r, EPA
United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EPA-454/R-99-035
September 1999
Air
FTIR EMISSIONS TEST AT AN IRON
FOUNDRY
Waupaca Foundry, Inc.
Plant No. 5, Tel City, Indiana
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FTIR EMISSIONS TEST AT AN IRON FOUNDRY
Waupaca Foundry, Inc.
Plant No. 5, Tell City, 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
Mr. Michael Ciolek
Work Assignment Manager
EPA Contract No. 68-D-98-027
Work Assignment 2-13
MRI Project No. 104951-1-013-04
September, 1999
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GENERAL DISCLAIMER
This document may have problems that one or more of the following disclaimer
statements refer to:
This document has been reproduced from the best copy furnished by the
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This document may contain tone-on-tone or color graphs, charts and/or
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The document is paginated as submitted by the original source.
Portions of this document are not fully legible due to the historical nature
of some of the material. However, it is the best reproduction available
from the original submission.
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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. 2-13. 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. 4-25 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 4-25 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 08.
This report presents the procedures, schedule, and test results for an emissions test
performed at Waupaca Foundry in Tel City, Indiana. The emissions test used Fourier transform
infrared (FTIR) sampling procedures to measure hazardous air pollutants (HAP's) and other
pollutants.
This report consists of one volume (354 pages) with seven sections and four appendices.
Midwest Research Institute
John Hosenfeld
Program Manager
Approved:
Jeff Shular
Director, Environmental Engineering Division
September 30,1999
in
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TABLE OF CONTENTS
1,0 INTRODUCTION 1-1
1.1 BACKGROUND 1-1
1.2 PROJECT SUMMARY 1-1
1,3 PROJECT PERSONNEL 1-5
2.0 PROCESS AND CONTROL EQUIPMENT OPERATION 2-1
2.1 INTRODUCTION 2-1
2.2 PROCESS DESCRIPTION 2-1
2.2.1 Iron Melting in Cupolas 2-1
2.2.2 Pouring, Cooling and Shakeout , 2-4
2.3 SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING
SOURCE TEST 2-5
2.3.1 Process Operating Data for Cupola Melting Operations 2-5
2.3.2 Process Operating Data for Pouring, Cooling and Shakeout
Operations 2-11
3.0 TEST LOCATIONS AND GAS COMPOSITION , 3-1
3.1 BAGHOUSE OUTLET - STACK 3-1
3.2 BAGHOUSE INLET DUCT 3-1
3.3 MOLD COOLING LINE 3-1
3.4 MOLD SHAKE-OUT HOUSING 3-5
3.5 VOLUMETRIC FLOW 3-5
4.0 RESULTS 4-1
4.1 TEST SCHEDULE 4-1
4.2 FIELD TEST PROBLEMS AND CHANGES 4-1
4.3 FTIR RESULTS 4-2
4.3.1 Mold Cooling Line and Shake-out Housing 4-2
4.3.2 Baghouse Inlet and Outlet 4-2
4.4 ANALYTE SPIKE RESULTS 4-2
5.0 TEST PROCEDURES 5-1
5.1 SAMPLING SYSTEM DESCRIPTION 5-1
5.1.1 Sample System Components 5-1
5.1.2 Sample Gas Stream Flow 5-3
5.2 FTIR SAMPLING PROCEDURES 5-3
5.2.1 Batch Samples .5-4
5.2.2 Continuous Sampling ., 5-4
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TABLE OF CONTENTS (CONTINUED)
5.3 ANALYTE SPIKING 5-5
5.3.1 Analyte Spiking Procedures 5-5
5.3.2 Analysis of Spiked Results 5-6
5.3.2.1 Determination of Formaldehyde Standard 5-6
5.3.2.2 Determination of Concentrations in Spike Mixtures 5-6
5.3.2.3 Determination of Percent Recovery 5-7
5.4 ANALYTICAL PROCEDURES 5-9
5.4.1 Computer Program Input 5-10
5.4.2 EPA Reference Spectra 5-11
5.5 FTIR SYSTEM 5-13
6.0 SUMMARY OF QA/QC PROCEDURES 6-1
6.1 SAMPLING AND TEST CONDITIONS 6-1
6.2 FTIR SPECTRA 6-2
7.0 REFERENCES 7-1
APPENDIX A - VOLUMETRIC FLOW DATA
A-l. MOLD COOLING AND SHAKE-OUT HOUSING LINE FLOW DATA
A-2. BAGHOUSE FLOW DATA
APPENDIX B - FTIR DATA
B-l. FTIR RESULTS TABLES
TABLE B-l. FTIR RESULTS FROM THE MOLD COOLING LINE
TABLE B-2. FTIR RESULTS FROM THE SHAKE-OUT HOUSING LINE
TABLE B-3. FTIR RESULTS AT THE BAGHOUSE INLET
TABLE B-4. FTIR RESULTS AT THE BAGHOUSE OUTLET
B-2. FTIR FIELD DATA RECORDS
B-3. FTIR FLOW AND TEMPERATURE READINGS
APPENDIX C - CALIBRATION GAS CERTIFICATES
APPENDIX D - TEST METHODS
D-l. EPA METHOD 320
D-2. EPA FTIR PROTOCOL
VI
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TABLE OF CONTENTS (CONTINUED)
Page
LIST OF FIGURES
Figure 2-1. Simplified schematic of cupola gas handling system , 2-2
Figure 2-2. Hourly melting rates during cupola testing 2-7
Figure 2-3. Blast air flow rate through cupola 2-10
Figure 3-1. Schematic of cupola gas handling system, sampling points A and B 3-2
Figure 3-2. Schematic of baghouse inlet and baghouse outlet. Sampling points
A and B, respectively 3-3
Figure 3-3. Schematic of mold cooling and mold shake-out gas handling system;
sampling points C and D 3-4
Figure 4-1. Example spectra of spiked and unspiked baghouse outlet samples 4-10
Figure 5-1. Sampling system schematic 5-2
LIST OF TABLES
TABLE 1-1. SUMMARY OF FTM RESULTS FROM THE MOLD COOLING
AND SHAKE-OUT HOUSING DUCTS 1-3
TABLE 1-2. SUMMARY OF FTIR RESULTS (ppm) AT THE CUPOLA
BAGHOUSE INLET AND OUTLET 1-4
TABLE 1-3. PROJECT PERSONNEL 1-5
TABLE 2-1. TYPICAL CUPOLA CHARGE MATERIALS 2-3
TABLE 2-2. SUMMARY OF CUPOLA CHARGING DURING THE TEST DAYS 2-6
TABLE 2-3. PROCESS DATA DURING THE DAYS OF CUPOLA TESTING 2-8
TABLE 2-4. PERIODS WHEN CUPOLA WAS "ON RELIEF' DURING TESTING ..... 2-9
TABLE 2-5. PROCESS IRON CHEMISTRY AT CUPOLA 2-11
TABLE 2-6. TYPICAL RESULTS FROM GREEN SAND ANALYSIS 2-12
TABLE 3-1. FLOW DATA AT WAPAUCA MOLD COOLING AND
SHAKE-OUT HOUSING PROCESSES 3-5
TABLE 3-2. CUPOLA BAGHOUSE INLET AND OUTLET GAS COMPOSITION
AND FLOW SUMMARIES 3-6
TABLE 4-1. TEST SCHEDULE AT WAUPACA FOUNDRY 4-1
TABLE 4-2. FORMALDEHYDE SPIKE RESULTS FROM THE MOLD COOLING
PROCESS , 4-5
TABLE 4-3. FORMALDEHYDE SPIKE RESULTS FROM THE WAUPACA
SHAKE-OUT HOUSING PROCESS 4-5
TABLE 4-4. TOLUENE SPIKE RESULTS FROM THE MOLD COOLING PROCESS ... 4-6
TABLE 4-5. TOLUENE SPIKE RESULTS FROM THE SHAKE-OUT HOUSING
PROCESS 4-6
TABLE 4-6. SUMMARY OF FORMALDEHYDE SPIKE RESULTS AT THE CUPOLA
BAGHOUSE INLET 4-7
Vll
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TABLE OF CONTENTS (CONTINUED)
Page
TABLE 4-7. SUMMARY OF FORMALDEHYDE SPIKE RESULTS AT THE CUPOLA
BAGHOUSE OUTLET 4-7
TABLE 4-8. SUMMARY OF TOLUENE SPIKE RESULTS AT THE CUPOLA
BAGHOUSE INLET 4-8
TABLE 4-9. SUMMARY OF TOLUENE SPIKE RESULTS AT THE CUPOLA
BAGHOUSE OUTLET 4-8
TABLE 4-10. COMPARISON OF FTIR SPECTRA OF SAMPLES FROM TOLUENE
(60 ppm) CYLINDER TO EPA TOLUENE REFERENCE SPECTRA 4-9
TABLE 5-1. DETERMINATION OF FORMALDEHYDE STANDARD
CONCENTRATION 5-6
TABLE 5-2. MEASURED ANALYTE CONCENTRATIONS AND MIXING FLOW
RATES FOR THE SPIKE MIXTURES 5-8
TABLE 5-3. PROGRAM INPUT FOR ANALYSIS OF MOLD COOLING
AND SHAKE-OUT HOUSING SAMPLE SPECTRA 5-11
TABLE 5-4. PROGRAM INPUT FOR ANALYSIS OF BAGHOUSE
INLET AND OUTLET SAMPLE SPECTRA 5-12
TABLE 5-5. PROGRAM INPUT FOR ANALYSIS OF CTS SPECTRA
AND PATH LENGTH DETERMINATION 5-13
TABLE 5-6. RESULTS OF PATH LENGTH DETERMINATION 5-13
Vlll
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1.0 INTRODUCTION
1.1 BACKGROUND
The Emission Measurement Center (EMC) of the U. S. EPA received a request 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), U, S. EPA, to perform emissions testing at iron foundries,
specifically on cupola emission control devices, as well as pouring, cooling, and shake-out
operations. The test program was performed in September, 1997 under Work Assignment 4-25,
under EPA Contract No. 68-D2-0165. This draft report was prepared under Work
Assignment 2-08, under Contract No. 68-W6-0048.
1.2 PROJECT SUMMARY
The cupola melting process is used to melt iron for casting into automotive and machine
parts. It is potentially a significant source of HAP emissions, including metal and organic
compounds. Emissions from the mold pouring, cooling, and shake-out are also potential sources
of HAP emissions.
The principal emission point at a cupola furnace is the exhaust from the furnace itself.
Emission controls for the Waupaca Plant No. 5 include a movable cap on the cupola, that seals
the charge, coarse grain separator, afterburner, drop out chamber, heat exchangers (recuperators),
dry calcium hydroxide injection system, pulse-jet baghouse, and stack. Cupola emissions testing
was conducted at the stack (outlet) and an inlet location to the baghouse to determine the
measurable emissions released during the melting process. Testing was also conducted at the
cooling line and shake-out housing ducts to determine the measurable emissions released during
the cooling and shake-out of the castings. Pouring operations had no emission capture or control
system; thus, no testing was conducted at the mold pouring location.
Three test runs were conducted at the cupola inlet and outlet locations over a three day
period simultaneously with manual method testing conducted by Pacific Environmental Services
(PES). One test run over a 4 hour (hr) period was conducted by FTIR only at both the cooling
line and shake-out housing locations. A summary of the FTIR results at the cooling and
shake-out housing locations is presented in Table 1-1. Emissions from the mold cooling and
shakeout housing included CO, methane, and ethylene. The emissions also contained a mixture
of heavier aliphatic hydrocarbon compounds. In the draft report the mixture of heavier
1-1
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hydrocarbons was represented by "hexane" because hexane and isooctane are the only aliphatic
hydrocarbons in the EPA library of HAP reference spectra. There are many hydrocarbon
compounds that are structurally similar to hexane and also have similar spectral features. After
the draft report was submitted, EPA directed MRI to measure quantitative spectra of some
additional hydrocarbon compounds. MRI selected candidate compounds that, based on their
infrared spectra in the region of the analyses, near 2900 cm"1, were likely to be components of
the sample mixture. MRI obtained commercially-prepared cylinder standards of butane, n-
heptane, pentane, 1-pentene, 2-methyl-l-pentene, 2-methyl-2butene, 2-methyl-2-pentene, and 3-
methylpentane. MRI then measured FTIR reference spectra of these compounds in the
laboratory. MRI also measured new high-temperature spectra of the HAPs hexane and isooctane.
Documentation of the new reference spectra and a brief description of the laboratory procedures
is presented in Appendix B.
The new spectra were used in revised analyses that gave the results presented in Table 1-1
and in Tables B-l and B-2. The new spectra made it possible to better represent the sample
mixture spectrum. Consequently hexane was not detected in mold cooling emissions, and was
only detected in one sample in the shakeout housing emissions. The reported hexane
concentrations are lower in the revised results because the spectrum of the sample hydrocarbon
mixture, which was represented by "hexane" in the draft results, is better represented by some of
the new spectra of other non-HAP hydrocarbons. In particular, 3-methylpentane and 1-pentene
were detected in cooling and shakeout housing process emissions. Butane and 2-methyl-2-
butene were also measured at the shakeout housing. The revised results give a more accurate
representation of the process emissions, but it's possible that other hydrocarbon compounds
could be measured in the emissions if their reference spectra were available.
The FTIR results from the cupola baghouse inlet and outlet locations are presented in
Table 1-2. Toluene was included in the analysis because this compound was spiked at the inlet
and outlet. Additional description of the results is in Section 4.
EPA Method 320 uses an extractive sampling procedure. A probe, pump, and heated line
are used to transport samples 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
1-2
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results were saved on computer media for review after the test is completed. A compact disk
containing all of the FTIR data was provided with the draft report.
TABLE 1-1. SUMMARY OF FTIR RESULTS FROM THE MOLD COOLING
AND SHAKE-OUT HOUSING DUCTS
Compound || Cooling Uncertainty || Shakeout Uncertainty
Toluene ppma
Ib/hr
kg/hr
Hexane ppm
Ib/hr
• kg/hr
Ethylene ppm
Ib/hr
kg/hr
Methane ppm
Ib/hr
kg/hr
Carbon Monoxide ppm
Ib/hr
kg/hr
Formaldehyde ppm
Ib/hr
kg/hr
3-Methylpentane ppm
Ib/hr
kg/hr
Butane ppm
Ib/hr
kg/hr
1-Pentene ppm
Ib/hr
kg/hr
2-Methyl-2butene ppm
Ib/hr
kg/hr
17.5 3.9
5.01
2.27
ND 30.6
13.3 0.8
1.158
0.525
178.5 2.6
8.859
4.017
402.3 28.1
34.95
15.85
ND 2.97
5.42 1.68
1.45
0.656
ND 34.90
17.9 3.89
3.88
1.76
ND 8.81
0.81 3.5
0.33
0.15
0.16 17.3
0.060
0.027
3.4 0.8
0.42
0.19
26.0 1.6
1.82
0.826
106.7 ' 19.1
13.06
5.92
ND 1.74
3.35 1.05
1.263
0.573
3.21 5.83
0.816
0.370
0.92 8.82
0.28
0.13
7.02 1.53
2.19
0.991
aAverage ppm concentration for the Run.
1-3
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TABLE 1-2. SUMMARY OF FTIR RESULTS (ppm) AT THE CUPOLA BAGHOUSE INLET AND OUTLET3
Compound
HC1
Toluene
Methane
Formaldehyde
ppmc
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
ppm
Ib/hr
kg/hr
9/8/97(12:02-17:07)
Inlet
33.5
5.2
2.4
ND
5.2
0.6
0.3
0.3
0.04
0.02
Uncb
3.3
2.9
1.2
1.7
Outlet
23.3
4.7
0.4
ND
4.7
0.7
0.1
ND
Unc
3.3
2.9
1.2
1.6
9/9/97(7:49-14:19)
Inlet
27.7
6.2
2.8
ND
5.3
0.6
0.3
ND
Unc
3.6
3.2
1.3
1.8
Outlet
16.3
4.6
0.6
0.4
0.3
0.1
4.9
1.1
0.1
ND
Unc
3.4
3.0
1.2
1.7
9/10/97(7:53- 14:19)
Inlet
29.7
6.7
3.0
ND
4.8
0.6
0.3
ND
Unc
3.3
2.9
1.2
1.7
Outlet
22.6
6.4
0.8
ND
4.7
1.0
0.1
ND
Unc
3.1
2.8
1.1
1.6
a PES did not complete a run on 9/8, but completed a manual run on 9/9 and two manual runs on 9/10. The PES flow data from 9/9 were used to calculate mass
emission rates for the MRI runs on 9/8 and 9/9. The PES flow data from their first manual run on 9/10 were used to calculate emission rates for the MRI run
on 9/10.
Estimated uncertainty in ppm in the reported concentration.
c Average ppm concentration for the Run.
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1.3 PROJECT PERSONNEL
The EPA test program was administered by the 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.
TABLE 1-3. PROJECT PERSONNEL
Organization and Title
Waupaca Foundry, Inc.
P.O. Box 249
311 S. Tower Road
Waupaca, WI 54981
Waupaca Foundry, Inc.
P.O. Box 189
9856 State Highway 66
Tell City, IN 47586
U. S. EPA, EMC
Work Assignment Manager
Work Assignment 4-25
U. S. EPA, EMC
Work Assignment Manager
Work Assignment 2-08
MRI
Work Assignment Leader
Work Assignment 4-25
Work Assignment 2-13
MRI
Work Assignment Leader
Work Assignment 2-08
Name
JeffLoeffler
Keith Tremblay
Michael K. Ciolek
Michael L. Toney
Thomas J. Geyer
John Hosenfeld
Phone Number
(715) 258-6629
(812)547-0700
(919)541-4921
(919)541-5247
(919)851-8181
Ext 3 120
(816)753-7600
Ext 1336
1-5
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2.0 PROCESS AND CONTROL EQUIPMENT OPERATION
The material in Section 2 was prepared by Research Triangle Institute and provided to
MRI by the EMC. It was included in the report without MRI review.
2.1 INTRODUCTION
The Waupaca foundry in Tell City, Indiana, is a completely new grey iron foundry that
started operation in February 1997. The foundry casts a diverse group of products, including
brake drums, shoes, rotors, calipers, and other parts. The plant operates one large cupola that
melts at a rate of about 60 tons/hr (tph), and operates four pouring lines. This section of the test
report provides a description of the cupola operation for iron melting, and the casting operation,
including pouring, cooling, and shake out.
2.2 PROCESS DESCRIPTION
2.2.1 Iron Melting in Cupolas
The Waupaca foundry in Tell City operates a large, water-cooled cupola that melts at a
rate of approximately 60 tph, with a blast rate of 10,000 to 15,000 standard cubic feet per
minute (scfm), which makes it a large cupola by U.S. industry standards. Figure 2-1 is a
simplified schematic of the cupola gas handling system and emission control equipment.
The cupola is charged with metal scrap, re-melt, coke, and limestone at the top of the
cupola, using one of two automated skip buckets. The level of metal within the cupola is
monitored, and the charge material in the skip bucket is dumped into the cupola when the level of
charge falls below a set level. The seal from the charge material and a draft on the cupola
prevent gases from escaping. If, for any reason, the charge material cannot be added to the
cupola within 5 minutes (min) of the level falling below the set point, the cupola will
automatically go "off blast" until the appropriate charge level in the cupola can be achieved.
The blast air is preheated to about 1,000°F in the blast air recuperator and is introduced
into the bottom of the cupola through 8 tuyeres. The blast is also enriched with oxygen under
certain melting conditions. The off gas from the cupola is removed at 250-300°F. The off-take
duct is lined with refractory material and leads to a coarse grain separator where heavy particles
are removed. The separator is cooled with non-contact water.
2-1
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Charge
(3) Oil heat exchangers
Exhaust Stack
Combustion
Chamber
CUPOLA
Solids Removed
Combustion Air
Exhaust fan
Figure 2-1. Simplified schematic of cupola gas handling system.
After removal of the heavy particles, the gas enters a large combustion chamber where
combustion air is introduced and the CO is burned. Two burners are used when necessary to
maintain the combustion temperature. The gas leaves the combustion chamber at approximately
1650°F, and enters a dropout chamber where additional heavy particles are removed. The hot
gas then passes through an air-to-air heat exchanger (blast air recuperator), followed by a series
of three oil heat exchangers that are used to cool the air. These oil heat exchangers are not
currently used for heat recovery. (Modifications may be made in the future to recover and use
the heat, such as for heating the building.)
The gas from the heat exchangers is injected with a dry mixture (mostly calcium
carbonate and magnesium oxide) in a venturi mixer that increases the gas velocity and suspends
the injected particles. Dry injection is used to improve pollutant removal in the baghouse.
2-2
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During the source test, the dry powder injection was turned off to afford better characterization of
uncontrolled emissions and baghouse efficiency for HAP constituents. The gas is then sent to a
10 module, negative pressure baghouse that uses a high temperature fabric designed to withstand
temperatures of up to 320°F. The temperature of the gas at this point is typically 280 to 290°F.
A fan pulls the gas through the system and discharges the cleaned gases through a stack.
The pressure drop across the baghouse is monitored, and when the pressure drop
increases to 6 inches (in.) of water, individual bag house compartments are cycled off-line, the
bags are cleaned with a pulses of air, then the compartments are brought back on-line. The
baghouse uses plenum pulsing. During testing, each compartment was off line for approximately
8 min for cleaning, with cleaning pulses occurring approximately every 30 seconds (sec) during
this interval.
The plant routinely monitors several parameters associated with the cupola, including
blast air and oxygen rate, and afterburner air addition rates, as well as temperature at various
points in the process. The combined air flow rate through the recuperator and the baghouse
system is not directly monitored, but can be estimated from the blast air, oxygen and afterburner
air addition rates. During testing, the combined flow rate of offgas was also measured by the test
crew at the final stack sampling location. The plant also records the amount of each type of
material added to the cupola by the automatic skip buckets for each charge load. The
composition of a typical charge is given in Table 2-1 and contains approximately 4 tons of iron.
The iron includes remelt from the foundry, steel scrap, and pig iron.
TABLE 2-1. TYPICAL CUPOLA CHARGE MATERIALS
Material
Remelt from foundry
Steel scrap
Pig ironb
Silicon bricks
Blend bricks (Si, Mn, Cr)
Silicon carbide
Coke
Limestone
Typical range (lbs/charge)a
3,500 to 4,500
3,200 to 4,000
600 to 1,400
70 to 105
260 to 300
2 10 to 250
500 to 900
280 to 300
f* Typical range observed during the test days.
Remelt, steel scrap, and gray iron bricks are the sources of iron and total 8,700 Ibs (4.35 tons) per charge.
2-3
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2-2.2 Pouring, Cooling and Shakeout
The plant has four lines for pouring, cooling, and shakeout. Silica sand, bentonite, and
seacoal constitute the molding sand, which is recycled about 50 times prior to disposal in a
monofill. Resins and a catalyst are used to produce warmbox cores. Some of the company's cast
products use cores, and others do not. During the source test, cores were not being used on any
of the lines. The lines are all similar except that Line 4, which is designed to handle larger
molds, has an automatic pouring station and the other lines do not. Line 4 is typically used for
casting the larger size parts.
Pouring emissions are not captured at any of the four pouring stations. Cooling emissions
are captured by hoods that cover the entire cooling line prior to shakeout. The shakeout
operation is totally enclosed and evacuated to capture the emissions. After shakeout, the parts
are transferred to a casting cooling house where they are placed on a metal "tree." The parts then
proceed to a "spinner house" and are shot blasted to remove residual sand. The spinner house is
also evacuated to the duct that removes emissions from shakeout. The captured emissions from
shakeout and cooling are sent to a baghouse for gas cleaning. There are three baghouse systems;
each system predominantly receives emissions vented from a single line, but a few of the vents
from a given line are routed to another line's baghouse system. Consequently, controlled
emissions represent contributions from multiple lines and multiple processes.
The ductwork for the cooling lines are interconnected with either other cooling lines or
shakeout enclosure ductwork. Therefore, it is impossible to get a representative sample for
cooling emissions that could be attributed to an entire cooling line. The least amount of
interconnection was on Line 4, so it was selected for emissions testing. The first third of the
cooling section of Line 4 was ducted to a single vent that had a long, straight vertical section
before connecting with other ductwork. Ports were installed in this straight section of the vent,
so that the uncontrolled emissions from the first third (approximately 20-25 min) of the cooling
line could be measured. The shakeout enclosure ductwork has a short vertical rise, then elbows
to a horizontal section where it is tied to the vent from the spinner housing and the last hood from
the cooling line. Ports were installed in the short vertical duct from the shakeout enclosure
approximately one foot (ft) above the roof of the enclosure prior to the point where the ducts
from the spinner house and the end of the cooling line join the shakeout enclosure duct. This
point represents uncontrolled emissions from the shakeout operations.
2-4
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2.3 SUMMARY OF PROCESS OPERATING DATA COLLECTED DURING SOURCE TEST
2.3.1 Process Operating Data for Cupola Melting Operations
Testing of the melting operations was conducted over a three-day period. Single test runs
were performed on September 8th and 9th, and two runs were performed on September 10th.
During testing, process information was collected from the operating room's computer control
panel. Process information collected included cupola charging data, process chemistry, gas flow
rates, temperatures, baghouse pressure drop, and cupola stack opacity.
Table 2-2 and Figure 2-2 present metal charging rates for the cupola during the three days
of testing. Table 2-2 and Figure 2-2 show that the average metal production rate for
September 8th was higher than on the 9 or 10 . Table 2-2 and Figure 2-2 also show that hourly
production rates varied significantly within a given day.
2-5
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TABLE 2-2. SUMMARY OF CUPOLA CHARGING DURING THE TEST DAYS
9/08/97
Time period
11:02-11:57
12:00-12:54
13:00-13:58
14:03-14:55
15:00-15:57
Average rate
(tons/hr)
Tons
charged
45
56
59
51
55
53.2
9/09/97
Time period
8:01-8:56
9:01-9:56
10:02-10:46
11:03-11:50
12:00-12:51
13:00-13:56
14:06-14:55
Average rate (tons/hr)
Tons
charged
47
52
42
35
26
58
30
41.4
9/10/97
Time period
7:01-7:56
8:03-8:54
9:01-9:59
10:04-10:55
11:01-11:57
, 12:03-12:59
13:03-13:41
14:02-14:58
15:01-15:28
16:13-16:56
17:00-17:56
18:01-18:57
19:02-19:58
Average rate
(tons/hr)
Tons
charged
48
35
49
47
54
59
40
' 35
32
45
51
56
55
46.6
2-6
-------
to
• 8-Sep H9-Sep DIG-Sep
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~ 30
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E
•c 20
3
O
10
0 -
)
--J
8
oo
o
o
H —
CD
8
cb
CD
o
H —
=
-
CO
8
o
8
=
o
8
6
o
-tJ
mm
8
NJ
-------
Table 2-3 presents average gas flow rates and temperatures for several locations in the
cupola flue gas system on September 8th, 9th, and 10th. As can be seen from Table 2-3, the
average blast rate was lowest on September 9th, and the cupola typically operated with oxygen
addition on that day. On September 8th and 10th, the average blast rate was higher, and oxygen
addition was not used. The average baghouse pressure drop was lower on September 9th than on
September 8th or 10th, (2.8 in. of water versus 4.4 in. of water), and the average opacity was
higher on September 9th than September 10th (5.7 percent versus 2.8 percent).
TABLE 2-3. PROCESS DATA DURING THE DAYS OF CUPOLA TESTING
Process Parameter
Average Value on Testing Date
September 8
September 9
September 10
Cupola process air flow information
Blast rate (scfm)
Oxygen addition (on/off)
Temperature in (F)
Temperature out (F)
14,794
off
1,156
330
9,131
on
1,067
232
13,665
off
1,101
297
Afterburner air flow information
Primary air (scfm)
Secondary air (scfm)
Cooling air (scfm)
Temperature out (F)
5,271
5,893
2,794
1,717
2,764
2,823
2,300
1,639
4,969
5,476
2,792
1,668
Baghouse information
Temperature in (F)
Pressure drop (inches H2O)
Opacity (%)
297
4.4
Not Recorded
281
2.8
5.7t
299
4.4
2.81"
^Average of opacity readouts recorded every 15 minutes; opacity readouts are 6-minute averages from KVB EPA-2
stack mounted opacity monitor.
Continuous records of blast air flow rates are presented in Figure 2-3. Blast air rates were
significantly reduced (i.e., the cupola was placed "on relief) for varying lengths of time on
September 9th and 10th. The specific times when the cupola was on relief are listed in Table 2-4.
2-8
-------
TABLE 2-4, PERIODS WHEN CUPOLA WAS "ON RELIEF" DURING TESTING
September 8
Continuous blast.
September 9
10:54-11:09
September 10
13:51 - 14:04
14:11-14:28
15:27 - 16:03
16:06 - 16:08
Table 2-5 presents average process iron chemistry values (from cupola) for September 9th
and 10 . Although process chemistry values were not recorded on September 8 , average trace
metal impurity levels were typical on all three days.
2-9
-------
18000
16000
8-September
- - - 9-September
10-September
2000
6:00 7:00 8:00 9:00 10:00 11:00 12:00 13:00 14:00 15:00 16:00 17:00 18:00 19:00 20:00 21:00 22:00 23:00 0:00
Clock time (hours:minutes)
FIGURE 3-3. BLAST AIR FLOW RATE THROUGH CUPOLA.
Figure 2-3. Blast air flow rate through cupola.
-------
TABLE 2-5. PROCESS IRON CHEMISTRY AT CUPOLAa
Element
ElCe
(Elemental Carbon Equivalents)
CalcC
(Calculated Carbon)
Si
Mn
P
S
Ni
Mo
Cr
Cu
Al
Ti
Sn
Mg
V
Pb
Concentration (%)
September 9
3,665
2.470
1.050
0.350
0.055
0.070
0.045
0.105
0.205
0.114
0.008
0.009
0.005
0.006
0.006
0.001
September 10
4.045
3.450
4.490
0.595
0.042
0.090
0.090
0.025
0.240
0.230
0.009
0.011
0.009
0.001
0.011
0.002
a The process chemistry values reported here are considered typical; the process chemistry values were not
specifically recorded on September 8, but were also considered typical.
2.3.2 Process Operating Data for Pouring, Cooling and Shakeout Operations
Emissions from cooling (first third section) and shakeout were measured on
September 5,1997. Line 4 employs an automated molding machine. Testing was conducted
only when the entire mold line was filled with recently poured molds. During the day of the
source test of the cooling and shakeout operations, Line 4 was used to cast brake drums. Each
mold produced two brake drums, and used 189 pounds (Ib) of poured metal. For the test day,
249 molds per operating hour were produced. Each mold contains 1393 Ib of green sand (lake
sand, sea coal, and bentonite), so the molds had a sand to metal ratio of 7.35:1.
The properties of the molding sand measured during the test day are given in Table 2-6.
A bonding agent was added to the sand in the amount of 38.1 Ib of bond per ton of sand mulled.
2-11
-------
The bonding agent is a dry mixture of coal, brittle asphalt, cellulose, bentonite, starch, and cereal.
The material safety data sheet for the product indicates no volatile components, and no hazardous
ingredients other than coal dust and crystalline quartz.
TABLE 2-6. TYPICAL RESULTS FROM GREEN SAND ANALYSIS
Property
Moisture (%)
Clay (%)
Loss on ignition (%, at 1800T)
Volatile content (%, at 900 °F)
Value
3.5
8.7
7.8
4.0
2-12
-------
3.0 TEST LOCATIONS AND GAS COMPOSITION
Figure 3-1 is a schematic showing an overview of the cupola gas handling system that
presents the locations of both cupola test points. The baghouse inlet (location "A") and the outlet
stack (location "B") were sampled concurrently.
Figure 3-2 is a schematic showing a closer view of the cupola test locations. Location
"A" was at the duct leading to the baghouse, and location "B" was at the exhaust stack following
the baghouse.
Figure 3-3 is a schematic with a view of test locations at the mold cooling and mold
shake-out housing. The sample location of the mold cooling line was the collector duct for the
first several cooling line vents. The shake-out housing was sampled at the duct drawing from the
enclosure.
3,1 BAGHOUSE OUTLET - STACK
The test ports on the stack are located at about 70 ft above ground level. Access to the
stack ports is at roof level, which can be reached by a ladder on the baghouse. Test ports on the
7 ft 9 in.-diameter stack allowed for concurrent FTIR and manual sampling.
3.2 BAGHOUSE INLET DUCT
The test ports on the inlet duct are located at roof level about 70 ft above the ground.
Ports allowed simultaneous testing by both FTTR and manual methods. The baghouse inlet and
outlet were sampled by FTIR concurrently using a dual line extractive sampling system.
3.3 MOLD COOLING LINE
Two ports were utilized on the vertical duct that collects the emissions from the first
seven take-off vents over the cooling line conveyer following the pouring station. That
vertically-oriented duct is inside the main facility. Sampling was conducted at a height of
approximately 30 ft above the facility floor to obtain volumetric flow, diluent, moisture, and
FTIR data across the diameter of the duct interior. A dual-line system was used to conduct
concurrent testing at the mold cooling line and shake-out housing.
3-1
-------
Charge Movable
I cap
Oil heat exchangers
Cupola
Exhaust
stack
Air-Air heat exchanger
Combustion
chamber
Heated
blast air
m Dry
injection
(Baghouse
inlet)
Blast air
Baghouse
Solids
removed
Cupola blower
Combustion air
B
(Baghouse
outlet)
O
U Ports
Roof
\
Exhaust fan
Figure 3-1. Schematic of cupola gas handling system, sampling points A and B.
-------
U)
i
U)
Sample Point B
Exhaust stack
(Baghouse outlet)
(4 ft. height)
3 in. ports ~~~
From other
heat exchangers
I
I
I
t
Oil heat
exchanger
Roof
I
I
I
I
Discharge
'///////7X
From baghouse
Sample Point A
(Baghouse inlet) To baghouse
t
Dry injection
Roof
~ 56 in. O.D., slight curvature
980075-02
Figure 3-2. Schematic of baghouse inlet and baghouse outlet. Sampling points A and B, respectively.
-------
Combines with
other ducts
c
(Mold
cooling
line)
XX XX X
Mold cooling
flow
Shakeout
housing
Spinner house
Mold cooling line
Figure 3-3. Schematic of mold cooling and mold shake-out gas handling system; sampling points C and D.
960075-03
-------
3.4 MOLD SHAKE-OUT HOUSING
The mold shake-out housing and its ducting system are located inside the main facility.
Two 3-in. test ports were installed and utilized on the vertical portion of the duct. At a height of
approximately 25 ft above the facility floor, sampling was conducted to obtain volumetric flow,
diluent, moisture, and FTIR data across the diameter of the duct interior.
3.5 VOLUMETRIC FLOW
Table 3-1 summarizes the gas composition and flow data for the mold cooling and mold
shake-out housing. Measurements for velocity, flow, and oxygen and carbon dioxide
concentrations were conducted and calculated following EPA Test Methods 1, 2, and 3B
referenced in 40 CFR Part 60, Appendix A. Moisture content of the stack gas was calculated
using wet bulb/dry bulb measurements. Records of volumetric flow data are located in
Appendix A.
Table 3-2 summarizes the gas composition and flow data provided by PES for the cupola
test locations. As part of their manual testing, PES provided volumetric flow rates, moisture
content, gas molecular weight, etc.; therefore, MRI did not conduct these tests.
TABLE 3-1. FLOW DATA AT WAPAUCA MOLD COOLING AND
SHAKE-OUT HOUSING PROCESSES3
Location
Date
Carbon Dioxide, %
Oxygen, %
Moisture Content, %
Gas Stream Velocity, fps
Volumetric Flow Rate, dscfm
Volumetric Flow Rate, dscmm
Stack diameter, in.
Stack area, ft2
Mold Cooling Line
OS-Sep-97
0.0
20.9
2.6
57.6
19,399
549.0
34.25
6.4
Shake-out Housing
05-Sep-97
0.0
20.9
5.4
81.1
26,576
753
34.25
6.4
Flow data uncorrected for Absolute Pressure - This permits a variance of +1-1% in volumetric flow.
