttot Constant
Average Sampling Rate (dscfm)
Standard Metered Volume (dscf)
Standard Metered Volume (deem)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity (fpm)
Stack Gas Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (scnvn)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isoklnetle
Percent Excess Air
Concentration (g/dsem)
Concentration (kg/hr)
Concentration (ppmv)
Emissions Hb/hh
240.0
29.40
29.41
0.18
116.46
16286.02
160.530
0.83
100.27
369.60
3.3
18.8
88.0
0.9840
0.217
0.84
0.612
-148.795
4.157
10.61
0.894
32.07
30.58
2865.84
873.51
324119.17
9179.06
260862.30
7387.62
103.25
418.70
0.00
0.00
0.00
0.00
-------
afiilityi
Date:
.ocatlon:
Number
Sample Type:
LWEail Chicago
6/25/97
Inlet
1
Muffl metals
fotal Sampling Time (mln)
Corrected Barometric Pressure (In Hg)
Absolute Stack Pressure (In H20)
Stack Static Pressure (in H2O)
Average Stack Temperature (*P)
Stack Area (sq in)
Actual Meter Volume (cu ft)
Average Meter Pressure (In H2O)
Average Meter Temperature ("F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Mozzie Diameter (in)
Pitot Constant
Average Sampling Rate (dtcfm)
Standard Metered Volume (dscf)
Standard Metered Volume (dscm)
Stack Moisture (%V)
Mole Fraction Dry Stack Gas
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity (fpm)
Stack Gas Velocity (mpm)
Volumetric Flow Rata.(acfm)
Volumetric Flow Rate (ecmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic
Percent Excess Air
Concentration (g/dscm)
Concentration (kg/hr)
Concentration (ppmv)
Emissions (Ib/hrt
240.0
29.36
28.95
-5.60
222.04
8190.00
67.248
1.66
92.08
93.20
2.5
19.0
88.5
0.9840
0.103
0.84
0.259
62.194
1.761
6.60
0.934
31.96
31.04
6236.47
1900.88
354699.39
10045.09
248105.45
7026.36
102.66
433.62
0.00
0.00
0.00
0.00
im mm*
-------
SEN
;', > 3-3'"
acility:
Date:
.ocatlon;
Run Number
Sample Type:
LTVlast Chicago
8/26/97
Total Sampling Time (mln)
Corrected Barometric Preaaure (in Hg)
Abaolute Stack Preaaure (in H2O)
Stack Static Pmaaure (in H2O)
Average Stack Temperature (*F)
Stack Area (aq In)
Actual Meter Volume (cu ft)
Average Meter Preaaure (In H2O)
Avenge Meter Temperature (*F)
Moiature Collected (g)
arbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nitrogen Concentration (%V)
Dry Gaa Meter Factor
Nozzle Diameter (in)
Pitot Constant
Average Sampling Rate (dacfm)
Standard Watered Volume (dscf)
Standard Metered Volume (dacm)
Stack Moiature (%V)
Mole Fraction Dry Stack Gaa
Dry Molecular Weight
Wet Molecular Weight
Stack Gaa Velocity (fpm)
Stack Gaa Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dacfm)
Volumetric Flow Rate (dacmm)
Percent iaokinetic
Percent Exceaa Air
Concentration (g/dacm)
Concentration (kg/hr)
Concentration (ppmv)
fto/hrt
240.0
29.46
29.04
-5.60
222.63
8190.00
68.915
1.62
93.31
98.60
3.3
18.8
88.0
0.9840
0.103
0.84
0.266
63.785
1.806
6.79
0.932
32.07
31.11
6057.63
1846.33
344521.82
9756.86
241027.11
6825.89
108.38
416.70
0.00
0.00
0.00
0.00
-------
SENT BY:EASTERN RESEARCH GROUP:10- 8-97 ; 5=20PM
9194611579-
91967700651*21
acility:
Date:
.ocation:
n Number:
Sample Type:
LTV East Chicago
6/27/97
Inlet
3
Mum metals
Total Sampling Time (mln)
Corrected Barometric Pressure (in Hg)
Absolute Stack Pressure (in H2O)
Stack Static Pressure (in H2O)
Average Stack Temperature (*F)
Stack Area (aq In)
Actual Meter Volume (cu ft)
Average Meter Pressure (In H2O)
Average Meter Temperature (*F)
Moisture Collected (g)
Carbon Dioxide Concentration (%V)
Oxygen Concentration (%V)
Nittrogen Concentration (%V)
Dry Gaa Meter Factor
Nozzle Diameter (in)
Pltot Constant
Average Sampling Rate (dscfm)
Standard Metered Volume (dsct)
Standard Metered Volume (deem)
Stack Moisture (%V)
Mole Fraction Dry Stack Oaa
Dry Molecular Weight
Wet Molecular Weight
Stack Gaa Velocity (fpm)
Stack Gaa Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (decmm)
Percent laoklnetic
Percent Exoeaa Air
Concentration; (g/dacm)
Concentration (kg/hr)
Concentration (ppmv)
Emiaaiona (Ib/hr)
240.0
29.51
29.10
-5.60
198.00
8190.00
67.276
1.68
96.88
96.60
3.3
18.8
88.0
0.9840
0.103
0.84
0.259
62.045
1.757
6.84
0.932
32.07
31.11
6181.78
1884.21
351688.97
9957.00
255583.34
7238.12
99.42
416.70
0.00
0.00
0.00
0.00
-------
APPENDIX B
FTIRDATA
-------
B-l FTIR FIELD DATA RECORDS
-------
LTV STEEL COMPANY INC.
Date
6/23/97
6/24/97
6/25/97
Time
16:48-16:49
13:33-13:59
14:00-14:58
15:03-15:41
16:03-16:25
16:29-16:44
8:27-9:15
9:27-10:03
10:15-10:30
10:30
10:33-10:46
10:48-10:51
11:11-11:29
11:32-11:47
12:06-12:07
12:06-12:07
12:17-12:34
12:36-12:50
12:53-13:05
13:09-13:21
13:21-13:40
13:34-13:37
13:38-13:39
13:40
13:47-13:55
13:58-14:12
14:16-14:31
14:35-14:50
14:54-15:09
15:05
15:12-15:46
15:15
15:17
15:33
15:49-16:07
16:10-16:25
16:31-16:47
16:52-16:57
17:02-17:27
17:34-18:03
18:05
Location
nlet
nlet
nlet
Outlet
nlet
nlet
Outlet
Inlet
Outlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Inlet
Inlet
Outlet
Outlet
Inlet
Outlet
Inlet
Inlet
Outlet
Spiked
X
X
X
X
X
X
LJnspiked
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Event/Notes
Ambient Sample
n inlet but from outlet
Port change
Filter change/ Analyzers off line
Filter change/Analyzers off line
Port change
Filter change
Leak check
Leak check
Port change
Changed glass wool plug at inlet
THC flame out/system check
THC off line/system check
Nitrogen purge
-------
LTV STEEL COMPANY INC.
Date
6/26/97
6/27/97
Time
9:09-9:41
9:53-10:51
10:55-11:25
11:29-11:55
11:57-12:21
12:24-12:32
12:33
12:33-12:34
12:33-12:34
12:35-13:05
13:08-13:33
13:39
14:00-14:30
14:45
14:33-15:03
15:07-15:35
15:39-15:51
15:59-16:33
16:44-17:22
8:35-9:14
9:15-9:46
9:40
9:49-10:18
10:21-10:51
10:53
11:06
11:07-11:42
11:44-12:14
12:16-12:45
12:25
12:49-12:50
12:50-13:17
13:17-13:46
Location
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Outlet
Outlet
Inlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Outlet
Inlet
Spiked
X
X
X
X
X
X
X
X
X J
X
Unspiked
X
X
X
X
X
X
X
X
X
X
X
X
Event/Notes
Port change
Analyzers off line/filter change
Analyzers off line/filter change
Take new background
Analyzer off line
Port change
Start outlet process software
Filter change
Filter change
Port change
-------
PROJECT NO.47Bl-OI.il
PLANT: LTV
FTIR FIELD DATA FORM
(FTIKStmfliitgDult)
DATE: t/13-14/1997
BAROMETRIC:
OPERATOR: Geter
SAMPLE
TIME
16:48-16:49
6/24/97
11:33-13:34
12:57-12:58
14:00
14.02-14:03
14:05-14:06
14:08 14:09
14:11
14:16-14:17
14:23-14:24
14:28-14:29
14:30
14:35-14:36
14:39-14:41
14:43-14:44
14:46
14:51-14:52
14:54-14:55
14:57-14:58
FILE
NAME
INLAOOOOI
1NLA1001
1 NLA 1002
INLSI003
INLSI004
1NLSI005
1NLSI006
INLS1007
INLSI008
INLSI009
INLSI010
INLSIOI1
INLSIOI2
INLSI013
INLSIOI4
PATH
36 puses
36 puses
36 puses
36puje>
36 puses
36 puses
36 panel
36 puses
36 puses
36 passes
36 puses
36 puses
36 puses
36 puses
36 puses
Ambient umple hoe 2/falet Line 2 check
Ambient air line 2/tnle< may be contaminated
w/ 25 A propane cal
Ambient air spike hoe open
Synchronized nine with HC analyzers
Probe @ inlet SF6 spike @ 1 Ipm
spiked w/SF6@ 1.00 Ipm 4ppmSF6
Spiked probe out of slack
Spiked probe ou of suck
Started toluene (121 ppm) spike <§> 1.0 Ipm
Toluene @ 1.0 Ipm
Toluene @ 1.0 Ipm
Toluene <3 1.0 Ipm
Turned toluene How (spike) to 2.00 Ipm
Toluene spike @ 2.00 Ipm
Toluene spike @ 2.00 Ipm
Toluene spike @ 2.00 Ipm
Turned on SF6 spike @ 14:46
SF6 spike @ 1.95 Ipm
SF6 spike @ 1.95 Ipm
SF6 spike @ 1.95 Ipm
NUMBEB
SCANS
50
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
BES
(cai-l>
1
1
CELL
TEMP(F)
121 C
121C
I2IC
I2IC
I2IC
I2IC
J2IC
I2IC
I2IC
I2IC
121C
SPIKED/
UNSHKED
Ambient
Ambient
in slack
S
S
S(tol)
S(iol)
S(tol)
S(tol)
S(lol)
S(SF6)
S(SF6)
S(SP6)
SAMPLE
COND.
SAMPLE
FLOW
138*2
138
138
137
140
140
140
140
140
140
140
140
140
140
BUG
623A
624B
624 B
624B
624B
624B
624 B
624 B
624B
624 B
624B
624B
624B
624B
-------
PROJECT NO.4701-08-II
PLANT:
FTIR FIELD DATA FORM
(FT1K Sam/timf DaU)
DATE:
6/J4/97
BAROMETRIC:
OPERATOR: Gtyer
SAMPLE
TIME
15:03
15:10-15:12
15:14-15:16
15:19-15:21
15.24
15.31-15.33
15:35-15:37
15:37-15:41
15:45
16:03 16.04
16:10-16:12
16:18-16:20
16:23-16:25
16:29-16:31
16:33-16:35
16:37-16:39
16:42-16:44
FILE
NAME
OUTS 1001
OUTS1002
OUTS 1003
OUTS1004
OUTS1005
OUTS1006
INLV10I4
INLV10I5
1NLV1016
INLV1017
INLV1018
INLVIOI9
INLV1020
INLVI021
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
SP6 to outlet @ 2.00 Ipm
SP6 spike® 2.001pm
SK spike® 2 00 1pm
SP6 spike® 2.00 1pm
toluene out @ 2 Ipm
toluene out @ 2 Ipm
toluene out @ 2 Ipm
toluene out ® 2 Ipm
Spike off
Inlet unspiked
Inlet unspiked
Inkl unspiked
Intel unspiked
Outlet unspiked
Outlet uospiked
Outlet unspiked
Outlet unspiked
The previous four were stored in the inlet
directory but are from the outlet
No official run today 6/24
NUMBER
SCANS
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
RES
-------
PROJECT NO. 47»1-0»11
PLANT:
FTIR FIELD DATA FORM
(FTIR Sampling D*a)
DATE:
6/25/97
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
8:27
8:378:40
8:42-8:45
8:48-8:51
8:52
8:52
8:59-9:01
9:04-9:07
9:10-9.12
9:15
9:15
9:23-9:25
9:289:331
9:349:36
9:389:41
9:43
9:43
9:50-9:53
9:55-9:58
10.00-10.02
10:09
10.15
10:19-10:20
10:23-10:25
10:28-10:30
10:33 10:35
10:37-10:39
10:40-10:42
10:44-10:46
10:48 10:51
FILE
NAME
OUTS2001
OUTS2002
OUTS2003
OUTS2004
OUTS2005
OUTS2006
INS2001
INS2002
INS2003
INS2004
1NS2005
INS2006
INS2007
OUTU2007
OUTU2008
OUTU2009
OUTU2010
INU2008
INU2009
INU2010
INU2011
OUTU2011
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passe*
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
Outlet SF6 spike flow @ 21pm
Outlet SF6 spike flow @ 21pm
Outlet SF6 spike flow @ 21pm
Outlet SF6 spike flow @ 21pm
Stop spike SF6
Oudel lolueoe spike @ 21pm
Outlet toluene spike @ 21pm
Outlet toluene spike @ 21pm
Oudel toluene spike @ 21pm
finish outlet spike
inlet toluene spike @ 2 Ipm
iolel toluene spike @ 2 Ipm
inlet toluene spike <§> 2 Ipm
inlet toluene spike @ 2 Ipm
inlet toluene spike @ 2 Ipm
finish toluene spike
inlet SF6 spike flow <3> 21pm
inlet SF6 spike flow @ 21pm
inlet SF6 spike flow @ 21pm
inlet SF6 spike flaw @ 21pm
Continuous flow through outlet
Outlet unspiked
Outlet unspiked
Outlet unspiked
Outlet unspiked
Inlet unspiked sample
Inlet unspiked sample
Inlet unspiked sample
Inlet unspiked sample
Oudel sample
NUMBER
SCANS
50
50
50
SO
50
50
50
SO
SO
SO
SO
SO
SO
50
50
50
50
50
50
50
SO
50
US
<ۥ-!)
1
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
121
SPDtEIV
UNSPIKED
s
s
s
s
s
s
s
s
s
s
s
s
s
s
s
u
u
u
u
u
u
u
u
u
SAMPLE
COND.
SAMPLE
PLOW
105
107
107
107
107
107
107
107
85
140
140
140
140
140
140
100
100
100
100
120
120
85
70
100
BKO
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
-------
FTIR FIELD DATA FORM
PROJECT NO. 4701-M-11
PLANT: LTV
(FTIKSamfUxgDa*)
DATE: 6Q5/97
BAROMETRIC:
OPERATOR:
/ 6
SAMPLE
TIME
10:57-10:59
11:01 11:03
11:0511:08
11 11 11:13
11.16-11.18
11:21-11:23
11.27-11:29
11:32-11:34
11:37-11:39
11:41-11:43
11:45-11:47
12:10
12:17-12:20
12:24-12:25
12:28-12:30
12:32 12:34
12:36-12:38
12.41 12.43
12:45-12:46
12.48-12.50
12:53-12:54
12:57-12:58
13:01 13:02
13:04-13:05
13:09-13:10
13:12 13:14
13:16-13:17
13:20 13:21
13:34
13:34 13.35
13.40
FILE
NAME
OUTU2012
OUTU2013
OUTU2014
INL2012
INL2013
INL2014
INL2015
OUT2015
OUT2016
OUT2017
OUT2018
1NLU2016
1NLU2017
INLU2018
IN1.U2019
OUTU2019
OUTU2020
OUTU2021
OUTU2022
INLU2020
INLU2021
INLU2022
INLU2023
OUTU2023
OUTU2024
OUTU2025
OUTU2026
INLU2024
PATH
36 passes
^36 passes
36 puses
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
Oudet sample
Outlet sample
Outlet sample
Inlet sample
[ales sample
Inlet sample
Inta sample
Outlet sample
Outlet sample
Oudet sample
Outlet sample
Manual runs restarted
Inlet sample (changed plug at inlet - 12:00)
Inlet sample
Inlet sample
Inlet sample
Outlet unspiked sample
Outlet unspiked sample
Outlet unspiked sample
Oudet unspiked sample
Inlet sample
Inlet sample
Inlet sample
Inlet sample
Outlet sample
Oudet sample
Oudei sample
Oudet sample
change plug on inlet probe
Inlet sample
leak check @ outlet probe is good
NUMSU
SCANS
50
50
50
50
SO
50
50
50
50
50
50
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
US
(OB-I)
CELL
TEMP(P)
121C
121C
121C
121C
• 121C
12IC
121C
121C
121C
121C
121C
121C
121C
121C
121C
12IC
121C
121C
121C
121C
121C
121C
121C
121C
121C
121C
SPUED/
UNSMKEO
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
u
SAMPLE
COND.
SAMPLE
PLOW
100
100
100
80
80
75
75
too
100
100
100
140
140
140
140
100
100
100
100
110
110
100
100/90
100
100
100
100
140
140
•KG
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625A
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625B
625C
-------
PROJECT NO. 4701-08-11
PLANT: LTV
FTIR FIELD DATA FORM
(PTIK Samftimg Data)
DATE:
6/15/97
BAROMETRIC: TJV.-T - 1
OPERATOR: £
SAMPLE
TIME
13:47-13:49
13:51-13:52
13:54-13:55
13:58-14:00
14:03-14:04
14:06-14:07
14:10-14:12
14:16-14:17
14:19-14:21
12:24-14:27
14:29-14:31
14:35-14:37
14:40-14:42
1-4:4-1-14:46
14:48-14:50
1-1:54-14:56
14:58 15:00
15:03-15:04
15:07-15:09
15:15
15:12-15:14
15:17-15:19
15:21-15:23
15:25 15:27
15:32-15:34
15:36-15:38
15:40-15:42
15:44-15:46
15:49-15:51
15:54 15:56
16:00-16:02
16:05-16:07
16:10 16:12
16:15 16:16
16:20-16:22
FILE
NAME
INLU2025
1NLU2026
INLU2027
OUTU2027
OUTU2028
OUTU2029
OITTU2030
INLV2028
INLV2029
INLV2030
INLV203I
OUTV203I
OUTV2032
OLTTV2033
OUTV2034
INLV2032
INI.V2033
INLV2034
INLV2035
OUTV2035
OWV2036
OUTV2037
OUTV2038
1NLV2036
INLV2037
INLV2038
INLV2039
OUTV2039
OUTV2040
OUTV204I
OUTV2042
INLV2040
INLV204I
INI.V2042
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
Intel sample
Inlet sample
Inlet sample
Outlet sample
Outlet ample
Outlet sample
Inlet sample
Inlet sample
Inlet sample
Inlet sample
Inlet sample
Outlet sample
Outlet sample
Outlet sample
Outlet sample
Inlet sample
Intel sample
Inlet sample
Inlet sample
Changed Glass wool plug ai inlet
Outlet sample
Outlet sample
Outlet sample
Outlet sample
Intel sample
Inlet sample
Inlet sample
Inlet sample
Outlet sample
Outlet sample
Outlet sample
Outlet sample
Inlet sample
Inlet sample
Inlet sample
NUMBER
SCANS
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
RES
(c»-l>
CELL
TEMP(F)
12IC
121C
I21C
I2IC
12IC
I2IC
I2IC
I2IC
12IC
I2IC
I2IC
I2IC
I2IC
I2IC
I21C
I2IC
I2IC
I2IC
12IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
SPIKED/
UNSPUtED
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
SAMPLE
COND.
SAMPLE
FLOW
140
140
140
95
95
95
95
125
no
110
100
100
100
100
100
85
90
50
50
100
100
100
100
140
140
140
!50*(THCofO
110
110
100
100
120
120
!20THCbatkon
BUG
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
-------
FTIR FIELD DATA FORM
PROJECT NO. 47Ql-Qg-l|
PLANT: LTV
(PTlf Sf
DATE:
BAROMETRIC: 7 f*»'? ' ^ •
OPERATOR: <£• «
SAMPLE
TIME
16:24-16:25
16:31 16:33
16:36-16:38
16:41-16:43
16:45-16:47
16:52-16:54
16:56-16:57
17:02
17:06-17:07
17:08-17:10
17:12-17:13
17:14
17:18 17:19
17:23 17:24
17:26-17:27
17:28
17.34 17.36
17:38-17:40
17:43-17:45
17:48
17:52-17:54
17:56-17:58
18:01-18:03
18:04
18:05
FILE
NAME
INLV2043
OUTU2043
OUTU2044
OimJ2045
OUTU2046
INLU2047
INLU2048
INLS2049
INLS2050
1NLS205I
INLS2052
1NLS2053
INLS2054
OUTS2047
OUTS2048
OUTS2049
OUTS2050
OUTS205I
OUTS2052
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 pastes
Inlet sampfe
Outlet sample
Outlet sample
Outlet sample
Outlet sample
NUMBER
SCANS
50/200
50/200
50/200
50/200
50/200
INLU2044.45.46 were misnamed but were actually outlet spectn
Inlet sample
Inlet simple
SF6 spike on @ 21pm
Mel spiked W/SF6
Inlet spiked w/SF6
Inlet spiked w/SF6
Toluene spike on lo Ihe inlet
Inlel spiked wAoluene 2 Ipm
Inlet spiked wAoluene 2 Ipm
Inlet spiked wAoluene 2 Ipm
Toluene spike lo Ihe outlet @ 2.001pm
Outlet sample
Outlet sample
Outlet sample
Slatted SF6 spike to outlet @ 2.00 Ipm
Outlet sample
Outlet sample
Outlet sample
Slop spike
Nitrogen purge
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
KCS
(C.-I)
1
1
1
1
1
1
1
1
I
1
1
1
1
1
1
1
1
1
1
CELL
TEMP(F)
I2IC
I2IC
I2IC
I2IC
I2IC
I2IC
121C
121C
I21C
12IC
121C
121C
121C
12IC
I2IC
121C
12IC
I2IC
I2IC
•••••Computer time 1 2 hrs behind - files from 6-25 am are logged as from 6/24 pm
SPIKED/
UNSPIKED
U
u
U
u
u
u
u
s
s
s
S(tol)
S(lol)
S(lol)
S(lol)
S(lol)
S(tol)
S(SF6L
S(SF6L
S(SF6)
SAMPLE
COND.
SAMPLE
FLOW
120
95
95
95
95
100
100
140
140
140
143
143
143
110
110
110
no
110
110
110
BKC
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
625C
-------
PROJECT NO.
47tl-0t-ll
FTIR FIELD DATA FORM
BAROMETRIC:
PLANT:
LTV
DATE:
-------
PROJECT NO. 4701-08-11
PLANT: LTV
FTIR FIELD DATA FORM
(FTIR SampliMg Data)
DATE:
6724/97
BAROMETRIC:
OPERATOR:
-l - 7(, 2
J
"*lvi
SAMPLE
TIME
13:08
13:23
13:33
13:39
14:00
14:3"0
14:33
15:03
15:07
15:35
15:39
15:49
15:51
15:53
15:59 16:01
16:05-16:07
16:09-16:11
16:14-16:16
16:17
16:23-16:25
16:27-16.29
16:31-16:33
16:35
16:44-16:47
16:50
16:55-16:58
17:00
17:06-17:09
17:12-17:15
17:17-17:20
FILE
NAME
16260138
16260164
16260165
16260196
16260199
16260231
16260234
16260264
16260268
16260281
INLS3007
INLS3008
INI.S3009
1NLS30IO
INLS301 1
1NLS3012
1NLS30I3
OUTS3009
OUTS3010
OUTS301I
OUTS3012
OUTS3013
OUTS3014
PATH
36 passes
36 pastes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
Outlet sample
Cell pressure - 758
Last outlet sample
Take new background
Inlet sample (start)
Slop inlet
Outlet sample
Slop outlet
Inlet sampk
Inlet slop
Outlet sample *spikc w/ propane for THC cal*
spike w/propane off
Oullel off
toluene spike - inlel
Intel spike - toluene (static)
Inlel spike - toluene (dynamic)
Inlel spike - toluene (static)
Inlel spike - toluene (static)
SF6 spike - inlel
SF6 spike - inlel
SF6 spike - inlel
SF6 spike - inlel
Oullel SF6 spike
Oullel SF6 spike
Oullel SF6 spike
Oullel SF6 spike
Outlet spike toluene 2 Ipm
Oullel spike toluene 2 Ipm
Oullel spike toluene 2 Ipm
Oullel spike toluene 2 Ipm
NUMBER
SCANS
50/200
200
SO
SO
SO
50
SO
SO
SO
SO
SO
so
so
so
so
so
so
so
so
BBS
(c»I)
1
1
1
1
1
CELL
TEMP(F)
me
121C
12IC
121C
121C
121
121
121
121
121
121
121
121
121
121
121
121
121
SPIKE1V
UNSPIKED
U
U
U
U
U
S
S
S
S
S
S
S
S
S
S
S
S
S
SAMPLE
COND.
SAMPLE
FLOW
total=90, cell-SIpm
lotal=IOO,cell~51pm
lexal=70,cell~51pm
lotal=8S,cell~Slpm
lotal=70,ceU~Slpm
not recorded
135
140
140
140
140
140
100
100
100
100
100
100
BltC
626B
626C
626C
626C
626C
626C
-------
FTIR FIELD DATA FORM
PROJECT NO. 4701-OH1
PLANT: LTV
DATE:
BAROMETRIC: 7
-------
PROJECT NO. 47i|-01-|l
PLANT: LTV
FTIR FIELD DATA FORM
(FTIXS*mfliMgData)
DATE:
unin
BAROMETRIC: 7 f I <^
OPERATOR:
4*f r
SAMPLE
TIME
12:45
12:49
12:50
12:54-12:55
12:56-12:58
13:01 13:02
13:03
13:06-13:08
13:11 13:12
13.15 13:16
13:16
13:21-13:22
13:24-13:26
13:27 13:29
13:30
13:35 13:37
13:40-13:41
13:43-13:45
nu
NAME
16270186
16270188
OUTS4007
OUTS4008
OUTS4009
OUTS40IO
OUTS40II
OUTS4012
INL4007
INL4008
INL4009
INL40IO
INL401 1
INL40I2
PATH
36 passe*
36 passes
36 panes
36 pas set
36 passes
36 passes
36puiet
36 puses
36 passes
36 passes
36 pastel
36 passes
36 passes
36 passes
Resun al last port
Sun filling with outlet sample
Rut outlet speOiura
Suited SF6 spike to outlet
Slop continuous monitoring
3uUet sample
Outlet sample
Dutlet isanplf
Suit tofatcne spike to outlet @ 21pm
Outlet sample
Outlet sample
Outlet sample
Sun toluene spike to inlet @ 21pm
Inlet sample
Inlet sample
Inlet sample
Sun SF6 spike to inlet
Inlet sample
Inlet sample
Inlet sample
NUMBU
SCANS
SO/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
50/200
US
(€»•«
1
CELL
TBMP(P)
I2IC
121
121
121
121
121
121
121
121
121
121
121
121
sratEof
uNsnuo
S(SF6)
S(SF6)
S(SF6)
S(tol)
S(tol)
S(tol)
S(u>l)
S(tol)
S(tol)
S(tol)
S(SF6)
S(SF6)
S(SF6)
SAMPLE
COND.
SAMPLE
PLOW
toul=90, cell-5lpm
90
90
90
90
90
90
90
90
90
90
90
85
BUG
-------
LTV Data Sheet for FTIR Sampling.
• Operator
Date
Sample time
File name
Path
Location/Notes
Oscans
Res (cm-1
Cell Temp (F
Spk/Unsp
Sample Cond
Sample Flow
BKG
«-*£**
(.0
•^
Pnlao
a/-
&&- \\*
A.
TTW
'^m
V
1
m
'I
<~Htt
-------
LTV Data Sheet (or FTIR Sampling
Operator
Dat
ample time File name Path
Location/Notes
fscans
Res (cm-1
Cell Temp (F)
Spk/Unsp
Sample Cond
Sample Flow
BKG
&±
Jk2_
u
I/O
oo
» i
,.0
»\
INLMlQVt)
-U.
_UL
-------
LTV Data Sheet for FTIR Sampling.
Operator
Date Sample time File name Path
Location/Notes
#scans
Res (cm-1
Cell Temp (F
Spk/Unsp
Sample Cond
Sample Flow
BKG
. f l
«v
•
Iv
XV
vv
Ma
i t
vx,
x X
;fr
IX
C4
\ \
___
II
100
J.J-
.Av
_Li_
130
~QS~
no
/oo
_l_v_
f of-
xv
Iv
JLx_
vVlkj
\\
\\
_!£_._.
If
4
-------
LTV Data Sheet for FTIR Sampling
• Operator
Date
ample time
File name
Path
Location/Notes
^
#scans
Res (cm-1
Cell Temp (F)
Spk/Unsp
Sample Cond
Sample Flow
BKG
tsfv M-~l
/ot>
M
J3Z__:;
111
fr
-------
LTV Data Sheet for FTIR Sampling.
Operator
>V
Date, Sample time File name Path
Location/Notes
Oscans
Res (cm-1
Cell Temp (F
Spk/Unsp
Sample Cond
Sample Flow
BKG
50
1. 4
U
42±
3021
|00
tell
- '450
o
So
!^L*_
v-v-
'£**-
/•to
rto
No
o
Q JT\J
-YL
i \
no
4
-------
LTV Data Sheet for FTIR Sampling.
Operator
iample time
File name
Path
Location/Notes
a:
fscans
(Hi**?
\«& (cm-1
Cell Temp (F)
Spk/Unsp
Sample Cond
Sample Flow
BKG
fc**
art v
MAn '
Alt-
v
±2L
'ft
AO
,iol-
nif
^L
m- ti/t
Vl'ttH
. /?
^/^_
jl^_
M°-
no
\v
yjtv A
cu-tof^:
«.00 J&l*t
7J&-
i\
1)0
Iv
v5 ^
-------
LTV Data Sheet for FTIR Sampling.
Operator
Date Sample time File name Path
Location/Notes
iscans Res(cm-1 Cell Temp (F) Spk/Unsp Sample Cond. Sample Flow BKG
/o
J0_
••ci
Iv
VI
r^
- /0V?
M
9Q
To~
Jjj_
_tL
\\
I
- SM/Z.T
\;
fcll
U2/H
IN
70
^"•7^1
_1A_
_2L
t^il^U
^2
IL *(.<>/*<•
Bb^^
110
HO
,lft (>-\ ^\"'\
ir i o i -j\ i
-------
LTV Data Sheet for FTIR Sampling.
Operator
Date
ample time
File name
Path
Location/Notes
iKscans
Res (cm-1
Cell Temp (F)
i*l
Spk/Unsp
L>AJ
Sample Cond
Samf
iO
e Flow
BKG
1»
TIE
"P5"
TT
moo
/&o
\H~SO
143}
ourier ^/V^P^'
_bL
^^
JD_
w
Tc-v^r
JiL
,-r^ -^
\3
ME
4iT
\N
NO".
OM'kcH
Vv
u
/fl£"
i«kj
Ul1- '1
-------
LTV Data Sheet for FTIR Sampling.
Operator
-------
LTV Data Sheet for FTIR Sampling.
Operator
-------
PROJECT NO.
PLANT:
47il-.ll
FTIR FIELD DATA FORM
(B*ctgrou»4 mud ctliltmtiom tftctn.)
DATE: V23/1997-W14/97
BAROMETRIC:
OPERATOR: Ceyer
SAMPLE
TIME
f6:28
16:39
17:09
6/24/97
9:39
9:50
9.55
11:25
12:50
12:56
12:04
12:15
RLE
NAME
BKG0623A
CTS0623A
SF60423A
BKG0624A
CTS0624A
CTS0624B
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
21 a,b,c,d,e
1530624a
1530624b
SF60624a
BKG0624B
36 passes
36 passes
N2 flow through cell
20.01 ppm elhylene
4.0 ppm SF6
Barometric Pressure
Vacuum leak check
T=0. P=3.2 loir
T=lmin.,P=14.4tofT
T=2 rain, P=23.2 lorr
N2 - 21pm through cell
20.01 ppm elhylene
20.01 ppm elhytene 2nd fill
NUMBER
SCANS
200
50/200
50/200
4% = - 33 ton
200
50/200
50/200
RES
(o»l)
1
1
1
1
1
1
CELL
TEMP(F)
121C
121C
12IC
121C
121C
121C
PRESSURE
751.6
750
749.2
748.9
749.9lorr
750
750
Toluene regulalor(540) had some contamination thai is being purged out - contamination mostly gone
Toluene 121 ppm
Toluene 121 ppm
4.0 ppm SF6
N2 4 Ipm through cell
50/200
1
still some contamination
50/200
200
1
1
12IC
121C
121C
750.5
749.9
•KG
A
623A
624A
624A
A
624A
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
flow @ 51pm
flow @ 51pm
flow @ 41pm
-------
PROJECT NO. 4701-08-11
PLANT: LTV
FTIR FIELD DATA FORM
(Background and c*likr*liom iptcUm.)
DATE: */2S/»7
BAROMETRIC:
OPERATOR:
Ceytr
SAMPI.E
VIMI:
8:17
8:41
12:10
12:14
13:40
18:36
18:40
FILE
NAME
BKG062SA
CTS0625A
BKG0625B
NIT01
BKG62SC
BKG625D
CTS0625B
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
N2 flowing
20 ppm elhylene (Taylor barometer)
Taylor Barometer x-2409
Slightly wetter than A
Nitrogen in cell compared to 62SB
Dryer than B
N2
Eihykne
NUMBER
SCANS
200
SO/200
200
200
200
200
RES
(cm-l)
1
1
1
1
1
1
CELL
TEMP(F)
121C
121C
121C
121C
121C
121C
PRESSURE
748.5
748.5
747
747.6
755
747.3
746.7
BKC
625A
625D
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
-------
PROJECT NO.
PLANT: LTV
4701-U-l I
FTIR FIELD DATA FORM
(Background and c*lilrmiio» tptctn.)
DATE: 6/26/97
BAROMETRIC:
OPERATOR:
Gtytr
SAMPLE
TIME
7:43
7:46
8.30
13:47
17:33
17:45
FILE
NAME
BKG0626A
CTS0626A
BKG0626B
BKG0626C
BKG0626D
CTS0626B
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
N2 through cell
20 ppm ethylene
N2 through cell
N2 through cell
N2 through cell
N2 through cell
NUMBER
SCANS
200
SO/200
200
200
200
200
RES
(OB-I)
^
CELL
TEMP(F)
I2IC
I2IC
121C
12IC
I21C
121C
PRESSURE
750.3
751.1
751.1
762
753
749.1
BUG
626A
626D
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
-------
PROJECT NO.
PLANT: LTV
4701-08-11
FTIR FIELD DATA FORM
(Background ami calibration iftclra.)
DATE: 6/27/97
BAROMETRIC:
OPERATOR:
Ceycr
SAMPLE
TIME
7:34
7:40
7:45
8:38
13:53
FILE
NAME
BKG0627A
CTS0627A
CTS0627B
BKG0627B
BKG0627C
CTS0627C
PATH
36 passes
36 passes
36 passes
36 passes
36 passes
36 passes
N2 through cell
20 ppm eihylene
20 ppm ethylene
N2 through cell
M2 through cell
20 ppm eihylene
NUMBER
SCANS
200
50
50
200
200
50
RES
(0*1)
CELL
TEMP(F)
121C
12IC
121C
I21C
121C
121C
PRESSURE
752.3
752.9
751.6
753.2
751.6
752.2
•KG
627A
627A
627C
APOD
NB/med
NB/med
NB/med
NB/med
NB/med
NB/med
NOTES
-------
Background and calibration spectra.
Operator
-------
Background and calibration spectra.
Operator
Date
Time
File Name
Path
Location/Notes
fscans
Res(cm-1)
Cell temp (F)
Pressure
BKG
Apod
Notes
-45L-
o
U i
wr.i
121 c
Vlo
YPT
r7R
OST
-------
B-2 FTIR FLOW AND TEMPERATURE READINGS
-------
L.
RUN NO.
DATE
SAMPLING LOCATION
PROJECT NO.
P- £_
OPERATOR.
TRAVERSE
POINT
NUMBER
CLOCK TIME
l24-hr.)
SAMPLING
TIME, tnln
GAS METER READING
(VJ. It'
INITIAL
DESIRED
ACTUAL
VELOCITY
HEAD
In. H,0
ORIFICE PRESSURE
DIFFERENTIAL
(AH). In H,0)
DESIRED ACTUAL
STACK
TEMP.
(T,).
•F
DRY GAS METER
TEMPERATURE
INLET
T. J. °F
OUTLET
T- J- '
tol
3.T
COMMENTS
-------
RUN NO.
DATE
SAMPLING LOCATION
PROJECT NO.
.ol.
t
OPERATOR
TRAVERSE
POINT
NUMBER
CLOCK TIME
SAMPLWG
TIME, mln
GAS METER READING
(V.), II3
INITIAL
DESIRED
ACTUAL
VELOCITY
HEAD
(AP.).
In. HjO
ORIFICE PRESSURE
DIFFERENTIAL
(AH). In H,0)
DESIRED ACTUAL
STACK
TEMP.
(T,J.
•F
DRY GAS METER
TEMPERATURE
INLET
IT. J. °
OUTLET
IT. , -
jMPINGER
o&L
tlf,
A0_
V?
n
111
1
US
^00
Lq_
iff
COMMENTS
-------
RUN NO. *
DATE Cf/^/'f'-J
1
TRAVERSE
POINT
NUMBER
\. CLOCK TIME
^024-hr.)
TIME, mln ^\
^^^--^
IO--2.O
*>''iz>
U'-1&
Info
VT-iA
i i:o
m/&C?
^cf/fi-O
/ «^3o
SAMPLING LOCATH
PROJECT NO.
)H MO ^f^J JivKfftolT *<«
GAS METER READING
(VJ. H1
INITIAL
DESIRED
ACTUAL
VELOCITY
HEAD
In. HjO
3,S
X? ^— —
^x* O
^ ij
^? (^
7.*J
?, 5"
^.-|
^* /
P-^
P-^
3. c^
ORIFICE PRESSURE
DIFFERENTIAL
(AH). In H20)
DESIRED
ACTUAL
JK
STACK
TEMP.
(T.I
"F
AVS
2«1
Al»o
?^\
ZHS
XA
y$\
^33
3 "3->
^I>^
•^5-
3o^
*5-
?s
^
3«5
^3^T
'^06'
3& sr
yoy
u.
m ^
<2??
•'So-l
?a'
^?f
>«|
3
-------
RUN NO.
DATE
SAMPLING LOCATION
PROJECT NO.
OPERATOR
TRAVERSE
POINT
NUMBER
"s\v^ CLOCK TIME
^vi (24-hr.)
SAMPUN(T\.
TIME, mln ^\
^^^-^^
lO'.XP
UV.TO
U'.-LJi
I I: SO
\-V.-L*
fZ'.il-
IV-T.T-
l^CO
• m* ;K)
(H-.^o
IS~90
GAS METER READING
(V. . II1
tuimi
DESIRED
ACTUAL
W
*
VELOCITY
HEAD
(Ap,).
In. H,0
ons
6--?t
0-7^
O.-7C9
o-SS
/^ P
o.T7
0-^1
P^9
r*i*
b/86.
ORIFICE PRESSURE
DIFFERENTIAL
(AH). In H,0)
DESIRED
fJ?*'
ACTUAL
^ X7
b
$
STACK
TEMP.
(T,).
°F
W*
t(«r
10
'If.
»vt
t4«
u"&
It A,
(17
uo
UCo
DRY GAS METER
TEMPERATURE
INLET
IT. J, °F
t-
^^
£ s
3.
fi«-
o r
££
1 S^
^4*1
iTs-
Q.'
u, X
^r
Ss
•a CD
"^1
Too
3«»
?*T1
^flO
e o
J«X
£n
3^
9«i
^30
^
u.
0
iu „:
CD £;
o I
£g
?*Z
^
2?j>
•So/
)o^
>do
Tfiffi>
^
av*
S?^
U-
«
lit Q_
^1
COMMENTS
-------
RUN NO. ^7
DATE p 7 ^V-t lG&>
Q5
ir.'°
lt'?<^
/x. /i
^"-*1
l^'-'VT
.
SAMPLING LOCATII
PROJECT NO.
IN LlV)S^l 5,'n^r Pkh-t" ^
GAS METER READING
(V.). IIJ
IUITIAI
DESIRED
ACTUAL
VELOCITY
HEAD
In. H,0
0. T
-?.C>
^/
^-(*
^.1
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2-1
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s-
liJ O-
-J M-
^^^^^^
3" 3
3o>r
Joo
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w
-$o)
*l
COMMENTS
-------
RUN NO.
DATE
SAMPLING LOCATION
PROJECT NO.
S/g*( $)«\t<
P \£-
OPERATOH.
.ol.
Z_Ii
TRAVERSE
POINT
NUMBER
^^ CLOCK TIME
SAMPLING^"*"''
TIME, mln ^\
^^^^
&\&£
6*135
\f)^
^^
\\\.t>'5
0^^
0,*U
o-^M
«*ct AA
,&*
Al*
o.?2
a.~7J,
o-io
ORIFICE PRESSURE
DIFFERENTIAL
(AH). InHjO)
DESIRED
fat c
ACTUAL
1
iH
l)i/
iH
u^
(|t
\vt
DRY GAS METER
TEMPERATURE
INLET
OUTLET
(T. J. °F
?'
i^
£«
u_
Z 0.
u_
flu
ag
.0- >-
S x
< 0
»O CO
u.
o
BO ^
6oc,
}«o
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5"*
9«o
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o
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27?
t
4
r/ v
-^JL
COMMENTS
-------
B-3 FTIR RESULTS
-------
TABLE B-l. FTIR RESULTS (ppm) AND EMISSION RATES AT THE LTV SCRUBBER INTLET •
Date
6/25/97
Time
9:27
»:33
9:37
9:43
9:54
9:58
10*2
10:36
10:39
10:43
10:47
11:13
11:18
11:24
11:29
12:20
12:26
12:30
12:34
12:54
12:59
13:03
13:06
13:46
13:49
13:52
13:56
14:17
14:21
14:27
14:32
14:56
15:00
15:05
15:09
15:34
Pile
Name"
NLS2M1
NLS2002
NLS2M3
NLS2M4
NLS2005
NLS200*
NLS2M7
NLV2008
NLV2009
NLV20IO
NLV2011
NLV20I2
NLV2013
NLV20I4
NLV2015
NLV2016
NLV2017
NLV20I8
NLV2019
NLV2020
NLV2021
NLV2022
NLV2023
NLV2024
NLV2025
NLV2026
NLV2027
NLV2028
NLV2029
NLV2030
NLV2031
NLV2032
NLV2033
NLV2034
NLV2035
NLV2036
Emissions
CO Unc Ibs/hr
734.7 IS 14.22
774.3 93 14.95
7MJ 9* 15 Jl
779.4 M 15.05
tllA 10.1 15.47
115.3 10.2 15.74
•l«.l 10J 15A4
874.2 11.5 16.87
851.7 11.4 16.44
846.4 11.2 16.34
853.7 11.2 16.48
811.4 10.4 15.66
801.9 10.5 15.48
811.6 10.7 15.67
818.0 10.9 15.79
842.6 10.8 16.27
858.5 11.2 16.57
854.5 11.4 16.50
861.5 11.5 16.63
826.7 11.0 15.96
858.2 11.5 16.57
837.6 11.1 16.17
843.7 11.3 16.29
824.5 11.1 15.92
818.4 10.8 15.80
816.0 11.0 15.75
820.3 11.2 15.83
814.3 10.9 15.72
829.2 11.7 16.01
867.3 12.2 16.74
881.8 12.6 17.02
783.6 10.5 15.13
788.4 10.6 15.22
799.1 10.9 15.43
815.2 H.3 15.74
814.5 11.2 15.72
Emissions
SO2 Unc Ibs/hr
71.2 1.7 3.14
15.5 1.8 3.77
S2J 1.9 3M
11.7 1.9 3.41
14.7 2.0 3J3
945 2.0 4.2*
100.8 2.0 4.45
118.3 2.2 5.22
98.0 2.2 4.33
91.5 2.2 4.04
102.8 2.2 4.54
1 10.0 2.1 4.85
102.1 2.2 4.51
91.2 2.2 4.02
93.0 2.2 4.10
80.3 2.2 3.54
81.8 2.3 3.61
86.5 2.3 3.82
92.4 2.3 4.08
123.9 2.2 5.47
137.9 2.3 6.08
114.9 2.3 5.07
105.0 2.3 4.63
76.8 2.3 3.39
64.4 2.3 2.84
71.7 2.3 3.17
91.7 2.3 4.05
75.9 2.3 3.35
63.6 2.4 2.81
77.9 2.5 3.44
103.1 2.5 4.55
100.7 2.2 4.44
85.2 2.2 3.76
84.7 2.3 3.74
91.6 2.3 4.04
97.9 2.3 4.32
Formal- Emission
dehyde Unc Ibs/hr
5.4 05 0.114
4J 05 0499
4.1 05 0.0*5
5.9 05 0.123
3.8 05 0479
3.8 05 0.07S
3.4 05 0.071
5.4 0.57 0.113
4.3 0.57 0.088
3.9 0.59 0.082
4.1 0.58 0.084
5.3 0.56 0.109
4.9 0.57 0.102
5.8 0.58 0.119
5.3 0.59 0.110
8.8 0.62 0.182
7.7 0.64 0.159
7.1 0.64 0.146
6.9 0.66 0.143
6.0 0.63 0.125
6.3 0.65 0.130
6.1 0.65 0.126
6.2 0.65 0.128
5.5 0.65 0.115
5.6 0.65 0.117
5.5 0.65 0.114
5.4 0.65 0.112
6.5 0.67 0.134
5.9 0.70 0.121
10.2 0.72 0.212
7.7 0.73 0.159
7.6 0.65 0.157
6.9 0.65 0.144
7.0 0.68 0.145
6.9 0.68 0.142
6.2 0.72 0.129
Emission
Methane Unc Ibs/hr
145 OJ 0.160
155 OJ 0.171
14.2 0.4 0.171
15.4 0.4 0.170
15J 0.4 d.174
155 0.4 0.171
15.2 0.4 0.16*
17.9 0.40 0.197
16.8 0.40 0.185
16.9 0.41 0.187
16.8 0.41 0.186
16.4 0.40 0.181
16.3 0.40 0.180
16.7 0.41 0.185
16.8 0.42 0.186
24.2 0.43 0.267
25.6 0.44 0.282
25.2 0.44 0.278
24.5 0.46 0.270
19.5 0.44 0.216
20.5 0.45 0.227
20.3 0.45 0.224
19.8 0.46 0.219
18.5 0.46 0.204
18.0 0.45 0.199
17.7 0.45 0.195
17.5 0.45 0.193
16.9 0.47 0.186
17.2 0.49 0.190
17.6 0.50 0.194
17.8 0.51 0.196
15.4 0.45 0.169
15.8 0.46 0.175
16.2 0.47 0.179
16.8 0.47 0.186
17.1 0.50 0.188
i-Heptane Unc
1.4 0.2
2J 0.2
IA 0.2
2A 0.2
3.0 0.2
3.1 0.2
3.1 0.2
3.3 0.3
3.4 0.3
3.4 0.3
3.5 0.3
3.2 0.3
3.4 0.3
3.6 0.3
3.6 0.3 I
1.8 0.3 1
2.1 0.3
2.3 0.3
2.4 0.3
2.4 0.3
2.7 0.3
2.7 0.3
2.9 0.3
2.3 0.3
2.6 0.3
2.8 0.3
2.8 0.3
2.9 0.3
3.1 0.3
3.1 0.3
3.4 0.3
2.7 0.3
2.9 0.3
3.0 0.3
3.2 0.3
2.7 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/25/97
Time
15:38
15:42
15:46
16:13
16:17
16:22
16:26
16:54
16:58
17:07
17:10
17:14
17:20
17:24
17:27
A
File
Nameb
NLV2037
NLV2038
NLV2039
NLV2040
NLV2041
NLV2042
NLV2043
NLV2047
NLV2048
NLS2049
NLS2050
NLS2051
NLS2052
NLS2053
NLS2054
verage — >
Emissions
CO Unc Ibs/hr
807.8 11.2 15.59
813.6 11.4 15.71
813.5 112 15.70
808.8 11.0 15.61
808.7 11.0 15.61
817.2 11.1 15.77
818.3 11.3 15.80
818.1 11.3 15.79
823.8 11.5 15.90
712.2 «.» 13.75
712.9 9.1 13.7*
721.2 9J 13.92
741.9 9.4 14.32
734.1 9.3 14.17
724.1 9J 14.02
827.8 11.2 15.98
Emissions
SO2 Unc Ibs/hr
84.9 2.4 3.75
83.7 2.4 3.69
104.9 2.3 4.63
80.2 2.3 3.54
85.7 2.3 3.78
88.7 2.3 3.91
85.6 2.3 3.78
1 14.7 2.4 5.06
1 14.5 2.4 5.05
U.4 1.9 3.90
7*4 2.0 3.47
714 2.1 3.17
•4J 2.0 3.72
*0.7 2.0 3.5*
744 2.0 3JO
93.6 2.3 4.13
Formal- Emissions
dehyde Unc Ibs/hr
5.3 0.71 0.110
5.9 0.70 0.122
4.9 0.69 0.101
5.6 0.70 0.115
5.1 0.70 0.107
5.2 0.69 0.109
5.3 0.71 0.110
5.5 0.7 0.114
5.4 0.7 0.113
4.7 0.* 0497
3.7 0.* (.077
5.1 0.* 0.10*
4.2 O.t 0.08*
43 0.* 0.090
4J O.i 0.088
6.0 0.66 0.125
Emissions
Methane Unc Ibs/hr
17.3 0.49 0.190
16.6 0.49 0.183
16.5 0.48 0.182
16.4 0.49 0.181
16.6 0.49 o'.183
17.0 0.48 0.187
17.5 0.50 0.193
16.9 0.5 0.186
16.7 0.5 0.185
13J 04 0.153
134 0.4 0.152
144 04 0.159
153 0.4 0.1*8
15.5 0.4 0.171
15.4 0.4 0.170
18.1 0.46 0.200
i-Heptane Unc
2.9 03
3.0 0.3
2.9 0.3
2.7 0.3
2.9 0.3
3.0 0.3
3.1 0.3
3.0 0.3
3.3 0.3
2.4 03
2.7 OJ
24 OJ
2.0 OJ
2.0 OJ
2.1 OJ
2.9 0.3
Date
6/26/97
Time
9:11
9:18
9:22
9:34
9:38
9:42
10:55
10:56
10:57
10:58
10:59
11:00
11:00
11:01
11:02
11:03
11.04
File
Name
NLS3001
NLS3002
NLS3003
NLS3004
NLS3005
NLS300*
16260004
16260005
16260006
16260007
16260008
16260009
16260010
I 62600 II
16260012
16260013
16260014
Emissions
CO Unc Ibs/hr
7*7.0 8.7 1441
753.1 t* 1434
7*84 9.0 1444
7*4.* 8.9 14.7*
800.2 ** 15.45
781.5 9J 15.09
847.2 10.7 16.35
851.7 10.9 16.44
860.3 11-2 16.61
862.8 HI 16.66
860.0 11. 1 16.60
861.7 11.1 16.63
870.8 II. 5 16.81
870.0 11.3 16.79
872.9 11.3 16.85
882.1 11.6 17.03
881.5 11.5 17.02
Emissions
SO, Unc Ibs/hr
114.4 1.7 545
101.1 1.7 4.4*
10*4 14 4.71
73.* 1.7 3.25
97.7 14 4J1
107.0 14 4.72
120.3 2.1 5.31
121.0 2.2 5.34
123.3 2.2 5.44
124.0 2.2 5.47
123.9 2.2 5.47
123.1 2.2 5.43
120.6 2.2 5.32
115.6 2.2 5.10
1 10.5 2.2 4.87
105.8 2.2 4.67
99.8 2.2__ 4.4.L.
