United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park. NC 27711
EPA-454/R-00-012
March 2000
Air
&EPA
Final Report of Lime Manufacturing Industry
Fourier Transform Infrared Spectroscopy
Redland Stone Products Company
San Antonio, Texas
C of Air
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Lime Kiln Source Characterization
Final Report
Contract No. 68-D7-0001
Work Assignment 2-03
Redland Stone Products
San Antonio, Texas
Prepared for:
Michael L. Toney
Emission Measurement Center
Emission, Monitoring, and Analysis Division
Office of Air Quality Planning and Standards
U. S. Environmental Protection Agency
Research Triangle Park, North Carolina 27711
January 2000
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL 60604-3590
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Table of Contents
Page
1.0 INTRODUCTION 1-1
1.1 Objectives 1-2
1.2 Brief Site Discussion 1-2
1.3 Emissions Measurements Program 1-2
1.3.1 Test Matrix 1-2
1.3.2 Test Schedule 1-3
1.3.3 Deviations from Test Plan/Schedule 1-3
1.4 Test Report 1-4
2.0 SUMMARY OF RESULTS 2-1
2.1 Emissions Test Log 2-1
2.2 FTIR Results 2-1
2.2.1 Overview 2-1
2.2.2 FTIR Emission Results 2-3
3.0 SAMPLING AND ANALYTICAL PROCEDURE 3-1
3.1 Determination of Gaseous Organic HAPs, HC1, and Criteria Pollutants
by FTIR 3-1
3.1.1 FTIR Sampling Equipment 3-1
3.1.2 Preparation for Sampling 3-4
3.1.3 Sampling and Analysis 3-6
3.1.4 FTIR Method Data Review Procedures 3-9
3.1.5 FTIR QA/QC Procedures 3-12
4.0 QUALITY ASSURANCE/QUALITY CONTROL 4-1
4.1 FTIR Analytical Quality Control 4-1
List of Appendices
Appendix A FTIR Data Spreadsheet Calculation QA/QC Sheets
Appendix B Gas Cylinder Certification Sheets
Appendix C Raw FTIR Data
Appendix D FTIR Field Data Sheets
Appendix E Pre-test Calculations
Appendix F Post-test Calculations
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List of Figures
Page
2-1 HCI Inlet Run - Redland Stone Products 2-5
2-2 HCI Outlet Run - Redland Stone Products 2-6
3-1 FTIR Sampling and Measurement System 3-3
List of Tables
Page
2-1 Emissions Test Log 2-1
2-2 Wet Scrubber FTIR HCI Results, ppmv 2-3
2-3 Other Species Detected by FTIR - Wet Scrubber Inlet 2-6
2-4 Other Species Detected by FTIR - Wet Scrubber Outlet 2-7
3-1 Typical FTIR Operating Parameters 3-6
3-2 Compounds for which Reference FTIR Spectra are Available in the ERG Spectral
Library 3-10
4-1 HCI QC Pre-Test Spike Results 4-3
4-2 HCI QC Post-Test Spike Results 4-4
4-3 Gas Standard Analysis Results 4-5
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1.0 INTRODUCTION
The purpose of this testing program is to: (I) quantify hydrogen chloride (HC1) emission
levels; and (2) gather screening data on other hazardous air pollutants (HAP) emissions from
lime production plants to support a national emission standard for hazardous air pollutants
(NESHAP).
Three measurement methods were conducted at this facility:
Fourier Transform Infrared Spectroscopy (FTIR) (EPA Draft Method 320);
Gas Filter Correlation - Infrared (GFC-IR) (EPA Method 322); and
• Dioxin/furan manual trains (EPA Method 23).
This report presents data from the FTIR measurements performed by Eastern Research Group.
The EPA Method 23, 25A, and 322 measurements were conducted by Pacific Environmental
Services, Inc. (PES), and Air Pollution Characterization and Control, Ltd. (APCC), under
subcontract to PES. Process data was collected by Research Triangle Institute, Inc. (RTI), under
contract to EPA. Please refer to the report prepared by PES for information and results of the
Method 23, 25 A, and 322 testing. For this test, screening means a measurement to determine
approximate levels of species other than HCl.
The lime kiln facility and sampling locations tested in this program are detailed in the
report prepared by PES.
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1.1 Objectives
The objective of the FTIR testing of the lime facility was to quantify HCl and perform
screening of other HAPs detectable by FTIR, using EPA Draft Method 320.
1.2 Brief Site Discussion
Testing was conducted at the Redland Stone Products in San Antonio, Texas. Testing
was performed on the inlet and outlet of a wet scrubber. Detailed site information can be found
in the report prepared by PES.