3-5
-------
TABLE 3-2. CUPOLA BAGHOUSE INLET AND OUTLET GAS COMPOSITION
AND FLOW SUMMARIES
Cupola Test Data3
Run Number
Date
1
09-Sep-97
2
10-Sep-97
3
10-Sep-97
Baghouse Inlet
Oxygen, %
Carbon Dioxide, %
Moisture Content, %
Volumetric Flow Rate, dscfm
Volumetric Flow Rate, dscmm
10.9
10.8
2.5
26,800
759
9.5
11.6
2.8
38,200
1,080
8.8
12.4
2.4
38,500
1,090
Baghouse Outlet (Stack)
Oxygen, %
Carbon Dioxide, %
Moisture Content, %
Volumetric Flow Rate, dscfm
Volumetric Flow Rate, dscmm
12.7
8.8
4.1
33,967
962
11.0
10.1
2.6
48,700
1,380
11.0
10.0
2.6
48,933
1,383
1 Data provided by PES.
3-6
-------
4.0 RESULTS
4.1 TEST SCHEDULE
The testing at Waupaca Foundry, Plant No. 5 was completed from September 5 to
September 10, 1997. Table 4-1 summarizes the sampling schedule. A complete record of all
FTIR sampling is in Appendix B. The FTIR sampling at the cupola locations was coordinated
with the manual sampling conducted by PES. The FTIR sampling at the mold cooling line and
the mold shake-out housing were conducted independently.
TABLE 4-1. TEST SCHEDULE AT WAUPACA FOUNDRY
Date
9/4/97
9/5/97
9/6/97
9/8/97
9/9/97
9/10/97
Task
Arrive on site and set up at mold cooling and shake-out.
Mold cooling and shake-out test run w/ FTIR.
15:23-19:11
Relocation to cupola testing area
Complete setup at cupola. Test Run 1 w/ FTIR.
12:56-17:05
Test Run 2. FTIR in conjunction with manual methods
by PES.
9:25-13:56
Test Run 3. FTIR in conjunction with manual methods
by PES.
8:15-12:33
Pack equipment and depart site
Location a
Mold cooling ("C") and
Shake-out ("D")
Baghouse
inlet ("A") and outlet ("B")
at Cupola
a Location descriptions are in Section 3.
4.2 FIELD TEST PROBLEMS AND CHANGES
The cupola gas at Waupaca contained high concentrations of both water vapor and
(carbon dioxide) CO2 with respect to other compounds. Analyte spiking for quality assurance
was conducted using toluene and formaldehyde vapor. The CO2 spectrum interfered with the
strongest toluene infrared band near 730 cm"1 so the weaker toluene absorbance, in the analytical
region 2,850-3,100 cm"1 range, was used for the analysis. The presence of other aliphatic
hydrocarbon species also contributed to the total infrared absorbance in this 2,850-3,100 cm"
region.
,-1
4-1
-------
The analyte spiking for the inlet sample system was introduced into the sample line at the
junction 50 ft downstream of the probe before and after Run 1 at the cupola. The plumbing was
modified for Run 2 and Run 3 to allow introduction of the spiking analyte at the inlet probe.
4.3 FTIR RESULTS
The FTIR results and the mass emissions are summarized in Tables 1-1 and 1-2. The
complete FTIR concentration results are presented in Appendix B in Tables B-l to B-4.
4.3.1 Mold Cooling Line and Shake-out Housing
The FTIR results at the cooling and shake-out housing ducts are summarized in
Table 1-1. The complete results for all of the samples from these locations are presented in
Tables B-l and B-2. The compounds detected consisted primarily of light hydrocarbon species
methane and ethylene. Some higher molecular weight hydrocarbon species were also detected.
In the draft report, the heavier hydrocarbons were reported as hexane. The revised analysis of the
cooling and shakeout spectra included reference spectra of additional hydrocarbon compounds.
The additional reference spectra were measured in the laboratory by MRL Additional
explanation of these spectra is provided in Section 1.2. Reference spectrum documentation is
provided in Appendix B.
Both toluene and formaldehyde were included in the analysis because some samples were
spiked with each of these compounds. Formaldehyde was not detected in the unspiked samples.
Toluene was detected in unspiked samples at the cooling and shake-out locations, but the
uncertainties were relatively high (Table 1-1).
4.3.2 Baghouse Inlet and Outlet
The emissions were similar at both locations and are summarized in Table 1-2. The
complete concentration results are in Tables B-3 and B-4. The samples contained moisture, CO2,
hydrogen chloride (HC1), and methane. Some samples were spiked with either toluene or
formaldehyde, but neither toluene nor formaldehyde was detected in any of the unspiked
samples.
4.4 ANALYTE SPIKE RESULTS
The revised cooling and shakeout spike results are slightly different from the draft report
results due to the effect of using the additional hydrocarbon reference spectra. A permeation tube
saturated with paraformaldehyde was heated to produce a vapor of the formaldehyde monomer.
A steady state concentration of formaldehyde vapor was maintained with a temperature controller
4-2
-------
set at 100°C and with a controlled flow of carrier gas. During spiking the carrier gas was
4.01 ppm SF6 in nitrogen.
The inlet and outlet locations were also spiked with toluene from a cylinder standard of
60 ppm toluene in nitrogen (Scott Specialty Gases, ± 2 percent). The toluene spike flow passed
through a mass flow meter and into the spike line where it was preheated before injection into the
sample at the back of the sample probe. Section 5.3 gives additional description of the analyte
spike QA procedure.
The formaldehyde spike results for the cooling and shake-out locations are presented in
Tables 4-2 and 4-3. The toluene spike results for the cooling and shake-out are summarized in
Tables 4-4 and 4-5. The formaldehyde spike results at the inlet and outlet are summarized in
Tables 4-6 and 4-7. The toluene spike results at the baghouse inlet and outlet are summarized in
Tables 4-8 and 4-9. The toluene and formaldehyde spike standards were quantitatively mixed
before the spike mixture was introduced to the sample stream. The analytical results for each
spiked analyte are presented separately. Section 5.3 gives a discussion of the procedure for
determining the analyte standard concentrations in the spike mixtures. The spike standard
concentrations are presented in Table 5-2. The spiked sample spectrum file names are identified
in Tables 4-2 to 4-9. These correspond to the sample file names in Section 5.3, where the
formaldehyde and toluene spike standard concentrations are given for each spike mixture.
Table 4-10 compares measured band areas of the EPA toluene reference spectra
(deresolved to 2.0 cm ) and spectra of samples taken directly from the 60 ppm toluene cylinder
standard. The cylinder standard spectrum was measured at the Waupaca test site. The band area
comparison differs from the comparison of the certified concentrations by about 35 percent. For
a given concentration, (ppm-M)/K, the infrared absorbance in the cylinder standard spectra is
about 35 percent greater than the absorbance in the EPA library spectra. Therefore, the library
spectra calculate a toluene concentration that is 35 percent lower than that calculated using the
cylinder standard spectra. Tables 4-4,4-5, 4-8, and 4-9 present the toluene spike recoveries
using both the library spectra and the cylinder standard spectra.
A similar effect was observed in some other field tests using another toluene cylinder
standard. One possibility is that there was a systematic error in the original toluene library
reference spectra. This could be assessed by evaluating several toluene gas standards from
different sources and doing a comparison similar to that shown in Table 4-10.
4-3
-------
The above observation is compound specific, and the information in Table 4-10 does not
apply to the measurements of other analytes. The deresolved calibration transfer standard (CTS)
spectra give a path length result that is consistent with the observed number of laser passes and
the instrument resolution. The disagreement is also not related to the deresolution of the toluene
spectra because the band areas in the original 0.25 cm"1 toluene spectra are nearly equal to the
band areas in the deresolved 2.0 cm1 versions of these spectra.
4-4
-------
TABLE 4-2. FORMALDEHYDE SPIKE RESULTS FROM THE MOLD COOLING PROCESS
Files
CoosplOl, 102,
CoosplO?
Average Formaldehyde Concentration
spike unspike (calc)
12.5 0.0 12.5
12.8 0.0 12.8
Average SF6 Concentration
spike unspike (calc)
0.442 0.000 0.442
0.545 0.000 0.544
DF Cexp A % Recovery
4.7 13.2 -0.6 95.0
3.8 16.2 -3.5 79.0
Calc is equal to the difference, spike - unspike for the analyte or for SF^. Cexp is the calculated formaldehyde concentration at 100 percent recovery in the
spiked samples. DF is the dilution factor calculated from the SF^ concentration. A is equal to Cexp - formaldehyde(calc).
TABLE 4-3. FORMALDEHYDE SPIKE RESULTS FROM THE WAUPACA SHAKE-OUT HOUSING PROCESS
Files
ShksplOl, 102
Shkspl07
Average Formaldehyde Concentration
spike unspike (calc)
14.7 0.0 14.7
18.7 0.0 18.7
Average SF6 Concentration
spike unspike SF6 (calc)
0.472 0.000 0.472
0.605 0.000 0.605
DF Cexp A % Recovery
4.4 14.0 0.6 104.6
3.5 18.0 0.7 103.8
Calc is equal to the difference, spike - unspike for the analyte or for SFg. Cexp is the calculated formaldehyde concentration at 100 percent recovery in the
spiked samples. DF is the dilution factor calculated from the SFg concentration. A is equal to Cexp — formaldehyde(calc).
-------
TABLE 4-4. TOLUENE SPIKE RESULTS FROM THE MOLD COOLING PROCESS
Files
coosplOl, 102
coosplO?
Average Toluene Concentration
spike unspike (calc)
20.4 18.9 1.5
16.5 16.4 0.1
Average SF6 Concentration
spike unspike (calcj^
0.442 0.000 0.442
0.545 0.000 0.545
DF Cexp A % Recovery
4.7 8.4 -6.9 17.6
3.0 10.4 -10.3 0.7
%Ra
11.3
0.45
Calc is equal to the difference, spike - unspike for the analyte or for SF^. Cexp is the calculated toluene concentration at 100 percent recovery in the spiked
samples. DF is the dilution factor calculated from the SFg concentration. A is equal to Cexp - toluene(calc). The toluene % recoveries were obtained using
EPA reference spectra of toluene.
a %R is the calculated percent recovery obtained if the spectra of the 60 ppm toluene cylinder standard are used in the analysis (see Table 4-10).
TABLE 4-5. TOLUENE SPIKE RESULTS FROM THE SHAKE-OUT HOUSING PROCESS
Files
shksplOl, 102
shksplO?
Average Toluene Concentration
spike unspike (calc)
11.3 0 11.3
9.3 0 9.3
Average SF6 Concentration
spike unspike (calc)
0.472 0.000 0.472
0.605 0.000 0.605
DF Cexp A % Recovery
4.4 9.0 2.3 125.7
•3.5 11.5 -2.2 80.7
%Ra
81.0
52.0
ON
Calc is equal to the difference, spike - unspike for the analyte or for SF^. Cexp is the calculated toluene concentration at 100 percent recovery in the spiked
samples, DF is the dilution factor calculated from the SF^ concentration. A is equal to the difference Cexp - toluene(calc). The toluene % recoveries were
obtained using EPA reference spectra of toluene.
a %R is the calculated percent recovery obtained if the spectra of the 60 ppm toluene cylinder standard are used in the analysis (see Table 4-10).
-------
TABLE 4-6. SUMMARY OF FORMALDEHYDE SPIKE RESULTS AT THE CUPOLA BAGHOUSE INLET
Files
insplOl, 102
inspllV
insp201
insp205
inspSOl
insp312
Average Formaldehyde Concentration
Date spike unspike (calc)
9/8/97 17.5 0.0 17.5
14.6 . 0.0 14.6
9/9/97 16.4 0.0 16.4
17.3 0.0 17.3
9/10/9 16.2 0.0 16.2
31.9 0.0 31.9
Average SF6 Concentration
spike unspike (calc)
0.561 0.000 0.561
0.484 0.000 0.484
1.175 0.000 1.175
0.619 0.000 0.619
0.595 0.000 0.595
1.141 0.000 1.141
DF Cexp A % Recovery
3.9 12.8 -4.7 137
3.0 11.4 3.2 128
3.3 13.2 3.2 124
3.3 13.2 4.1 131
3.5 12.4 3.9 131
2.8 26.7 5.2 120
Calc is equal to the difference, spike - unspike for the analyte or for SFg. Cexp is the calculated formaldehyde concentration at 100 percent recovery in the
spiked samples. DF is the dilution factor calculated from the SFg concentration. A is equal to Cexp - formaldehyde(calc).
TABLE 4-7. SUMMARY OF FORMALDEHYDE SPIKE RESULTS AT THE CUPOLA BAGHOUSE OUTLET
Files
outsplOl
outsplll
outsp201
outsp208
outsp301
outsp316
Average Formaldehyde Concentration
Date spike unspike (calc)
9/8/97
9/9/97
9/10/9
9/10/9
15.0 0.0 15.0
12.9 0.0 12.9
13.4 0.0 13.4
14.1 0.0 14.1
14.0 0.0 14.0
25.7 0.0 25.7
Average SF6 Concentration
spike unspike (calc)
0.450 0.000 0.450
0.465 0.000 0.465
0.923 0.000 0.923
0.497 0.000 0.497
0.504 0.000 0.504
0.904 0.000 0.904
DF Cexp A % Recovery
4.9 10.3 4.7 145
3.2 11.0 2.0 118
4.2 10.3 3.0 129
4.0 10.6 3.5 133
4.3 9.9 4.0 141
2.4 31.2 -5.4 83
Calc is equal to the difference, spike - unspike for the analyte or for SFg. Cexp is the calculated formaldehyde concentration at 100 percent recovery in the
spiked samples. DF is the dilution factor calculated from the SFg concentration. A is equal to Cexp - formaldehyde(calc).
-------
TABLE 4-8. SUMMARY OF TOLUENE SPIKE RESULTS AT THE CUPOLA BAGHOUSE INLET
Files
insplOl,
InspllV
insp205
inspSOl
Average Toluene Concentration
Date spike unspike (calc)
9/8/97
9/9/97
9/10/9
10.5 0.0 10.5
24.4 0.0 24.4
14.2 0.0 14.2
12.5 0.0 12.5
Average SF6 Concentration
spike unspike (calc)
0.561 0.000 0.561
0.484 0.000 0.484
0.619 0.000 0.619
0.595 0.000 0.595
DF Cexp A %Recovery
3.9 7.6 2.9 138.3
3.0 17.4 7.0 140.3
3.3 9.8 4.4 144.8
3.5 7.9 4.6 157.9
%Ra
88.8
90.0
92.9
101.3
Calc is equal to the difference, spike - unspike for the analyte or for SF^. Cexp is the calculated toluene concentration at 100 percent recovery in the spiked
samples. DF is the dilution factor calculated from the SFg concentration. A is equal to the difference Cexp - toluene(calc). The toluene % recoveries were
obtained using EPA reference spectra of toluene.
a %R is the calculated percent recovery obtained if the spectra of the 60 ppm toluene cylinder standard are used in the analysis (see Table 4-10).
TABLE 4-9. SUMMARY OF TOLUENE SPIKE RESULTS AT THE CUPOLA BAGHOUSE OUTLET
Files
outsplOl
outsplll
outsp301
Average Toluene Concentration
Date spike unspike (calc)
9/8/97
9/9/97
9/10/9
7.6 0.0 7.6
21.2 0.0 21.2
10.0 0.0 10.0
Average SF6 Concentration
spike unspike (calc)
0.450 0.000 0.450
0.465 0.000 0.465
0.504 0.000 0.504
DF Cexp A % Recovery
4.9 6.1 1.5 124.5
3.2 16.7 4.5 126.9
4.3 6.3 3.6 157.4
%Ra
79.9
81.4
101.0
oo
Calc is equal to the difference, spike - unspike for the analyte or for SF^. Cexp is the calculated toluene concentration at 100 percent recovery in the spiked
samples. DF is the dilution factor calculated from the SFg concentration. A is equal to the difference Cexp — toluene(calc). The toluene % recoveries were
obtained using EPA reference spectra of toluene.
a %R is the calculated percent recovery obtained if the spectra of the 60 ppm toluene cylinder standard are used in the analysis (see Table 4-10).
-------
TABLE 4-10. COMPARISON OF FTIR SPECTRA OF SAMPLES FROM TOLUENE (60 ppm) CYLINDER
TO EPA TOLUENE REFERENCE SPECTRA3
Toluene
Spectra
153a4ara (2cm- 1)
153a4arc (2cm-l)
to!0905a
to!0905b
to!0909ab
Source
EPA
library
EPA
library
Waupaca
Waupaca
Waupaca
Band
Area
23.4
4.3
10.2
10.1
10.5
Region (cm )
3160.8-2650.1
3160.8-2650.1
Spectra comparison
based on band areas
Ratio (Ra)b
5.4
1.0
2.4
2.3
2.4
1/Ra
0.184
1.000
0.423
0.427
0.411
Comparison of spectra based on
standard concentrations
(ppm-m)/K
4.94
1.04
1.58
1.58
1.58
Ratio (Rc)c
4.8
1.0
1.5
1.5
1.5
1/Rc
0.210
1.000
0.655
0.655
0.655
aThe relevant comparison is Rc/Ra for to!0905a,b and to!0909ab, which is about 65 percent.
bRatio of band area to band area of 153a4arc.
cRatio of concentration to concentration of 153a4arc.
-------
-------
5.0 TEST PROCEDURES
The procedures followed in this field test are described in the EPA Method 320 for using
FTIR spectroscopy to measure HAP's and the EPA Protocol for extractive FTIR testing at
industrial point sources. 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, and
analyze the spectra for compounds not in the EPA library. Concentrations are reported for
compounds that could be measured with FTIR reference spectra. Additionally, manual
measurements of gas temperature, gas velocities, moisture, CC>2, and O2 were used to calculate
the mass emissions rates. MRI collected data for the mold cooling and the shake-out lines, and
PES collected the data at the baghouse inlet and outlet.
5.1 SAMPLING SYSTEM DESCRIPTION
A schematic of the extractive sampling and spiking system is shown in Figure 5-1.
5.1.1 Sample System Components
The sampling system consists of three separate components:
• two sample probe assemblies
• two sample lines and pumps
• a gas distribution manifold cart.
All wetted surfaces of the system are made of unreactive materials, Teflon®, stainless
steel, or glass and are maintained at temperatures at or above 300° F to prevent condensation.
The sample probe assembly consists of the sample probe, a pre-filter, a primary
paniculate filter, and an electronically actuated spike valve. The sample probe is a standard
heated probe assembly with a pitot tube and thermocouple. The pre-filter is a threaded piece of
tubing loaded with glass wool attached to the end of sample probe. The primary filter is a
Balston paniculate filter with a 99 percent removal efficiency at 0.1 f^m. The actuated spike
valve is controlled by a radio transmitter connected to a switch on the sample manifold cart. All
sample probe assembly components are attached to or enclosed in an insulated metal box.
The sample lines are standard heated sample lines with three % in. Teflon tubes in 10, 25,
50, and 100 ft lengths. The pumps are heated, single-headed diaphragm pumps manufactured by
either KNF Neuberger or Air Dimensions. These pumps can sample at rates up to 20 liters per
minute (Lpm) depending on the pressure drop created by the components installed upstream.
5-1
-------
Data Storage & Analysis FTIR Spectrometer Heated Cell
Heated Probe #1
Heated Probe #2
Vent
^UsUx
9^
t
in
Vent
A
Flow Meter
>
Vent
A
IjFlow Meter
d
Flow Meter
Calibration
Spike UM
Secondary PM Filter
Heated Manifold Box
Gas/
20ft. of heated line
Calibration Standards
Heated Probe Box #1
3-Way Valve
Iston® Filter
Bundles are 50-300-*- ft. long.
Sample Una
Calibration Gas / Spike Line
fgiJ
Heated Probe BOK #2
3-WayVahre
Balaton® Fitter
Sample Transfer Line (Heated Bundle) #1
Bundles are 50-300+ ft. long.
Heated
Pump #1
Sample Line
Calibration Gas / Spike Line
20 ft. of heated line
Unheated line
Heated Pump #2
MFM - Mass Flow Meter
Sample Transfer Line (Heated Bundle) #2
Figure 5-1. Sampling system schematic.
-------
The gas distribution manifold was constructed for FTIR sampling by MRI. It is built onto
a cart that can be operated inside the MRI mobile lab or in an alternate location, if necessary.
The manifold consists of a secondary particulate filter, control valves, rotameters, back pressure
regulators and gauges, and a mass flow controller. The manifold can control two sample gas
stream inputs, and eight calibration gases; it has three individual outputs for analyzers. The cart
also contains a computer work station and controls for the spike valves and mass flow controller.
5.1.2 Sample Gas Stream Flow
Exhaust gas was withdrawn through the sample probe and transported to the gas
distribution manifold. The mold cooling and shake-out processes were each sampled alternately
with the two gas handling systems during a single run. The baghouse inlet and outlet were
sampled alternately over three runs. Inside the manifold the gas passed through separate.
secondary particulate filters. Downstream of the secondary filters, a portion of either gas stream
could be directed to the FTIR gas cell. The remainder of each gas stream was exhausted through
a manifold vent. The baghouse inlet and outlet were sampled alternately (i.e., inlet sample was
analyzed for an interval while the outlet sample was exhausted, then outlet sample was analyzed
while the inlet sample was vented). A location was selected for analysis using the four-way gas
selection valve on the manifold outlet to the instrument. Gas flow to the instrument was
regulated with a needle valve on a rotameter at the manifold outlet.
5.2 FTIR SAMPLING PROCEDURES
For each run, two locations were sampled using two separate sample systems that were
both connected to the main manifold (Figure 5-1). In the first run, the mold cooling and shake-
out housing were sampled together and for three runs the baghouse inlet and baghouse outlet
were sampled together. A single FTIR instrument was used to analyze samples from both
locations during a test run. The manifold's four-way valves allowed the sample from either of
two locations to be directed alternately to the FTIR cell. Sample flow was controlled by a needle
valve and measured with a rotameter.
FTIR sampling was conducted using either the batch or the continuous sampling
procedures. All data were collected according to the Method 320 sampling procedure, which are
described below.
5-3
-------
5.2.1 Batch Samples
In this procedure, the 4-way valve on the manifold outlet was turned to divert a portion of
the sample flow to the FTIR cell. A positive flow to the main manifold outlet vent was
maintained as the cell was filled to just above ambient pressure. The cell inlet valve was then
closed to isolate the sample, the cell outlet valve was opened to vent the cell to ambient pressure,
the spectrum of the static sample was recorded, and the cell was evacuated for the next sample.
This procedure was repeated to collect a desired number of discreet samples.
Batch sampling has the advantage that every sample is independent from the other
samples. The time resolution of the measurements is limited by the interval required to evacuate
a sample, pressurize the cell, and record a spectrum. All of the calibration transfer standards, and
spiked samples were collected using this procedure. Several spectra in each run were also
collected in this manner.
5.2.2 Continuous Sampling
The cell was filled as in the batch sampling procedure, but the cell inlet and outlet valves
were kept open to allow gas to continuously flow through the cell. The inlet and outlet flows
were regulated to keep the sample in the cell at ambient pressure. The flow through the cell was
maintained at about 5 Lpm. The cell volume was about 7 liters (L).
The FTIR instrument was automated to record spectra of the flowing sample about every
2 min and the quantitative analysis was automated to measure pollutant concentrations as each
spectrum was recorded. The analytical program was revised after the test was completed and all
of the spectra were reanalyzed.
This procedure with automated data collection was used during each of the test runs.
Because spectra were collected continuously as the sample flowed through the cell, there was
mixing between consecutive samples. The interval between independent measurements (and the
time resolution) depends on the sample flow rate (through the cell) and the cell volume.
The Time Constant (TC) defined by Performance Specification 15 for FTIR continuous
emissions monitoring systems (CEMS), is the period for one cell volume to flow through the
cell. The TC determines the minimum interval for complete removal of an analyte from the cell
volume. It depends on the sampling rate (Rs in Lpm), the cell volume (Vcell in L) and the
analyte's chemical and physical properties. Performance Specification 15 defines 5 * TC as the
minimum interval between independent samples.
5-4
-------
T-I/~< cell
TC '
A stainless steel tube ran from the cell inlet connection point to the front interior 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 and minimized the likelihood of a short circuiting flow.
5.3 ANALYTE SPIKING
Since there was little information available about HAP emissions from this source, there
was no plan for validating specific HAP's at this test. MRI conducted limited spiking for quality
assurance (QA) purposes using a toluene in nitrogen standard and a vapor-generated
formaldehyde standard.
5-3.1 Analyte Spiking Procedures
The infrared spectrum is ideally suited for analyzing and evaluating spiked samples
because many compounds have distinct infrared spectra.
The reason for analyte spiking is to provide a QA check that the sampling system can
transport the spiked analytes 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.
The spike procedure follows Sections 9.2 and 13 of EPA 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 will comprise
about 1/10 or less of the spiked sample. The actual dilution depends on the ratio of the sample
and spike flow rates. The expected concentration of the spiked component is determined using a
tracer gas, in this test SF6. The SF6 concentration in the direct sample divided by the SF6
concentration in the spiked sample(s) is used as the spike dilution factor (DF). The analyte
standard concentration divided by DF gives the expected value of the spiked analyte
concentration.
5-5
-------
5.3.2 Analysis of Spiked Results
5.3.2.1 Determination of Formaldehyde Standard
Formaldehyde vapor was produced by heating a permeation tube filled with solid
paraformaldehyde. The tube was placed in a vapor generation oven (Kintek) equipped with a
temperature controller and mass flow meter to regulate the carrier gas. The oven was raised to
100°C, and the vapor of the formaldehyde monomer was purged with a continuous flow of a
carrier gas. For spiking the carrier gas was a constant flow from the SF6 cylinder standard
(4.01 ppm in nitrogen at ± 2 percent, Scott Specialty Gases). The SF6 cylinder certification had
expired before the test. The SFg concentration was confirmed by comparison to spectra of SF6
from another cylinder. The SF6 concentration was confirmed to be within 1.5 percent of the
certified concentration of 4.01 ppm. When spiking was not performed the formaldehyde vapor
was continuously vented using a low flow of nitrogen as the carrier gas. Using this device it was
practical to generate a very stable concentration output of formaldehyde. The concentration of
this formaldehyde standard was determined with respect to formaldehyde reference spectra in the
EPA FTIR spectral library (Table 5-1).
TABLE 5-1. DETERMINATION OF FORMALDEHYDE STANDARD CONCENTRATION
Date
9/5/97
9/9/97
File name of
Direct Measurement
FORMAL01
FKM0909A
Average ->
Formaldehyde
ppma
77.3
80.0
78.7
Uncertainty
1.1
1.0
1.1
a Measured between 3160.8 and 2650.1 cm using EPA reference spectrum 087b4anb, deresolved to 2.0 cm" .
The vapor generation oven was kept at 100°C and the carrier gas flow rate was 1.00 Lpm. Nitrogen was the carrier
gas for the direct-to-cell measurements of formaldehyde.
5.3.2.2 Determination of Concentrations in Spike Mixtures
Frequently the output formaldehyde from the vapor generation oven was mixed
quantitatively with the toluene standard so that sample stream could be spiked with toluene, SF6
and formaldehyde simultaneously. Mixing the two spike streams together introduced another
dilution factor that had to be accounted for to determine the concentrations of each component of
the spike mixture. The concentration of each component in the spike mixtures was determined
independently by preparing a separate analytical computer program. The input for the computer
5-6
-------
program consisted of reference spectra of each analyte in the mixtures. For SF6 and toluene
spectra the program used spectra of samples taken directly from the cylinder standards and
measured in the FTER cell. For formaldehyde the program used a spectrum in the EPA library.
The program was used to analyze spectra of each of the spike mixtures, which were measured
directly in the FTER gas cell. Table 5-2 present the results from this analysis. Table 5-2 also
shows the mass flow meter readings used to prepare the spike mixtures, the files names for the
direct-to-cell measurements of each mixture, and the file names of the samples that were spiked
with each mixture.
The measured concentrations in Table 5-2 were used to determine the percent recoveries
in Tables 4-2 to 4-9: the SF6 concentrations were used to determine the DF, and the toluene and
formaldehyde concentrations were combined with DF to determine the C and the percent
recoveries for those analytes.
5.3.2.3 Determination of Percent Recovery
The expected concentration of the spiked component was determined using the tracer gas,
SF6. In the following discussion the "direct" measurement refers to the measured concentration
in the spike mixture before it was added to the sample stream (i.e., the concentrations presented
in Table 5-2).
The DF was determined by the ratio of the measured SF6 concentration in the direct
measurement of the spike mixture, SF6(direct^, to the measured SF6 concentration in the spiked
samples, SF6(spike).
cp
DF = 6(direct) (2)
SF
01 6(spike)
The direct measurement of the analyte concentration in the spike mixture divided by DF gives
the expected concentration for a 100 percent recovery of the analyte spike, Cexp.
«" DF
where:
analyte/direct) = The concentration of either toluene or formaldehyde from the direct
measurement of the spiked mixture (from Table 5-2).
5-7
-------
TABLE 5-2. MEASURED ANALYTE CONCENTRATIONS AND MIXING FLOW RATES FOR THE SPIKE MIXTURES
Date
9/5/97
9/8/97
9/9/97
9/10/97
Spiked Sample Files
shksplOl, 102, 107
coosplOl, 102, 107
outsplOl
inspl01,insp!02
outsplll, inspl!7
insp201,outsp201
insp205, outsp208
insp301, outsp301
outsp316, insp312
File name of Direct
Measurement
average (sfto!2, sfto!3)
average (sf6to!4, sftolOS)
sfto!06
sft0909a
sft0909b
average (sft0909a, sft909b)d
sft0910a
sft0910b
Toluenea Tolueneb
(ppm) (ppm)
39.8
29.7
53.0
31.8
27.6
25.7
19.1
34.2
20.5
17.8
SF6
(ppm)
2.090
2.191
1.475
3.841
2.013
2.069
3.226
Formaldehyde
(ppm)
62.2
50.1
34.8
41.8
44.1
43.0
43.1
75.5
Mixing Flow Rates (Lpm)c
Formaldehyde Toluene
1.00 1.00
1.00 1.00
1.00 2.00
2.00 xx
1.00 1.00
1.00 1.00
2.00 1.00
Ln
i
00
a Toluene concentration determined using EPA reference spectrum "153a4arc" deresolved to 2.0 cm l.
Toluene concentration determined using spectrum of sample taken directly from 60 ppm toluene cylinder standard. See Section 3-4 and Table 15 for
additional explanation.
c The mass flow meter on the Kintek (formaldehyde) vapor generator was used to control the SF^ carrier gas flow. A separate mass flow meter was used to
control the flow from the 60 ppm toluene gas standard.
The formaldehyde concentration in these two mixtures can be averaged because increasing the carrier gas flow from 1.0 Lpm to 2.0 Lpm dilutes the
formaldehyde concentration in the vapor generation output. This dilution is similar to using a 1.0 Lpm carrier gas flow and then mixing the vapor generation
output with a 1.0 Lpm flow from the toluene standard.
-------
The actual spike recovery in Tables 4-2 to 4-9 is the percent difference between the measured
analyte concentrations in the spiked samples and C
f* Jll f*
% Recovery = x 100 (4)
Cexp
where:
calc = the analyte concentration in the spike samples, spiked - unspiked.
5.4 ANALYTICAL PROCEDURES
t*i
Analytical procedures in the EPA FTIR Protocol were followed for this test. A
computer program was prepared with reference spectra shown in Table 4-7. The computer
program6 used mathematical techniques based on a K-matrix analysis.7
Initially, the sample spectra were reviewed to determined appropriate input for the
computer program. Next an analysis was run on the sample spectra using reference spectra
listed in Tables 5-3 and 5-4. The estimated uncertainty results for the undetected species were
reported in Tables 1-1 and 1-2. Finally, compounds undetected in the initial analysis were
removed from the program and the spectra were analyzed again using reference spectra only for
the detected compounds. The results from this second analytical run are summarized in
Tables 1-1 and 1-2 and reported in Appendix B.
The same program that did the analysis calculated the residual spectra (the difference
between the observed and least squares fit absorbance values). Three residuals, one for each of
the three analytical regions, were calculated for each sample spectrum. All of the residuals were
stored electronically and are included with the electronic copy of the sample data provided with
this report. The computer program calculated the standard l*sigma uncertainty for each
analytical result, but the reported uncertainties are equal to 4*sigma. The program was modified
to report as a non-detect any concentration less than 2*uncertainty.
The concentrations were corrected for differences in absorption path length and
temperature between the reference and sample spectra.
5-9
-------
where:
CCOIT = concentration, corrected for path length and temperature.
Ccalc = unconnected sample concentration.
Lr = cell path length(s) (meters) used in recording the reference spectrum.
Ls = cell path length (meters) used in recording the sample spectra.
Ts = absolute temperature (Kelvin) of the sample gas when confined in the FTIR gas cell.
Tr = absolute temperature(s) (Kelvin) of gas cell used in recording the reference spectra.
The ambient pressure recorded over the three days of the test averaged about 755 mm Hg
so no pressure correction was applied to the results.
The sample path length was estimated by measuring the number of laser passes through
the infrared gas cell. These measurements were recorded in the data records. The actual sample
path length, Ls was calculated by comparing the sample CTS spectra to CTS (reference) spectra
in the EPA FTIR reference spectrum library. The reference CTS spectra, which were recorded
with the toluene reference spectra and are included in the EPA library, were used as input for a
K-matrix analysis of the CTS spectra collected at the Waupaca field test. The calculated average
cell path length resulting from this analysis and the variation among the Waupaca sample CTS
spectra are reported in Section 4.4.1.
5-4.1 Computer Program Input
The reference spectra used in the program input are summarized in Table 5-3 for the
analysis of the cooling and shake-out housing data and in Table 5-4 for the analysis of the
baghouse inlet and outlet data. Results from MRI's analysis are presented in Tables 1-1 and 1-2
and Tables B-l to B-4.
The program input for the cupola baghouse inlet and outlet included spectra of water
vapor, CO2, methane, toluene, formaldehyde, HC1, and hexane. The toluene and formaldehyde
were included to analyze the spiked samples. The program input for the cooling and shake-out
samples was similar, but HC1 was not included in the analysis.
Table 5-5 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
5-10
-------
spectra: by using Section K.2.2 of the EPA FTIR protocol. The program analyzed the main two
ethylene bands centered near 2,989 and 949 cm"1. Table 5-6 summarizes the results of the CTS
analysis. The cell path length from this analysis was used as Lg in equation 4.
5-4.2 EPA Reference Spectra
The formaldehyde and toluene spectra used in the MRI analysis were taken from the EPA
reference spectrum library (http://www.epa.gov/ttn/emc/ftir.html). To deresolve the spectra to
2.0 cm" , the sampling resolution, the original sample and background interferograms were
truncated to the first 8,192 data points. The new interferograms were then Fourier transformed
using Norton-Beer medium apodization and no zero filling. The transformation parameters were
chosen to agree with those used to collect the sample absorbance spectra. The new 2.0 cm
formaldehyde and toluene single-beam spectra were combined with their deresolved single-beam
background spectra and converted to absorbance. This procedure was used to prepare spectral
standards for the HAP's and other compounds included in the analyses.
TABLE 5-3. PROGRAM INPUT FOR ANALYSIS OF MOLD COOLING
AND SHAKE-OUT HOUSING SAMPLE SPECTRA
Compound name
Water
Carbon monoxide
Carbon dioxide
Formaldehyde
Methane
Toluene
Ethylene
SF6
Hexane
butane
n-heptane
pentane
1-pentene
2-methyl- 1 -pentene
File name
194f2sub
co20829a
193b4a_a
087b4anb
196clbsb
153a4arc
CTS0820b
Sf60819a
0950709a
but0715a
hep0716a
pen0715a
Ipe0712a
2mlp716a
Region No.
1,2,3
1
1,2,3
3
3
3
2
2
3
3
3
3
3
3
ISCa
100a
167.1
415a
100.0
80.1
103.0
20.1
4.01
46.9
100.0
49.97
49.99
50.1
50.08
Reference
Meters
22
11.25
22
3
10.4
10.4
10.3
11.25
10.3
10.3
10.3
10.3
T (K)
394
373
394
298
394
394
399
397.8
398.3
397.9
399
398.2
5-11
-------
Compound name
2-methyl-2butene
2-methyl-2-pentene
Isooctane
3-methylpentane,
File name
2m2b716a
2m2p713a
1650715a
3mp0713a
Region No.