Formal- • Emissions
dehyde Unc Ibs/hr
8.0 04 0.1*5
5.7 0.4 0.118
4.7 0.4 0498
5.7 0.4 0.119
4.4 OJ 0.091
44 0.5 0.099
2.3 0.53 0.047
2.2 0.54 0.045
2.3 0.54 0.047
2.3 0.54 0.048
2.3 0.55 0.048
2.4 0.55 0.049
2.4 0.57 0.049
2.4 0.56 0.050
2.3 0.58 0.048
2.3 0.58 0.048
3.3 _ _OSL QJH7
Emissions
Methane Unc Ibs/hr
154 OJ 0.170
14.5 OJ 0.1*0
144 OJ 0.159
14.2 OJ 0.157
15.0 OJ 0.1**
15J OJ 0.1*9
17.4 0.37 0.192
17.5 0.38 0.193
17.7 0.38 0.195
17.7 0.38 0.195
17.8 0.38 0.197
18.0 0.38 0.198
18.1 0.40 0.200
18.1 0.39 0.200
18.2 0.40 0.201
18.4 0.40 0.203
jji.5. jyg jyjy
i-Heptane Unc
14 0.2
1.9 0.2
2.0 0.2
1.5 0.2
1.7 0.2
1.7 0.2
2.7 0.2
2.9 0.2
3.1 0.2
3.3 0.2
3.3 0.2
3.5 0.3
3.6 0.3
3.7 0.3
3.7 0.3
3.9 0.3
^^y ^jy
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
11:05
11.06
11:07
11:08
11.09
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:16
11:17
11:18
11:19
11:20
11.21
11:21
11:22
11:57
11:58
11:59
12:00
12:01
12:02
12:02
1203
12:04
12:05
1206
1207
12:08
12:09
12:10
12:10
File
Name
16260015
16260016
16260017
16260018
16260019
16260020
16260021
16260022
16260023
16260024
16260025
16260026
16260027
16260028
16260029
16260030
16260031
16260032
16260033
16260034
16260067
16260068
16260069
16260070
16260071
16260072
16260073
16260074
16260075
16260076
16260077
16260078
16260079
16260080
16260081
16260082
Emissions
CO Unc Ibs/hr
888.8 11.7 17.16
892.4 12.0 17.23
894.4 12.0 17.27
898.1 12.1 17.34
897.3 12.0 17.32
901.1 12.3 17.40
900.2 12.2 17.38
898.7 12.0 17.35
892.9 11.9 17.24
890.8 12.0 17.20
882.3 11.9 17.03
884.0 11.9 17.07
865.4 11.5 16.71
861.1 11.4 16.62
860.6 11.5 16.61
850.2 11.1 16.41
846.2 11.0 16.33
850.3 11.1 16.41
852.1 11.2 16.45
855.1 11.2 16.51
846.8 11.0 16.35
849.8 11.1 16.41
845.5 11.0 16.32
850.4 11.0 16.42
848.2 11.0 16.37
854.6 11.3 16.50
862.1 11.3 16.64
866.0 11.5 16.72
863.1 11.1 16.66
866.3 11.2 16.72
862.8 11.1 16.65
878.7 11.6 16.%
871.0 11.3 16.81
871.5 11.2 16.82
878.9 11.5 16.97
877.9 11.5 16.95
Emissions
SO2 Unc Ibs/hr
96.4 2.3 4.25
95.5 2.3 4.21
98.0 2.3 4.32
102.4 2.3 4.52
108.4 2.3 4.78
115.6 2.3 5.10
124.2 2.3 5.48
132.1 2.3 5.83
136.5 2.3 6.02
136.7 2.3 6.03
135.0 2.3 5.96
131.2 2.3 5.79
121.6 2.2 5.36
111.9 2.2 4.94
106.2 2.2 4.69
103.6 2.2 4.57
104.0 2.2 4.59
106.4 2.2 4.70
107.6 2.2 4.75
II 0.0 2.2 4.85
100.8 2.2 4.45
100.4 2.2 4.43
98.5 2.2 4.35
95.7 2.2 4.22
94.1 2.2 4.15
95.2 2.2 4.20
96.4 2.3 4.25
96.9 2.2 4.28
95.9 2.3 4.23
94.4 2.3 4.17
93.4 2.2 4.12
93.0 2.3 4.10
91.9 2.3 4.06
92.5 2.2 4.08
92.9 2.3 4.10
93.1 2.3 4.11
Formal- Emission
dehyde Unc Ibs/hr
2.2 0.58 0.045
2.3 0.59 0.047
2.4 0.59 0.049
2.4 0.59 0.049
2.4 0.59 0.050
2.5 0.60 0.052
2.5 0.60 0.052
2.6 0.58 0.055
2.7 0.59 0.055
2.7 0.58 0.057
2.8 0.58 0.057
2.9 0.58 0.059
2.8 0.57 0.057
2.7 0.57 0.057
2.7 0.57 0.055
2.6 0.57 0.054
2.6 0.57 0.054
2.6 0.57 0.054
2.7 0.57 0.056
2.7 0.57 0.056
3.2 0.59 0.065
3.4 0.60 0.071
3.5 0.59 0.073
3.7 0.59 0.076
3.7 0.59 0.077
3.8 0.58 0.080
3.9 0.60 0.081
4.0 0.60 0.083
4.1 0.60 0.085
4.2 0.59 0.087
4.2 0.59 0.088
4.3 0.60 0.088
4.5 0.59 0.093
4.5 0.59 0.094
4.8 0.60 0.099
4.8 0.59 0.100
Emissions
Methane Unc Ibs/hr
18.5 0.41 0.205
18.6 0.41 0.206
18.8 0.41 0.207
19.0 0.41 0.209
18.9 0.41 d.208
18.9 0.42 0.209
18.9 0.42 0.208
18.9 0.41 0.209
18.8 0.41 0.208
18.7 0.41 0.207
18.6 0.41 0.205
18.4 0.40 0.203
18.2 0.40 0.201
18.0 0.40 0.198
18.0 0.40 0.198
17.9 0.40 0.197
17.9 0.40 0.197
18.1 0.40 0.199
18.2 0.39 0.201
18.2 0.40 0.201
20.7 0.41 0.228
20.8 0.42 0.230
20.9 0.41 0.231
21.2 0.41 0.234
i-Heptane Unc
4.0 0.3
4.0 0.3
4.1 0.3
4.2 0.3
4.2 . 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.5 0.3
4.5 0.3
4.5 0.3
3.6 0.3
3.8 0.3
3.9 0.3
3.9 0.3
21.5 0.41 0.237 1 4.0 0.3
21.8 0.41 0.241 1 4.1 0.3
22.1 0.42 0.244
22.3 0.42 0.246
22.3 0.42 0.246
22.5 0.41 0.249
22.7 0.41 0.250
22.9 0.42 0.253
23.0 0.41 0.254
23.3 0.41 0.257
23.3 0.42 0.257
23.5 0.41 0.259
4.2 0.3
4.2 0.3
4.3 0.3
4.3 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.5 0.3
4.5 0.3 1
4.5 0.3 1
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
12:11
12:12
12:13
12:14
12.15
12:16
12:17
12:18
12:19
12:34
12:34
12:35
12:36
12:37
12:38
12:39
12:40
12:41
12:42
12:43
12:44
12:44
12:45
12:46
12:47
12:48
12:49
12.50
12:51
12:52
12:53
12:54
12:54
12:55
12.56
12:57
File
Name
16260083
16260084
16260085
16260086
16260087
16260088
16260089
16260090
16260091
16260103
16260104
16260105
16260106
16260107
16260108
16260109
16260110
162601 1 1
16260112
16260113
16260114
16260115
16260116
16260117
16260118
16260119
16260120
16260121
16260122
16260123
16260124
16260125
16260126
16260127
16260128
16260129
Emissions
CO Unc Ibs/hr
876.2 11.6 16.91
877.3 11.3 16.94
876.6 11.5 16.92
873.8 11.3 16.87
876.5 11.6 16.92
874.4 11.3 16.88
867.5 11.2 16.75
870.2 11.2 16.80
871.4 11.3 16.82
882.6 11.8 17.04
879.1 11.6 16.97
878.0 11.6 16.95
878.6 11.7 16.%
882.1 11.8 17.03
881.0 11.7 17.01
886.6 11.9 17.11
878.9 11.7 16.97
877.3 11.6 16.93
874.9 11.7 16.89
871.3 11.6 16.82
871.0 11.6 16.81
863.7 11.3 16.67
859.6 11.2 16.59
864.0 11.3 16.68
863.3 11.3 16.66
869.0 11.5 16.77
860.2 1 1.2 16.61
860.7 11.2 16.62
863.8 11.3 16.67
867.9 11.5 16.75
872.6 11.5 16.85
875.6 11.6 16.90
881.1 11.8 17.01
886.0 11.8 17.10
887.6 11.8 17.13
888.2 118 17.14
Emissions
SO2 Unc Ibs/hr
92.3 2.3 4.07
91.7 2.3 4.05
90.4 2.3 3.99
89.3 2.3 3.94
87.9 2.3 3.88
86.9 2.3 3.84
86.1 2.3 3.80
85.6 2.3 3.78
85.5 2.3 3.77
89.2 2.3 3.94
90.6 2.3 4.00
91.0 2.3 4.01
89.3 2.3 3.94
87.9 2.4 3.88
86.8 2.3 3.83
86.9 2.4 3.83
86.9 2.4 3.84
86.5 2.3 3.82
85.2 2.3 3.76
84.0 2.3 3.71
82.6 2.3 3.64
80.6 2.3 3.55
78.8 2.3 3.48
77.2 2.3 3.41
75.1 2.3 3.31
72.8 2.3 3.21
69.4 2.3 3.06
66.8 2.3 2.95
64.6 2.3 2.85
62.6 2.3 2.76
62.6 2.4 2.76
62.8 2.4 2.77
64.1 2.4 2.83
66.7 2.4 2.94
70.8 2.4 3.12
74.5 2.4 3.29
Formal- Emission
dehyde Unc Ibs/hr
4.9 0.59 0.101
4.9 0.60 0.102
5.0 0.60 0.103
5.0 0.60 0.103
5.0 0.60 0.103
4.9 0.60 0.102
4.9 0.62 0.102
4.8 0.61 0.100
4.8 0.61 0.100
4.0 0.62 0.082
4.2 0.62 0.087
4.2 0.63 0.088
4.3 0.63 0.089
4.4 0.62 0.091
4.5 0.63 0.093
4.5 0.63 0.093
4.6 0.63 0.094
4.5 0.64 0.094
4.5 0.64 0.094
4.6 0.63 0.096
4.6 0.62 0.096
4.6 0.62 0.095
4.7 0.62 0.096
4.6 0.62 0.095
4.7 0.61 0.097
4.6 0.64 0.095
4.5 0.63 0.094
4.5 0.62 0.093
4.3 0.64 0.090
4.4 0.63 - 0.092
4.4 0.66 0.090
4.5 0.64 0.093
4.6 0.65 0.095
4.8 0.65 0.100
4.9 0.67 0.101
5.1 0.66 0.105
Emission
Methane Unc Ibs/hr
23.6 0.41 0.260
23.6 0.42 0.261
23.6 0.42 0.260
23.7 0.42 0.261
23.8 0.42 6.263
23.9 0.42 0.263
23.8 0.43 0.262
23.8 0.43 0.262
24.0 0.43 0.265
24.5 0.44 0.270
24.3 0.43 0.268
24.2 0.44 0.267
24.3 0.44 0.268
24.4 0.43 0.269
24.6 0.44 0.271
24.6 0.44 0.272
24.5 0.44 0.271
24.5 0.45 0.270
24.4 0.44 0.269
24.5 0.44 0.270
24.6 0.43 0.271
24.6 0.44 0.271
24.6 0.43 0.271
24.8 0.43 0.273
24.9 0.43 0.275
24.9 0.45 0.274
25.0 0.44 0.276
25.2 0.44 0.278
25.2 0.45 0.278
25.6 0.44 0.283
25.8 0.46 0.284
26.3 0.45 0.290
26.8 0.45 0.296
27.1 0.46 0.299
27.4 0.46 0.302
27.3 0.46 0.301
i-Heptane Unc
4.5 0.3
4.6 0.3
4.5 0.3
4.6 0.3
4.6 0.3 1
4.6 0.3 1
4.5 0.3
4.6 0.3
4.6 0.3
3.9 0.3
4.0 0.3
4.1 0.3
4.2 0.3
4.2 0.3
4.3 0.3
4.4 0.3
4.5 0.3
4.5 0.3
4.5 0.3
4.6 0.3
4.6 0.3
4.6 0.3 1
4.7 0.3 1
4.7 0.3
4.7 0.3
4.6 0.3
4.6 0.3
4.7 0.3
4.6 0.3
4.8 0.3
4.7 0.3
4.8 0.3
4.7 0.3
4.8 0.3
4.8 0.3
4.8 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
12:58
12:59
13:00
13:01
13:02
13:03
13:04
I4.OO
14:00
14:01
14:02
14:03
14:04
14.O5
14.06
14:07
14:08
14.09
14:09
14:10
14:11
14:12
14:13
14:14
14:15
14:16
14:17
14:18
14:18
14.19
14:20
14:21
14.22
14:23
14:24
14.25
File
Name
16260130
16260131
16260132
16260133
16260134
16260135
16260136
16260165
16260166
16260167
16260168
16260169
16260170
16260171
16260172
16260173
16260174
16260175
16260176
16260177
16260178
16260179
16260180
16260181
16260182
16260183
16260184
16260185
16260186
16260187
16260188
16260189
16260190
16260191
16260192
16260193
Emissions
CO Unc Ibs/hr
892.2 12.0 17.22
886.7 11.8 17.12
879.8 11.7 16.98
877.3 11.5 16.94
884.7 11.7 17.08
878.8 11.7 16.%
878.0 11.6 16.95
814.8 10.4 15.73
817.2 10.6 15.78
808.4 10.3 15.61
807.9 10.4 15.60
806.9 10.4 15.58
807.7 10.5 15.59
798.2 10.2 15.41
799.3 10.3 15.43
802.9 10.4 15.50
803.8 10.3 15.52
805.9 10.5 15.56
803.7 10.5 15.51
804.9 10.4 15.54
808.8 10.6 15.61
813.2 10.7 15.70
814.2 10.7 15.72
816.6 10.7 15.76
818.1 10.7 15.79
819.0 10.8 15.81
818.5 10.7 15.80
816.2 10.8 15.76
818.2 10.8 15.79
821.1 10.9 15.85
812.0 10.6 15.67
816.1 10.7 15.75
812.9 10-8 15.69
810.0 10.8 15.64
809.2 10.6 15.62
811.3 10.8 15.66
Emissions
Sd Unc Ibs/hr
78.8 2.4 3.48
80.4 2.4 3.55
80.1 2.4 3.53
79.6 2.4 3.51
79.9 2.4 3.52
79.2 2.4 3.50
78.3 2.4 3.46
69.0 2.1 3.04
67.1 2.2 2.%
64.8 2.2 2.86
61.9 2.2 2.73
59.3 2.2 2.62
57.1 2.2 2.52
54.5 2.1 2.40
53.2 2.2 2.35
52.5 2.2 2.31
52.3 2.1 2.31
52.1 2.2 2.30
51.0 2.2 2.25
51.3 2.2 2.26
50.6 2.2 2.23
49.7 2.2 2.19
49.1 2.2 2.16
48.4 2.2 2.14
47.9 2.2 2.11
47.7 2.2 2.10
47.7 2.2 2.10
48.9 2.2 2.16
50.7 2.2 2.24
52.8 2.3 2.33
54.2 2.2 2.39
55.8 2.2 2.46
56.3 2.2 2.48
55.3 2.2 2.44
55.1 2,2 2.43
54.4 2.2 2.40
Formal- Emission
dehyde Unc Ibs/hr
5.2 0.67 0.107
5.2 0.68 0.108
5.3 0.65 0.109
5.5 0.65 0.113
5.5 0.66 0.114
5.6 0.66 0.116
5.6 0.66 0.115
4.4 0.58 0.091
4.6 0.61 0.096
4.7 0.61 0.098
4.9 0.60 0.101
4.8 0.61 0.100
4.9 0.62 0.100
4.9 0.60 0.101
4.9 0.61 0.101
4.9 0.61 0.101
4.8 0.60 0.099
4.7 0.62 0.097
4.6 0.62 0.096
4.7 0.61 0.097
4.6 0.63 0.096
4.6 0.63 0.096
4.6 0.63 0.096
4.7 0.63 0.097
4.7 0.63 0.097
4.7 0.65 0.097
4.7 0.64 0.097
4.7 0.64 0.098
4.7 0.65 0.097
4.7 0.66 0.097
4.7 0.64 0.097
4.7 0.65 0.098
4.7 0.65 0.097
4.7 0.64 0.097
4.7 0.65 0.097
4.7 0.64 0.098
Emission
Methane Unc Ibs/hr
27.3 0.46 0.302
27.1 0.47 0.299
26.8 0.45 0.295
26.5 0.45 0.292
26.2 0.46 b.289
25.9 0.46 0.285
25.5 0.46 0.281
17.1 0.41 0.189
17.0 0.43 0.187
16.9 0.43 0.186
16.9 0.42 0.186
16.8 0.43 0.185
16.8 0.43 0.185
16.8 0.42 0.185
17.1 0.43 0.188
17.4 0.43 0.192
17.5 0.42 0.193
17.3 0.43 0.191
17.1 0.43 0.189
17.1 0.43 0.189
17.1 0.44 0.189
17.2 0.44 0.190
17.3 0.44 0.191
17.3 0.44 0.191
17.4 0.44 0.192
17.3 0.45 0.191
17.5 0.44 0.193
17.5 0.45 0.193
17.6 0.45 0.194
17.4 0.46 0.192
17.4 0.45 0.192
17.4 0.46 0.192
17.3 0.45 0.190
17.2 0.45 0.190
17.2 0.45 0.190
17.2 0.44 0.190
i-Heptane Unc
4.8 0.3
4.9 0.3
4.8 0.3
4.8 0.3
4.6 0.3
4.7 0.3
4.7 0.3
2.3 0.3
2.3 0.3
2.4 0.3
2.5 0.3
2.6 0.3
2.6 0.3
2.7 0.3
2.8 0.3
2.9 0.3
2.9 0.3
3.0 0.3
3.0 0.3
3.1 0.3
3.2 0.3
3.2 0.3
3.2 0.3
3.3 0.3
3.3 0.3 I
3.4 0.3 I
3.4 0.3
3.4 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.6 0.3
3.6 0.3
3.6 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
6/26/97
Time
14:26
14:27
14:28
15:06
15:07
15:08
15.09
15:10
15.10
15:11
15:12
15:13
15:14
15:15
15:16
15:17
15:18
15:19
15:19
15:20
15:21
15:22
15:23
15:24
15:25
15:26
15.27
15:28
15:29
15:29
15:30
15:31
15:32
15:33
14:00
16:06
File
Name
6260194
6260195
16260196
16260234
16260235
16260236
16260237
16260238
16260239
16260240
16260241
16260242
16260243
16260244
16260245
16260246
16260247
16260248
16260249
16260250
16260251
16260252
16260253
16260254
16260255
16260256
16260257
16260258
16260259
16260260
16260261
16260262
16260263
16260264
NLS3007
NLS3008
Emissions
CO Unc Ibs/hr
803.6 10.5 15.51
804.9 10.4 15.54
811.7 10.6 15.67
815.1 11.0 15.73
809.0 10.8 15.62
803.5 10.5 15.51
796.0 10.2 15.37
796.6 10.2 15.38
803.5 10.6 15.51
808.8 11.0 15.61
802.5 10.6 15.49
799.9 10.5 15.44
799.5 10.4 15.43
800.9 10.4 15.46
805.8 10.7 15.56
805.6 10.4 15.55
805.8 10.5 15.56
805.6 10.4 15.55
805.5 10.4 15.55
815.4 10.9 15.74
812.7 10.5 15.69
815.1 10.6 15.74
821.3 10.9 15.85
824.2 10.9 15.91
824.8 10.9 15.92
814.1 10.6 15.72
825.8 11.1 15.94
824.2 10.9 15.91
825.0 11-0 15.93
814.6 10.5 15.73
823.7 10.9 15.90
818.2 10.6 15.80
823.7 10.9 15.90
828.0 11.0 15.98
703.9 8.2 13.59
763.2 9J 14.73
Emissions
SOj Unc Ibs/hr
54.4 2.2 2.40
53.6 2.2 2.37
53.1 2.2 2.34
52.9 2.2 2.34
52.0 2.2 2.30
52.6 2.2 2.32
52.9 2.2 2.33
53.6 2.2 2.37
54.5 2.2 2.41
55.5 2.3 2.45
56.2 2.2 2.48
56.2 2.2 2.48
56.8 2.2 2.50
57.0 2.2 2.52
57.6 2.2 2.54
57.9 2.2 2.55
57.6 2.2 2.54
58.0 2.2 2.56
58.5 2.2 2.58
59.7 2.2 2.64
60.0 2.2 2.65
60.7 2.2 2.68
61.3 2.2 2.71
60.7 2.2 2.68
60.3 2.2 2.66
59.9 2.2 2.64
61.5 2.3 2.72
62.4 2.2 2.75
63.9 2.2 2.82
64.1 2.2 2.83
64.4 2.2 2.84
63.7 2.2 2.81
62.8 2.2 2.77
61.6 2.3 2.72
23.9 1.8 1.05
39.1 1.9 1.72
Formal- Emission
dehyde Unc Ibs/hr
4.7 0.65 0.097
4.7 0.64 0.098
4.7 0.63 0.096
3.8 0.63 0.079
4.4 0.63 0.091
4.6 0.64 0.096
4.8 0.64 0.099
4.9 0.64 0.101
4.9 0.65 0.102
5.0 0.66 0.104
5.0 0.65 0.103
5.1 0.64 0.105
5.0 0.64 0.104
5.0 0.65 0.104
5.1 0.64 0.105
5.1 0.64 0.105
5.1 0.64 0.107
5.2 0.64 0.107
5.1 0.65 0.106
5.2 0.64 0.109
5.2 0.65 0.107
5.2 0.63 0.108
5.1 0.65 0.106
5.3 0.65 0.110
5.2 0.65 0.107
5.3 0.65 0.110
5.3 0.66 0.109
5.2 0.66 0.108
5.2 0.66 0.108
5.3 0.65 0.109
5.3 0.66 0.110
5.2 0.65 0.108
5.3 0.67 0.109
5.2 0.67 O.J08
4J OS 0.1*1
5.0 0.6 0.1*4
Emissions
Methane Unc Ibs/hr
17.0 0.45 0.188
17.1 0.44 0.189
17.2 0.44 0.190
17.0 0.44 0.188
17.0 0.44 'o.!88
16.8 0.45 0.186
16.8 0.45 0.186
16.8 0.45 0.185
16.7 0.46 0.184
16.8 0.46 0.186
16.7 0.45 0.185
16.7 0.45 0.184
16.7 0.44 0.184
16.7 0.45 0.184
16.7 0.45 0.185
16.8 0.45 0.185
16.9 0.44 0.186
16.8 0.45 0.186
16.8 0.45 0.185
16.8 0.45 0.186
16.8 0.45 0.185
16.9 0.44 0.186
17.0 0.45 0.187
17.0 0.45 0.188
17.0 0.45 0.188
17.0 0.45 0.188
17.2 0.46 0.190
17.2 0.46 0.190
17.1 0.46 0.188
17.1 0.45 0.189
17.2 0.46 0.189
17.2 0.45 0.190
17.2 0.46 0.190
17.4 0.47 0.192
14.4 0.4 0.15*
IS-5 0.4 0.171
i-Heptane Unc
3.6 0.3
3.6 0.3
3.6 0.3
2.7 0.3
2.8 0.3
2.8 0.3
2.8 0.3
2.9 0.3
3.0 0.3
3.0 0.3
3.1 0.3
3.1 0.3
3.2 0.3
3.2 0.3
3.3 0.3
3.3 0.3
3.3 0.3
3.3 0.3
3.2 0.3
3.4 0.3
3.4 0.3
3.5 0.3
3.4 0.3
3.5 0.3
3.4 0.3
3.6 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.5 0.3
3.6 0.3
1.4 0.2
1.9 OJ
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
Time
1*:IO
U:15
l*:24
1*:33
File
Name
NLS3009
NLS3010
NLS3011
NLS3012
NLS3013
Emissions
CO Unc Ibs/hr
7134 M 13.71
O34 (4 13.20
7124 IJ 13.7*
71*4 1.5 1344
7235 15 1347
1 6/26/97 Average ->| 847.3 ll.l 16.36
Emissions
SO2 Unc Ibs/hr
50.2 14 2.21
434 1.7 143
4*.4 14 245
42.4 14 147
53.7 14 2J7
79.0 2.3 3.49
Formal- Emissions
dehyde Unc Ibs/hr
4.5 OJ 0493
44 0.5 049*
4.4 05 0490
44 05 049*
44 05 0.095
4.3 0.62 0.088
Emissions
Methane Unc Ibs/hr
14J 0.4 0.15S
13.7 0.4 0.151
14.0 0.4 0.155
144 0.4 0.154
14.2 0.4 O.'l57
20.1 0.43 0.222
i- Heptane Unc
14 OJ
1.4 0.2
2-2 0.2
2J 0.2
2J 0.2
3.9 0.3
Date
6/27/97
Time
9:21
»:25
9:29
9:35
9:40
9:44
10:21
10:22
10:23
10:23
10:24
10:25
10:26
10:27
10:28
10:29
10.30
10:31
10:32
10:33
10:33
10:34
10:35
10:36
10.37
10:38
10:39
File
Name
NLS4001
NLS4002
NLS4003
NLS4004
NLS4005
NLS400*
16270035
16270036
16270037
16270038
16270039
16270040
16270041
16270042
16270043
16270044
16270045
16270046
16270047
16270048
16270049
16270050
16270051
16270052
16270053
16270054
16270055
Emissions
CO Unc Ibs/hr
7704 94 144
7*5.1 9.0 14J
7*0.2 9.0 14.7
7*0.* 14 14.7
7*5.4 9.0 144
7*7.7 9.1 144
864.0 11.34 16.7
858.2 11.25 16.6
855.2 11.15 16.5
850.5 11.12 16.4
844.4 11.07 16.3
838.0 10.77 16.2
836.0 10.92 16.1
828.7 10.94 16.0
824.4 10.57 15.9
822.7 10.68 15.9
821.8 10.66 15.9
815.7 10.45 15.7
814.2 10.52 15.7
812.2 10.33 15.7
812.3 10.58 15.7
813.9 10.45 15.7
830.7 10.92 16.0
833.2 10.91 16.1
842.1 1125 16.3
8451 -11.14 16.3
849.2 11.22 16.4
Emissions
SO, Unc Ibs/hr
112.0 1.7 4441
1024 1.7 4.499
99.2 1.7 4J75
M.I 1.7 4J42
9*4 1.7 4.271
»*.2 14 4.24*
115.5 1.98 5.095
114.3 1.96 5.043
112.8 1.96 4.977
111.0 1.98 4.900
108.9 1.95 4.805
108.0 1.95 4.765
107.7 1.92 4.753
108.3 1.93 4.778
108.7 1.92 4.794
110.6 1.91 4.881
109.7 1.88 4.839
107.0 1.90 4.721
101.9 1.90 4.498
96.0 1.92 4.235
91.0 1.93 4.014
86.1 1.95 3.800
82.4 1.98 3.636
79.7 1.97 3.515
79.2 1.99 3.494
80.5 2.01 3.552
83.6 2.04 3.689
Formal- Emission
dehyde Unc Ibs/hr
4.5 0.4 0494
43 0.4 04*1
34 0.4 OJI1
34 0.4 0.0(1
3.5 0.4 0473
3.2 04 »4*t
3.2 0.50 0.066
3.6 0.50 0.074
3.9 0.51 0.081
3.7 0.51 0.076
3.8 0.50 0.078
3.8 0.50 0.079
3.8 0.49 0.079
3:8 0.49 0.079
3.8 0.50 0.078
3.8 0.50 0.079
3.8 0.48 0.078
3.7 0.49 0.077
3.7 0.49 0.076
3.7 0.50 0.076
3.6 0.51 0.075
3.6 0.51 0.074
3.5 0.54 0.073
3.5 0.51 0.072
3.5 0.52 0.072
3.3 0.53 0.068
3.2 0.54 0066
Emission
Methane Unc Ibs/hr
14.2 OJ 0.157
134 OJ 0.152
14.0 OJ 0.155
13J OJ 0.147
134 OJ 0.150
13.4 OJ 0.148
16.3 0.35 0.180
16.2 0.35 0.179
15.9 0.35 0.175
15.8 0.36 0.174
15.7 0.35 0.173
15.7 0.36 0.173
15.6 0.35 0.172
15.5 0.35 0.171
15.3 0.35 0.169
15.3 0.35 0.169
15.3 0.34 0.169
15.2 0.35 0.168
15.2 0.35 0.168
15.3 0.36 0.168
15.2 0.36 0.168
15.3 0.36 0.169
15.4 0.38 0.170
15.7 0.36 0.173
15.8 0.37 0.174
15.9 0.37 0.176
16.1 0.38 0.177
i-Heplane Unc
1.7 0.2
14 0.2
2.0 0.2
2.4 0.2
23 0.2
2.* 0.2
3.5 0.2
3.5 0.2 I
3.6 0.2 I
3.6 0.2
3.6 0.2
3.7 0.2
3.7 0.2
3.8 0.2
3.8 0.2
3.8 0.2 I
3.9 0.2 1
3.8 0.2
3.9 0.2
3.9 0.2
3.9 0.3
3.9 0.3
3.9 0.3
4.0 0.2
4.0 0.3
4.1 0.3
4.1 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/27/97
Time
10:40
10:41
10:42
10:42
10:43
10:44
10:45
10:46
10:47
10:48
10:49
11:07
11. -08
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:15
11:16
11:17
11:18
11:19
11:20
11:21
11.22
11:23
11:24
11:24
11:25
11:26
11:27
11:28
11:29
File
Name
6270056
6270057
6270058
6270059
6270060
16270061
6270062
6270063
6270064
16270065
16270066
16270081
16270082
16270083
16270084
16270085
16270086
16270087
16270088
16270089
16270090
16270091
16270092
16270093
16270094
16270095
16270096
16270097
16270098
16270099
16270100
16270101
16270102
16270103
16270104
16270105
Emissions
CO Unc Ibs/hr
851.5 11.30 16.4
859.2 11.60 16.6
855.7 11.51 16.5
851.7 11.40 16.4
859.5 11.81 16.6
859.0 11.63 16.6
856.2 11.64 16.5
856.0 11.70 16.5
850.2 11.56 16.4
847.3 11.55 16.4
841.2 11.23 16.2
905.2 13.09 17.5
892.9 12.58 17.2
890.0 12.70 17.2
888.6 12.52 17.2
885.8 12.42 17.1
884.9 12.33 17.1
883.9 12.50 17.1
884.1 12.63 17.1
873.7 12.07 16.9
873.4 12.28 16.9
871.4 12.56 16.8
859.7 11.84 16.6
861.1 12.11 16.6
850.7 11.51 16.4
865.2 12.94 16.7
850.5 11.71 16.4
848.2 11.84 16.4
849.4 11.70 16.4
853.5 11.99 16.5
857.3 12.00 16.5
865.3 12.37 16.7
866.7 12.17 16.7
865.9 12.08 16.7
873.3 12.24 16.9
874.0 12.34 16.9
Emissions
SO2 Unc Ibs/hr
87.5 2.02 3.860
92.3 2.04 4.073
95.8 2.05 4.229
98.1 2.01 4.329
99.4 2.05 4.385
99.9 2.04 4.407
100.1 2.05 4.419
98.3 2.06 4.339
96.3 2.07 4.250
94.0 2.07 4.146
90.8 2.07 4.006
81.4 2.20 3.590
85.8 2.21 3.784
89.4 2.22 3.947
93.0 2.18 4.102
98.3 2.21 4.337
102.5 2.21 4.524
105.4 2.19 4.651
107.6 2.20 4.747
107.4 2.15 4.739
106.1 2.18 4.683
104.5 2.13 4.612
101.7 2.14 4.488
99.6 2.17 4.395
96.4 2.16 4.252
93.2 2.17 4.113
88.2 2.19 3.892
83.8 2.13 3.698
80.0 2.14 3.529
76.8 2.18 3.390
73.6 2.19 3.246
69.9 2.18 3.086
66.6 2.20 2.937
64.0 2.20 2.825
63.2 2.20 2.790
63.2 2.21 2.788
Formal- Emission
dehyde Unc Ibs/hr
3.1 0.53 0.065
3.0 0.53 0.063
3.0 0.53 0.063
3.0 0.52 0.062
3.1 0.53 0.064
3.1 0.53 0.065
3.1 0.53 0.064
3.2 0.54 0.066
3.2 0.55 0.066
3.3 0.55 0.068
3.3 0.55 0.069
2.2 0.59 0.045
1.9 0.58 0.040
2.0 0.58 0.041
2.1 0.58 0.042
2.0 0.59 0.041
2.0 0.59 0.042
2.1 0.59 0.043
2.2 0.60 0.045
2.3 0.58 0.048
2.3 0.59 0.048
2.3 0.57 0.048
2.4 0.57 0.049
2.3 0.59 0.048
2.5 0.58 0.051
2.5 0.59 0.052
2.4 0.58 0.050
2.5 0.58 0.052
2.6 0.59 0.053
2.5 0.60 0.052
2.6 0.61 0.054
2.6 0.60 0.054
2.6 0.61 0.054
2.5 0.61 0.052
2.5 0.62 0.052
2.6 0.61 0.053
Emission
Methane Unc Ibs/hr
16.2 0.37 0.178
16.3 0.38 0.179
16.3 0.38 0.179
16.3 0.37 0.180
16.4 0.38 d.180
16.4 0.37 0.181
16.5 0.38 0.182
16.4 0.38 0.181
16.3 0.39 0.179
16.4 0.39 0.181
16.2 0.39 0.179
17.2 0.41 0.190
17.0 0.41 0.188
16.8 0.41 0.185
16.6 0.41 0.184
16.7 0.42 0.184
16.7 0.42 0.184
16.4 0.41 0.181
16.3 0.43 0.180
16.2 0.41 0.179
16.1 0.42 0.178
16.1 0.41 0.178
16.1 0.41 0.178
16.0 0.42 0.177
16.0 0.41 0.177
16.0 0.42 0.177
16.0 0.41 0.177
16.1 0.41 0.177
16.2 0.42 0.179
16.2 0.42 0.179
16.3 0.43 0.180
16.5 0.43 0.182
16.7 0.43 0.184
16.8 0.43 0.185
16.8 0.44 0.185
17.0 0.43 0.187
i-Heptane Unc
4.2 0.3
4.2 0.3
4.2 0.3
4.2 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.3 0.3
3.8 0.3
3.8 0.3
3.9 0.3
4.0 0.3
4.1 0.3
4.2 0.3
4.2 0.3
4.3 0.3
4.3 0.3
4.3 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.4 0.3
4.5 0.3
4.5 0.3
4.6 0.3
4.5 0.3
4.6 0.3
4.5 0.3
4.6 0.3
4.6 0.3
4.7 0.3
4.7 0.3
4.7 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/27/97
Time
11:30
11:31
11:32
11:33
11:33
11:34
11:35
11:36
11:37
11:38
11:39
11:40
12:15
12:16
12:17
12:18
12.19
12:20
12:21
12:21
12:22
12:23
12.24
12:25
12:26
12:27
12:28
12:29
12:30
12:31
12:32
12:33
12:33
12:34
12:35
12:36
File
Name
16270106
16270107
16270108
16270109
16270110
16270111
16270112
16270113
16270114
16270115
16270116
16270117
16270152
16270153
16270154
16270155
16270156
16270157
16270158
16270159
16270160
16270161
16270162
16270163
16270164
16270165
16270166
16270167
16270168
16270169
16270170
16270171
16270172
16270173
16270174
16270175
Emissions
CO Unc Ibs/hr
878.6 12.76 17.0
868.4 11.77 16.8
878.7 1X21 17.0
880.6 12.50 17.0
871.5 11.86 16.8
865.9 1 1.79 16.7
857.3 11.45 16.5
848.0 11.24 16.4
834.2 11.04 16.1
824.7 10.81 15.9
815.7 10.64 15.7
806.3 10.57 15.6
840.4 11.52 16.2
836.4 11.38 16.1
831.1 11.12 16.0
827.8 11.02 16.0
821.2 11.13 15.9
814.6 10.83 15.7
816.1 11.07 15.8
817.5 11.14 15.8
811.4 10.82 15.7
813.7 11.15 15.7
811.6 10.89 15.7
813.9 10.91 15.7
819.4 11.23 15.8
827.2 11.33 16.0
841.1 11.83 16.2
846.8 11.98 16.3
852.0 12.18 16.4
862.3 12.42 16.6
855.7 12.03 16.5
862.3 12.26 16.6
857.4 12.19 16.6
846.9 11.65 16.3
849.3 12.20 16.4
845.6 11.83 16.3
Emissions
SO2 Unc Ibs/hr
64.3 2.19 2.836
66.2 2.18 2.920
69.9 2.15 3.083
75.1 2.14 3.315
80.0 2.14 3.529
86.8 2.12 3.830
92.0 2.11 4.061
95.8 2.10 4.229
97.6 2.07 4.308
96.4 2.05 4.254
92.9 2.02 4.099
87.6 1.99 3.866
60.8 2.15 2.684
62.6 2.14 2.761
63.8 2.17 2.815
63.4 2.17 2.799
61.5 2.15 2.714
58.7 2.14 2.592
55.0 2.16 2.427
52.5 2.17 2.317
50.1 2.18 2.210
47.8 2.18 2.107
45.4 2.17 2.001
43.1 2.16 1.903
42.4 2.20 1.872
42.7 2.19 1.884
44.0 2.24 1.940
45.5 2.26 2.009
47.0 2.27 2.072
49.4 2.30 2.181
52.1 2.30 2.298
56.6 2.33 2.498
61.0 2.27 2.690
66.0 2.28 2.911
71.1 2.24 3.137
77.0 2.26 3.398
Formal- Emission
dehyde Unc Ibs/hr
2.6 0.61 0.055
2.6 0.61 0.054
2.7 0.61 0.056
2.9 0.59 0.059
3.0 0.59 0.062
3.1 0.59 0.064
3.1 0.59 0.065
3.2 0.59 0.066
3.2 0.58 0.066
3.2 0.57 0.066
3.1 0.57 0.065
3.2 0.56 0.065
1.8 0.62 0.037
2.0 0.62 0.042
2.1 0.64 0.044
2.2 0.63 0.045
2.3 0.63 0.047
2.2 0.63 0.046
2.3 0.64 0.047
2.2 0.64 0.046
2.2 0.65 0.046
2.4 0.65 0.050
2.7 0.65 0.055
2.8 0.64 0.059
2.9 0.65 0.060
3.0 0.66 0.061
3.0 0.67 0.062
3.0 0.68 0.063
3.0 0.68 0.063
3.1 0.69 0.065
3.1 0.69 0.065
3.3 0.71 0.068
3.4 0.70 0.070
3.5 0.70 0.072
3.6 0,69 0.074
3.7 0.70 0.077
Emissions
Methane Unc Ibs/hr
16.9 0.43 0.186
16.8 0.43 0.186
16.7 0.43 0.184
16.7 0.42 0.185
16.5 0.42 (J.I82
16.4 0.42 0.181
16.2 0.42 0.179
15.9 0.41 0.176
15.7 0.41 0.173
15.5 0.40 0.171
15.3 0.40 0.168
15.1 0.40 0.167
15.9 0.44 0.176
16.0 0.44 0.176
15.9 0.45 0.176
15.9 0.45 0.175
15.8 0.45 0.175
15.7 0.45 0.173
15.7 0.45 0.174
15.8 0.46 0.174
15.7 0.46 0.173
15.7 0.46 0.174
15.7 0.46 0.173
15.8 0.45 0.174
16.0 0.46 0.176
16.1 0.47 0.178
16.4 0.48 0.181
16.5 0.48 0.182
16.6 0.48 0.183
16.8 0.49 0.185
16.9 0.49 0.186
16.9 0.50 0.186
16.9 0.50 0.186
16.8 0.50 0.185
16.9 0.48 0.187
16.9 0.49 0.187
i-Heptane Unc
4.7 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.6 0.3
4.6 0.3
4.6 0.3
4.6 0.3
4.2 0.3
4.2 0.3
4.3 0.3 I
4.3 0.3 1
4.4 0.3
4.5 0.3
4.5 0.3
4.5 0.3
4.6 0.3
4.6 0.3
4.6 0.3
4.6 0.3
4.7 0.3
4.6 0.3
4.7 0.3
4.7 0.3
4.7 0.3
4.8 0.3
4.7 0.3
4.7 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/27/97
Time
12:37
12:38
12:39
12:40
12:41
12:42
12:42
12:43
12:44
13:22
13:25
13:29
13:34
13:41
13:45
File
Name
16270176
16270177
16270178
16270179
16270180
16270181
16270182
16270183
16270184
NLS4M7
NLS4MS
NLS4M9
NLS4010
NLS4011
NLS4012
Average — >
Emissions
CO Unc Ibs/hr
846.3 12.11 16.3
833.2 11.50 16.1
839.5 11.80 16.2
834.2 11.70 16.1
834.1 11.73 16.1
832.1 11.76 16.1
835.2 11.74 16.1
83S.1 11.69 16.1
838.3 11.67 16.2
(90.5 83 133
(I5J tS 13.2
(91.1 M 133
718.2 8J 13.9
(723 8.2 13.0
(57.2 8.1 12.7
847.6 11.59 16.4
Emissions
SO2 Unc Ibs/hr
81.9 2.23 3.612
85.2 2.22 3.759
87.5 2.25 3.860
88.9 2.23 3.924
89.9 2.21 3.966
91.3 2.20 4.031
93.2 2.21 4.112
96.3 2.21 4.251
99.9 2.23 4.406
(1.4 I* 2.7*7
54.2 1.9 2391
43.7 1.9 l.»3«
40.9 1.9 2417
59.0 1.8 2403
48.1 IJ 2.124
83.3 2.12 3.675
Formal- Emissions
dehyde Unc Ibs/hr
3.8 0.69 0.080
3.9 0.68 0.080
4.0 0.70 0.083
4.0 0.69 0.083
4.1 0.68 0.085
4.2 0.67 0.088
4.4 0.68 0.090
4.7 0.68 0.097
4.7 0.69 0.098
4.0 04 0.0*2
3J 0.( 0.079
3.7 04 0.077
3.» 0.( 0.011
3.7 0.5 0.077
3.9 0.5 0.080
3.0 0.59 0.063
Emissions
Methane Unc Ibs/hr
16.9 0.49 0.186
16.9 0.48 0.186
16.9 0.49 0.186
16.8 0.49 0.185
16.7 0.48 6.184
16.8 0.47 0.185
16.7 0.48 0.184
16.7 0.48 0.184
16.6 0.49 0.183
143 0.4 0.157
14.1 0.4 0.155
14.0 0.4 0.155
143 0.4 0.157
12.4 0.4 0.137
11.4 0.4 0.126
16.2 0.42 0.179
i-Heptane Unc
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
4.8 0.3
2.2 03
23 03
2.4 03
3.0 03
3.2 0.2
33 0.2