1.3 Emissions Measurements Program
This section provides an overview of the emissions measurement program conducted at
the Redland Stone Products in San Antonio, Texas. Included in this section are summaries of the
test matrix, test schedule, and authorized deviations from the test plan. Additional details on
these topics are provided in the sections that follow.
1.3.1 Test Matrix
The complete sampling and analytical matrix performed are presented in the report
prepared by PES. In this report, only FTIR-related test matrix will be provided. FTIR
spectroscopy was used, in accordance with EPA Draft Method 320, to quantify HCl and, in a
screening capacity, to measure other HAPs that FTIR can detect.
FTER measurements were conducted in two sets:
• Unconditioned; and
• Conditioned.
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Unconditioned sampling was conducted during the extent of the EPA Method 23 dioxin
manual train runs. These runs were approximately 3 hours in duration. After completion of a
dioxin run, the FTIR measured conditioned sample gas for a 1-hour period to screen for aromatic
species such as benzene, toluene, etc.
During each run (i.e., unconditioned or conditioned) the FTIR analysis time was divided
equally between inlet and outlet samples. Each location was monitored for at least a total of
25 minutes. Some data points were discarded for each set due to inlet/outlet sample mixing in
the FTIR analysis cell. The actual amount of data points discarded is given later in this report.
This procedure ensures the remaining data points were data truly representing the location being
tested in that set.
1.3.2 Test Schedule
The test schedule for EPA Methods 23, 25A, and 322 measurements is given by the
report prepared by PES. Section 2.1 gives the test log for the FTIR testing at this site.
1.3.3 Deviations from Test Plan/Schedule
Deviations from the original FTIR Site-Specific Test Plan (SSTP) are listed below:
• Testing was originally planned for 15 minute intervals between the inlet and
outlet. The measurements consisted of collecting 30 minute intervals alternating
from the inlet and the outlet, in order to synchronize with the GFC-IR
measurements performed by APCC.
• The EPA Work Assignment Manager authorized 1 hour total sample collection of
the conditioned samples, '/2 hour each on inlet and outlet. If detection of other
HAPs was determined, then the run would extend to the full two hours, as
originally planned. In this case, no additional HAPs were detected in the
conditioned samples.
• Some indicated sampling system temperatures were below the 350°F target that
was stated in the test plan. These temperatures are the highest attainable with
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these sampling components. It was determined after completion of the test
program that the measured temperature of some of the sampling system
components was a sensitive function of thermocouple location. When test
thermocouples were inserted in the sample-wetted regions of the sampling system,
they indicated temperatures above 350°F in all cases.
1.4 Test Report
This final report, presenting all data collected and the results of the analyses, has been
prepared in four sections, and an appendix as described below:
• Section 1 provides an introduction to the testing effort and includes a brief
description of the test site and an overview of the emissions measurement
program;
• Section 2 gives a summary of the test results for the FTTR results for HC1 and
other detected species:
• Section 3 presents detailed descriptions of the sampling and analysis procedures;
and;
• Section 4 provides details of the quality assurance/quality control (QA/QC)
procedures used on this program and the QC results.
A detailed description of the site, sampling locations, process and plant operation during the field
test is provided in the PES-prepared report. Copies of the field data sheets and FTIR
concentration data are contained in the appendices.
Six appendices are found in this report. They are organized as follows:
• Appendix A contains spreadsheet QA/QC review sheets;
• Appendix B contains QC gas cylinder certification sheets;
• Appendix C contains raw FTIR data;
• Appendix D contains FTIR field data sheets;
• Appendix E contains pre-test calculations; and
• Appendix F contains post-test calculations.
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2.0 SUMMARY OF RESULTS
This section provides the FTIR results of the emissions test program conducted at the
Redland Stone Products in San Antonio, Texas on June 28, 1998. Results for the extractive
FTIR test conducted for HC1 and screening for selected HAPs are provided in this section.
Other (non-HAP) species detected are also reported. Testing was performed at the inlet and
outlet of the wet scrubber.
2.1 Emissions Test Log
ERG performed extractive FTIR measurements for HCl and other HAPs. Table 2-1
presents the emissions test log that shows the test date, location, run number, test type, and run
times for each method.
Table 2-1. Emissions Test Log
Date
6/28/98
6/28/98
6/28/98
Location
Wet Scrubber (inlet/outlet)
Wet Scrubber (inlet/outlet)
Wet Scrubber (inlet/outlet)
Run
Number
Spike 1
Run 1
Spike 2
Test Type
FTIR HC! Spike
(inlet/outlet)
FTIR (Unconditioned)
FTIR (Conditioned)
FTIR HCl Spike (inlet/
outlet)
Run Time .