3
3
3
3
ISCa
50.04
51.4
50.3
50.0
Reference
Meters
10.3
10,3
10.3
10.3
T (K)
398.2
398.6
398.3
398.5
Region No.
1
2
3
Upper cm
2,142.0
1,275.0
3,160.8
Lower cm
2,035.6
789.3
2,650.1
Indicates an arbitrary concentration was used for the interferant.
TABLE 5-4. PROGRAM INPUT FOR ANALYSIS OF BAGHOUSE
INLET AND OUTLET SAMPLE SPECTRA
Compound name
Water
Carbon monoxide
Sulfur Dioxide
Carbon dioxide
Formaldehyde
HC1
Methane
Toluene
Hexane
Ethylene
SF6
Ammonia
File name
194f2sub
co20829a
198clbsc
193b4a_a
087b4anb
097b4asd
196clbsb
153a4arc
095a4asd
CTS0820b
Sf60819a
174a4ast
Region No.
1,2,3
1
2
1,2,3
3
3
3
3
3
2
2
2
ISCa
100 a
167.1
89.5
415 a
100.0
72.2
80.1
103.0
101.6
20.1
4.01
500.0
Reference
Meters
22
22
11.25
2.25
22
3
3
10.4
10.4
3
T (K)
394
394
373
373
394
298
298
394
394
298
Region No.
1
2
3
Upper cm
2,142.0
1,275.0
3,160.8
Lower cm
2,035.6
789.3
2,650.1
a Indicates an arbitrary concentration was used for the interferant.
5-12
-------
TABLE 5-5. PROGRAM INPUT FOR ANALYSIS OF CTS SPECTRA
AND PATH LENGTH DETERMINATION
Compound name
Ethylene a
Ethylene
File name
cts0814b.spc
cts0814c.spc
ASC
1.007
1.007
ISC
1.014
0.999
% Difference
0.7349
0.7350
This spectrum was used in the analysis of the Waupaca CTS spectra.
TABLE 5-6. RESULTS OF PATH LENGTH DETERMINATION
CTS spectra
100 ppm Ethylene
CTS0904A
CTS0905A
CTS0905B
CTS0905C
CTS0908A
CTS0908B
CTS0908C
CTS0909A
CTS0909B
CTS0910A
CTS0910B
Average Path Length (m)
Standard Deviation
Path length calculations
Meters
10.91
10.81
10.79
10.60
10.62
10.61
10.52
10.50
10.40
10.46
10.67
10.63
0.16
Delta a
0.29
0.18
0.17
-0.02
-0.01
-0.01
-0.11
-0.13
-0.23
-0.17
0.04
% Delta
2.70
1.71
1.56
-0.23
-0.08
-0.12
-1.03
-1.19
-2.14
-1.57
0.39
a The difference between the calculated and average values.
5.5 FTIR SYSTEM
A KVB/Analect Diamond 20 spectrometer was used to collect all of the data in this field
test. The gas cell is a heated variable path (D-22H) gas cell from Infrared Analysis, Inc. The
path length of the cell was set at 20 laser passes and measured to be about 10.6 meters using the
CTS reference and sample spectra. The interior cell walls have been treated with a Teflon®
5-13
-------
coating to minimize potential analyte losses. A mercury/cadmium/ telluride (MCT) liquid
nitrogen detector was used. The spectra were recorded at a nominal resolution of 2.0 cm .
The optical path length was measured by shining an He/Ne laser through the cell and
adjusting the mirror tilt to obtain the desired number of laser spots on the field mirror. Each laser
spot indicates two laser passes through the cell. The number of passes was recorded on the field
data sheets in Appendix B. The path length in meters was determined by comparing calibration
transfer standard (CTS, ethylene in nitrogen) spectra measured in the field to CTS spectra in the
EPA reference spectrum library. The procedure for determining the cell path length is described
in Section 5.4.
5-14
-------
6.0 SUMMARY OF QA/QC 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 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.
Listed below are 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
• Length of time to measure spectrum
6-1
-------
• Time spectrum was collected
• Time and conditions of recorded background spectrum
• Time and conditions of relevant CTS spectra
• Apodization
Hard copy records were also kept of all flue gas measurements, such as sample flow,
temperature, moisture, and diluent data.
Effluent was allowed to flow through the entire sampling system for at least 5 min before
a sampling run started or after changing to a different test location. FTIR spectra were
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 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 100 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 was recorded whenever a CTS spectrum was collected. The CTS spectra were
compared to CTS spectra in the EPA library. This comparison is used to quantify differences
between the library spectra and the field spectra so library spectra of 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 stored for data analysis. Sample absorbance spectra can be regenerated from
the raw interferograms, if necessary. A copy of the data was provided with the draft report.
To measure HAP's detected in the gas stream MRI used spectra from the EPA library,
when available.
6-2
-------
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. "Computer-Assisted Quantitative Infrared Spectroscopy," Gregory L. McClure (ed.),
ASTM Special Publication 934 (ASTM), 1987.
5. "Multivariate Least-Squares Methods Applied to the Quantitative Spectral Analysis of
Multicomponent Mixtures," Applied Spectroscopy, 39(10), 73-84, 1985.
6. "An Examination of a Least Squares Fit FTIR Spectral Analysis Method," G. M.
Plummer and W. K. Reagen, Air and Waste Management Association, Paper
Number 96-WA65.03, 1996.
7-1
-------
APPENDIX A
VOLUMETRIC FLOW DATA
-------
A-l. MOLD COOLING AND SHAKE-OUT HOUSING LINE FLOW DATA
-------
Project Waupaca Foundry, Plant No. 5, Tell City, IN
Project Number 3804.25 / 4701.08.08
Source Mold Cooling Line (Location C) / Shakeout Housing (Location D)
Sample Location Combined Cooling Line Duct / Shakout Housing Duct
Run Number
Date
Time
Barometric Pressure
Velocity Head
Pitot Tube Coefficient
*— '-'2, dry basis
*~*2 , dry basi s
^2, dry basis
Static Pressure
Stack Pressure
Stack Temperature,°F
Stack Temperature, °R
Water Vapor, proportion
Mole Fraction of dry gas
Dry Molecular Weight
Actual Molecular Weight
Gas Stream Velocity
Stack Diameter
Stack Area
Actual Volumetric Flow
Standard Volumetric Flow
Standard Volumetric Flow
Pfaar
/&Pavg
Cp
%
%
%
PS
Pg
Ts
Ts
BWS
Md
Ms
ft/sec
in
ft2
wacfm
dscfm
dscmm
la
5-Sep-97
14:47
29.63
0.9688
0.84
0
20.9
79.1
0
29.63
120.80
580.80
0.026
0.97
28.84
28.55
57.65
34.25
6.40
22130
19399
549
Ic
5-Sep-97
15:15
29.63
1.3576
0.84
0
20.9
79.1
0
29.63
119.93
579.93
0.054
0.95
28.84
28.25
81.14
34.25
6.40
31149
26576
753
-------
BWS
Moisture Calculation With WB/DB Measurement
Run cool shake
Pbar 29.63 29.63
Ps 00
Ts(DB) 121.2 126.6
Ts(WB) 83.8 99.2
Psat 1.175 1.876
Calculations
Pstack 29.63 29.63
dT 37.4 27.4
Pp H20 0,7795 1.5913
BWS 0.0263 0.0537
Page 1
51
-------
Data Input
Project Waupaca Foundry, Plant No. 5, Tell City, III
Project Dumber 3804 . 25 / -1701.08.08
Source Mold Cooling Line (Location C) .' Shakeout Housing (Location [
Sample Location Combined Cooling Line Duct / Shakout Housing Duct
Stack Diameter in. 34.25 (both)
Cp 0.84 s-type pitot
Operators Weal/Edwards/Raile
Port
NE
Date 05-Sep-97
Time 14:47
Ts(DB) 121.2
Ts(WB) 83.8
Pbar 29.63
Pt NA
Ps 0
O2 % 20.9
CO2 % 0
Run - Cool
Point
1
2
3
4
5
6
7
8
Q
10
11
12
1
2
3
4
5
6
7
8
9
10
11
12
dP
0.
0.
0.
0.
0.
0.
1
1
1 .
1 .
1 .
1 .
0.
0.
. 1
1.
1 .
1
0;
0.
0.
0.
0.
0.
61
83
93
85
78
83
. 1
. 2
15
25
35
25
59
96
. 1
15
15
. 1
71
.69
.68
.71
. 91
. 96
sqrt dP
0.
0.
0.
0.
0.
0.
1 .
1 .
1
1 .
I
\
0
0
1
1
1
1
0
0
0
0
0
0
7810
9110
9644
9220
.8832
. 9110
,0488
.0954
.0724
.1180
.1619
.1180
.7681
.9798
.0488
.0724
.0724
.0488
.8426
.8307
.8246
.8426
.9539
. 9798
Ts
97
115
120.
120.
121
119.
119.
125.
125.
125.
126 .
126.
101 .
114.
115
122 .
123.
123 .
126
126
126.
126.
126.
126 .
Date 05-Sep-97
Time 15:15
Ts(DB) 126.6
Ts(WB) 99.2
Pbar 29.63
Pt NA
Ps 0
O2 % 20.9
CO2 % 0
Run - Shake
dP
4
2
2
4
4
4
8
4
o
4
6
6
2
6
2
4
2
2
1
2
2
2
2
1
1
1
1
1
1
1
2
2
2
2
2
1
1
1
1
1
1
.85
2
.05
.05
.05
.05
.9
.8
.75
.7
.8
.65
. 9
.2
. 3
. 25
. 35
.45
.75
.4
. 35
. 35
.4
.25
sqrt dP
1.
1 .
1 .
1 .
1.
1.
1 .
1 ,
1 .
1 .
1 .
1 .
1 .
1 ,
1 .
1 .
1 .
1 .
1
1
1
1
I
I ,
3601
4142
4318
4318
.4318
.4318
. 3784
.3416
.3229
.3038
,3416
.2845
.3784
.4832
.5166
.5000
.5330
.5652
.3229
. 1832
.1619
. 1619
.1832
.1160
Ts
94 .4
99
100.6
99. 6
99.8
101.2
111.2
115.8
116
122.6
130.6
130.4
119
123.8
126.2
127.6
128.8
129.6
129.6
133.4
134
135
134 .8
135.4
Average
0.9688 120.8
1.3576 119.9
Page 1
-------
VELOCITY TRAVERSE DATA
Project No,
Run No. _
Plant
Date
Sampling Location
Operator(s)
f. Qa-'?e
-------
VELOCITY TRAVERSE DATA
Project No.
Run No. _
Plant _
fire In
Date .
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
*s
JE
SAMPLING LOC
INSIDE OF FAR
OUTSIDE OF
INSIDE OF NEA
OUTSIDE OF
STACK I.D., (01
NEAREST UPST
NEAREST OOWf
CALCULATOR.
TRAVERSE
POINT
NUMBER
Aj.t. 1
2-
3
S.a£ '*-'£ J*/<* £*~
WALL TO
NIPPLE, (DISTANCE A)
R WALL TO
NIPPLE. (DISTANCE B)
STANCE A • DISTANCE
REAM DISTURBANCE
77^:"
3-f
^ 3y^V"
/ >r "
/ $ ' \ ,
W*
X* XX
KTRF All DISTURBANCE *»'
£ . fJ&ti*
FRACTION
OF STACK 1,0.
.0-1
.6(1
,HB
.177
, >r
. ?r £
,bYf
-r-rr-.75"^
,8>3
.33+*
• fj7
•ff?
,e;M
. r
^ , jff
7
. 6^f
STACK 1.0.
3Y.*f
M
II
••
,,
*.
t<
1
*
11
«'
,1
„
I*
"
u
it
tl
,.
PRODUCT OF
COLUMNS 2 AND 3
(TO NEAREST 1 8 INCH)
«.7i?
^.W>"
y.c<^>
SCHEMATIC OF SAMPLING LOCATION
DISTANCE B
3-tf
•i
M
^.06Z- "
^. 5V 3
/^ . //7
tr
M
j.}.o?.«?!
Slfl.A/j nn |fi -l^" J, a 1" ,- ^5 . frfr?
?
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, t?^//- | ««
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n
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33, r?/
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(t
,.
1* .
i (
/'
u
M
1'
M
t«
,.
('
1'
1'
<•
it
TRAVERSE POINT LOCATION
FROM OUTSIDE OF NIPPLE
(SUM OF COLUMNS 4 & 5)
3,77
s.ss
J.tf
//. 8 1
/r.y
?j-.;y
A ^/ ^ "7 -* . J/? ^^
**^' * -^ J . ^ / |7™ Q« / i
J/.W
JJ.¥^
J5"- * /
36'. 75
3.^7
J"-5T
?.#?
7.3'
n.Qt
/f.y}
ifj • •* i
-^ Q & \j
31. ^Y
33. yi
35"- 3-'
3b.?S
?A (Dun 232
4 72
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
PLANT .
FE _J
SAMPLING LOCATION
INSIDE OF FAR WALL TO
OUTSIDE OF NIPPLE. (DISTANCE A)
INSIDE OF NEAR WALL TO
OUTSIDE OF NIPPLE. (DISTANCE B)
STACK I.D.. (DISTANCE A • DISTANCE B
NEAREST UPSTREAM DISTURBANCE _
NEAREST DOWNSTREAM DISTURBANCE
CALCULATOR...
Pi~**rr 1* 'S
SCHEMATIC OF SAMPLING LOCATION
TRAVERSE
POINT
NUMBER
£ . i>J- '
r
?
i
f
i i
"7
8
f
10
f/
t>
f,f. / +2^*
Is
3
¥
.r
6
t
B
f
/o
f)
/>
FRACTION
OF STACK 1,0.
.<*'
,o6l
.1/8
,ill
trS
•Itf
,6^
• 7f
,W
• #9r-
. 933
,979
,o3-\
•oil
. n%
..'77
.>r
.3$T
. feVf
,?r
STACK 1.0.
?Y.*r
-.
..
"
"
o
•*
i •
,» i
/•
//
PRODUCT OF
COLUMNS 2 AND 3
(TO NEAREST 1 1 INCH)
0/7/7
^??f
y.c^?-
<£-<.•«>>•
1?. y^3
/pi. ,/ff
r>.*?'
>3". fr^S
/•1s. ;^^
jp./*?
31 'Iff
33. $3!
•• o.in
•>
;•
it
1 1
ft
i.Wt
H -OH>
i.O^r
B.?63
f>- ifl
H.eli
, Bs3
,£87- i "
• f 3 '} "
'771
n
?$. '^B
25. X>?
i^^rr
n.o;
DISTANCE B
5->r
/ 1
,t
• •
t t
11
tl
II
/I
1 1
f >
'<
»*
• 1
1 •
it
; I
,•
/I
v»
•>
/.
/I
"
TRAVERSE POINT LOCATION
FROM OUTSIDE OF NIPPLE
(SUM OF COLUMNS 485)
M7
£-Sf
2*y3'
//.?/
tS-Hl
2f-*i
s£.W
j/.yf
JJ. ^6
jf. >/
34 - 7ff
3.17
.C^T
•7.>f
9.3'
/i.9i
/f.*/
2$.3i
W.1*{
3>-ii
33. U
It. '78
'A (Dun 232
472
-------
PROJECT NO.
PLANT: I '
FTIR FIELD DATA FORM
(Moisture Data * Wet Bulb and Dry Bulb Method)
BAROMETRIC
OPERATOR:
DATE
°Wftl
i^tf
-
LOCATION
C>j/dU^~-
SW-bCu-f-
TIME
24-HR
/yfc/7
tV6
DRY BULB
TEMPERATURES
»{F)
1X1.2-
M-(,
WET BULB
TEMPERATURES
lw(P)
??3r
ff,2-
BAROMETR1C
PRESSURE
Pb«r
*£&-
~75Z
-75"^-
TOTAL
PRESSURE
TP
In. w.c.
VELOCITY
HEAD
Delta P
In. w.c.
Uo
W
PITOT
COEFFICIENT
C*
0f
L
CARBON
DIOXIDE
Dry-bub
% fcy wl.
(?
e?
OXYGEN
Dry bub
•AbyvoL
/a'/
^^j
MIDWEST RESEARCH INSTITUTE
My Documenls/rnRFORM/Ficld«u4.XLS
08-29-97
-------
Vi"J > •""• *A
"
'7 '-'A
. n
6A6S
OXYGEN AND CARBON DIOXIDE BY ORSAT
PROJECT NO.
OPERATOR
rt >'•"< *' nuMNn JH'-V'.^ *»"- vw
i \V»
PLING LOCATION (
IME(24hr-CLOCK) .
PEIBAG GRAB) -,
DATE
v-
'AbV'T
V- .» ••'• j
Kt} ORSAT LEAK CHECK BEFORE ANALYSIS:
BURETTE CHANGE IN 4 MIN.
PIPETTES CHANGE IN 4 MIN.
ORSAT LEAK CHECK AFTER ANALYSIS:
BURETTE CHANGE IN 4 MIN.
PIPETTES CHANGE IN 4 MIN.
^x^^^kjf^
GAS ^\^
C02
Oo (NET IS SiCdNO
£• j^
READINtS MINUS ACTUAL
tOg HEADING)
1
READING
1
2
1
2
--JCT
^^
2
ACTUAL
READING
\^X^
^^
3
1
2
NET
•*"J~
^
3
ACTUAL
READING^
1
2
1
2
^r
"^\
^AVERAGE
NET
VOLUME
^^^
H-tl StV SURMMaWt (821(1
CO 2 >4% .3% by Volume
.2% by Volume
Acceptance Criteria
02 ;
.2% by Volume
<15% .3% by Volume
Comments:
0
^( v^ii fo\Vt\
-------
OXYGEN AND CARBON DIOXIDE BY ORSAT
PROJECT NO.
SAMPLE NO
PLANT SAMPLING LOCATION
ANALYSIS TIME (24hf-CLOCK)
SAMPLE TYPCBSi? GRAB)
OPERATOR.
RUN NO __
DATE 1'lT'Tl
57* <
ORSAT LEAK CHECK BEFORE ANALYSIS:
BURETTE ^>JI CHANGE IN4 MIN.
PIPETTES fiW CHANGE IN 4 MIN.
ORSAT LEAK CHECK AFTER ANALYSIS:
BURETTE —Hsxl CHANGE IN 4 MIN.
PIPETTES /frff CHANGE IN 4 MIN.
\. RUN
GAS ^"\^
C02
02 (NET IS SECOND
READING MINUS ACTUAL
CCv, READING)
t
ACTUAL
READING
1 0.0
2 0.0
3 O.o
1 fr"
2 }<>,
-------
OXYGEN AND CARBON DIOXIDE BY ORSAT
SAMPLE NO.
PLANT SAMPLING LOCATION
ANALYSIS TIME (24hr-CLOCK)
SAMPLE TYPE |® GRAB)
OPERATOR 0.fi'**L
RUN NO.
77
ORSAT LEAK CHECK BEFORE ANALYSIS:
BURETTE A-*5 CHANGE IN 4 MIN.
PIPETTES ^frf CHANGE IN 4 MIN.
ORSAT LEAK MECK AFTER ANALYSIS:
BURETTE fa* CHANGE IN 4 MIN.
PIPETTES fi** CHANGE IN 4 MIN.
\. RUN
GAS ^\^
C02
02 (NET IS SECOND
READING MINUS ACTUAL
COg READING)
1
ACTUAL
READING
1 0.0
200
3 o.o
1 fr.l
2 2° 7
3 ^t> -7
NET
O 0
y$>t
2
ACTUAL
READING
1
2 6, f»
3
1
2 f0-]
3
NET
3
ACTUAL
READING
1
2
3
1
2
3
NET
AVERAGE
NET
VOLUME
fl II SEV SUmUN*Mt OMI9I
CO-
Comments:
Acceptance Criteria
.3% by Volume
.2% by Volume
£ 15%
< 15%
.2% by Volume
,3% by Volume
-------
A-2. BAGHOUSE FLOW DATA
-------
02'05.9S 18:48 tJl919941023
PES RTF NC
'11002 005
PARTICULATE/METALS EMISSIONS SAMPLING AND FLUE GAS
PARAMETERS - CUPOLA BAGHOUSE INLET
THE WAUPACA FOUNDRY - TELL CITY, INDIANA
Run No.
Date
Total Sampling Time, min
Average Sampling Rate, dscfrn *
Sample Volume:
dacfb
dscrn*
Average Flue Gas Temp., °F
02 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Flue Gas Volumetric Flow Rate:
acfin*
dscfin*
dscmm"
Isokinetic Sampling Ratio, %
I-M29-1
9/9/97
240.5
0,342
82.208
2.328
275
10.9
10.8
2.5
39,900
26,800
759
104.0
I-M29-2
9/10/97
240
0.481
115.471
3.270
301
9.5
11.6
2.8
58,900
38,200
1,080
102.7
I-M29-3
9/10/97
240
0.493
118.408
3.353
302
8.8
12.4
2.4
59,300
38,500
1,090
106.5
Average
0.439
105.362
2.984
293
9.7
11.6
2.6
52,700
34,500
976
104.4
* Dty standard cubic feet per minute it 68° F (20° C) and 1 Mm.
b Dty itsndinl cubic feel at 68° F (20° C) and 1 itra.
* Dry standard cubic meters at 68° F (20° Q and 1 aim.
* Actual cubic feet per minute at exhaust gas conditions.
* Dry standard cubic meters per minute at 68° F (20° C) and 1 attn.
-------
02 05-98 18:4S S1919941Q234
PES RTF NC
i!003 003
P ARTICULATE/METALS EMISSIONS SAMPLING AND EXHAUST GAS
PARAMETERS - CUPOLA BAGHOUSE OUTLET
THE WAUPACA FOUNDRY - TELL CITY, INDIANA
RUB No.
Date
Total Sampling Time, min
Average Sampling Rate, dscfm *
Sample Volume:
dsef*
dsems
Average Exhaust Gas Temp., "F
02 Concentration, % by Volume
COi Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfin4
dscfim*
dscmm*
Isokinetic Sampling Ratio, %
O-M29-1
9/9/97
240
0,378
90,633
2.566
231
12.7
8,8
5.5
45,000
32,100
908
103.1
O-M29-2
9/10/97
240
0.580
139.162
3.941
253
11.0
10.1
2,6
69,600
49,700
1,410
1022
O-M29-3
9/10/97
240
0.552
132.547
3.753
254
11.0
10.0
2.8
68200
48,500
1,370
99.7
Average
0.503
120.781
3.420
246
11.6
9.6
3.6
60,900
43,400
1,230
101.7
* Dry standard cubic feet per minute it 68° F (20° C) and 1 atm.
b Dry standard cubic feet at 68" F (20° C) and 1 atm.
* Dry standard cubic metes at 68° F (20° C) tod 1 sem.
4 Actual cubic fleet per minute at exhaust gas conditions.
* Dry standard cubic meters per minute at 68° F (20° Q and 1 asm.
-------
02-05-98 18:48
S19199410234
PES RTF NC
005
SVOHAPS EMISSIONS SAMPLING AND EXHAUST GAS PARAMETERS
CUPOLA BAGHOUSE OUTLET
THE WAUPACA FOUNDRY - TELL CITY, INDIANA
Run No.
Date
Total Sampling Time, min
Average Sampling Rate, dscfin *
Sample Volume:
dscfb
dscm'
Average Exhaust Gas Temp., °F
O2 Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate:
acfin*
dscfin*
dscmm'
Isokinetic Sampling Ratio, %
BO-0010-1
9/9/97
240
0.458
110.023
3.116
234
12.7
8.8
3.4
46,600
33,800
957
99.4
BO-0010-2
9/10/97
240
0.627
150.485
4.261
258
11.0
10.1
2.7
66,700
47,200
1,340
97.3
BO-0010-3
9/10/97
240
0.690
165.500
4.686
256
11.0
10.0
2.6
69,300
49,200
1,390
102.6
Average
0.592
142,003
4.021
249
11.6
9.6
2.9
60,900
43,400
1,230
99.7
* Diy standard cubic feet per minutt at 68* F (2Q* C) tad 1 ma.
b Dry standard cubk feet at 68° F (20a C) and I itm.
e Dry standard cubic meters ai 68° F (20° C) and 1 tun.
4 Actual cubic feet per minute at exhaust gas conditions,
1 Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
-------
02 03 98 16:48 018199410234
PES RTF N'C
ilOOS- 005
PCDDi/PCDFs EMISSIONS SAMPLING AND EXHAUST GAS PARAMETERS
CUPOLA BAGHOUSE OUTLET
THE WAUPACA FOUNDRY - TELL CITY, INDIANA
Run No.
Date
Total Sampling Time, min
Average Sampling Rate, dscfin *
Sample Volume:
dscf
dscm'
Average Exhaust Gas Temp., °F
Oj Concentration, % by Volume
CO2 Concentration, % by Volume
Moisture, % by Volume
Exhaust Gas Volumetric Flow Rate;
acfin4
dscfin1
dscmm*
Isokinetic Sampling Ratio, %
BO-23-1
9/9/97
240
0.486
116.671
3.304
230
12.7 '
8.8
3.4
49,400
36,000
1,020
98.9
BO-23-2
9/10/97
240
0.669
160.663
4.549
258
11.0
10.1
2.6
69,500
49,200
1,390
99.7
BO-23-3
9/10/97
240
0.660
158.414
4.486
254
11.0
10.0
2.4
68,800
49,100
1,390
98.5
Average
0.605
145.249
4.113
247
11.6
9.6
2.8
62,600
44,800
1,270
99.0
* Dry standard cubic feet per minute at 68" F (20" C) and 1 ann.
b Dry standard cubic feet at 68° F (20" C) and 1 atm.
* Dry standard cubic meters at 68° F (20° C) and 1 am.
* Actual cubic feet per minute at exhaust gas conditions.
* Dry standard cubic meters per minute at 68° F (20° C) and 1 atm.
-------
APPENDIX B
FTIR DATA
-------
WAUPACA
Date
9/9/97
9/10/97
Time
10:30
10:39
10:50-11:00
11:08-11:17
11:28-11:34
11:44
11:50
11:57
12:24
12:50
13:24
13:50
14:05
14:11
14:29
15:05
15:25
7:20
7:49
8:00
8:10
8:15-8:27
8:34-8:47
9:00
9:07
9:40
10:05
10:29
11:05
11:17-11:37
11:45-12:07
12:15-12:33
12:45
12:53
13:04
13:26
Location
Outlet
Outlet
Inlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Inlet
Outlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Outlet
Inlet
Spiked
X
X
X
X
X
X
X
X
Unspiked
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Event/Notes
N2 only direct to cell
Background - N2 only
Spike direct to cell
Outlet - air through
Background - N2 only
Leak check inlet and outlet
Direct to cell spike
Background
N2 only - Background
Spike direct to cell
Background - N2 only
-------
WAUPACA
Date
9/8/97
9/9/97
Time
9:30
9:45-9:53
9:55
10:15
10:54
11:20
13:15
14:10
14:20-14:24
15:23-15:33
15:37-16:02
16:11-16:27
16:41-16:58
17:21
17:41
18:03
18:07
18:29
18:50
19:11
19:31
19:45
10:24
11:07
12:02-12:18
12:27-12:40
12:46
12:56-13:27
13:25
13:42-13:49
14:04-14:15
14:28-14:33
14:45-15:09
15:18-15:30
15:39
16:09
1639
16:55
17:05
17:10
17:13
17:28
7:10
7:27
7:47
8:00
8:11
8:24
8:57-9:06
9:25-9:44
9:54-10:08
10:16
Location
Cooling stack
Cooling line
Shakeout line
Shakeout line
Cooling line
Cooling line
Shakeout line
Cooling line
Shakeout line
Cooling line
Inlet
Outlet
Inlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Outlet
Inlet
Inlet
Outlet
Outlet
Outlet '
Inlet
Outlet
Spiked
X
X
X
X
X
X
X
X
X
X
X
X
Unspiked
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X
Event/Notes
Background, N2 only
Calibration
Leak check
Process down
Background, N2 only
[SF6 to spike line
Process restarted
SF6 into Kintek
N2only
Shakeout probe in stack
N2 only direct to cell
N2 only - Background
Background - N2 only
direct to cell - spike
Background- N2 direct to cell
Changed outlet probe
Background - N2 only
Probes pulled out of stack
Inlet and Outlet pass leak checks
N2only
Inlet and Outlet pass leak checks
Background
Spike direct to cell
N2 only in background
-------
B-l. FTIR RESULTS TABLES
-------
TABLE B-l. FTIR RESULTS FROM THE MOLD COOLING LINE
-------
TABLE B-l. FTIR RESULTS AT MOLD COOLING LINE
Date Time File name '
9/5/97
15:25
15:35
16:12
16:18
16:23
16:30
17:07
17:09
17:12
17:14
17:16
17:18
17:20
17:44
17:46
17:48
17:50
17:52
17:54
17:57
17:59
18:05
18:29
18:31
18:33
18:35
19:11
COOSP101
COOSP102
COOUN103
COOUN104
COOUN105
COOUN106
19050001
19050002
19050003
19050004
19050005
19050006
19050007
19050018
19050019
19050020
19050021
19050022
19050023
19050024
19050025
19050028
19050039
19050040
19050041
19050042
COOSP107
Average — >
Toluene
ppm Unc 2
19.9 3.1
20.8 3.5
19.5 4:0
18.7 4.0
19.3 4.0
18.2 3.9
19.0 4.0
18.6 3.9
18.6 3.9
19.0 4.0
18.7 4.0
17.8 3.9
17.2 3.8
16.8 4.0
17.4 4.1
17.6 4.1
17.9 4.2
18.1 4.2
18.2 4.1
18.2 4.2
17.3 4.1
9.2 2.0
16.6 3.9
16.5 3.9
16.5 3.9
16.1 3.9
16.5 3.2
17.5 3.9
Hexane
ppm Unc
0.0 22.2
0.0 25.0
0.0 31.5
0.0 31.3
0.0 31.9
0.0 31.0
0.0 31.0
0.0 30.6
0.0 30.7
0.0 31.2
0.0 31.1
0.0 30.5
0.0 30.1
0.0 31.4
0.0 31.9
0.0 32.2
0.0 32.7
0.0 32.9
0.0 32.5
0.0 32.8
0.0 32.3
0.0 13.4
0.0 30.7
0.0 30.6
0.0 30.8
0.0 30.5
0.0 22.7
0.0 30.6
Ethylene
ppm Unc
7.3 0.8
8.1 0.9
13.5 0.8
13.2 0.8
13.6 0.8
13.2 0.8
13.6 0.8
13.5 0.8
13.6 0.8
13.8 0.8
13.7 0.8
13.3 0.8
13.1 0.8
13.2 0.8
13.5 0.8
13.7 0.8
13.9 0.8
14.0 0.8
14.1 0.8
14.1 0.8
13.6 0.8
7.4 0.4
13.5 0.8
13.5 0.8
13.5 0.8
13.3 0.8
5.3 1.1
13.3 0.8
SF6
ppm 3 Unc
0.440 0.018
0.445 0.019
0.000 0.019
0.000 0.018
0.000 0.019
0.000 0.018
0.000 0.019
0.000 0.018
0.000 0.018
0.000 0.019
0.000 0.019
0.000 0.018
0.000 0.018
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.010
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.018
0.545 0.023
0.000 0.018
Methane
ppm Unc
129-3 1.9
139.9 2.1
189.6 2.7
184.4 2.6
189.1 2.7
182.1 2.6
189.5 2.6
187.2 2.6
187.3 2.6
189.9 2.7
188.1 2.6
182.4 2.6
178.9 2.6
174.3 2.7
177.4 2.7
179.0 2.7
181.4 2.8
183.0 2.8
184.2 2.8
184.1 2.8
178.6 2.7
74.3 1.2
179.9 2.6
179.9 2.6
180.3 2.6
178.2 2.6
125.2 2.0
178.5 2.6
CO
ppm Unc
337.9 20.3
354.1 23.6
438.4 27.5
417.3 27.3
425.0 27.9
421.0 27.7
441.9 27.1
437.0 27.0
436.8 27.3
438.5 27.8
434.0 27.9
424.2 27.6
419.4 27.7
385.4 30.0
389.7 30.3
392.5 30.5
396.6 30.8
396.8 30.9
399.5 30.7
396.8 30.8
387.2 30.4
196.0 14.5
397.0 28.4
396.9 28.4
395.8 28.4
392.0 28.2
325.6 22.0
402.3 28.1
Formaldehyde
ppm Unc
12.8 1.7
12.3 1.9
0.0 3.0
0.0 3.0
0.0 3.1
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 3.0
0.0 2.9
0.0 2.9
0.0 3.0
0.0 3.1
0.0 3.1
0.0 3.2
0.0 3.2
0.0 3.1
0.0 3.2
0.0 3.1
0.0 1.3
0.0 3.0
0.0 3.0
0.0 3.0
0.0 2.9
12.8 1.8
0.0 3.0
1 The samples indicated in bold type, "COOSP101, "COOSP102" and "COOSP107," were spiked with a mixture o f formaldehyde vapor, toluene vapor, and SF6. The spike
results are presented in Seciton 4.4, and the analyte spike procedure is discussed in Section 5.3.1.
2 Unc is th estimated uncertainty in the measurement.
3 SF6 was spiked as a tracer gas to determine to spike dilution. SF6 was not detected in the gas stream.
-------
TABLE B-l. Continued.
Date Time File name '
9/5/97
15:25
15:35
16:12
. 16:18
16:23
16:30
17:07
17:09
17:12
17:14
17:16
17:18
17:20
17:44
17:46
17:48
17:50
17:52
17:54
17:57
17:59
18:05
18:29
18:31
18:33
18:35
19:11 .
COOSP101
COOSP102
COOUN103
COOUN104
COOUN105
COOUN106
19050001
19050002
19050003
19050004
19050005
19050006
19050007
19050018
19050019
19050020
19050021
19050022
19050023
19050024
19050025
19050028
19050039
19050040
19050041
19050042
COOSP107
Average — >
3 -Methylepentane
ppm Unc 2
3.9 1.2
4J 1.4
5.6 1.7
5.4 1.7
5.6 1.7
5.5 1.7
5.9 1.7
5.8 1.7
5.8 1.7
5.8 1.7
5.8 1.7
5.6 1.7
5.4 1.7
5.3 1.7
5.4 1.7
5.5 1.8
5.5 1.8
5.6 1.8
5.6 1.8
5.6 1.8
5.4 1.8
2.1 0.8
5.5 1.7
5.5 1.7
5.5 1.7
5.4 1.7
7.8 0.7
5.4 1.7
1 -Pentene
ppm Unc
10.9 33
11.1 3.7
18.0 4.0
17.1 3.9
17.7 4.0
16.9 3.9
18.1 3.9
17.8 3.9
18.0 3.9
18.4 4.0
18.2 3.9
17.6 3.9
17.2 3.8
17.6 4.0
18.2 4.0
18.5 4.1
18.8 4.1
19.0 4.2
19.1 4.1
19.0 4.2
18.2 4.1
13.2 1.8
18.0 3.9
18.0 3.9
18.1 3.9
17.8 3.9
0.0 11.7
17.9 3.9
The samples indicated in bold type, "COOSP101, "COOSP102" and "COOSP107," were spiked with a mixture o f formaldehyde vapor, toluene vapor, and SF6. The spike
results are presented in Seciton 4.4, and the analyte spike procedure is discussed in Section 5.3.1.
2 Unc is th estimated uncertainty in the measurement.
3 SF6 was spiked as a tracer gas to determine to spike dilution. SF6 was not detected in the gas stream.
-------
Toluene Concentrations at Cooling Process (9/5/97)
25.0
20.0 -
15.0
B
a.
1
I
10.0
5.0
0.0
15:00
15:28 15:57 16:26 16:55 17:24 17:52 18:21 18:50 19:19
Time
-------
Ethylene Concentrations at Cooling Process (9/5/97)
16,0
14.0
12.0
10.0
i
Q,
£>
§ 8.0 -
JS
•**
H
6.0
4.0 -
2.0
0.0
15:00 15:28 15:57 16:26 16:55 17:24
17:52
18:21 18:50
19:19
Time
-------
200,0
Methane Concentrations at Cooling Process (9/5/97)
180.0
160.0
140.0
i
a.