4.4 0.3
Date
6/25/97
Time
9:27
9:33
9:37
9:43
9:54
9:58
10:02
10:36
10:39
10:43
10:47
11:13
11:18
11:24
11:29
12:20
12:26
File
Name
1NLS1001
INLS2002
INLS2003
INLS2004
INLS2005
lNLS200t
INLS2007
INLV2008
INLV2009
INLV2010
INLV201 1
INLV20I2
INLV20I3
INLV2014
INLV2015
INLV20I6
INLV20I7
Emissions
Ethylene Unc Ibs/hr
1.9 0.5 0.03(
24 0.4 0.049
2.7 0.5 0.051
13 0.5 0.047
34 0.5 0.0(9
34 0.5 O.M9
33 OS 0.068
3.6 0.52 0.070
3.3 0.52 0.063
3.2 0.52 0.063
3.2 0.53 0.062
3.2 0.51 0.062
3.2 0.52 0.062
3.2 0.52 0.062
3.3 0.53 0.063
6.4 0.54 0.123
7.0 0.55 0.136
Emissions
\mmonia Unc Ibs/hr
14 03 0.019
3.5 03 0.041
43 0.4 0.050
3.8 0.4 0.045
43 0.4 0.051
4.8 0.4 0.05*
4.9 0.4 0.058
3.1 0.4 0.037
4.6 0.4 0.054
5.5 0.4 0.064
5.7 0.4 0.067
3.4 0.4 0.039
4.6 0.4 0.054
4.6 0.4 0.054
4.9 0.4 0.057
3.4 0.4 0.040
4.6 0.4 0.053
Emissions
Toluene Unc Ibs/hr
48.1 0.7 0.5
2(.7 OJ 03
2(4 OJ 03
2(J 0.9 03
1.2
U
1.2
1.3
1.3
1.4
1.3
1.3
1.3
1.4
1.4
7.8 1.0 0.086
8.4 1.0 0.093
1-Pentene Unc
4.1 04
3J 04
3J 04
4.0 0.7
33 04
3.1 04
2J 04
4.1 0.7
3.2 0.7
3.2 0.7
3.2 0.7
3.6 0.7
3.4 0.7
3.8 0.7
3.7 0.7
9.9 0.8
9.9 0.8
2-Methyl-
2-Bulene Unc
04
04
0.7
0.7 04
04
04
04
0.7
0.7
0.7
0.7
0.7
0.7
0.7
0.7
2.3
2.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/25/97
Time
12:30
12:34
12:54
12:59
13:03
13:06
13:46
13:49
13:52
13:56
14:17
14:21
14:27
14:32
14:56
1500
15:05
15:09
15:34
15:38
15:42
15:46
16:13
16:17
16.22
16:26
16:54
16:58
17:07
17:1*
17:14
17:20
17:24
17:27
File
Name
INLV2018
INLV20I9
1NLV2020
INLV2021
INLV2022
1NLV2023
INLV2024
1NLV2025
INLV2026
INLW027
INLV2028
INLV2029
INLV2030
INLV2031
INLV2032
INLV2033
INLV2034
1NLV2035
INLV2036
INLW037
INLV2038
INLV2039
1NLV2040
INLV2041
1NLV2042
1NLV2043
INLV2047
1NLV2048
INLS2049
1NLS2050
1NLS20S1
INLS2052
INLS2053
INLS20S4
Average — >
Emissions
Ethylene Unc Ibs/hr
7.0 0.55 0.135
6.7 0.56 0.129
4.9 0.54 0.095
5.0 0.56 0.097
5.2 0.55 0.100
4.9 0.56 0.095
4.3 0.55 0.083
4.1 0.54 0.080
4.0 0.54 0.078
3.8 0.55 0.073
3.5 0.56 0.067
3.7 0.58 0.071
3.5 0.59 0.068
3.8 0.60 0.074
3.0 0.53 0.058
3.1 0.54 0.061
3.1 0.55 0.060
3.3 0.56 0.064
3.6 0.56 0.070
3.4 0.57 0.066
3.3 0.57 0.063
3.4 0.56 0.066
3.2 0.55 0.062
3.3 0.55 0.063
3.5 0.54 0.067
3.6 0.56 0.070
3.4 0.6 0.067
3.4 0.6 0.066
3.2 OS 0.«*2
33 05 0.064
33 05 0.043
2.7 05 0.052
2.8 05 0.054
2.9 05 O.OS6
4.0 0.55 0.077
Emissions
Vmmonia Unc Ibs/hr
5.1 0.4 0.060
5.2 0.4 0.061
3.) 0.4 0.036
4.1 0.4 0.048
4.3 0.4 0.050
4.7 0.4 0.055
6.2 0.4 0.073
6.7 0.4 0.079
7.2 0.4 0.085
7.2 0.4 0.085
3.4 0.4 0.040
4.5 0.5 0.053
3.2 0.5 0.037
4.3 0.5 0.050
3.1 0.4 0.036
4.0 0.4 0.046
4.4 0.4 0.052
4.5 0.4 0.053
4.2 0.4 0.050
5.2 0.5 0.061
5.2 0.5 0.061
5.7 0.4 0.067
3.3 0.4 0.038
4.0 0.4 0.047
4.1 0.4 0.048
4.8 0.4 0.056
3.3 0.5 0.039
4.4 0.5 0.052
35 0.4 0441
4.0 0.4 0.047
4.0 0.4 0.04*
4.1 0.4 0.04*
3.» 0.4 0.046
4.2 0.4 0.050
4.6 0.4 0.054
Emission
Toluene Unc Ibs/hr
8.5 1.0 0.094
8.3 1.1 0.092
6.6 1.0 0.072
6.6 1.1 0.073
6.7 1.1 0.074
6.7 1.1 0.074
6.3 1.1 0.069
6.4 I.I 0.070
6.2 I.I 0.068
6.2 I.I 0.068
5.7 1.1 0.062
5.6 I.I 0.062
4.0 1.3 0.044
5.7 1.2 0.063
4.4 1.1 0.049
4.7 1.1 0.051
4.9 I.I O.Q54
4.9 I.I 0.054
4.7 1.2 0.052
4.9 1.2 0.054
4.7 1.2 0.051
4.8 1.1 0.053
4.2 1.1 0.046
4.5 I.I 0.050
4.5 1.1 0.049
4.7 1.2 0.052
1.7
1.7
35 14 OJ3»
M
15
32J 1.1 0.363
34 J M 0-375
34.* 1.1 OJ82
4.2 1.2 0.047
1-Pentene Unc
9.5 0.8
9.3 0.8
7.2 0.8
7.6 0.8
7.3 0.8
7.1 0.8
7.3 0.8
7.4 0.8
7.0 0.8
7.0 0.8
7.2 0.8
7.3 0.9
8.7 1.0
8.4 0.9
6.8 0.8
6.8 0.8
7.1 0.8
7.2 0.8
7.1 0.9
6.5 0.9
6.7 0.9
6.0 0.8
6.4 0.9
6.2 0.8
6.3 0.8
6.7 0.9
6.5 0.9
6.4 0.9
45 0.7
4J 0.8
5J OJ
5J 03
53 OJ
5.2 0.8
6.6 0.8
2-Methyl-
2-Bulene Unc
2.3
2.4
2.3
2.4
1 2.4
2.4
2.4
2.4
2.4
2.4-
2.5
2.6
2.1 0.8
2.7
2.4
2.4
2.5
2.5
2.7
2.6
2.6
2.6
26
2.6
2.6
2.6
2.7
2.7
2.2
23
2.4
1.2 0.7
IJ 0.7
1.4 0.7
0. 1 2. 1
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
6/26/97
Time
9:11
•:1«
9:22
9:34
9:3«
9:42
10:55
10:56
10:57
10:58
10:59
11:00
11:00
11:01
11:02
11:03
11:04
11:05
11.06
11:07
11:08
11:09
11:09
11:10
11:11
11:12
11:13
11:14
11:15
11:16
11:17
11:18
11:19
11:20
11:21
11.21
File
Name
INLS3001
1NLS3M2
1NLS3M3
INLS3004
INLS3005
INLS30M
16260004
16260005
16260006
16260007
16260008
16260009
16260010
16260011
16260012
16260013
16260014
16260015
16260016
16260017
16260018
16260019
16260020
16260021
16260022
16260023
16260024
16260025
16260026
16260027
16260028
16260029
16260030
16260031
16260032
16260033
Emissions
Ethylene Unc Ibs/hr
3.4 0.4 •-•**
3.2 0.4 0.041
3J 03 0.0*4
2.1 0.4 0.041
2.5 0.4 M4>
13 0.4 0.041
3.6 0.51 0.070
3.7 0.52 0.071
3.7 0.52 0.072
3.8 0.52 0.073
3.8 0.52 0.074
3.9 0.53 0.075
3.9 0.54 0.075
3.9 0.53 0.075
4.0 0.54 0.077
4.0 0.54 0.077
4.0 0.53 0.077
4.1 0.54 0.079
4.2 0.55 0.080
4.2 0.55 0.081
4.3 0.55 0.083
4.3 0.55 0.082
4.3 0.56 0.083
4.3 0.56 0.083
4.3 0.55 0.083
4.3 0.55 0.083
4.3 0.55 0.082
4.2 0.55 0.081
4.1 0.54 0.080
4.0 0.53 0.078
4.0 0.53 0.078
4.0 0.53 0.077
4.1 0.53 0.078
4.1 0.53 0.078
4.1 0.52 0.079
4.1 0.52 0.080
Emissions
\mmonia Unc Ibs/hr
1.4 oj 0.01*
1J 03 0.011
2J OJ 0.027
2.1 OJ 0.025
2.9 OJ 0.034
2.9 OJ 0.034
4.3 0.4 0.050
5.1 0.4 0.060
5.6 0.4 0.066
6.0 0.4 0.070
6.2 0.4 0.073
6.4 0.4 0.075
6.6 0.4 0.078
6.7 0.4 0.079
6.7 0.4 0.079
6.8 0.4 0.080
6.8 0.4 0.080
7.0 0.4 0.082
7.2 0.4 0.085
7.4 0.4 0.087
7.5 0.4 0.088
7.7 0.4 0.090
7.8 0.4 0.091
7.9 0.4 0.092
8.0 0.4 0.093
8.0 0.4 0.094
8.0 0.4 0.094
8.0 0.4 0.094
8.1 0.4 0.095
8.1 0.4 0.095
8.0 0.4 0.094
8.0 0.4 0.094
7.9 0.4 0.093
8.0 0.4 0.094
8.1 0.4 0.095
8.1 0.4 0.095
Emission
Toluene Unc Ibs/hr
4.0 0.7 0.044
4.1 0.7 0.045
4.1 0.7 0.045
32.5 0.7 OJ5<
33.5 OJ OJ*9
33.4 OJ OJM
4.3 0.9 0.047
4.3 0.9 0.047
4.5 0.9 0.050
4.4 0.9 0.049
4.7 0.9 0.051
4.7 0.9 0.051
4.7 0.9 0.052
5.0 0.9 0.055
4.9 0.9 0.054
4.8 0.9 0.053
4.9 0.9 0.054
4.8 1.0 0.053
5.3 1.0- 0.058
5.2 1.0 0.058
5.3 1.0 0.058
5.3 1.0 0.058
5.1 1.0 0.057
5.2 1.0 0.057
5.0 1.0 0.055
5.0 1.0 0.055
5.0 1.0 0.055
5.1 1.0 0.056
5.0 1.0 0.055
4.9 0.9 0.054
4.8 0.9 0.052
4.7 0.9 0.052
4.8 0.9 0.052
4.7 0.9 0.051
4.7 0.9 0.052
4.9 0.9 0.054
1-Pentene Unc
4.7 OJ
3.5 03
3J OJ
3J 0.*
3.7 04
3.* 0.*
3.0 0.7
2.9 0.7
2.8 0.7
2.8 0.7
2.9 0.7
2.8 0.7
2.8 0.7
2.8 0.7
2.8 0.7
2.8 0.7
2.8 0.7
2.7 0.7
3.0 0.7
3.0 0.7
3.1 0.7
3.1 0.7
3.0 0.7
3.0 0.7
2.9 0.7
3.0 0.7
2.7 0.7
2.6 0.7
2.7 0.7
2.4 0.7
2.3 0.7
2.4 0.7
2.4 0.7
2.4 0.7
2.3 0.7
2.4 0.7
2-Methyl-
2-Butene Unc
13
1.5
1.5
1.4 03
1 1.0 03
1.0 03 1
2.0
2.0
2.0
2.0
2.0
2.0
2.1
2.1
2.1
0.8
0.7
0.8
0.8
0.8 1
0.8 1
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.8
0.7
0.8
0.7
0.8
0.7
0.7
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
11:22
11:57
11:58
11:59
12:00
12:01
1202
12:02
12:03
12:04
12:05
124)6
12,07
12:08
12:09
12:10
12:10
12:11
12:12
12:13
12:14
12:15
12:16
12:17
12:18
12:19
12:34
12:34
12:35
12:36
12:37
12:38
12:39
12:40
12:41
12:42
File
Name
16260034
16260067
16260068
16260069
16260070
16260071
16260072
16260073
16260074
16260075
16260076
16260077
16260078
16260079
16260080
16260081
16260082
16260083
16260084
16260085
16260086
16260087
16260088
16260089
16260090
16260091
16260103
16260104
16260105
16260106
16260107
16260108
16260109
162601 10
162601 1 1
16260112
Emissions
Ethylene Unc Ibs/hr
4.2 0.53 0.081
5.1 0.53 0.098
5.1 0.53 0.098
5.1 0.54 0.099
5.2 0.54 0.100
5.2 0.54 0.101
5.4 0.54 0.104
5.5 0.54 0.106
5.6 0.54 0.107
5.5 0.54 0.107
5.7 0.54 0.109
5.7 0.54 0.110
5.8 0.54 0.112
5.8 0.54 0.112
5.9 0.54 0.114
6.0 0.55 0.115
6.1 0.54 0.117
6.0 0.54 0.116
6.0 0.55 0.117
6.1 0.55 0.117
6.1 0.55 0.118
6.1 0.54 0.118
6.1 0.54 0.118
6.2 0.55 0.119
6.1 0.55 0.118
6.2 0.55 0.119
6.5 0.56 0.126
6.4 0.56 0.124
6.4 0.56 0.124
6.4 0.56 0.123
6.5 0.56 0.125
6.5 0.56 0.127
6.5 0.57 0.126
6.5 0.56 0.127
6.5 0.56 0.125
6.4 0.56 0.125
Emissions
Ammonia Unc Ibs/hr
8.1 0.4 0.096
6.7 0.4 0.079
7.1 0.4 0.083
7.3 0.4 0.085
7.5 0.4 0.088
7.5 0.4 0.089
7.7 0.4 0.090
7.8 0.4 0.092
8.0 0.4 0.093
8.0 0.4 0.094
7.9 0.4 0.093
8.0 0.4 0.094
8.1 0.4 0.095
8.3 0.4 0.097
8.3 0.4 0.098
8.3 0.4 0.098
8.3 0.4 0.098
8.3 0.4 0.098
8.4 0.4 0.098
8.4 0.4 0.099
8.4 0.4 0.099
8.3 0.4 0.097
8.3 0.4 0.098
8.3 0.4 0.098
8.4 0.4 0.099
8.4 0.4 0.099
7.5 0.4 0.088
7.9 0.4 0.093
8.3 0.4 0.098
8.6 0.4 0.101
9.0 0.4 0.106
9.4 0.4 0.1 10
9.6 0.5 0.113
9.7 0.4 0.114
9.8 0.4 0.115
9.9 0.4 0.116
Emission
Toluene Unc Ibs/hr
5.0 0.9 0.055
5.1 1.0 0.056
4.9 1.0 0.054
5.0 1.0 0.056
5.3 i.O 0.058
5.3 1.0 0.058
5.4 1.0 0.059
5.4 1.0 0.060
5.8 1.0 0.063
5.8 1.0 0.064
5.9 1.0 0.065
6.1 1.0 0.068
5.8 1.0 0.064
6.0 1.0 0.066
5.9 1.0 0.065
6.2 1.0 0.069
6.1 1.0 0.067
6.2 1.0 0.069
6.0 1.0 0.066
6.3 1.0 0.070
6.3 1.0 0.070
6.2 1.0 0.068
6.1 1.0 0.067
6.2 1.0 0.068
6.3 1.0 0.069
6.2 1.0 0.068
6.4 1.0 0.070
6.4 1.0 0.070
6.1 1.0 0.067
6.3 1.0 0.069
6.4 1.0 0.071
6.6 1.0 0.073
6.5 1.0 0.071
6.4 1.0 0.070
6.3 1.1 0.070
6.3 1.0 0.070
1-Pentene Unc
2.3 0.7
3.6 0.7
3.6 0.7
3.7 0.7
3.8 0.7
3.8 0.7
3.8 0.7
4.0 0.7
4.0 0.7
4.0 0.7
4.0 0.7
4.0 0.7
4.1 0.7
4.2 0.7
4.2 0.7
4.4 0.7
4.4 0.7
4.4 0.7
4.4 0.7
4.5 0.7
4.5 0.7
4.5 0.7
4.5 0.7
4.6 0.8
4.6 0.7
4.6 0.7
5.1 0.8
5.1 0.8
5.1 0.8
5.1 0.8
5.2 0.8
5.2 0.8
5.2 0.8
5.0 0.8
5.1 0.8
5.1 0.8
2-Methyl-
2-Butene Unc
0.8
2.2
2.2
2.2
' . 2.2
22
2.1
2.2
2.2
0.8
0.8
0.8
2.2
2.2
0.8
0.8
0.8
0.8
0.8
0.8
0.8
2.2
2.2
2.2
0.8
2.2
2.3
2.3
2.3
2.3
2.3
2.3
2.3
2.3
2.3
2.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
12:43
12:44
12:44
12:45
12:46
12:47
12.48
12:49
12:50
12:51
12:52
12:53
12:54
12:54
12:55
12:56
12:57
12:58
12:59
13:00
13:01
13:02
13:03
13:04
14:00
14:00
14:01
14:02
14:03
14:04
14:05
14:06
14:07
14:08
14:09
14:09
File
Name
16260113
16260114
16260115
162601 16
16260117
16260118
16260119
16260120
16260121
16260122
16260123
16260124
16260125
16260126
16260127
16260128
16260129
16260130
16260131
16260132
16260133
16260134
16260135
16260136
16260165
16260166
16260167
16*260168
16260169
16260170
16260171
16260172
16260173
16260174
16260175
16260176
Emissions
Ethylene Unc Ibs/hr
6.5 0.56 0.126
6.5 0.56 0.126
6.5 0.56 0.126
6.5 0.55 0.126
6.6 0.55 0.128
6.7 0.55 0.129
6.6 0.55 0.128
6.7 0.55 0.130
6.7 0.56 0.129
6.9 0.56 0.132
6.9 0.56 0.134
7.0 0.57 0.135
7.3 0.57 0.140
7.4 0.57 0.144
7.6 0.57 0.146
7.6 0.58 0.148
7.6 0.58 0.147
7.6 0.59 0.147
7.6 0.58 0.146
7.4 0.58 0.143
7.3 0.57 0.141
7.2 0.58 0.140
7.1 0.57 0.138
7.0 0.57 0.135
3.6 0.51 0.070
3.6 0.52 0.070
3.7 0.52 0.071
3.6 0.52 0.071
3.6 0.52 0.070
3.6 0.52 0.070
3.6 0.51 0.070
3.6 0.52 0.070
3.6 0.52 0.070
3.7 0.51 0.071
3.7 0.52 0.071
3.7 0.52 0.071
Emissions
\mmonia Unc Ibs/hr
9.8 0.4 0.116
9.8 0.4 0.115
9.8 0.4 0.115
9.8 0.4 0.115
9.9 0.4 0.116
10.1 0.4 0.119
10.3 0.4 0.121
10.3 0.4 0.121
10.3 0.4 0.121
10.3 0.4 0.120
10.2 0.4 0.120
10.1 0.5 0.119
10.0 0.4 0.118
10.0 0.5 0.117
9.9 0.5 0.117
10.0 0.5 O.I 17
10.1 0.5 0.118
10.1 0.5 0.118
9.9 0.5 0.117
9.8 0.5 0.115
9.6 0.5 0.113
9.5 0.5 0.1 11
9.3 0.5 0.110
9.2 0.5 0.109
6.3 0.4 0.074
6.5 0.4 0.077
6.7 0.4 0.079
7.0 0.4 0.082
7.2 0.4 0.084
7.4 0.4 0.087
7.7 0.4 0.090
7.9 0.4 0.093
8.1 0.4 0.095
8.2 0.4 0.097
8.3 0.4 0.098
8.4 0.4 0.098
Emission
Toluene Unc Ibs/hr
6.6 1.0 0.073
6.7 1.0 0.074
6.5 1.0 0.072
6.6 1.0 0.073
6.5 1.0 0.071
6.4 1.0 0.070
5.7 1.1 0.063
5.8 1.1 0.064
6.6 1.0 0.073
5.8 1.1 0.064
6.8 1.0 0.075
6.6 1.1 0.073
6.9 1.1 0.076
7.2 1.1 0.080
7.6 1.1 0.084
7.4 1.1 0.081
7.6 1.1 0.084
7.3 1.1 0.080
7.5 1.1 0.083
7.2 1.1 0.079
7.1 1.1 0.078
6.1 1.2 0.068
5.9 1.2 0.065
5.7 1.2 0.063
6.1 1.0 0.067
6.0 1.0 0.066
6.1 1.0 0.067
6.1 1.0 0.067
5.9 1.0 0.065
6.0 1.0 . 0.066
6.2 1.0 0.068
6.0 1.0 0.067
6.1 1.0 0.068
6.0 1.0 0.067
5.9 1.0 0.065
6.1 1.0 0.068
1-Pentene Unc
5.0 0.8
4.9 0.8
4.9 0.8
4.8 0.8
4.9 0.8
4.9 0.7
4.1 0.9
4.2 0.9
5.1 0.8
4.2 0.9
5.2 0.8
5.4 0.8
5.6 0.8
5.9 0.8
5.7 0.9
6.1 0.8
6.2 0.8
6.1 0.8
5.7 0.9
5.8 0.8
5.8 0.8
5.1 0.9
4.7 1.0
4.5 1.0
5.8 0.7
6.0 0.7
6.0 0.7
5.9 0.7
5.8 0.7
6.0 0.8
5.9 0.7
5.9 0.7
5.8 0.7
5.8 0.7
5.7 0.8
5.8 0.8
2-Methyl-
2-Butene Unc
0.8
0.8
2.3
2.3
1 2.3
2.2
1.3 0.7
1.4 0.7
2.3
1.5 0.7
2.3
2.4
2.3
2.4
2.4
2.4
2.4
2.4
2.4
24
24
1.6 0.8
1.7 0.8
1.6 0.8
2.2
2.3
2.3
2.2
2.3
"
22
2.3
2.3
2.2
2.3
2.3
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
14:10
14:11
14:12
14:13
14:14
14:15
14:16
14:17
14:18
14:18
14:19
14:20
14:21
14.22
14:23
14:24
14:25
14:26
14.27
14:28
1506
1507
15:08
15.O9
15:10
15:10
15:11
15:12
15:13
15:14
15:15
15:16
15.17
15:18
15:19
15:19
File
Name
16260177
16260178
16260179
16260180
16260181
16260182
16260183
16260184
16260185
16260186
16260187
16260188
16260189
16260190
16260191
16260192
16260193
16260194
16260195
16260196
16260234
16260235
16260236
16260237
16260238
16260239
16260240
16260241'
16260242
16260243
16260244
16260245
16260246
16260247
16260248
16260249
Emissions
Ethylene Unc Ibs/hr
3.6 0.52 0.071
3.7 0.52 0.071
3.7 0.53 0.072
3.7 0.53 0.072
3.7 0.53 0.072
3.7 0.53 0.072
3.7 0.53 0.073
3.8 0.53 0.073
3.8 0.54 0.073
3.8 0.54 0.073
3.8 0.54 0.073
3.7 0.53 0.072
3.7 0.54 0.072
3.7 0.53 0.071
3.7 0.53 0.071
3.6 0.53 0.070
3.6 0.53 0.070
3.6 0.53 0.070
3.6 0.53 0.070
3.7 0.53 0.071
3.6 0.53 0.069
3.5 0.53 0.067
3.5 0.53 0.068
3.5 0.53 0.067
3.5 0.53 0.068
3.5 0.53 0.067
3.5 0.54 0.068
3.5 0.53 0.067
3.4 0.53 0.066
3.4 0.53 0.065
3.4 0.53 0.065
3.4 0.53 0.067
3.4 0.53 0.065
3.5 0.53 0.067
3.5 0.53 0.067
3.4 0.53 0.066
Emissions
\mmonia Unc Ibs/hr
8.5 0.4 0.100
8.6 0.4 0.101
8.7 0.4 0.102
8.7 0.4 0.102
8.7 0.4 0.102
8.7 0.4 0.103
8.9 0.4 0.105
9.0 0.4 0.106
9.0 0.4 0.106
9.1 0.4 0.107
9.1 0.4 0.107
9.0 0.4 0.106
9.0 0.4 0.106
9.0 0.4 0.106
8.9 0.4 0.105
9.0 0.4 0.106
9.1 0.4 0.107
9.3 0.4 0.109
9.4 0.4 0.110
9.3 0.4 0.110
4.9 0.4 0.058
5.3 0.4 0.062
5.8 0.4 0.068
6.1 0.4 0.071
6.4 0.4 0.075
6.6 0.4 0.077
6.8 0.4 0.080
7.0 0.4 0.082
7.1 0.4 0.083
7.2 0.4 0.085
7.4 0.4 0.086
7.5 0.4 0.088
7.7 0.4 0.090
7.8 0.4 0.092
7.9 0.4 0.093
8.0 0.4 0.094
Emission
Toluene Unc Ibs/hr
6.0 .0 0.066
6.2 .0 0.068
6.1 .0 0.067
6.2 .0 0.068
6.1 .0 0.068
6.2 .0 0.068
6.2 .1 0.069
6.1 .0 0.068
6.5 .1 0.071
6.3 .1 0.070
6.2 .1 0.068
6.3 1.1 0.070
6.2 1.1 0.068
6.2 1.1 0.068
6.1 1.1 0.068
6.2 1.1 0.069
6.0 1.0 0.066
6.0 1.1 0.066
6.2 1.6 0.069
5.9 1.0 0.066
5.6 1.0 0.062
5.5 1.0 0.061
5.4 1.1 0.059
5.5 1.1 0.060
5.6 1.1 0.062
5.5 I.I 0.061
5.4 .1 0.060
5.2 .1 0.057
5.5 .1 0.060
5.3 .0 0.059
5.5 .1 0.060
5.5 1.1 0.060
5.7 1.1 0.063
5.6 1.0 0.062
5.5 I.I 0.061
4.9 l.l 0.055
1 -Pentene Unc
5.7 0.7
5.8 0.8
5.8 0.8
5.9 0.8
5.7 0.8
5.9 0.8
5.9 0.8
5.8 0.8
5.9 0.8
5.8 0.8
5.8 0.8
5.8 0.8
5.8 0.8
5.7 0.8
5.6 0.8
5.5 0.8
5.4 0.8
5.6 0.8
5.7 0.8
5.6 0.8
5.3 0.8
5.5 0.8
5.7 0.8
5.8 0.8
5.8 0.8
5.7 0.8
5.7 0.8
5.7 0.8
5.6 0.8
5.5 0.8
5.6 0.8
5.6 0.8
5.7 0.8
5.7 0.8
5.7 0.8
5.3 -0.9
Z-Methyl-
2-Butene Unc
2.3
2.3
2.3
2.3
1 2.3
2.3
2.4
2.3
2.4
2.4
2.4
2.4
2.4
2.4
2.4
2.4
2.3
2.4
2.3
2.3
2.3
2.3
2.4
2.4
2.4
2.4
2.4
2.4
2.4
2.3
2.4
2.4
2.4
2.3
2.4
1.0 0.7
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/26/97
Time
15:20
15.21
15:22
15:23
15:24
15:25
15:26
15:27
15:28
15:29
15:29
15:30
15:31
15:32
15:33
16:00
16:06
16:10
16:15
16:14
16:2*
16:33
File
Name
16260250
16260251
16260252
16260253
16260254
16260255
16260256
16260257
16260258
16260259
16260260
16260261
16260262
16260263
16260264
INLS3007
INLS3008
INLS3009
INLS3010
INLS3011
INLS3012
INLS3013
Avenge — >
Emissions
Ethylene Unc Ibs/hr
3.5 0.53 0.068
3.5 0.53 0.067
3.4 0.53 0.067
3.5 0.53 0.067
3.5 0.53 0.067
3.5 0.53 0.068
3.5 0.54 0.067
3.5 0.54 0.068
3.5 0.54 0.068
3.5 0.53 0.067
3.5 0.53 0.068
3.5 0.54 0.067
3.4 0.53 0.066
3.5 0.54 0.067
3.5 0.54 0.068
2.0 0.4 0.039
2.4 0.5 0.046
2.0 0.4 0.038
1.8 0.4 0.036
3.4 0.5 0.066
33 0.5 0.068
3.* 0.5 0.06*
4.8 0.54 0.092
Emissions
Vmmonia Unc Ibs/hr
8.1 0.4 0.095
8.0 0.4 0.094
8.0 0.4 0.094
8.0 0.4 0.094
8.2 0.4 0.096
8.2 0.4 0.096
8.3 0.4 0.097
8.4 0.4 0.099
8.5 0.4 0.100
8.5 0.4 0.100
8.5 0.4 0.100
8.5 0.4 0.100
8.4 0.4 0.099
8.4 0.4 0.099
8.5 0.4 0.100
3.2 OJ 0.03S
4.7 0.4 0.056
5.0 OJ 0.059
4.6 OJ 0.054
44 OJ O.OS7
5J OJ 0.062
S3 OJ 0.062
8.2 0.4 0.096
Emissions
Toluene Unc Ibs/hr
5.6 1.1 0.061
5.5 1.1 0.060
5.5 1.0 0.061
4.9 1.2 0.054
5.7 1.1 0.063
4.9 1.1 0.054
5.7 l.l 0.063
5.0 1.2 0.055
4.8 1.2 0.053
4.5 1.2 0.050
4.9 1.1 0.054
4.9 1.2 0.054
4.9 1.2 0.054
5.0 1.2 0.056
4.9 1.2 0.054
45.6 0.9 0.503
47.2 1.0 0420
50J 0.9 0.560
51.0 0.9 0563
5.5 OJ 0.061
4.4 OJ 0.049
4.5 OJ 0.049
5.8 1.0 0.063
1-Pentene Unc
5.6 0.8
5.8 0.8
5.7 0.8
5.3 0.9
5.8 0.8
5.3 0.9
5.9 0.8
5.4 0.9
5.3 0.9
5.2 0.9
5.3 0.9
5.3 0.9
5.2 0.9
5.3 0.9
5.4 0.9
5.1 0.7
5.6 0.7
5.1 0.7
5.0 0.7
4J 0.6
4.9 0.6
4.9 04
4.7 0.8
2-Methyl-
2-Butene Unc
2.4
2.4
2.3
1.0 0.7
1 0.8
1.0 0.7
2.4
1.0 0.8
1.1 0.7
1.2 0.8
1.2 0.7
1.2 0.8
1.1 0.7
1.2 0.8
1.2 0.8
1J 0.6
.1.7 0.6
14 0.6
IS 0.6
1.9
1.9
1.9
O.I 1.8
Date
6/27/97
Time
:21
:25
:29
:3S
:40
:44
10:21
10:22
File
Name
INLS4001
INLS4002
INLS4003
INLS4004
INLS4005
1NLS4006
16270035
16270036
Emissions
Ethylene Unc Ibs/hr
2J 0.4 OJ45
2.0 0.4 0.039
2.0 0.4 0.040
3.2 0.4 0.061
3.2 0.5 0.062
3.1 OS 0.061
3.4 0.48 , 0.065
3.3 0.47 0.063
Emissions
Vmmonia Unc Ibs/hr
3.5 OJ 0.041
4.0 OJ 0.047
4.7 OJ 0.055
4.6 OJ 0.054
4.7 0 J 0.055
4.7 OJ 0.055
4.7 0.38 0.056
4.8 0.37 0.057
Emissions
Toluene Unc Ibs/hr
3SJ OJ 0.419
37.5 0.7 0.414
37J 0.7 0.414
3.7 0.7 0.041
33 0.7 0.039
34 0.7 0.040
4.2 0.82 0.047
4.1 0.82 0.046
1-Pentene Unc
4.0 04
3.4 OJ
3J OJ
24 OJ
2.5 OJ
2.4 OJ
3.0 0.6
3.1 M
Z-Methyl-
2-Butene Unc
OJ OJ
1J OJ
1J OJ
0.9 OJ
OJ OJ
0.7 OJ
0.7
(12
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/2797
Time
10:23
10:23
10:24
10:25
10:26
10:27
10:28
10:29
10:30
10:31
10:32
10:33
10.33
10:34
10.35
10:36
10:37
10:38
10:39
10:40
10:41
10:42
10:42
10:43
10:44
10:45
10:46
10:47
10:48
10:49
11:07
11:08
11:09
11:10
11:11
11:12
File
Name
16270037
16270038
16270039
16270040
16270041
16270042
16270043
16270044
16270045
16270046
16270047
16270048
16270049
16270050
16270051
16270052
16270053
16270054
16270055
16270056
16270057
16270058
16270059
16270060
16270061
16270062
16270063
16270064
16270065
16270066
16270081
16270082
16270083
16270084
16270085
16270086
Emissions
Ethylene Unc Ibs/hr
32 0.47 0.062
3.2 0.47 0.062
3.1 0.47 0.060
3.1 0.47 0.059
3.0 0.46 0.058
3.0 0.46 0.058
2.9 0.46 0.056
2.9 0.46 0.056
2.9 0.45 0.056
2.9 0.45 0.057
2.9 0.45 0.056
2.9 0.46 0.057
2.9 0.46 0.055
2.9 0.47 0.057
3.0 0.48 0.057
3.0 0.47 0.058
3.1 0.48 0.059
3.1 0.48 0.061
3.1 0.49 0.060
3.2 0.49 0.062
3.2 0.49 0.062
3.3 0.49 0.063
3.2 0.48 0.063
3.3 0.49 0.064
3.3 0.49 0.064
3.3 0.49 0.065
3.3 0.49 0.064
3.3 0.50 0.064
3.3 0.50 0.065
3.2 0.50 0.063
3.7 0.53 0.071
3.7 0.53 0.071
3.6 0.53 0.070
3.6 0.52 0.070
3.6 0.53 0.069
3.5 0.53 0.068
Emissions
\mmonia Unc Ibs/hr
5.0 0.37 0.059
5.3 0.38 0.063
5.6 0.37 0.066
5.9 0.37 0.069
6.1 0.37 0.071
6.2 0.37 0.073
6.4 0.37 0.075
6.4 0.36 0.075
6.5 0.36 0.076
6.6 0.36 0.077
6.7 0.36 0.079
6.8 0.37 0.080
7.0 0.37 0.083
7.2 0.37 0.084
7.4 0.38 0.086
7.5 0.38 0.087
7.6 0.38 0.089
7.7 0.38 0.090
7.7 0.39 0.090
7.7 0.39 0.091
7.6 0.39 0.090
7.6 0.39 0.089
7.5 0.38 0.088
7.6 0.39 0.089
7.6 0.39 0.090
7.7 0.39 0.090
7.7 0.39 0.090
7.7 0.39 0.090
7.6 0.40 0.089
7.5 0.40 0.088
5.1 0.42 0.060
5.5 0.42 0.065
5.9 0.42 0.069
6.2 0.42 0.072
6.4 0.42 0.075
6.6 0.42 0.077
Emission
Toluene Unc Ibs/hr
4.2 0.83 0.046
1.16
1.14
1.15
1.13
1.12
1.13
1.13
1.10
1.12
1.12
1.15
1.17
1.17
1.22
1.16
1.18
1.20
1.22
1.20
1.21
1.21
1.17
1.21
1.20
1.22
1.22
1.24
1.24
1.26
4.4 0.97 0.049
1.33
1.33
1.33
1.34
1.35
1-Pentene Unc
3.2 0.6
2.3 0.7
2.3 0.7
2.2 0.7
2.0 0.7
1.9 0.6
1.8 0.7
1.9 0.7
1.7 0.6
1.8 0.6
1.7 0.6
1.7 0.7
1.8 0.7
1.8 0.7
1.9 0.7
1.9 0.7
2.0 0.7
2.0 0.7
2.0 0.7
1.9 0.7
1.9 0.7
2.0 0.7
2.0 0.7
2.1 0.7
2.0 0.7
2.0 0.7
1.9 0.7
2.1 0.7
2.1 0.7
2.0 0.7
3.0 0.7
2.2 0.8
2.1 0.8
2.0 0.8
2.0 0.8
1.8 0.8
2-Methyl-
2-Butene Unc
0.7
1.5 0.5
1.5 0.5
1.4 0.5
' 1.5 0.5
1.5 0.5
1.5 0.5
1.6 0.5
1.6 0.5
1.5 0.5
1.6 0.5
1.6 0.5
1.6 0.5
1.7 0.5
1.6 0.6
1.7 0.5
1.7 0.6
1.7 0.6
1.7 0.6
1.7 0.6
1.7 0.6
1.8 0.6
1.8 0.6
1.7 0.6
1.8 0.6
1.8 0.6
1.9 0.6
1.8 0.6
1.8 0.6
1.8 0.6
0.8
1.3 0.6
1.3 0.6
1.4 0.6
1.4 0.6
1.5 0.6
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/27/97
Time
11:13
11:14
11:15
11:15
11:16
11:17
11:18
11.19
11:20
11.21
11:22
11:23
11)24
11:24
11:25
11:26
11:27
11:28
11:29
11:30
11:31
11:32
11:33
11:33
11:34
11:35
11:36
11:37
11:38
1111'
11:40
12:15
12:16
12:17
12:18
12:19
File
Name
16270087
16270088
16270089
16270090
16270091
16270092
16270093
16270094
16270095
16270096
16270097
16270098
16270099
16270100
16270101
16270102
16270103
16270104
16270105
16270106
16270107
16270108
16270109
16270110
16270111
16270112
16270113
16270114
16270115
!',!/OII6
16270117
16270152
16270153
16270154
16270155
16270156
Emissions
Ethylene Unc Ibs/hr
3.5 0.53 0.068
3.5 0.53 0.067
3.4 0.52 0.066
3.4 0.52 0.065
3.4 0.51 0.066
3.3 0.51 0.065
3.3 0.52 0.064
3.3 0.52 0.063
3.5 0.52 0.068
3.4 0.52 0.065
3.3 0.51 0.064
3.4 0.51 0.065
3.4 0.52 0.065
3.4 0.53 0.066
3.4 0.52 0.066
3.5 0.53 0.067
3.5 0.53 0.067
3.6 0.53 0.070
3.5 0.53 0.068
3.5 0.53 0.068
3.4 0.52 0.067
3.5 0.52 0.067
3.5 0.51 0.067
3.5 0.51 0.067
3.3 0.51 0.065
3.3 0.51 0.064
3.2 0.50 0.062
3.1 0.50 0.061
3.1 0.49 0.059
3.0 0.48 0.058
3.0 0.48 0.058
3.4 0.51 0.066
3.4 0.51 0.066
3.4 0.52 0.066
3.4 0.52 0.067
3.4 0.52 0.066
Emissions
\mmonia Unc Ibs/hr
6.8 0.42 0.080
7.1 0.42 0.083
7.1 0.41 0.084
7.1 0.42 0.084
7.1 0.41 0.084
7.2 0.41 0.084
7.2 0.41 0.084
7.3 0.41 0.085
7.5 0.41 0.088
7.6 0.42 0.089
7.5 0.41 0.088
7.6 0.41 0.089
7.8 0.42 0.091
7.9 0.42 0.093
8.1 0.42 0.095
8.1 0.42 0.095
8.1 0.42 0.095
8.1 0.42 0.095
8.1 0.42 0.095
8.1 0.42 0.096
8.1 0.42 0.095
8.1 0.41 0.095
8.1 0.41 0.095
8.2 0.41 0.096
8.2 0.40 0.097
8.2 0.40 0.0%
8.1 0.40 0.095
8.0 0.39 0.094
8.0 0.39 0.094
8.0 0.39 0.094
8.0 0.38 0.094
5.3 0.41 0.062
5.7 0.41 0.067
6.1 0.41 0.071
6.3 0.41 0.074
6.6 0.41 0.077
Emission
Toluene Unc Ibs/hr
1.34
1.37
1.32
1.35
1.31
1.31
1.34
1.32
1.35
1.33
1.33
1.34
1.37
1.38
1.38
1.40
1.39
1.42
1.40
1.39
1.39
1.39
1.35
1.35
1.35
1.35
1.34
1.32
1.29
1.31
1.28
1.43
1.42
1.46
1.45
1.45
1-Pentene Unc
1.7 0.8
1.8 0.8
1.6 0.8
1.7 0.8
1.5 0.8
1.5 0.8
1.7 0.8
1.6 0.8
1.5 0.8
1.7 0.8
1.6 0.8
1.7 0.8
1.6 0.8
1.9 0.8
1.9 0.8
2.0 0.8
2.0 0.8
2.0 0.8
1.9 0.8
1.9 0.8
2.0 0.8
1.9 0.8
1.9 0.8
2.0 0.8
1.8 0.8
1.7 0.8
1.6 0.8
1.4 0.8
1.4 0.7
1.2 0.8
1.4 0.7
1.5 0.8
1.7 0.8
1.7 0.8
1.7 0.8
1.5 0.8
2-Methyl-
2-Butene Unc
1.5 0.6
1.5 0.6
1.5 0.6
1.5 0.6
'l.5 0.6
1.5 0.6
1.6 0.6
1.7 0.6 1
1.7 0.6 1
1.7 0.6
1.6 0.6
1.7 0.6
1.6 0.6
1.7 0.6
1.7 0.6
1.8 0.7
1.7 0.7
1.8 0.7
1.8 0.7
1.8 0.7
1.8 0.7
1.8 0.7
1.8 0.6
1.9 0.6
1.8 0.6
1.9 0.6
1.8 0.6
1.8 0.6
1.7 0.6
1.7 0.6
1.6 0.6
1.2 0.7
1.3 0.7
1.2 0.7
1.2 0.7
1.3 0.7
-------
TABLE B-l. CONTINUED (LTV Scrubber Inlet)
Date
6/27/97
Time
1220
12:21
12:21
12:22
12:23
12:24
12:25
12:26
12.27
12:28
12:29
12:30
12:31
12:32
12:33
12:33
12:34
12:35
12:36
12:37
12:38
12:39
12:40
12:41
12:42
12:42
12:43
12:44
13:22
13:25
13:29
13:34
13:41
13:45
File
Name
16270157
16270158
16270159
16270160
16270161
16270162
16270163
16270164
16270165
16270166
16270167
16270168
16270169
16270170
16270171
16270172
16270173
16270174
16270175
16270176
16270177
16270178
16270179
16270180
16270181
16270182
16270183
16270184
INLS4007
INLS4M8
INLS4M9
1NLS4010
1NLS4011
INLS4012
Average — >
Emissions
Ethylene Unc Ibs/hr
3.4 0.51 0.065
3.4 0.52 0.066
3.4 0.52 0.066
3.4 0.52 0.066
3.4 052 0.065
3.4 0.52 0.065
3.4 052 0.065
3.5 0.53 0.067
3.5 0.53 0.067
3.6 0.54 0.070
3.6 0.54 0.070
3.7 0.54 0.071
3.8 0.55 0.073
3.8 0.55 0.074
3.9 0.56 0.076
4.0 0.54 0.077
4.0 0.55 0.077
4.0 0.54 0.077
4.0 0.54 0.076
3.9 0.53 0.075
3.9 0.53 0.076
3.9 0.54 0.076
3.9 0.53 0.076
3.8 0.53 0.074
3.8 0.53 0.074
3.9 0.53 0.075
3.9 0.53 0.075
3.8 0.53 0.074
2.3 0.4 O.M4
2.1 0.4 0.041
2.2 05 0.042
4.2 05 0.0(2
3.6 05 0.070
3.2 05 0.063
3.4 0.51 0.066
Emissions
Vmmonia Unc Ibs/hr
6.7 0.41 0.079
6.9 0.41 0.081
7.0 0.41 0.082
7.1 0.42 0.084
7.4 0.42 0.086
7.5 0.41 0.088
7.5 0.41 0.089
7.6 0.42 0.090
7.7 0.42 0.091
7.8 0.43 0.092
7.9 0.43 0.092
7.9 0.43 0.092
7.9 0.44 0.092
7.8 0.44 0.092
7.9 0.44 0.093
g.O 0.43 0.094
8.1 0.43 0.095
8.2 0.43 0.096
8.1 0.43 0.096
8.1 0.43 0.095
8.0 0.42 0.094
8.0 0.43 0.094
7.9 0.42 0.093
7.9 0.42 0.093
7.9 0.42 0.092
7.9 0.42 0.093
8.0 0.42 0.094
8.0 0.43 0.094
2.6 OJ 0.030
3.4 0.4 0.042
4.0 0.4 0.047
4.2 0.4 0.050
4.7 0.4 0.055
5.1 OJ 0.061
7.3 0.40 0.085
Emission
Toluene Unc Ibs/hr
1.45
1.47
1.48
1.50
1.49
1.49
1.47
1.49
1.51
1.55
1.56
1.57
1.60
1.58
1.63
1.61
1.61
1.58
1.60
1.59
1.57
1.60
158
1.57
1.54
1.57
1.57
1.59
54.7 1.0 0.603
573 l-« 0.632
57.4 1.1 0433
1J
IJ
1.2
0.2 1.34 0.002
1-Pentene Unc
1.5 0.8
1.5 0.8
1.5 0.8
1.5 0.9
1.6 0.9
1.7 0.9
1.8 0.8
1.8 0.9
2.0 0.9
2.2 0.9
2.3 0.9
2.4 0.9
2.4 0.9
2.6 0.9
2.8 0.9
2.8 0.9
2.7 0.9
2.6 0.9
2.8 0.9
2.8 0.9
2.6 0.9
2.6 0.9
2.6 0.9
2.6 0.9
2.6 0.9
2.7 0.9
2.8 0.9
2.8 0.9
3J 0.7
3.0 0*
3.2 tA
2.1 0.7
14 0.7
1.7 0.6
2.0 0.8
2-Meihyl-
2-Buiene Unc
1.3 0.7
1.3 0.7
1.4 0.7
1.3 0.7
' 1.4 0.7
1.4 0.7
1.5 0.7
1.5 0.7
1.5 0.7
1.5 0.7
1.5 0.7
1.6 0.7
1.6 0.7
1.6 0.7
1.6 0.8
1.6 0.7
1.6 0.7 1
1.6 0.7 I
1.5 0.7
1.5 0.7
1.5 0.7
1.5 0.7
1.6 0.7
1.5 0.7
1.6 0.7
1.6 0.7
1.6 0.7
1.6 0.7
1.2 0.6
1J 0.7
1_» 0.7
1.1 0.4
0.6
0.6
1.5 06
* Blank spaces indicate the compound was no) delected in that sample. These are included in the averages as zero concentrations.