08:13-10:13
10:34-13:54
16:20- 17:03
13:57-14:32
2.2 FTIR Results
2.2.1 Overview
FTIR data for HCl and other species in unconditioned sample gas were collected at the
inlet and outlet of the wet scrubber. FTIR data collection of unconditioned samples was
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synchronized with EPA Method 23 manual dioxin/furan testing and EPA Method 322 GFC-IR
HC1 measurements. Conditioned samples were measured by FTIR for other HAP species.
FTIR data were collected by alternating sample analysis between inlet and outlet every
30 minutes. Inlet and outlet samples were drawn on a continuous basis; only the FTIR sample
analysis was alternated between inlet and outlet. The first (23 outlet and 18 inlet) data points
from each 30 minute measurement period were discarded to eliminate data for samples
containing both inlet and outlet sample gas. These discarded data points correspond to the
apparent response time of the complete FTIR sampling and analysis system (details on
measurement of system response time are given below). This response time is somewhat greater
than usual, due to the presence of very fine lime dust in the 2 micron FTIR cell filter. The
measurement run contained a total of 36 and 28 1-minute average data points for both inlet and
outlet measurements, after discarding the transfer data points. A 1-minute average data point is
generated by analysis of a composite spectrum consisting of an average of 43 FTIR spectra
collected over the 1 minute period.
Section 2.1 gives the schedule of the tests performed at the Redland Stone Products in
San Antonio, Texas. Both unconditioned and conditioned samples were analyzed. Conditioned
samples were generated by passing the raw sample gas through a water vapor/carbon dioxide
scrubbing system (see Section 3.1.1 for details). Conditioned samples extracted from the wet
scrubber were measured after unconditioned sample extraction for the next hour. One minute
average data points were generated by analysis of the composite spectrum consisting of an
average of 43 FTIR spectra collected over the 1 minute period. These results are reported in
Section 2.2.2.2.
The wet scrubber removal efficiency for HC1 was measured from the inlet/outlet data
from each location and is reported in Section 2.2.2.1.
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2.2.2 FTIR Emission Results
This section contains the FTIR HCI test results for the wet scrubber inlet and outlet.
2.2.2.1 FTIR HCI Test Results. The estimated FTIR HCI detection limit for this
study was between 0.14 and 0.17 parts per million by volume (ppmv). Approximately half the
FTIR instrument analysis time was split equally between inlet and outlet. Results given below
are organized by location. HCI removal efficiency was also calculated for the run. Raw data are
presented in Appendix C listing each measured species 1-minute average concentration. All HCI
emission runs were collected during the unconditioned tests.
Wet Scrubber - Outlet/Inlet HCI Results—Table 2-2 gives a summary of the wet
scrubber outlet/inlet FTIR HCI results. Appendix C provides 1-minute averages for all target
species. The measured HCI removal efficiency due to the wet scrubber was 78.5 percent,
assuming that the sample gas composition to the inlet of the scrubber did not change significantly
during the outlet testing. Figures 2-1 and 2-2 show a real-time graph for the inlet and outlet runs,
respectively.
Table 2-2. Wet Scrubber FTIR HCI Results, ppmv
Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Run 1
6/28/98
10:34 - 13:54
Inlet
21.05
0.52
22.07
19.89
36
Outlet
4.69
0.28
5.21
4.28
28
78.5
SD - Standard Deviation
NDP - Number of data points measured
RE- Removal Efficiency in percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
NOTE: Raw data presented in Appendix C.
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2.2.2.2 Other Species Detected by FTIR. Other species were detected during the
unconditioned and conditioned FTIR test runs. These species were measured concurrently with
HC1. Results given below are organized by location. No additional HAPs were detected in the
conditioned samples.
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Figure 2-1. HCI Inlet Run - Red Land Stone Products
22.50
22.00
18.50
co ^r in CD
COO)OT-CMCO'3'CO' O T— CJCO^t"lOCDh-cioO)O
^y;^c^cMCMCMi— ^^^*— *— T-cvicMCMCMCMO*—'— T-^T— T-T-T— »— T--»— CM
^^T-'^^^^c\ic\jc\icMc\icMc\ic\i6Jc\ic\icMcoOTconwc6nwcocoCT
Time
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Figure 2-2. HCI Outlet Run - Red Land Stone Products
6.00
5.00
4.00
Q. 3.00
Q.