&
120.0 -I
100.0
80.0
60.0
40.0
20.0 -
0.0
15:00
15:28
15:57
16:26
16:55
17:24
17:52
18:21
18:50
19:19
Time
-------
500.0
CO Concentrations at Cooling Process (9/5/97)
450.0
400.0
350.0
300.0 -
& 250.0
O
u
200.0
150.0
100.0
50.0 -
0.0
15:00
15:28
15:57
16:26
16:55
17:24
17:52
18:21
18:50
19:19
Time
-------
Formaldehyde Concentrations at Cooling Process (9/5/97)
14.0
12.0
10.0
8°
CL
&
I 6.0
•a
•a
4.0
2.0
0.0
-2.0
15:00 15:28 15:57 16:26 16:55 17:24
17:52
18:21
18:50 19:19
Time
-------
3-Methylpentane Concentrations at Cooling Process (9/5/97)
9.0
8.0
7,0
6.0
5.0
E
a.
&
4.0
3.0
2.0
1.0 -
0.0
15:00 15:28 15:57 16:26 16:55 17:24 17:52 18:21 18:50 19:19
Time
-------
1-Pentene Concentrations at Cooling Process (9/5/97)
25,0
20.0
15.0
S
a.
&
10.0
15:28 15:57 16:26
16:55 17:24
Time
17:52 18:21 18:50 19:19
-------
TABLE B-2. FTIR RESULTS FROM THE SHAKE-OUT HOUSING LINE
-------
TABLE B-2. FTIR RESULTS AT THE SHAKE-OUT HOUSING
Date Time File name '
9/5/97
15:51
16:05
16:42
16:50
16:55
17:00
17:22
17:24
17:27
17:29
17:31
17:33
17:35
17:37
18:10
18:12
18:14
18:16
18:18
18:20
18:22
1«:57
SHKSP101
SHKSP102
SHKUN103
SHKUN104
SHKUN105
SHKUN106
19050008
19050009
19050010
1905001 1
19050012
19050013
19050014
19050015
19050030
19050031
19050032
19050033
19050034
19050035
19050036
SHKSP107
Average — >
Toluene
ppm Unc 2
ll.i u
11.5 1.8
0.0 2.5
0.0 3.4
0.0 3.6
0.0 3.5
15.4 3.3
0.0 2.4
0.0 3.8
0.0 3.5
0.0 3.3
0.0 3.7
0.0 3.8
0.0 3.8
0.0 3.8
0.0 3.9
0.0 4.0
0.0 3.7
0.0 3.9
0.0 3.7
0.0 3.9
93 2,0
0.8 3.5
Hexane
ppm Unc
0.0 12.1
0.0 11. 8
3.0 0.2
0.0 17.1
0.0 18.0
0.0 17.4
0.0 21.9
0.0 12.2
0.0 18.8
0.0 17.4
0.0 16.6
0.0 1 8.3
0.0 18.8
0.0 18.8
0.0 19.1
0.0 19.2
0.0 20.1
0.0 18.6
0.0 19.3
0.0 18.4
0.0 19.2
0.0 11.8
0.2 17.3
Ethylene
ppm Unc
0.0 0.8
0.0 0.8
1.8 0.6
2.7 0.7
2.9 0.8
2.8 0.7
10.9 0.6
2.1 0.5
3.0 0.8
2.6 0.8
2.6 0.7
3.2 0.8
3.4 0.8
3.3 0.8
3.3 0.8
3.3 0.8
3.5 0.9
3.2 0.8
3.3 0.8
3.2 0.8
3.3 0.8
0,0 1.4
3.4 0.8
SF6
ppm Unc
0.464 0.016
0.479 0.016
0.000 0.014
0.000 0.017
0.000 0.018
0.000 0.018
0.000 0.014
0.000 0.012
0.000 0.019
0.000 0.018
0.000 0.017
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.019
0.000 0.020
0.000 0.020
0.000 0.019
0.000 0.020 _
0.000 0.019
0.000 0.020
0.605 0.026
0.000 0.018
Methane
ppm Unc
10.7 1.2
13.7 1.2
12.2 1.0
17.8 1.6
19.1 1.7
18.4 1.6
130.2 1.9
15.5 1.2
19.0 1.8
16.0 1.6
16.8 1.5
21.4 1.7
23.5 1.7
22.4 1.7
23.0 1.7
22.7 1.7
24.1 1.8
22.5 1.7
23.6 1.7
22.8 1.7
23.6 1.7
11.7 13.
26.0 1.6
CO
ppm Unc
91.1 133
93.4 12.8
78.1 13.8
96.9 17.8
96.2 18.3
94.8 17.9
331.7 21.9
76.1 13.0
102.7 20.1
100.5 19.0
97.2 18.4
104.1 19.9
106.1 20.4
102.4 20.4
91.4 20.2
98.6 20.6
97.5 21.2
85.8 19.7
89.4 20.4
90.2 19.8
86.9 20.3
703 13.2
106.7 19.1
Formaldehyde
ppm Unc
14.6 1.0
14.7 1.0
0.0 1.2
0.0 1.7
0.0 1.7
0.0 1.7
0.0 2.1
0.0 1.2
0.0 1.8
0.0 1.7
0.0 1.6
0.0 1.8
0.0 1.8
0.0 1.8
0.0 1.8
0.0 1.9
0.0 1.9
0.0 1.8
0.0 1.9
0.0 1.8
0.0 1.9
18.7 1.1
0.0 1.7
1 The samples indicated in bold type, "SHKSP101, "SHKSP102" and "SHKSP107,"
are presented in Seciton 4.4, and the analyte spike procedure is discussed in Section
were spiked with a mixture of formaldehyde vapor, toluene vapor, and SF6. The spike results
5.3.1.
2 Unc is th estimated uncertainty in the measurement.
3 SF6 was spiked as a tracer gas to determine to spike dilution. SFS was not detected in the gas stream.
-------
TABLE B-2. Continued.
Date Time File name l
9/5/97
15:51
16:05
16:42
16:50
16:55
17:00
17:22
17:24
17:27
17:29
17:31
17:33
17:35
17:37
18:10
18:12
18:14
18:16
18:18
18:20
18:22
18:57
SHKSP101
SHKSP102
SHKUN103
SHKUN104
SHKUN105
SHKUN106
19050008
19050009
19050010
19050011
19050012
19050013
19050014
19050015
19050030
19050031
19050032
19050033
19050034
19050035
19050036
SHKSP107
Average — >
3-Methylepentane
ppm Unc 2
0.0 1.0
0.0 1.0
0.0 0.9
4.2 •• 0.5
4.5 0.5
4.3 0.5
3.6 1.2
3.6 0.4
3.7 1.4
4.4 0.5
3.8 0.5
3.2 1.3
3.4 1.4
3.3 1.4
3.1 1.4
3.1 1.4
3.4 1.4
3.0 1.3
3.1 1.4
3.0 1.3
3.1 1.4
0.0 1.1
3.4 1.0
Butane
ppm Unc
0.0 3.9
0.0 3.8
0.0 2.8
0.0 4.0
0.0 4.3
0.0 4.1
0.0 24.9
0.0 13.9
4.8 4.5
0.0 4.1
0.0 3.9
5.3 4.3
5.7 4.4
5.6 4.4
5.6 4.4
5.7 4.5
6.1 4.7
5.5 4.3
5.7 4.5
5.4 4.3
5.7 4.5
0.0 3.8
3.2 5.8
1-Pentene
ppm Unc
0.0 6.1
0.0 6,1
0.0 6.4
0.0 8.8
0.0 9.3
0.0 9.0
17.5 2.9
0.0 6.3
0.0 9.7
0.0 8.9
0.0 8.5
0.0 9.4
0.0 9.7
0.0 9.7
0.0 9.8
0.0 9.9
0.0 10.3
0.0 9.6
0.0 9.9
0.0 9.5
0.0 9.9
0.0 6.1
0.9 8.8
2-Methyl-2butene
ppm Unc
6.4 1.0
6.6 1.0
0.0 0.9
8.2 1.2
8.9 1.2
8.5 1.2
0.0 6.3
6.8 0.9
9.5 1.4
8.5 1.2
6.9 1.1
7.8 1.3
8.5 1.4
8.3 1.4
7.5 1.4
7.5 1.4
8.3 1.5
7.0 1.3
7.3 1.4
6.9 1.3
7.2 1.4
8,4 1.1
7.0 1.5
1 The samples indicated in bold type, "SHKSP101, "SHKSP102" and "SHKSP107," were spiked with a mixture of formaldehyde vapor, toluene vapor, and SF6. The spike results
are presented in Seciton 4.4, and die analyte spike procedure is discussed in Section 5.3.1.
2 Unc is th estimated uncertainty in the measurement.
3 SF6 was spiked as a tracer gas to determine to spike dilution. SF6 was not detected in the gas stream.
-------
Toluene Concentrations at The Shakeout Housing (9/5/97)
18.0
16.0
14.0 -I
12.0
10.0
i
§ 8-0
e
H
6.0
4.0 -
2.0
0.0 -
-2.0
15
•MM*
:30
15:58
16:27
16:56
17:25
Time
17:54
18:22
18:51
19:20
-------
12.0
Ethylene Concentrations at The Shakeout Housing (9/5/97)
10.0
8.0 -
a 6.0
Ok
a
^»
« 4.0
2.0 -
0.0
-2.0
15:30 15:58 16:27 16:56
17:25
Time
17:54 18:22 18:51 19:20
-------
Methane Concentrations at The Shakeout Housing (9/5/97)
140.0
120.0
100.0
a.
&
4)
I
80.0
60.0
40.0
20.0 -
0.0
15
:30
15:58 16:27
16:56
17:25
Time
17:54 18:22
18:51
19:20
-------
CO Concentrations at The Shakeout Housing (9/5/97)
350,0
300.0
250,0
200.0
a
0.
&
O
u
150.0
100.0
50.0
0.0
15:30 15:58 16:27 16:56
17:25
Time
17:54
18:22 18:51
19:20
-------
Formaldehyde Concentrations at The Shakeout Housing (9/5/97)
23.0
18.0
13.0
4)
•o
o 8.0
u,
3.0
-2.0
Spiked Samples
15:30 15:58 16:27 16:56
17:25
Time
17:54 18:22 18:51 19:20
-------
3-Methylpentane Concentrations at The Shakeout Housing (9/5/97)
5.0
4.0 -
3.0
I 2.0
&
1.0
0.0
-1.0
15:30 15:58 16:27 16:56
17:25
Time
17:54 18:22 18:51 19:20
-------
7.0
n-Butane Concentrations at The Shakeout Housing (9/5/97)
6,0
5,0 -
4.0
I 3.0 -I
2.0 -
1.0 -
0.0
-1.0
15:30
15:58
16:27
16:56
17:25
Time
17:54
18:22
18:51
19:20
-------
1-Pentene Concentrations at The Shakeout Housing (9/5/97)
23.0
18,0
13.0
a
o.
&
8.0
3.0
-2.0
15:30
•MM*
15:58 16:27 16:56
17:25
Time
17:54 18:22 18:51 19:20
-------
11.0
2-Methyl-2-Butene Concentrations at The Shakeout Housing (9/5/97)
9.0
7.0
5.0
3.0
1.0
-1.0
15:30 15:58 16:27 16:56
17:25
Time
17:54 18:22 18:51 19:20
-------
TABLE B-3. FTIR RESULTS AT THE BAGHOUSE INLET
-------
TABLE B-3. FTIR RESULTS AT THE CUPOLA BAGHOUSE INLET
>aie Time File name
9/8/97
12:02 INLSP101
12:09 INLSP102
12:18 INLSP103
12:59 INLUN104
13:05 INLUN105
13:13 INLUN106
13:20 INLUN107
13:30 INLUN108
13:45 INLUN109
13:53 INLUN110
14:30 INLUNlll
14:35 INLUN112
14:40 INLUN113
15:21 INLUN114
15:27 INLUN115
15:33 INLUN116-
16:11 19080015
16:14 19080016
16:16 19080017
16:31 19080024
17:07 INLSP117
Average — >
HCl
ppm Uncertainty
17.58 2.37
17.11 2.15
3.80 0.52
31.73 3.15
30.94 3.22
34.37 3.32
29.57 3.23
41.78 3.45
27.15 3.23
27.25 3.26
31.64 3.27
34.65 3.08
32.32 3.08
30.83 3.53
29.90 3.29
31.63 3.27
43.96 3.59
43.10 3.59
41.10 3.57
27.81 3.38
12.99 2.15
33.51 3.32
Toluene
ppm Uncertainty
10.27 2.08
10.73 1.89
0.00 0.43
0.00 2.78
0.00 2.85
0.00 2.94
0.00 2.86
0.00 3.05
0.00 2.86
0.00 2.89
0.00 2.90
0.00 2.73
0.00 2.73
0.00 3.13
0.00 2.91
0.00 2.89
0.00 3.18
0.00 3.18
0.00 3.15
0.00 2.98
24.42 1.46
0.00 2.94
Methane
ppm Uncertainty
3.43 0.84
3,16 0.76
0.00 0.17
5.24 1.12
5.31 . 1.14
5.48 1.18
5.15 1.15
5.79 1,23
4,99 1.15
5,05 1.16
5.12 1.16
4.95 1.09
4.84 1.09
5.14 1.25
4.87 1.17
4.86 1.16
5.42 1.27
5.38 1.27
5.29 1.27
5.32 1.19
3.97 0.76
5.19 1.18
Formaldehyde
ppm Uncertainty
17.37 1.17
17.66 1.07
1.56 0.24
0,00 1.57
0.00 1.61
0.00 1.66
0.00 1.62
0.00 1.73
0.00 1.62
0.00 1.64
0,00 1.64
0.00 1.54
0.00 1.54
0.00 1.77
0,00 1.65
0.00 1.64
0.00 1.80
0.00 1.80
0.00 1.78
4.30 1.55
14.64 0.91
0.25 1.66
V,
-------
TABLE B-3. FTIR RESULTS AT THE CUPOLA BAGHOUSE INLET
)ate Time File name
9/9/97
7:49 INLSP201
9:55 INLUN202
10:03 INLUN203
10:11 INLUN204
10:52 INLSP205
11:01 INLSP206
11:09 INLUN207
11:20 INLUN208
12:00 19090001
12:03 19090002
12:05 19090003
12:07 19090004
12:09 19090005
12:11 19090006
12:13 19090007
12:16 19090008
12:52 19090023
12:54 19090024
12:56 19090025
12:59 19090026
13:01 19090027
13:03 19090028
13:05 19090029
13:07 19090030
13:09 19090031
13:12 19090032
13:14 19090033
13:16 19090034
HC1
ppm Uncertainty
7.74 2.52
33.77 3.53
35.02 3.58
33.29 3.62
12.62 2.68
25.69 3.85
22.85 4.55
18.72 3.61
18.49 3.15
19.77 3.16
20.61 3.17
21.24 3.14
21.67 3.13
22.17 3.14
22.60 3.12
23.19 3.14
24.18 3.53
25.19 3.57
25.79 3.60
26.36 3.62
27.41 3.59
29.70 3.64
31.42 3.66
32.28 3.64
32.84 3.65
33.68 3.68
34.50 3.73
34.82 3.85
Toluene
ppm Uncertainty
0.00 2.23
0.00 3.13
0.00 3.18
0.00 3.21
14.15 2.35
0.00 3.41
0.00 4.04
0.00 3.20
0.00 2.79
0.00 2.81
0.00 2.81
0.00 2.79
0.00 2.78
0.00 2.78
0.00 2.77
0.00 2.79
0.00 3.13
0.00 3.17
0.00 3.20
0.00 3.22
0.00 3.19
0.00 3.24
0.00 3.25
0.00 3.23
0.00 3.24
0.00 3.27
0.00 3.32
0.00 3.42
Methane
ppm Uncertainty
3.38 0.89
5.48 1.25
5.53 1.27
5.49 1.28
4.00 0.95
17.29 1.36
5.79 1.62
4.51 1.28
4.66 1.12
4.69 1.12
4.73 1.13
4.71 1.11
4.74 1.11
4.72 1.11
4.72 1.11
4.77 1.11
5.10 1.25
5.21 1.27
5.25 1.28
5.33 1.28
5.33 1.27
5.46 1.29
5.56 1.30
5.59 1.29
5.61 1.29
5.62 1.31
5.69 1.33
5.83 1.37
Formaldehyde
ppm Uncertainty
16.37 1.16
0.00 1.77
0.00 1.80
0.00 1.82
17.34 1.33
3.74 1.62
0.00 2.28
0.00 1.81
0.00 1.58
0.00 1.59
0.00 1.59
0.00 1.58
0.00 1.57
0.00 1.57
0.00 1.57
0.00 1.58
0.00 1.77
0.00 1.79
0.00 1.81
0.00 1.82
0.00 1.80
0.00 1.83
0.00 1.84
0.00 1.83
0.00 1.83
0.00 1.85
0.00 1.88
0.00 1.93
-------
TABLE B-3. FTIR RESULTS AT THE CUPOLA BAGHOUSE INLET
Dale Time File name
13:18 19090035
13:20 19090036
13:52 19090051
13:54 19090052
13:57 19090053
14:19 INSP209
Average — >
HCl
ppm Uncertainty
34.71 3.90
34.45 3.89
29.84 3.89
30.25 3,86
29.86 3.60
11.67 2.65
27.69 3.56
Toluene
ppm Uncertainty
0.00 3.46
0.00 3.46
0.00 3.46
0.00 3.42
0.00 3.19
15.61 2.32
0.00 3.16
Methane
ppm Uncertainty
5.87 1.39
5.85 1.38
5.63 1.38
5.64 1.37
5.35 1.28
4.08 0.94
5.28 1.27
Formaldehyde
ppm Uncertainty
0.00 1.96
0.00 1.95
0.00 1,96
0.00 1.94
0,00 1.81
18.60 1.31
0.00 1.79
-------
TABLE B-3. FTIR RESULTS AT THE CUPOLA BAGHOUSE INLET
Dale Time File name
9/10/97
7:53 INLSP301
8:37 INLUN3Q2
8:44 INLUN303
8:50 INLUN304
9:11 19100001
9:41 19100015
9:43 19100016
9:45 19100017
9:47 19100018
9:49 19100019
9:52 19100020
9:54 19100021
9:56 19100022
9:58 19100023
10:00 19100024
10:33 19100039
10:35 19100040
10:37 19100041
10:39 19100042
10:41 19100043
10:43 19100044
10:45 19100045
10:48 19100046
10:50 19100047
10:52 19100048
10:54 19100049
10:56 19100050
10:58 19100051
HC1
ppm Uncertainty
17.02 2.70
39.90 3.67
38.41 3.74
35.86 3.55
24.82 3.20
38.26 3,43
40.25 3.45
42.10 3.51
42.41 3.51
40.58 3.47
39.16 3.48
38.11 3.46
37.21 3.45
36.49 3.44
36.72 3.45
35.63 3.31
32.74 3.29
28.97 3.26
25.04 3.22
21.66 3.18
20.30 3.22
20.09 3.26
21.09 3.33
22.46 3.37
23.61 3.35
24.49 3.38
24.57 3.37
23.93 3.34
Toluene
ppm Uncertainty
12.51 2.37
0.00 3.25
0.00 3.31
0.00 3.14
0.00 2.84
0.00 3.04
0.00 3.06
0.00 3.11
0.00 3.11
0.00 3.08
0.00 3.08
0.00 3.07
0.00 3.06
0.00 3.05
0.00 3.06
0.00 2.93
0.00 2.91
0.00 2.88
0.00 2.85
0.00 2.82
0.00 2.85
0.00 2.89
0.00 2.94
0.00 2.98
0.00 2.96
0.00 2.99
0.00 2.99
0.00 2.96
Methane
ppm Uncertainty
3.93 0.95
5.12 1.30
5.12 1.33
4.72 1.26
5.29 1.14
5.50 1.22
5,56 1.23
5.67 1.24
5.65 1.25
5.51 1.23
5.47 1.23
5.41 1.23
5.34 1.23
5.31 1.22
5.32 , 1.23
4.92 1.17
4.78 1.17
4.62 1.16
4.41 1.14
4.29 1.13
4.20 1.14
4.21 1.15
4.32 1.18
4.40 1.19
4.41 1.19
4.46 1.20
4.40 1.19
4.33 1.18
Formaldehyde
ppm Uncertainty
16.24 1.34
0.00 1.84
0.00 1.87
0.00 1.78
0.00 1.61
0.00 1.72
0.00 1.73
0.00 1.76
0.00 1.76
0.00 1,74
0.00 1.74
0.00 1.74
0.00 1.73
0.00 1.73
0.00 1.73
0.00 1.66
0.00 1.65
0.00 1.63
0.00 1.61
0.00 1.59
0.00 1.61
0.00 1.63
0.00 1.67
0.00 1.69
0.00 1.68
0.00 1.69
0,00 1.69
0.00 1.67
-------
TABLE B-3. FTIR RESULTS AT THE CUPOLA BAOHOUSE INLET
Date Time File name
11:49 INLUN305
11:55 INLUN306
11:58 INLUN307
12:00 INLUN308
12:03 INLUN309
12:05 INLUN310
12:10 INLUN311
12:56 INLSP312
Average -->
HCl
ppm Uncertainty
36.39 3.19
25.60 3.00
22.57 2.96
20.30 2.95
17.37 2.92
15.92 2.90
15.49 2.97
7.24 1.95
29.66 3.31
Toluene
ppm Uncertainty
0.00 2.82
0.00 2.66
0,00 2.62
0.00 2.61
0.00 2.59
0.00 2.57
0.00 2.63
13.36 1.71
0.00 2.93
Methane
ppm Uncertainty
5.07 1.13
4.54 1.06
4.35 1.05
4.27 1.05
4.13 1.04
4.06 1.03
4.04 1.05
2.63 0.69
4.80 1.17
Formaldehyde
ppm Uncertainty
0.00 1.60
0.00 1.50
0.00 1.48
0.00 1.48
0.00 1.46
0.00 1.45
0.00 1.49
31.93 0.97
0.00 1.66
-------
TABLE B-4. FTIR RESULTS AT THE BAGHOUSE OUTLET
-------
TABLE B-4. FTIR RESULTS AT THE CUPOLA BAGHOUSE OUTLET.
)ate Time File name
9/8/97 12:30 ODTSPioi
12:41 OUTSP102
14:06 OUTUN103
14:11 OUTUN104
14:18 OUTUN105
14:47 OUTUN106
14:54 OUTON107
15:00 OUTUN108
15:05 OUTON109
15:12 OUTON110
15:41 19080001
15:43 19080002
15:46 19080003
15:48 19080004
15:50 19080005
15:52 19080006
15:54 19080007
15:56 19080008
15:59 19080009
16:01 19080010
16:03 19080011
16:05 19080012
16:22 19080020
16:24 19080021
16:26 19080022
16:29 19080023
16:57 ourspili
Average — >
HCl
ppm Uncertainty
15.24 2.59
3.63 0.60
20.97 2.90
22.67 2.91
23.28 2.93
22.02 3.04
21.36 3.19
21.39 3.11
21.56 2.99
21.24 3.00
20.78 3.33
21.94 3.39
22.29 3.41
22.49 3.41
21.90 3.41
21.77 3.41
21.96 3.41
22.21 3.42
21.99 3.40
22.41 3.40
22.81 3.38
23.12 3.38
29.85 3.42
30.04 3.44
29.91 3.44
29.32 3.43
14.33 2.41
23.30 3.27
Toluene
ppm Uncertainly
7.59 2.27
0.00 0.50
0.00 2.57
0.00 2.58
0.00 2.60
0.00 2.69
0.00 2.82
0.00 2.75
0.00 2.65
0.00 2.66
0.00 2.95
0.00 3.00
0.00 3.02
0.00 3.02
0.00 3.02
0.00 3.02
0.00 3.02
0.00 3.03
0.00 3.01
0.00 3.01
0.00 2.99
0.00 2.99
0.00 3.03
0.00 3.04
0.00 3.04
0.00 3.04
21.20 1.63
0.00 2.90
Methane
ppm Uncertainly
3.26 0.92
0.00 0.20
4.58 1.03
4.61 1.03
4.63 1.04
4.65 1.08
4.77 1.13
4.63 1.10
4.48 1.06
4.44 1.06
4.73 1.18
4.83 1.20
4.85 1.21
4.86 1.21 •
4.79 1.21
4.76 1.21
4.76 1.21
4.75 1.21
4.73 1.20
4.73 1.20
4.73 1.20
4.75 1.20
4.95 1.21
4.95 1.22
4.94 1.22
4.88 1.22
4.13 0.85
4.74 1.16
Formaldehyde
ppm Uncertainty
14.95 1.28
1.68 0.28
0.00 1.45
0.00 1.46
0.00 1.47
0.00 1.52
0.00 1.59
0.00 1.55
0.00 1.50
0.00 1.50
0.00 1.67
0.00 1.70
0.00 1.71
0.00 1.71
0.00 1.71
0.00 1.71
0.00 1.71
0.00 1.71
0.00 1.70
0.00 1.70
0.00 1.69
0.00 1.69
0.00 1.71
0.00 1.72
0.00 1.72
0.00 1.72
12.93 1.01
0.00 1.64
-------
TABLE B-4. FTIR RESULTS AT THE CUPOLA BAGHOUSE OUTLET.
)ate Time File name
9/9/97 8:02 OUTSP201
8:26 OUTSP202
9:27 OUTUN203
9:33 OUTUN204
9:40 OUTUN205
9:47 OUTUN206
10:19 OUTUN207
10:33 OUTSP208
10:41 OUTUN209
11:31 OUTUN210
11:37 OUTUN211
12:24 19090011
12:26 19090012
12:28 19090013
12:33 19090014
12:35 19090015
12:37 19090016
12:39 19090017
12:41 19090018
12:44 19090019
12:46 19090020
13:27 19090039
13:29 19090040
13:31 19090041
13:33 19090042
13:35 19090043
13:37 19090044
13:39 19090045
13:42 19090046
13:44 19090047
13:46 19090048
Average — >
HCl
ppm Uncertainty
10.80 2.68
1.65 0.42
18.03 3.26
20.30 3.20
21.34 3.22
21.33 3.22
21.10 3.35
14.80 2.56
18.78 3.46
12.43 3.42
12.04 3.24
16.08 4.81
13.23 3.09
13.66 3.18
13.94 3.23
13.88 3.23
13.96 3.27
14.18 3.31
14.00 3.31
13.67 3.30
13.70 3.32
17.22 3.58
17.22 3.52
17.36 3.52
17.35 3.57
16.85 3.50
16.90 3.47
17.17 3.50
17.00 3.46
17.13 3.45
18.07 3.75
16.30 3.39
Toluene
ppm Uncertainty
0.00 2.36
0.00 0.33
0.00 2.90
0.00 2.85
0.00 2.86
0.00 2.86
0.00 2.97
11.22 2.24
0.00 3.06
0.00 3.03
0.00 2.87
0.00 4.26
0.00 2.75
0.00 2.82
0.00 2.87
0.00 2.87
0.00 2.90
0.00 2.94
0.00 2.94
0.00 2.93
0.00 2.95
0.00 3.18
0.00 3.12
0.00 3.13
0.00 3.17
0.00 3.10
0.00 3.08
0.00 3.11
0.00 3.07
0.00 3.06
0.00 3.33
0.39 3.01
Methane
ppm Uncertainty
3.47 0.95
0.00 0.13
5.04 1.16
4.98 1.14
5.01 1.14
5.00 1.14
4.93 1.19
3.79 0.90
4.81 1.23
4.33 1.21
4.09 1.15
6.95 1.71
4.54 1.10
4.64 1.13
4.67 1.15
4.67 1.15
4.69 1.16
4.72 1.18
4.71 1.17
4.69 1.17
4.70 1.18
5.12 1.27
5.06 1.25
5.06 1.25
5.10 1.27
5.02 1.24
5.00 1.23
5.02 1.24
5.00 1.23
4.96 1.22
5.25 1.33
4.88 1.20
Formaldehyde
ppm Uncertainty
13.38 1.23
1.23 0.19
0.00 1.64
0.00 1.61
0.00 1.62
0.00 1.62
0.00 1.68
14.10 1.27
0.00 1.73
0.00 1.71
0.00 1.62
0.00 2.41
0.00 1.55
0.00 1.60
0.00 1.62
0.00 1.62
0.00 1.64
0.00 1.66
0.00 1.66
0.00 1.66
0.00 1.67
0.00 1.80
0.00 1.77
0.00 1.77
0.00 1.79
0.00 1.76
0.00 1.74
0.00 1.76
0.00 1.74
0.00 1.73
0.00 1.88
0.00 1.70
-------
TABLE B-4, FT1R RESULTS AT THE CUPOLA BAGHOUSE OUTLET,
Jale Time File name
9/10/97 8:03 OUTSBOi
8:19 OUTON302
8:25 OUTUN303
8:31 OUTON304
9:13 19100002
9:15 19100003
9:17 19100004
9:19 19100005
9:21 19100006
9:24 19100007
9:26 19100008
9:28 19100009
9:30 19100010
9:32 19100011
10:07 19100027
10:09 19100028
10:11 19100029
10:13 19100030
10:15 19100031
10:17 19100032
10:20 19100033
10:22 19100034
10:24 19100035
10:26 19100036
11:20 OUTUN305
11:26 OUTUN306
11:35 OUTON307
11:41 OUTUN308
12:18 OUTUN309
12:21 OUTUN310
12:24 OUTUN311
12:29 OUTUN312
12:31 OUTON313
12:33 OUTUN314
12:36 OUTUN315
12:48 OUTSP316
Average -->
HCl
ppm Uncertainly
15.73 2.71
19.45 3.18
20.97 3.34
21.67 3.36
25.50 3.21
26.02 3.21
26.29 3.19
26.47 3.19
27.13 3.21
28.19 3.22
28.71 3.20
28.96 3.22
28.59 3,25
28.79 3.25
27.90 3.23
27.98 3.19
27.34 3,13
26.53 3.11
25.42 3.09
24.07 3.06
22.81 3.04
21.97 3.03
21.62 3.02
22,64 3.04
16.00 2.92
19.13 2.92
21,27 2.98
22.53 3.05
13.41 2.96
13.98 2,96
14.70 2.97
15.18 3.05
15.32 3.10
15.43 3.09
15.72 3.08
10,09 2.29
22.58 3.12
Toluene
ppm Uncertainty
9.98 2.37
0.00 2.81
0.00 2.96
0.00 2.97
0.00 2.85
0.00 2.85
0.00 2.84
0.00 2.83
0.00 2.85
0.00 2.86
0.00 2.84
0.00 2.86
0.00 2.88
0.00 2.88
0.00 2.86
0.00 2.83
0.00 2.77
0.00 2.76
0.00 2.74
0.00 2.71
0.00 2.69
0.00 2.68
0.00 2.67
0.00 2.69
0.00 2.59
0.00 2.59
0.00 2.65
0.00 2.71
0.00 2.62
0.00 2.62
0.00 2.63
0.00 2.70
0.00 2.75
0.00 2.73
0.00 2.73
10.73 2.01
0.00 2.76
Methane
ppm Uncertainty
3.69 0.96
4.17 1.13
4.43 1.18
4.39 1.19
5.32 1.14
5.32 1.14
5.30 1.13
5.27 1.13
5.27 1.14
5.30 1.14
5.27 1.14
5.29 1.14
5.30 1,15
5.29 1.15
4.93 1.15
4.86 1.13
4.83 1.11
4.76 1.11
4.69 1.10
4.57 1.09
4.49 1.08
4.43 1.07
4.40 1.07
4.42 1.08
4.49 1.04
4.55 1.04
4.67 1.06
4.80 1.08
4.25 1.05
4.23 1.05
4.26 1.05
4.37 1.08
4.42 1.10
4.40 1.10
4.43 1.09
3.13 0.81
4.74 1.11
Foim aldehyde
ppm Uncertainty
13.96 1.34
0.00 1.59
0.00 1.67
0.00 1.68
0.00 1.61
0.00 1.61
0.00 1.60
0.00 1.60
0.00 1.61
0.00 1.62
0.00 1.61
0.00 1.62
0.00 1.63
0.00 1.63
0.00 1.62
0.00 1.60
0.00 1.57
0.00 1.56
0.00 1.55
0.00 1.53
0.00 1.52
0.00 1.51
0.00 1.51
0.00 1.52
0.00 1.47
0.00 1.46
0.00 1.50
0.00 1.53
0.00 1.48
0.00 1.48
0.00 1.49
0.00 1.53
0.00 1.56
0.00 1.55
0.00 1.54
25.75 1.13
0.00 1.56
-------
B-2. FTIR FIELD DATA RECORDS
-------
PROJECT NO. 4781-Qi.Qg
PLANT: Waunaca Foundar» Inc.
FTIR FIELD DATA FORM
(FTIR Sampling Dat*)
DATE:
9/4/97
BAROMETRIC: 758 mm
OPERATOR: LMH
SAMPLE
TIME
19:11
FILE
NAME
BKGOSKMb
CTSOSKMa
PATH
"Jilrogen in cell
20 ppm eihylene
_
NUMBER
SCANS
500
250
RES
(«•-!>
2
2
«
CELL
TEMP(F)
130C
130C
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
•KG
BKG0904b
V)
-------
PROJECT NO. 4701-08-08
PLANT: Wauoaca Foundar? Inc.
FTIR FIELD DATA FORM
(FTIR Stmpiing D*t»)
DATE:
9/5/97
BAROMETRIC: 755 mm Hg
OPERATOR:
SAMPLE
TIME
9:30
9:45
9:53
9:55
10:00
10:11
10:15
10:54
11:20
13:15
13:30
13:53
14:10
14:20
14:24
15:00
15:23
FILE
NAME
BKG0905a
BKGCHK01
CTS0905a
CTS0905b
SF60905a
SF60905b
TOL0905a
SFTOL01
BKO0905b
SF60905c
SF60905d
SP60905e
FORMAL01
SFTOL02
N20NLY01
BKG0905c
COOSP10I
PATH
20m
20m
Imogen flowing
M2 only as nitrogen absorbance
20 ppm ethylene
20 ppm ethylene
>ak check- tell at vacuum
4 ppm SF6 - direct to cell
4 ppm SF6 - direct to cell
Toluene 60 ppm - direct to cell
frocessdown
SP6 through IdiHek at 1 1pm and mixed with
toluene at 1 1pm, formaldehyde only been in
oven for 90 mm @ 100C
(Bad leak in Kintek)
N2
SF6 @4.97 1pm to spike line
Shakeout - sample rale @ 4.0 1pm
5P6 (5)4.97 1pm - sample rale <§> 4,0 1pm
Spike line ** Kintek was venting -VOID samples
SP6 @ 5.00 Ipm - sample rale @ 4.0 1pm
Process restarted - Computer clock is 1-hr
ahead of recorded limes
Refilled Dewar
Formaldehyde in N2 - direct to cell
NUMBER
SCANS
500
250
250
250
250
250
500
250
250
250
250
1.0 1pm @ 100C - Permeation tube=94,OOOnanoL/min (-90 ppm)
Serial* 22 14
SF6 4 ppm Cg> 1 1pm into Kintek
Toluene 60 ppm, 1 1pm into MFC
formaldehyde @ 100C and I 1pm
N2only
Background - N2 only
Probe inserted in cooling slack w/ spike
Cooling slack
Spiking W/SF6 (4ppm) and formaldehyde at 1.0 1pm
and 100C and toluene (60ppm) @ 1 .0 Ipm
cell flow = 3.5 1pm, vent flow = 2 1pm
250
250
500
250
RES
(CB-l)
2
2
2
2
2
2
2
2
»
2
" 2
2
2
2
2
2
CELL
TEMP (ft
130C
130C
130C
130C
130C
130C
I30C
I30C
130C
130C
DOC
130C
130C
130C
130C
SPIKED/
UNSPIKED
spike
spike
spike
spike
spike
SAMPLE
COND.