" File Names are in the data records in Appendix B. Bold face type indicates a sample (hat was spiked with SF, or toluene. Spiked samples are not included in ihe run averages.
-------
TABLE B-2. FTIR RESULTS (ppm) AND EMISSION RATES AT THE LTV SCRUBBER OUTLET'
Date
6/25/97
Time
«:41
S-.46
8:52
9:02
9:0*
9:13
10:15
10:22
10:26
10:31
10:54
11:00
11:04
11:08
11:34
11:39
11:43
11:47
12:39
12:43
12:47
12:50
13:11
13:15
13:18
13:22
14:01
14:04
14:08
14:12
14:37
14:42
14:46
14:51
15:15
15:19
15:24
File
Nameb
OUTS2M1
OUTS2002
OUTS2003
OUTS20M
OUTS2005
OUTS200*
OITT2U007
OUTV2008
OUTV2009
OUTV20IO
OVJTV2011
OUTV2012
OUTV20I3
OUTV2014
OUTV2015
OUTV2016
OUTV2017
OUTV2018
OUTV2019
OUTV2020
OUTV2021
OUTV2022
OUTV2023
OUTV2024
OUTV2025
OUTV2026
OUTV2027
OUTV2028
OUTV2029
OUTV2030
OUTV2031
OUTV2032
OUTV2033
OUTV2034
OUTV2035
OUTV2036
OUTV2037
Emissions
CO Unc Ibs/hr
791.4 10J 17.41
113.2 11J 17.73
>11J 124 17.70
7*54 13.9 17.13
747.2 144 14.73
749.0 14 A 14.77
827.9 19.3 18.05
846.8 24.8 18.46
861.8 26.6 18.79
871.5 23.8 19.00
831.2 17.1 18.12
858.8 20.S 18.72
841.1 20.1 18.34
845.6 21.5 18.43
794.3 17.9 17.32
779.7 16.5 17.00
787.8 18.6 17.17
793.4 20.3 17.30
853.1 17.8 18.60
842.0 19.3 18.35
814.3 24.1 17.75
815.1 19.4 17.77
823.7 21.6 17.%
828.9 16.0 18.07
826.2 15.8 18.01
763.2 72.8 16.64
759.5 22.3 16.56
788.9 48.7 17.20
791.9 15.3 17.26
799.9 14.4 17.44
826.8 19.1 18.02
797.0 18.4 17.38
791.6 17.3 17.26
780.5 19.4 17.02
779.2 l«3 16.99
768.7 21.1 16.76
780.4 17.7 I7.Q1
Emissions
SO2 Unc Ibs/hr
32.0 23 Ij40
33J 2.4 lj*
39.4 2.5 1.9*
27.4 2.9 1.34
19.1 3.0 0.95
19.7 3.0 0.91
35.9 3.5 1.79
37.9 3.5 1.89
22.8 3.6 1.14
20.0 3.6 1.00
26.5 3.2 1.32
31.4 3.5 1.56
28.0 3.5 1.39
34.8 3.5 1.74
20.5 3.5 1.02
22.0 3.4 1.09
21.1 3.5 1.05
13.3 3.6 0.66
22.9 3.4 1.14
21.1 3.6 1.05
29.9 3.7 1.49
43.4 3.6 2.16
30.7 3.6 1.53
32.7 3.3 1.63
30.7 3.2 1.53
24.3 4.1 1.21
14.6 3.8 0.73
12.7 3.8 0.63
13.2 3.2 0.66
14.2 3.1 0.71
54.1 3.6 2.70
44.7 3.6 2.23
35.4 3.5 1.77
35.1 3.6 1.75
17.1 3.6 0.85
13.9 3.9 0.69
6.8 3.6 0.34
Formal- Emission
dehyde Unc Ibs/hr
9.2 0.4 0.215
(.0 0.7 0.141
4.1 0.7 0.142
(.4 OJ 0.150
13 0.9 0.193
IS 0.9 0.175
9.0 1.0 0.210
9.4 1.0 0.219
5.8 1.0 0.135
6.0 1.0 0.139
12.3 0.9 0.288
5.5 1.0 0.128
5.5 1.0 0.129
6.2 1.0 0.144
5.3 1.0 0.124
5.7 1.0 0.134
3.6 1.1 0.084
3.4 I.I 0.079
8.4 1.0 0.196
8.2 I.I 0.192
5.4 1.1 0.127
5.4 1.1 0.126
4.5 1.1 0.105
6.6 1.0 0.154
5.0 1.0 0.118
6.6 1.2 0.153
7.4 1.2 0.174
9.2 1.2 0.215
10.6 1.0 0.247
8.3 1.0 0.194
7.7 1.1 0.181
8.2 1.1 0.192
8.7 I.I 0.204
8.0 I.I 0.188
7.5 1.1 0.174
7.3 1.2 0.171
»7 ll n?"*
Emission
Methane Unc Ibs/hr
14J 0.4 0.1S4
15.0 0.5 O.U7
14J 0.5 0.114
14.5 0.6 0.181
14.1 0.4 10.174
14.1 0.4 0.175
14.9 0.7 0.186
15.5 0.7 0.194
15.4 0.7 0.192
16.2 0.7 0.201
15.5 0.7 0.193
15.9 0.7 0.198
15.8 0.7 0.197
15.3 0.7 0.190
14.8 0.7 0.185
15.0 0.7 0.186
16.1 0.7 0.201
15.8 0.7 0.197
21.5 0.7 0.268
20.3 0.8 0.253
18.7 0.8 0.233
17.9 0.8 0.223
18.0 0.8 0.225
18.2 0.7 0.227
18.4 0.7 0.229
16.5 0.9 0.206
14.5 0.8 0.181
15.6 0.8 0.195
15.7 0.7 0.195
15.7 0.7 0.196
15.5 0.8 0.192
14.6 0.8 0.182
14.3 0.8 0.179
13.7 0.8 0.171
15.1 0.8 0.188
14.6 0.8 0.182
ld.8 ^ fUf5
i-Heptane Unc
3.0
1.9 OJ
1.9 OJ
4.1
4J
4.4
5.1
5.1
2.0 0.5
5.2
2.8 0.4
2.3 0.5
2.3 0.5
2.3 ' 0.5
5.2
5.2
5.3
5.4
5.1
5.5
5.6
5.6
5.6
5.1
1.4 0.5
6.3
5.9
1.4 0.5
1.9 0.5
2.1 0.4
5.5
5.6
5.6
5.7
5.8
6.1
•Ml
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/25/97
Time
15:28
15:52
15:57
16:03
16:08
16:33
16:39
16:43
16:48
17:34
17:41
17:4*
17:5*
U:M
18:04
File
Name"
OUTV2038
OUTV2039
OUTV2040
OUTV2041
OUTV2042
OUTV2043
INLV2044
INLV2045
INLV2046
OUTS2047
OUTS2048
OUTS2049
OLTS2050
OUTS2051
OUTS2052
Avenge — >
Emissions
CO Unc Ibs/hr
791.7 20.0 17.26
776.4 21.5 16.92
779.9 27.7 17.00
781.9 20.1 17.05
772.7 17.4 16.85
812.1 17.2 17.70
808.6 23.2 17.63
796.7 20.3 17.37
801.1 24.7 17.46
7473 13.9 16.29
76*3 14.0 U.71
782.5 15.1 17.0*
744.2 13.7 16J7
728.4 14.7 1548
727.7 14.2 15J6
807.3 21.9 17.60
Emissions
SO2 Unc Ibs/hr
6.7 3.7 0.34
14.6 3.8 0.73
10.7 3.8 0.53
19.0 3.7 0.95
16.0 3.6 0.80
24.8 3.6 1.23
31.8 3.8 1.58
27.9 3.7 1.39
27.9 3.7 1.39
US 3.2 9J2
14.0 3.2 0.70
253 33 1.24
30.4 3.1 1.52
23.0 3.4 1.15
18.8 33 0.94
24.8 3.6 1.23
Formal- Emissions
dehyde Unc Ibs/hr
7.7 1.2 0.180
7.0 1.2 0.164
8.1 1.2 0.189
8.4 1.2 0.197
8.5 1.1 0.199
8.1 I.I 0.190
7.6 1.2 0.177
7.9 1.2 0.184
7.9 1.2 0.184
74 1.1 0.177
8.0 1.1 O.U4
8.7 1.1 0.202
8.2 1.1 0.1*2
7.7 1.1 0.180
7.5 1.1 0.174
7.3 1.1 0.170
Emissions
Methane Unc Ibs/hr
15.0 0.8 0.187
14.0 0.8 0.174
14.0 0.8 0.175
13.9 0.8 0.173
14.1 0.8 6.175
16.4 0.8 0.204
16.0 0.9 0.199
15.5 0.8 0.193
15.0 0.8 0.187
15.7 OJ 0.196
15.9 OJ 0.198
144 OJ 0.207
15.5 0.7 0.193
143 OJ 0.178
14.0 OJ 0.175
15.8 0.8 0.197
i-Heptane Unc
5.9
6.0
6.0
5.9
5.7
5.8
6.1
6.0
6.1
5.4
5.5
5.7
5.4
5.8
5.7
0.5 4.5
Date
6/26/97
Time
9:53
9:59
10:04
10:21
10:24
10:37
10:43
10:49
11:28
11:29
11:30
11:31
11:32
11:33
11:33
11.34
File
Name
OUTS3001
OUTS3002
OUTS3003
OUTS3004
OUTS3005
OUTS3006
OUTS3007
OUTS3008
16260038
16260039
16260040
16260041
16260042
16260043
16260044
16260045
Emissions
CO Unc Ibs/hr
785J 114 17.11
•48.5 13J 18.50
851.4 14.5 183*
780 J 11.2 17.02
777.7 113 U.95
7824 11.1 17.06
7853 113 17.12
7715 11.7 16.98
841.2 14.4 18.34
841.4 14.8 18.34
844.4 15.1 18.41
837.9 15.0 18.27
837.7 15.4 18.26
836.2 15.5 18.23
824.5 14.8 17.97
824.3 15.0 17.97
Emissions
SO2 Unc Ibs/hr
51.5 2.4 237
55.0 2.7 2.74
503 2J 2.51
48.1 23 2.40
38J 2.4 1.93
50.4 23 2.51
51J 2.4 2.58
57.0 2.4 2J4
46.2 2.9 2.30
44.7 3.0 2.23
42.8 3.0 2.13
41.2 3.0 2.05
40.6 3.1 2.02
38.9 3.1 1.94
37.1 3.0 |.85
35.6 3.1 1.77
Formalde Emissions
hyde Unc Ibs/hr
73 04 0.172
4.9 0.7 0.160
«.«• 0.7 0.141
*J 04 0.145
63 04 0.147
5.9 04 0.139
54 04 0.136
5.9 04 0.138
2.8 0.8 0.065
3.2 0.8 0.075
2.6 0.9 0.062
2.4 0.9 0.055
2.3 0.9 0.053
2.2 0.9 0.052
2.2 0.9 0:052
2.2 0.9 0.052
Emission
Methane Unc Ibs/hr
144 0.4 0.182
16.6 OS 0.200
16.0 0.5 0.199
14.5 0.4 0.181
14.4 OS 0.180
14.1 0.4 0.176
14.1 0.4 0.176
13.9 0.5 0.173
17.1 0.6 0.212
17.1 0.6 0.213
17.1 0.6 0.213
17.2 0.6 0.214
17.3 0.6 0.215
17.4 0.6 0.216
17.2 0.6 0.214
17.2 0.6 0,214
i-Heptane Unc
1.6 03
1.9 OJ
2.0 03
1.4 03
1.5 03
1.9 03
1.9 03
1.0 03
3.3 0.4
3.2 0.4
3.1 0.4
3.1 0.4
3.0 0.4
3.0 0.4
3.0 04
2.9 0.4
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date Time
6/26/97
6/26/97
11:35
11:36
11:37
11:38
11:39
11:40
11:41
11.42
11:42
11:43
11:44
11:45
11:46
11:47
11:48
11:49
11:50
11:51
11:52
11:53
12:23
12:24
12:25
12:25
12:26
12:27
12:28
12:29
12:30
13:07
13:08
13:09
13:10
13:11
13:12
13:13
File
Name
16260046
16260047
16260048
16260049
16260050
16260051
16260052
16260053
16260054
16260055
16260056
16260057
16260058
16260059
16260060
16260061
16260062
16260063
16260064
16260065
16260093
16260094
16260095
16260096
16260097
16260098
16260099
16260100
16260101
16260138
16260139
16260140
16260141
16260142
16260143
16260144
Emissions
CO Unc Ibs/hr
818.9 15.0 17.85
822.0 15.3 17.92
818.3 14.8 17.84
818.5 15.0 17.84
817.0 14.8 17.81
823.5 15.1 17.95
821.3 14.8 17.90
824.5 15.1 17.97
824.9 14.7 17.98
832.7 15.4 18.15
842.3 16.1 18.36
836.7 15.5 18.24
845.8 15.8 18.44
842.2 15.3 18.36
847.4 16.1 18.47
849.4 15.9 18.52
846.6 15.9 18.46
844.1 16.0 18.40
840.3 15.5 18.32
841.3 16.0 18.34
868.4 16.0 18.93
859.5 15.9 18.74
850.2 15.1 18.53
854.4 16.1 18.63
850.2 15.9 18.53
851.9 16.2 18.57
847.6 16.1 18.48
856.4 16.5 18.67
858.1 16.5 18.71
878.6 17.0 19.15
877.6 17.3 19.13
875.2 18.2 19.08
866.0 19.0 18.88
867.4 22.4 18.91
858.6 40.8 18.72
864.3 41.2 18.84
Emissions
SO2 Unc Ibs/hr
34.0 3.0 1.70
32.9 3.1 1.64
30.7 3.1 1.53
28.5 3.1 1.42
26.5 3.1 1.32
26.1 3.1 1.30
25.2 3.1 1.26
24.8 3.2 1.23
24.3 3.1 1.21
25.2 3.1 1.25
26.4 3.1 1.31
27.8 3.1 1.38
28.9 3.2 1.44
29.9 3.2 1.49
30.3 3.2 1.51
31.1 3.2 1.55
31.7 3.2 1.58
32.2 3.2 1.61
31.6 3.2 1.58
31.0 3.2 1.55
18.4 3.1 0.92
18.1 3.1 0.90
18.3 3.2 0.91
18.8 3.3 0.93
18.2 3.3 0.91
19.2 3.2 0.96
19.0 3.3 0.95
18.2 3.3 0.91
17.6 3.3 0.88
5.4 3.2 0.27
4.7 3.3 0.23
3.5
3.7
3.9
4.0
4.1
Formalde Emission
hyde Unc Ibs/hr
2.2 0.9 0.051
2.3 0.9 0.053
2.2 0.9 0.051
2.3 0.9 0.053
2.2 0.9 0.052
2.2 0.9 0.052
2.2 0.9 0.053
2.3 0.9 0.054
2.3 0.9 0.053
2.3 0.9 0.053
2.3 0.9 0.054
2.3 0.9 0.054
2.3 0.9 0.055
2.4 0.9 0.055
2.4 0.9 0.056
2.4 0.9 0.056
2.4 0.9 0.057
2.5 0.9 0.058
2.5 0.9- 0.058
2.6 0.9 0.061
3.5 0.9 0..083
3.7 0.9 0.087
3.5 0.9 0.082
3.5 1.0 0.082
3.5 1.0 0.081
3.4 1.0 0.079
3.4 1.0 0.080
3.5 1.0 0.081
3.5 1.0 0.082
1.8 0.9 0.041
2.2 1.0, 0.051
2.3 1.0 0.055
2.4 1.1 0.056
2.5 1.1 0.057
2.5 1.2 0.060
2.6 1.2 0.061
Emission
Methane Unc Ibs/hr
17.1 0.6 0.213
17.1 0.6 0.212
16.9 0.6 0.211
17.1 0.6 0.213
17.2 0.6 0.214
17.3 0.6 0.215
17.4 0.6 0.217
18.0 0.6 0.225
18.2 0.6 0.226
18.0 0.6 0.224
18.1 0.6 0.225
17.9 0.6 0.223
18.0 0.6 0.225
18.2 0.6 0.227
18.3 0.6 0.229
18.4 0.7 0.229
18.4 0.6 0.230
18.5 0.6 0.230
18.5 0.6 0.230
18.5 0.7 0.230
22.3 0.6 0.278
22.5 0.6 0.280
22.4 0.7 0.279
22.3 0.7 0.278
22.6 0.7 . 0.281
22.4 0.7 0.279
22.2 0.7 0.277
22.4 0.7 0.279
22.6 0.7 0.282
22.4 0.7 0.278
22.2 0.7 0.276
22.3 0.7 0.277
22.1 0.8 0.275
21.5 0.8 0.268
21.3 0.8 0.265
21.2 0.8 0.264
i-Heptane Unc
2.9 0.4
2.9 0.4
2.9 0.4
2.9 0.4
2.8 0.4
2.9 0.4
2.8 0.4
2.9 0.4
2.9 0.4
2.9 0.4
2.9 0.4
2.8 0.4
2.9 0.4
2.9 0.4
2.8 0.4
2.8 0.4
2.8 0.4
2.8 0.4
2.8 0.4
2.7 0.4
3.4 0.4
3.2 0.4 I
3.0 0.4 1
3.0 0.4
2.9 0.4
3.0 0.4
2.9 0.4
2.9 0.4
2.9 0.4
3.7 0.4
3.6 0.5
3.4 0.5
3.2 0.5
3.1 0.5
3.0 0.5
2.9 0.6
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date Time
6/26/97
13:14
13:15
13:16
13:16
13:17
13.18
13:19
13:20
13:21
13:22
13:23
13:24
13^25
13:26
13:27
13:27
13:28
13:29
13:30
13:31
14:32
14:33
14:34
14:35
14:36
14:37
14:38
14:39
14:40
14:40
14:41
14:42
14:43
14:44
14:45
14:46
File
Name
16260145
16260146
16260147
16260148
16260149
16260150
16260151
16260152
16260153
16260154
16260155
16260156
16260157
16260158
16260159
16260160
16260161
16260162
16260163
16260164
16260199
16260200
16260201
16260202
16260203
16260204
16260205
16260206
16260207
16260208
16260209
16260210
16260211
16260212
16260213
16260214
Emissions
CO Unc Ibs/hr
847.4 50.5 18.47
860.2 49.2 18.75
846.8 40.7 18.46
863.6 49.4 18.83
856.6 42.7 18.67
849.5 39.1 18.52
869.3 40.9 18.95
848.5 40.0 18.50
841.0 39.4 18.33
847.7 49.7 18.48
835.9 50.4 18.22
833.7 55.9 18.18
855.6 49.1 18.65
829.9 39.2 18.09
839.9 45.9 18.31
846.8 49.2 . 18.46
829.2 55.5 18.08
837.3 55.9 18.25
817.2 60.0 17.82
833.7 60.5 18.17
779.9 55.6 17.00
780.9 49.2 17.02
776.0 59.9 16.92
785.5 59.6 17.12
778.7 59.8 16.98
780.2 59.9 17.01
790.3 59.7 17.23
782.5 59.8 17.06
785.1 59.6 17.12
787.8 59.9 17.17
772.5 59.8 16.84
772.7 60.1 16.84
766.0 60.2 16.70
770.8 59.9 16.80
769.3 60.3 16.77
779.5 60.4 16.99
Emissions
SO2 Unc Ibs/hr
4.2
4.2
4.2
4.2
4.2
4.1
4.1
4.2
5.1 4.2 0.25
6.0 4.2 0.30
6.1 4.2 0.30
6.5 4.3 0.32
7.2 4.3 0.36
8.3 4.2 0.41
8.2 4.3 0.41
7.2 4.4 0.36
6.4 4.4 0.32
7.0 4.4 0.35
7.5 4.5 0.37
9.1 4.4 0.45
4.5
4.5
4.7
4.7
4.6
4.8
4.7
4.7
4.8
4.8
4.8
4.7
4.7
4.7
4.6
4.7
Formalde Emission
hyde Unc Ibs/hr
2.8 1.2 0.066
2.8 1.2 0.066
3.0 1.2 0.070
2.9 1.2 0.069
3.1 1.2 0.071
3.0 1.2 0.071
3.1 1.2 0.073
3.0 1.2 0.071
3.1 1.2 0.072
3.1 1.2 0.074
3.1 1.2 0.073
3.2 1.2 0.074
3.3 1.2 0.076
3.1 1.2 0.073
3.1 1.3 0.072
3.1 1.3 0.073
3.1 1.3 0.072
3.0 1.3 0.070
3.1 1.3 0.073
3.1 1.3 0.073
1.4 1.3 0.032
2.0 1.3 0.047
2.5 1.4 0.059
2.8 1.4 0.067
3.0 1.3 0.069
3.0 1.4 0.070
2.7 1.4 0.063
3.3 1.4 0.078
3.3 1.4 0.078
3.3 1.4 0.078
3.5 1.4 0.082
3.7 1.4 0.086
3.3 1.4 0.076
2.7 1.4 0.063
3.1 1.4 0.072
3.4 1.4 0.080
Emission
Methane Unc Ibs/hr
21.0 0.9 0.261
20.7 0.9 0.257
20.5 0.9 0.255
20.3 0.9 0.253
20.1 0.9 b,250
19.9 0.8 0.248
19.8 0.8 0.247
19.5 0.9 0.243
19.3 0.9 0.240
18.9 0.9 0.236
18.8 0.9 0.234
18.5 0.9 0.230
18.2 0.9 0.227
18.1 0.9 0.225
17.8 0.9 0.221
17.8 0.9 0.222
17.6 0.9 0.220
17.6 0.9 0.220
17.5 0.9 0.218
17.3 0.9 0.216
15.5 0.9 0.193
15.4 0.9 0.192
15.5 1.0 0.193
15.6 1.0 0.195
15.8 0.9 0.196
15.7 1.0 0.195
15.8 1.0 0.196
15.7 1.0 0.195
15.7 1.0 0.195
15.6 1.0 0.194
15.6 1.0 0.194
15.5 1.0 0.194
15.6 1.0 0.194
15.7 1.0 0.196
15.7 1.0 0.196
15.5 1.0 0.193
i-Heptane Unc
2.9 0.6
2.8 0.6
2.9 0.6
2.8 0.6
2.8 0.6
2.9 0.5
2.9 0.5
2.8 0.6
2.8 0.6
2.8 0.6 1
2.8 0.6 1
2.8 0.6
2.8 . 0.6
2.8 0.6
2.7 0.6
2.7 0.6
2.7 0.6
2.7 0.6
2.6 0.6
2.6 0.6
1.1 0.6
1.0 0.6
1.1 0.6
1.1 0.6
1.3 0.6 1
1.1 06 1
1.4 0.6
1.2 0.6
1.2 0.6
1.2 0.6
I.I 06
6.9
1.1 0.6 1
1.3 0.6 I
1.0 0-6 1
6.9 1
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/26/97
*#6/97
me
<*l
fu
0.097
34 ft* OX»S>
3.4 04 OX*i
>4
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
CO
Unc
Emissions
Ibs/hr
SO2
Unc
Emissions
Ibs/hr
Pormalde
hyde
Emissions
Unc Ibs/hr
Methane Unc
Emissions
Ibs/hr
i-Heptane Unc
TMJt
814.8
lt.1
U.ie
3.5
5.9
1.1
0.13S
16.2
04
OJ02
U.8
3.9
0.59
2.9
l.l
0.067
17.7
0.8
0.221
2.2
S.6
11
Date
6/27/97
6/27/97
Time
S:4*
»:51
«:55
9:03
9:01
9:13
9:48
9:49
9:50
9:51
9:52
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10.02
10:03
10.O4
10:05
10:06
10:07
10:08
10:09
10:10
File
Name
OUTS4M1
OUTS4901
OUTS4903
OUTS4M4
OUTS4905
OUTS490*
16270001
16270002
16270003
16270004
16270005
16270006
16270007
16270008
16270009
16270010
16270011
16270012
16270013
16270014
16270015
16270016 •
16270017
16270018
16270019
16270020
16270021
16270022
16270023
16270024
16270025
Emissions
CO Unc Ibs/hr
77«4 1*4 M.79
7*4.4 SO.* HM
7M.1 49.4 174*
713.7 494 174»
7*1.1 62.1 1*J9
740.4 47.* 1«.14
902.9 65.0 19.68
909.2 64.5 19.82
909.1 64.1 19.82
909.5 64.3 19.83
900.2 66.0 19.63
904.7 64.6 19.72
911.0 64.3 19.86
901.4 63.8 19.65
901.5 64.5 19.65
901.5 64.3 19.65
898.1 64.4 19.58
894.4 64.3 19.50
892.9 64.1 19.47
828.0 57.1 18.05
845.8 58.7 18.44
817.9 56.4 17.83
887.7 64.5 19.35
900.3 64.1 19.63
900.5 63.9 19.63
899.2 64.4 19.60
906.3 63.8 19.76
909.8 63.7 19.83
913.4 63.7 19.91
873.1 58.6 19.03
916.9 64.1 19.99
Emissions
SO2 Unc Ibs/hr
21J 3.1 1.0*
25.9 34 1.29
28.* 3.* 1.42
294 3.* 1.45
29.7 3.7 1.48
29J 3.7 1.4*
31.6 4.7 1.57
30.8 4.8 1.54
30.2 4.8 1.50
29.3 4.9 1.46
28.4 4.9 1.41
28.3 5.0 1.41
30.0 5.0 1.49
31.7 5.0 1.58
33.2 5.1 1.65
34.3 5.1 1.71
34.4 5.0 1.71
34.2 5.0 1.70
33.2 5.0 1.65
30.7 5.0 1.53
28.0 5.0 1.40
25.4 5.0 1.26
21.9 5.0 1.09
19.2 5.1 0.95
18.1 5.0 0.90
17.0 5.0 0.85
16.5 4.9 0.82
16.5 5.0 0.82
16.2 5.0 0.81
15.4 5.0 0.77
14.5 S.I 0.72
Formalde Emission
hyde Unc Ibs/hr
114 94 0.257
5* 14 9.131
5J 0.9 9.135
5.* 1.0 9.131
54 1.0 0.135
5J 14 0.122
1.2 1.2 0.029
1.7 1.2 0.040
1.8 1.2 0.043
1.9 1.3 0.045
2.0 1.3 0.047
2.1 1.3 0.050
2.1 1.3 ' 0.049
2.2 1.3 0.051
2.2 1.3 0.051
2.2 1.3 0.052
2.3 1.3 0.053
2.3 1.3 0.053
2.3 1.3 0.055
2.4 1.3 0.057
2.4 1.3 0.055
2.5 1.3 0.058
2.5 1.3 0.058
2.5 1.3 0.058
2.5 1.3 0.058
2.5 1.3 0.058
2.5 1.3 0.058
2.4 1.3 0.057
2.5 1.3 0.059
2.6 1.3 0.060
2.6 1.3 0.061
Emission
Methane Unc Ibs/hr
11.7 0.* 0.145
114 0.7 0.147
12.2 0.7 0.151
124 0.7 0.159
124 0.7 0.157
12.2 0.7 0.152
14.5 0.9 0.181
14.5 0.9 0.180
14.5 0.9 0.181
14.3 0.9 0.178
14.2 0.9 0.176
14.4 0.9 0.180
14.1 0.9 0.175
14.2 0.9 0.176
14.0 0.9 0.174
13.8 0.9 0.172
14.2 0.9 0.176
14.1 0.9 0.176
13.9 0.9 0.173
13.8 0.9 0.172
13.6 0.9 0.169
13.6 0.9 0.170
13.5 0.9 0.168
13.7 0.9 0.171
13.7 0.9 0.171
14.0 0.9 0.174
14.1 0.9 0.176
14.3 0.9 0.178
14.5 0.9 0.181
14.6 0.9 0.182
14.6 0.9 0.182
1
i-Heptane Unc
4.0
4.9
44
4.9
5.1
5.0
0.8 0.6
0.9 0.6
1.0 0.6
0.9 0.6
1.0 0.6
1.0 0.6
1.0 0.6
1.0 0.6
1.0 0.6
1.0 0.6
1.1 0.6
1.1 0.6
I.I 0.6
1.2 0.6
I.I 0.6
1.2 0.6
1.2 0.6
1.2 0.6
1.2 0.6
1.3 0.6
1.4 0.6
1.3 0.6
1.4 0.6
1.4 0.6
1.5 0.6
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date Time
6/27/97
10:11
10:12
10:12
10:13
10:14
10:15
10:16
10:53
10:54
10:55
10:56
10:57
10:58
10:59
11:00
11:01
11:01
11:02
11:03
11:47
11.48
11:48
11:49
11:50
11:51
11:52
11:53
11:54
11:55
11:56
11:56
11:57
11:58
11:59
12:00
12:01
File
Name
16270026
16270027
16270028
16270029
16270030
16270031
16270032
16270068
16270069
16270070
16270071
16270072
16270073
16270074
16270075
16270076
16270077
16270078
16270079
16270122
16270123
16270124
16270125
16270126
16270127
16270128
16270129
16270130
16270131
16270132
16270133
16270134
16270135
16270136
16270137
16270138
Emissions
CO Unc Ibs/hr
911.4 64.2 19.87
910.S 64.1 19.85
913.3 63.8 19.91
913.3 63.5 19.91
907.2 63.7 19.78
914.6 635 19.94
906.6 63.2 19.76
885.4 64.9 19.30
886.7 64.4 19.33
891.2 64.4 19.43
899.1 64.0 19.60
900.1 63.6 19.62
898.6 62.9 19.59
903.2 62.9 19.69
911.1 62.8 19.86
916.8 62.6 19.99
915.2 63.2 19.95
921.1 63.0 20.08
924.8 62.3 20.16
796.6 18.2 17.37
796.1 17.4 17.36
795.5 17.1 17.34
797.7 17.4 17.39
791.5 39.7 17.25
796.9 58.8 17.37
787.8 58.5 17.17
790.4 59.3 17.23
807.0 48.4 17.59
802.3 59.7 17.49
831.4 60.3 18.12
814.0 58.2 17.74
802.5 57.5 17.49
815.6 57.6 17.78
819.2 58.6 17.86
814.3 59.4 17.75
785.9 57.9 17.13
Emissions
SO2 Unc Ibs/hr
13.6 5.2 0.68
13.5 5.2 0.67
14.3 5.1 0.71
15.3 5.3 0.76
16.6 5.2 0.83
17.8 5.3 0.89
18.9 5.4 0.94
4.7
4.8
5.0
5.1
5.2
5.3
5.3
5.5
5.6
5.4
5.6
5.6
3.7
3.7
3.8
3.8
4.1
5.2
5.1
4.8
4.5
4.7
5.0
5.3
5.2
5.1
5.0
4.9
4.8
Formalde Emission
hyde Unc Ibs/hr
2.6 1.4 0.060
2.6 1.4 0.060
2.6 1.3 0.060
2.7 1.3 0.062
2.6 1.4 0.061
2.6 1.4 0.062
2.6 1.4 0.060
1.3
1.3
1.4
1.5 1.4 0.035
1.7 1.4 0.039
1.7 1.4 0.040
1.7 1.4 0.039
1.8 1.4 0.042
1.8 1.4 0.043
1.8 1.4 0.041
1.7 1.5 0.039
1.8 1.5 0.043
2.7 1.0 0.062
2.7 1.0 0.064
2.8 1.0 0.065
2.8 1.0 0.065
2.5 1.1 0.058
1.3
1.5 1.3 0.034
2.2 1.3 0.051
2.5 1.2 0.059
2.4 1.3 0.055
2.1 1.3 0.049
2.0 1.4 0.046
2.2 1.4 0.052
2.4 1.4 0.055
2.5 1.4 0.059
2.7 1.4 0.063
2.7 1.4 0.063
Emission
Methane Unc Ibs/hr
14.4 1.0 0.180
14.5 1.0 0.181
14.5 0.9 0.181
14.9 0.9 0.185
14.7 1.0 0.183
14.6 1.0 0.182
14.7 1.0 0.183
14.1 0.9 0.176
14.1 0.9 0.176
14.1 1.0 0.176
14.2 1.0 0.177
14.2 1.0 0.177
14.4 1.0 0.179
14.5 1.0 0.180
14.6 1.0 0.182
14.9 1.0 0.185
14.9 1.0 0.185
14.9 1.0 0.185
15.1 1.0 0.188
13.9 0.7 0.173
13.8 0.7 0.172
13.9 0.7 0.173
13.9 0.7 0.173
13.6 0.8 0.170
13.4 0.9 0.166
13.5 0.9 0.169
13.5 0.9 0.169
13.8 0.9 0.172
13.9 0.9 0.173
13.8 0.9 0.172
13.7 1.0 0.171
13.5 1.0 0.168
13.7 1.0 0.171
13.4 1.0 0.168
13.5 1.0 0.168
13.4 1.0 0.167
i-Heptane Unc
1.4 0.6
1.3 0.6
1.4 0.6
1.4 0.6
1.3 0.6
1.3 0.6
1.3 0.6
1.9 0.6
1.9 0.6
1.7 0.6
1.8 0.6
1.7 0.6
1.7 0.6
1.6 0.6
1.6 0.7
1.7 0.7
1.6 0.7
1.5 0.7
1.5 0.7
3.6 0.5
3.6 0.5
3.5 0.5
3.5 0.5
3.2 0.5
2.6 0.6
2.6 0.6
2.8 0.6
2.9 0.6
2.9 0.6
2.6 0.6
2.4 0.6
2.4 0.6
2.5 0.6
2.4 0.6
2.5 0.6
2.5 0.6
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date Time
6/27/97
12.02
1203
1204
12:05
12O5
12O6
12.07
1208
12.09
12:10
12:11
12.12
12:49
12:50
12:51
12:55
12:59
13:02
13:09
13:12
13:1*
File
Name
16270139
16270140
16270141
16270142
16270143
16270144
16270145
16270146
16270147
16270148
16270149
16270150
16270186
16270187
16270188
OUT4S007
OUTS40M
OUTS4009
OUTS401*
OUTS4011
OUTS4012
Avenge — >
Emissions
CO Unc »bs/hr
796.1 58.3 17.35
791.1 58.5 17.25
788.5 58.6 17.19
784.0 58.5 17.09
777.8 54.1 16.96
782.2 58.4 17.05
811.3 60.4 17.69
780.9 59.2 17.02
767.0 58.6 16.72
764.9 58.8 16.67
765.5 58.8 16.69
752.4 58.0 16.40
785.8 57.1 17.13
769.8 58.0 16.78
742.5 56.8 16.19
478.7 754 14.80
484.2 49.6 14.»4
72C.O 24J 1547
763.1 43.1 14.43
771.0 42.7 14J1
752.3 48.4 14.40
853.6 58.7 18.61
Emissions
SO2 Unc Ibs/hr
4.8
4.7
4.6
4.6
4.7
4.7
4.6
4.6
4.5
4.5
4.7
4.7
5.3
5.2
5.0
4.7
4.2
3.»
34
3.9
3.9
10.0 4.92 0.50
Formalde Emissions
hyde Unc Ibs/hr
2.8 1.4 0.066
2.9 1.3 0.069
2.9 1.3 0.068
2.8 1.3 0.066
2.7 1.3 0.064
2.9 1.4 0.067
2.9 1.3 0.067
2.9 1.3 0.069
3.0 1.3 0.069
2.8 1.3 0.066
2.8 1.4 .0.066
2.8 1.4 0.065
2.3 1.5 0.053
4.1 1.5 0.097
3.1 1.5 0.072
5.7 1.4 0.133
3.9 13 0.091
2.0 1.2 «.*44
3.7 1.2 04(7
2.9 1.2 0.068
2.5 1.2 0.05*
2.3 1.3 0.053
Emission
Methane Unc Ibs/hr
13.4 1.0 0.167
13.6 0.9 0.169
13.6 0.9 0.170
13.5 0.9 0.168
13.4 0.9 0.167
13.4 1.0 0.167
13.4 0.9 0.166
13.2 0.9 0.165
13.1 0.9 0.163
13.0 0.9 0.162
12.9 1.0 0.161
13.0 1.0 0.162
13.6 1.1 0.169
13.2 1.1 0.164
12.3 1.0 0.153
11.2 1.0 0.139
11 J 0.9 0.139
12 J 0.9 0.153
14.5 04 O.UO
144 0.9 0.182
14.1 0.9 0.174
13.9 0.9 0.174
i-Heptane Unc
2.4 0.6
2.6 0.6
2.6 0.6
2.4 0.6
2.4 0.6
2.4 0.6
2.5 0.6
2.5 0.6
2.4 0.6
2.4 0.6
2.4 0.6
2.3 0.6
7.7
7.6
7.5
7.2
2.1 0.6
2.0 0.6
4.1
6.1
6J
1.8 0.9
Dale Time
6/25/97
1:41
«:44
8:52
9:02
9:08
9:13
10:15
10:22
10:26
10:31
Hie Name
OUTS2001
OUTS2002
OUTS2003
OUTS2004
OUTS2005
OUTS2006
OUT2U007
OUTV2008
OUTV2009
OUTV2010
Emissions
Elhylene Unc Ibi/hr
2J 04 0.049
3.1 04 0.048
33 0.4 0.071
3J 0.7 0.072
3.1 0.7 0.048
3.2 0.7 0.070
3.8 0.8 0.083
3.7 0.8 0.081
4.1 0.9 0.089
4.3 0.9 0.094
Emissions
Ammonia Unc Ita/hr
0.4
0.5
OS
OS
04
0.4
0.8 0.7 0.010
0.7
0.7
0.7
Emissions
Toluene Unc Ibs/hr
1.4
1.5
IS
23.4 IJ • 0.291
23.7 1.4 0.295
234 1.4 0.292
2.3
2.3
2.4
2.4
I'Pentene Unc
4.4 1.4
SS 04
5.2 04
9.1 0.4
9.7 0.4
9J 0.4
8.9 2.1
8.7 2.1
6.3 1.3
8.9 2.2
Penune Unc
24 04
1.0
1.4
I.I
1.2
1.2
1.4 1.0
2.0 I.I
2.2
1.4 I.I
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Due
6/25/97
Time
10:54
11:00
11:04
11:08
11.34
11:39
11:43
11:47
12:39
12:43
12:47
12:50
13:11
13:15
13:18
13:22
14:01
14:04
14:08
14:12
14:37
14:42
14:46
14:51
15:15
15:19
15:24
15:28
15:52
15:57
16:03
16:08
16:33
16:39
16:43
16:48
17:36
RleNime
OUTV201 1
OUTV20I2
OUTV2013
OUTV2014
OUTV2015
OUTV2016
OUTV2017
OUTV2018
OUTV2019
OUTV2020
OUTV2021
OUTV2022
OUTV2023
OUTV2024
OUTV2025
OUTV2026
OUTV2027
OUTV2028
OUTV2029
OUTV2030
OUTV2031
OUTV2032
OUTV2033
OUTV2034
OUTV2035
OUTV2036
OUTV2037
OUTV2038
OUTV2039
OUTV2040
OUTV2041
OUTV2042
OUTV2043
INLV2044
INLV2045
INLV2046
OUTS2047
Emiuiooi
Ethylene Unc Ibs/hr
3.2 0.8 0.070
4.1 OA 0.089
4.1 0.8 0.091
4.0 0.8 0.087
4.1 0.8 0.090
4.1 0.8 0.090
4.5 0.8 0.099
4.7 0.9 0.104
6.7 0.8 0.147
6.5 0.9 0.142
6.3 0.9 0.137
5.8 0.9 0.128
6.0 0.9 0.130
5.7 0.8 0.124
5.8 0.8 0.126
5.8 1.0 0.126
4.2 0.9 0.092
3.8 0.9 0.084
3.4 0.8 0.075
3.7 0.7 0.081
4.3 0.9 0.093
4.0 0.9 0.088
3.8 0.8 0.084
3.9 0.9 0.086
4.2 0.9 0.091
4.1 0.9 0.090
3.8 0.9 0.084
4.0 0.9 0.088
3.8 0.9 0.084
3.8 0.9 0.082
3.6 0.9 0.078
3.7 0.9 0.081
4.3 0.9 0.094
4.6 0.9 0.100
4.3 0.9 0.094
4.2 0.9 0.091
3.7 0.8 0.080
Emiuiom
Ammonia Unc Ibs/hr
1.3 0.6 0.018
0.7
0.7
0.7
1.7 0.7 0.022
0.8 0.7 0.011
0.7
0.7
1.3 0.6 0.017
0.7
0.7
0.7
1.4 0.7 0.019
0.6
0.6
0.8
0.8 0.7 0.0 II
0.7
0.6
0.6
1.4 0.7 0.018
0.7 0.7 0.010
0.7
0.7
1.7 0.7 0.022
0.9 0.7 0.012
0.7
0.7
1.5 0.7 0.020
0.9 0.7 0.012
0.7
0.7
1.5 0.7 0.019
0.8 0.7 0.011
0.7
0.7
1.5 0.6 0.019
Emisnoiu
Toluene Unc Itn/ki
2.2
2.3
2.3
2.3
2.4
2.3
2.4
2.4
7.3 1.7 0.091
6.7 1.8 0.084
6.4 1.8 0.080
6.0 1.8 0.075
6.3 1.8 0.078
6.2 1.7 0.077
5.8 1.6 0.072
5.7 2.0 0.070
2.7
7.0 2.0 0.087
6.7 1.7 0.083
4.9 1.6 0.061
2.5
2.6
2.5
2.6
2.6
2.8
2.6
2.7
2.7
2.7
2.7
2.6
2.6
2.8
2.7
2.8
M.9 1J 0.335
1 -Penlene Unc
7.2 1.1
5.8 1.2
5.9 1.2
5.8 1.2
7.0 2.2
7.0 2.2
7.2 2.2
9.4 0.5
14.8 0.5
13.7 0.5
11.5 0.5
11.1 0.5
11.6 0.5
12.4 0.5
8.4 1.2
11.5 0.6
13.0 0.5
12.1 1.5
11.6 1.3
9.2 1.2
12.2 2.3
14.2 0.5
13.8 0.5
13.2 0.5
13.8 0.5
13.3 0.6
14.1 0.5
13.6 0.5
13.1 0.5
13.6 0.5
13.6 0.5
13.6 0.5
1 5.1 0.5
14.4 0.6
14.0 0.6
13.9 0.6
11.0 23
PentAAG Unc
2.0
2.1
2.2
2.2
1 1.9 I.I
1.7 I.I
1.1 I.I
1.1
1.1
1.1
1.2
1.2
1.2
I.I
1.6
1.3
1.2
3.3
2.8
1.5
1.3 1.1
1.2
1.2
1.2
1.2
1.3
1.2
1.2
1.2
1.2
1.2
1.2
1.2
1.3
1.2
1.3
1.4 1.1
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/25/97
Time
17:41
17:44
17-.S4
1I:M
18:04
File Name
OUTS2048
OUTS2049
OUTS2050
OUTS2051
OUTS2052
Average — >
Emissions
Elhylcne Unc Ibi/hr
4.» OJ 0487
4.4 OJ M»S
4S OJ 0.099
45 OJ OJ99
43 0.9 0494
4.4 0.9 0.097
Emissions
Ammonia Unc ibs/hr
OJ 04 0.011
04
0.*
0.*
04
0.4 0.7 0.006
Emissions
Toluene Unc Ibi/hr
273 U 0340
273 1J 0340
2.4
24
24
1.7 2.3 0.021
1-Penlene Unc
11.7 2J
144 OJ
10.7 2.2
12J OS
12.4 OJ
11.2 1.0
Pemane Unc
13 1.1
1.2
1.4 1.1
1.2
1 1.2
0.3 1.4
Dale
6/26/97
Time
»:S3
9.59
10:04
10:21
10:2*
10:37
10:43
10:4*
11:28
11.29
11:30
11:31
11:32
11:33
11:33
11:34
11:35
11:36
11:37
11:38
11:39
11:40
11:41
11:42
11:42
11:43
11:44
11.45
RleName
OUTS3001
OUTS3M1
OUTS3003
OUTS3004
OUTS3005
OUTS3006
OUTS3007
OUTS3008
16260038
16260039
16260040
16260041
16260042
16260043
16260044
16260045
16260046
16260047
16260048
16260049
16260050
16260051
16260052
16260053
16260054
16260055
16260056
16260057
p«H|*tfjfly|f
Elhylene Unc Ibs/hr
2.7 04 OJ59
3.5 04 OJ077
3.7 0.7 04*1
2.7 04 0459
2.8 04 0.0*0
3J 04 0.077
3J 04 0.077
3.4 04 0475
4.8 0.7 0.105
4.8 0.7 0.105
4.9 0.7 0.108
5.0 0.7 0.109
5.0 0.7 0.110
5.1 0.7 O.I 11
5.0 0.7 0.110
5.1 0.7 0.112
5.1 0.7 O.I 11
5.1 0.7 O.I 10
5.1 0.7 0.111
5.1 0.7 0.112
5.1 0.7 0.112
5.2 0.7 0.113
5.2 0.7 0.114
5.3 0.8 0.115
5.3 0.7 0.116
5.4 0.7 0.117
5.4 0.7 0.119
5.5 0.8 Q.I19
Emissions
Ammonia Unc Ibs/hr
1.0 OJ 0.014
OJ OJ 0.011
04 OJ 0.009
0.4
OJ
0.4
OJ
OJ
4.0 0.6 0.053
3.7 0.6 0.049
3.2 0.6 0.042
2.8 0.6 0.038
2.6 0.6 0.034
2.4 0.6 0.032
2.2 0.6 0.029
2.1 0.6 0.028
2.0 0.6 0.026
1.9 0.6 0.025
1.8 0.6 0.024
1.8 0.6 0.023
1.7 0.6 0.022
1.6 0.6 0.022
1.6 0.6 0.021
1.5 0.6 0.020
1.5 0.6 0.020
1.4 06 0.019
1.4 0.6 0.019
1.4 0.6 0.018
Emissions
Toluene Unc Ibs/hr
2iJ 1.1 0355
73 1.2 0490
1.7
28.1 1.1 0349
283 1.1 0352
1.4
U
1J
1.9
1.9
1.9
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.1
2.1
2.0
2.1
2.0
2.1
l-Pentene Unc
64 0.8
43 0.9
5.9 0.9
5.4 OJ
5.4 OJ
4J 0.8
44 0.8
4.2 OJ
3.9 1.0
4.0 1.0
4.0 1.0
3.8 I.I
3.8 I.I
3.7 I.I
3.8 I.I
3.8 I.I
3.7 I.I
3.8 1.1
3.8 I.I
3.7 1.1
4.0 I.I
3.8 I.I
4.2 I.I
4.2 I.I
4.2 1.1
4.2 I.I
4.2 I.I
4.4 I.I
Penune Unc
1.9
14
1.6
1.4
1.4
13
1.4
1.4
1.8
1.8
1.8
1.8
1.9
1.9
1.9
1.8
1.9
1.9
1.9
1.9
1.9
1.9
1.9
1.9
1.9
1.9
1.9
1.9
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date Time
6/26/97
11:46
11:47
11:48
11.49
11:50
11:51
11:52
11:53
12:23
12:24
12:25
12:25
12:26
12:27
12:28
12:29
12:30
13:07
13:08
13:09
13:10
13:11
13:12
13:13
13:14
13:15
13:16
13:16
13:17
13:18
13:19
13:20
13:21
13:22
13:23
13.24
13:25
File Name
16260058
16260059
16260060
16260061
16260062
16260063
16260064
16260065
16260093
16260094
16260095
16260096
16260097
16260098
16260099
16260100
16260101
16260138
16260139
16260140
16260141
16260142
16260143
16260144
16260145
16260146
16260147
16260148.