-
SAMPLE
FLOW
5 1pm
5 Ipm
5 Ipm
5 1pm
51pm
5 1pm
5 1pm
51pm
5 1pm
5 lorn
1 1pm
2 1pm
51pm
5 1pm
3.5 1pm
BKti
BKG0905a
BKG0905a
BKG0905a
BKG0905a
BKG0905a
BKG0905b
BKG0905b
BKG0905b
BKG0905b
BKG0905b
BKG0905b
BKG0905t
-------
PROJECT NO. 4701-08-08
PLANT: Waupaca boundary Inc.
FTIR FIELD DATA FORM
(FT1R Sampling Data)
DATE:
9/5/97
BAROMETRIC; 755 mm Hi-
OPERATOR:
SAMPLE
TIME
15:33
15:37
15:39
16:02
16:11
16:15
16:21
16:27
16:41
16:48
16:53
16:58
17:05
17:21
17:38
17:41
17:58
FILE
NAME
COOSP102
SHKSP101
SHKSP102
COOUN103
COOUN104
COOUN105
COOUN106
SHKUN103
SHKUN104
SHKUN105
SHKUN106
19050001
1905007
1905008
1905009
19050010
19050015
19050016
19050017
19050018
19050025
19050026
19050027
PATH
20m
20m
20m
20m
20m
20m
20m
20m
Pooling w/spike
Shake out - probe in stack with spike
Stakeout w/spike
same spike
Stakeout w/spike
Pooling line only
Coding line only
Pooling line only
Pooling line only
Stakeout line
Shakeout line
Shakeoul line
Stakeout line
Stan continuous process software
Cooling
Slop - last good file
Change to shakeout
Evacuated cell
Shakeout
Stop
Switch lines and evacuate cell
Switch lines and evacuate cell
Continuous Software
Cooling line
Stop
Change line - Evacuate cell
Change line - Evacuate cell
NUMBER
SCANS
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
RES
(cm-!)
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
CELL
TEMP (F)
130C
130C
130C
130C
130C
130C
130C
130C
130C
130C
130C
130C
130C
130C
274
274
274
SPIKED/
IJNSP1KED
spike
spike
spike
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
SAMPLE
CON0.
cooling line
cooling line
cooling line
' cooling Hue
shakeout
shakeout
shakeout
shakeout
shakeoul
shakeout
shakeou
SAMPLE
FLOW
5 1pm
5 1pm
5 1pm
5 1pm
5 Ipm
51pm
5 1pm
5 1pm
5 1pm
5 1pm
51pm
5 1pm
5 Ipm
5 1pm
BKG
BKG 0905c
BKG 0905c
BKG 0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
-------
PROJECT NO. 47U1-OJH3
PLANT: Waupaca Foundarv Inc.
FTIR FIELD DATA FORM
(FT1R Sampling Data)
DATE:
BAROMETRIC: 755 mm He
OPERATOR:
SAMPLE
TIME
18:03
18:07
18:29
18:35
18:50
19:11
19:23
19:31
19:38
19:45
FILE
NAME
19050028
19050030
19050036
19050037-38
19050039
1905042
SHKSP107
COOSP107
SFTOL03
N20NLY02
CTS0905c
BKG0905d
PATH
Cooling e*~BAD**)
•teevacuale cell
Shakeout
Slop
Change line - Evacuate cell
Cooling line
Stop
Shakeout w/spike
spike is SF6 (4ppm) @ 1 .0 1pm
formaldehyde @ 1 OOC @ 1 .0 1pm
Toluene (60 ppm) @ 1.0 1pm
Sample rale 3,0 1pm
venl - 1 .0 1pm
Cooling line w/spike
Spike = 1.0 Ipm SP6 in formaldehyde @ 100C
w/1 .0 1pm toluene (Toluene is 60 ppm and SP6
is 4 ppm)
Direct to cell •
spike mix 1.0 1pm SF6 @ 4 ppm
and 1 .0 1pm toluene
and formaldehyde @ 100C
Formaldehyde @ ~ 94,000 nanoL/min
N2 only direct to cell
Ethylene 20 gpm
N2 only - Background
NUMBER
SCANS
250
250
250
250
250
250
250
250
500
RES
(crn-1)
2
2
2
2
2
2
2
2
2
CELL
TEMP(F)
274
274
274
274
274
274
274
274
274
SPIKED/
UNSPIKED
UN
UN
UN
spike
spike
spike
UN
SAMPLE
COND.
SAMPLE
FLOW
5 1pm
5 1pm
5 Ipm
3.0 1pm
3.0 1pm
2.0 1pm
5.0 Ipm
5.0 Ipm
5.0 1pm
BKG
0905c
0905c
0905c
0905c
0905c
0905c
0905c
0905c
-------
PROJECT NO. 4701-08-OE
PLANT: Waupuca Foundarv Inc.
FTIR FIELD DATA FORM
(FTIR Sampling Data)
DATE:
9/8/97
BAROMETRIC: 747 mm Hy
OPERATOR: LMH
SAMPLE
TIME
9:45
10:24
10:36
10:45
10:SO
10:59
11:07
12:02
._
12:09
12:18
12:27
12:40
12:46
PILE
NAME
BKG0908a
N2ONLY03
CTS0908a
CTS0908b
SFTOL04
SFTOL05
1NLSP101
INLSP102
INLSP103
OUTSP101
OUTSP102
BKG0908b
PA™
20m
20m
Detector filled
lackgraund - N2 only
N2only
20 ppm Ethylene
20 ppm Elhylene
Changed filler line #2 - inlet flow = 12 Ipm
Direct to cell spike
SF6 4 ppm @ 1 .0 1pm
w/ formaldehyde @ 1 OOC and toluene 60 ppm
6) 1 .0 Ipm (toluene = 60.6 ppm) from Scott
gas cylinder #ALM052730 MRI POt 029872
NUMBER
SCANS
500
250
250
250
250
RES
(OB-I)
2
2
2
2
2
(FORMALDEHYDE ABSORBANCE WAS LESS THAN 9/5/97)
same as above
Spike lo inlet - formaldehyde OK
Cell flow = 3,0 1pm
Vent flow = 2.0 1pm
same as above
N2 only - flood N2 into line
spike = 10 1pm of N2 only
(line #1 = outlet, Line 12 = inlet)
inlet and outlet leak checks good
Spike w/toluene 60 ppm @ 1 .0 Ipm
formaldehyde @ 100C and SF6 @ \ .0 Ipm
cell flow = 3.0 1pm
vent flow = 2.0 1pm - OUTLET
N2 only - Sample line
Outlet sample line
Background - N2 direct lo cell
250
250
250
250
250
250
500
2
2
2
- 2-
2
2
2
CELL
TEMP(F)
274
274
274
274
274
274
274
274
274
275
275
275
SPIKED/
UNSPIKED
-
SP
SAMPLE
COND.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
SAMPLE
FLOW
5.0Ipm
5.0 Ipm
5.0 1pm
5.01pm
2.0 Ipm
2.0 1pm
3.01pm
... -
3.01pm
3.0 Ipm
3.01pm
5.0 Ipm
5.0 1pm
BKG
BKO0908a
BKO0908a
BKG0908a
BKG0908a
BKG0908a
BKG0908a
BKG0908a
BKG0908a
BKG0908a
BKG0908a
-------
PROJECT NO. 4701-08-08
PLANT: Waunaca Foundarv IDC.
FTIR FIELD DATA FORM
(FTIR Sampling Date)
DATE:
BAROMETRIC: 747 mm HE
OPERATOR: LMH
SAMPLE
TIME
12:56
13:02
13:10
13:1?
13:27
13:28
13:42
13:49
14:04
14:09
14:15
14:28
14:33
14:38
14:45
14:51
14:58
15.03
15:09
15:18
15:23
15:25
15:30
FILE
NAME
1NLUN104
INLUN105
INLUN106
INLUN107
INLUN108
INLUN109
INLUNHO
OUTUN103
OUTUN104
OUTUN105
INLUN111
INLUN112
1NLUN113
OUTUN106
OUTUN107
OUTUN108
OUTUN109
OUTUN110
1NLUN114
INLUN115
INLUN116
PATH
nlci sample
Inlet sample
Inlet sample
inlet sample
inlet sample
Shut probe box of outlet down to check pilots
Changed outlet probe
Inlet sample
Inlet sample
Outlet
Outlet
Outlet
Inlet
Inlet
Inlet
Outlet
Outlet
Outlet
Owlet
Gimlet
Inlet
Refilled dewar
Inlet
Inlet
NUMBER
SCANS
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
' RES
(cm-1)
2
2
2
2
2
2
2
2
2
2
2
2
2
2
- 2
2
2
2
2
2
2
CELL
TEMP (F)
274
274
274
274
274
274
274
275
275
275
274
274
274
274
274
274
274
274
274
274
274
SPIKED/
UNSPIKED
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
SAMPLE
COND.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
SAMPLE
FLOW
5.0 1pm
5.0 1pm
5.0 Ipm
5.0 Ipm
5.0 1pm
5.0 Ipm
5.0 1pm
5.0 Ipm
5.01pm
5.0 1pm
5.0 ipm
5.0 1pm
5.0 Ipm
5.0 Ipm
5.0 1pm
5.0 Ipm
5.0 1pm
5.0 1pm
5.0 Ipm
5.0 1pm
5.01pm
BKC
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
0908b
09086
0908b
0908b
-------
PROJECT NO. 4701-08-08
PLANT: Wnupaca Foundarv inc.
FTIR FIELD DATA FORM
(FUR Sampling D»ti)
DATE:
BAROMETRIC: 747 mm Hg
OPERATOR; LMH
SAMPLE
TIME
15:39
16:04
16:09
16:15
16:28
16:39
16:55
17:05
17:11
17:21
17:10
17:13
17:28
17:33
17:39
FILE
NAME
19080001
19080012
19080015
19080017
19080018-19
19080020
19080023
BKG0908c
OUTSPlll
INLSP117
CTS0908c
SFTO106
N2ONLY04
OUTAIR01
INAIR01
PATH
Outlet stait continuous sampling
Outlet
Stop
Change to inlet evacuate 19080013 and 19080014
Inlet
Slop
evacuate cell
Outlet - Continuous software
Stop
N2 only - Background
Spike - loluene 60 ppm @ 2.0 1pm
SF6 4 ppm @ 1 .0 1pm and formaldehyde @ 100C
loluene high in this spike
Spike - same as above
Elhylene 20 ppm, direct lo cell
Spike direct to cell
Same as spikes above
Toluene, 60 ppm @ 2.0 1pm
SF64ppm@ 1.01pm
Formaldehyde @100C
Probes pulled out of slack
Inlet and outlet pass leak check
N2Only
Air only
Air only
NUMBER
SCANS
250
250
250
500
500
250
250
250
250
RES
(cm-1)
2
2
2
2
2
2
2
2
2
CELL
TEMP (F)
274
274
273
274
274
274
274
274
274
SPIKED/
UNSP1KED
UN
UN
UN
UN
spike
spike
SAMPLE
COND.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
SAMPLE
FLOW
5.0 Ipm
5.0 Ipm
5.01pm
5.0 Ipm
5.0 Ipm
5.0 Ipm
5.0 1pm
5.0 1pm
5.0 1pm
BK<;
0908b
0908b
0908b
0908c
0908c
0908c
0908c
0908c
-------
PROJECT NO. 4701-08-08
PLANT: Waupxca Foundarv Inc.
FTIR FIELD DATA FORM
(FT1R Sampling Data)
DATE:
919197
BAROMETRIC: 745 mm Hy
OPERATOR:
SAMPLE
TIME
7:10
7:15
7:22
7:27
7:37-
7:47
8:00
8:11
8:24
8:57
9:06
9:25
9:31
9:36
9:44
9:54
10:00
10:08
10:16
10:30
10:39
10:30
FILE
NAME
EVC0908
BKG0909a
CTS0909a
INSP201
OUTSP201
SPT0909a
OUTSP202
BKO0909b
BKO0909c
OUTUN203
OUTUN204
OUTUN205
OUTUN206
INLUN202
INLUN203
1NLUN204
OUTUN207
OUTSP208
OUTUN209
PATH
20m
Jassed inlet and outlet check
liled detector
Evacuated cell - 0,9 nun Hg
background
ilhylene 20 ppm
Inlet - spike
SF6 - 4ppm @ 2,0 1pm
with formaldehyde @ 100C
Cell flow = 3,0 1pm, vent flow = 2.0 1pm
Outlet spike
same as above (no toluene)
Cell leak check @ vacuum 0.6 mmHg in 60 sec
Spike direct lo cell
same as mix above {no toluene)
N2 only in line , OUTLET .
N2 only, background
N2 only, background
Outlet
Outlet
Outlet
Outlet
Purge and evaluate
INLET
INLET
INLET
Outlet
Outlet spike
Toluene, 60 ppm @ 1.0 1pm
SF6, 4ppm @ 1.0 1pm w/form @ 100C
Cell flow = 3. Olpm
Vent flow = 3.0 Ipm
Outlet only
Manual sampling started
NUMBER
SCANS
250
500
250
250
250
250
250
500
500
250
250
250
250
250
250
250
250
250
250
RES
(«*•«
2
2
2
2
2
2
2 "
2"
2
2
2
2
2
2
2
2
2
2
CELL
TEMP(F)
275
274
274
274
274
274
274
274
275
275
275
275
275
275
275
275
275
275
SPIKED/
UNSPIKED
SP
SP
SP
SP
UN
UN
UN
UN
UN
UN
UN
UN
spike
UN
SAMPLE
CON0.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
SAMPLE
FLOW
5.0 Ipm
5.0 1pm
3.01pm
3.01pm
3.01pm
3.0 Ipm
5.01pm
5.0 1pm
5.0 Ipm
5.0 Ipm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 Ipm
5.0 1pm
5.01pm
3.0 Ipm
3.0 1pm
BKG
0908c
0909a
0909a
0909a
0909a
0909a
0909c
0909c
0909c
0909c
0909c
0909c
0909c
0909c
0909c
0909t
-------
PROJECT NO.
PLANT: Hi
FTIR FIELD DATA FORM
(FT1R Sampling Data)
DATE:
y/y/97
BAROMETRIC: 745 mm Hy
OPERATOR: LMH
SAMPLE
TIME
10:50
11:00
11:00
11:08
11:17
•11:24
11:28
11:34
11:44
11:50
11:57
12:24
12:46
12:50
13:20
13:24
13:46
13:50
13:56
14:05
14:11
14:29
14:36
14:49
14:57
15:05
15:13
15:25
FILE
NAME
1NLSP205
1NSP207
INUN207
1NUN208
OUTUN2IO
OUTUN2I1
NIT0909a
BKGMOM
19090001
19090008
19090009
19090010
19090011
19090012
19090020
19090023
19090036
19090037-38
19090039
19090048
19090051
19090053
OUTSP112
INSP209
SFT0909b
TOL0909a
FRM0909a
CTS0909b
OUTAK02
INLAIR02
BKQ0909e
PATH
nleupikt
•1 inlet probe box
toluene = 1.0 Ipm, SF6 = 1.0 Jpm, form = 100C
Cell flow = 3.0 1pm, vent = 2,0 Ipm
nlrt only - No spike
"rooeii weal to lower production
Inlet
Inlet
Refilled N2 detector
Outlet
Outlet
1 OlpmanJ
SR>. 4ppm w/fonnaldehyde perm tube @ 100C
NUMBER
SCANS
250
250
250
250
250
500
250
250
250
250
250
250
carried at 1.0 Ipm, cell flow -2.0 Ipm, vent flow = ZO 1pm
Outlet pulled from stack - passed leak check
Inlet spike (same as above)
Spike - direct to cell (same as above)
Toluene, 60 ppm, direct
Formaldehyde <§) 1 .0 1pm and 100 C
Fthylcne. 20 ppm
Outlet - air through
Inlet air sample line
N2oruy
250
250
250
250
250
250
500
EES
(c»-I)
2
2
2
2
2
2
2
2
2
2
2
2
2
. 2
2
2
2
2
2
CELL
TEMP (F)
275
274
274
274
274
275
275
275
275
275
275
274
274
274
274
274
275
275
274
SPIKED/
UNSPIKED
SP
UN
UN
UN
UN
UN
UN
UN
UN
SP
SP
SP
SP
SP
SAMPLE
COND.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
static
dynamic
SAMPLE
FLOW
3.01pm
3.01pm
3.0Ipm
3.01pm
3.01pm
5.01pm
5.01pm
5.01pm
5.01pm
5.01pm
5.01pm
2,01pm
2.01pm
2.01pm
1,01pm
5.01pm
5.0 1pm
BKG
0909c
0909c
0909c
0909c
0909c
0909d
0909d
0909d
0909d
0909d
0909d
0909d
0909d
0909d
090W
0909d
0909d
-------
PROJECT NO, 4701-QS-08
WaiumcaFoundarvIiic.
FTIR FIELD DATA FORM
(FT1H Sampling D*t»)
DATE:
9/10/97
BAROMETRIC: 74S mm He
OPERATOR: LM|J
SAMPLE
TIME
7:20
7:30
7:38
7:49
8:00
8:04
8:10
8:10
8:15
8:22
8:27
8:34
8:41
8:47
8:55
9:00
9:07
9:31
9:40
9:59
10:05
10:25
10:29
10:58
11.05
11:17
11:23
11:32
11:37
FILE
NAME
BKG0910a
CTS0910a
INLSP301
OUTSP301
SFTO910a
OUTUN302
OUTUN303
OUTUN304
INLUN302
INLUN303
INLUN304
N20910a
BKG0910b
19100001
19100011
1910012-14
1910015
1810024
1910027
1910036
1910039
1910051
BKQ0910c
OUTUN305
OUTUN306
OUTUN307
OUTUN308
PATH
Lxak check inlet and outlet
^2 only background
3lhykrnc 20 ppm
Spike -Inlet
SF6 4ppm @ 1 .0 1pm w/form @ 1 OOC
and toluene 60 ppm @ 1 .0 1pm
Cell = 2.5 1pm, vent = 2.0 1pm
Spike - outlet (same as above)
Cell leak check under vacuum 1 mm Hg in 99sec
Direct to cell spike (same as above)
Manual sampling started
Outlet
Outlet
Outlet
Inlet
Inlet
Inlet
N2 only
Background
Outlet - continuous software
Stop
Evacuate cell
Inlet
Slop
Outlet
Stop
Inlet
Stop
N2 only - background
Outlet
Outlet
Outlet
Outlet
NUMBER
SCANS
500
250
250
250
250
250
250
250
250
250
250
250
500
250
250
250
250
500
250
250
250
250
RES
(cm-1)
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
CELL
TEMP(F)
274
274
274
274
274
274
274
274
274
274
274
275
275
275
275
275
275
275
275
275
275
SPIKED/
UNSPIKED
SP
SP
SP
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
UN
SAMPLE
COND.
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
dynamic
SAMPLE
FLOW
5.0 1pm
5.0 ipm
2.5 Ipm
2.5 1pm
2.0 Ipm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 Ipm
5.0 Ipm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 1pm
5.0 Ipm
5.01pm
5.0 1pm
5.0 Ipm
5.0 1pm
BKC
0910a
0910a
091 Oa
091 Oa
0910a
091 Oa
0910a
0910a
0910a
0910a
0910b
0910b
091 Ob
0910b
0910c
0910c
091 Oc
09 10i:
091 Oc
-------
PROJECT NO. 4701-01-08
PLANT: Waiipaca I oundarv inc.
FTIR FIELD DATA FORM
(FTIR Sampling D*t»)
DATE; 9/10/9?
BAROMETRIC: 745 mm US
OPERATOR: LMH
SAMPLE
TIME
11:45
11:52
11:55
11:57
12:00
12:02'
12:07
12:15
12:18
12:20
12:25
12:28
12:30
12:33
12:45
12:53
13:04
13:11
13:18
13:26
FILE
NAME
1NUN30S
1NUN306
INUN307
INUN308
INUN309
INUN310
INUN311
OUTUN309
OUTUN310
OUTUN311
OUTUN312
OUTUN313
OUTUN314
OUTUN315
OUTSP316
INSP312
SFT0910b
CTS0910b
N20910b
BKG0910d
PATH
inlet
Inlet
Met
Inlet
Inlet
Inlet
Iiilet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet
Outlet spike
SF6 4ppm (ffi 2.0 1pm w/formaldehyde @ 1 1 OC
and toluene 60 ppm @ 1 .0 1pm
cell = 3.0 1pm, vent =2.0 1pm
Mel - spike (same as above)
Spike direct to cell
Kihylenc 20 ppm
N2 only in cell
Background - N2
NUMBER
SCANS
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
250
500
RES
(cm-1)
2
' 2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
2
CELL
TEMP
-------
0 v/V"
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
'-'*'
PLANT:__Wau|»aca Foundry, Inc. Tell City, IN_
BATE:
4ii
OPERATOR:
SAMI'I.K
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMIIEU
SCAN.S
KKS
(cm-l)
CRLL
SPIKED/
UNSriKED
SAMPLE
COND.
SAMPLE
FLOW
UKG
»"«. C»V\
if* US*
•X*
26"
V
A
A-
I
MlinVKST KI-SF.ARCII INS'ITIXITE
08-27-97
-------
PROJECT NO. 38»4-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
PLANT:_Waupaca Foundry, Inc. Tell City, IN_
BATE:
BA ROMETRIC: '^ h
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMBER
SCANS
KKS
(mil)
CELL
SPIKED/
UNSP1KED
SAMPLE
COND.
SAMPLE
FLOW
UKG
S-'U
S'*?'
J
U
\\
VN
|6
»\
t^-Ji.
r\
W
5 So
AJL
fi
^L
^
^v Klyl>uuinicirix/l'riKI:OKKI/l:wliliila].\US f
fr\ Ccr*\f>*ltf ""/tC^ |5 ff^f/tcJ^ nklt-J PT ./fc*/Jfi) f}^\p f
MIIHVI-ST RluSKARCll INSriTUTI-:
OK-27-97
-------
/ \
FTIR FIELD DATA FORM
PROJECT NO. 3804-25
PLANT:_Waunaca Foundry, Inc. Tell City, 1N_
(FTIR Sampling Data)
DATE:
BAROMETRIC
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTES
NUMItEK
SCANS
HKS
(cm I)
TEMP(^)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
ItKC.
a
.u.
>*«•
f
~YV \0
-^%
IS'
o - p.-Y
Cv-Jiv
,
J ,
^
*-^>
v ^ \ r.\ \
v. (A^U /IM 4vs/*-tf~5
08-27-97
5-
-------
r \
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
.7*5
PLANT:_Waui»aca Foundry, Inc. Tell City, IN_
DATE:
OPERATOR:
(III
SAMPLE
TIME
FILE
NAME
PATH
LOCATION / NOTILS
NUMUKK
SCANS
KKS
(Cllll)
CELL
SPIKED/
UNSPIKEI)
SAMPLE
COND.
SAMPLE
FLOW
UKO
If-
^
3i-7
f?~
V
UI-SHAKCM INS II I'll IK
My I J«»cimicnis/l Tl|{|;< MtM/l-'k-
->
OH-27-97
-------
FTIR FIELD DATA FORM
PROJECT NO. 3804-25
PLANT: \
SAMPLE
TIME
O 'HV
O'.Vi
|S ''Q >
\VO
Yv> Tfv
VV*5*
XT'&o
Vaupaca Foundry, Inc. Tell Citj
FILE
NAME
y.-^v.
gtaSoQit
\V~>«°A5
H^e-i^V
In*;*'- IJS
Q.1*
S ft C c c^Tt^
* T J W finiH
I'isSo^l
^OSou^
\*\o5om
*•
Cl|p'^f ^'j
PAT1I
_
VW6o-jiT
- ^
,1N
CPT/R Sampling Data)
DATE: f^>Vn
'
LOCATION / NOTES
Cc^flNX
c A\ ' •
*P
lOviS
$oH\r*A^C '
•n ^
- tkt^.
J
ijil Vi" '.
^>i.U« ITk^j.tl
I1 1 *T
„ div.
~C ' \ C " \\
\ ^
IWK
1
^UwVso^
<^\a
r
CJ\R,r>
OPERATOR: ,//Vll4
CELL
TEMP (F)
*nH
•*.
VS
N\
57V
SPIKED/
I INSPIRED
UN
^ \
v.
v
\\
Sf>'0-
SAMPLE
COND.
SAMPLE
5"J/w
'
V*"
I \
^ \
»x
3 0 ^y.
UKC
OK'S-,
V
^
%\
V^
//
Q!l
D
r-i(5^.
'^i,
MIOWr.ST ttl .SIwXHCII INSTITUTE
My l)<>ciHiicirts/I"nU|;(lKM/l"
0,,
IXIS
08-27^97
-------
FT1R FIELD DATA FORM
PROJECT NO. 3804-25 (FTIR Sampling Data)
PLANT:_Waii|iiica Foundry, Inc.
SAMPLE
TIME
fV V\
ftM?
(V-'M
t*Y 3 1
W-^S
FILE
NAME
^.cc^Ul
JTV^CV^
N3LOJC\4i«
^
C.TStfioSc.
B&vtiil)^
d
PATH
Tell City, IN DATE:
,|c
i
LOCATION / NOTES
GtW L.-f i.J ^/>i^
Sfwj. ; 1 .->»«- v« j^^i1"'
fSii^cV ^o G\^
Sn,\C* /V\ , x 1 .0 I *• *C 61/
a4 '-°J/M* r-l\i'«ftt
r,,4 fgiJ* iK,J» fl |60*C
M-, i.\ ^.t<} f-»C'^
*
^xlwvv JLOpp^v
« M
^w~v J^Vw ^~~ |^S\C V- **v f ^ *^* " ^J
» **
BAROMETRIC:
'O OPERATOR: ".MU
NIIMUEK
SCANS
of^'J
»
'i)r~
1
>^
?uu
KICS
(cm-l)
ol
.«
ffc'i-MtVt,
•
--
J
CELL
TEMI'(F)
^74
XN
1
«Je @^
«*
is
^\
4>|
SI'IKEU/
UNSPIKEU
V»&
>-.
c 7Jf(«:c'/
* ,
•v
U«v
SAMPLE
COND,
ft/i»^/*lir
SAMPLE
FLOW
?.JJ I.JJ-
4.U ^j,^
^ ° Av.
5 «• ^- -
^"-(-: iU*
T
ItKC
ofoSc
XV
l\
U
Mii)\vi-:s"r
'II INSTITlrri-.
My |)«M-IIIIICII|S/|"| IKI'OltM/I-icUliilii I.XUS
OK-27-97
-------
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
PLANT:_Wnu|>aca Foundry, Inc. Tell City, IN
DATE:
BAROMETRIC
OPERATOR:
SAMPLE
IIMK
FILE
NAME
PATH
I/1CATION / NO TKS
NUMBER
SSCANS
MES
(cm-l)
CELL
TEMP(F)
SPIKEU/
UNSPIKIIO
SAMPLE
COND.
SAMPLE
FLOW
I1KC
T-
§00
'•%
cjf
\.,
-17V
55
/~
1o
M
Atw
fo
\\
W
1 1
ji *p h
MIDWKSTRESI- ARCH INSTITUTE
\tf \, 1 1.1 /
My Uacuiiwiib/FnRI-<)RKl/FieUbU3..\LS.
08-27-97
-------
PROJECT NO. 38«4-2S
FTIR FIELD DATA FORM
(FTiR Sampling Data)
7/7*
' '
PLANT:_Waui»aca Foundry, Inc. Tell City, 1N_
DATE:
BAROMETRIC: ' " " )
OPERATOR:
SAMPLK
TIME
FILE
NAME
PATH
LOCATION / NOTKS
NIIMUKK
SCANS
UKS
(cm!)
CELL
TEMI'(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
DKC
SP
•jp.
a
1%
l\
- n
/I
ivly
n
11.
n
E
tl
Mii>wi:s'i KKSKAHCII INSTITUTI-:
My Uocuinciils/ri I|U"« >RM/l:ii:Ii|sila3.XLS
08-27-97 /O
-------
PROJECT NO. 3804-25
FT1R FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
. TV?
PLANT: \
SAMPLE
TIME
\^i%
\i\'. 33
>H'18
H15
f^'J/
'M*-58
Yi-o^
» b -.t.'N
sV^t
itr.VL
ls\as
\*> 3~>
OOT
<»^
iS-V\
IG'oH
tr\vA
IV. 01
\v.\S
Vaupaca Foundry, Inc.
FILE
NAME
nU*m
tnWril) A
IftlltAlll
'V^l°^o
rt^«K<\l«1
oJWlot
o^*v\M\V\
"\lM/iH5
1*WU&
L-CT
f(?f
NDMDER
SCANS
55^
xN
^<-
»S
^ -
J^O
l^SOoiiJ
JL?C-
HES
(cni-I)
«4
»-
1-
u
a
; ,.
. — o
OPERATOR: fiM H
CELL
TEMP (If)
^">'i
0
Nx
x- J
A^\
^
SeiKEUI
UNSPIKE1)
Mn
(X
,-
\N
O.A
^
SAMPLE
COND.
«/urt*MA
H
4,
N-
J^/\«(^>t
J
^
SAMPLE
FLOW
f.o ^
W
V
\^
__— ' —
•
S
^
*
}
ofo^J>
^
MIOWKST KKSKAIU^It INSITHfl'li _ , My lAicuniciiLs/Knitl-'OKM/FicldiihiJ.XLS (18-27-97
-------
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
BAROMETRIC:
PLANT;_Wati|iaca Foundry, Inc. Tell City, IN_
DATE:
OPERATOR:
SAMPLE
T1MB
FILE
NAME
PATH
LOCATION / NOTES
NUMUEH
SCANS
HltS
(.111 I)
CELL
TRMI'(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
HKC
O JT
JL
*
>ac
±a
WA\
JOM
$ °t^
wax
v> ^p*)
-0
\s
IT- 3ft
-o
MIOWKST RESEARCH INSTITUTE
My IJouimeiilx/ITIIWJRM/FieMiilaJ.Xf -S
08-27-97
-------
PROJECT NO. 3804-25
f\«\ tcl«rci C«
FTIR FIELD DATA FORM
(F7W Sampling Data)
PLANT:_Waupaca Foundry, Inc. Tell City, 1N_
TOP
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
FILE
NAMK
PATH
LOCATION /NOTES
NUMIlliU
SCANS
HliS
(Hill)
CELL
TEMP (K)
SI'IKED/
DNSPIKE1)
SAMPLE
COND.
SAMPLE
FLOW
BKG
T<5
11Z-1
JL
201
J.
i^
^t£-i
^f
CO
\\
\\
~ CA
IE
f^-
M1DW1 'ESEAROIIINSTmrrE
My Douiu
RKI/FicMala).XI.S
)8-2?-97
-------
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
PLANT:_Wau|iaca Foundry, Inc. Tell City, IN_
DATE:
BAROMETRIC:
OPERATOR:
I
SAMPLE
TIME
FILE
NAME
PATH
LOCATION /NOTES
NUMUEU
SCANS
RES
(CIU-I)
CELL
TEMP(F)
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
BKC
Tt
plKCjtc.jQJ)(\d
Jyiufr,
¥*
A/,
Un/
1%
\\
II
' 31
wJitr
i^LJ
MIDWI 'tl'-SUARCII INSTJTirrE
My Duvuiuciils/r ' WWicWula3.XlS
18-27-97
-------
PROJECT NO. 3804-25
PLANT;_Wau|iaca Foundry, Inc. Tell City, IN.
FTIR FIELD DATA FORM
(FTIR Sampling Data)
DATE:
BAROMETRIC:
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
M1CATION / NOTES
NUMUEH
SCANS
HES
(Wll-l)
CELL
SPIKED/
UNSPIKED
SAMPLE
COND.
SAMPLE
FLOW
BKG
4c
/rr wtsr
T»\
/06 l
c«i\ )£« S
~f
n'.oo
UC/v7
~EK
IfciUN
n
i
1 1
MIDWI"
-------
PROJECT NO. 3804-25
FTIR FIELD DATA FORM
(FTIR Sampling Data)
PLANT:_W«upaca Foundry, Int Tell City, IN_
DATE:
BAROMETRIC;
OPERATOR:
SAMPLE
TIME
FILE
NAME
PATH
LOCATION /NOTES
NUMBER
SCANS
HES
(Cill-I)
CELL
TEMP(F)
SPIKED/
UNSPIKKl)
SAMPLE
«JND.
SAMPLE
FLOW
UKC
5
j$*±
, (/ -
^
Q /
"T
fl
¥
JSL
Mimvr • i
A
My Doaiiiwnb/1- ''
diiluS Xl-S
K-27-97 ^
-------
FTIR FIELD DATA FORM
PROJECT NO. 3804-25 (FTIR Sampling Data)
PLANT: V
SAMPLE
TIME
K'.S*)
fv.fcS
fV. »1
|5'>?
Vuupaca Foundry, Inc.
FILE
NAME
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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 FTIR 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 FUR 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 their
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
Page
1.0 INTRODUCTION i
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 CTS 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
111
-------
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 FTIR 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
bTIR reference spectra is comprised primarily of hazardous air pollutants (HAPs) identified in
Title HI 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.
Laboratoiy Reference Spectrum Plan EPA Contract No, 68-D-98-027, MRI Work Assignments 2-12 and 2-13
Draft June 14, 1999 paie '
-------
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 ffl 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 50 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 2
-------
TAB LEI. ORGANIC COMPOUNDS SELECTED FOR THE LABORATORY STUDY
Compound Name
n-hexanea
n-heptane
Pentane
isooctane3
1-pentene
2-methyl,l-pentene
2-methyl,2-butene
2-methyl,2-pentene
3-methylpentane
Butane
Boiling Point (°C)
69
98.4
36.1
99.2
30
60.7
38,6
67J
63.3
-0.5
a Hexane and isooctane are HAPs. Their reference spectra will be re-measured because the reference
spectra in the EPA library were measured at ambient temperature.
The instrument is an Analect Instruments (Orbital Sciences) RFX-6S optical bench
equipped with a mercury-cadmium-teUuride (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, MR! Work Assignments 2-12 and 2-13
Draft June 14. 1999 Page *
-------
Cylinder gas inlets
Calibration
manifold
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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 ail 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 CTS gas. The
CTS spectrum will be recorded as the cell is continuously purged with the CTS 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, MRI Work Assignments 2-12 and 2-13
Page 4
-------
After the background and CTS 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 flow will be monitored with a mass flow meter before
the gas enters a heated line, and with a rotameter after the gas exits the cell. The mass flow
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 Pa8e 5
-------
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 IR gas cell.
3.4 Sample Temperature
The ER 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 ethytene 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 Plan EPA Contract No. 68-D-98-027, MRI Work Assignments 2-12 and 2-13
Draft June 14.1999
-------
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 Spectra* PlanEPA Contract No. 68-D-98-027, MRI Work Assignments 2-12 ind 2-f 3
Draft June 14, 1999 S
-------
Project No. _ MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
OPERATOR: _
Initials
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, (r\)
Vacuum Leak Check Procedure:
Evacuate ceE to baseline pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (1^,)
Leave cell isolated for one minute Time P,,^
Record time and cell pressure i
Calculate "leak rate" for 1 minute Time
Calculate "leak rate" as percentage of total pressure
% VL = (AP/Pb)* 100
|% VL| should be < 4 % Vt
Record Nitrogen Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using ceE 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
Record Cell path length setting
Evacuate Cell
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 interferopam were copied to directories.
Record CTS Spectrum File Name
Reviewed by: Date .
-------
Project No. MIDWEST RESEARCH INSTITUTE
FriR Reference Spectrum Checklist
DATE: OPERATOR:
Initials
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
Reviewed by: ; Date:.
-------
Project No. MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE: OPERATOR:
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)
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 (1 to 5 LPM)
Record cylinder ED Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferograrn 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 Rle Name
Close cylinders
Evacuate or Purge CTS from cell using nitrogen
Leave ceil under low nitrogen purge or under vacuum
Fill MCT detector dewir
Reviewed by: Date:,
-------
D TRANSFER
D EXCHANGE
TO MvAu*st
SS2-0
/oo
SHIPPING ORDER
MIDWEST RESEARCH INSTITUTE
425 Voikw Boulevard, Kansas City, Missouri 84110
D RETURN FOR CREDIT
D RETURN FOR REPAIR
144099
REFER TO THIS NO. IN
ALL CORRESPONDENCE
VIA
D A.M.