16260149
16260150
16260151
16260152
16260153
16260154
16260155
16260156
16260157
Emisrioiu
Elhylene line Ita/hr
5.5 0.8 0.119
5.5 0.8 0.121
5.6 0.8 0.122
5.6 0.8 0.121
5.6 0.8 0.122
5.7 0.8 0.124
5.6 0.8 0.123
5.7 0.8 0.124
6.8 0.7 0.149
6.9 0.7 0.152
7.0 0.8 0.153
7.0 0.8 0.153
7.0 0.8 6.153
7.1 0.8 0.154
7.0 0.8 0.153
7.1 0.8 0.154
7.1 0.8 0.156
7.1 0.8 0.155
7.0 0.8 0.153
6.9 0.8 . 0.151
7.1 0.8 0.154
7.1 0.9 0.156
7.2 0.9 0.157
7.2 1.0 0.157
7.1 1.0 0.155
6.9 1.0 0.151
6.8 1.0 0.150
6.7 1.0 0.146
6.6 1.0 0.143
6.4 0.9 0.140
6.4 1.0 0.140
6.3 10 0.138
6.5 1.0 0.142
6.4 10 0.139
6.3 1.0 0.137
6.1 I" 0.134
6.1 1-0 0.134
Emission*
Ammonia Unc Ibtflu
1.4 0.6 0.018
1.3 0.6 0.018
1.3 0.6 0.017
1.2 0.6 0.016
1.2 0.6 0.016
1.2 0.6 0.016
1.1 0.6 0.015
1.1 0.6 0.015
4.4 0.6 0.058
4.0 0.6 0.053
3.5 0.6 0.046
3.2 0.6 0.042
2.9 0.6 0.039
2.7 0.6 0.036
2.6 0.6 0.034
2.4 0.6 0.032
2.3 0.6 0.031
3.9 0.6 0.052
3.7 0.6 0.049
3.4 0.7 0.046
3.3 0.7 0.044
3.2 0.7 0.042
3.0 0.8 0.040
2.9 0.8 0.038
2.7 0.8 0.036
. 2.6 0.8 0.034
2.4 0.8 0.032
2.3 0.8 0.030
2.1 0.8 0.028
2.0 0.8 0.027
1.9 0.8 0.025
1.8 0.8 0.024
l.g 0.8 0.024
1.7 0.8 0.023
1.7 0.8 0.022
1.7 0.8 0.022
1.6 0.8 0.021
Emissions
Toluene Unc \biflit
2.1
2.1
2.1
2.1
2.1
2.1
2.1
2.1
5.0 1.5 0.063
4.6 1.5 0.057
4.7 1.5 0.059
4.7 1.6 0.058
4.6 1.6 0.058
4.4 1.6 0.055
4.8 1.6 0.059
4.4 1.6 0.055
4.7 1.6 0.058
2.2
2.3
2.3
2.5
2.6
2.7
2.7
2.8
2.8
2.8
2.8
2.8
2.7
2.7
2.8
2.8
2.8
2.8
2.9
2.8
1-Pemene Unc
4.4 I.I
4.4 1.1
4.6 1.1
4.6 1.1
4.7 I.I
4.5 1.1
4.6 1.1
4.7 I.I
5.7 1.1
5.9 1.1
6.0 I.I
6.1 1.2
6.0 1.2
5.9 1.2
6.1 1.2
6.1 1.2
6.2 1.2
5.0 1.2
5.4 1.2
5.8 1.3
6.1 1.3
6.3 1.4
6.3 1.4
6.5 1.5
6.6 1.5
6.5 1.5
6.4 1.5
6.4 1.5
6.4 1.5
6.2 1.5
6.0 1.5
6.1 1.5
6.1 1.5
6.1 1.5
5.9 1.5
6.0 1.5
5.9 1.5
Peniane Unc
2.0
2.0
2.0
2.0
1 2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.1
2.1
2.1
2.1
2.1
2.,
20
21 1
2.2
2.3
2.4
2.5
2.6
26
27
2.6
2.6
2.6
2.5
2.6
2.6
2.6
2.7
2.6
2.7
2.6.
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Dale
6/26/97
Time
13.26
13:27
13:27
13:28
13:29
13:30
13:31
14.32
14:33
14:34
14:35
14:36
14:37
14:38
14:39
14:40
14:40
14:41
14:42
14:43
14:44
14:45
14:46
14:47
14:48
14:49
14:50
14:51
14.51
14:52
14:53
14:54
14:55
14:56
14:57
14:58
14:59
File Name
16260158
16260159
16260160
16260161
16260162
16260163
16260164
16260199
16260200
16260201
16260202
16260203
16260204
16260205
16260206
16260207
16260208
16260209
16260210
16260211
16260212
16260213
16260214
16260215
16260216
16260217
16260218
16260219
16260220
16260221
16260222
16260223
16260224
16260225
16260226
16260227
16260228
Emissions
Elhylene Unc Ibi/hr
6.1 1.0 0.132
6.0 1.0 0.131
6.0 1.0 0.130
6.0 1.1 0.131
6.0 1.1 0.132
5.9 1.1 0.129
5.9 1.1 0.130
6.5 1.0 0.142
6.6 1.1 0.143
6.7 1.1 0.146
6.7 1.1 0.147
6.7 I.I 0.146
6.8 1.1 0.148
6.7 1.1 0.147
6.8 I.I 0.149
6.9 1.1 0.150
6.8 1.1 0.149
6.8 1.1 0.149
6.7 I.I 0.147
6.7 1.1 0.146
6.6 1.1 0.144
6.4 I.I 0.140
6.4 1.1 0.140
6.3 1.1 0.138
6.2 1.1 0.136
6.1 I.I 0.133
6.0 I.I 0.131
5.9 1.1 0.129
5.9 1.0 0.129
5.7 1.0 0.125
5.8 I.I 0.127
5.8 11 0.126
5.7 1.0 0.125
5.7 1-0 0.125
5.8 1-0 0.126
5.8 1-0 0.127
6.0 II 0.130
Emissions
Ammonia Unc Ibs/hr
1.6 0.8 0.021
1.5 0.8 0.020
1.5 0.8 0.020
1.5 0.8 0.019
1.5 0.8 0.020
1.4 0.9 0.019
1.4 0.8 0.019
3.7 0.9 0.050
3.6 0.9 0.047
3.3 0.9 0.044
3.1 0.9 0.041
2.9 0.9 0.038
2.7 0.9 0.035
2.5 0.9 0.034
2.5 0.9 0.033
2.3 0.9 0.030
2.2 0.9 0.029
2.1 0.9 0.028
2.1 0.9 0.027
1.9 0.9 0.026
1.8 0.9 0.024
1.7 0.9 0.023
1.6 0.9 0.022
1.6 0.9 0.021
1.6 0.9 0.021
1.5 0.9 0.020
1.4 0.9 0.019
1.4 0.9 0.019
1.4 0.9 0.019
1.3 0.9 0.018
1.3 0.9 0.017
1.3 0.9 0.017
1.2 0.9 0.016
1.2 0.9 0.016
1.2 0.9 0.015
1.2 0.8 0.016
1.2 0.9 0.016
Emissions
Toluene Unc Ibs/hr
2.8
2.9
2.9
2.9
2.9
3.0
3.0
5.4 2.2 0.067
5.5 2.2 0.069
5.5 2.3 0.069
5.6 2.3 0.070
5.0 2.2 0.062
5.2 2.3 0.065
2.4
5.3 2.3 0.066
5.0 2.3 0.063
5.1 2.3 0.064
5.5 2.3 0.069
6.0 2.2 0.075
5.4 2.3 0.067
2.4
5.1 2.3 0.063
6.1 2.2 0.076
5.1 2.2 0.064
3.2
5.9 2.2 0.073
5.3 2.2 0.066
2.3
5.8 2.2 0.073
5.0 2.2 0.062
5.2 2.3 0.065
5.5 2.2 0.068
3.1
3.0
5.2 2.2 0.065
3.1
3.0
1 -Penlene Unc
5.8 1.5
5.8 1.6
6.0 1.5
5.8 1.6
5.7 1.6
5.9 1.6
5.9 1.6
7.8 1.6
8.3 1.6
8.4 1.7
8.6 1.7
8.1 1.6
8.7 1.7
8.4 1.7
8.5 1.7
8.4 1.7
8.5 1.7
8.7 1.7
11.3 0.6
8.4 1.7
8.3 1.7
8.6 1.7
11.2 0.6
8.4 1.7
8.2 1.7
11.2 0.6
11.1 0.6
7.9 1.7
10.9 0.6
8.1 1.7
8.4 1.7
10.7 0.6
7.9 1.6
7.8 1.6
10.3 0.6
7.7 1.6
7.8 1.6
Penlane Unc |
2.6 1
2.7 1
2.7
2.7
1 2.8
2.8
2.8
2.1
2.2
2.2
2.3
2.2
2.3
2.3
3.0
3.0
2.3
3.0
1.4
3.0
2.3
2.9
1.9
2.2
3.0
1.9
1.4
2.2
1.4
2.9
3.0
1.9
2.9
2.9
1.9
2.1
2.1
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/26/97
me
<*i
V*
Emissions
Elhylene Unc Ibs/hr
6.0 1.0 0.131
6.2 1.1 0.135
6.2 1.1 0.135
44. M o.ow
' ai . • •'• **• onm
U . • M. • 0,056
24 • ' 04 ' 0.$
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/27/97
Time
9:49
9:50
9:51
9:52
9:52
9:53
9:54
9:55
9:56
9:57
9:58
9:59
10:00
10:01
10:02
10:02
10.O3
10:04
10:05
1006
10:07
10:08
10:09
10:10
10:11
10:12
10:12
10:13
10:14
10.15
10:16
10:53
10:54
10:55
10:56
10:57
10:58
file Name
16270002
16270003
16270004
16270005
16270006
16270007
16270008
16270009
16270010
1627001 1
16270012
16270013
16270014
16270015
16270016
16270017
16270018
16270019
16270020
16270021
16270022
16270023
16270024
16270025
16270026
16270027
16270028
16270029
16270030
16270031
16270032
16270068
16270069
16270070
16270071
16270072
16270073
Emission!
Elhylene Unc Ibj/hr
5.2 1.2 0.114
S.2 1.1 0.115
5.3 1.2 0.115
5.3 1.2 0.116
5.3 1.2 0.116
5.3 1.2 0.117
S.4 1.2 0.117
5.3 1.2 0.116
5.3 1.2 0.116
5.3 1.2 0.116
5.3 1.2 0.115
5.3 1.2 0.116
5.2 1.2 0.114
5.2 1.2 0.114
5.2 1.2 0.114
5.2 1.2 0.114
5.3 1.2 0.115
5.2 1.2 OJI4
5.3 1.2 0.116
5.4 1.2 0.117
5.4 1.2 . 0.118
5.5 1.2 0.119
5.4 1.2 0.119
5.5 1.2 0.119
5.4 1.3 0.119
5.5 1.2 0.121
5.6 1.2 0.121
5.6 1.3 0.123
5.6 1.3 0.122
5.6 1.3 0.122
5.6 1.3 0.122
5.2 1.1 0.114
5.5 1.1 0.120
5.8 1.2 0.127
6.0 1.2 0.130
6.3 1.2 0.137
6.5 1.2 0.141
Emission!
Ammonia Unc Ibi/hr
2.3 0.9 0.030
2.1 0.9 0.028
1.9 0.9 0.025
1.8 0.9 0.024
1.7 0.9 0.023
1.6 1.0 0.021
1.5 0.9 0.020
1.5 1.0 0.020
1.4 1.0 0.019
1.4 1.0 0.019
1.4 0.9 0.019
1.3 1.0 0.018
1.4 1.0 0.018
1.4 0.9 0.018
1.3 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.3 1.0 0.018
1.4 0.9 0.018
1.4 0.9 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.018
1.4 1.0 0.019
1.4 1.0 0.019
1.4 1.0 0.018
1.4 1.0 0.019
2.2 0.9 0.029
2.0 0.9 0.026
1.8 1.0 0.024
1.7 1.0 0.023
1.6 1.0 0.022
1.6 1.0 0.021
Emission!
Toluene Unc Ibi^ir
2.8
2.8
2.9
2.9
2.9
2.9
2.9
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.1
3.1
3.1
3.1
3.1
3.1
3.1
3.2
2.9
3.0
3.1
3.1
3.2
3.2
l-Penlene Unc
6.6 1.5
6.3 1.5
6.7 1.6
6.5 1.6
6.7 1.6
6.6 1.6
6.6 1.6
6.7 1.6
6.7 1.6
6.3 1.6
6.3 1.6
6.6 1.6
6.3 1.6
6.4 1.6
6.2 1.6
6.3 1.6
6.5 1.6
6.4 1.6
6.3 1.6
6.4 1.6
6.6 1.6
6.4 1.6
6.7 1.6
6.5 1.6
6.9 1.7
7.0 1.7
6.8 1.7
6.8 1.7
7.1 1.7
7.0 1.7
7.1 1.7
5.3 1.6
5.7 1.6
6.2 1.7
5.9 1.7
6.3 1.7
6.2 1.7
Penune Unc
2.7
2.7
2.7
2.7
1 2.7
2.8
2.8
2.8
2.9
2.8
2.8
2.8
2.8
2.8
2.8
2.8
2.9
2.8
2.8
2.8
2.9
2.8
2.8
2.9
2.9
2.9
2.9
2.9
2.9
3.0
3.0
2.7
2.8
2.9
2.9
3.0
3.0
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Date
6/27/97
Time
10:59
11:00
11:01
11:01
11:02
11.03
11:47
11:48
11:48
11:49
11:50
11:51
11:52
11:53
11:54
11:55
11:56
11:56
11:57
11.58
11:59
12:00
12:01
12:02
12:03
12:04
12:05
12:05
12:06
12:07
12:08
12:09
12:10
12.11
12:12
12:49
12:50
File Name
16270074
16270075
16270076
16270077
16270078
16270079
16270122
16270123
16270124
16270125
16270126
16270127
16270128
16270129
16270130
16270131
16270132
16270133
16270134
16270135
16270136
16270137
16270138
16270139
16270140
16270141
16270142
16270143
16270144
16270145
16270146
16270147
16270148
16270149
16270150
16270186
16270187
Enuuioni
Elhylene line Ibs/hr
6.7 1.2 0.145
6.9 1.3 0.151
7.0 1.3 0.153
6.9 1.3 0.151
7.1 1.3 0.155
7.1 1.3 0.156
5.1 0.9 O.I 11
5.3 0.9 0.115
5.5 0.9 0.120
5.6 0.9 0.123
6.2 1.0 0.134
7.5 1.3 0.163
7.6 1.2 0.165
7.2 1.2 0.157
7.0 1.1 0.153
7.1 I.I 0.154
7.4 1.2 0.162
7.7 1.3 0.168
7.5 1.2 0.164
7.4 1.2 0.161
7.2 1.2 0.157
7.0 1.2 0.154
6.8 1.1 0.149
6.8 1.1 0.148
6.7 1.1 0.147
6.7 1.1 0.145
6.6 1.1 0.144
6.5 1.1 0.142
6.5 1.1 0.142
6.4 I.I 0.140
6.4 1.1 0.140
6.3 I.I 0.138
6.3 1.1 0.138
6.5 I.I 0.141
6.5 I.I 0.142
4.9 1.2 0.107
4.7 1.3 0.102
Enuuioni
Ammonia Unc tta/ta
1.5 1.0 0.020
1.5 1.0 0.020
1.5 1.1 0.020
1.4 1.0 0.019
1.4 1.1 0.019
1.4 I.I 0.019
2.1 0.7 0.028
1.9 0.7 0.025
1.7 0.7 0.023
1.7 0.7 0.022
1.7 0.8 0.022
1.7 1.0 0.022
1.6 1.0 0.021
1.6 1.0 0.021
1.6 0.9 0.021
1.6 0.9 0.022
1.6 1.0 0.021
1.6 1.0 0.022
1.7 1.0 0.022
1.7 1.0 0.023
1.8 1.0 0.024
1.8 1.0 0.024
1.8 0.9 0.024
1.8 0.9 0.024
1.8 0.9 0.024
1.9 0.9 0.025
1.9 ' 0.9 0.025
1.9 0.9 0.025
1.8 0.9 0.024
1.9 0.9 0.025
1.9 0.9 0.025
1.8 0.9 0.024
1.9 0.9 0.025
1.9 0.9 0.025
1.9 0.9 0.025
3.3 1.0 0.044
3.l_ 1.0 0.04.1
Emiuiom
Toluene Unc Itayhr
3.2
3.3
3.3
3.3
3.4
3.4
2.3
2.3
2.3
2.3
2.6
3.1
3.0
3.0
2.8
2.9
3.1
3.2
3.2
3.2
3.2
3.1
3.1
3.1
3.1
3.0
3.1
3.1
3.1
3.1
3.0
3.1
3.1
3.1
3.1
3.5
6.5. 25 0.081
1-Penleoe Unc
6.7 1.7
6.9 1.8
6.6 1.8
6.8 1.8
7.1 1.8
7.2 1.8
4.1 1.2
4.0 1.2
4.1 1.2
4.3 1.3
4.8 1.4
5.1 1.6
5.2 1.6
5.3 1.6
5.1 1.5
5.2 1.5
5.5 1.7
5.9 1.7
5.9 1.7
5.7 1.7
6.1 1.7
5.7 1.7
5.6 1.7
6.0 1.7
5.5 1.6
5.6 1.6
5.8 1.7
5.6 1.6
5.7 1.7
5.4 1.6
5.5 1.6
5.5 1.6
5.4 1.6
5.4 1.7
5.5 1.7
11.0 0.7
-11.2 £.7
PenCane Unc
3.0
3.1
3.1
3.1
1 3.2
3.2
2.1
2.1
2.2
2.2
2.4
2.9
2.1
28 1
2.6
2.7
2.9
3.0
3.0
3.0
3.0
2.9
30
2.9
2.9
2.8
2.9
2.9
2.9
2.9
2.9
2.9
2.9
2.9
2.9
2.1
£.1
-------
TABLE B-2. CONTINUED. (LTV Scrubber Outlet)
Dale
6/27/97
Time
12:51
12:55
12:59
13:02
13:09
13:12
13:16
File Name
16270188
OUT4S007
OUTS4008
OUTS4009
OUTS4010
OUTS4011
OUTS4012
Average — >
Emissions
Ethylene Unc Un/hr
4.8 1.3 0.106
5.1 U 0.111
5.1 1.1 0.111
53 1.0 0.116
44 04 0.107
5.1 04 0.111
4.6 04 0.101
6.0 1.2 0.131
Emission]
Ammonia Unc Itn/hr
3.0 0.9 0.039
2.9 0.9 0.039
2.4 0.8 0.031
1.7 0.7 0.023
1.2 0.7 0.015
1.1 0.7 0.014
1.0 0.7 0.013
1.7 0.9 0.023
Emissions
Toluene Unc Ibs/hr
3.4
33
3.0
2.8
24.6 2.0 0306.
25.7 2.0 0320
253 2.0 0315
0.1 3.0 0.001
1-Pentene Unc
10.5 0.7
11.1 0.7
4.6 1.6
4.2 1.5
9.6 0.6
10.0 0.6
9.1 0.6
6.3 1.6
Pentane Unc
2.1
1.5
2J
2.7
1 1.7
1.7
1.7
2.8
' Blank space* indicate the compound was not detected in that sample. These arc included in the averages as zero concentrations.
9 Hie Names are in the data records in Appendii B. Bold face type inrtinlrs a sample that was spiked with SFt or toluene. Spiked samples are not included in the mn averages.
-------
TABLE B-3. SUMMARY OF SPIKED AND UNSPIKED CONCENTRATIONS AT LTV '
LTVUkt
File Name
Rail SUrt
INLS2002
1NLS2003
INLS2004
INLS2005
INLS2006
INLS2007
RwilEMl
INLV2046
INLV2047
INLV2048
INLS2049
INLS2050
INLS20S1
[NLS2052
INLS2053
INLS2054
Ron 2 Start
INLS300I
INLS3002
INLS3003
INLS3004
D4LS3005
INLS3006
16260004
16260005
16260006
Date Time
6/25/97 9:33
9:37
9:43
9:54
9:58
10:02
Avenge Spike
Average Unspike
6/25/97 16:48
16:54
16:58
17:07
17:10
17:14
17:20
17:24
17:27
Average Spike
Average Unspike
6/26/97 9:11
9:18
9:22
9:34
9:38
9:42
10:55
10:56
10:57
Average Spike
Average Unspike
Toluene
Spiked
ppm
26.7
26.6
26.2
26.5
32.9
34.0
34.6
33.8
32.5
33.5
33.4
33.1
Umpiked
ppm
0.0
0.0
0.0
0.0
3.5
0.0
0.0
1.2
4.3
4.3
4.5
4.4
SF6
Spiked
ppm
0.536
0.555
0.553
0.548
0.665
0.668
0.664
0.666
0.660
0.658
0.657
0.658
Unspiked
ppm
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
LTV Outlet
File Name Date Time
Rim 1 Start
OUTS2001 6/25/97 8:41
OUTS2002 8:46
OUTS2003 8:52
OUTS2004 9:02
OUTS2005 9:08
OUTS2006 9:13
Avenge Spike
Average Unspike
RunlEarf
INLV2044 6/25/97 16:39
INLV2045 16:43
INLV2046 16:48
OUTS2047 17:36
OUTS2048 17:41
OUTS2049 17:46
OUTS20SO 17:56
OUTS2051 18:00
OUTS2052 18:04
Average Spike
Avenge Unspike
Run 2 SUrt
OUTS3001 6/26/97 9:53
OUTS3002 9:59
OUTS3003 10:04
OUTS3004 10:21
OUTS3005 10:26
OUTS3006 10:37
OUTS3007 10:43
OUTS3008 10:49
Average Spike
Average Unspike
Toluene
Spiked
ppm
Spiked
23.4
23.7
23.4
23.5
26.9
27.3
27.3
27.2
28.5
28.1
28.3
28.3
Unspikec
ppm
Unspiked
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
SF6
Spiked
ppm
Spiked
0.465
0.479
0.479
0.474
0.504
0.515
0.515
0.512
0.568
0.562
0.559
0.563
Unspike*
ppm
UnspikH
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
0.000
' These results are taken from Tables B-1 and B-2 and arc summarized in Table 4-3.
-------
TABLE B-3. SUMMARY OF SPIKED AND UNSP1KED CONCENTRATIONS AT LTV"
LTV Inlet
File Name Date Time
RnnlEai
16260261 6/26/97 11:30
16260262 13:31
16260263 13:32
16260264 13:33
INLS3007 16:00
INLS3008 16:06
INLS3009 16:10
INLS3010 16:13
INLS3011 16:24
INLS3012 16:28
INLS3013 16:33
Average Spike
Avenge Urapike
Run3SUrt
INLS4001 6/27/97 9:21
INLS4002 9:23
INLS4003 9:29
[NLS4004 9:35
INLS4005 9:40
INLS4006 9:44
16270035 10:21
16270036 10:22
16270037 10:23
Avenge Spike
Average Unspike
Rim 3 End
16270182 6/27/97 12:42
16270183 12:43
16270184 • 12:44
INLS4007 13:22
INLS4008 . 13:25
INLS4009 13:29
INLS4010 13:36
INLS4011 13:41
INLS4012 13:45
Average Spike
Average Unspike
Toluene
Spiked Unspiked
ppm ppm
4.9
4.9
5.0
47.2
50.8
51.0
49.6
4.9
38.0
37.5
37.5
•
4.2
4.1
4.2
37.7
4.2
0.0
0.0
0.0
54.7
57.3
57.4
56.5
0.0
SF6
Spiked Unspiked
ppm ppm
0.000
0.000
0.000
0.997
1.038
1.029
1.022
0.000
0.730
0.749
0.756
0.000
0.000
0.000
0.745
0.000
0.000
0.000
0.000
1.167
1.223
1.243
1.211
0.000
LTV Outlet
File Name Date Time
Run 2 End
OUTS3009 6/26/97 16:48
OUTS3010 16:53
OUTS301 1 16:58
OUTS3012 17:09
OUTS3013 17:15
OUTS30I4 17:20
Avenge Spike
Average Unspike
Rim 3 Start
OUTS4001 6/27/97 8:46
OUTS4002 8:51
OUTS4003 8:55
OUTS4004 9:03
OUTS4005 9:08
OUTS4006 9:13
Average Spike
Average Unspike
Run 3 End
OUT4S007 6/27/97 12:55
OUTS4008 12:59
OUTS4009 13:02
OUTS4010 13:09
OUTS4011 13:12
OUTS4012 13:16
Average Spike
Avenge Unspike
Toluene
Spiked Unspiked
ppm ppm
0.0
0.0
4.1
29.0
29.1
28.8
29.0
1.4
0.0
0.0
0.0
28.2
29.0
285
28.6
0.0
0.0
0.0
0.0
24.6
25.7
25.3
25.2
0.0
SF6
Spiked Unspikec
ppm ppm
0.571
0.574
0.573
0.000 '
0.000
0.000
0.572
0.000
0.542
0.344
0.532
0.000
0.000
0.000
0.539
0.000
0.438
0.487
0.490
0.000
0.000
0.000
0.472
0.000
* These results are taken from Tables B-l and B-2 and are summarized in Table 4-3.
-------
1000
CO Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlet -e—Oullei
800-
i
600
i
400
200
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
1000
CO Concentrations at LTV Inlet and Outlet (6/26/97)
•Inlet -G— Outlet
800-
600
400
200
THC Cal Gas Dilution
8:30
9:30
10:30
11:30
12:30
13:30
Time
14:30
15:30
16:30
17:30
-------
CO Concentrations at LTV Inlet and Outlet (6/27/97)
lnlei -e-Outlet]
1000
800
600-
400
200-
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
160
SO2 Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlet
Outlet
140
120
100
80
60
40
20
8:30
9:30
10:30 11:30
12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
SO2 Concentrations at LTV Inlet and Outlet (6/26/97)
•Inlet -O— Outlet
150
§
130 -
110
90-
70 -
50-
30
10
-10
\
8:30 9:30 10:30 11:30 12:30
13:30
Time
OODOOD
14:30 15:30 16:30 17:30
-------
SO2 Concentrations at LTV Inlet and Outlet (6/27/97)
•Inlet -d— Outlet
130
110-
90
§.
70
50
30
10
-10
Vfr«*
-------
20
Formaldehyde Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlet —9— Outlet
15
10
5
eft
-------
Formaldehyde Concentrations at LTV Inlet and Outlet (6/26/97)
•Inlet -0— Outlet
10
8
0
THC Cal Gas Dilution
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
Formaldehyde Concentrations at LTV Inlet and Outlet (6/27/97)
•Inlet O Outlet
12
10
8
2-
8:30
9:30
10:30 11:30 12:30 13:30
Time
-------
30
Methane Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlel -O— Outlet
25 -
20
15
10
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
Methane Concentrations at LTV Inlet and Outlet (6/26/97)
30
•Inlet -«—Outlet
25 -
20
15
10
THC Cal Gas Dilution
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15.30 16:30 17.30
-------
Methane Concentrations at LTV Inlet and Outlet (6/27/97)
•Inlet
Outlet
30
25 -
20
15
10
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
10
Etbylene Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlei
— &— Outlet
8 -
6
2 -
8:30
9:30
10:30
11:30
12:30
13:30
Time
14:30
15:30
16:30
17:30
-------
Ethylene Concentrations at LTV Inlet and Outlet (6/26/97)
10
-Inlet -G— Outlet
8 -
0
THC Cal Gas Dilution
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
Ethylene Concentrations at LTV Inlet and Outlet (6/27/97)
•Inlet -Q— Outlet
10
8
6
i
4
2
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
Ammonia Concentrations at LTV Inlet and Outlet (6/25/97)
•Inlel -d—Ouilel
10
8-
I 4
a.
r
-2
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
Ammonia Concentrations at LTV Inlet and Outlet (6/26/97)
•Inlet -0— OuUet
12
10
8
6-
4
2
r
-2
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30 15:30 16:30 17:30
-------
Ammonia Concentrations at LTV Inlet and Outlet (6/27/97)
•Inlet O Outlet
10
8-
6
r
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
Toluene Concentrations at LTV Inlet and Outlet (6/25/97)
50
•Inlet
-Outlet
45
40
35
30
25
20
is ^
10
5
0
-5
8:30
0 G
9:30
10:30
11:30
12:30
13:30
Time
14:30
(BSD Q89D
15:30
16:30
17:30
-------
Toluene Concentrations at LTV Inlet and Outlet (6/26/97)
•Inlet
•Gullet
55 -
45 -
35
I
Ok
25
15
-5
8:30 9:30 10:30 11:30 12:30
13:30
Time
14:30
15:30 16:30 17:30
-------
Toluene Concentrations at LTV Inlet and Outlet (6/27/97)
-Inlet
•Outlet
55 -
45
35
25
15
5
-5
8:30
9:30
10:30
11:30
12:30
13:30
Time
-------
B-4 HYDROCARBON REFERENCE SPECTRA
-------
Reference Spectra of Hydrocarbon Compounds
The purpose of measuring reference spectra of some hydrocarbon compounds was to aid the
analyses of FI1K. sample spectra from iron and steel foundries and from integrated iron and steel
plants. Four facilities were tested at these sources. At each facility hydrocarbon compounds were
detected in the emissions. Because the EPA library of FTIR reference spectra contains only
spectra of hazardous air pollutant (HAP) compounds, only quantitative reference spectra of
hexane and isooctane were available to analyze the sample hydrocarbon emissions. As a result the
hydrocarbon emissions were represented primarily by "hexane" in the draft report results. Many
hydrocarbon compounds have infrared spectra which are similar to that of hexane in the spectral
region near 2900 cm'1. MRI selected nine candidate hydrocarbon compounds and measured then-
reference spectra in the laboratory. In addition MRI measured new high-temperature reference
spectra of hexane and isooctane. The new reference spectra of these 11 compounds were
included in revised analyses of the sample spectra. The FTIR results presented in the revised test
reports show the measured concentrations of the detected hydrocarbons and also show revised
concentrations of hexane and toluene. The hexane concentrations, in particular, are generally
lower because the infrared absorbance from the hydrocarbon emissions is partly measured by the
new reference spectra. As an example, figure B-1 illustrates the similarities among a sample
spectrum and reference spectra of hexane and n-heptane.
MRI prepared a laboratory plan specifying the procedures for measuring the reference spectra.
The EPA-approved laboratory plan is included in this appendix. The data sheets, check lists and
other documentation are also included. During the measurements some minor changes were made
to the laboratory plan procedures. These changes don't affect the data quality, but did allow the
measurements to be completed in less time. This was necessary because the plan review process
was more length than anticipated.
The following changes were to the procedures. The spectra were measured at 1.0 cm'1 resolution,
which was the highest resolution of the sample spectra. It was unnecessary to use a heated line
connection between the mass flow meter and the gas cell because the gas temperature in the cell
was maintained without the heated line. Leak checks were conducted at positive pressure only
because all of the laboratory measurements were conducted at ambient pressure. The reference
spectra, CTS spectra, and background spectra will be provided on a disk with a separate reference
spectrum report.
-------
3000
2950 2900
Wavenumbers (cm'1)
2850
Figure B-l Top trace, example sample spectrum, middle trace, n-heptane reference spectrum; bottom trace, n-hexane reference
Spectrum.
-------
LABORATORY PLAN FOR
REFERENCE SPECTRUM MEASUREMENTS
DRAFT
Prepared for
Office of Air Quality Planning and Standards
Emissions, Monitoring and Analysis Division
Emission Measurement Center (MD-19)
Research Triangle Park, North Carolina 27711
Mr. Michael Ciolek
Work Assignment Manager
EPA Contract No. 68-D-98-027
Work Assignment 2-12 and 2-13
MRI Project No. 4951-12 and 4951-13
June 14,1999
MIDWEST RESEARCH INSTITUTE 5520 Dillard Road, Suite 100, Gary, NC 27511-9232 • (919) 851-8181
-------
TABLE OF CONTENTS
1.0 INTRODUCTION 1
1.1 Objective 1
1.2 Background 2
2.0 TECHNICAL APPROACH 2
2.1 Measurement System 2
2.2 Procedure 3
3.0 QUALITY ASSURANCE AND QUALITY CONTROL 5
3.1 Spectra Archiving ' 5
3.2 CIS Spectra 6
3.3 Sample Pressure 6
3.4 Sample Temperature 6
3.5 Spectra 6
3.6 Cell Path Length 6
3.7 Reporting 6
3.8 Documentation 7
FIGURE AND TABLE LIST
Figure 1. Measurement system configuration 4
TABLE 1. ORGANIC COMPOUNDS SELECTED FOR THE LABORATORY STUDY .... 3
in
-------
Laboratory Plan For Reference Spectrum Measurements
EPA Contract No. 68-D-98-027, Work Assignments 2-12 and 2-13
MRI Work Assignments 4951-12 and 4951-13
1.0 INTRODUCTION
In 1997 Midwest Research Institute (MRI) completed FITR field tests at two iron and
steel sintering facilities and at two iron and steel foundries. The tests were completed under EPA
Contract No. 68-D2-0165, work assignments 4-20 and 4-25 for the sintering plants and
foundries, respectively. The draft test reports were completed in 1998 under EPA Contract
No. 68-W6-0048, work assignment 2-08, tasks 11 and 08 for the sintering plants and foundries,
respectively.
Results from the data analyses indicated that the emissions from some locations included
a mixture of hydrocarbon compounds, one of which was hexane. The EPA spectral library of
MIR reference spectra is comprised primarily of hazardous air pollutants (HAPs) identified in
Title ffl of the 1990 Clean Air Act Amendments and, therefore, contains a limited number of
aliphatic hydrocarbon compounds. MRI will measure reference spectra of some additional
organic compounds that may have been part of the sample mixtures. The new reference spectra
will be used in revised analyses of the sample spectra. The revised analyses will provide a better
measure of the non-hexane sample components and, therefore, more accurate hexane
measurements.
A Quality Assurance Project Plan (QAPP) was submitted for each source under EPA
Contract No. 68-D2-0165, work assignments 4-20 and 4-25. When the QAPPs were prepared it
was not anticipated that laboratory measurements would be required. This document describes
the laboratory procedures and is an addition to the QAPPs.
This document outlines the technical approach and specifies the laboratory procedures
that will be followed to measure the FTIR reference spectra. Electronic copies of the new
reference spectra will be submitted to EPA with corresponding documentation. The laboratory
procedures are consistent with EPA's Protocol for the Use of Extractive Fourier Transform
Infrared (FTIR) Spectrometry for the Analyses of Gaseous Emissions From Stationary Sources,
revised 1996.
1.1 Objective
The objective is to obtain accurate hexane measurements from FTIR spectra recorded at
field tests at iron and steel sintering plants and at steel foundry plants. The approach is to
measure reference spectra of some organic compounds that are not included in the EPA reference
spectrum library and then use these new reference spectra in revised analyses of the field test
spectra. The revised analyses will provide better discrimination of the hexane component from
the absorbance bands of the organic mixture.
Laboratory Reference Spectnun Plan EPA Contract No. 68-D-98-027, MRI Work Assignments 2-12 and 2-13
Draft June 14, 1999 , Page
-------
1.2 Background
Spectra of samples measured at the field test sites contained infrared absorbance features
that may be due to a mixture of non-aromatic organic compounds. The samples were measured
using quantitative reference spectra in the EPA library and the hexane reference spectra provided
the best model for the observed absorbance features. The EPA library contains a limited number
of reference spectra, primarily HAPs, listed in Title HI of the 1990 Clean Air Act Amendments,
which includes hexane. To obtain accurate measurements of target components it is helpful to
use reference spectra of all compounds in the sample gas mixture. In this case it was decided to
measure reference spectra of some additional organic compounds, which are similar in structure
and have spectral features similar to hexane. The revised analyses will measure the sample
absorbance in the 2900 cm*1 region using a combination of the hexane and new reference
spectra. The revised analyses should provide more accurate hexane measurements, by measuring
the non-hexane sample components more accurately.
2.0 TECHNICAL APPROACH
The analytical region used to measure hexane lies near 2900 cm"1. Other aliphatic
hydrocarbons with structures similar to hexane exhibit similar absorbance band shapes in this
region. MRI viewed spectra of aliphatic organic compounds to identify some likely components
of the sample spectra. Table 1 identifies the compounds that were selected for reference
spectrum measurements. Cylinder standards of the selected compounds will be purchased from a
commercial gas supplier. The standards will be about SO ppm of the analyte in a balance of
nitrogen. The cylinders will contain gravimetric standards (analytical accuracy of ±1 percent) in
a balance of nitrogen.
2.1 Measurement System
A controlled, measured flow of the gas standard will be directed from the cylinder to the
infrared gas cell. The gas cell is a CIC Photonics Pathfinder. This is a variable path White cell
with an adjustable path length from 0.4 to 10 meters. The path lengths have been verified by
measurements of ethylene spectra compared to ethylene spectra in the EPA FTIR spectral library.
The inner cell surface is nickel coated alloy to minimize reactions of corrosive compounds with
the cell surfaces. The cell windows are ZnSe. The cell is heat-wrapped and insulated.
Temperature controllers and digital readout are used to control and monitor the cell temperature
in two heating zones. The gas temperature inside the cell will be recorded using a T-type
thermocouple temperature probe inserted through a 1/4 in. Swagelok fitting. The gas
temperature will be maintained at about 120°C. Documentation of the temperature probe and
thermometer calibration will be provided with the report.
Laboratory Reference Spectrum Plan EPA Contract No. 68-D-98-027. MRI Work Assignments 2-12 and 2-13
Draft June 14. 1999 Page
-------
Compound Name
n-hexanea
n-heptane
Pentane
isooctane*
1-pentene
2-methyl,l-pentene
2-mcthyl,2-butene
2-methy!,2-pentene
3-methylpentane
Butane
- -"— *.'—"« *«j_ i^r~m\si\.r-i i wrv. i j 1 \JLJ I
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98.4
36.1
99.2
30
60.7
38.6
67.3
63.3
-05
i will be re-measured because the
spectra in the EPA library were measured at ambient temperature.
The instrument is an Analect Instruments (Orbital Sciences) RFX-65 optical bench
equipped with a mercury-cadmium-telluride (MCT) detector. The RFX-65 instrument is capable
of measuring spectra at 0.125 cm"1 resolution. The reference spectra will be measured at
0.25 cm"1 or 0.50 cm'1 resolution. Gas pressure in the sample cell will be measured using an
Edwards barocell pressure sensor equipped with an Edwards model 1570 digital readout. A
record of the pressure sensor calibration will be provided with the report.
A continuous flow of the gas standard will be maintained through the cell as the spectra
are recorded. A mass flow meter will be used to monitor the gas flow (Sierra Instruments, Inc.,
model No. 822S-L-2-OK1-PV1-V1-A1,0 to 5 liters per minute).
The instrument system will be configured to measure 0.25 cm"1 or 0.50 cm"1 resolution
spectra. The measurement configuration is shown in Figure 1. Calibration transfer standards
(CTS) will be measured each day before any reference spectra are measured and after reference
spectra measurements are completed for the day.
2.2 Procedure
Information will be recorded in a laboratory notebook. Additionally, the instrument
operator will use check lists to document that all procedures are completed. There will be three
checklists for (1) daily startup prior to any reference measurements, (2) reference spectrum
measurements, and (3) daily shut down after reference measurements are completed. Example
checklists are at the end of this document.
The information recorded in the laboratory notebook includes; the cell temperature,
ambient pressure, background, CTS and spectrum file names, sample temperatures and pressures
for each measurement, cell path length settings, number of background and sample scans,
instrument
Laboratory Reference Spectrum Plan EPA Contract No. 68-D-98-027. MRI Work Assignments 2-12 and 2^3
Draft June 14. 1999 Page 3
-------
Cylinder gas inlets
Calibration
manifold
Vent
Figure 1. Measurement system configuration.
PG = pressure gauge; TP = temperature probe; MFM = mass flow meter.
resolution, gas standard concentration, sample cylinder identification, and sample flow rates for
each measurement. Certificates of Analysis for all gas standards used in the project will be
provided with the report.
The MCT detector will be cooled with liquid nitrogen and allowed to stabilize before
measurements begin.
The cell will be filled with dry nitrogen and vented to ambient pressure. The pressure, in
torr, will be recorded from the digital barocell readout. The cell will then be evacuated and leak
checked under vacuum to verify that the vacuum pressure leak, or out-gassing, is no greater than
4 percent of the cell volume within a 1-minute period. The cell will then be filled with nitrogen
and a background will be recorded as the cell is continuously purged with dry nitrogen. After the
background spectrum is completed the cell will be evacuated and filled with the CIS gas. The
CTS spectrum will be recorded as the cell is continuously purged with the CIS gas standard.
The purge flow rates will be 0.5 to 1.0 LPM (liters per minute) as measured by the mass flow
meter.
Laboratory Reference Spectrum Plan
Draft June 14, 1999
EPA Contract No. 68-D-98-027, MRJ Work Assignments 2-12 and 2-13
Page 4
-------
After the background and CIS measurements are completed the cell will be filled with a
reference gas sample. The reference spectra will be recorded as the cell is continuously purged at
0.5 to 1.0 LPM with gas standard. The gas How will be monitored with a mass How meter before
the gas enters a heated line, and with a rotameter after the gas exits the cell. The mass How
meter is calibrated for nitrogen in the range 0 to 5 LPM. The purpose of the heated line
connection is to help maintain the gas temperature inside the cell. This may only require placing
a heat wrap on the line where the gas enters the cell.
The gas temperature of each nitrogen background, CTS, and reference gas will be
recorded as its spectrum is collected.
Several preliminary spectra will be recorded to verify that the in-cell gas concentration
has stabilized. Stabilization usually occurs within 5 minutes after the gas is first introduced into
the cell with the measurement system that will be used for this project. Duplicate (or more)
reference spectra will be collected for each flowing sample. The second reference spectrum will
be recorded at least 5 minutes after the first spectrum is completed while the continuous gas flow
is maintained.
At least 100 scans will be co-added for all background, CTS , and reference
interferograms.
A new background single beam spectrum will be recorded for each new compound or
more frequently if the absorbance base line deviates by more than ±0.02 absorbance units from
zero absorbance in the analytical region.
After reference spectrum measurements are completed each day, the background and CTS
measurements will be repeated.
The CTS gas will be an ethylene gas standard, either 30 or lOOppm in nitrogen
(±1 percent) or methane (about 50 ppm in nitrogen, ±1 percent). The methane CTS may be
particularly suitable for the analytical region near 2900 cm"1.
3.0 QUALITY ASSURANCE AND QUALITY CONTROL
The following procedures will be followed to assure data quality.
3.1 Spectra Archiving
Two copies of all recorded spectra will be stored, one copy on the computer hard drive
and a second copy on an external storage medium. The raw interferograms will be stored in
addition to the absorbance spectra. After the data are collected, the absorbance spectra will be
converted to Grams (Galactic Industries) spectral format. The spectra will be reviewed by a
second analyst and all of the spectra, including the Grams versions will be provided with a report
and documentation of the reference spectra.
Laboratory Reference Spectrum Plan EPA Contract No. 68-D-98-027. MRI Work Assignments 2-12 and 2-13
Draft June 14,1999 ^
-------
3.2 CTS Spectra
The CTS spectra will provide a record of the instrument stability over the entire project.
The precision of the CTS absorbance response will be analyzed and reported. All of the CTS
spectra will be archived with the background and reference spectra.
3.3 Sample Pressure
The barocell gauge calibration will be NIST traceable and will be documented in the
reference spectrum report. The ambient pressure will be recorded daily and all of the samples
will be maintained near ambient pressure within the ER gas cell.
3.4 Sample Temperature
The [R gas cell is equipped with a heating jacket and temperature controllers. The
temperature controller readings will be recorded whenever spectra are recorded. Additionally,
the temperature of each gas sample will be measured as its spectrum is collected using a
calibrated temperature probe and digital thermometer. The calibration record will be provided
with the reference spectrum report. The gas sample will be preheated before entering the cell by
passing through a heated 20 ft. Teflon line. The Teflon line temperature will be maintained at
about 120°C. The line temperature controllers will be adjusted to keep the gas sample
temperature near 120°C.
3.5 Spectra
MRI will record parameters used to collect each interferogram and to generate each
absorbance spectrum. These parameters include: spectral resolution, number of background and
sample scans, cell path length, and apodization. The documentation will be sufficient to allow an
independent analyst to reproduce the reference absorbance spectra from the raw interferograms.
3.6 Cell Path Length
The cell path length for various settings is provided by the manufacturer's documentation.
The path length will be verified by comparing ethylene CTS spectra to ethylene CTS spectra in
the EPA spectral library.
3.7 Reporting
A report will be prepared that describes the reference spectrum procedures. The report
will include documentation of the laboratory activities, copies of data sheets and check lists, and
an electronic copy of all spectra and interferograms.
Laboratory Reference Spectrum Plw EPA Contract No. 68-D-98-027. MRI Work Assignments 2-12 and 2-13
Draft June 14, 1999 Page
-------
3.8 Documentation
Laboratory analysts will use three check lists to document data recording activities. The
check lists are appended to this plan. The checklists: (1) record start up activities such as
instrument settings, background and CTS spectra, (2) record reference spectra activities, and
(3) record daily shut down procedures, including post-reference spectra background and CTS
measurements.
In addition to the check lists the operator will record notations in a laboratory notebook.
Copies of the check lists and note book pages will be provided with the reference spectrum
report.
A draft of the reference spectrum report will be provided with the revised test reports.
The reference spectrum report will then be finalized and submitted separately.
Laboratory Reference Spectrum Plan EPA Contract No. 68-D-98-027, MRI Work Assignments 2-12 and 2-13
Draft June 14, 1999
-------
SHIPPING ORDER
MIDWEST RESEARCH INSTITUTE
425 Votk«f Boulevard, Kansas City, Missouri 64110
D TRANSFER O RETURN FOR CREDIT
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REFERENCE
QUANTITY
DESCRIPTION OF MATERIAL
PRESENT LOCATK
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PACKING SLIP
MRI11 (R«v. 8/92)
-------
Code: MRI-0701
Revision: 3
Effective: 10/23/98
Page: 12 of 12
Attachment 1
Instrument Found Out of Tolerance
Instrument: /5"7o
Manufacturer
r: -*T
MRI Number:
Serial Number:
Acceptance Criteria:
/
Date of calibration or test that revealed the out of tolerance condition:
Date of previous calibration: t.g~-e-~ U^faO Date: .
^-~ jZl? j$* *^^
Reviewed by: ^^J^rst?J^*&^ Date: _
5/7-fbrr Ai . Mayf^f i)
I hereby certify that I have received a copy of this report and will notify the appropriate
people and take the appropriate actions necessary to determine what data may have been
corrupted and what corrective actions are indicated.
(Responsible person)
MIU-QA\MIU-070I.DOC
-------
Code: MRI-0722
Revision: 0
Effective: 03/22^99
Page: 6 of 6
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MRI No. _4fc^£|f?3Model No.
Report No. L •_—
Attachment 1
Pressure Gauge Calibration Data Sheet
/ Type /T7o
Serial No c/237
Noun
-------
Code: MR]-0721
Revision: 0
Effective; 01/29/99
Page: 9 of 9
MRI No.:
Noun:T
Attachment
Calibration Data Sheet
Model No/Type: TT&' -UK-It. Serial No.:T
-------
Code: MRI-072I
Revision: 0
Effective: 01/29/99
Page: 9 of 9
Attachment
Calibration Data Sheet
Model No/Type:
Serial No.:
Noun:"rW/necea/j /e. Ambient Tempera
Applied temperature
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ofMRJ-0701 and ISO 10012-1.