D P.M.
Q PREPAID
Q COLLECT
INSURE: Q YES D NO
AMOUNT
REQUESTED BY
a
Charge No. _
or
Bill Recipient Acct No.
REFERENCE
QUANTITY
DESCRIPTION OF MATERIAL
PRESENT LOCAHOt
H" /f 2-(
S,GNED
PACKING SLIP
MRI11 (Rev. 8/92)
-------
Attachment 1
Instrument Found Out of Tolerance
Code: MRI-0701
Revision: 3
Effective: 10/23/98
Page: 12 of 12
Instrument:
Manufacturer
MRI Number:
Serial Number:
+ y-
Acceptance Criteria:
r
Date of calibration or test that revealed the out of tolerance condition:
Date of previous calibration:
Responsible person:
Tested/Calibrated
Reviewed by:.
.(Must receive a copy of this report)
. Date: _
Date:
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)
MM-QA\MIU-a70I.DOC
-------
Code: MRJ-0722
Revision: 0
Effective: 03/22/99
Page: 6 of 6
MRI No.
Report N<
Attachment 1
Pressure Gauge Calibration Data Sheet
-£jf?3Model No. / Type ISlQ Serial No. J/237
"""OCg-<
Ambient Temperature "73*/= Ambient Humidity M %
Applied Pressure
Initial Check
Final Check
Tolerance ±
Pass
Fail
1.2.
7op
1.6
foo
Cumulative uncertainties of the standards used to perform this calibration did not exceed the requirements
ofMRI-0701 and ISO 10012-1.
Standards Use± MRI No
Notes/Adjustments/Kepairs/Modifications:
oxcafgea *0C.afietLhaviS:
fai.0 Giccurocy*) t AQC %
4 D.«)Sfa PS
t 0 £>t%
. Toat.ie.ckr
Limitations for use:
***
Date Calibrated:
Calibration Performed b
Reviewed by:
Date Due Recalibration:
-------
Code: MRI-0721
Revision: 0
Effective: 01/29/99
Page: 9 of 9
Attachment
Calibration Data Sheet
MRI No.: • — — ~
•__» __.
Noun: T TJ^//»Kt.
So,**^
S«>*^.
Sa>*N.^_
Sa/*^_
3.:T2iI30_ Repoi
Ambient Humidity
Tolerance i
°C_
/.O
1.0
y.0
/.f
2.2
3,0
TNo.:
^/l
Pass
c^-
«--
*—
*-
—
/
Fail
Cumulative uncertainries of the standards used to perform this calibration did not exceed the requirements
ofMRI-0701 and ISO 10012-1.
Standards used: MRI No.
Date calibrated
Date due calibration
Notes^Adjusrments/Repairs/Modifications:
Limitations for use:
irrutatio
Date Calibrated:
Calibration Performed
>X
Reviewed by: ^--y.^
MRI-OADMRI-07:i
-------
Code: MRI-0721
Revision: 0
Effective: 01/29/99
Page: 9 of 9
Attachment
Calibration Data Sheet
r
"Tkfshsrieks
Applied temperature
"* l< Of,
T - E.&O C.
T~i ~IOo9C
"^r" o'c.
*7~' IOQ 'C
V fso V
"Y"* 2o^ "c.
*7"" 3«iJ *c
IV7~* fao *c.
Ambient Tempera
Initial check
-a^o.Vfe.
-/00.3'c.
-e.**c.
^.7'c.
/^9 7 ° c
f
-------
SI'li
Scott Specialty Gases
pped 6141 EASTON ROAD, BLDG 1 PO BOX 310
From; PLUMSTEADVILLE PA 18949-0310
Phone: 215-766-8861 Pax: 215-766-2070
C1RTIPXCATB OP ANALYSIS
MIDWEST RESEARCH
SCOTT KLAMM
425 VOLKER BLVD
KANSAS CITY
MO 64110
PROJECT #: 01-01788-006
PO#: 033452
ITEM #: 01021951 5AL
DATE: 3/31/98
CYLINDER #: ALM02S384
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +/-5%
BLEND TYPE
COMPONENT
BTHYLENE
'NITROGEN
CERTIFIED WORKING STD
REQUESTED QAS
CONG HOLSS
20.
PPM
BALANCE
ANALYSIS
(MOLKS)
20.0
PPM
BALANCE
ANALYST:
-------
Scott Specialty Gases
sped
From:
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
GARY 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
GRAVIMETRI (
MASTER GAS
REQUESTED GAS
CONG MOLES
ANALYSIS
(MOLES)
50.
PPM
BALANCE
52.6
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
-------
Scott Specialty Gases
sped
From:
1750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE
0 F
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE 100
GARY 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
CONG MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
49.6
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
L. BAYLOR
-------
Scott Specialty Gases
shipped
From:
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
GARY NC 27511
PROJECT #: 12-34167-OOS
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
ANALYST:
W
-------
Scott Specialty Gases
Tpped
From:
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
GARY 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
ANALYST:
CAYLOR
-------
Scott Specialty Gases
shipped
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
GARY NC
27511
PROJECT #: 12-34167-005
P0#: 038545
ITEM #: 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
CONG MOLES
2 -METHYL-2 -PENTENE
NITROGEN
50,
PPM
BALANCE
ANALYSIS
(MOLES)
51,4
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
B.M. BECTO
-------
Scott Specialty Gases
pped
From:
1750 EAST CLUB BLVD
DURHAM NC 27704
Phone: 919-220-0803
CERTIFICATE
O F
Fax: 919-220-0808
ANALYSIS
MIDWEST RESEARCH
CROSSROADS CORP PARK
5520 DILLARD RD,SUITE'100
GARY NC 27511
PROJECT #: 12-34167-004
P0#: 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
CONG MOLES
ANALYSIS
(MOLES)
2-METHYL 2-BUTENE
NITROGEN
50.
PPM
BALANCE
50 .04
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
-------
Scott Specialty Gases
""S Hipped
From:
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
GARY 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
CONC MOLES
ANALYSIS
(MOLES)
2 -METHYL-1-PENTENE
NITROGEN
50.
PPM
BALANCE
50.08
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
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
GARY NC 27511
PROJECT #: 12-34167-002
P0#: 038545
ITEM #: 1202P2019421AL
DATE: 5/27/99
CYLINDER #: 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
ANALYST:
B.M. BECTON
-------
Scott Specialty Gases
fppecl
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
GARY NC 27511
PROJECT #: 12-34162-003
P0#: 038546
ITEM #: 1202N2007311AL
DATE: 5/26/99
CYLINDER #: AAL21337
FILL PRESSURE: 2000 PSIG
ANALYTICAL ACCURACY: +-1%
PRODUCT EXPIRATION: 5/26/2000
BLEN
COMPONENT
N-HEPTANE
NITROGEN
r:D7\YTMT:"T'R 1C MASTER GAS
REQUESTED GAS
CONG MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
49.97 PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
L. TAYLOR
-------
Scott Specialty Gases
Tpped
From:
1750 EAST CLUB BLVD
DURHAM
Phone; 919-220-0803
NC 27704
CERTIFICATE OF
Fax: 919-220-080!
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
CONG MOLES
50.
PPM
BALANCE
ANALYSIS
(MOLES)
51.3
PPM
BALANCE
NIST TRACEABLE BY WEIGHT
ANALYST:
B.M. BECTON
-------
Project No 'ml' ' 2- > i? MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATO_£iH OPERATOR:
Check cell temperature
Verify temperature using thennocouple probe and hand-held readout 31.*
Purge cell with dry nitrogen and vent to ambient pressure y uq «
Record ambient pressure in ceo, (PJ
—^fl^L_
•¥«e««a Leek Check Procedure; ^^e»^wJ< Piyrsu*^ ) J
Evacuate cell to baseline pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (1^) ^'o~? .'Vf 775".
Leave cell isolated for one minute Ti™8 PR*
Record time and cell pressure (r^J /t:oi* ;
-------
Project No, —f?5l-/l; ft MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATE 1r_
fnitmU
Check cefl temperatur*
Verify temperature using thermocouple probe and hand-held readout ——
Purge ceU with dry nitrogen and vent to ambient pressure • ~~"""^~"
Record ambient prennrt id ceB, (PJ
Vacnnaa Leak Check Procedure
Evacuate ceil to baseline pressure,
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (P,^)
Leave cell isolated for one minute Tune
Record tune and cell pressure (1^)
Calculate leak rate* for 1 minute Time
Calculate 'leak rate" as percentage of total pressure
:% VL| shouldbe<4
Record Nttrofea Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Baroceil 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 CeU path length setting
H'immeliCell
Fill Cell with CTS ga»
Open cell oodet and purge cell with CTS at sampling rate (1 toSLFM)
Record cylinder ID Number
Record CTS gat cylinder identity and concentration
Record and copy spectrum and interferogram to C-drive and back up using CTS batch file.
Record Barvtron pressure during collect
--SeCovd iafocmattcp OB sfnAgiouuJ aai Calibmtlmu' Jam rhatf * ^t
Verify that spectrum and tnterferogram were copied to directories.
Record CTS Spectrum File Nam*
Reviewed by
*T
-------
Project No. m <~ ^ ' * MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATR^US^-) OPERATOR: T.
Check ceffl tempenjar*
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure ia ctfl, (PJ
Leak Check Procedure:
SeS-- E*»ceUtol»S3iSS£,
Isolate cell (close cell Met and cell outlet)
Recordtime and baseline pressure (PJ /p'.^.VO
Leave cell isolated for one minute Tin*
Record time and cell pressure (I*.,) (Q'^S'-IO
Calculate 'leak rate" for 1 minute Tun0
Calculate "leak rate' as percentage of total pressure ' £j>
%Vt«(AP/r\)«100 ffOi
|%Vt|shouldbe<4
To*) '
Record Nitrogen Background 0
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell BaroceU gauge
Record nitrogen flow rate (about sampling flow rate)
Collect Background (AQBK) under continuous flow and ambient pressure
Record information ia data book,
Copy Background to C-drive and backup using batch file.
Record CTS Spectra*
Record Cell pub teogdi setting
JEuacuete Cell
9/f.flH Cell wife CIS ftt «ffi*
Open cell outfit and purge cell witn CTS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CTS gas cylinder identity and concentration
Record and copy spectrum and interferogrun to C-drive and back up using CTS batch fife, * 3H&
Record Barytron pressure during collect *T5X'7 gf
Reojrd information on "Background and Calibrations" data sheet ^—
Venfy that spectrum and interferognun were copied to directories. —^^
Record CTS Spectrum RleNam* . jC3Sif±l*
Review*! by: _A^fc^=^I Pat*: 1[*m
-------
Project No.
II. l^»
MIDWEST RESEARCH INsnTUTE
DAILY CHECKLIST
Start up Procedure
Check
OPERATOR:
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambkat pressure at cefl, (PJ
pressure,
Record time and baseline pressure (p^j
Leave cell isolated for out "timi*
Record time ami cell pressure (!»,„)
Calcuiats "leak rate" for 1 minute
it ;
Time
Calculate "leak rate" as percentage of total pressure
%V,.(AP/!U*100
|%Vt|shouldb«<4
Record Nitrogen Backfrooad
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell BaroceU 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 Spectnm
Record Cell path length setting
Fill Cell with CTS fa*
Open cell code* and purge cefl win, CTS at sampling rate (I to S 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 coped to directories.
Record CTS Spectrum File Nam*
Reviewed by:
Date:
I&itiils
tSfo^'C
*J*tM
-------
^J6" No* ^1S| ''2 ,i ° MIDWEST RESEARCH CNSTTTUTE
DAILY CHECKLIST
Start up Procedure
DATE" " ' " ' OPERATOR:
Check cefl temperature
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure ia cefl, (PJ
J£acaw»te*k Check Procedure:
|£jec$ate cell to baseline' pressure.
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (rt^) *?'. S*."i *
Leave cell isolated for one minute Tra*
Record time and cell pressure (law) &'/&'• 1°
Calculate 'leak rate" for 1 minute Time
Calculate "leak rate* as percentage of total pressure ^p
|%VL| shouldbe<4 *VL
I
Record Nttrogea Beckgroand
Purge ceil 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
-------
ft°lecl No- n>l "rl ,1^ MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
OPERATOR: T.
Check cefl temperature
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure in cefl, (PJ
i Leak Check Proctdmy
Evaguaficell to baseline
L***"^
Isolate cell (clow cell inlet and cell outlet)
Record time and baseline pressure (1*^) jo^aso*? rf^l. H
Leave cell isolated for one minute ^ime Pom
Record time and cell pressure (!*„) _/.»_',«
-------
ProJ6^ N°- "^r /*-, I"? MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATE .,,,,7-1 OPERATOR:
Check cefl tempentnr*
Verify temperature using thermocouple probe and hand-held readout
Purge cell with dry nitrogen and vent to ambient pressure
Record ambient pressure to cefl, (PJ
I Check Procedure v
B cell to baseline pressure. '***"
Isolate cell (close cell inlet and cell outlet)
Record time and baseline pressure (1*^) IL'^f^jf 77V«^ ^Ic,
Leave cell isolated for one minute Time p^ /
Record time and cell pressure (PJ tt^tfrf "7*7 7*. 8
Calculate "leak rate" for 1 minute Time p^,
Calculate "leak rate" as percentage of total pressure ^p
.' %VL»(AP/Pb)*100 tt0^
|%Vt| shouldbe<4 %VL
Record NHrofen Beckcroood
Purge ceil 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 Spectm
Record Cell path length setting
Fill Cell with CTS g»
Open cell outlet and purge cell with CTS at sampling rate (1 toSLPM)
Record cylinder ID NomiMr
Record CTS gas cylinder identity and concentration
Record and copy spectrum and iaterferogmm 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 aad interferognm wen copied to directories.
RecordCTS Spectrum File Nam*
n.f -///I
Reviewed by:
-------
Pr°JecJ N°- »"!-"*, .' MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Start up Procedure
DATS 1liln _ --
OPERATOR:
Check cefl tempentar*
Verify temperature using thermocouple probe and hand-held readout
Purge ceil with dry nitrogen and veal to ambient pressure
Record .mbknt prmor. in c*a,
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC;
OPERATOR:
TIME
FILE
NAME
(DW)
PATH
NOTES
NUMBER
SCANS
Renlulkiii
(cm-l)
GM
TEMP(F>
GM
PRESSURE
•KG
APOD
10:11
e.f
5-00
l.o
30.0 *
l.otfA\
7^7 /f
n
Do
(.0
IS!.}
c.nc h*dcNfy99v»951\l2Vefi\fiir dai« shoru for reference! xli
07-07-99
Reviewed by,
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC:
DATE:
OPERATOR: /.
TIME
FILE
NAME
(OW)
PATH
NOTES
NUMBER
SCANS
Roolulloo
CM
TEMP 09"'
GM
PRESSURE
•KG
APOD
/.
re.***?
0.
t.O
foo
1,0
, 7
fgo
1.0
. rt
cmc hick\fy99v»95 IV! 2VcfWlir dalt iheett for refcrcncej il<
07-07-99
Rc»iewed by
-------
PROJECT NO. 4951 12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
DATE:
BAROMETRIC:
OPERATOR: *' «*
TIME
FILE
NAME
(OW)
FATH
NOTES
NUMBER
SCANS
Renlulloa
(CBI-l)
CM
TEMP(F)
CM
PRESSURE
BIG
APOD
/?',(*
0, f •* */**«
Ao
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
DATE:
BAROMETRIC:
OPERATOR: "7
TIME
FILE
NAME
(DM)
PATH
NOTES
NUMBER
RMolutloD
GM
TEMP(F)
CM
PRESSURE
•KG
AMJD
,,;
<*»
/B.0-J
/•€>
73% f
11
i.O
l -«=>
-75$
1 1.
MM%
f.o
foO
/- 0
7S¥.
it
1.0
i.O
f.o
cmc b»d:Nfy99v495IMZVefiXflir
-------
PROJECT NO. 4951-12 and 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC: 7-S"*
DATE:
OPERATOR: 7T
TIME
FILE
NAME
(Dtal)
PATH
NOTES
NUMBER
SCANS
ReaolitlloB
(cm-1)
GM
TEMP(F)
GM
PRESSURE
•KG
APOD
1.0
1. 0<*L ?M
t.e>
756- /
o. 7}
f.o
»*fr. I
1211.0
/f & 0113 A
lf.0 "
0.
/•o
c? C.H it*
(f.ff
(.0
10.0 ">
cmc_b»dc\fyS>9vl95l\l 2Nrefi\/iir dau theelt for refcrmceruls
07-07-99
Reviewed by
-------
PROJECT NO. 4*51-12 »»d 13
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC:
DATE:
OPERATOR:
T.
TIME
FILE
NAME
(DM)
fATH
NOTES
NUMBER
SCANS
CM
TKMF(F)
Gm
mmsun
•EG
AMD
£*•
«, o
- \
ii v
r.
7S-7- /
• . o
*>«>
7ft. 4
/&;•
**•* tr
(.0
7'$*
0707-99
Reviewed by.
-------
PROJECT NO. 4fSI-12«Mll3
SITE: NCO Laboratory
FTIR DATA FORM
Background and Calibration Spectra
BAROMETRIC: ~?$ $• "2-
DATE:
OPERATOR:
TIME
FILE
NAME
(DW)
PATH
NOTES
NUMBER
SCANS
CM
•tmtryf
CM
ntESSUKK
we
APOD
ir,
Q *.
ff
1.0
1.0
Tit. ft
1."
I.O
~l((, A
t.O
cmc_b.dt>^y9?M95l\IZ>rffSftir *<« iheeti forrefeiaioet.xli
07-07-99
Reviewed by .
-------
Project No. "» —^i_ MIDWEST RESEARCH INSTITUTl
FllK Reference Spectrum Checklist
' DAm_J_lll^ OPERATOR: 1".
Reference Spectrum Sample u ^,-_.
'iro'M^
Start Tim* (.«-«••- c+vjt* i /5'J.i
Record Cell path length setting
Record Background Spectrum File Nam*
RecordCTS 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 now rate
Allow to equilibrate for 5 minute*
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferognun to backup directories
EndTim* if'.ft
Reviewed by: f/l(pAJ-^ Date:,
-------
Project No. —W/ ->* , (j>. MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATE 7'"Vfo OPERATOR: f
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 &*Xv~*i9 $*»• "^*
Record sample pressure in cell __2£L£_EP*~
Record sample flow rate through cell /.<>«? t.i3*
Start spectrum collect program thb
Record information in data book rf^
^^^^^/
Copy Spectrum and Interferograin to backup directories 4]\t
End Tun* /<;<4>
$(e.( *L>
Reviewed bjr ____J&l&Lfl*^l . • Dat*-
-------
Project No.
MIDWEST RESEARCH INSTITUTl
FTIR Reference Spectrum Checklist
DATE
OPERATOR:
Reference Spectrum Sample
Start Tim*
Record Cell path length setting
Record Background Spectrum File Name
Record CTS Spectrum Hie Nam*
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 minntr*
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:
Initial*
Date:
-------
No.
DATE
MIDWEST RESEARCH INSTITUTE
FT® Reference Spectrum Checklist
OPERATOR: T.(>«+ f
Initials
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Name
RecordCTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number • •
Record Cylinder Concentration
Record Spectrum File Ham*
Fill cell to ambient pressure with gas from cylinder standard
Open ceil outlet vent valve
Adjust sample flow through ceil to 0.5 to 1 LPM. Record now rate
Allow to equilibrate for 5 minutes C*£it»C*P L**, A
Record sample pressure in cell
Record sample flow rate through ceil
Stan spectrum collect program
Record information in data book
Copy Spectrum and tnterferogram to backup directories
End Time
Reviewed by:
-------
Project No. •''I MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATS V OPERATOR:
Reference Spectrum Sampto
Start Tia»
Record Cell path length setting
Record Background Spectrum File Name
Record Compound Nam*
.....
Record Cylinder Identification Number • * JilL
Record Cylinder ConcentranoB M ^,
Record Spectrum Rle Nam« Htj»rtia A
Fill cell to ambient pressure with gas from cylinder standard >» ^
Open cell outlet vent valve
Adjust sample flow throughcell to 0.5 to 1 LPM. Record flow rate
Allow to equilibrate for S
Record sample pressure in cell lff.l»
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 bv; Q^ f (f^f^^ Dates
-------
Project No..
-11.
MIDWEST RESEARCH INSTITUTE
FliR Reference Spectrum Checklist
DATE-
OPERATOR:
7"-
Reference Spectrum Sample
Start Time
Record Cell path length settinf
Record Background Spectrum File Name
Record CTS Spectrum FUe Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Nam*
Fill cell to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell to 0.5 to I LPM Record flow rate
Allow to equilibrate for 5 minutes C^SuM*^ ^*»» /I
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
£-5el
-------
ProJect No n^) "'—L£* MIDWEST RESEARCH INSTTTUTE
FTIR Reference Spectrum Checklist
DATE: It* m OPERATOR:
Reference Spectrum Sample
Start Tiia» ~
Record Cell path length setting ~~/»~
Record Background Spectrum File Name
Record CTS Spectrum File Nam*
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum File Nam*
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 mamtr*
Record sample pressure in ceil
Record sample flow rate through ceil
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviawad by L/l (a-tAsf~*^ . Date:.
-------
Project No. Mtlfr' '^-^ MIDWEST RESEARCH INSTITUTE
FITR Reference Spectrum Checklist
DATE 11ff>m OPERATOR:
Reference Spectrum Sample
Start Tim*
Record Cell path length setting \0-°'i>
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 ceil to ambient pressure with gu from cylinder standard
Open ceil outlet vent valve
Adjust sample flow through cell to 0,5 to I LPM. Record flow rate
Allow to equilibrate for 5 minute* t^i&**njp §V" *
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Inierferogram to backup directories
End Time
Initials
Reviewed by:
-------
Project No. ^1$\'Cl . MIDWEST RESEARCH INSTITUTE
FT1R Reference Spectrum Checklist
DATE 1 *m OPERATOR;
— _ hiri^lf
Reference Spectrum Sample -3
Record Cell path length setting
Record Background Spectrum File Name
RecordCTS Spectrum Pile Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration 50tfl
Record Spectrum File Name j^
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 f ^?o trV*
Start spectrum collect program f\(*
Record information in data book T l&
Copy Specerum and mterferogram to backup directories ^f*
EwiTims K'i?0
Reviewed by:
-------
Project No. _J12£lllLi<2.
DATS
MIDWEST RESEARCH INSTITUTE
FUR Reference Spectnim Checklist
OPERATOR:
f. £
Reference Spectrum Sample
Start Tim*
Record Ceil 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 minium (L*&v»***ff P"* *
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferograin to backup directories
End Time
Reviewed by:
Date
-------
^J601 No- M^>' f17 MIDWEST RESEARCH INSTITUTE
FTBR Reference Spectrum Checklist
DATE 1 l,i In OPERATOR: T,
Initials
/
Reference Spectrum Sample
Start Time £^«*a»^ f*****4"!
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 1LPM Record flow rate
Allow to equilibrate for 5 minute*
Record sample pressure in ceil
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
EndTime
125,2.
A /> _ ««(.../ a A
Reviewed by:,
-------
froJ6" No- —1 L)— MIDWEST RESEARCH INSTITUTE
FUR Reference Spectrum Checklist
DATE
it
OPERATOR-
~~ — rniriaJs
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 ceil to 0,5 to I LPM Record flow rate
Allow to equilibrate for 5 minute*
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogr&m to backup directories -]jl
End Time
gavi^adhy- VIW**S _ Date:.
-------
Project No. ~ f MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DATP- I n^ltCl
UAr& UH.n OPERATOR;
Reference Spectrum Sample A"
Start Time
{if:
Record Ceil path length setting _-
Record Background Spectrum File Name
RecoidCTSSpecmanlTtoNtin*
Record Compound N«a§
Record Cylinder Identification Number •
Record Cylinder Concentradon
Record Spectrum File Name &«.tf7 IJTA
Fill cell to ambient pressure with gu from cylinder standard
Open cell outlet vent valve
Adjust sample flow through cell W 0,5 » 1 LFM. Recotd flow rat* ^/6 | .01 U? ^
Allow to equilibrate for 5 minute*
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect prograiii
Record information in data book
Copy Spectrum and toerfefogram K3 backup directories 4\
End Time
Reviewed by; V\ ^^^ _ • Date:
-------
Project No. t/°t
MIDWEST RESEARCH INSTITUTE
FliR Reference Spectrum Checklist
DATE
OPERATOR:
Tnitinl.f
Reference Spectrum Sample
Stan Time
Record Cell path length setting
Record Background Spectrum File Name
RecordCTS Spectrum File Name
Record Compound Name
Record Cylinder Identificauon 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
Reviewed by:
-------
Project No.
MIDWEST RESEARCH INSTITUTl
FTTR Reference Spectrum Checklist
OPERATOR:
Reference Spectrum Sample
Start Tune
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 gu from cylinder standard
Open cell outlet venl valve
Adjust sample flow through cell 10 O.S to 1 LPNl Record flow rate
Allow to equilibrate for 5 minute*
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:,
Daw
Tnifinl«
L o "2-
-------
: No. —H? ?,(,_!—jj— MIDWEST RESEARCH INSTITUTE
FTTR Reference Spectrum Checklist
DATE 7/ffr/tf
OPERATOR:
Initials
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 Nam*
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 minute*
Record sample pressure in ceil
Record sample flow rate through ceil
Start spectrum collect program
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Tune
Havtewed hv VJtf, /-*"^ DatK "Mlto|11
-------
Project No. *"•" '' ) MIDWEST RESEARCH INSTITUTE
FtIR Reference Spectrum Checklist
DATE i - i • • OPERATOR: «f.
Reference Spectrum Sample ^ 2 -<*»*&Ljf -•* - lt»f*~J
StartTixne "' /tf^f
Record Cell path length setnag "~~~~~~~
Record Background Spectrum Hie Name
Record CTS Spectnim File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectnim 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 Cr£l&*»t9 n*** "
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and lalerferogram to backup directories
End Time
Reviewed by:
-------
Project No MIDWEST RESEARCH INSTTTUTl
MLK Reference Spectrum Checklist
DATE OPERATOR:
Initials
Reference Spectrum Sample
Start Tims
Record Cell path length setting
Record Background Spectrum Hie Name
Record CTS Spectrum File Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum Hie Name
Fill ceil 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 minute*
Record sample pressure in cell
Record sample flow rat* through cell
Start spectrum collect program
Record information in data book
Cepy Spectrum and Interferogram to backup directories
End Time
Reviewed by;
-------
No. U^Ht \\
MIDW1ST RESEARCH INSTITUTE
FTtK Reference Spectrum Checklist
DATE 7('U|11 OPERATOR:,
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum Me Name
Record CTS Spectrum File Name ,
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration fO,e>'& 9?**
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 miruitnt 3f(#
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in data book
Copy Spectrum and taterferogram to backup directories
End Time
Reviewed by: ' Date:.
-------
Project No, 11$ I-it j '"* MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
DAm-_4±iii OPERATOR_. r.fe
Initials
Reference Spectrum Sample
Start Time
Record Cell path length setting
Record Background Spectrum File Hum
ReecriCTS Spectrum file Name
Record Compound Name
Record Cylinder Identification Number
Record Cylinder Concentration
-------
Project No. -fKI-1^ . MIDWEST RESEARCH INSTITUTE
FTIR Reference Spectrum Checklist
OPERATOR: T.
Reference Spectrum Sample
Start Time
Record Cell path length setting o
Record Background Spectrum File Name -f/u A
RecordCTSSpectrumFileNarne ^^
Record Compound Name j.
Record Cylinder Identification Number
Record Cylinder Concentration
Record Spectrum FUe 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 g.1"?
Allow to equilibrate for 5 minutes
Record sample pressure in cell >/fc 75Y../
Record sample flow rate through cell O.qf
Start spectrum collect program /\<,
Record information in data book
Copy Spectrum and Interferogram to backup directories
End Time
Reviewed by: ^^__^^_________^_^_^_____ Date:.
-------
Project No, f^r ' )17 MIDWEST RESEARCH INSTmJTl
FTIR Reference Spectrum Checklist
DATE: 1/|fc V) OPERATOR: T-6
Reference Spectrum Sample
Start Tim*
Record Cell path length serting
Record Background Spectrum File Name
Record CTS Spectrum File Name
Record Compound Nam*
Rect^ Cylinder Identification Number AAt.li
Record Cylinder Concentration
Record Spectrum File Nam*
Fill ceil to ambient pressure with gas from cylinder standard
Open cell outlet vent valve
Adjust sample flow through ceil to 0,5 to 1 LPM. Record flow rate
Allow to equilibrate for 5 minutes 3fe
Record sample pressure in cell
Record sample flow rate through cell
Start spectrum collect program
Record information in dan book
Copy Spectrum aad Interferogram to backup directories
End Time
Reviewed by: ; Date:.
-------
FT1R DATA FORM
Sampling Data
PROJECT NO. 4951-12 and 13
BAROMETRIC;
. */
SITE: NCO Laboratory DATE:
Time
,<-.»<
1 5 •.•»<•
emc bacfcN
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PROJECT NO. 4951-12 and 13
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-------
PROJECT NO. 4951-12 and 13
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FTIR DATA FORM
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-------
Project No. ^?l'lt } ^ MIDWEST RESEARCH IN
DAILY CHECKLIST
Shut Down Procedure
OPERATO*
Initials
Purge sample from cell using ambient air or nitrogen
Record Nttrofca Backfrouad
Purge cell with dry nitrogen ^
Verily 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 CTSgiS
Opencell outlet and purge cell with CIS at sampling rate (1 to 5 LPM)
Record cylinder ID Number
Record CIS gas cylinder identity and concentration
Record and copy spectrum and interferogram to C-drive and back up using CIS batch file.
Record Barytron pressure during collect
Record information on "Background and Calibrations" data sheet
Verify that spectrum and interferogram wen copied to directories.
RecoidCTS Spectrum Hie Nam*
Clos« cylinders
Evacuate or Porg«CTS from call using nitrogen
Leaw cell under low nitrogen purge or under vacuum
Reviewed by:
-------
Project No.
>1.
MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE
OPERATOR;
— —- y - |
Purge sample from cell using ambient air or nitrogen
Record Nttrogea Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell BaroceU 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 CIS at sampling rate (I to 5 LPM)
Record cylinder ED 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 wen copied to directories.
Record CTS Spectrum File Name
Close cylinders
Evacuate cc Purge CTS from cell using nitrogen
Leave ceil under low nitrogen purge or under vacuum
FdlMCTctoectadewn
Reviewed by:
DatK.
7f<
11
-------
P*°i«:«No. L_ MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
-/ . l . .
DATE
OPERATOR:
Initials
Purge sample from cell using ambient air or nitrogen
Record Nitrogea 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 (&QBK) 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
Op« 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 ),(<* MJK>«*<
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 Calibrations1' data sheet
Verify that spectrum and interferogram were copied to directories.
Record CTS Spectrum file Name
Close cylinders
Evacuate or Purge CTS bom cell using nitrogen
Leave cell unds* tow nitrogen purge or under vacuum
Fill MCT detector dcwv
Reviewed by:
-------
ft°J«« No. TO-'*-,/**- MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DAm '"''" OPERATOR: T.
Initials
Pwge sample from cell using ambient ait or nitrogen
Record NHrofta Background
Purge cell with dry nitrogen
Verify ceU 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 ED Number
Record CTS gas cylinder identity and concentration 2,0}
Record and copy spectrum and interferogram to C-
-------
Pr°ject No .-^1*1-—i-lH. MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE 1r>v
OPERATOR:
Tnitjufo
Purge sample from cell using ambient air or nitrogen
Record Nftrofta Backfroond
Purge cell with dry nitrogen
Verily cell is as dry as previous background
Record ambient pressure using cell Barocell gauge • Q
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 iff^
Opencell outlet and purge cell with CTS at sampling rate (1 to 5 LPM) jrfj> Jj/K» 2f^^J ^
Record cylinder ID Number
_^^___
Record CTS gas cylinder identity and concentration • ,fc j^u. £^UK — «.
Record and copy spectrum, and interferognrn to C-drive and back up using CTS batch file. d '&
Record Barytron pressure during collect '75t{>'7
Record informatioQ on "Background and Calibrations* data sheet ^
Verify that spectrum and inttrferograai were copied to directories.
Record CTS Spectrum File Name _
Cose cylinders _
Evacuate or Purge CTS from cell using nitrogen $1
Leave ceil under low nitrogen purge or under vacuum PH*
Fill MCT detector deww —"^
Reviewed by: I b
-------
Project No. f^f I - f* ,rt MIDWEST RESEARCH INSTITUTE
DAILY CHECKLIST
Shut Down Procedure
DATE: |H OPERATOR:
Purge sample from cell using ambient air or nitrogen „
Record Nttrofea Background *$
Purge cell with dry nitrogen 9^
Verify ceil is as dry as previous background i
Record ambient pressure using cell Barocell gauge ^
Record nitrogen flow rate (about sampling flow rate)
Collect Background
-------
Project No. JHS|-^f»_ ^^ msEAR(M ^SmUTE
DAILY CHECKLIST
Shut Down Procedure
DATE: "7 1141 *xi „„_ ^
__Li_«ciin OPERATOR; T.
Purge sample from cell using ambient air or nitrogen
Record Nitrogta Background
Purge cell with dry nitrogen
Verify cell is as dry as previous background
Record ambient pressure using cell Baroceil 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 Gle.
Record CTS Spcctrtm
Fill Cell with CTS gas
•MT
Open cell outlet and purge ceil with CTS at sampling rate (1 to 5 LPM) •*'//
Record cylinder ID Number iiuB,«ii
JHjQCj^^^J!
Record CTS gas cylinder identity and concentraticw yg^ .-^
Record and copy spectrum and inierferogram to C-drive and back up using CTS batch file. ^Q
Record Barytronpressure during collect w\(t
Record information on 'Background and Calibrations" data sheet
Verify that spectrum and interferogram wen copied to directories.
Record CTS Spectrum file N«
Close cylinders
Evacuate or Purge CTS from cell using nitrogen
Leave cell under low nitrogen purge or under vacuum
Fill MCT detector dewmr
Reviewed bvt * I V^f-^^ Datec
-------
APPENDIX C
CALIBRATION GAS CERTIFICATES
-------
01-05<'98 18:58
©215 788 0320
SCOTT
21010
Scott Specialty Gases
6141 EASTON ROAD
Shipped PLUMSTEADVILLE
From: Phone: 215-766-8861
PA 18949-0310
CERTIFICATE OF
PO BOX 310
Pax: 215-766-2070
ANALYSIS
MIDWEST RESEARCH
TOM GBYER
425 VOLKER BLVD
KANSAS CITY
MO 64110
PROJECT #; 01-88514-002
PO#: 029257
ITEM #: 01023*22 1AL
DATE: 4/10/97
CYLINDER #: ALM010610
PILL PRESSURE: 1980 PSIG
ANALYTICAL ACCURACY t +-5%
BLEND TYPE : GRAVIMETRIC MASTER GAS
UQOEST1D GAS
COMPONENT COMC MOLS8
SULFUR HEXAFLUORIDE 4. PfM
NITROOSH '
XNALYSI5
3.8,9
ANALYS
-------
12'22*9
10:39
FAl 18105892134
SCOTT SPECIALTY
Scott Specialty Gases
1290 COMBERMERE STREET
TROY | MI 48083
Phone: 248-589-2950
C E R T I F I
C A T E OF
Fax: 248-589-2134
ANALYSIS
MIDWEST RESEARCH
MELISSA TUCKER; # 026075
425 VOLKER BLVD
KANSAS CITY
MO 64110
PROJECT #: 05-97268-002
PO#: 026075
ITEM #: 05023822 4A
DATE; 6/03/96
CYLINDER #: *7853 j
PILL PRESSURE: 2000 PSI
BLEND'TYPE : CERTIFIED MASTER GAS
COMPONENT
SULFUR H1XAFLUORIDB-
NITROGSS
ANALYTICAL ACCURACY: +/- 2%
PRODUCT EXPIRATION: 6/03/1997
REQUESTED GAS
CONG MOLES
ANALYSIS
(MOLES)
4.