Standards used: MRJ No
Notes/Adjusrments/Repairs/Modifications:
Limitations for use
Date Calibrated:
Calibration Performed
Reviewed by:
Date Due Recalibration: S"-7-OO1 Cal Interval: _/.
Date: C-?-?/
Date: J""/^ - '
-------
^^51^
Scott Specialty Gases
pped 6141 EASTON ROAD, BLDG 1 PO BOX 310
From: PLUMSTEADVILLE PA 18949-0310
Phone: 215-766-8861 Fax: 215-766-2070
CERTIFICATE OP ANALYSIS
MIDWEST RESEARCH
SCOTT KLAMM
425 VOLKER BLVD
KANSAS CITY
MO 64110
PROJECT #: 01-01788-006
P0#: 033452
ITEM #: 01021951 SAL
DATE: 3/31/98
CYLINDER #; ALM025384
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +/-5%
BLEND TYPE
COMPONENT
ETHYLENE
NITROGEN
CERTIFIED WORKING STD
REQUESTED OAS
CONC MOLB8
20.
PPM
BALANCE
ANALYSIS
(MOLES)
20.0
PPM
BALANCE
-------
Scott Specialty Gases
?ped
From:
1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
NC 27704
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC 27511
PROJECT #: 12-34162-005
P0#: 038546
ITEM #: 12022751 1AL
DATE: 5/26/99
CYLINDER #: ALM046483
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000
BLEND TYPE
COMPONENT
METHANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
52.6
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
B.M > BECTON
-------
Scott Specialty Gases
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1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
NC 27704
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC
PROJECT #: 12-34162-004
P0#: 038546
ITEM #: 12022232 1AL
DATE: 5/25/99
27511
CYLINDER #: ALM045092
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/25/2000
BLEND TYPE
•COMPONENT
N-HEXANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
49.6
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST: / S~\
L. BAYLOR
-------
Scott Specialty Gases
snipped
From:
1750 EAST CLUB BLVD
DURHAM
•Phone: 919-220-0803
NC 27704
Fax: 919-220-0808
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
GARY NC 27511
PROJECT tf: 12-34167-006
P0#: 038545
ITEM #: 1202M2034951AL
DATE: 5/27/99
CYLINDER #: ALM037409
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/27/2000
BLEND TYPE :
COMPONENT
3-METHYLPENTANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONG MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
50.0
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
-------
Scott Specialty Gases
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1750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC 27511
PROJECT #: 12-34162-006
P0#: 038546
ITEM #: 1202P2000801AL
DATE: 5/27/99
CYLINDER #: ALM041358
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: + -1%
PRODUCT EXPIRATION: 5/27/2000
BLEND TYPE
COMPONENT
N-PENTANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONG MOLES
50
PPM
BALANCE
ANALYSIS
(MOLES)
49.99 PPM
BALANCE
NIST TRACEABLE BY WEIGHT
-------
Scott Specialty Gases
pped
From:
1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
NC 27704
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC
27511
PROJECT #: 12-34167-005
P0#: 038545
ITEM tf: 1202M2034941AL
DATE: 5/26/99
CYLINDER #: ALM054078
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000
BLEND TYPE
COMPONENT
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
2 -METHYL-2 -PENTENE
NITROGEN
-50.
PPM
BALANCE
ANALYSIS
(MOLES)
51.4
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
-------
Scott Specialty Gases
Shipped
From:
1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
NC 27704
Fa-x: 919-220-0808
CERTIFICATE OP ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY • NC 27511
PROJECT #: 12-34167-004
PQ#: 038545
ITEM #: 1202M2034961AL
DATE: 5/26/99
CYLINDER #: ALM005876
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000.
BLEND TYPE
COMPONENT
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
ANALYSIS
(MOLES)
2-METHYL 2-BUTENE
NITROGEN
50.
PPM
BALANCE
50.04
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
-------
Scott Specialty Gases
bhipped
From:
L750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE OP
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC
27511
PROJECT #: 12-34167-003
P0#: 038545
ITEM #: 1202M2034971AL
DATE: 5/26/99
CYLINDER #: ALM017936
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000
BLEND TYPE
COMPONENT
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONG MOLES
ANALYSIS
(MOLES)
2 -METHYL-1-PENTENE
NITROGEN
50.
PPM
BALANCE
50.08
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
-------
Scott Specialty Gases
From:
ped
1750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
-"-I
PROJECT #: 12-34162-003
P0#: 038546
ITEM #: 1202N2007311AL
DATE: 5/26/99
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC 27511
CYLINDER #: AAL21337
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000
COMPONENT
N-HEPTANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
ANALYSIS
(MOLES)
50.
PPM
BALANCE
49.97
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
L. TAYLOR
-------
Scott Specialty Gases
Tpped
From:
1750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE OF
Fax: 919-220-080!
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
CARY NC
PROJECT #: 12-34167-002
P0#: 038545
ITEM #: 1202P2019421AL
DATE: 5/27/99
27511
CYLINDER ft: ALM041929
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/27/2000
BLEND TYPE
COMPONENT
1-PENTENE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONG MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
50.1 PPM
BALANCE
NIST TRACEABLE BY WEIGHT
-------
Scott Specialty Gases
Tpped
From:
1750 EAST CLUB BLVD
DURHAM
Phone: 919-220-0803
27704
CERTIFICATE OF
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
GARY ' . NC
27511
PROJECT #: 12-34162-001
P0#: 038546
ITEM #: 12021152 1AL
DATE: 5/25/99
CYLINDER #: ALM020217
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/25/2000
BLEND TYPE
COMPONENT
N-BUTANE
NITROGEN
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONC MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
51.3
PPM
BALANCE
MIST TRACEABLE BY WEIGHT
ANALYST:
B.M. BECTON
-------
Project No. . ^>'' ' ^ , ' ^ MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Startup Procedure
OPERATOR:
Check cell temperature ft au.
Verify temperature using thermocouple probe and hand-held readout 3^
Purge cell with dry nitrogen and vent to ambient pressure 7/9 «?
Record ambient pressure in ceo, (PJ
i Leak Check Procedure: £
Evacuate cell to baseline pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P^ If. o~J .''/$' 77$"./
Leave cell Isolated for one minute Tune Pn*
Record time and cell pressure (Pn^J ^.'ao ;y:
Calculate "leak rate" for 1 minute Time
Calculate "leak rate" as percentage of total pressure ^p
%VL.(AP/Pk)« 100
i VL| should be < 4 • % V,
Record Nitrogen Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book. ___^
Copy Background to C-drive and backup using batch file. 3L
i
Record CTS Spectra
Record Cell path length sedinj
BiaaBieCell
Fill Cell with CTS ga»
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferognm to C-drive and back up using CTS batch file
Record Barytron pressure during collect u 141 .P
RiuuniUifummiiiiiMiiTliiiU """I "llin ' ' +r^"
W.1 .
.i i,e* (^7? i.r&fW
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum FUeNamo rr4070? .
Reviewed by: ^AY^' • D
-------
Project No. —^Sl-ll ; |^_ MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATE IT
Check ceO temperature
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cell, (P^)
Vacuum Leak Check Procedure;
Evacuate cell to baseline pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P^
Leave cell isolated for one minute Time
Record time and cell pressure (Pa»»)
Calculate "leak rate" for 1 minute Time
Calculate "leak rate" as percentage of total pressure
%VL»(AP/Pb)« 100
|%VL|shouldbe<4
Record Nitrogen Background
Purge cell with dry nitrogen
Verify ceil is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file.
Record CIS Spectra*
Record Cell path length setting
Fill Cell with CTS gas
Open cell outlet and purge cell with CTS at sampling rate (1 toSLPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration . 29-°
Record and copy spectrum and interferogram to C-drive and back up using CTS batchfile. ty*
Record Barytron pressure during collect
%&eeord iafannaiion an *BaJcyp«id-aaeVmB>aUouj' Jala \\u*\ 9 &
Verify that spectrum and interfere gram were copied to directories.
Record CTS Spectrum File Name , fT?»T«T*
Reviewed by: J\C/<"]A/ " Date:
-------
Proj"1 No 7 '' l<2 , ' MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Stan up Procedure
DATE: 1-8'J-l r.PERATOR: T
Check cell temperatort
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cell, (PJ
>riiaiuu Leak Check Procedure:
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P,^) f 0 '• 3^.VP
Leave cell isolated for one minute Time Pnte
Record time and cell pressure (P^ (0',tf'lO 77?
Calculate "leak rate" for 1 minute Timc Pn»
APaP^-P™, ' . /v?
Calculate "leak rate" as percentage of total pressure
%VL»(AP/Pb)MOO
|%Vt| shouldbe<4 fr %^^o
i i
1
Record Nttrofen Backfround
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book. ^
Copy Background to C-drive and backup using batch file.
Record CTS Spectra
Record Cell path length settmf
16.0"*)
-Rfl Cell with CTS gaa
Open cell oudec and purge cell with CTS at sampling rate (1 toSLPM)
Record cylinder ID Number
Record CTS gas cyUoder identity and concentration
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet.
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
Reviewed by: iflfaf-^ Date:
-------
Project No.
MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATE
OPERATOR:
C
Check ctjtftemperatare
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cad, (P^)
J£MBtifi Leak Check Procedure: ' ^
"''It * ****** ^tibpSgae pressure.
""^olate cell (close cell inlet and cell outlet) 4*
Record time and baseline pressure (P^) jf ;oQ '. 10
Leave cell isolated for one minute Time ».
Record time and cell pressure (P^ ^^ Al'.^'.^Q
Calculate "leak rate" for 1 mimu« Time
Calculate "leak rate" as percentage of total pressure
%VL = (AP/Pb)«100
|%VL|shouldbe<4
Record NhrotenBcckcroond
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background IAQBK) under continuous flow and ambient pressure
Record information in data book,
Copy Background to C-drive and backup using batch file.
Record CTS Spectrum
Record Cell path length setting
Fill Cell with CTS gaa
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet.
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
Reviewed by:
Date:
-------
^ject No. ^1*1 -i* J '"? MIDWEST RESEARCH DNSTITUTE
DAILY CHECKLIST
Stan up Procedure
DATE " ' " ' OPERATOR:
Check cefl tempentara
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cell, (PJ
; Check Procedure:
|$acuate cell to baseune pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P^J ?'. $*•"» ° 77^/"*
Leave cell isolated for one minute Time P^
Record time and cell pressure (P^ &',&'> 1° Tl'f.O
Calculate "leak rate" for 1 minute Time POM
* "am ' "aw* 0.10
Calculate "leak rate" as percentage of total pressure ^p
%VL-(AP/Pb)«lOO ^Y \
|%VL|shouldbe<4 '% VL
Record Nitrogen Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate) i,l
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file. _
RecordCTS!
Record Cell path length setting
•EuacdaleCett
Fill Cell with CTS ga» <*lb
Open cell outlet andpurp cell with CTS at sampling rate (I toSLPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and inlerferognm to C-drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
Reviewed by: ^•HCQ*. Datec
-------
Project No /aeaateCeU
Fill Cell widiCTS ga*
Open cell outlet and purge cell with CTS at sampling rate (1 toSLPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferognm to C-drive and back up using CTS batch file. ji**
Record Barytron pressure during collect
Record information on "Background and Calibration*" data sheet
Verify that spectrum and interferognm were copied to directories.
Record CTS Spectrum File Name
Reviewed by: jjL-J/Sj • Date: __f U/«
v fi y '
-------
Project No.
/*• l"?
MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATE
OPERATOR: 7".
Check cell temperature
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cell, (P»)
Vacuum Leak Check Procedure: v
n^ Evacuate cell to baseline pressure. '*"*
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P^
Leave cell isolated for one minute
Record time and cell pressure (?„„)
Calculate "leak rate" for t minute
P.*
7-7 V.S
Time
Calculate "leak rate" as percentage of total pressure
. %VL»(AP/Pk)MOO
|% VL| shouldbe<4
l.o
Record NUrof en Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file.
Record CTS Spectra**
Record Cell pern length setting
tf
Fill Cell with CTS gas
Open cell oudet and purge cell with CTS at sampling rate (1 toSLPM)
Record cylinder ID Number
Record CTS gat cylinder ideality and concentration
Record and copy spectrum and interferogram to C -drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify th«t spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
ty_
ALUifltf
___ys_
jrKjltfrt
Reviewed by:
Date:
7
-------
Pr°Ject No Si^M' '^ , >:gZ: Vp
Leave cell isolated for one minute T™* POM
Record time and cell pressure (P^)
-------
PROJECT NO. 4951-12 and 13
FTIR DATA FORM
Background and Calibration Spectra
DA ROMETRIC: 7V?.
SITE: NCO Laboratory
TIME
10 /Y-)
,,:V7
*,,'
-i3^r>t—
U<>-
FILE
NAME
r3K&07
-------
PROJECT NO. 4951-12 and 13
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC:
SITE: NCO Laboratory DATE: /7 'git*)
TIME
10:10
«:«
A.,*
/*:*"
FILE
NAME
6K&0TBSA
CT^o"7°8 rt
&K&oflifoft
Cf$ &lo%k
'
(Dtol)
PATH
«.o,
,...,
/0.03
,a^
NOTES
A/, VZi^^ ce& & o-tvifi
^0.0 ^p«< &£*-<•** (O 0.10 Lfa
fj & O.So LAq
°£**^- K<~>
fto.o fp*.
NUMBER
SCANS
^0
f*0
, &
fco
•
Resolulloa
(cm-l)
/. 0
'.O
1.0
1.0
OPERATOR:
Get
^V.o
»»
u^n.
,w
Gas
PRESSURE
7*.-*
-,».-,
7V,. ,
*«•
'• ^o-«c-tr~
'
BKG
—
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—
%r*
cmc_b«ekVy99vt95l\12v«efiN(tii thli iheeU foi referencej.xli Reviewed b)
07-07-99 Dan
APOD
~/~,
«
«»A
^,
i
' *^-V
B 1/tl'f
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
DATE:
BAROMETRIC:
OPERATOR:
TIME
FILE
NAME
(DUI)
fATH
NOTES
NUMBER
SCANS
Re*olulloo
(cm-l)
Gu
TEMP(F)
Gai
PRESSURE
BKG
APOD
(.0
fcxe
'-0
. 3
'. 0
4
IT-
to.
9*
t.O
n
5*°
!.£>
it
AfMl
1,0
0
/. 10
l.o
emc_back\fy99vt9SI\l2\refs\flirdauihecuforrererences.xli
0707-99
Reviewed by
Due
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC:
DATE:
OPERATOR: f
TIME
FILE
NAME
(DUI)
PATH
NOTES
NUMBER
SCANS
Resolution
(cm-1)
Gu
TEMP(F)
Gas
PRESSURE
BKG
APOD
( i
l.o
•;»-*
C.
/. o
75V.'
1.0*
l.o
-70
cn
-------
PROJECT NO. 4951-12 and 13
FT1R DATA FORM
Background and Calibration Spectra
BAROMETRIC:
SITE: NCO Laboratory DATE: I/1*/*?
TIME
«;v.
,.,#-
tr.to
,2!*o
<*'.«
WMO
H:*
FILE
NAME
8K60 7(2 A
£-l\o7i*A
CT$O*1lx&
11 & 0113 A
*»^,
CTJO7I2.£-
/ 1(f rftn 6
(DUI)
PATH
,~,
*..«•»
• O.O-IT
,..»^
io.o~v
I0./) ">
,..M
NOTES
/t?z ty£**tjA, fe^S @ tt>2 (-fi*l
%».» ff**- f*&jUi~ M.' xt'j.
tZiZZZf™
£) ^_ A A « .^tf >l*
r^* Ol ™ T ^ T» ^*
yft-^Vfr f»>
/Oj ^* /«/"7 J-P^i
Jto»& MX**1- <^W|'«->— • /9
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NUMBER
SCANS
5T.O
jToo
r-
^> .
~
S-
roo
•
RCMlultOD
(cml)
/.O
AO
/. 0
Ao
f-o
l.o
<-o
OPERATOR:
GM
TEMP(F)
«..,
;«.«,
.».»
/«./
^./
,».?
».«
.
CM
PRESSURE
7S&. 3
7«.,
T5">"' ^
75^'?
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w.<
7T <£«*»«*-
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—
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-
^
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-
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'«
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:mc_b«kNfy99vl95l\l?*ef»\flirdiu theeu forreferences.xls Reviewed by J
07-07.9Q Due ?/'*/'
-------
FTIR DATA FORM
Background and Calibration Spectra
PROJECT NO. 4951-12 Md 13
SITE: NCO Laboratory DATE:
TIME
i
I2\ff
lav*
1*5
,t»
j^',^,0
FILE
NAME
*.>„„.
CT«,«
,„„,„
0K£0 7//0
^,,
*««
,
(DM)
PATH
,~>
„..>
/-,
IW>
W-*"*
,.^
NOTES
A>p M*»^u f*eP(S ,.o*t.f*\
flLMfaf >f y
^*-^^.-s
/Oi.Q_ I-*O LPs\
' | ^^J
M^Ctl^
BAROMETRIC: 7-"- " ^
7/^A?
NUMRER
SCANS
*-
^
i*0
*<*
ff-
$<*
"ST
• . 0
r.«
1. O
/,*
1.0
(.0
OPERATOR:
GM
TEMP(F)
»,s
,*!.*
IfS ,a
,»5-.,
/«.
£%
Gm
PRESSURE
7i"7. /
7r7-/
,«.
7*6.4
7".«
-,^
T.&ty^-
•KG
-
/,
/f
—
7/5-0-
7«»
;mc_b»d(\fy99v«95 1M ZWMftir
-------
PROJECT NO. 4951-12 «nd 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC:
DATE:
OPERATOR:
TIME
FILE
NAME
(DM)
fATH
NOTES
NUMIEK
SCANS
Rc^altoa
Gm
GM
PRESSURE
•KG
APOD
ii •. » r
gk6oi '<• A
Q
1.0
l.»o if A
1.0
7/4 /f
ft.oii.fAi
7/U
I.O
emc_badMy9?495l\lZVefMtir (fate ihceu for refennoei.xlt
07-07-99
Reviewed by
/
_#/W 7
-------
Project No. 1"^>< ''Z ,'. MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
DATE 7-q^e, OPERATOR:
.
Initials
Reference Spectrum Sample
Start Time LJL&+' eJbit I /sl^
Record Cell path length setting I0 t •*,
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate l.oo
Allow to equilibrate for 5 minutes
Record sample pressure in cell 7f).
Record sample flow rate through cell _
Start spectrum collect program. _
Record information in data book _
Copy Spectrum and Interferogiain to backup directories _
End Time
Reviewed by: ~{Afj»A*-^ Date:
-------
Project No. —c/?// -/'7-,l(^ MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checldist
DATE: 7*V91 OPERATOR:
Initials
Reference Spectrum Sample
Stan Time /5'.X*
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LFM Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
B«^«u,M hy (j/| & "T^ . Dat*
-------
Pr°Ject No 1———i ' ,. MIDWEST RESEARCH INSTITUTE
MIX Reference Spectrum Checklist
DATE: fr/1-lq OPERATOR:
Initials
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name ^ eni 4 A . c
Record Compound Name - - '
Record Cylinder Identification Number
Record Cylinder Concentration j"0.f ttr*
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate I.QO
Allow to equilibrate for 5 minutes &fa
Record sample pressure in cell _
Record sample flow rate through cell jo*
^^^^^^^^T
Start spectrum collect program
Record information in data book __
Copy Spectrum and Interferogram to backup directories __
End Time ,
Reviewed by: V\V*f^ Date:
Jlf
-------
No
MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
DATE:
OPERATOR:
Reference Spectrum Sample
Sun Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes C/v# ++*V It**. AT
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Tune
Initials
. f a c
Q
Reviewed by:
Date: -1/IiM
-------
Project No. ^?''1 V— MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checldist
DATE: 1'a, i'i OPERATOR:
Initials
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number /)*«•
Record Cylinder Concentration M^,
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate i.jtf it*
Allow to equilibrate for 5 """"**« £,
Record sample pressure in cell _
Record sample flow rate through cell _
Start spectrum collect program _
Record information in data book _
Copy Spectrum and Interferogram to backup directories _
End Time _
Reviewed by: Pf \^^/^^ Date:
-------
Project No. l1"M "<
-------
froj60' No- 11 * 1 x 'a ( '^ MIDWEST RESEARCH INSTITUTE
rTIK Reference Spectrum Checklist
DATE_2lili™ OPERATOR:
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LFM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record Information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Initials
p«ii«—rfky V \(a-u^-^' . Data
-------
Pr°J«ct No ^P' '*" )^ MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
DATE: "Ml*m OPERATOR:
Reference Spectrum Sample
Start Time
Record Cell path length setting \0-o~h
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LFM. Record flow rate
Allow to equilibrate for 5 minutes (^&»*ut9 ^v" *
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Initials
Reviewed hv " \ l£j. ^^—- Date:
-------
N°- 2 - MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE:
OPERATOR:
Initial*
Reference Spectrum Sample
StartTime
Record Cell path length setting /«.»•)
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration 5a.a
Record Spectrum File Name • j/H Pol/"*^
Fill cell to ambient pressure with gas from cylinder standard
Open ceil outlet vent valve
Adjust sample flow through cell to O.S to I LPM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by y / L/^ ^^" Date:
-------
froj*501 NO Hi- L!_ MIDWEST RESEARCH INSTITUTE
FTIK Reference Spectrum Checklist
DATE
OPERATOR:
Initials
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM Record flow rate
Allow to equilibrate for 5 minutes d^glt**-****' »"• n
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by:
-------
fr^60' No M^?(- I* (i? _ MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE: -l/ttfll OPERATOR:
Initials
Reference Spectrum Sample
Start Time (.
Record Cell path length setting
Record Background Spectrum File Name
Record CIS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record How rate
Allow to equilibrate for 5 ™j«"tM
Record sample pressure in cell
Record sample flow rate through cell
Stan spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by: dub*/*— Date:
-------
Project No.
DATE:
MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
OPERATOR:
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
_(•*>( 0
Reviewed by:.
Date:.
-------
No
MIDWEST RESEARCH INSTITUTE
HLK Reference Spectrum Checklist
DATE:
l[\*\«\«\
OPERATOR: ^<£<
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Nam*
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 """"««
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Initial*
A-
/*/•• **
'0.0"*
j%
-------
Prcj"" No. '•HE/-!'*- j^ MIDWEST RESEARCH INSTITUTE
. Reference Spectrum Checklist
DATE:
OPERATOR. "fi 6 «*i tf~~
- Initials
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Stan spectrum collect program
Record information in data book j\ tf
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by. 3fM *\(s^/ DatK
-------
No ^ ' ' ^
DATE:
MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
OPERATOR: f . 6-*S ^"
Initials
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name -7 /1 ft
Record CIS Spectrum File Name O"' ftlil * ft
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minntfti
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by:
-------
No. 'f ' MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
DATE: ((*p1 OPERATOR: f.
Reviewed by;
Initials
Reference Spectrum Sample 7 -
Start Time ,?;ot
Record Cell path length setting IO ,0 «,
Record Background Spectrum File Name 2KJaO~lla A
RecordCTS Spectrum file Name
Record Compound Name ,
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name ?
-------
Proi6" No. H > '' | ' MIDWESJ RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
OPERATOR, -r. 6oi /t**.
Record Spectrum Fde Name ,24<167/fc 0
Fill cell to ambient pressure with gas from cylinder standard
-------
Project No MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE' OPERATOR:
Initials
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Stan spectrum collect program
Record information in data book
Opy Spectrum and Interferogram to backup directories
End Time
Reviewed by: Date:.
-------
Project No. U ^Ht I*1?
t^_ MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE: 7 'UM1 OPERATOR:
Initials
Reference Spectrum Sample 7->*.*< u« -| - /*
-------
froj*" N°. 'if? I ' I"* , '^ MIDWEST RESEARCH INSTITUTE
Kl'lK Reference Spectrum Checklist
DATE
1.1 OPERATOR: f~- 6»<
Initials
Reference Spectrum Sample
Start Time
Record Cell path length setting
•y/u*
Record Background Spectrum File Name CTTTiVA
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by ; Date:
-------
No "'^ '|Vjl MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE -7tU (19 OPERATOR:
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name
Initials
Record CTS Spectrum Rle Name ^ c,nuM
Record Compound Name . y/
Record Cylinder Identification Number AfoLZ \ >yT
Record Cylinder Concentration 'f^.^l t»*
Record Spectrum File Name VatoTH, ft
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LPM. Record flow rate 0.1*7
Allow to equilibrate for 5 minutes Sfo
Record sample pressure in cell
Record sample flow rate through cell O.qf
Start spectrum collect program
Record information in data book T,|
-------
: No. 13M '—^ _ MIDWEST RESEARCH INSTITUTE
rTIK Reference Spectrum Checklist
DATE l||u|l«> OPERATOR:
Initials
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name
RecordCTS Spectrum Rle Name tTy.->«.
Record Compound Name —
Record Cylinder Identification Number AAv
Record Cylinder Concentration H^.
Record Spectrum File Name
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to 1 LFM. Record flow rate
Allow to equilibrate for 5 minutes
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
EndTime
ffi
»(
Reviewed by. Date:.
-------
PROJECT NO. 4951-12 and 13
FTIR DATA FORM
Sampling Data
BAROMETRIC:
SITE: NCO Laboratory DATE:
Time
,<-.*<
,*,*.
File
Name
MfeM«
&
i
(DM)
Path
,...>
,..^
NOTES
^p i 0 i,f*\
ML PIO *i&o*$2—
Af /*' M ( pi *-
7/1/11
Scans
*<*>
Soo
ResolulloB
. (ca-I)
...
(.0
\
OPERATOR: / « <*-7*<-
Gu
Temp(*C)
^A
I3C...
Flow
Rate
,.».,*
'.e,^ if*
Gu
Pressure
™*
,s,.,'
BKG
-i
7»
-------
PROJECT NO. 4951-12 and 13
FTIR DATA FORM
Sampling Data
BAROMETRIC:
SITE: NCO Laboratory DATE:
Time
ir,f
*-.»*
»:»>
,t>.
cmc back\
07-07-99
File
Name
\Pi01fZA
V Ptofi*^
fkfOll*-^
(-H/Vll^
I
(Dial)
Path
,.«
,.,,
«»
JO.*"*?
NOTES
""^K
«..•„- ,-fc^.
^^•^'V
<-
«-
f*>
ReMlulloo
, (cm-l)
(.0
l.o
I."
,.o
t
OPERATOR: 7^ <^i7*/~
Gat
Trap CO
,*.
.*.,
• Zfc.*
.*.^
Flow
Rate
A.U*
;^,t*»
/.«t/.
/.«»O t^Al
S
Gat
Pressure
w*
75f. 6
,«.*
1S,.
fy99V»95 l\12Vref »Miir dau iheeu for referencei.xli Reviev
•KG
*
&
•
*
«
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Sampling Data
DATE:
BAROMETRIC:
OPERATOR: '
Time
File
Name
(DM)
fatfc
NOTES
Scan*
RejolulloB
. (cm-1)
Gas
Temp CO
Flow
Rate
Gas
Preourc
•KG
1.0
i ->
h .
emc_bmck^y99vt95l\l^ref^lhrdau ihecu foe referencei «l»
0701-99
Reviewed by
Due -r/t
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Sampling Data
DATE:
BAROMETRIC.
OPERATOR:
Time
Flic
Name
(DM)
Pilb
NOTiS
Scans
Reiolulloo
. (cm-l)
Gu
Temp (*C)
Flow
Rile
G«J
Pressure
•KG
/-o
• o.o-^
l.o
t.O
-i St.
l-t; ft
• O.e'V
(.0
i.o
\2H.Q
(.0
cmc b«ck\fy99v!95l\12Vcfi\fiir dau iheeu for icfrrencrj xlj
07-07-99
Reviewed by
Dale.
-------
FTIR DATA FORM
Sampling Data
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
DATE:
BAROMETRIC:
OPERATOR:
Time
File
Name
(DM)
Path
NOTES
SCUM
Reiolulton
. (cm-1)
GM
Temp CO
Flow
Rale
Ga*
Pressure
BKG
to.o
'3 -
f<7(;
/.O
*<*>
l.o
* f
(.0
12?.
-if (.A
i .O
0*1
<>•**
7/fc/l
l.o
•25. -
emcJudtfy99vl95l\IZ\rcfi\AirdaUiheeU for reference! ilj
0707-99
Reviewed by
Dale " ?//<«/11
-------
No '•Hi'!'11 ) v MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE: 1-1-1°! OPERATOR: *f.
Initials
Purge sample from cell using ambient air or nitrogen
Record Nitrojen Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file.
Record CTS Spectrum
Evacuate Cell
Fill Cell with CTS gas.
Open cell outlet and purge cell with CTS at sampling rate (I to 5 LPM) ^____^
Record cylinder ID Number _________
Record CTS gas cylinder identity and concentration ________
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file. _________
Record Barytron pressure during collect _______
Record information on " Background and Calibrations" data sheet _______
Verify that spectrum and interferogram were copied to directories. _________
Record CTS Spectrum File Name eVTV?*") «•-
Close cylinder*
Evacuate or Purg« CTS from call uring nitrogen
Leave cell uadcr low nitrogen purge or under vacuum
Fill MCT detector dew«r
Reviewed by: f* \^\~^ DtiK
-------
Project No.
MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE:
OPERATOR:
Purge sample from cell using ambient air or nitrogen
Record Nitrof en Backfround
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file.
Record CTS Spectrum
Fill Cell with CTS gas
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Na
Close cylinders
Evacuate or Purge CTS from cell using nitrogen
Leave cell under low nitrogen purge or under vacuum
Fill MCTdettctordewv
Reviewed by:
Date:.
Initials
75-1.0
-------
ProJ60' No -— MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATRJl^VI OPERATOR.
Initials
Purge sample from cell using ambient air or nitrogen
Record Nitrof en Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background jt/.
Record ambient pressure using ceil Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C -drive and backup using batch file.
Record CTS Spectrum
Fill Cell with CTS gas
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM)
Record cylinder ED Number
Record CTS gas cylinder identity and concentration )K * te /•&. %C**t. 30
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file. *
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
Close cylinders
Evacuate or Purg» CTS from cell using nitrogen
Leave cell under low nitrogen purge or under vacuum
Fill MCT detector dew
Reviewed by: $/*.»* [ft* **-~ Date:
-------
^J*61No P>r'*-tr> MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE lh*m OPERATOR: T.
Initials
Purge sample from cell using ambient air or nitrogen
Record Nitrogen Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge .
Record nitrogen flow rate (about sampling flow rate) .?
\Jr
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book. fyr '
Copy Background to C-drive and backup using batch file.
Record CT S Spectnm
Fill Cell with CTS gas *j<
Open cell outlet and purge cell with CTS at sampling rate (1 to SLPM) I,to
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferognm to C-drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations' data sheet
Verify that spectrum and interferognm were copied to directories. fj^f
Record CTS Spectrum File Name
Close cylinder*
Evacuate or Purge CTS from cell using nitrogen
Leave cell under low nitrogen purge or under vacuum
Fill MCT detector demr
Reviewed by: V I It*-^^ Da«.
-------
Project No. ._H V I "' i_LL MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE 1pm OPERATOR:
Initial^
Purge sample from cell using ambient air or nitrogen
Record Nltrof en Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge • Q *f)
Record nitrogen flow rate (about sampling flow rate) nib
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C-drive and backup using batch file.
Record CTS Spectrum
^vaCuateCell
Fill Cell with CTS gas
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM) dp p^* *,» •»» i •*.
9 fa-S
Record cylinder ID Number ^ _______
Record GTS gas cylinder identity and concentration
-------
No — V'' l* MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE _Jl1 OPERATOR:
-------
PrcJ661 No 1V' ->1 & MIDWEST RESEARCH INSTITUTE
DAJLY CHECKLIST
Shut Down Procedure
DATE T|u«h^ OPERATOR: "T.6
Initials
Purge sample from cell using ambient air or nitrogen
Record Ntooten Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Barocell gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information in data book.
Copy Background to C -drive and backup using batch file.
Record CTS Spectra*
fill Cell with CTS gas
Open cell outlet and purge cell with CTS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferogram to C -drive and back up using CTS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum File Name
Close cylinders
Evacuate or Purge CTS from cell using nitrogen
Leave cell under low nitrogen purge or under vacuum
Fill MCT detector dewv
Reviewed by: */^V DatK
-------
APPENDIX C
EQUIPMENT CALIBRATION CERTIFICATES
-------
Equipment Description
THC 1 -- JUM Model VE-7
THC 2 -- Ratfisch Model RS-55CA
Data Logger -- Labtech Notebook
Computer -- Winbook 486-100
Printer -- Panasonic Model KXP1180
Cal Gas Dilution System - Environics Model 2020
-------
C-l CALIBRATION GAS CERTIFICATES
-------
Scott Specialty Gases
6141 BASTON ROAD PO BOX 310
Prom: PLUMSTBADVILLB PA 18949-0310
Phon«: 213-766-8861 Fax: 215-766-2070
CERTIFICATE OP ANALYSIS
MIDWEST RESEARCH PROJECT #: 01-89796-005
DAVE ALBURTY, X1S25 PO#: 029872
425 VOLKBR BLVD ITBM #: 01023912 4AL
DATS: 5/13/97
KANSAS CITY MO 64110
CYLINDER *: ALM057730 ANALYTICAL ACCURACY: W- 2%
FILL PRESSURE: 2000 PSIO
BLEND TYPE : CERTIFIED MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT gQMC MQLB3 (MOLSS1
TOLUEHS 120. PPM 121. PPM
AIR BALANCE BALANCE
t^ Vs
\ *
\*
\:
>«.
1&
ANALYST:
GENYA
-------
S£°ttSpe^ty Gases
J>ped
From:
1290 COMBERMERE STREET
TROY v
Phone: 248-5891-2950
C E R T I P I
MIDWEST RESEARCH
MELISSA TUCKER; * 02S075
425 VOLKER SLVD
KANSAS CITY
OF
Fax: 248-589-2.134
ANALYSIS
MO 64110
CYLINDER #: "A7853
FILL PRESSURE: 2000 PSI
BLEND TYPE : CERTIFIED MAS'
ANALYTICAL ACCURACY: "/I"2%
PRODUCT EXPIRATION: 6/03/1997
COKPONENT
SULFUR HBXAFLUORIDE
NITROGEN
:TER GAS
REQUESTED QAS
CQNC MOT.gfl
4.
PPM
BALANCE
ANALYSIS
(MOLB5)
4.01 PPM
BALANCE
CERTIFIED MASTER GAS
ANALYST:
-------
so;—
Scott Specialty Gases
6141 BASTON ROAD PC BOX 310
From: PLDMSTBADVILLB PA 18949-0310
Phox»: 215-766-8861 Pax: 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH PROJECT ft: 01-88514-001
TOM GEYER PO#: 029257
425 VOLXER BLVD ITEM #: 01021951 1AL
DATS: 3/25/97
KANSAS CITY MO 64110
CYLINDER ft: ALM023940 ANALYTICAL ACCURACY: +-1%
FILL PRESSURE: 2000 PSIG
BLEND TYPE : GRAVIMETRIC MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT gQ»C MTlT.gg (MOT.US 1
BTHYLENS 20. PPM 20.01 PPM
NITROGEN BALANCE BALANCE
•t
is
V*
ANALYST:
GENYA
-------
- E : ; s P £ c
. . 4 I •• 998 6399
'.13
UQU1D CARBONIC
CYUNMR OU PH09UCTS
CUSTOM* (MV. | iMOurt. M»T.
mffTMMNO.
Mil
COMCBCnUllON
1. COMMNEHT
AKtt¥BIMUDMIOa&4N
«/ rum ICNIUTIW
M/er/t9
so « Morn* e irww CONC. im ««• s
ft 2«10tO S « C »74S1«4 OOMC. Iff* ppi I
» un mm u v» ntQMisn
UVT CUIHU110NBA7B
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-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf *: 1, Description: AIR , Size: 10000. SCCM , K-factor: 1.0
SERIAL «
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceable
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of £&F ( _ C) and a pressure of 29.92 in.Hg (760Torr)
Set Flow
5 X 500.0 CCM
10 X 1000.0 CCM
20 X 2000.0 CCM
30 X 3000.0 CCM
40 X 4000.0 CCM
50 X 5000.0 CCM
60 X 6000.0 CCM
70 X 7000.0 CCM
80 X 3000.0 CCM
90 X 9000.0 CCM
100X 10000. CCM
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at 16:22:00
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Date:.
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf *: 2, Description: AIR , Size: 10000. SCCM, K-factcr: 1.
SERIAL *
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceabli
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of AtF ( _ C) and a pressure of 29.92 in.Hg ( 760Torw
5
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50
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2000.0 CCM
3000.0 CCM
4000.0 CCM
5000.0 CCM
6000.0 CCM
7000.0 CCM
8000.0 CCM
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-------
ENVIROHICS FLOW CONTROLLER CALIBRATION SHEET
Mf *: 3, Description: AIR , Size: 1000.0 SCCM, K-factor: 1.0
SERIAL *
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Primary Flow Standard Calibration System. This calibration Is referenced to
dry air at a temperature of 3£F ( _ C) and a pressure of 29.92 in.Hg (7.6flTorr)
5
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30
40
50
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70
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100.0
200.0
300.0
400.0
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600.0
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306.67
408.82
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at 17:55:QC
-------
ENVIRONICS FLOW CONTROLLER CALIBRATION SHEET
Mf *: 4, Description: AIR , Size: 100.0 SCCM, K-factor:
SERIAL »
This flow controller was calibrated using a Sierra Cal Bench(TM), a traceabU
Primary Flow Standard Calibration System. This calibration is referenced to
dry air at a temperature of i*F ( _ C) and a pressure of 29.92 in.Hg ( 760Tor«
5 *
10 *
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CCM
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CCM
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5,236 CCM
10.269 CCM
20.434 CCM
30.524 CCM
40.606 CCM
50.S36 CCM
60.583 CCM
70.779 CCM
80.917 CCM
91 .035 CCM
101.12 CCM
Calibration data was last saved on
Friday 03 January 97
at 19:11:00
Verified by:.
* 6
Date :_/
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APPENDIX D
TEST METHODS
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D-l EPA METHOD 320
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1
Appendix A of part 63 is amended by adding, in numerical
order, Methods 320 and 321 to read as follows:
Appendix A to Part 63-Test Methods
*****
TEST METHOD 320
MEASUREMENT OF VAP01 PHASE 01GANIC AND IN01GANIC EMISSIONS
BY EXTRACTIVE FOU1IE1 T1ANSF01M INFRAIED (FTI1) SPECT10SCOPY
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
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2
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
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3
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
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4
may be increased by increasing the cell path length or (to
some extent) using a higher resolution. Both modifications
also cause a corresponding increased absorbance for all
compounds in the sample, and a decrease in the signal
throughput. For this reason the practical lower detection
range (quantitation limit) usually depends on sample
characteristics such as moisture content of the gas, the
presence of other interferants, and losses in the sampling
system.
1.3 Sensitivity. The limit of sensitivity for an optical
configuration and integration time is determined using
appendix D of the Protocol: Minimum Analyte Uncertainty,
(MAU). The MAU depends on the RMSD noise in an analytical
region, and on the absorptivity of the analyte in the same
region.
1.4 Data Quality. Data quality shall be determined by
executing Protocol pre-test procedures in appendices B to H
of the protocol and post-test procedures in appendices I and
J of the protocol.
1.4.1 Measurement objectives shall be established by the
choice of detection limit (DLt) and analytical uncertainty
(AUt) 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
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5
gathered in a pre-test site survey. Spectral interferants
shall be identified using the selected DLt and AUt and band
areas from reference spectra and interferant spectra. The
baseline noise of the system shall be measured in each
analytical region to determine the MAU of the instrument
configuration for each analyte and interferant (MIUt) .
1.4.3 Data quality for the application shall be determined,
in part, by measuring the RMS (root mean square) noise level
in each analytical spectral region (appendix C of the
Protocol). The RMS noise is defined as the RMSD of the
absorbance values in an analytical region from the mean
absorbance value in the region.
1'. 4.4 The MAU is the minimum analyte concentration for
which the AUt can be maintained; if the measured analyte
concentration is less than MAUif then data quality are
unacceptable.
2.0 Summary of Method.
2.1 Principle. References 4 through 7 provide background
material on infrared spectroscopy and quantitative analysis.
A summary is given in this section.
2.1.1 Infrared absorption spectroscopy is performed by
directing an infrared beam through a sample to a detector.
The frequency-dependent infrared absorbance of the sample is
measured by comparing this detector signal (single.beam
spectrum) to a signal obtained without a sample in the beam
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6
path (background).
2.1.2 Most molecules absorb infrared radiation and the
absorbance occurs in a characteristic and reproducible
pattern. The infrared spectrum measures fundamental
molecular properties and a compound can be identified from
its infrared spectrum alone.
2.1.3 Within constraints, there is a linear relationship
between infrared absorption and compound concentration. If
this frequency dependent relationship (absorptivity) is
known (measured), it can be used to determine compound
concentration in a sample mixture.
2.1.4 Absorptivity is measured by preparing, in the
laboratory, standard samples of compounds at known
concentrations and measuring the FTIR "reference spectra" of
these standard samples. These "reference spectra" are then
used in sample analysis: (1) compounds are detected by
matching sample absorbance bands with bands in reference
spectra, and (2) concentrations are measured by comparing
sample band intensities with reference band intensities.
2.1.5 This method is self-validating provided that the
results meet the performance requirement of the QA spike in
sections 8.6.2 and 9.0 of this method, and results from a
previous method validation study support the use of this
method in the application.
2.2 Sampling and Analysis. In extractive sampling a probe
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7
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.
At = atb CL (1)
where:
At = absorbance at a given frequency of the ith sample
component.
3i = absorption coefficient (absorptivity) of the ith
sample component.
b = path length of the cell.
ct = concentration of the ith sample component.
2.2.2 Analyte spiking is used for quality assurance (QA).
In this procedure (section 8.6.2 of this method) an analyte
is spiked into the gas stream at the back end of the sample
probe. Analyte concentrations in the spiked samples are
compared to analyte concentrations in unspiked samples.
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8
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 instrumental test methods is
qualified to install and operate the sampling system. This
includes installing the probe and heated line assembly,
operating the analyte. spike system, and performing moisture
and flow measurements.
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9
3.0 Definitions.
See appendix A of the Protocol for definitions relating
to infrared spectroscopy. Additional definitions are given
in sections 3.1 through 3.29.
3.1 Analyte. A compound that this method is used to
measure. The term "target analyte" is also used. This
method is multi-component and a number of analytes can be
targeted for a test.
3.2 Reference Spectrum. Infrared spectrum of an analyte
prepared under controlled, documented, and reproducible
laboratory conditions according to procedures in section 4.6
of the Protocol. A library of reference spectra is used to
measure analytes in gas samples.
3.3 Standard Spectrum. A spectrum that has been prepared
from a reference spectrum through a (documented)
mathematical operation. A common example is de-resolving of
reference spectra to lower-resolution standard spectra
(Protocol, appendix K to the addendum of this method).
Standard spectra, prepared by approved, and documented,
procedures can be used as reference spectra for analysis.
3.4 Concentration. In this method concentration is
expressed as a molar concentration, in ppm-meters, or in
(ppm-meters)/K, where K is the absolute temperature
(Kelvin). The latter units allow the direct comparison of
concentrations from systems using different optical
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10
configurations or sampling temperatures.
3.5 Interferant. A compound in the sample matrix whose
infrared spectrum overlaps with part of an analyte spectrum.
The most accurate analyte measurements are achieved when
reference spectra of interferants are used in the
quantitative analysis with the analyte reference spectra.
The presence of an interferant can increase the analytical
uncertainty in the measured analyte concentration.
3.6 Gas Cell. A gas containment cell that can be
evacuated. It is equipped with the optical components to
pass the infrared beam through the sample to the detector.
Important cell features include: path length (or range if
variable), temperature range, materials of construction, and
total gas volume.
3.7 Sampling System. Equipment used to extract the sample
from the test location and transport the sample gas to the
FTIR analyzer. This includes sample conditioning systems.
3.8 Sample Analysis. The process of interpreting the
infrared spectra to obtain sample analyte concentrations.
This process is usually automated using a software routine
employing a classical least squares (els), partial least
squares (pis), or K- or P- matrix method.
3.9 One hundred percent line. A double beam transmittance
spectrum obtained by combining_two background single beam
spectra. Ideally, this line is equal to 100 percent
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11
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 df 0.021 to -0.022). Such
deviations indicate a change in the instrument throughput
relative to the background single beam.
3.11 Batch Sampling. A procedure where spectra of
discreet, static samples are collected. The gas cell is
filled with sample and the cell is isolated. The spectrum
is collected. Finally, the cell is evacuated to prepare for
the next sample.
3.12 Continuous Sampling. A procedure where spectra are
collected while sample gas is flowing through the cell at a
measured rate.
3.13 Sampling resolution. The spectral resolution used to
collect sample spectra.
3.14 Truncation. Limiting the number of interferogram data
points by deleting points farthest from the center burst
(zero path difference, ZPD).
3.15 Zero filling. The addition of points to the
interferogram. The position of each added point Is
interpolated from neighboring real data points. Zero
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12
filling adds no information to the interferogram, but
affects line shapes in the absorbance spectrum (and possibly
analytical results).
3.16 Reference CTS. Calibration Transfer Standard spectra
that were collected with reference spectra.
3.17 .CTS Standard. CTS spectrum produced by applying a de-
resolution procedure to a reference CTS.
3.18 Test CTS. CTS spectra collected at the sampling
resolution using the same optical configuration as for
sample spectra. Test spectra help verify the resolution,
temperature and path length of the ETIR system.
3.19 RMSD. Root Mean Square Difference/ defined in EPA
FTIR Protocol, appendix A.
3.20 Sensitivity. The noise-limited compound-dependent
detection limit for the FTIR system configuration. This is
estimated by the MAU. It depends on the RMSD in an
analytical region of a zero absorbance line.
3.21 Quantitation Limit. The lower limit of detection for
the FTIR system configuration in the sample spectra. This
is estimated by mathematically subtracting scaled reference
spectra of analytes and interferences from sample spectra,
then measuring the RMSD in an analytical region of the
subtracted spectrum. Since the noise in subtracted sample
spectra may be much greater than in a zero absorbance
spectrum, the quantitation limit is generally much higher
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13
than the sensitivity. Removing spectral interferences from
the sample or improving the spectral subtraction can lower
the quantitation limit toward' (but not below) the
sensitivity.
3.22 Independent Sample. A unique volume of sample gas;
there is no mixing of gas between two consecutive
independent samples. In continuous sampling two independent
samples are separated by at least 5 cell volumes. The
interval between independent measurements depends on the
cell volume and the sample flow rate (through the cell).
3.23 Measurement. A single spectrum of flue gas contained
in the FTIR cell.
3.24 Run. A run consists of a series of measurements. At
a minimum a run includes 8 independent measurements spaced
over 1 hour.
3.25 Validation. Validation of FTIR measurements is
described in sections 13.0 through 13.4 of this method.
Validation is used to verify the test procedures for
measuring specific analytes at a source. Validation
provides proof that the method works under certain test
conditions.