PPM
BALANCE
4.01
PPM
BALANCE
CERTIFIED MASTER GAS
ANALYST:
-------
01 05 98 18:58 ®213 788 0320 SCOTT 3lOOS
Scott Specialty Gases
6141 SASTON ROAD PO BOX 310
From": PLUMSTEADVXLLE PA 18949-0310
Phona: 215-766-8861 Fax: 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH PROJECT #: 01-88514-001
TOM GSYER PO#: 029257
425 VOLKER BLVD ITEM #: 01021951 1AL
DATS: 3/25/97
KANSAS CITY MO 64110
CYLINDER #: ALM023940 ANALYTICAL ACCURACY: +-1%
FILL PRESSURE: 2000 PSIG
BLEND TYPE : GRAVIMETRIC MASTER GAS
REQUESTED GAS ANALYSIS
COMPONENT CQMC MOLES (MQU
STHYLSNK 20. PPM 20.01
NITROOKN BALANCE BALANCE
.-..»•*-
% f
T- V
ANALYST;
GKNYA
-------
12 22 97 10:37 FA! 13103892134
SCOTT SPECIALTY
Scott Specialty Cjases
_?ped
From :
1290 COMBERMERE STREET
TROY
Phone: 248-589-2950
C E R T I F I
MIDWEST RESEARCH
LANCE HENNING
425 VOLKER BLVD
KANSAS CITY
CYLINDER #: A7649
FILL PRESSURE: 2000 PS±
BLEND TYPE
COMPONENT
BTHYLENB
NITROGEN
MI 48083
GATE OF
Fax: 248-589-2134
ANALYSIS
MO 64110
PROJECT #: 05-16958-001
P0#: 031195
ITEM #: 05021951 1A
DATE: 9/02/97
ANALYTICAL ACCURACY: + /- 1%
PRODUCT EXPIRATION: 9/03/2000
GRAVIMETRIC MASTER GAS
REQUESTED GAS
CONG MOLES
20.
PPM
BALANCE
ANALYSIS
(MOLES)
19.38 PPM
BALANCE
GRAVIMETRIC MASTER GAS
CERTIFIED TO HAVE BEEN BLENDED
AGAINST NIST TRACEABLE WEIGHTS
AND VERIFIED CORRECT BY
INDEPENDENT ANALYSIS.
ANALYST:
-------
01/03.98 18:57 ©215 786 0320 SCOTT '1007
Scott Specialty Gases
6141 BASTON ROAD PQ BOX 310
1WJMSTEADVILLI PA 18949-0310
Phona: 21S-7S6-8861 Pax; 215-766-2070
CERTIFICATE OF ANALYSIS
MIDWEST RESEARCH PROJECT #: 01-89796-004
DAVE ALBXJRTY, X1525 POf: 029872
425 VOLKBR BLVD ITSM #: 01023912 4AL
DATS: S/13/97
KANSAS CITY HO 64110
CYLINDER #: ALM052730 ANALYTICAL ACCURACY: +/- 2%
FILL PRESSURE: 2000 PSIG
BLSND TYPE : CERTIFIED MASTER GAS -
REQUESTED GAS ANALYSIS
gouge MQLB
TOLUENE 60. PPM 60.6 PPM
AIR BALANCE BALANCE
C
ANALYST:
QENYAVKOOTT
SMMA,OMTWIW• BUJMgTi*CWIitM' P*S*DiM».TX• ,
-------
APPENDIX D
TEST METHODS
-------
D-l EPA METHOD 320
-------
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 ORGANIC AND INORGANIC EMISSIONS
BY EXTRACTIVE FOURIER TRANSFORM INFRARED (FTIR) SPECTROSCOPY
1.0 Introduction.
Persons unfamiliar with basic elements of FTIR
spectroscopy should not attempt to use this method. This
method describes sampling and analytical procedures for
extractive emission measurements using Fourier transform
infrared (FTIR) spectroscopy. Detailed analytical
procedures for interpreting infrared spectra are described
in the "Protocol for the Use of Extractive Fourier Transform
Infrared (FTIR) Spectrometry in Analyses of Gaseous
Emissions from Stationary Sources," hereafter referred to as
the "Protocol." Definitions not' given in this method are
given in appendix A of the Protocol. References to specific
sections in the Protocol are made throughout this Method.
For additional information refer to references 1 and 2, and
other EPA reports, which describe the use of FTIR
spectrometry in specific field measurement applications and
validation tests. The sampling procedure described here is
-------
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 urn). This m-rchod 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
-------
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
-------
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,
(MAO). 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
(AUJ for each analyte.
1.4.2 An instrumental configuration shall be selected. An
estimate of gas composition shall be made based on previous
test data, data from a similar source or information
-------
5
gathered in a pre-test site survey. Spectral interferants
shall be identified using the selected DLi and AUt and band
areas from reference spectra and interferant spectra. The
baseline noise of the system shall be measured in each
analytical region to determine the MAU of the instrument
configuration for each analyte and interferant (MIUJ .
1.4.3 Data quality for the application shall be determined,
in part, by measuring the RMS (root mean square) noise level
in each analytical spectral region (appendix C of the
Protocol). The 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 MAUU 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
-------
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
metho.d in the application.
2.2 Sampling and Analysis. In extractive sampling a probe
-------
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.
Ai = ai b ci CO
where:
Ai = absorbance at a given frequency of the ith sample
component.
at = absorption coefficient (absorptivity) of the ith
sample component.
b = path length of the cell.
G! = 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.
-------
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 SPA FTIR spectral library
on the EMTIC (Emission. Measurement Technical Information
Center) computer bulletin board service and at internet
address http://info.arnold.af.mi1/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.
-------
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
-------
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
-------
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 of 0.021 to -0.022). Such
deviations indicate a change in the instrument throughput
relative to the background single beam.
3.11 Batch Sampling. A procedure where spectra of
discreet, static samples are collected. The gas cell is
filled with sample and the cell is isolated. The spectrum
is collected. Finally, the cell is evacuated to prepare for
the next sample.
3.12 Continuous Sampling. A procedure where spectra are
collected while sample gas is flowing through the cell at a
measured rate.
3.13 Sampling resolution. The spectral resolution used to
collect sample spectra.
3.14 Truncation. Limiting the number of interferogram data
points by deleting points farthest from the center burst
(zero path difference, ZPD).
3.15 Zero filling. The addition of points to the
interferogram. The position of each added point is
interpolated from neighboring real data points. Zero
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filling adds no information to the interferogram, but
affects line shapes in the absorbance spectrum (and possibly
analytical results).
3.16 Reference CTS. Calibration Transfer Standard spectra
that were collected with reference spectra,
3.17 CTS Standard. CTS spectrum produced by applying a de-
resolution procedure to a reference CTS.
3.18 Test CTS. CTS spectra collected at the sampling
resolution using the same optical configuration as for
sample spectra. Test spectra help verify the resolution,
temperature and path length of the FTIR system.
3.19 RMSD. Root Mean Square Difference, defined in EPA
FTIR Protocol, appendix A.
3.20 Sensitivity. The noise-limited compound-dependent
detection limit for the FTIR system configuration. This is
estimated by the MAU. It depends on the RMSD in an
analytical region of a zero absorbance line.
3.21 Quantitation Limit. The lower limit of detection for
the FTIR system configuration in the sample spectra. This
is estimated by mathematically subtracting scaled reference
spectra of analytes and interferences from sample spectra,
then measuring the RMSD in an analytical region of the
subtracted spectrum. Since the noise in subtracted sample
spectra may be much greater than in a zero absorbance
spectrum, the quantitation limit is generally much higher
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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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3.27 Screening. Screening is used when there is little or
no available information about a source. The purpose of
screening is to determine what analytes are emitted and to
obtain information about important sample characteristics
such as moisture, temperature, and interferences. Screening
results are semi-quantitative (estimated concentrations) or
qualitative (identification only). Various optical and
sampling configurations may be used. Sample conditioning
systems may be evaluated for their effectiveness in removing
interferences. It is unnecessary to perform a complete run
under any set of sampling conditions. Spiking is not
necessary, but spiking can be a useful screening tool for
evaluating the sampling system, especially if a reactive or
soluble analyte is used for the spike.
3.28 Emissions Test. An FTIR emissions test is performed
according specific sampling and analytical procedures.
These procedures, for the target analytes and the source,
are based on previous screening and validation results.
Emission results are quantitative. A QA spike (sections
8.6,2 and 9.2 of this method) is performed under each set of
sampling conditions using a representative analyte. Flow,
gas temperature and diluent data are recorded concurrently
with the FTIR measurements to provide mass emission rates
for detected compounds.
3.29 Surrogate. A surrogate is a compound that is used in
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a QA spike procedure {section 8.6.2 of this method) to
represent other compounds. The chemical and physical
properties of a surrogate shall be similar to the compounds
it is chosen to represent. Under given sampling conditions,
usually a single sampling factor is of primary concern for
measuring the target analytes: for example, the surrogate
spike results can be representative for analytes that are
more reactive, more soluble, have a lower absorptivity, or
have a lower vapor pressure than the surrogate itself.
4.0 Interferences,
Interferences are divided into two classifications:
analytical and sampling.
4.1 Analytical Interferences. An analytical interference
is a spectral feature that complicates {in extreme cases may
prevent) the analysis of an analyte. Analytical
interferences are classified as background or spectral
interference.
4.1.1 Background Interference.' This results from a change
in throughput relative to the single beam background. It is
corrected by collecting a new background and proceeding with
the test. In severe instances the cause must be identified
and corrected. Potential causes include: (1) deposits on
reflective surfaces or transmitting windows, (2) changes in
detector sensitivity, (3) a change in the infrared source
output, or (4) failure in the instrument electronics. In
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routine sampling throughput may degrade over several hours.
Periodically a new background must be collected, but no
other corrective action will be required.
4.1.2 Spectral Interference. This results from the
presence of interfering compound(s) (interferant) in the
sample. Interferant spectral features overlap analyte
spectral features. Any compound with an infrared spectrum,
including analytes, can potentially be an interferant. The
Protocol measures absorbance band overlap in each analytical
region to determine if potential interferants shall be
classified as known interferants (FTIR Protocol, section 4.9
and appendix B). Water vapor and C02 are common spectral
interferants. Both of these compounds have strong infrared
spectra and are present in many sample matrices at high
concentrations relative to analytes. The extent of
interference depends on the (1) interferant concentration,
(2) analyte concentration, and (3) the degree of band
overlap. Choosing an alternate analytical region can
minimize or avoid the spectral interference. For example,
C02 interferes with the analysis of the 670 cm'1 benzene
band. However, benzene can also be measured near 3000 cm*1
(with less sensitivity).
4.2 Sampling System Interferences. These prevent analytes
from reaching the instrument. The analyte spike procedure
is designed to measure sampling system interference, if any.
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4.2.1 Temperature. A temperature that is too low causes
condensation of analytes or water vapor. The materials of
the sampling system and the FTIR gas cell usually set the
upper limit of temperature.
4.2.2 Reactive Species. Anything that reacts with
analytes. Some analytes, like formaldehyde, polymerize at
lower temperatures.
4.2.3 Materials. Poor choice of material for probe, or
sampling line may remove some analytes. For example, HF
reacts with glass components.
4.2.4 Moisture. In addition to being a spectral
interferant, condensed moisture removes soluble compounds.
5.0 Safety.
The hazards of performing this method are those
associated with any stack sampling method and the same
precautions shall be followed. Many HAPs are suspected
carcinogens or present other serious health risks.- Exposure
to these compounds should be avoided in all circumstances.
For instructions on the safe handling of any particular
compound, refer to its material safety data sheet. When
using analyte standards, always ensure that gases are
properly vented and that the gas handling system is leak
free. (Always perform a leak check with the system under
maximum vacuum and, again, with the system at greater than
ambient pressure.) Refer to section 8.2 of this method for
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leak check procedures. This method does not address all of
the potential safety risks associated with its use. Anyone
performing this method must follow safety and health
practices consistent with applicable legal requirements and
with prudent practice for each application.
6.0 Equipment and Supplies.
Note:Mentionof trade names or specific products does
not constitute endorsement by the Envircnmental
Protection Acrencv.
The equipment- and supplies are based on the schematic
of a sampling system shown in Figure 1. Either the batch or
continuous sampling procedures may be used with this
sampling system. Alternative sampling configurations may
also be used, provided that the data quality objectives are
met as determined in the post-analysis evaluation. Other
equipment or supplies may be necessary, depending on the
design of the sampling system or the specific target
analytes.
6.1 Sampling Probe. Glass, stainless steel, or other
appropriate material of sufficient length and physical
integrity to sustain heating, prevent adsorption of
analytes, and to transport analytes to the infrared gas
cell. Special materials or configurations may be required
in some applications. For instance, high stack sample
temperatures may require special steel or cooling the probe.
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For very high moisture sources it may be desirable to use a
dilution probe.
6.2 Particulate Filters. A glass wool plug (optional)
inserted at the probe tip (for large particulate removal)
and a filter (required) rated for 99 percent removal
efficiency at 1-micron (e.g., Balston") connected at the
outlet of the heated probe.
6.3 Sampling Line/Heating System. Heated (sufficient to
prevent condensation) stainless steel,
polytetrafluoroethane, or other material inert to the
analytes.
6.4 Gas Distribution Manifold. A heated manifold allowing
the operator to control flows of gas standards and samples
directly to the FTIR system or through sample conditioning
systems. Usually includes heated flow meter, heated valve
for selecting and sending sample to the analyzer, and a by-
pass vent.' This is typically constructed of stainless steel
tubing and fittings, and high-temperature valves.
6.5 Stainless Steel Tubing. Type 316, appropriate diameter
(e.g., 3/8 in.) and length for heated connections. Higher
grade stainless may be desirable in some applications.
6.6 Calibration/Analyte Spike Assembly. A three way valve
assembly (or equivalent) to introduce analyte or surrogate
spikes into the sampling system at the outlet of the probe
upstream of the out-of-stack particulate filter and the FTIR
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analytical system.
6.7 Mass Flow Meter (MFM). These are used for measuring
analyte -spike flow. The MFM shall be calibrated in the range
of 0 to 5 L/min and be accurate to ± 2 percent (or better)
of the flow meter span.
6.8 Gas Regulators. Appropriate for individual gas
standards.
6.9 Polytetrafluoroethane Tubing. Diameter (e.g., 3/8' in.)
and length suitable to connect cylinder regulators to gas
standard manifold.
6.10 Sample Pump. A leak-free pump (e.g., KNF") , with by-
pass valve, capable of producing a sample flow rate of at
least 10 L/min through 100 ft of sample line. If the pump
is positioned upstream of the distribution manifold and FTIR
system, use a heated pump that is constructed from materials
non-reactive to the analytes. If the pump is located
downstream of the FTIR system, the gas cell sample pressure
will be lower than ambient pressure and it must be recorded
at regular intervals.
6.11 Gas Sample Manifold. Secondary manifold to control
sample flow at the inlet to the FTIR manifold. This is
optional, but includes a by-pass vent and heated rotameter.
6.12 Rotameter. A 0 to 20 L/min rotameter. This meter
need not be calibrated.
6.13 FTIR Analytical System. Spectrometer and detector,
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capable of measuring the analytes to the chosen detection
limit. The system shall include a personal computer with
compatible software allowing automated collection of
spectra.
6.14 FTIR Cell Pump. Required for the batch sampling
technique, capable of evacuating the FTIR cell volume within
2 minutes. The pumping speed'shall allow the operator to
obtain 8 sample spectra in 1 hour.
6.15 Absolute Pressure Gauge. Capable of measuring
pressure from 0 to 1000 mmHg to within ± 2.5 iranHg (e.g.,
Baratron") .
6.16 Temperature Gauge. Capable of measuring the cell
temperature to within ± 2°C.
6.17 Sample Conditioning. One option is a condenser
system, which is used for moisture removal. This can be
helpful in the measurement of some analytes. Other sample
conditioning procedures may be devised for the removal of
moisture or other interfering species.
6.17.1 The analyte spike procedure of section 9.2 of this
method, the QA spike procedure of section 8.6.2 of this
method, and the validation procedure of section 13 of this
method demonstrate whether the sample conditioning affects
analyte concentrations. Alternatively, measurements can be
made with two parallel FTIR systems; one measuring
conditioned sample, the other measuring unconditioned
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sample.
6.17.2 Another option is sample dilution. The dilution
factor measurement must be documented and accounted for in
the reported concentrations. An alternative to dilution is
to lower the sensitivity of the FTIR system by decreasing
the cell path length, or to use a short-path cell in
conjunction with a long path cell to measure more than one
concentration range.
7.0 Reagents and Standards.
7.1 Analyte(s) and Tracer Gas. Obtain a certified gas
cylinder mixture containing all of the analyte{5} 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 (GTS) according to section
4.5 of the FTIR Protocol. Obtain a National Institute of
Standards and Technology (NIST) traceable gravimetric
standard of the CTS (± 2 percent).
7.3 Reference Spectra. Obtain reference spectra for each
analyte, interferant, surrogate, CTS, and tracer. If EPA
reference spectra are not available, use reference spectra
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prepared according to procedures in section 4.6 of the EPA
FTIR Protocol. '
8.0 Sampling and Analysis Procedure.
Three types of testing can be performed: (1) screening,
(2) emissions test, and (3) validation. Each is defined in
section 3 of this method.- Determine the purpose(s) of. the
FTIR test. Test requirements include: (a) AUU DLlf 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, (Pmin), FTIR cell volume (Vss) , estimated sample
absorption pathlength, Ls', estimated sample pressure, Ps',
Ts', signal integration time (tss) , minimum instrumental
linewidth, MIL, fractional error, and (d) analytical
regions, e.g., m = 1 to M, lower wavenumber position, FLm,
center wavenumber position, FCm, and upper wavenumber
position, FUm, plus interferants, upper wavenumber position
of the CTS absorption band, FFUm, lower wavenumber position
of the CTS absorption band, FFLm, wavenumber range FNU to
FNL. If necessary, sample and acquire an initial spectrum.
From analysis of this preliminary spectrum determine a
suitable operational path length. Set up the sampling train
as shown in Figure 1 or use an appropriate alternative
configuration. Sections 8.1 through 8.11 of this method
provide guidance- on pre-test calculations in the EPA
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protocol, sampling and analytical procedures, and post-test
protocol calculations.
8.1 Pretest Preparations and Evaluations. Using the
procedure in section 4.0 of the FTIR Protocol, determine the
optimum sampling system configuration for measuring the
target analytes. Use available information to make
reasonable assumptions about moisture content and other
interferences.
8.1.1 Analytes. Select the required detection limit (DLt)
and the maximum permissible analytical uncertainty (AUJ for
each analyte (labeled from 1 to i). Estimate, if possible,
the maximum expected concentration for each analyte, CMAXt.
The expected measurement range is fixed by 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 (FRUt) , The
FRU is determined for each analyte by comparing CTS spectra
taken before and after the reference spectra were measured.
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The EPA para-xylene reference spectra were collected on
10/31/91 and 11/01/91 with corresponding CIS spectra
"ctslOSla," and "ctsllOlb." The CTS spectra are used to
estimate the reproducibility (FRO) in the system that was
used to collect the references. The FRO must be < AO.
Appendix E of the protocol is used to calculate the FRO from
CTS spectra. Figure 2 plots results for 0.25 cm"1 CTS
spectra in EPA reference library: S3 (ctsllOlb - ctslOSla),
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 MAD and protocol
appendix D gives the MAO 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 s 200 mL/min.
8.2.2 Analytical System Leak check. Leak check the FTIR
cell under vacuum and under pressure (greater than ambient).
Leak check connecting tubing and inlet manifold under
pressure.
8.2.2.1 For the evacuated sample technique, close the valve
to the FTIR cell, and evacuate the absorption cell to the
minimum absolute pressure Pmln. Close the valve to the pump,
and determine the change in pressure APV after 2 minutes.
8.2.2.2 For both the evacuated sample and purging
techniques, pressurize the system to about 100 mmHg above
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atmospheric pressure. Isolate the pump and determine the
change in pressure APP after 2 minutes.
8.2.2.3 Measure the barometric pressure, Pb in mmHg.
8.2.2.4 Determine the percent leak volume %VL for the
signal integration time tss and for APmax, i.e., the larger of
APV or APP, as follows:
AP
where 50 = 100% divided by the leak-check time of 2 minutes.
8.2.2.5 Leak volumes in excess of 4 percent of the FTIR
system volume Vss are unacceptable.
8.3 Detector Linearity. Once an optical configuration is
chosen, use one of the procedures of sections 8.3.1 through
8.3.3 to verify that the detector response is linear. If
the detector response is not linear, decrease the aperture,
or attenuate the infrared beam. After a change in the
instrument configuration perform a linearity check until it
is demonstrated that the detector response is linear.
8.3.1 Vary the power incident on the detector by modifying
the aperture setting. Measure the background and CTS at
three instrument aperture settings: (1) at the aperture
setting to be used in the testing, (2) at one half this .
aperture and (3) at twice the proposed testing aperture.
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Compare the three CTS spectra. CTS band areas shall agree
to within the uncertainty of the cylinder standard and the
RMSD noise in the system. If test aperture is the maximum
aperture, collect CTS spectrum at maximum aperture, then
close the aperture to reduce the IR throughput by half.
Collect a second background and CTS at the smaller aperture
setting and compare the spectra again.
8.3.2 Use neutral density filters to attenuate the infrared
beam. Set up the FTIR system as it will be used in the test
measurements. Collect a CTS spectrum. Use a neutral
density filter to attenuate the infrared beam (either
immediately after the source or the interferometer) to
approximately 1/2 its original intensity. Collect a second
CTS spectrum. Use another filter to attenuate the infrared
beam to approximately 1/4 its original intensity. Collect a
third background and CTS spectrum. Compare the CTS spectra.
CTS band areas shall agree to within the uncertainty of the
cylinder standard and the RMSD noise in the system.
8.3.3 Observe the single beam instrument response in a
frequency region where the detector response is known to be
zero. Verify that the detector response is "flat" and equal
to zero in these regions.
8.4 Data Storage Requirements. All field test spectra
shall be stored on a computer disk and a second backup copy
must stored on a separate disk. The stored information
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includes sample interferograins, processed absorbance
spectra, background interferograms, CTS sample
interferograms and CTS absorbance spectra. Additionally,
documentation of all sample conditions, instrument settings,
and test records must be recorded on hard copy or on
computer medium. Table 1 gives a sample presentation of
documentation,
8.5 Background Spectrum. Evacuate the gas cell to s 5.
mmHg, and fill with dry nitrogen gas to ambient pressure (or
purge the cell with 10 volumes of dry nitrogen). Verify
that no significant amounts of absorbing species (for
example water vapor and C02) are present. Collect a
background spectrum, using a signal averaging period equal
to or greater than the averaging period for the sample
spectra. Assign a unique file name to the background
spectrum. Store two copies of the background interferogram
and processed single-beam spectrum on separate computer
disks (one copy is the back-up).
8.5.1 Interference Spectra. If possible, collect spectra
of known and suspected major interferences using the same
optical system that will be used in the field measurements.
This can be done on-site or earlier. A number of gases,
e.g. C02, S02, CO, NH3, are readily available from cylinder
gas suppliers.
8.5.2 Water vapor spectra can be prepared by the following
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procedure. Fill a sample tube with distilled water.
Evacuate above the sample and remove dissolved gasses by
alternately freezing and thawing the water while evacuating.
Allow water vapor into the FTIR cell, then dilute to
atmospheric pressure with nitrogen or dry air. If
quantitative water spectra are required, follow the
reference spectrum procedure for neat samples (protocol,
section 4.6). Often, interference spectra need not be
quantitative, but for best results the absorbance must be
comparable to the interference absorbance in the sample
spectra.
8.6 Pre-Test Calibrations
8.6.1 Calibration Transfer Standard. Evacuate the gas cell
to s 5 mmHg absolute pressure, and fill the FTIR cell to
atmospheric pressure with the CTS gas. Alternatively, purge
the cell with 10 cell volumes of CTS gas. (If purge is
used, verify that the CTS concentration in the cell is
stable by collecting two spectra 2 minutes apart as the CTS
gas continues to flow. If the absorbance in the second
spectrum is no greater than in the first, within the
uncertainty of the gas standard, then this can be used as
the CTS spectrum.) Record the spectrum.
8.6.2 QA Spike. This procedure assumes that the method has
been validated for at least some of the target analytes at
the source. For emissions testing perform a QA spike. Use
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a certified standard, if possible, of an analyte, which has
been validated at the source. One analyte standard can
serve as a QA surrogate for other analytes which are less
reactive or less soluble than the standard. Perform the
spike procedure of section 9.2 of this method. Record
spectra of at least three independent (section 3.22 of this
method) -spiked samples. Calculate the spiked component of
the analyte concentration. If the average spiked
concentration is within 0.7 to 1.3 times the expected
concentration, then proceed with the testing. If
applicable, apply the correction factor from the Method 301
of this appendix validation test (not the result from the QA
spike).
8.7 Sampling. If analyte concentrations vary rapidly with
time, continuous sampling is preferable using the smallest
cell volume, fastest sampling rate and fastest spectra
collection rate possible. Continuous sampling requires the
least operator intervention even without an automated
sampling system. For continuous monitoring at one location
over long periods, Continuous sampling is preferred. Batch
sampling and continuous static sampling are used for
screening and performing test runs of finite duration.
Either technique is preferred for sampling several locations
in a matter of days. Batch sampling gives reasonably good
time resolution and ensures that each spectrum measures a
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discreet (and unique) sample volume. Continuous static (and
continuous) sampling provide a very stable background over
long periods. Like batch sampling, continuous static
sampling also ensures that each spectrum measures a unique
sample volume. It is essential that the leak check
procedure under vacuum (section 8.2 of this method) is
passed if the batch sampling procedure is used. It is
essential that the leak check procedure under positive
pressure is passed if the continuous static or continuous
sampling procedures are used. The sampling techniques are
described in sections 8.7,1 through 8.7.2 of this method.
8.7.1 Batch Sampling. Evacuate the absorbance cell to
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 integration times shall be sufficient to
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achieve the required signal-to-noise ratio. Obtain an
absorbance spectrum by filling the cell with N2. Measure
the RMSD in each analytical region in this absorbance
spectrum. Verify that the number of scans used is
sufficient to achieve the target MAU.
8.8.2 Assign a unique file name to each spectrum.
8.8.3 Store two copies of sample interferograms and
processed spectra on separate computer disks,
8.8.4 For each sample spectrum, document the sampling
conditions/ the sampling time (while the cell was being
filled), the time the spectrum was recorded, the
instrumental conditions (path length, temperature, pressure,
resolution, signal integration time), and the spectral file
name. Keep a hard copy of these data sheets.
8.9 Signal Transmittance. While sampling, monitor the
signal transmittance. If signal transmittance (relative to
the background) changes by 5 percent or more (absorbance =
-.02 to .02) in any analytical spectral region, obtain a new
background spectrum.
8.10 Post-test CTS. After the sampling run, record another
GTS spectrum.
8.11 Post-test QA.
8.11.1 Inspect the sample spectra immediately after the run
to verify that the gas matrix composition was close to the
expected (assumed) gas matrix.
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8.11.2 Verify that the sampling and instrumental parameters
were appropriate for the conditions encountered. For
example, if the moisture is much greater than anticipated,
it may be necessary to use a shorter path length or dilute
the sample.
8.11.3 Compare the pre- and post-test CTS spectra. The
peak absorbance in pre- and 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 s 10 percent of the total sample flow, when
possible. (Note; Use the rotameter at the end of the
sampling train to estimate the required spike/tracer gas
flow rate.) Use a flow device, e.g., mass flow meter (± 2
percent), to monitor the spike flow'rate. Record the spike
flow rate every 10 minutes.
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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 = 6(5P*> (3)
where :
CS = DF*Spifa?dir + Unspike(l-DF) (4)
DF «• Dilution factor of the spike gas; this value
shall be alO.
SF6(dlir) = SF6 (or tracer gas) concentration measured
directly in undiluted spike gas.
SFS!splc) = Diluted SFS (or tracer gas) concentration
measured in a spiked sample.
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37
Spikedu = Concentration of the analyte in the spike
standard measured by filling the FTIR cell
directly.
CS = Expected concentration of the spiked samples,
Unspike = Native concentration of analytes in unspiked
samples
10.0 Calibration and Standardization.
10.1 Signal-to-Noise Ratio (S/N). The RMSD in the noise
must be less than one tenth of the minimum analyte peak
absorbance in each analytical region. For example if the
minimum peak absorbance is 0.01 at the required DL, then
RMSD measured over the entire analytical region must be
& 0.001.
10.2 Absorbance Path length. Verify the absorbance path
length by comparing reference CTS spectra to test CTS
spectra. See appendix E of the FTIR Protocol.
10.3 Instrument Resolution. Measure the line width of
appropriate test CTS band(s) to verify instrument
resolution. Alternatively, compare CTS spectra to a
reference CTS spectrum, if available, measured at the
nominal resolution.
10.4 Apodization Function. In transforming the sample
interferograms to absorbance spectra use the same
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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 (TJ and absolute
pressure (PJ . Connect a wet test meter (or a calibrated
dry gas meter), and slowly draw room air into the cell.
Measure the meter volume (VJ , meter absolute temperature
(Tm) , and meter absolute pressure (Pm); and the cell final
absolute temperature (Tf) and absolute pressure (P£) .
Calculate the FTIR cell volume Vss, including that of the
connecting tubing, as follows:
?„
V 'm
m T
(5)
T, Tt
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, MAO, FCO) shall be performed using the de-resolved
standard spectra.
11.2 Data Analysis. Various analytical programs are
available for relating sample absorbance to a concentration
standard. Calculated concentrations shall be verified by
analyzing residual baselines after mathematically
subtracting scaled reference spectra from the sample
spectra. A full description of the data analysis and
calculations is contained in the FTIR Protocol (sections
4.0, 5.0, 6.0 and appendices). Correct the calculated
concentrations in the sample spectra for differences in
absorption path length and temperature between the reference
and sample spectra using equation 6,
c,
coir
C (6)
cilc
where:
Ccorr = Concentration, corrected for path length.
Coaic = Concentration, initial calculation (output of the
analytical program designed for the compound).
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40
Lr = Reference spectra path length.
Ls = Sample spectra path length.
T, •» Absolute temperature of the sample gas, K.
Tr = Absolute gas temperature of reference spectra, K.
Ps » 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 HC1, the certified accuracy in a commercially
available standard may be no better than ± 5 percent.
12,2.3 Temperature. Temperature measurements of the cell
shall be quite accurate. If practical, it is preferable to
measure sample temperature directly, by inserting a
thermocouple into the cell chamber instead of monitoring the
cell outer wall temperature.
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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42
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 ETIR 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 ETIR 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 =
TC2).
13.4 Statistical Treatment. The statistical procedure of
EPA Method 301 of this appendix, section 6.3 is used to
evaluate the bias and precision. For FTIR testing a
validation "run" is defined as spectra of 24 independent
samples, 12 of which are spiked with the analyte(s) and 12
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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:
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 & CF s 1.3. If is determined that the bias is
significant and CF > ± 30 percent, then the test method is
considered to "not valid."
13.4.3 If measurements do not pass validation, evaluate the
sampling system, instrument configuration, and analytical
system to determine if improper set-up or a malfunction was
the cause. If so, repair the system and repeat the
validation.
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46
14,0 Pollution Prevention.
The extracted sample gas is vented outside the
enclosure containing the ETIR 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
(FTIE) 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".
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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 CFI 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-vlbrational
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, Che»ical 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.
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48
Table 1. EXAMPLE PRESENTATION OF SAMPLING DOCUMENTATION.
Smmflt TlM
Sp*ctr« f 11. MM*
•ackcra«*4 File DMM
Suple cMiUlaalBg
fr*c*>« cMdltiva
Smmfle TiM
Spectrwi File
laterrerograa
••MlntiM
Sc»m»
Ap
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49
Calibmtiofi Qu LilM
Mace Flow
M*t*r [~~
-f-^-U
I
To Calbratton
Puirp»2
Figure 1. Extractive FTIR sampling system.
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50
.8-
.6-
.4-
FRU = SRMS(FU-FL)/BAV
SRMS = . 00147
BAV = 3.662
;JxA^
AiWWUk
.2
0-
p-xylene
1050
1000
1 I
950 900
Wavenumbers
850
800
750
Figure 2. Fractional Reproducibility. Top: average of ctslOSla and
ctsllOlb. Bottom: Reference spectrum of p-xylene.
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D-2 EPA FTIR PROTOCOL
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Page 1
PROTOCOL FOE THE USE OF EXTRACTIVE FOURIER TRANSFORM
INFRARED (FTIR) SPECTROMETRY FOR THE ANALYSES OF GASEOUS
EMISSIONS FROM STATIONARY SOURCES
INTRODUCTION
The purpose of this document is to set general guidelines
for the use of modern FTIR spectroscopic methods for the analysis
of gas samples extracted from the effluent of stationary emission
sources. This document outlines techniques for developing and
evaluating such methods and sets basic requirements for reporting
and quality assurance procedures.
1.0 NOMENCLATURE
1.1 Appendix A lists definitions of the symbols and terms
used in this Protocol, many of which have been taken directly
from American Society for Testing and Materials (ASTM)
publication 2 131-90af entitled "Terminology Relating to
Molecular Spectroscopy."
1.2 Except in the case of background spectra or where
otherwise noted, the term "spectrum" refers to a double-beam
spectrum in units of absorbance vs. wavenumber (cm"1).
1.3 The term "Study" in this document refers to a
publication that has been subjected to EPA- or peer-review.
2.0 APPLICABILITY AND ANALYTICAL PRINCIPLE
2.1 Applicability. This Protocol applies to the
determination of compound-specific concentrations in single- and
multiple-component gas phase samples using double-beam absorption
spectroscopy in the mid-infrared band. It does not specifically
address other FTIR applications, such as single-beam
spectroscopy, analysis of open-path (non-enclosed) samples, and
continuous measurement techniques. If multiple spectrometers,
absorption cells, or instrumental linewidths are used in such
analyses-, each distinct operational configuration of the system
must be evaluated separately according to this Protocol.
2.2 Analytical Principle.
2.2.1 In the mid-infrared band, most molecules exhibit
characteristic gas phase absorption spectra that may be recorded
by FTIR systems. Such systems consist of a source of mid-
infrared radiation, an interferometer, an enclosed sample cell of
known absorption pathlength, an infrared detector, optical
elements for the .transfer of infrared radiation between
components, and gas flow control and measurement components.
Adjunct and integral computer systems are used for controlling
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BPA FTIR Protocol
the instrument , processing the signal, and for performing both
Fourier transforms and quantitative analyses of spectral data.
2.2.2 The absorption spectra of pure gases and of mixtures
of gases are described by a linear absorbance theory referred to
as Beer's Law. Using this law, modern FTIR systems use
computerized analytical programs to quantify compounds by
comparing the absorption spectra of known (reference) gas samples
to the absorption spectrum of the sample gas. Some standard
mathematical techniques used for comparisons are classical least
squares, inverse least squares, cross -cor relation, 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 07 PROTOCOL REQUIREMENTS
The characteristics that distinguish FTIR systems from gas
analyzers used in instrumental gas analysis methods (e.g.,
EPA Methods 6C and 7E) are: (1) Computers are necessary to
obtain and analyze data; (2) chemical concentrations can be
quantified using previously recorded infrared reference spectra;
and (3) analytical assumptions and results, including possible
effects of interfering compounds, can be evaluated after the
quantitative analysis. The following general principles and
requirements of this Protocol are based on these characteristics.
3.1 Veriflability and Reproducibility of Results. Store
all data and document data analysis techniques sufficient to
allow an independent agent to reproduce the analytical results
from the raw interferometric data.
3.2 Transfer of Reference Spectra. To determine whether
reference spectra recorded under one set of conditions (e.g.,
optical bench, instrumental linewidth, absorption pathlength,
detector performance, pressure, and temperature) can be used to
analyze sample spectra taken under a different set of conditions,
quantitatively compare "calibration transfer standards" (CTS) and
reference spectra as described in this Protocol. (Note; The CTS
may, but need not, include analytes of interest) . To effect
this, record the absorption spectra of the CTS (a) immediately
before and immediately after recording reference spectra and
(b) immediately after recording sample spectra.
3.3 Evaluation of FTIR Analyses. The applicability,
accuracy, and precision of FTIR measurements are influenced by a
number of interrelated factors, which may be divided into two
classes: ,
3.3.1 Sample-Independent Factors. Examples ^are system
configuration and performance (e.g., detector sensitivity and
infrared source output), quality and applicability of reference
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EPA FTIR PrOtOCOl
lngit.fr 1Af
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 PHI-TEST PREPARATIONS AMD EVALUATIONS
Before testing, demonstrate the suitability of FTIR
spectrometry for the desired application according to the
procedures of this section.
4.1 Identify Test Requirements. Identify and record the
test requirements described below in 4.1.1 through 4.1.5. These
values set the desired or required goals of the proposed
analysis; the description of methods for determining whether
these goals are actually met during the analysis comprises the
majority of this Protocol.
4.1.1 Analytes (specific chemical species) of interest.
Label the analytes from i » 1 to I.
4.1.2 Analytical uncertainty limit (&%) . The AU.^ is the
maximum permissible fractional uncertainty of analysis for the
i"1 analyfce 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
, ppm) .
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EPA FTIR Protocol
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 1 through
N-j,_ 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 (pmin' mmHg) and the
infrared absorption cell volume (Vss, liter) . Select the
techniques and/or equipment for the measurement of sample
pressures and temperatures.
4.4 Select Spectroscopic System. Select a spectroscopic
configuration for the application. Approximate the absorption
pathlength (Lg' , meter), sample pressure (Pgf, kPa) , 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 Tg' 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.
Note: It may be necessary to choose preliminary analytical
regions (see Section 4.7), identify the minimum analyte
linewidths, or estimate the system noise level (see
Section 4.12) before selecting the CTS. More than one
compound may be needed to meet the criteria; if so, obtain
separate cylinders for each compound.
4.5.1 The central wavenumber position of each analytical
region lies within 25 percent of the wavenumber position of at
least one CTS absorption band.
4.5.2 The absorption bands in 4.5.1 exhibit peak
absorbances greater ' than ten times the value RMSgST (see
Sectioh 4.12) but less than 1.5 absorbance units.
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EPA FTIR Protocol
4, TOOK
4.5.3 At least one absorption CTS band within the operating
range of the FTIR instrument has an instrument -independent
linewidth no greater than the narrowest analyte absorption band;
perform and document measurements or cite Studies to determine
analyte and CTS compound linewidths.
4.5.4 For each analytical region, specify the upper and
lower wavenumber positions (FFUm and FFLm, respectively) that
bracket the CTS absorption band or bands for the associated
analytical region. Specify the wavenumber range, FNU to FNL,
containing the absorption band that meets the criterion of
Section 4.5.3.
4.5.5 Associate, whenever possible, a single set of CTS gas
cylinders with a set of reference spectra. Replacement CTS gas
cylinders shall contain the same compounds at concentrations
within 5 percent of that of the original CTS cylinders; the
entire absorption spectra (not individual spectral segments) of
the replacement gas shall be scaled by a factor between 0.95 and
1.05 to match the original CTS spectra.
4.6 Prepare Reference Spectra.
Note; Reference spectra are available in a permanent soft
copy from the EPA spectral library on the EMTIC (Emission
Measurement Technical Information Center) computer bulletin
board; they may be used if applicable.
4.6.1 Select the reference absorption pathlength (LR) of
the cell.
4.6.2 Obtain or prepare a set of chemical standards for
each analyte, potential and known spectral interferants, and CTS.
Select the concentrations of the chemical standards to correspond
to the top of the desired range.
4.6.2.1 Commercially- Prepared Chemical Standards. Chemical
standards for many compounds may be obtained from independent
sources, such as a specialty gas manufacturer, chemical company,
or commercial laboratory. These standards (accurate to within
±2 percent) shall be prepared according to EPA Protocol 1 (see
Reference D) or shall be traceable to NIST standards. Obtain
from the supplier an estimate of the stability of the analyte
concentration; obtain and follow all the supplier's
recommendations for recertifying the analyte concentration.
4.6.2.2 Self -Prepared Chemical Standards. Chemical
standards may be prepared as follows: Dilute certified
commercially prepared chemical gases or pure analytes with ultra-
pure carrier (UPC) grade nitrogen according to the barometric and
volumetric techniques generally described in Reference A,
Section A4.6.
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EPA FTIR Protocol -_ -
-IA, 193*; _ ___ ge
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 concent rat ion -
pathlength product (ASCPP) for each compound shall be higher than
the maximum estimated concentration-pathlength products for both
analytes and known interferants in the effluent gas. For each
analyte, the minimum ASCPP shall be no greater than ten times the
concentration-pathlength product of that analyte at its required
detection limit.
4.6.4 Permanently store the background and interferograms
in digitized form. Document details of the mathematical process
for generating the spectra from these interferograms. Record the
sample pressure (PR) , sample temperature (TR) , reference
absorption pathlength (LR) , and interf erogram signal integration
period (tSR) . Signal integration periods for the background
interferograms shall be *tSR. Values of PR, Lj,, 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-PTIR) technique as follows:
4.6.5.1 Record the response of the secondary technique to
each of the four standards prepared.
4.6.5.2 Perform a linear regression of the response values
(dependant variable) versus the accepted standard concentration
(ASC) values (independent variable) , with the regression
constrained to pass through the zero -response, zero ASC point.
4.6.5.3 Calculate the average fractional difference between
the actual response values and the regression-predicted values
(those calculated from the regression line using the four ASC
values as the independent variable) .
4.6.5.4 If the average fractional difference value
calculated in Section 4.6.5.3 is larger for any compound than the
corresponding Am, 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
-------
EPA PTIR Protocol
yage 7
analytical region (FI^, FC^, and FUm/ respectively) . Specify the
analytes and interferants which exhibit absorption in each
region.
4.8 Determine Fractional Reproducibility Uncertainties.
Using Appendix E, calculate the fractional reproducibility
uncertainty for each analyte (FRU^ from a comparison of {Ri} and
{R2}. If FRUi > AUi 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)] tn® analyte
concentrations, the known interferant concentrations, and the
baseline slope and intercept values. If the sample absorption
pathlength (Lg) , sample gas temperature (Ts) or sample gas
pressure (Pg) during the actual sample analyses differ from LR,
TR, and Pp, use a program or set of programs that applies
multiplicative corrections to the derived concentrations to
account for these variations, and that provides as output both
the corrected and uncorrected values. Include in the report of
the analysis (see Section 7.0) the details of any transformations
applied to the original reference spectra (e.g.,
differentiation) , in such a fashion that all analytical results
may be verified by an independent agent from the reference
spectra and data spectra alone.
4.11 Determine • the Fractional Calibration Uncertainty.
Calculate the fractional calibration uncertainty for each analyte
(FCUj_) according to Appendix F, and compare these values to the
-------
IP* PTia Protocol
fractional uncertainty limits (AUj_; see Section 4.1). if
FCUi > AU^} , either the reference spectra or analytical programs
for that analyte are unsuitable.
4.12 Verify System Configuration Suitability. Using
Appendix C, measure or obtain estimates of the noise level
(RMSRST' absorbance) of the FTIR system; alternatively, construct
the complete spectrometer system and determine the values RMSe
using Appendix G, Estimate the minimum measurement uncertainty
for each analyte (MAUj, ppm) and known interferant (Mra., ppm)
using Appendix D. Verify that (a) MttJ± < (AUt} (DL±) , FRU± < AU< ,
and FCUi < AUi for each analyte and that (b) the CTS chosen meets
the requirements listed in Section 4.5.
5.0 SAMPLING AMD 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
(LR) and leak volume (VL) , where VL - L£ tsg. 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 PR and record a set of CTS spectra {R3}. Store the
background ana unsealed CTS single beam interferograms and
spectra. Using Appendix H, calculate the sample absorption
pathlength (La) for each analytical region. The values Lg shall
not differ from the approximated sample pathlength Lg* (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 S§.
-------
IPA ?Tim ProtOCOl
,14.
Multiple sample spectra may be recorded according to
the procedures of Section 5.4 before performing Sections 5 5
and 5.6,
5.5 Quantify Analyte Concentrations. Calculate the
unsealed analyte concentrations mA± and unsealed interferant
concentrations RUI» 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 " l^sFiFs) / (^sBs7*) • Calculate the final analyte and
interferant concentrations RSA± - RLPSRUAi and RSIk " RLPSRUIk-
5.6 Determine Fractional Analysis Uncertainty. Fill the
absorption cell with CTS at the pressure Pg. Record a set of CTS
spectra {R4}. Store the background and CTS single beam
interf erograms . 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 interf erograms 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:
-------
BS>A FTIR Protocol in
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 S.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 the procedures of
Sections 4, 5, and 6 will be required. Software copies of
reference spectra and sample spectra will be retained for some
minimum time following the actual testing.]
-------
SPA FTIR Protocol Paae 11
- - 3
8.0 REFERENCES
A) Standard Practices for General Techniques of Infrared
Quantitative Analysis (American Society for Testing and
Materials, Designation E 168-88) .
B) The Coblentz Society Specifications for Evaluation of
Research Quality Analytical Infrared Reference Spectra
(Class II); Anal. Chemistry i?, 945A (1975); Appl.
Spectroacopy 44 4. pp. 211-215, 1990.
C) Standard Practices for General Techniques for Qualitative
Infrared Analysis, American Society for Testing and
Materials, Designation E 1252-88.
D) "Traeeability 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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82A FTI1 ftrotocol «=«« i ->
fage 12
APPENDIX A
DEFINITIONS OF TERMS AND SYMBOLS
A.I Definitions of Terma
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 patalength - in a spectrophotometer, the distance,
measured in the direction of propagation of the beam of
radiant energy, between the surface of the specimen on which
the radiant energy is incident and the surface of the
specimen from which it is emergent.
analytical region - a contiguous wavenumber region (equivalently,
a contiguous set of absorbance spectrum data points) used in
the quantitative analysis for one or more analyte.
Note; The quantitative result for a single analyte may be
based on data from more than one analytical region.
apodliatlon - 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's law - the direct proportionality of the absorbance of a
compound in a homogeneous sample to its concentration.
calibration transfer standard (CTS) gas - a gas standard of a
compound used to achieve and/or demonstrate suitable
quantitative agreement between sample spectra and the
reference spectra; see Section 4.5.1.
compound - a substance possessing a distinct, unique molecular
structure.
concentration (c) - the quantity of a compound contained in a
unit quantity of sample. The unit "ppm" (number, or mole,
basis) is recommended.
concentration-pathlength product - the mathematical product of
concentration of the species and absorption pathlength. For
-------
S1A PTXR Protocol
reference spectra, this is a known quantity; for sample
spectra, it is the quantity directly determined from. Beer's
law. The units " centimeters -ppm" or "meters -ppm" are
recommended.
derivative absorption spectrum - a plot of rate of change of
absorbance or of any function of absorbance with respect to
wavelength or any function of wavelength.
double beam spectrum - a transmission or absorbance spectrum
derived by dividing the sample single beam spectrum by the
background spectrum.
Note; The term "double-beam" is used elsewhere to denote a
spectrum in which the sample and background interferograms
are collected simultaneously " along physically distinct
absorption paths. Here, the term denotes a spectrum in
which the sample and background interferograms are collected
at different times along the same absorption path.
fast Fourier transform (FFT) - a method of speeding up the
computation of a discrete FT by factoring the data into
sparse matrices containing mostly zeros.
flyback - interferometer motion during which no data are
recorded.
Fourier transform (FT) - the mathematical process for converting
an amplitude -time spectrum to an amplitude -frequency
spectrum, or vice versa.
Fourier transform infrared (FTIR) spectrometer - an analytical
system that employs a source of mid- infrared radiation, an
interferometer, an enclosed sample cell of known absorption
pathlength, an infrared detector, optical elements that
transfer infrared radiation between components, and a
computer system. The time -domain detector response
(interferogram) is processed by a Fourier transform to yield
a representation of the detector response vs. infrared
frequency-
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.
interferogram, I (o) - ' record of the modulated component of the
interference signal measured as a function of retardation by
the detector.
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EPA PT1R Protocol
..... _______ eage
interferometer - device that divides a beam of radiant energy
into two or more paths, generate an optical path difference
between the beams, and recombines them in order to produce
repetitive interference maxima and minima as the optical
retardation is varied.
linewidth - the full width at half maximum of an absorption band
in units of wavenumbers (on"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, 9 - optical path difference between two beams in an
interferometer; also known as "optical path difference" or
"optical retardation."
scaa - 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 inter ferogram,
representing the detector response vs. wavenumber.
Nqte; 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.
The equivalent ISO term is "certified reference
material . "
transmittanee, 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.
-------
BPA FTIR Protocol
15
wavenumber, v - the number of waves per unit length.
Note: The usual unit of wavenumber is the reciprocal
centimeter, cm"1. The wavenumber is the reciprocal of the
wavelength, X, when X is expressed in centimeters.
zero-filling - the addition of zero-valued points to the end of a
measured interferogram.
Nats: Performing the FT of a zero-filled interferogram
results in correctly interpolated points in the computed
spectrum.
A.2 Definitions of Mathematical Symbols
Af absorbance - the logarithm to the base 10 of the reciprocal of
the transmittance (T).
A = Iog10 (•£) = -log,0T (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 (DI^) and analytical
uncertainty limit
- average absorbance of the itn analyte in the m*-*1
analytical region, at the concentration (CL^) corresponding
to the product of its required detection limit (DL^) and
analytical uncertainty limit (AU^) .
ASC, accepted standard concentration - the concentration value
assigned to a chemical standard.
ASCPP, accepted standard concentration-pathlength product - for
a chemical standard, the product of the ASC and the sample
absorption pathlength. The units "centimeters-ppm" or
"meters-ppm" are recommended.
AUj, analytical uncertainty limit - the maximum permissible
fractional uncertainty of analysis for the itn analyte
concentration, expressed as a fraction of the analyte
concentration determined in the analysis.
AVT^ - average estimated total absorbance in the mtn analytical
region.
CKNNk - estimated concentration of the ktn known interferant.
- estimated maximum concentration of the itn analyte.
-------
BPA FTIR Protocol oa«<=> i c
•»*,- •"><»« _ _ __ m _ rage 15
- estimated concentration of the jth potential interferant.
DL±, required detection limit - for the ith analyte, the lowest
concentration of the analyte for which its overall
fractional uncertainty (OFU,i) is required to be less than
the analytical uncertainty limit (AU.^) .
- center wavenumber position of the mth analytical region.
f fractional analytical uncertainty - calculated uncertainty
in the measured concentration of the ifc" 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 position of the CTS absorption band
associated with the mttt analytical region.
- upper wavenumber position of the CTS absorption band
associated with the mtn* analytical region.
- lower wavenumber position of the m^n analytical region.
PMUif fractional model uncertainty - calculated uncertainty in
the measured concentration of the i"1 analyte because of
errors in the absorption model employed.
FMjj - lower wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands .
- upper wavenumber position of the CTS spectrum containing an
absorption band at least as narrow as the analyte absorption
bands .
FEtJj, 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.
FTJm - upper wavenumber position of the mth analytical region.
IAI-i_ - band area of the jth potential interferant in the mc"
3 analytical region, at its expected concentration (CPOTj).
im " average absorbance of the ith analyte in the mth
analytical region, at its expected concentration (CPOTj }.
-------
SPA FTXR Protocol p _
g
Isci or k' indicated standard concentration - the concentration
from the computerized analytical program for a single -
compound reference spectrum for the itn analyte or ktfi known
interf erant .
kPa - kilo -Pascal (see Pascal) .
Lg' - estimated sample absorption pathlength.
LR - reference absorption pathlength.
Lg - actual sample absorption pathlength.
- mean of the MAUim over the appropriate analytical regions.
jn, minimum analyte uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
(AUjJ in the measurement of the itn analyte, based on
spectral data in the mtn analytical region, can be
maintained.
- mean of the MIUjm over the appropriate analytical regions.
MIUjm, minimus interf erant uncertainty - the calculated minimum
concentration for which the analytical uncertainty limit
CPOTj/20 in the measurement of the jtn interf erant, 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 erant s .
Hw - number of known interf erants .
N«,_._ - the number of scans averaged to obtain an interferogram.
OPUj - the overall fractional uncertainty in an analyte
concentration determined in the analysis (OFU^ - MAX{FRU^,
pcuif FAU±, mm±}) .
Pascal (Pa) - metric unit of static pressure, equal to one Newton
per square meter; one atmosphere is equal to 101,325 Pa;
-------
SPA PTIR Protocol
ing,,-* IA 1005 page ia
1/760 atmosphere (one Torr, or one millimeter Hg) is eoual
to 133.322 Pa.
pxnin " minimum pressure of the sampling system during the
sampling procedure.
Pg' - estimated sample pressure.
PR - reference pressure.
Pg - actual sample pressure.
RMSgjj - measured noise level of the FTIR system in the mth
analytical region.
RMSD, root mean square difference - a measure of accuracy
determined by the following equation:
J (!)£-.?
«)
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" (Aj^) is
defined as
(3)
RSAj_ - the (calculated) final concentration of the ith analyte.
RSIk - the (calculated) final concentration of the kth known
interferant.
tflca_, scan time - time used to acquire a single scan, not
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 Ngcan and
scan time tgcan/ ts - Ngcantgcan.
• signal integration period used in recording reference
spectra.
-------
EPA PTIR Protocol Faae 19
ingulf li, a
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 k for
quantities related to the analyte i; see Appendix D.
Note that some terms are missing, e.g., BAVm, OCU, RMSSm, SUBS,
SICif SACif Ss
-------
EPA FTIE Protocol «=„« -»«
Align**. IAJ ma« *age 20
APPENDIX B
IDENTIFYING SPECTRAL INTERPERANTS
B.1 General
B.I.I Assume a fixed absorption pathlength equal to the
value Ls'.
B.I.2 Use band area calculations to compare the relative
absorption strengths of the analytes and potential interferants.
In the mcn analytical region (FI^ to FTJm), use either rectangular
or trapezoidal approximations to determine the band areas
described below (see Reference A, Sections A.3.1 through A.3.3);
document any baseline corrections applied to the spectra.
B.I.3 Use the average total absorbance of the analytes and
potential interferants in each analytical region to determine
whether the analytical region is suitable for analyte
concentration determinations.
Note; The average absorbance in an analytical region is the
band area divided by the width of the analytical region in
wavenumbers. The average total absorbance in an analytical
region is the sum of the average absorbances of all analytes
and potential interferants.
B.2 Calculations
B.2.1 Prepare spectral representations of each analyte at
the concentration CL^ - pLi) (AUj_) , where DL| is the required
detection limit and AU4 is the maximum permissible analytical
uncertainty. For the nr"n analytical region, calculate the band
area (AAIim) and average absorbance (AAV^m) from these scaled
analyte spectra.
B.2.2 Prepare spectral representations of each potential
interferant at its expected concentration (CPOTj). For the mtn
analytical region, calculate the band area (lATjj.) and average
absorbance (IAVjm) from these scaled potentfai 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.l.
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., IAZ.im > 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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KPA FTIR Protocol Paae 21
IQQg ^
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
Potential Interferant
Labels
l IAI1:L
IAJ:L
FIGURE B.2 Presentation of Known Interferant Calculations
Analytical Regions
l .... M
Analyte Labels
. AAI1M
Known Interferant
Labels
1 lAIn
* *
K IAIK1
Total Average — —
Absorbance AVT, AVTM
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BPA PTIR FrotOCOl Da«« ->->
u. nsfi Page 22
APPENDIX C
ESTIMATING NOISE LEVELS
C.1 General
C.I.I The root-mean-square (RMS) noise level is the
standard measure of noise in this Protocol. The IMS noise level
of a contiguous segment of a spectrum is defined as the RMS
difference (RMSD) between the absorbance values which form the
segment and the mean value of that segment (see Appendix A) .
C.I.2 The RMS noise value in double-beam absorbance
spectra is assumed to be inversely proportional to: (a) the
square root of the signal integration period of the sample single
beam spectra from which it is formed, and (b) to the total
infrared power transmitted through the interferometer and
absorption cell.
C.I.3 Practically, the assumption of C.I.2 allow the RMS
noise level of a complete system to be estimated from the
following four quantities:
(a) RMS^^H - 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) tj^M - the manufacturer's signal integration time used
to det ermine
(c) tss - the signal integration time for the analyses.
(d) TP - the manufacturer's estimate of the fraction of the
total infrared power transmitted by the absorption cell
and transfer optics from . the interferometer to the
detector.
C.2 Calculation*
C.2.1 Obtain the values of RMS^^, tj«N' and TP from the
manufacturers of the equipment, or determine the noise level by
direct measurements with the completely constructed system
proposed in Section 4,
C.2.2 Calculate the noise value of the system (RMSEST) as
follows:
RMS^ TP
(4)
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BPA FTIR PrOtOCOl Darro
tAJ iQQg _ __ __ _ rage
APPENDIX D
ESTIMATING MINIMUM CONCENTRATION MEASUREMENT
UNCERTAINTIES (MAU and MIU)
D . 1 General
Estimate the minimum concentration measurement uncertainties
for the icn analyte (MAU^ and jtn interferant (MIILi) based on
the spectral data in the mcn analytical region by comparing the
analyte band area in the analytical region (AAIim) and estimating
or measuring the noise level of the system (RMSEST or RMSSm) .
Note; For a single analytical region, the MAU or MIU value
is the concentration of the analyte or interferant for which
the band area is equal to the product of the analytical
region width (in wavenumbers) and the noise level of the
system (in absorbance units) . If data from more than one
analytical region is used in the determination of an analyte
concentration, the MAU or MIU is the mean of the separate
MAU or MIU values calculated for each analytical region.
D.2 Calculations
D.2.1 For each analytical region, set RMS - RMSSm ^f
measured (Appendix G) , or set RMS = RMSEST if estimated (Appendix
C) .
D.2. 2 For each analyte associated with the analytical
region, calculate
(RMS) (DLt ) (AUt
in
D.2.3 If only the mtn analytical region is used to
calculate the concentration of the itn analyte, set MAUj_ = MAUim.
D.2.4 If a number of analytical regions are used to
calculate the concentration of the ith analyte, set MAUi 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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EPA PTIR Protocol Paqe 24
- 3
Wlk w«,ulk ^g)
ke{m'j
where the weight Wi}c is defined for each term in the sum aa
D.2.5 Repeat Sections D.2.1 through D.2.4 to calculate the
analogous values MIU-i for the interferants j - 1 to J. Replace
the value (AUj_) (DLji in the above equations with CPOTj/20;
replace the value AMjjn in the above equations with IAIjffl.
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SfA PTIR Protocol
Align.*- 1A,
APPENDIX E
DETERMINING FRACTIONAL REPRODUCIBILITY UNCERTAINTIES (FRU)
E . 1 General
To estimate the reproducibility of the spectroseqpic 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.
E . 2 Calculations
E.2.1 The CTS spectra {Rl} consist of N spectra, denoted by
, i»l, N. Similarly, the CTS spectra {R2} consist of N
ctra, denoted by 32±, i«l, N. Each S^ is the spectrum of a
, .
spectra, denoted by
single compound, where i denotes the compound and k denotes
the set {Rk} of which SJH is a member. Form the spectra 83
according to S3^ - S2jL-S1;j for each i. Form the spectra S4
according to
E.2.2 Each analytical region m is associated with a portion
of the CTS spectra S2^ 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 nand area calculation.
Denote the result by BAVm.
E.2.4 For each m and the associated i, calculate the RMSD
of S3^ between the absorbance values and their mean in the
wavenumber range FFUm to FFI^. 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 mtn analytical region is used to
calculate the concentration of the itn analyte, set
E.2.7 If a number p^ of analytical regions are used to
calculate the concentration of the ic" analyte, set FRUj_ equal to
the weighted mean of the appropriate FM_ values calculated above,
Mathematically, if the set of analytical regions employed is
{m' } , then
Wik FMk (8)
ke{m'}
where the Wi]c are calculated as described in Appendix D.
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BPA PTIE Protocol «-,„«,
ge
APPENDIX P
DETERMINING FRACTIONAL CALIBRATION UNCERTAINTIES (FCU5
7 . 1 General
P. 1.1 The concentrations yielded by the computerized
analytical program applied to each single -compound reference
spectrum are defined as the indicated standard concentrations
(ISC' a) . The ISC values for a single compound spectrum should
ideally equal the accepted standard concentration (ASC) for one
analyte or interferant, and should ideally be zero for all other
compounds. Variations from these results are caused by errors in
the ASC values, variations from the Beer's law (or modified
Beer's law) model used to determine the concentrations, and noise
in the spectra. When the first two effects dominate, the
systematic nature of the errors is often apparent,* take steps to
correct them.
F.I. 2 When the calibration error appears non- systematic,
apply the following method to estimate the fractional calibration
uncertainty (FCU) for each compound. The FCU is defined as the
mean fractional error between the ASC and the ISC for all
reference spectra with non- zero ASC for that compound. The FCU
for each compound shall be less than the required fractional
uncertainty specified in Section 4.1.
F.l. 3 The computerized analytical programs shall also be
required to yield acceptably low concentrations for compounds
with ISC-Q 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) .
7.2 Calculations
F.2.1 Apply each analytical program to each reference
spectrum. Prepare a similar table as that in Figure F.I to
present the ISC and ASC values for each analyte and interferant
in each reference spectrum. Maintain the order of reference file
names and compounds employed in preparing Figure F.I.
F.2.2 For all reference spectra in Figure F.I, verify that
the absolute value of the ISC's are less than the compound's MAU
(for analytes) or MIU (for 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 ith analyte) over all reference
spectra. Prepare a similar table as that in Figure F.2 to
present the FCU± and analytical uncertainty limit (AU.^) for each
analyte.
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ISA FTIR Protocol
Page 27
FIGURE F.I
Presentation of Accepted Standard Concentrations (ASC's)
and Indicated Standard Concentrations (ISC's)
Compound
Name
Reference
Spectrum
File Name
ASC
(ppm)
Xlf™*/
A
•
jaalytes
i»l
J
ISG
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SPA PTIH Protocol Facie 28
ingnif 14, THfi 3
APPENDIX G
MEASURING NOISE LEVELS
G.I General
The root-mean-square (RMS) noise level is the standard
measure of noise. The RMS noise level of a contiguous segment of
a spectrum is the RMSD between the absorbance values that form
the segment and the mean value of the segment (see Appendix A).
G.2 Calculations
G.2.1 Evacuate the absorption cell or fill it with UPC
grade nitrogen at approximately one atmosphere total pressure.
G.2.2 Record two single beam spectra of signal integration
period tss.
G.2.3 Form the double beam absorption spectrum from these
two single beam spectra, and calculate the noise level RMSSm in
the M analytical regions.
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BPA PTIR Protocol -^ OQ
ii.gn.*. id, 1005 __ . Fage 29
APPENDIX H
DETERMINING SAMPLE ABSORPTION PATHLENGTH (L«) AND
FRACTIONAL ANALYTICAL UNCERTAINTY (FAU)
H.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 (Tg), 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.I.I Before sampling, determine the sample absorption
pathlength using least squares analysis. Determine the ratio
LS/LR by comparing the spectral sets {Rl} and {R3}, which are
recorded using the same CTS at Lg and LR, and Tg and TR, but both
at PR.
H.I.2 Determine the fractional analysis uncertainty (FAU)
for each analyte by comparing a scaled CTS spectral set, recorded
at Lg, Tg, and Pg, 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 AR containing the absorbance values from all
segments of {Rl} that are associated with the analytical regions;
the members of the array are ARJ , i = 1, n. Form a similar one-
dimensional array Ag from the absorbance values in the spectral
set {R3}; the members of the array are Asi, i - 1, n. Based on
the model AC - rAR + E, determine the least-squares estimate of
r', the value o£ 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 AR as described in Section H.2.1, using values from {Rl} to
form AR, and values from {R4} to form Ag. Calculate the values
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iPA FTXR Protocol
Page 30
and
(10)
The fractional analytical uncertainty is defined as
FAU
NRMS
"lA
B
AV
(11)
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SPA PTIR Protocol
APPENDIX I
DETERMINING FRACTIONAL MODEL UNCERTAINTIES (FMU)
I . 1 General
To prepare analytical programs for PTIR 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 Calculations
1.2.1 For each analyte {with scaled concentration RSA^) ,
select a reference spectrum SA^_ with indicated standard
concentration ISC^. Calculate the scaling factors
. Ti Ls P
Tg LR PR ISCt
and form the spectra SACi by scaling each SA^ by the factor RAj_.
1.2.2 For each interferant, select a reference spectrum SIk
with indicated standard concentration ISCk. Calculate the
scaling factors
RI
K
P
3
Ts LR PR ISC,
and form the spectra SICk by scaling each SIk by the factor Rlk.
1.2.3 For each' analytical region, determine by visual
inspection which of the spectra SAC-L and SICk exhibit absorbance
bands within the analytical region. Subtract each spectrum SAC.j_
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SPA PTIR Protocol Paae 32
1*. THfi _ a
and SICj^ exhibiting absorbance from the sample spectrum Sg to
form the spectrum SUBg . To save analysis time and to avoidf the
introduction of unwanted noise into the subtracted spectrum, it
is recommended that the calculation be made (l) only for those
spectral data points within the analytical regions, and (2) for
each analytical region separately using the original spectrum Ss.
1.2.4 For each analytical region m, calculate the RMSD of
SUBg between the absorbance values and their mean in the region
FFUm to FFI^. Denote the result by lMSSm.
1.2.5 For each analyte i, calculate the quantity
PM -
^"
for each analytical region associated with the analyte.
1.2.6 If only the mt^1 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 itl1 analyte, set FM^ equal to
the weighted mean of the appropriate FM_ values calculated above.
Mathematically, if the set of analytical regions employed is
{m' } , then
FMUt = Wik FMk
ketm'}
where WiJc is calculated as described in Appendix D.
-------
EPA PTIR Protocol Paae 33
^
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 OFUj_ - MAX{PRUi, FCU.^, FAl^, FMU.^} and
OCU- -
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FTIR Protocol
APPENDIX K
SPECTRAL DS- RESOLUTION PROCEDURES
K.I General .
High resolution reference spectra can be converted into
lower resolution standard spectra for use in quantitative
analysis of sample spectra. This is accomplished by truncating
the number of data points in the original reference sample and
background interf erograms .
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 GTS
spectrum to a CTS spectrum measured on the sampling instrument.
(b) The Fourier transformation of truncated interf erograms
(and their conversion to absorbance spectra) is performed using
the same apodization function (and other mathematical
corrections) used in converting the sample interf erograms 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 ethyl ene spectrum (cts0305a)
to 1 cm"1 resolution. The 0.2S cm"1 CTS spectrum was collected
during the EPA reference spectrum program on March 5, 1992. The
original data (in this example) are in KVB/Analect FX-70 format.
(i) decamp cts0305a.aif, 0305dres,l, 16384, 1
"decomp" converts cts0305a to an ASCII file with name
0305dres. The resulting ASCII interf erogram file is truncated to
16384 data points. Convert background interf erogram
(bkg0305a.aif ) to ASCII in the same way.
(ii) compose 0305dres, 0305dres.aif , 1
"Compose" transforms truncated interferograms back to spectral
format.
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EPA FTIR Protocol
-,. gni.fr IA iaa«:
(iii) IG2SP 0305dres.aif,0305dres.dsf,3,l,low cm"1, high on'1
"IG2SP" converts inter ferogram 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) OVDR 0305dres.dsf,bkg0305a.dsf,0305dres.dlf
"DVDR" ratios the transformed sample spectrum against the
background .
(v) ABSB 0305dres.dlf,0305dres.dlf
"ABSB" converts the spectrum to absorbance.
The resolution of the resulting spectrum should be verified
by comparison to a CTS spectrum collected at the nominal
resolution. Refer to Section K.3.
K.2.2 Alternate KVB/Analect Procedure -- In either DOS
(FX-70) or Windows version (FX-80) use the "Extract" command
directly on the interferogram.
(i) EXTRACT CTS0305a.aif, 0305dres.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. 3Jlis procedure assumes familiarity
with basic functions of Grains™.
This procedure is specifically for using Grams to truncate
and transform reference interferograms that have been imported
into Grams from the KVB/Analect format. Table K-l shows data
files and parameter values that are used in the following
procedure .
The choice of all parameters in the ICOMPUTE.AB call of step
3 below should be fixed to the shown values, with the exception
of the " Apodization" parameter. This parameter should be set
(for both background and sample single beam conversions) to the
type of apodization function chosen for the de-resolved spectral
library.
TABLE K-l. GRAMS DATA FILES AND DE - RESOLUTION PARAMETERS.
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SPA FTIR Protocol Paqe 36
3
Desired Nominal Spectral
Resolution (cm"1)
0.25
0.50
1.0
2.0
Data File Name
Z002SO.sav
ZOOSOO.sav
ZOlOOO.sav
Z02000.aav
Parameter UN"
Value
65137
32769
16385
8193
(i) Import using "File/Import" the desired *.aif file. Clear
all open data slots.
(ii) Open the resulting *.spc interferogram as file #1.
(iii) Xflip - If the x-axis is increasing- from left to rigftt,
and the ZPD burst appears near the left end of the trace, omit
tnis 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.
xflipi#s-#s{fO,#m+50
(iv) Sun ICOICPtJTE.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: M Last; 0 Type: Single Beam
Zero Fill: None Apodization: (as desired)
Phasing: User
Points: 1024 Interpolation: Linear Phase :
Calculate
(v) As in step (iii) , in the "Arithmetic/Calc" menu item
enter and then run the following commands (refer to Table l for
appropriate "FILB," which may be in a directory other than
"c:\mdgrams.*)
setffp 7898.8805, 0 i loadspc *e!\mdgrams\ WI1M" t #2-ts+#2
(vi) Use "Page Up" to activate file #2, and then use the
"Pile/Save A»" menu item with an appropriate file name to save
the result.
K.3 Verification o£ New Resolution
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BPA FTIR Protocol Ds»«£» -arr
37
K.3.1 Obtain interferograms of reference sample and
background spectra. Truncate interferograms and convert to
abaorbance 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 fqr 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 (O.Oi) .
WSSj. x n(FFU1 - FFLj) ^ ^ (lg)
- ease
RMSS-RMSD in the ith 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.
Ategt.CTS-banci area in the ith analytical region of the test CTS.
-------
TECHNICAL REPORT DATA
(Pleau nod Initructtora on tht rertme lit fore camp,
REPORT NO.
EPA-454/R-99-035
2.
TITLE AND SUBTITLE
FT3R Emissions Test at an Iron Foundry
Watpaca Foundry, Inc. , Plant No. 5, Tell City, Indiana
9. REPORT DATE
1999
8. PERFORMING ORGANIZATION COOK
AUTHOR(S)
EMAD
8. PERFORMING ORGANIZATION MPQHT NO.
PERFORMING OROANIZATION NAME AND ADDRESS
10. PROGRAM ELEMENT NO,.
11. CONTRACT/GRANT NO. •
MIDWEST Research Institute (VKL)
EPA Cant. 68-D-98-Q27
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency
Research Triangle Park, N.C. 27711
13. TYPE OF REPORT AND PERIOD COVERED
Final Emission Test Report -"
14. SPONSORING AGENCY CODE
ERA/2DO/04
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The purpose of this testing program was to obtain entissions data by using FttR sampling at iron
foundries, specifically on cupola emission control devices as well as pouring, cooling, and shake-out
operations to support a national emission standard for hazardous air pollutants (NESHAP).
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c, cos ATI Field/Group
MALT Support for the Iron
& Steel Foundry Industry
18. DISTRIBUTION STATEMENT
RELEASE
19. SECURITY CLASS t Tlits Report>
l\. NO. OF PAGES
356
2O. SECURITY CLASS iT/i/J
22. PRICE
EPA Form 2220—I (R«». 4—77) PREVIOUS EDITION is OBSOUETE
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