3.26 Validation Run. A validation run consists of at least
24 measurements of independent samples. Half of the samples
are spiked and half are not spiked. The length of the run
is determined by the interval between independent samples.
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14
3.27 Screening. Screening is used when there is little or
no available information about a source. The purpose of
screening is to determine what analytes are emitted and to
obtain information about important sample characteristics
such as moisture, temperature, and interferences. Screening
results are semi-quantitative (estimated concentrations) or
qualitative (identification only). Various optical and
sampling configurations may be used. Sample conditioning
systems may be evaluated for their effectiveness in removing
interferences. It is unnecessary to perform a complete run
under any set of sampling conditions. Spiking is not
necessary, but spiking can be a useful screening tool for
evaluating the sampling system, especially if a reactive or
soluble analyte is used for the spike.
3.28 Emissions Test. An FTIR emissions test is performed
according specific sampling and analytical procedures.
These procedures, for the target analytes and the source,
are based on previous screening and validation results.
Emission results are quantitative. A QA spike (sections
8.6.2 and 9.2 of this method) is performed under each set of
sampling conditions using a representative analyte. Flow,
gas temperature and diluent data are recorded concurrently
with the FTIR measurements to provide mass emission rates
for detected compounds.
3.29 Surrogate. A surrogate is a compound that is used in
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15
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 arid sampling.
4.1 Analytical Interferences. An analytical interference
is a spectral feature that complicates (in extreme cases may
prevent) the analysis of an analyte. Analytical
interferences are classified as background or spectral
interference.
4.1.1 Background Interference. This results from a change
in throughput relative to the single beam background. It is
corrected by collecting a new background and proceeding with
the test. In severe instances the cause must be identified
and corrected. Potential causes include: (1) deposits on
reflective surfaces or transmitting windows, (2) changes in
detector sensitivity, (3) a change in the infrared source
output, or (4) failure in the instrument electronics. In
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16
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,
COZ interferes with the analysis of the 670 cm'1 benzene
band. However, benzene can also be measured near 3000 cm"1
(with less sensitivity).
4.2 Sampling System Interferences. These prevent analytes
from reaching the instrument. The analyte spike procedure
is designed to measure sampling system interference, if any.
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17
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
-------
18
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 doe^
not constitute endorsement by the Environmental,
Protection Agency.
The equipment and supplies are based on the schematic
of a sampling system shown in Figure 1. Either the batch or
continuous sampling procedures may be used with this
sampling system. Alternative sampling configurations may
also be used, provided that the.data quality objectives are
met as determined in the post-analysis evaluation. Other
equipment or supplies may be necessary, depending on the
design of the sampling system or the specific target
analytes.
6.1 Sampling Probe. Glass, stainless steel, or other
appropriate material of sufficient length and physical
integrity to sustain heating, prevent adsorption of
analytes, and to transport analytes to the infrared gas
cell. Special materials or configurations may be required
in some applications. For instance, high stack sample
temperatures may. require special steel or cooling the probe.
-------
19
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 but-of-stack particulate filter and the FTIR
-------
20
analytical system.
6.7 Mass Flow Meter (MFM). These are used for measuring
analyte spike flow. The MFM shall be calibrated in the range
of 0 to 5 L/min and be accurate to ± 2 percent (or better)
of the flow meter span.
6.8 Gas Regulators. Appropriate for individual gas
standards.
6.9 Polytetrafluoroethane Tubing. Diameter (e.g., 3/8 in.)
and length suitable to connect cylinder regulators to gas
standard manifold.
6.10 Sample Pump. A leak-free pump (e.g., KNF") , with by-
pass valve, capable of producing a sample flow rate of at
least 10 L/min through 100 ft of sample line. If the pump
is positioned upstream of the distribution manifold and FTIR
system, use a heated pump that is constructed from materials
non-reactive to the analytes. If the pump is located
downstream of the FTIR system, the gas cell sample pressure
will be lower than ambient pressure and it must be recorded
at regular intervals.
6.11 Gas Sample Manifold. Secondary manifold to control
sample flow at the inlet to the FTIR manifold. This is
optional, but includes a by-pass vent and heated rotameter.
6.12 Rotameter. A 0 to 20 L/min rotameter. This meter
need not be calibrated.
6.13 FTIR Analytical System. Spectrometer and detector,
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21
capable of measuring the analytes to the chosen detection
limit. The system shall include a personal computer with
compatible software allowing automated collection of
spectra.
6.14 FTIR Cell Pump. Required for the batch sampling
technique, capable of evacuating the FTIR cell volume within
2 minutes. The pumping speed shall allow the operator to
obtain 8 sample spectra in 1 hour.
6.15 Absolute Pressure Gauge. Capable of measuring
pressure from 0 to 1000 mmHg to within ±2.5 mmHg (e.g.,
Baratron") .
6.16 Temperature Gauge. Capable of measuring the cell
temperature to within ± 2°C.
6.17 Sample Conditioning. One option is a condenser
system, which is used for moisture removal. This can be
helpful in the measurement of some analytes. Other sample
conditioning procedures may be devised for the removal of
moisture or other interfering species.
6.17.1 The analyte spike procedure of section 9.2 of this
method, the QA spike procedure of section 8.6.2 of this
method, and the validation procedure of section 13 of this
method demonstrate whether the sample conditioning affects
analyte concentrations. Alternatively, measurements can be
made with two parallel FTIR systems; one measuring
conditioned sample, the other measuring unconditioned
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22
sample.
6.17.2 Another option is sample dilution. The dilution
factor measurement must be documented and accounted for in
the reported concentrations. An alternative to dilution is
to lower the sensitivity of the FTIR system by decreasing
the cell path length, or to use a short-path cell in
conjunction with a long path cell to measure more than one
concentration range.
7.0 Reagents and Standards.
7.1 Analyte(s) and Tracer Gas. Obtain a certified gas
cylinder mixture containing all of the analyte(s) at
concentrations within ± 2 percent of the emission source
levels (expressed in ppm-meter/K). If practical, the
analyte standard cylinder shall also contain the tracer gas
at a concentration which gives a measurable absorbance at a
dilution factor of at least 10:1. Two ppm SF6 is sufficient
for a path length of 22 meters at 250 °F.
7.2 Calibration Transfer Standard(s). Select the
calibration transfer standards (CTS) according to section
4.5 of the FTIR Protocol. Obtain a National Institute of
Standards and Technology (NIST) traceable gravimetric
standard of the CTS (± 2 percent).
7.3 Reference Spectra. Obtain reference spectra for each
analyte, interferant, surrogate, CTS, and tracer. If EPA
reference spectra are not available, use reference spectra
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23
prepared according to procedures in section 4.6 of the EPA
FTIR Protocol. '
8.0 Sampling and Analysis Procedure.
Three types of testing can be performed: (1) screening,
(2) emissions test, and (3) validation. Each is defined in
section 3 of this method. Determine the purpose(s) of the
FTIR test. Test requirements include: (a) AUt, DLt, overall
fractional uncertainty, OFUt, maximum expected concentration
(CMAXJ , and t^, for each, (b) potential interferants, (c)
sampling system factors, e.g., minimum absolute cell
pressure, (PmiB), FTIR cell volume (Vss) , estimated sample
absorption pathlength, Ls', estimated sample pressure, Ps',
Ts', signal integration time (tss) , minimum instrumental
linewidth, MIL, fractional error, and (d) analytical
regions, e.g., m = 1 to M, lower wavenumber position, FLm,
center wavenumber position, FCm, and upper wavenumber
position, FUm, plus interferants, upper wavenumber position
of the CTS absorption band, FFUm, lower wavenumber position
of the CTS absorption band, FFLm, wavenumber range FNU to
FNL. If necessary, sample and acquire an initial spectrum.
From analysis of this preliminary spectrum determine a
suitable operational path length. Set up the sampling train
as shown in Figure 1 or use an appropriate alternative
configuration. Sections 8.1 through 8.11 of this method
provide guidance pn pre-test calculations in the EPA
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24
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 (AUt) for
each analyte (labeled from 1 to i). Estimate, if possible,
the maximum expected concentration for each analyte, CMAXt.
The expected measurement range Ls fixed by DLt and CMAXi for
each analyte (i).
8.1.2 Potential Interferants. List the potential
interferants. This usually includes water vapor and C02,
but may also include some analytes and other compounds.
8.1.3. Optical Configuration. Choose an optical
configuration that can measure all of the analytes within
the absorbance range of .01 to 1.0 (this may require more
than one path length). Use Protocol sections 4.3 to 4.8 for
guidance in choosing a configuration and measuring CTS.
8.1.4. Fractional Reproducibility Uncertainty (FRUJ . The
FRU is determined for each analyte by comparing CTS spectra
taken before and after the reference spectra were measured.
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25
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 FRO 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
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26
if their presence (even if transient) in the samples is
considered possible. The program output shall be in ppm (or
ppb) and shall be corrected for differences between the
reference path length, LR, temperature, TR, and pressure, PR,
and the conditions used for collecting the sample spectra.
If sampling is performed at ambient pressure, then any
pressure correction is usually small relative to corrections
for path length and temperature, and may be neglected.
8.2 Leak-check.
8.2.1 Sampling System. A typical FTIR extractive sampling
train is shown in Figure 1. Leak check from the probe tip
to pump outlet as follows: Connect a 0- to 250-mL/min rate
meter (rotameter or bubble meter) to the outlet of the pump.
Close off the inlet to the probe, and record the leak rate.
The leak rate shall be * 200 mL/min.
8.2.2 Analytical System Leak check. Leak check the FTIR
cell under vacuum and under pressure (greater than ambient).
Leak check connecting tubing and inlet manifold under
pressure.
8.2.2.1 For the evacuated sample technique, close the valve
to the FTIR cell, and evacuate the absorption cell to the
minimum absolute pressure Pmin. Close the valve to the pump,
and determine the change in pressure APV after 2 minutes.
8.2.2.2 For both the evacuated sample and purgihg
techniques, pressurize the system to about 100 mmHg above
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27
atmospheric pressure. Isolate the pump and determine the
change in pressure APP after 2 minutes.
8.2.2.3 Measure the barometric pressure, Pb in mmHg.
8.2.2.4 Determine the percent leak volume %VL for the
signal integration time tss and for APmax, i.e., the larger of
APV or APP, as follows:
AP
rss
where 50 =» 100% divided by the leak-check time of 2 minutes.
8.2.2.5 Leak volumes in excess of 4 percent of the FTIR
system volume Vss are unacceptable.
8.3 Detector Linearity. Once an optical configuration is
chosen, use one of the procedures of sections 8.3.1 through
8.3.3 to verify that the detector response is linear. If
the detector response is not linear, decrease the aperture,
or attenuate the infrared beam. After a change in the
instrument configuration perform a linearity check until it
is demonstrated that the detector response is linear.
8.3.1 Vary the power incident on the detector by modifying
the aperture setting. Measure the background and CTS at
three instrument aperture settings: (1) at the aperture
setting to be used in the testing, (2) at one half this
aperture and (3) at twice the proposed testing aperture.
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28
Compare the three CTS spectra. CTS band areas shall agree
to within the uncertainty of the cylinder standard and the
RMSD noise in the system. If test aperture is the maximum
aperture, collect CTS spectrum at maximum aperture, then
close the aperture to reduce the IR throughput by half.
Collect a second background and CTS at the smaller aperture
setting and compare the spectra again.
8.3.2 Use neutral density filters to attenuate the infrared
beam. Set up the FTIR system as it will be used in the test
measurements. Collect a CTS spectrum. Use a neutral
density filter to attenuate the infrared beam (either
immediately after the source or the interferometer) to
approximately 1/2 its original intensity. Collect a second
CTS spectrum. Use another filter to attenuate the infrared
beam to approximately 1/4 its original intensity. Collect a
third background and CTS spectrum. Compare the CTS spectra.
CTS band areas shall agree to within the uncertainty of the
cylinder standard and the RMSD noise in the system.
8.3.3 Observe the single beam instrument response in a
frequency region where the detector response is known to be
zero. Verify that the detector response is "flat" and equal
to zero in these regions.
8.4 Data Storage Requirements. All field test spectra
shall be stored on a computer disk and a second backup copy
must stored on a. separate disk. The stored information
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29
includes sample interferograms, processed absorbance
spectra, background interferograms, CIS 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
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30
procedure. Fill a sample tube with distilled water.
Evacuate above the sample and remove dissolved gasses by
alternately freezing and thawing the water while evacuating.
Allow water vapor into the FTIR cell, then dilute to
atmospheric pressure with nitrogen or dry air. If
quantitative water spectra are required, follow the
reference spectrum procedure for neat samples (protocol,
section 4.6). Often, interference spectra need not be
quantitative, but for best results the absorbance must be
comparable to the interference absorbance in the sample
spectra.
8.6 Pre-Test Calibrations
8.6.1 Calibration Transfer Standard. Evacuate the gas cell
to * 5 mmHg absolute pressure, and fill the FTIR cell to
atmospheric pressure with the CTS gas. Alternatively, purge
the cell with 10 cell volumes of CTS gas. (If purge is
used, verify that the CTS concentration in the cell is
stable by collecting two spectra 2 minutes apart as the CTS
gas continues to flow. If the absorbance in the second
spectrum is no greater than in the first, within the
uncertainty of the gas standard, then this can be used as
the CTS spectrum.) Record the spectrum.
8.6.2 QA Spike. This procedure assumes that the method has
been validated for at least some of the target analytes at
the source. For emissions testing perform a QA spike. Use
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31
a certified standard, if possible, of an analyte, which has
been validated at the source. One analyte standard can
serve as a QA surrogate for other analytes which are less
reactive or less soluble than the standard. Perform the
spike procedure of section 9.2 of this method. Record
spectra of at least three independent (section 3.22 of this
method) spiked samples. Calculate the spiked component of
the analyte concentration. If the average spiked
concentration is within 0.7 to 1.3 times the expected
concentration, then proceed with the testing. If
applicable, apply the correction factor from the Method 301
of this appendix validation test (not the result from the QA
spike).
8.7 Sampling. If analyte concentrations vary rapidly with
time, continuous sampling is preferable using the smallest
cell volume, fastest sampling rate and fastest spectra
collection rate possible. Continuous sampling requires the
least operator intervention even without an automated
sampling system. For continuous monitoring at one location
over long periods, Continuous sampling is preferred. Batch
sampling and continuous static sampling are used for
screening and performing test runs of finite duration.
Either technique is preferred for sampling several locations
in a matter of days. Batch sampling gives reasonably good
time resolution and ensures that each spectrum measures a
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32
discreet (and unique) sample volume. Continuous static (and
continuous) sampling provide a very stable background over
long periods. Like batch sampling, continuous static
sampling also ensures that each spectrum measures a unique
sample volume. It is essential that the leak check
procedure under vacuum (section 8.2 of this method) is
passed if the batch sampling procedure is used. It is
essential that the leak check procedure under positive
pressure is passed if the continuous static or continuous
sampling procedures are used. The sampling techniques are
described in sections 8.7.1 through 8.7.2 of this method.
8.7.1 Batch Sampling, Evacuate the absorbance cell to
s 5 mmHg absolute pressure. Fill the cell with exhaust gas
to ambient pressure, isolate the cell, and record the
spectrum. Before taking the next sample, evacuate the cell
until no spectral evidence of sample 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 iategration times shall be sufficient to
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33
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.
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34
8.11.2 Verify that the sampling and instrumental parameters
were appropriate for the conditions encountered. For
example, if the moisture is much greater than anticipated,
it may be necessary to use a shorter path length or dilute
the sample.
8.11.3 Compare the pre- and post-test CIS spectra. The
peak absorbance in pre- and pos.t-test CTS must be ± 5
percent of the mean value. See appendix E of the FTIR
Protocol.
9.0 Quality Control.
Use analyte spiking (sections 8.6.2, 9.2 and 13.0 of
this method) to verify that the sampling system can
transport the analytes from the probe to the FTIR system.
9.1 Spike Materials. Use a certified standard (accurate to
± 2 percent) of the target analyte, if one can be obtained.
If a certified standard cannot be obtained, follow the
procedures in section 4.6.2.2 of the FTIR Protocol.
9.2 Spiking Procedure. QA spiking (section 8.6.2 of this
method) is a calibration procedure used before testing. QA
spiking involves following the spike procedure of sections
9.2.1 through 9.2.3 of this method to obtain at least three
spiked samples. The analyte concentrations in the spiked
samples shall be compared to the expected spike
concentration to verify that the sampling/analytical system
is working properly. Usually, when QA spiking is used, the
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35
method has already been validated at a similar source for
the analyte in question. The QA spike demonstrates that the
validated sampling/analytical conditions are being
duplicated. If the QA spike fails then the
sampling/analytical system shall be repaired before testing
proceeds. The method validation procedure (section 13.0 of
this method) involves a more extensive use of the analyte
spike procedure of sections 9.2.1 through 9.2.3 of this
method. Spectra of at least 12 independent spiked and 12
independent unspiked samples are recorded. The
concentration results are analyzed statistically to
determine if there is a systematic bias in the method for
measuring a particular analyte. If there is a systematic
bias, within the limits allowed by Method 301 of this
appendix, then a correction factor shall be applied to the
analytical results. If the systematic bias is greater than
the allowed limits, this method is not valid and cannot be
used.
9.2.1 Introduce the spike/tracer gas at a constant flow
rate of i 10 percent of the total sample flow, when
possible. (Note: Use the rotameter at the end of the
sampling train to estimate the required spike/tracer gas
flow rate.) Use a flow device, e.g., mass flow meter (± 2
percent), to monitor the spike flow rate. Record- the spike
flow rate every-10 minutes.
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36
9.2.2 Determine the response time (RT) of the system by
continuously collecting spectra of the spiked effluent until
the spectrum of the spiked component is constant for 5
minutes. The RT is the interval from the first measurement
until the spike becomes constant. Wait for twice the
duration of the RT, then collect spectra of two independent
spiked gas samples. Duplicate analyses of the spiked
concentration shall be within 5 percent of the mean of the
two measurements.
9.2.3 Calculate the dilution ratio using the tracer gas as
follows:
DF =
(3)
where:
CS = DF+Spike^ + Unspike(l-DF)
(4)
DF
SF,
S(dir)
SF,
6(splt)
Dilution factor of the spike gas; this value
shall be 210.
SF« (or tracer gas) concentration measured
directly in undiluted spike gas.
Diluted SFS (or tracer gas) concentration
measured in a spiked sample.
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37
sPiJcedlr = Concentration of the analyte in the spike
standard measured by filling the FTIR cell
directly.
CS = Expected concentration of the spiked samples.
Unspike = Native concentration of analytes in unspiked
samples
10.0 Calibration and Standardization.
10.1 Signal-to-Noise Ratio (S/N). The RMSD in the noise
must be less than one tenth of the minimum analyte peak
absorbance in each analytical region. For example if the
minimum peak absorbance is 0.01 at the required DL, then
RMSD measured over the entire analytical region must be
•s 0.001.
10.2 Absorbance Path length. Verify the absorbance path
length by comparing reference CTS spectra to test CTS
spectra. See appendix E of the FTIR Protocol.
10.3 Instrument Resolution. Measure the line width of
appropriate test CTS band(s) to verify instrument
resolution. Alternatively, compare CTS spectra to a
reference CTS spectrum, if available, measured at the
nominal resolution.
10.4 Apodization Function. In transforming the sample
interferograms to absorbance spectra use the same
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38
apodization function that was used in transforming the
reference spectra.
10.5 FTIR Cell Volume. Evacuate the cell to * 5 mmHg.
Measure the initial absolute temperature (Tt) and absolute
pressure (PJ . Connect a wet test meter (or a calibrated
dry gas meter), and slowly draw room air into the cell.
Measure the meter volume (VJ , meter absolute temperature
(TJ , and meter absolute pressure (PJ; and the cell final
absolute temperature (Tf) and absolute pressure (Pt) .
Calculate the FTIR cell volume Vss, including that of the
connecting tubing, as follows:
V -£
m
(5)
11.0 Data Analysis and Calculations.
Analyte concentrations shall be measured using
reference spectra from the EPA FTIR spectral library. When
EPA library spectra are not available, the procedures in
section 4.6 of the Protocol shall be followed to prepare
reference spectra of all the target analytes.
11.1 Spectral De-resolution. Reference spectra can be
converted to lower resolution standard spectra (section 3.3
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39
of this method) by truncating the original reference sample
and background interferograms. Appendix K of the FTIR
Protocol gives specific deresolution procedures. Deresolved
spectra shall be transformed using the same apodization
function and level of zero filling as the sample spectra.
Additionally, pre-test FTIR protocol calculations (e.g.,
FRU, MAU, FCU) shall be performed using the de-resolved
standard spectra.
11.2 Data Analysis. Various analytical programs are
available for relating sample absorbance to a concentration
standard. Calculated concentrations shall be verified by
analyzing residual baselines after mathematically
subtracting scaled reference spectra from the sample
spectra. A full description of the data analysis and
calculations is contained in the FTIR Protocol (sections
4.0, 5.0, 6.0 and appendices). Correct the calculated
concentrations in the sample spectra for differences in
absorption path length and temperature between the reference
and sample spectra using equation 6,
\
IL ilL
where:
Ccorc = Concentration, corrected for path length.
Cc.ic = Concentration, initial calculation (output of the
analytical program designed for the compound).
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40
Lr = Reference spectra path length.
L, = Sample spectra path length.
T3 = Absolute temperature of the sample gas, K.
Tc = Absolute gas temperature of reference spectra, K.
P, - Sample cell pressure.
Pr = Reference spectrum sample pressure.
12.0 Method Performance.
12.1 Spectral Quality. Refer to the FTIR Protocol
appendices for analytical requirements, evaluation of data
quality, and .analysis of uncertainty.
12.2 Sampling QA/QC. The analyte spike procedure of
section 9 of this method, the QA spike of section 8.6.2 of
this method, and the validation procedure of section 13 of
this method are used to evaluate the performance of the
sampling system and to quantify sampling system effects, if
any, on the measured concentrations. This method is self-
validating provided that the results meet the performance
requirement of the QA spike in sections 9.0 and 8.6.2 of
this method and results from a previous method validation
study support the use of this method in the application.
Several factors can contribute to uncertainty in the
measurement of spiked samples. Factors which can be
controlled to provide better accuracy in the spiking
procedure are listed in sections 12.2.1 through 12.2.4 of
this method.
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41
12.2.1 Flow meter. An accurate mass flow meter is accurate
to ± 1 percent of its span. If a flow of 1 L/min is
monitored, with such a MFM, which is calibrated in the range
of 0-5 L/min, the flow measurement has an uncertainty of 5
percent. This may be improved by re-calibrating the meter
at the specific flow rate to be used.
12.2.2' Calibration gas. Usually the calibration standard
is certified to within ± 2 percent. With reactive analytes,
such as HCl, the certified accuracy in a commercially
available standard may be no better than ± 5 percent.
12.2.3 Temperature. Temperature measurements of the cell
shall be quite accurate. If practical, it is preferable to
measure sample temperature directly, by inserting a
thermocouple into the cell chamber instead of monitoring the
cell outer wall temperature.
12.2.4 Pressure. Accuracy depends on the accuracy of the
barometer, but fluctuations in pressure throughout a day may
be as much as 2.5 percent due to.weather variations.
13.0 Method Validation Procedure.
This validation procedure, which is based on EPA Method
301 (40 CFR part 63, appendix A), may be used to validate
this method for the analytes in a gas matrix. Validation at
one source may also apply to another type of source, if it
can be shown that the exhaust gas characteristics are
similar at both -sources.
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13.1 Section 5.3 of Method 301 (40 CFR part 63, appendix
A) , the Analyte Spike procedure, is used with these
modifications. The statistical analysis of the results
follows section 6.3 of EPA Method 301. Section 3 of this
method defines terms that are not defined in Method 301.
13.1.1 The analyte spike is performed dynamically. This
means the spike flow is continuous and constant as spiked
samples are measured.
13.1.2 The spike gas is introduced at the back of the
sample probe.
13.1.3 Spiked effluent is carried through all sampling
components downstream of the probe.
13.1.4 A single FTIR system (or more) may be used to
collect and analyze spectra (not quadruplicate integrated
sampling trains).
13.1.5 All of the validation measurements are performed
sequentially in a single "run" (section 3.26 of this
method).
13.1.6 The measurements analyzed statistically are each
independent (section 3.22 of this method).
13.1.7 A validation data set can consist of more than 12
spiked and 12 unspiked measurements.
13.2 Batch Sampling. The procedure in sections 13.2.1
through 13.2.2 may be used for stable processes. If process
emissions are highly variable, the procedure in section
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43
13.2.3 shall be used.
13.2.1 With a single FTIR instrument and sampling system,
begin by collecting spectra of two unspiked samples.
Introduce the spike flow into the sampling system and allow
10 cell volumes to purge the sampling system and FTIR cell.
Collect spectra of two spiked samples. Turn off the spike
and allow 10 cell volumes of unspiked sample to purge the
FTIR cell. Repeat this procedure until the 24 (or more)
samples are collected.
13.2.2 In batch sampling, collect spectra of 24 distinct
samples. (Each distinct sample consists of filling the cell
to ambient pressure after the cell has been evacuated.)
13.2.3 Alternatively, a separate probe assembly, line, and
sample pump can be used for spiked sample. Verify and
document that sampling conditions are the same in both the
spiked and the unspiked sampling systems. This can be done
by wrapping both sample lines in the same heated bundle.
Keep the same flow rate in both sample lines. Measure
samples in sequence in pairs. After two spiked samples are
measured, evacuate the FTIR cell, and turn the manifold
valve so that spiked sample flows to the FTIR cell. Allow
the connecting line from the manifold to the FTIR cell to
purge thoroughly (the time depends on the line length and
flow rate). Collect a pair of spiked samples. Repeat the
procedure until 'at least 24 measurements are completed.
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44
13.3 Simultaneous Measurements With Two FTIR Systems. If
unspiked effluent concentrations of the target analyte(s)
vary significantly with time, it may be desirable to perform
synchronized measurements of spiked and unspiked sample.
Use two FTIR systems, each with its own cell and sampling
system to perform simultaneous spiked and unspiked
measurements. The optical configurations shall be similar,
if possible. The sampling configurations shall be the same.
One sampling system and FTIR analyzer shall be used to
measure spiked effluent. The other sampling system and FTIR
analyzer shall be used to measure unspiked flue gas. Both
systems shall use the same sampling procedure (i.e., batch
or continuous).
13.3.1 If batch sampling is used, synchronize the cell
evacuation, cell filling, and collection of spectra. Fill
both cells at the same rate (in cell volumes per unit time).
13.3.2 If continuous sampling is used, adjust the sample
flow through each gas cell so that the same number of cell
volumes pass through each cell in a given time (i.e. TCt =
TC,).
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
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45
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 - CS (7)
where:
B = Bias at spike level.
Sm = Mean concentration of the analyte spiked
samples.
CS = Expected concentration of the spiked samples.
13.4.2 Correction Factor. Use section 6.3.2.2 of Method
301 of this appendix to evaluate the statistical
significance of the bias. If it is determined that the bias
is significant, then use section 6.3.3 of Method 301 to
calculate a correction factor (CF). Analytical results of
the test method are multiplied by the correction factor, if
0.7 s CF * 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.
-------
46
14.0 Pollution Prevention.
The extracted sample gas is vented outside the
enclosure containing the FTIR system and gas manifold after
the analysis. In typical method applications the vented
sample volume is a small fraction of the source volumetric
flow and its composition is identical to that emitted from
the source. When analyte spiking is used, spiked pollutants
are vented with the extracted sample gas. Approximately 1.6
x 10*4 to 3.2 x 10*4 Ibs of .a single HAP may be vented to the
atmosphere in a typical validation run of 3 hours. (This
assumes a molar mass of 50 to 100 g, spike rate of 1.0
L/min, and a standard concentration of 100 ppm). Minimize
emissions by keeping the spike flow off when not in use.
15.0 Waste Management.
Small volumes of laboratory gas standards can be vented
through a laboratory hood. Neat samples must be packed and
disposed according to applicable regulations. Surplus
materials may be returned to supplier for disposal.
16.0 References.
1. "Field Validation Test Using Fourier Transform Infrared
(FTIR) Spectrometry To Measure Formaldehyde, Phenol and
Methanol at a Wool Fiberglass Production Facility." Draft.
U.S. Environmental Protection Agency Report, EPA Contract
No. 68D20163, Work Assignment 1-32, September 1994.
2. "FTIR Method Validation at a Coal-Fired Boiler".
-------
47
Prepared for U.S. Environmental Protection Agency, Research
Triangle Park, NC. Publication No.: EPA-454/R95-004, NTIS
No.: PB95-193199. July, 1993.
3. "Method 301 - Field Validation of Pollutant Measurement
Methods from Various Waste Media," 40 CF1 part 63, appendix
A.
4. "Molecular Vibrations; The Theory of Infrared and Raman
Vibrational Spectra," E. Bright Wilson, J. C. Decius, and P.
C. Cross, Dover Publications, Inc., 1980. For a less
intensive treatment of molecular rotational-vibrational
spectra see, for example, "Physical Chemistry," G. M.
Barrow, chapters 12, 13, and 14, McGraw Hill, Inc., 1979.
5. "Fourier Transform Infrared Spectrometry, " Peter R.
Griffiths and James de Haseth, Cheaical 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.
-------
48
Table 1. EXAMPLE PRESENTATION OF SAMPLING DOCUMENTATION.
TlM
Ml*
•ack|r«M4 fil* IMM
fll*
••••l.tlM
CaU
CIS
-------
49
Flow How IB F tow in How
Urtw MMw IhMUr
Swnpte Qa* Dakwy MandoM
Pump 12
Figure 1. Extractive FTIR sampling system.
-------
50
.8-
.6-
0
FRU = SRMS(FU-FL)/BAV
SRMS = .00147
BAV = 3.662
FM = FRU = .086
p-xylene
1050
1000
i i
950 900
Wavenumbers
i
850
800
750
Figure 2. Fractional Reproducibility. Top: average of cts!031a and
ctsllOlb. Bottom: Reference spectrum of p-xylene.
-------
D-2 EPA FTIR PROTOCOL
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Page 1
PROTOCOL FOR THB USB OP EXTRACTIVE POURIBR TRANSFORM
INFRARED (FTIR) SPECTROMBTRY 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 . B 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 AMD 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
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BPA PTIR Protocol
1V •""** _ _ Page 2
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 PTIR 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 7B) are: (1) Computers are necessary to
obtain and analyze data; (2) chemical concentrations can be
quantified using previously recorded infrared reference spectra;
and (3) analytical assumptions and results, including possible
effects of interfering compounds, can be evaluated after the
quantitative analysis. The following general principles and
requirements of this Protocol are based on these characteristics.
3.1 Verifiability and Reproducibility of Results. Store
all data and document data analysis techniques sufficient to
allow an independent agent to reproduce the analytical results
from the raw interferometric data.
3.2 Transfer of Reference Spectra. To determine whether
reference spectra recorded under one set of conditions (e.g.,
optical bench, instrumental linewidth, absorption pathlength,
detector performance, pressure, and temperature) can be used to
analyze sample spectra taken under a different set of conditions,
quantitatively compare "calibration transfer standards" (CTS) and
reference spectra as described in this Protocol. (_____£: 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
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EPA ?TIR Protocol
Page 3
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 AND EVALUATIONS
Before testing, demonstrate the suitability of FTIR
spec trome try 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 (AU^ . The M]i is the
maximum permissible fractional uncertainty of analysis for the
i"1 analyte concentration, expressed as a fraction of the analyte
concentration in the sample.
4.1.3 Required detection limit for each analyte (DL^, ppm) .
The detection limit is the lowest concentration of an analyte for
which its overall fractional uncertainty (OFUj) is required to be
less than its analytical uncertainty limit (AU^ .
4.1.4 Maximum expected concentration of each analyte
(CMAXi( ppm) .
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BPA PTIR Protocol
g<5
4.2 Identify Potential Interf erants . Considering the
chemistry of the process or results of previous Studies, identify
potential interf erants, 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 i through
NJ, where the subscript "j" pertains to potential interf erants .
Estimate the concentrations of these compounds in the effluent
(CPOTj, 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 interf erants or to
protect the sampling and analytical components. Determine the
minimum absolute sample system pressure (P^in' mmHg) and the
infrared absorption cell volume (VSS' !i£er) . 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 (Lg', meter), sample pressure (Pg'/ fcPa) , absolute
sample temperature Tg', and signal integration period (tgg/
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 TO' is less
than one half the smallest value AU^ (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.
Notat It may be necessary to choose preliminary analytical
region* (see Section 4.7), identify the minimum analyte
linewidtha, 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.
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SPA PTIR Protocol _
ge 5
4.5.3 At least one absorption CTS band within the operating
range of the FTIR instrument has an instrument -independent
linewidth no greater than the narrowest analyte absorption band-
perform and document measurements or cite Studies to determine
analyte and CTS compound linewidths.
4.5.4 For each analytical region, specify the upper and
lower wavenumber positions (FFU- and FFL-, respectively) that
bracket the CTS absorption band or bands for the associated
analytical region. Specify the wavenumber range, FNU to FNL,
containing the absorption band that 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 (LR) of
the cell.
4.6.2 Obtain or prepare a set of chemical standards for
each analyte, potential and known spectral interferants, and CTS.
Select the concentrations of the chemical standards to correspond
to the top of the desired range.
4.6.2.1 Commercially -Prepared Chemical Standards. Chemical
standards for many compounds may be obtained from independent
sources, such as a specialty gas manufacturer, chemical company,
or commercial laboratory. These standards (accurate to within
±2 percent) shall be prepared according to EPA Protocol l (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.
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SPA PTIR Protocol
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 (L«) , and interferogram signal integration
period (tSR) . Signal integration periods for the background
inter ferograme shall be *tSR. 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 aa 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 AU4, 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
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SPA PTIR Protocol
>..j..««. i-, iogg Page 7
analytical region (FI^, FC^, and FU respectively) . Specify the
analytes. and interferants which Exhibit absorption in each
region. * e ^"
4.8 Determine Fractional Reproducibility Uncertainties
Using Appendix B, calculate the fractional reproducibility
uncertainty for each analyte (FRU^ from a comparison of {Ri} 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 (PR)] che 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 (Pa) during the actual sample analyses differ from LR,
TR, and P«, 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
according to Appendix F, and compare these values to the
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BPA PTZR Protocol
i"tr-«- ^ ™a* , Page 8
fractional uncertainty limits (AUt; see Section 4 i) if
FCUi > AUi), either the reference spectra or analytical programs
for that analyte are unsuitable. t^uatcua
4.12 Verify System Configuration Suitability. Using
Appendix C, measure or obtain estimates of the noise level
(RMSEST, absorbance) of the FTIR system; alternatively, construct
the complete spectrometer system and determine the values RMSG
using Appendix G. Estimate the minimum measurement uncertainty
for each analyte (MAUj, ppm) and known interferant (MIUV, ppm)
using Appendix D. Verify that (a) MAU^ < (AIM (DL^) , FRUH < AlL,
and FCUi < ta± 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
(LJJ) and leak volume (VL) , where VL - l^ tss. Leak volumes shall
be s4 percent of Vss.
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 Pa and record a set of CTS spectra {R3}. Store the
background and unsealed CTS single beam inter ferograms and
spectra. Using Appendix H, calculate the sample absorption
pathlength (Lg) for each analytical region. The values Lc 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 Pg. 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.
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BPA PTIR Protocol
KfitS: Multiple sample spectra may be recorded according to
the procedures of Section 5.4 before performing Sections 5.5
5.5 Quantify Analyte Concentrations. Calculate the
unsealed analyte concentrations R\JAi and unsealed interferant
concentrations RUIj, 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)/(LsPsTp) . Calculate the final analyte and
interferant concentrations RSAi - RLpsRUAi and RSIk - RLpsRUI)c-
5.6 Determine Fractional Analysis Uncertainty. Pill the
absorption cell with CTS at the pressure Pg. 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 EVALUATIONS
Estimate the overall accuracy of the analyses performed in
Section 5 as follows:
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BPA FTXR Protocol p
Page 10
6.1 Qualitatively Confirm the Assumed Matrix. Examine each
analytical region of the sample spectrum for spectral evidence of
unexpected or unidentified interf erants . If found, identify the
interfering compounds (see Reference C for guidance) and add them
to the list of known interf erants. Repeat the procedures of
Section 4 to include the interf erants in the uncertainty
calculations and analysis procedures. Verify that the MAU and
FCU values do not increase beyond acceptable levels for the
application requirements. Re -calculate the analyte
concentrations (Section 5.5) in the affected analytical regions.
6.2 Quantitatively Evaluate Fractional Model Uncertainty
(FMU) . Perform the procedures of either Section 6.2.1 or 6.2.2:
6.2.1 Using Appendix I, determine the fractional model
error (FMU) for each analyte.
6.2.2 Provide statistically determined uncertainties FMU
for each analyte which are equivalent to two standard deviations
at the 95% confidence level. Such determinations, if employed,
must be based on mathematical examinations of the pertinent
sample spectra (not the reference spectra alone) . Include in the
report of the analysis (see Section 7.0) a complete description
of the determination of the concentration uncertainties.
6.3 Estimate Overall Concentration Uncertainty (OCU) .
Using Appendix J, determine the overall concentration uncertainty
(OCU) for each analyte. If the OCU is larger than the required
accuracy for any analyte, repeat Sections 4 and 6.
7.0 REPORTING REQUIREMENTS
[Documentation pertaining to virtually all tne procedures of
Sections 4, 5, and 6 will be required. Software copies of
reference spectre end saaple spectra will be retained for some
minimum time following the actual testing.]
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BPA PTIR Protocol Parro
eage
8.0 R2FBS2NCSS
A) Standard Practices for General Techniques of Infrared
Quantitative Analysis (American Society for Testing and
Materials, Designation E 168-88) .
B) The Coblentz Society Specifications for Evaluation of
Research Quality Analytical Infrared Reference Spectra
(Class II); Anal. Chemistry il, 945A (1975); Appl.
Sp«ctro«copy 444. pp. 211-215, 1990.
C) Standard Practices for General Techniques for Qualitative
Infrared Analysis, American Society for Testing and
Materials, Designation B 1252-88.
D) "Traceability Protocol for Establishing True Concentrations
of Gases Used for Calibration and Audits of Continuous
Emissions Monitors (Protocol Number 1)," June 1978, Quality
Assurance Handbook for Air Pollution Measurement Systems,
Volume III, Stationary Source Specific Methods, EPA- 600/4-
77-027b, August 1977.
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BPA PTIR Protocol
i..g,..». IA. iQQg ___ Page 12
APPENDIX A
DEFINITIONS OF TERMS AND SYMBOLS
A.I 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.
The quantitative result for a single analyte may be
based on data from more than one analytical region.
apodixation - modification of the IL3 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'* law - the direct proportionality of the absorbance of a
compound in a homogeneous sample to its concentration.
calibration transfer standard (CTS) gas - a gas standard of a
compound used to achieve and/or demonstrate suitable
quantitative agreement between sample spectra and the
reference spectra; see Section 4.5.1.
compound - a substance possessing a distinct, unique molecular
structure.
concentration (c) - the quantity of a compound contained in a
unit quantity of sample. The unit "ppm" (number, or mole,
basis) is recommended.
concentration-ptthlengtn product - the mathematical product of
concentration of the species and absorption pathlength. For
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BPA PTIR Protocol -
13
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- pern" 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.
fact Fourier transform (PPT) - a method of speeding up the
computation of a discrete FT by factoring the data into
sparse matrices containing mostly zeros.
flyback - interferometer motion during which no data are
recorded .
Fourier transform (FT) - the mathematical process for converting
an amplitude -time spectrum to an amplitude -frequency
spectrum, or vice versa.
Fourier transform infrared {FTIR) spectrometer - an analytical
system that employs a source of mid- infrared radiation, an
interferometer, an enclosed sample cell of known absorption
pathlength, an infrared detector, optical elements that
transfer infrared radiation between components, and a
computer system. The time -domain detector response
( interf erogram) is processed by a Fourier transform to yield
a representation of the detector response vs. infrared
frequency.
Note; 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, v - the number of cycles per unit time.
infrared - the portion of the electromagnetic spectrum containing
wavelengths from approximately 0.78 to 800 microns.
interf erogram, I (a) - ' record of the modulated component of the
interference signal measured as a function of retardation by
the detector.
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SPA PTZR Protocol
Page 14
interferometer - device chat 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"1) .
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 -trans formed 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.
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BPA PTIR Protocol _
IA. IPO* _ Page 15
wavenumber, v - the number of waves per unit length.
Hffltfi: The usual unit of wavenumber is the reciprocal
centimeter, on'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.
Performing the FT of a zero- filled interferogram
results in correctly interpolated points in the computed
spectrum.
A. 2 Definition* of Mathematical Symbol*
A, absorbance - the logarithm to the base 10 of the reciprocal of
the transmittance (T) .
(1)
^ - band area of the itn analyte in the mtn analytical
region, at the concentration (CLj) corresponding to the
product of its required detection limit (DL^) and analytical
uncertainty limit (AU^) .
^ • average absorbance of the itn analyte in the mth
analytical region, at the concentration (CLj) corresponding
to the product of its required detection limit (DL^) and
analytical uncertainty limit (AU^) .
ASC, accept •£ standard concentration - the concentration value
assigned to a chemical standard.
ASCPP, accepted standard concentration-pathlength product - for
a chemical standard, the product of the ASC and the sample
absorption pathlength. The units "centimeters-ppm" or
"meters -ppm" are recommended.
AUj, analytical uncertainty limit - the maximum permissible
fractional uncertainty of analysis for the irn analyte
concentration, expressed as a fraction of the analyte
concentration determined in the analysis.
AVTm - average estimated total absorbance in the mtn analytical
region.
fc • estimated concentration of the ktn known interferant.
^ • estimated maximum concentration of the itn analyte.
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SPA PTIR Protocol
CPOTj - 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 (OFm) is required to be less than
the analytical uncertainty limit
- center wavenumber position of the mch analytical region.
, fractional analytical uncertainty - calculated uncertainty
in the measured concentration of the i"1 analyte because of
errors in the mathematical comparison of reference and
sample spectra.
, fractional calibration uncertainty • calculated uncertainty
in the measured concentration of the i"1 analyte because of
errors in Beer's law modeling of the reference spectra
concentrations.
- lower wavenumber jpos it ion of the CTS absorption band
associated with the or" analytical region.
PPUm • upper wavenumber position of the CTS absorption band
associated with the mtn analytical region.
- lower wavenumber position of the mtn analytical region.
, fractional model uncertainty - calculated uncertainty in
the measured concentration of the itn analyte because of
errors in the absorption model employed.
PNL - lower wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands .
PH., - upper wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands.
j, fractional reproducibility uncertainty' - calculated
uncertainty in the measured concentration of the icn analyte
because of errors in the reproducibility of spectra from the
FTIR system.
• upper wavenumber position of the mth analytical region.
., - band area of the jth potential .interferant in the mth
analytical region, at its expected concentration (CPOTj).
IAV4_ • average absorbance of the ith analyte in the mth
analytical region, at its expected concentration (CPOTj).
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KPA PTZR Protocol
•»•*, T»Q* __ _ ; _ . Page 17
Isci or It' in<*icated standard concentration - the concentration
from the computerized analytical program for a ainqle-
compound reference spectrum for the itn analyte or kt^ known
*aiuwu
interf erant .
kPa - kilo-Pascal (see Pascal) .
Lg' - estimated sample absorption pathlength.
I«a • reference absorption pathlength.
Ls - actual sample absorption pathlength.
MAUA - mean of the MAUim over the appropriate analytical regions.
MAU^, minimum analyte uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
(Al^) in the measurement of the it5 analyte, based on
spectral data in the mtn analytical region, can be
maintained.
MIUj • mean of the MIUjm over the appropriate analytical regions.
MXT7ja, minimum interferant uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
CPOTj/20 in the measurement of the jtn interferant, based on
spectral data in the mtn analytical region, can be
maintained.
MIL, minimum instrumental linewidth - the minimum linewidth from
the FTIR system, in wavenumbers.
Note; 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) .
N^ - number of analytes.
NJ - number of potential interf erants .
Nfc - number of known interf erants .
N - the number of scans averaged to obtain an inter ferogram.
OFTJj • the overall fractional uncertainty in an analyte
concentration determined in the analysis
Pascal (Pa) - metric unit of static pressure; equal to one Newton
per square meter; one atmosphere is equal to 101,325 Pa;
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SPA PTIR Protocol
•>* ™«* Page 18
? a)8 herS (°ne T°rr' °r °ne millimeter H9) is equal
to133 322p
pmin / minimum pressure of the sampling system during the
sampling procedure. 3
Pg' - estimated sample pressure.
PR - reference pressure.
Ps - actual sample pressure.
"^Sm " measured noise level of the PTIR system in the mch
analytical region.
RMSD, root mean square difference - a measure of accuracy
determined by the following equation:
RMSD - A /!\ V e,2 (2)
where:
n - the number of observations for which the accuracy is
determined.
e^ - 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 (A^) and the mean of the values" (Ajyj) is
defined as
RMSD
(3)
N
• the (calculated) final concentration of the itn analyte.
, - the (calculated) final concentration of the ktn known
' interferant.
time - time used to acquire a single scan, not
scan*
including flyback.
ts, 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 tgcan, ts - N8cantgcan.
tga - signal integration period used in recording reference
spectra.
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SPA PTIR Protocol
Pa ere
^
tgg • signal integration period used in recording sample spectra.
TR - absolute temperature of gases used in recording reference
spectra.
Tg - 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.
Vgg - volume of the infrared absorption cell, including parts of
attached tubing.
*ik " weight used to average over analytical regions fc for
quantities related to the analyte i; see Appendix D.
Note that some terms are missing, e.g., BAVm, OCU, RMSSm, SUBS,
, Ss
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SPA PTIR Protocol
A.^.-t. -i* ioag Page 20
APPENDIX B
IDENTIFYING SPECTRAL INTERFERANTS
B.I G«n«r«l
B.l.i Assume a fixed absorption pathlength equal to the
vcLXuls Q *
B.I.2 Use band area calculations to compare the relative
absorption strengths of the analytes and potential interferants
In the mcn analytical region (FI^ to FUm), use either rectangular
or trapezoidal approximations to determine the band areas
described below (see Reference A, Sections A.3.1 through A.3.3);
document any baseline corrections applied to the spectra.
B.l.3 Use the average total absorbance of the analytes and
potential interferants in each analytical region to determine
whether the analytical region is suitable for analyte
concentration determinations.
The average absorbance in an analytical region is the
band area divided by the width of the analytical region in
wavenumbers. The average total absorbance in an analytical
region is the sum of the average absorbances of all analytes
and potential interferants.
B.2 Calculation*
B.2.1 Prepare spectral representations of each analyte at
the concentration CLj - (DL^) (AU^) , where DL^ is the required
detection limit and AU* is the maximum permissible analytical
uncertainty. For the mr" analytical region, calculate the band
area (AAI^) and average absorbance (AAVim) from these scaled
analyte spectra.
B.2.2 Prepare spectral representations of each potential
interferant at its expected concentration (CPOTj). For the mcn
analytical region, calculate the band area (UuHm) and average
absorbance (IAVjm) 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., IAI.,_ > 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.
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BSX FTIR Protocol
21
B.2.5 Calculate the average total absorbance (AVT_) 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
. t*lm
Potential Interferant
Labels
IA113L . . . IAI1M
FIGURE B.2 Presentation of Known Interferant Calculations
Analytical Regions
1 .... M
Analyte Labels
. AAI1M
Known Interferant
Labels
1 lAIu
IAIK1 .
Total Average
Absorbance AVT± AVTM
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B9A PTIR Protocol
22
APPENDIX C
ESTIMATING NOISE LEVELS
C.I General
C.l.l 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) RMStguf - the noise level of the system (in absorbance
units) , without the absorption cell and transfer optics,
under those conditions necessary to yield the specified
minimum instrumental linewidth. e.g., Jacquinot " stop
size.
(b) tjflyy - the manufacturer's signal integration time used
todet ermine
tgs - 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^^, tva^, 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 (RMSBST) as
follows:
i
(4)
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BPA ?TIR Protocol _
a..j..-> IA. TOO* __ _____ _ _ _ Pa3e 23
APPENDIX D
ESTIMATING MINIMUM CONCENTRATION MEASUREMENT
UNCERTAINTIES (MAU and MIU)
D.I General
Estimate the minimum concentration measurement uncertainties
for the icn analyte (MAU^ and jtn interferant (MIU..) based on
the spectral data in the mcn analytical region by comparing the
analyte band area in the analytical region (AAIj-) and estimating
or measuring the noise level of the system (RMSEST or RMSSm) .
For a single analytical .region, the MAU or MIU value
is the concentration of the analyte or interferant for which
the band area is equal to the product of the analytical
region width (in wavenumbers) and the noise level of the
system (in absorbance units) . If data from more than one
analytical region is used in the determination of an analyte
concentration, the MAU or MIU is the mean of the separate
MAU or MIU values calculated for each analytical region.
D.2 Calculation*
D.2.1 For each analytical region, set RMS • RMSSm if
measured (Appendix G) , or set RMS - RMSEST if estimated (Appendix
C) .
D.2. 2 For each analyte associated with the analytical
region, calculate
(RMS) (DL, ) (AUt ) <5>
D.2. 3 If only the mth analytical region is used to
calculate the concentration of the itn analyte, set MAUi - MAUim.
D.2. 4 If a number of analytical regions are used to
calculate the concentration of the ith analyte, set MAUj_ equal to
the weighted mean of the appropriate MAUim values calculated
above; the weight for each term in the mean is equal to the
fraction of the total wavenumber range used for the calculation
represented by each analytical region. Mathematically, if the
set of analytical regions employed is {m'}» then the, MAU for each
analytical region is
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SPA FTIR Protocol
Paoa
age
MAU, = £ Wlk MAUik
(6)
where the weight Wi}c is defined for each term in the sum as
(7)
0,2.5 Repeat Sections D.2.1 through D.2.4 to calculate the
analogous values MlUa for the interferants j - l to J. Replace
the value (AU^) (DL/y in the above equations with CPOT../20;
replace the value AAI^ in the above equations with IAIjm.
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BPA PTIB Protocol
25
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
sli' i-1' N- Similarly, the CTS spectra {R2} consist of N
spectra, denoted by S2i, i-1, N. Each Ski is the spectrum of a
single compound, where i denotes the compound and k denotes
the set {Rk} of which SIH is a member. Form the spectra S
according to S3i - S2i-S1J for each i. Form the spectra S4
according to S4^ - [S2i+SliI/2 for each i.
E.2.2 Each analytical region m is associated with a portion
of the CTS spectra Sjj and S**, for a particular i, with lower
and upper wavenumber limits FFI^ and FFUm, respectively.
E.2.3 For each m and the associated i, calculate the band
area of S4j_ in the wavenumber range FFU,_ to FFI^. Follow the
guidelines of Section B.I. 2 for this band area calculation.
Denote the result by BAVm.
E.2.4 For each m and the associated i, calculate the RMSD
of S3i between the absorbance values and their mean in the
wavenumber range FFUm to FFL^. Denote the result by SRMSm.
E.2.5 For each analytical region m, calculate the quantity
- SRMSm(FFUm-FFLm)/BAVm
E.2.6 If only the mth analytical region is used to
calculate the concentration of the itn analyte, set
B.2. 7 If a number pA of analytical regions are used to
calculate the concentration of the ic" analyte, set FRl^ equal to
the weighted mean of the appropriate FM_ values calculated above.
Mathematically, if the set of analytical regions employed is
{m' } , then
Wlk FMk (8)
where the Wi]c are calculated as described in Appendix D.
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BPA PTIR Protocol
*"triii- •>*, •">afi _ ; ___ . Page 26
APPENDIX F
DETERMINING FRACTIONAL CALIBRATION UNCERTAINTIES (PCU)
P . 1 6«n«r«l
P.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 f rom , 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) .
P . 2 Calculations
F.2.1 Apply each analytical program to each reference
spectrum. Prepare a similar table as that in Figure F.l 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 interferant s) .
F.2.3 For each analyte reference spectrum, calculate the
quantity (ASC- ISC) /ASC. For each analyte, calculate the mean of
these values (the FCU^ for the icn analyte) over all reference
spectra. Prepare a similar table as that in Figure F.2 to
present the FO^ and analytical uncertainty limit (AU^ for each
analyte .
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BPA ?TIR Protocol
Page 27
FIGURE F.I
Presentation of Accepted Standard Concentrations (ASC's)
and Indicated Standard Concentrations (ISC's)
f*jUM«uuimt
:: \«VUI|WUIK*
Name
i: Reference
!•' SpectmiB .
FiteNamc
ASG
Qjpm)
Aoalytes
i*l
i-
ISC (ppm)
. -:^ >:, fo
]
*!.. .......
teifenu
I
i
its
FIGURE F.2
Presentation of Fractional Calibration Uncertainties (FCU's)
and Analytical Uncertainties (AU's)
Analyte
f.-- Name^
FCU
(%>
AU
(%>;
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SPA FTIR PrOtOCOl Oarra
age
APPENDIX G
MEASURING NOISE LEVELS
0.1 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) .
0.2 Calculation*
G.2.1 Evacuate the absorption cell or fill it with UPC
grade nitrogen at approximately one atmosphere total pressure.
G.2.2 Record two single beam spectra of signal integration
period tss.
G.2.3 Form the double beam absorption spectrum from these
two single beam spectra, and calculate the noise level RMS^ in
the M analytical regions.
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SPA PTIR Protocol _
29
APPENDIX H
DETERMINING SAMPLE ABSORPTION PATHLENGTH (Lc) AND
FRACTIONAL ANALYTICAL UNCERTAINTY (FAUJ
B.I General
Reference spectra recorded at absorption pathlength (Lp)
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 (Pg) . 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.l.l 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 Ls and LR, and Ts and TR, but both
at PR.
H.l. 2 Determine the fractional analysis uncertainty (FAU)
for each analyte by comparing a scaled CTS spectral set, recorded
at Ls, Ts, and PC, 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 Ag containing the absorbance values from all
segments of {Rl} that are associated with the analytical regions;
the members of the array are ARj, i - l, n. Form a similar one-
dimensional array Ag from the absorbance values in the spectral
set {R3}; the members of the array are A^, i - 1, n. Based on
the model AC - rAR + B, determine the least -squares estimate of
r' , the value or r which minimizes the square error E*.
Calculate the sample absorption pathlength Ls - r'(Ts/TR)LR.
H.2. 2 Fractional Analysis Uncertainty. Perform and
document separate linear baseline corrections to each analytical
region in the spectral sets {Rl} and {R4}. Form the arrays Ag
and Ap as described in Section H.2.1, using values from {Rl} to
form AR, and values from {R4} to form Ag . Calculate the values
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SPA PTXR Protocol
Page 30
NRMS,
(9)
and
IA«, - 4
(10)
The fractional analytical uncertainty is defined as
FAO
IA
1AV
(11)
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BPA FTIR Protocol «- ,,
31
APPENDIX I
DETERMINING FRACTIONAL MODEL UNCERTAINTIES (FMU)
I.I General
To prepare analytical programs for FTIR analyses, the sample
constituents must first be assumed; the calculations in this
appendix, based upon a simulation of the sample spectrum, verify
the appropriateness of these assumptions. The simulated spectra
consist of the sum of single compound reference spectra scaled to
represent their contributions to the sample absorbance spectrum;
scaling factors are based on the indicated standard
concentrations (ISC) and measured (sample) analyte and
interferant concentrations, the sample and reference absorption
pathlengths, and the sample and reference gas pressures. No
band- shape correction for differences in the temperature of the
sample and reference spectra gases is made; such errors are
included in the FMU estimate. The actual and simulated sample
spectra are quantitatively compared to determine the fractional
model uncertainty; this comparison uses the reference spectra
band areas and residuals in the difference spectrum formed from
the actual and simulated sample spectra.
I . 2 Calculation*
1.2.1 For each analyte (with scaled concentration RSAj_) ,
select a reference spectrum SAi with indicated standard
concentration ISCj_. Calculate the scaling factors
TR L3 P3 RSAt
"
and form the spectra SACi by scaling each S^ by the factor
1.2.2 For each interferant, select a reference spectrum SIk
with indicated standard concentration ISC^. Calculate the
scaling factors
, TR L3 Ps RSIk (13)
k Ts LR PR ISC,
and form the spectra SIC^ by scaling each SIk by the factor RIk.
1.2.3 For each' analytical region, determine by visual
inspection which of the spectra SACi and SIC^ exhibit absorbance
bands within the analytical region. Subtract each spectrum
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BPA PTia Protocol
and SICfc exhibiting absorbance from the sample spectrum sg to
form the spectrum SUBg. To save analysis time and to avoid: the
introduction of unwanted noise into the subtracted spectrum, it
is recommended that the calculation be made (1) only for those
spectral data points within the analytical regions, and (2) for
each analytical region separately using the original spectrum Sg.
1.2.4 For each analytical region m, calculate the RMSD of
SUBg between the absorbance values and their mean in the region
FPUm to FFLjjj. Denote the result by RMSSm.
1.2.5 For each analyte i, calculate the quantity
RMSSa(FFUB-FFLB)AUiDLi
for each analytical region associated with the analyte.
1.2.6 If only the mth analytical region is used to
calculate the concentration of the itn analyte, set
1.2.7 If a number of analytical regions are used to
calculate the concentration of the itn analyte, set FMj equal to
the weighted mean of the appropriate FM_ values calculated above.
Mathematically, if the set of analytical regions employed is
{m' } , then
wlk FM
where Wi]c is calculated as described in Appendix D
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BPA PTIR Protocol
Paae
*
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 OFU^ - MAX{FRUi( FCUif FAU.^, FMUjJ and
-------
BPA PTIR Protocol _
*"tp'"" i*. •""»* . Page 34
APPENDIX K
SPECTRAL DE-RESOLUTION PROCEDURES
X.I Q«n«ral.
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 interferograma.
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.2 Procedures
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 BPA reference spectrum program on March 5, 1992. The
original data (in this example) are in KVB/Analect FX-70 format.
(i) dacoap ct»0305a.»if,0305dres,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) conpos* 0305dr««,0305drea.aif,1
"Compose" transforms truncated interferograms back to spectral
format.
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BPA FTIR Protocol
35
(iii) IQ2SP 0305drea.aif,0305drefl.ds£,3,l,low cm'1,high on'1
"IG2SP" converts interferogram to a single beam spectrum
using Norton-Beer medium apodization, 3, and no zero filling i
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 0305dre«.d»£,bkg0305a.d«f,0305dre«.dlf
"DVDR" ratios the transformed sample spectrum against the
background.
(v) ABSB 0305dr««.dlf,0305drefl.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
(PX-70) or Windows version (FX-80) use the "Extract" command
directly on the interferogram.
(i) EXTRACT CTS0305a.aif,0305dr«s.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. J&is procedure assumes familiarity
with basic functions of Grams™.
Thia procedure is specifically for using Grams to truncate
and transform reference interferograms that have been imported
into Grama 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 PILES AND DE- RESOLUTION PARAMETERS.
-------
BPA PTIR Protocol Paae 36
J
Desired Nominal Spectral
Resolution (cm'1)
0.25
0.50
1.0
2.0
Data Pile Name
Z00250.sav
ZOOSOO.sav
ZOlOOO.sav
Z02000.sav
Parameter "N"
Value
65537
32769
16385
8193
(i) Import using "Pile/Import" the desired *.aif file. Clear
all open data slots.
(ii) Open the resulting *.spc interferogram as file 1*1..
(iii) Xflip - If the x-axia ia 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.
xfliptfs-ts(iO,IN)+50
(iv) Run ICGKPQTB.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: If Last: 0 Type: Single Beam
Zero Pill: None Apodization: (as desired)
Phasing: User
Pointa: 1024 Interpolation: Linear Phase :
Calculate
(v) As in step (iii) , in the "Arithmetic/Calc" menu item
enter and then run the following commands (refer to Table l for
appropriate "PILB, " which may be in a directory other than
" c : \mdgrams . " )
setffp 7898.8805, 0 t loadspc aci\mdgrams\ PXLB" t i2«fs+#2
(vi) Use "Pag* Up" to activate file #2, and then use the
"Pile/Save A»" menu item with an appropriate file name to save
the result. ' .
X.3 Verification of Hew Resolution
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KPA FTIR Protocol
K.3.1 Obtain interferograms of reference sample and
background spectra. Truncate inter ferograma 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).
-FFLj ^ >Q5 (lg)
RMSS-RMSD in the itn 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
analytical region.
Atest-CTS-band area in the ith analvtical region of the test CTS.
-------
D-3 EPA METHOD 25A
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CBNTBR
NSPS TEST METHOD
METHOD 25A-DETERMINATION OP TOTAL GASEOUS ORGANIC
CONCENTRATION 0SINO A FLAME IONIZATION ANALYZER
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total gaseous
organic concentration of vapors consisting primarily of alkanes, alkenes, and/or
arenes (aromatic hydrocarbons). The concentration is expressed in terms of
propane (or other appropriate organic calibration gas) or in terms of carbon.
1.2 Principle. A gas sample is extracted from the source through a heated
sample line, if necessary, and glass fiber filter to a flame ionization analyzer
(FIA). Results are reported as volume concentration equivalents of the
calibration gas or as carbon equivalents.
2. Definition*
2.1 Measurement System*. The total equipment required for the determination
of the gas concentration. The system consists o'f the following major subsystems:
2.1.1 Sample Interface. That portion of the system that is used for one or more
of the following: sample acquisition, sample transportation, sample
conditioning, or protection of the analyzer from the effects of the stack
effluent.
2.1.2 Organic Analyser. That portion of the system that senses organic
concentration and generates an output proportional to the gas concentration.
2.2 Spaa Value. The upper limit of a gas concentration measurement range that
is specified for affected source categories in the applicable part of the
regulations. The span value is established in the applicable regulation and is
usually 1.5 to 2.5 times the applicable emission limit. If no span value is
provided, use a span value equivalent to 1.5 to 2.5 times the expected
concentration. For convenience, the span value should correspond to 100 percent
of the recorder scale.
2.3 Calibration Oas. A known concentration of a gas in an appropriate diluent
gas.
2.4 Zero Drift. The difference in the measurement system response to a zero
level calibration gas before and after a stated period of operation during which
no unscheduled maintenance, repair, or adjustment took place.
2.5 Calibration drift. The difference in the measurement system response to
a midlevel calibration gas before and after a stated period of operation during
which no unscheduled maintenance, repair or adjustment took place.
2.6 Response Time. The time interval from a step change in pollutant
concentration at the inlet to the emission measurement system to the time at
which 95 percent of the corresponding final value is reached as displayed on the
recorder.
2.7 Calibration Error. The difference between the gas concentration indicated
by the measurement system and the known concentration of the calibration gas.
Prepared by Emission Measurement Branch BMTIC TM-25A
Technical Support Division,. OAQPS, EPA June 23,
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EMTIC TM-25AEMTIC NSPS TEST METHOD '' *" Pa
3. Apparatus.
A schematic of an acceptable measurement system is shown in Figure 25A-1
The essential components of the measurement system are described below:
3.1 Organic Concentration Analyzer. A flame ionization analyzer (FIA) capable
of meeting or exceeding the specifications in this method.
3.2 Sample Probe. Stainless steel, or equivalent, three-hole rake type
Sample holes shall be 4 mm in diameter or smaller and located at 16 7 50 and
33.3 percent of the equivalent stack diameter. Alternatively, a single op4ning
probe may be used so that a gas sample is collected from the centrally located
10 percent area of the stack cross-section.
3.3 Sample Line. Stainless steel or Teflon * tubing to transport the sample
gas to the analyzer. The sample line should be heated, if necessary, to prevent
condensation in the line.
3.4 Calibration Valve Assembly. A three way valve assembly to direct the zero
and calibration gases to the analyzers is recommended. Other methods, such as
quick-connect lines, to route calibration gas to the analyzers are applicable.
3.5 Particulate Filter. An in-stack or an out-of-stack glass fiber filter is
recommended if exhaust gas particulate loading is significant. An out-of-stack
filter should be heated to prevent any condensation.
* Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
3.6 Recorder. A strip-chart recorder, analog computer, or digital recorder for
recording measurement data. The minimum data recording requirement is one
measurement value per minute, Note: This method is often applied in highly
explosive areas. Caution and care should be exercised in choice of equipment and
installation.
4. Calibration and Other Gases.
Gases used for calibrations, fuel, and combustion air (if required) are
contained in compressed gas cylinders. Preparation of calibration gases shall
be done according to the procedure in Protocol No. 1, listed in Citation 2 of
Bibliography. Additionally, the manufacturer of the cylinder should provide a
recommended shelf life for each calibration gas cylinder over which the
concentration does not change more than ±2 percent from the certified value. For
calibration gas values not generally available (i.e., organics between 1 and 10
percent by volume), alternative methods for preparing calibration gas mixtures,
such as dilution systems, may be used with prior approval of the Administrator.
Calibration gases usually consist of propane in air or nitrogen and are
determined in terms of the span value. Organic compounds other than propane can
be used following the above guidelines and making the appropriate corrections for
response factor.
4.1 Fuel. A 40 percent H2/60 percent N2 gas mixture is recommended to avoid
an oxygen synergism effect that reportedly occurs when oxygen concentration
varies significantly from a^mean value.
4.2 Zero Oas. High purity air with less than 0.1 parts per million by volume
(ppmv) of organic material (propane or carbon equivalent) or less than 0.1
percent of the span value, 'whichever is greater.
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EMTIC TM-25A EMTIC NSPS TEST METHOD " Pagp -
4.3 Low-level Calibration Oaa. An organic calibration gas with a concentration
equivalent to 25 to 35 percent of the applicable span value. concentration
4.4 Mid-level Calibration Qas. An organic calibration gas with a concentration
equivalent to 45 to 55 percent of the applicable span value.
4.5 High-level Calibration Qas. An organic calibration gas with a
concentration equivalent to 30 to 90 percent of the applicable span value.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than ±3 percent of the span value.
5.2 Calibration Drift. Less than ±3 percent of span value.
5.3 Calibration Brror. Less than ±5 percent of the calibration gas value.
6. Pretest Preparations
6.1 Selection of Sampling Site. The location of the sampling site is 'generally
specified by the applicable regulation or purpose of the test; i.e., exhaust
stack, inlet line, etc. The sample port shall be located at least 1.5 meters or
2 equivalent diameters upstream of the gas discharge to the atmosphere.
6.2 Location of Sample Probe. Install the sample probe so that the probe is
centrally located in the stack, pipe, or duct and is sealed tightly at the stack
port connection.
6.3 measurement system Preparation. Prior to the emission test, assemble the
measurement system following the manufacturer's written instructions in preparing
the sample interface and the organic analyzer. Make the system operable.
FIA equipment can be calibrated for almost any range of total organics
concentrations. For high concentrations of organics (>1.0 percent by volume as
propane) modifications to most commonly available analyzers are necessary. One
accepted method of equipment modification is to decrease the size of the sample
to the analyzer through the use of a smaller diameter sample capillary. Direct
and continuous measurement of organic concentration is a necessary consideration
when determining any modification design.
6.4 Calibration Brror Test. Immediately prior to the test series, (within 2
hours of the start of the test) introduce zero gas and high-level calibration gas
at the calibration valve assembly. Adjust the analyzer output to the appropriate
levels, if necessary. Calculate the predicted response for the low-level and
mid-level gases baaed on a linear response line between the zero.and high-level
responses. Then introduce low-level and mid-level calibration gases successively
to the measurement system. Record the analyzer responses for low-level and mid-
level calibration gases and determine the differences between the measurement
system responses and the predicted responses. These differences must be less
than 5 percent of the respective calibration gas value. If not, the measurement
system is not acceptable and must be replaced or repaired prior to testing. No
adjustments to the measurement system shall be conducted after the calibration
and before the drift check (Section 7.3). If adjustments are necessary before
the completion of the test series, perform the drift checks prior to the required
adjustments and repeat the calibration following the adjustments. If multiple
electronic ranges are to be used, each additional range must be checked with a
mid-level calibration gas to verify the multiplication factor.
6.5 Response Time Test. Introduce Zero gas into the measurement system at the
calibration valve assembly. When the system output has stabilized, switch
quickly to the high-level calibration gas. Record the time from the
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EMTIC TM-25A EMTIC NSPS TEST METHOD page 4
concentration change to the measurement system response equivalent to 95 percent
of the step change. Repeat the test three times and average the results.
7. Emission Measurement Test Procedure
7.1 Organic Measurement. Begin sampling at the start of the test period,
recording time and any required process information as appropriate. In
particular, note on the recording chart periods of process interruption or cyclic
operation.
7.2 Drift Determination. Immediately following the completion of the test
period and hourly during the test period, reintroduce the zero and mid-level
calibration gases, one at a time, to the measurement system at the calibration
valve assembly. (Make no adjustments to the measurement system until after both
the zero and calibration drift checks are made.) Record the analyzer response.
If the drift values exceed the specified limits, invalidate the test results
preceding the check and repeat the test following corrections to the measurement
system. Alternatively, recalibrate the test measurement system as in Section 6.4
and report the results using both sets of calibration data (i.e., data determined
prior to the test period and data determined following the test period).
9. Organic Concentration calculations
Determine the average organic concentration in terms of ppmv as propane or
other calibration gas. The average shall be determined by the integration of the
output recording over the period specified in the applicable regulation. If
results are required in terms of ppmv as carbon, adjust measured concentrations
using Equation 25A-1.
Cc = KCmeag Eq. 25A-1
Where:
Cc = Organic concentration as carbon, ppmv.
cm.«= Organic concentration as measured, ppmv.
K = Carbon equivalent correction factor.
K = 2 for ethane.
K = 3 for propane.
K = 4 for butane.
K = Appropriate response factor for other organic calibration
gases.
9. Bibliography
1 Measurement of Volatile Organic Compounds-Guideline Series. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-450/2-78-041. June 1978. p. 46-54.
2. Traceability Protocol for Establishing True Concentrations
Used for Calibration and Audits of Continuous Source
Monitors (Protocol No. 1). U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory. Research Triangle
Park, NC. June '1978.
-------
EMTIC TM-25A EMTIC NSPS TEST METHOD ?age 5
3. Gasoline Vapor Emission Laboratory Evaluation-Pare 2. U.S.
Environmental Protection Agency, Office of Air Quality Planning and
Standards. Research Triangle Park, NC. EMB Report No. 75-GAS-6.
August 1975.
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EMTIC TM-25A
EMTIC NSPS TEST METHOD
Page
Probe
CalixWton
Valve
Pump
Slack
Figure 25A-1. Organic Concentration Measurement System.
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D-4 EPA DRAFT METHOD 205
-------
EMISSION MEASUREMENT TECHNICAL INFORMATION CENTER
TEST METIOB
DRAFT--DO NOT CITE OR QUOTE
The EPA proposes to amend Title 40, Chapter I, Part 51 of the Code of
Federal Regulations as follows:
1. The authority citation for Part 51 continues to read as follows-
Authority: Section 110 of the Clean Air Act as amended. 42 U.S.C. 7410.
2. Appendix M, Table of Contents is amended by adding an entry to read as
follows:
Method 205—Verification of Gas Dilution Systems for Field Instrument
Calibrations
3. By adding Method 205 to read as follows:
Method 205 - Verification of Gas iilutioa Systems
for FieU lastnmeat Calibrations
1. INTROiOCnON
1.1 Applicability. A gas dilution system can provide known values of
calibration gases through controlled dilution of high-level calibration gases
with an appropriate dilution gas. The instrumental test methods in 40 CFR Pact
60 — e.g., Methods 3A, 6C, 7E, 10, 15, 16, 20, 25A and 25B -- require on-site,
multi-point calibration using gases of known concentrations. A gas dilution
system that produces known low-level calibration gases from high-level
calibration gases, with a degree of confidence similar to that for Protocol1
gases, may be used for compliance tests in lieu of multiple calibration gases
when the gas dilution system is demonstrated to meet the requirements of this
method. The Administrator may also use a gas dilution system in order to produce
a wide range of Cylinder Gas Audit concentrations when conducting performance
specifications according to Appendix F, 40 CFR Part 60. As long as the
acceptance criteria of this method are met, this method is applicable to gas
dilution systems using any type of dilution technology, not solely the ones
mentioned in this method.
1.2 Principle. The gas dilution system shall be evaluated on one analyzer once
during each field test. A precalibrated analyzer is chosen, at the discretion
of the source owner or operator, to demonstrate that the gas dilution system
produces predictable gas concentrations spanning a range of concentrations.
After meeting the requirements of this method, the remaining analyzers may be
calibrated with the dilution system in accordance to the requirements of the
applicable method for the duration of the field test. In Methods 15 and 16, 40
CFR Part 60, Appendix A, reactive compounds may be lost in the gas dilution
system. Also, in Methods 25A and 25B, 40 CFR Part 60, Appendix A, calibration
with target compounds other than propane is allowed. In these cases, a
laboratory evaluation is required once per year in order to assure the.
Administrator that the system will dilute these reactive gases without
significant loss. Note: The laboratory evaluation is required only if the
source owner or operator plans to utilize the dilution system to prepare gases
mentioned above as being reactive.
2. SPECIFICATIONS
2.1 Gas iilotioa Systea. The gas dilution system shall produce calibration
gases whose measured values are within ±2 percent of the predicted values. The
predicted values are calculated based on the certified concentration of the
supply gas (Protocol gases, when available, are recommended for their accuracy)
and the gas flow rates (or dilution ratios) through the gas dilution system.
Prepared by Eaissioa Measvreaeat Brack OTIC TM-205
Technical Support Division, OAQPS, EPA
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EMTIC TM-205 EMTIC NESHAP TEST METHOD ?aga 3
injection shall differ by more Chan ±2 percent from the average instrument
response for that dilution. 3.2.5 For each level of dilution, calculate the
difference between the average concentration output recorded by the analyzer and
the predicted concentration calculated in Section 3.2.2. The average
concentration output from the analyzer shall be within +2 percent of the
predicted value.
3.2.6 Introduce the mid-level supply gas directly into the analyzer, bypassing
the gas dilution system. Repeat the procedure twice more, for a total of three
mid-level supply gas injections. Calculate the average analyzer output
concentration for the mid-level supply gas. The difference between the certified
concentration of the mid-level supply gas and the average instrument response
shall be within ±2 percent.
3.3- If the gas dilution system meets the criteria listed in Section 3.2, the gas
dilution system may be used throughout that field test. If the gas dilution
system fails any of the criteria listed in Section 3.2, and the tester corrects
the problem with the gas dilution system, the procedure in Section 3.2 must be
repeated in its entirety and all the criteria in Section 3.2 must be met in order
for the gas dilution system to be utilized in the test.
4. REFERENCES
1. "EPA Traceability Protocol for Assay and Certification of Gaseous
Calibration Standards," EPA-600/R93/224, Revised September 1993.
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D-5 HC1 VALIDATION PAPER
-------
For Presentation at the Air & Waste Management Association's 90th Annual
& Exhibition, June 8-13,1997, Toronto, Ontario, Canada
97-MP74.05
Validation of EPA FTIR Method For Measuring HC1
Thomas J. Geyer
Midwest Research Institute, Suite 350, 401 Harrison Oaks Boulevard, Gary, North Carolina 27513
Grant M. Plummer
Rho Squared, 703 Ninth Street, Suite 183, Durham, North Carolina 27705
Introduction
In 1997 EPA is preparing to publish a sampling method (Draft Method 320)' based on the use of Fourier
transform infrared (FTIR) spectroscopy to measure emissions of hazardous air pollutants (HAPs). This
method establishes sampling procedures for measuring HAPs and employs analytical procedures in the
EPA FTIR Protocol.2
In 1996 EPA conducted a field test at a source with HC1 emissions. The test goal was to use the FTIR
Draft Method 320 to measure vapor phase pollutants at this source. Measurements were conducted on
the inlet and outlet of a control device. Hydrogen chloride (HC1) was a target pollutant for this source
and, for this reason, some samples were spiked from a cylinder containing a standard concentration of
103 ppm HC1. Results of HC1 measurements are presented along with a Method 3013 statistical analysis
of spiked and unspiked samples, and a comparison of results obtained using EPA reference spectra and
results obtained using spectra of the HC1 gas standard to measure the sample concentrations.
Experimental
The source tested in this project was a coal burning process with a relatively low moisture content (3 to
4% by volume). Rue gas temperatures were between 400 and SOOT. The principal components of the
gas stream were water vapor, CCh, SO?, and NO.
Sampling System
The sampling system is depicted in Figure I. The sample was extracted through a 4-ft long, 0.5-in
diameter stainless steel probe. Sample was transported through heated 3/8-in Teflon line using a KNF
Neuberger heated head sample pump (Model NO35 ST.111). A Balston particulate filter (holder Model
Number 30-25, filter element Model Number 100-25-BH, 99 percent removal efficiency at 0.1 ^im) was
connected in-line at the outlet of the sample probe. The sample line was heat wrapped and insulated.
Temperature controllers were used to monitor and regulate the sample line temperature at about 350° F.
The stainless steel manifold contained 3/8-in tubing, rotameters and 4-way valves to monitor and control
the sample flow to the FTIR gas cell. The manifold temperature was maintained between 300 to 310°F.
-------
V" \ :
The FTIR system included an Analect instruments Model RFX-40 interferometer equipped with .
band MCT detector. Samples were contained in an Infrared Analysis Model D22H variable path ^
The cell temperature was maintained at 250T. ~
Sampling Procedure
A series of discreet batch samples was collected by filling the cell above ambient pressure and closing the
inlet valve to isolate the sample. An outlet valve was briefly opened to vent the sample to ambient
pressure. The spectrum of the static sample was recorded. Then the cell was evacuated for the next
sample. Each spectrum consisted of 50 co-added scans. The minimum time between consecutive
samples was about 2 minutes. Inlet and outlet runs were conducted at the same time: the two location
were sampled alternately with the one FTIR system. The minimum time between consecutive
measurements was about 3 to 5 minutes.
Path Length Determinations
Two path lengths were used in this test. The cell was adjusted to 40 beam passes for the first two test
runs and reduced to 20 beam passes for a third test run. The number of beam passes was measured by
shining a He/Ne laser through the optical path and observing the number of laser spots on the field
mirror. The path lengths in meters were determined by comparing CTS EPA reference spectra to the
CTS spectra collected at each path length.
Absorption path lengths were determined from a comparison of the field test CTS spectra and EPA
library CTS spectra of ethylene (CiH^ . For high temperature spectra, the EPA library interferograms
ctsOl I5a.aif and bkgOl 15a.aif were de-resolved to the appropriate spectral resolution (either 1 or 2 cm'1)
according to the procedures of reference 2 (Appendix K). The same procedure was used to generate
low-temperature spectra from the original interferometric data in the EPA library files cts0829a.aif and
bkg0829a.aif. The resulting files were used in least squares fits to the appropriate field CTS spectra (see
reference 2, Appendix H) in two regions (the FP, or "fingerprint" region from 790 to 1139 cm' and the
CH, or "CH-stretch region" from 2760 to 3326 cm"1). The fit results for each region, test, and set of test
sampling conditions were averaged. They and their average uncertainties are presented in Table I. The
CH values were used in analytical region 4 where HC1 was measured.
Analyte Spiking
Draft Method 3201 contains a procedure for spiking the flue gas with one or more of the target analytes.
The spike procedure closely follows Section 6.3 of reference 3. The primary purpose of analyte spiking
is to provide a quality assurance check on the sampling system to determine if analyte losses occur in
transport to the analyzer. A second purpose is to test the analytical program to verify that the analyte(s)
can be measured in the sample matrix. If at least 12 (independent) spiked and 12 (independent) unspiked
samples are measured then a Method 301 statistical analysis can be performed on the results to "validate"
the method.
Figure 1 shows the sampling configuration used for the analyte spike. This procedure is described in
detail elsewhere1. In this test, a measured flow of the gas standard was preheated to the sample line
temperature before being introduced'into the extracted flue gas at the back of the probe. The spiked
sample then passed through all of the sample components to the gas cell where the spectrum was
recorded. A series of unspiked samples was measured, the spike was turned on and then a complete
-------
V"A ~^i( 5
series of spiked samples was measured. The spike then was aimed off to make additional unspike
measurements. Ideally, the spike comprises 1/10 or less of the sample mixture. The dilution is esurr
by comparing the spike How to the total flow, but the actual dilution is determined measuring a tracer
(SF6) concentration in the spiked samples and comparing that to tracer concentration in the undiluted
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averaged to prov^e a "reduced absorptivity" (see Reference 9), which was stored in the spectra
097.aif and employed in ail subsequent HC1 analyses. The HC1 analysis was applied to the de-resc
EPA library HCI spectra to determine the fractional calibration uncertainty (FCU), which is presented -n
Table 2.
During the test MRI recorded spectra of samples taken directly from an HC1 cylinder standard (103 ppm
HC1 in nitrogen, ± 5% accuracy from Scott Specialty Gases). Four independent HC1 "calibration" spectra
were measured at each of the two instrument configurations used to collect the data presented in Figures
2 and 3. The Fractional Calibration Uncertainty for each set of four spectra and the analytical region for
the "Multicomp" analysis is presented in Table 2.
Even though the two sets of results are identified by the program names "4FTT" and "Mulitcomp," it is
important to note that the "Multicomp" results were reproduced by the program "4FIT" when the HC1
calibration spectra were used as input for "4FIT." Therefore, any differences in the analyses are not
attributable to the programs, but to the use of different input spectra.
Results
HCI Concentrations
Table 3 summarizes results from the three test runs at the two locations. The agreement between the
"4F1T' and the "Multicomp" analyses is very good except for the third run. This run was conducted after
the path length had been decreased from 40 to 20 laser passes.
The two comparisons plotted in Figures 2 and 3 are indicated in Table 3. The Run 2 outlet results
(Figure 2) are typical of those obtained for the Run 2 inlet results recorded on the same day and the Run
1 inlet and outlet results recorded a day earlier. The close agreement was typical also for two data sets
collected at another field test in one test run. For 3 of the 6 data sets presented in Table 3, the results
obtained with program "4FTT," using de-resolved EPA library reference spectra and the CTS-derived
absorption path lengths, are nearly identical (within the 4 o uncertainty) to those obtained using
"Multicomp," which employed the field HQ calibration standard spectra without an explicit absorption
path length determination. The average percent difference of the Run 2 inlet results was slightly higher
than the 4a uncertainty, but this percent difference corresponded to an average difference of 1.7 ppm.
The error bars in Figures 2 and 3 correspond to the 4a statistical uncertainties in the "4FIT" HQ
concentrations.
Method 301 Analysis
Tables 4 and 5 present the results of the method 301 statistical analysis of the spiked and unspiked
"4FIT' and "Multicomp" Run 3 outlet results, respectively. Note that the nearly constant difference of
about 19 percent in the two analyses has almost no effect on the Method 301 statistical analyses, which
indicate no significant bias in the HCI measurements. This is because the statistical treatment analyzes
differences between spiked and unspiked measurements and compares the differences to an expected
value of the spike. Since the same offset is apparent in the "Multicomp" analysis of both the spiked and
unspiked results, the calculated bias is not affected.
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': i'5
This is another indication that the difference in the "4FTT" and "Multicomp" run 3 results is not due cc a
measurement or analytical error. It is likely due either to an anomaly in the Run 3 path length
determination for the CH stretch region or to an error associated with using the HC1 "calibration spectra
as input for the "Multicomp" program. As stated above, the "4FIT" program reproduced the
"Multicomp" results when using the HC1 "calibration" spectra as input.
Discussion
The uncertainties for the four data sets in Runs I and 2 are approximately equal to the small differences
between the "4FTT' and "Multicomp" results. The excellent agreement of the two analyses is noteworthy
for several reasons. HC1 is notoriously difficult both in terms of sampling and data analysis, due
(respectively) to the compound's high chemical reactivity and the details of the infrared spectrum which
make the analysis susceptible to instrument resolution errors. The results also provide a direct
comparison between two fundamentally different analytical approaches, one relying on in situ calibration
of the instrument using actual calibration gas standards, and the other using the calibration transfer
concept
This comparison is somewhat clouded by the results depicted in Figure 3, which show the HC1
concentration determined during Run 3 at the outlet. These are also typical of the results for another data
set recorded on the same day at the inlet Unlike the Runs 1 and 2 data, the Run 3 data indicate a
statistically meaningful difference of approximately 18% between the "4FIT" and "Multicomp" results.
We stress that this difference is not attributable to errors in the computer programs, which produced
reliable results in these and many independent test cases. Rather, the difference seems be related to an
anomaly in the absorption path length determinations presented in Table 1. Note that the CTS-derived
absorption path length for (nominally) 20 passes, corresponding to the Run 3 data, are 10.2 meters 14.3
meters for the CH-stretch and "fingerprint" (FP) analytical regions. The difference between the CH and
FP results is much larger for this particular day of testing than on the other two test days, represented in
the table by the 16- and 40- pass results. (It is also anomalous with respect to results obtained using the
same instrument in another field test completed within nine days of the testing addressed here.)
Moreover, were the average of the CH and FP region values (12.2 meters) used for the HC1
concentration values rather than the CH region value of 10.2 meters, the level of agreement between the
two sets of analytical results for the Run 3 data would be comparable to that of the Run I and 2 data
discussed immediately above.
We have attempted to determine the cause of this difference by considering of a number of possible
operational and instrumental problems. However, no single systematic effect seems sufficient Because
consistent path length determinations were carried out both before and after the HC1 measurements in
question, a sudden change in instrument performance must be ruled out. Gas pressure and dilution
effects cannot cause the type of wavenumber-dependent effects observed in the CTS spectra; subsequent
laboratory measurements of C2H4 indicated that temperature variations, like pressure and dilution effects,
would lead to path length errors in the same direction for the CH and FP regions. Because the same EPA
CTS ethylene spectra were used in all the path length determinations and led to excellent statistical results
in all cases, potential data processing errors in the deresoluton procedure are also insufficient to explain
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the anomalous results. However, we note that the observed 18% discrepancy still allows high cc,
in the data and the infrared technique, and the discrepancy is obvious mainly because of the overall;,
quality of the data set and statistical results.
Conclusions
The evaluation presented in this paper demonstrates that the EPA FTTR Protocol analytical procedures
based on the use of laboratory reference spectra to determine analyte concentrations in sample spectra
give excellent, and verifiable, results. This is true even for HC1, which is difficult to sample, and even
when the reference spectra are deresolved to match the sample spectra.
Two independent analyses using different programs and different spectral input data were performed on 6
FTTR data sets collected at a site with HC1 emissions. The alternate analyses produced nearly identical
results in 4 of the data sets. In two of the data sets the agreement was also good, but the average
discrepancy of about 18 percent between results produced by the alternate analyses was larger than the
average measurement uncertainty of about 5.5 percent. A preliminary evaluation of this discrepancy has
not determined the exact cause, but it is probably attributable to an anomaly in the measurement of the
absorption path length for the one test run.
These results also demonstrate the need for careful instrument performance checks and preparation of
library reference spectra. Strict QA/QC standard procedures are required to produce .accurate
measurements. The Method 301 validation results showed no significant bias in the FTIR measurements
of HC1 at this test, but the validation procedure cannot reveal a constant offset "error" that is applied
equally to both spiked and unspiked samples.
Acknowledgments
The field test discussed in this paper was funded by the Emission Measurement Center of the United
States Environmental Protection Agency.
References
I) Draft Method 320, "Measurement of Vapor Phase Organic and Inorganic Emissions by Extractive
Fourier Transform Infrared (FTIR) Spectroscopy," EPA Contract No. 68-D2-0165, Work Assignment
3-08, July, 1996.
2) "Protocol For The Use of FTTR Spectrometry to Perform Extractive Emissions Testing at
Industrial Sources," EPA Contract No. 68-D2-0165, Work Assignment 3-12, EMTIC Bulletin Board.
September, 1996.
3) "Method 301 - Field Validation of Pollutant Measurement Methods from Various Waste Media," 40
CFR Part 63, Appendix A.
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y7-.MP~4.io
4. D.M. HaaJand and R.G. Easterling, "Improved Sensitivity of Infrared Spectroscopy by the App -n
of Least Squares Methods," Appl. Spectrosc. 34(5):539-548 (1980).
5. D.M. Haaland and R.G. Easterling, "Application of New Least-Squares Methods for the Quantitative
Infrared Analysis of Multicomponent Samples," Aool. Soectrosc. 36(6):665-673 (1982).
6. D.M. Haaland, R.G. Easterling and D.A. Vopicka, "Multivariate Least-Squares Methods Applied to
the Quantitative Spectral Analysis of Multicomponent Samples," Appl. Spectrosc. 39(l):73-84 (1985).
7. W.C. Hamilton, Statistics in Physical Science. Ronald Press Co., New York, 1964, Chapter 4.
8. P.R. Griffiths and J.A. DeHaseth, Fourier Transform Infrared Spectroscopv. John Wiley and Sons,
New York, 1986, ISBN 0-471-09902-3.
9. G. M. Plummer and W. K. Reagen, "An Examination of a Least Squares Fit FTIR Spectral Analysis
Method," Air and Waste Management Association. Paper Number 96-WA65.03, Nashville, 1996.
10. T. J. Geyer, "Method 301 Validation of Fourier Transform Infrared (FTIR) spectroscopy
For Measuring Formaldehyde and Carbonyl Sulfide," Air and Waste Management Association, Paper
Number. 96-RA110.03, Nashville, 1996.
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Table 1. Pathlength Determination Results.
CTS Conditions
# Passes Temp (10
16 293
Run 3 (Figure 3)
Run2 (Figure 2)
20 293
20 393
40 293
40 393
CH region
Result (m) % uncert.
6.5 2.9
tl.O 2.6
10.2 2.5
19.2 5.5
20.2 2.6
FP region !
Result (m) % uncert. i
6.7 1.3
11.3 1.6
14.3 22
20.0 1.8
23.4 1.6
Table 2. Fractional Calibration Uncertainties (FCU in Reference 2) For the Two Quantitative Analyses.
Compound
HC1 "4fit"
HC1 "Mcomp"
Run 2*
Run 3 *
FCU(%)
4.6
1.05
3.14
Analytical Region (cm'1)
2747 - 2848
2569-2871
* Spectra of four samples from the cylinder standard (103 ppm HC1 in nitrogen) were used in the
'Mcomp" analysis. The spectra were measured at the same instrument configuration used in each run.
Table 3. Summary of results comparisons in 4 runs (8 data sets).
Data Set
Run 1 Inlet
Run 1 Outlet
Run 2 Inlet
Run 2 Outlet (Figure 2)
Run 3 Inlet
Run 3 Outlet (Figure 3)
Average "4FTT"
Results
HC1 ppm % 4 • o l
43.3 3.9
34.5 4.1
14.8 7.7
48.0 4.5
62.5 5.6
58.0 5.5
Average "Multicomp"
Result
HCl ppm
42.1
32.9
13.1
46.4
50.9
47.3
% Difference l
2.9
4.4
11.8*
3.2
18.6
18.4
No. of Results1
36
30
16
33
41
52
1 - Average percent uncertainty in the 4FTT results.
2 - Equals (4FIT-Multicomp)/4FIT.
3 - Equals the number of spectra included in the average. Results from condenser and ambient air
samples were not included in the averages.
4 - Flow restriction during this run may have caused HO losses resulting in lower measured
concentrations for this run. An average difference of 1.7 ppm corresponded to a relatively large percent
difference of 11.8 % on the smaller average concentration for this run.
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Table 4. Method 301 statistical analysis of "4FTT' HC1 results in Figure 3.
97.MP~4.05
Unspiked
Run Average =
Statistical
Results
HC1 ppm
57.18 *
SD =
F =
RSD=
Bias =
t =
d i (d ,)2
9.68 52.561
2.093
0.491
3.7
•0.088
0.12
HC1 ppm
62.14 *
SD =
SDpooled =
Exp Cone =
CF =
Spiked
di
4.74
1.466
1.807
5.05
1.02
(d '-
25.784
* Represents the average result in 12 unspiked or spiked samples. Statistical variables are described in
Section 6.3 of EPA Method 301.3 Procedure for determining spiked dilution factor and expected
concentration, Exp Cone, is described in reference 10.
Table 5. Summary of Method 301 statistical analysis of "Multicomp" results in Figure 3.
Unspiked
Run Average =
Statistical
Results
HC1 ppm
45.88 *
SD =
RSD=
Bias =
d [ (d i)2
8.62 34.242
1.689
0.628
3.7
-0.070
0.11
Spiked
HC1 ppm
50.86 *
SD =
SDpooled =
Exp Cone =
CF =
di
3.51
1.338
1.524
5.05
1.01
(d,)2
21.496
* Represents the average result in 12 unspiked or spiked samples. Statistical variables are described in
Section 6.3 of EPA Method 301.3 Procedure for determining spiked dilution factor and expected
concentration, Exp Cone, is described in reference 10.
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Figure 1. Extractive sampling system.
V.ol
Untie.ilril line
Healed Line
la C*III**U*«a O..*
Cy1lii*l*il
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TECHNICAL REPORT DATA
' (Peon mad liuaueaoM.en tht mtnt btfon compitttitgt
1. REPORT NO.
EPA-454/R-99-Q33
2.
3. RECIPIENT'S ACCESSION NCv
4. TITLE ANO SUBTITLE
FTIR and Method 25A Emissions Test at an Integrated Iron and Steel
Manufacturing Plant
Indiana Harbor Wbrks of LTV Steel Co. Inc. East Chicaao
9. REPORT DATE
SEPTEMBER 1999
0. PERFORMING ORQANIZATIOWCOOI
7. AUTHORIS)
EMAD
8. PERFORMING ORGANIZATION REPORT NO.
I. PERFORMING ORGANIZATION NAME ANO ADDRESS
1O. PROGRAM ELEMENT NO..
11. CONTHACT7GRA,NT NO. •
Midwest Research Institute (MRI)
EPA Cant, 68D98027
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency
Research Triangle Park, N.C. 27711
13. TYPE OP REPORT ANO PIRIOO COVERED
14. SPONSORING AGENCY CODE
EPA/200/04
16. SUPPLEMENTARY NOTES
16. ABSTRACT
The purpose of this testing program was to obtain emissions data by using FTIR and EPA Method 25a on
a sintering process to quantify and characterize HAP emissions and the performance of the control unit
for MACT development for this industry .(Integrated Iron and Steel).
i7. MACT Rule Support,
KEY WORDS ANO DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI FieU/Gioup
MACT Support for the
Integrated Iron and Steel
Industry (Sintering)
18. DISTRIBUTION STATEMENT
RELEASE UNLIMITED
19. SECURITY CLASS f Tins Report!
21. NO. OF PAGES
415
20. SECURITY CLASS tTiiispaget
11. PRICE
EPA Form 2220-1 (R«». 4-77) PREVIOUS EDITION is OBSOLETE
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