U
O
2.00
1.00
0.00
-i 1 r-
-i 1 1 1 1 r-
J§> ,
> .
£• .& .• .«?• .«^ .#• .#• .«?• .^- .«?>• .«?• .«r
O* K^" KV)" K^* K*^" fc.1^" ik.^* K*^' k.^" ^>* ^ * k.0/' tfi/' I/* Q/* I/* Ox" Q/" ^)' *^)" ^)* ^?>* ^>" ^)* '*>*
i^%^NN,\\^^\ ^v" \ ^ \ *\ \ ^" ^ \. *\ ^ ^ ^ ^
Time
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Wet Scrubber - Outlet/Inlet for Other Species Results—Table 2-3 and 2-4 gives the
summary of the wet scrubber for the inlet and outlet FTIR results for other species found during
the standard Draft Method 320 extractive analysis, respectively.
Table 2-3. Other Species Detected by FTIR - Wet Scrubber Inlet
(All values are ppmv, except CO2 and H,O in percent)
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
CO2
U
15.3
0.557
16.0
14.5
36
0.062
NO2
U
2.91
1.11
4.63
1.59
36
1.8
S02
U
177
83.4
306
59
36
9.7
CO
U
23.0
12.2
48.1
7.39
36
0.36
NO
U
408
27.0
448
365
36
8.0
C +
4
U
0.80
0.04
0.87
0.73
36
0.33
H2O
U
6.22
0.176
6.44
5.95
36
0.13
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
Std. Dev. = Standard Deviation
Max. = Maximum
Min. = Minimum
NOTE: Raw data presented in Appendix C.
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Table 2-4. Other Species Detected by FTIR - Wet Scrubber Outlet
(All values are ppmv, except CO2 and H2O in percent)
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
C02
U
12.3
0.423
13.0
11.7
28
0.062
NO2
U
2.82
1.41
4.89
<2.31
28
2.31
SO2
U
16.0
37.8
129
<7.6
28
7.6
CO
U
22.1
22.1
73.8
6.45
28
0.49
NO
U
328
30.3
363
265
28
7.5
C +
*-4
U
1.08
0.05
1.16
0.95
28
0.53
H2O
U
17.3
0.141
17.5
17.1
28
0.12
U/C - Unconditioned (U) or Conditioned (C) Sample;
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent);
NDP - Number of data points;
EDL - Estimated detection limit for spectral region used for analysis.
Std. Dev. = Standard Deviation
Max. = Maximum
Min. = Minimum
NOTE: Raw data presented in Appendix C.
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3.0 SAMPLING AND ANALYTICAL PROCEDURE
The sampling and analytical procedure used by ERG for the lime plant test program is
extractive FTIR Spectroscopy, conducted in accordance with EPA Draft Method 320. In this
section, description of the FTIR method used is provided.
3.1 Determination of Gaseous Organic HAPs, HCI, and Criteria Pollutants by
FTIR
The extractive FTIR measurement method is based on continuous extraction of sample
gas from the stack, transporting the sample to the FTIR spectrometer and performing real-time
spectral measurement of the sample gas. The sample gas spectra are analyzed in real time for
target analytes, archived and possibly re-analyzed at a later date for other target analytes. This
section provides details on the FTIR sampling and measurement system.
3.1.1 FTIR Sampling Equipment
The FTIR measurement system meets the sampling and analysis requirements set forth in
EPA Draft Method 320, "Measurement of Vapor Phase Organic and Inorganic Emissions By
Extractive Fourier Transform Infrared Spectroscopy." This system has been used with complete
success with many source categories, and can also be adapted to switch quickly between two
sources (i.e., inlet and outlet) with a single FTIR spectrometer.
The sampling and measurement system consists of the following components:
• Heated probe;
• Heated filter;
• Heat-traced Teflon® sample line;
• Teflon® diaphragm, heated-head sample pump;
• FTIR spectrometer;
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• FTIR sample conditioning system; and
• QA/QC apparatus.
Figure 3-1 illustrates the extractive unconditioned FTIR sampling and measurement
system. In operation at a stationary source, the sample is continuously extracted from the stack
through the heated probe. Sample gas is then sent into a heated filter assembly that will remove
any particulate matter from the sample stream to protect the remainder of the sampling and
analysis system. The probe liner and filter body consist of glass, and the filter element is
polytetrafluoroethylene (PTFE or Teflon®). In addition to providing an inert surface, the glass
filter holder allows the operator to observe the filter loading during sampling operations. The
probe and filter are contained in a heated box mounted on the stack and maintained at a nominal
temperature of 177° C (350° F). A second probe/filter, heat-traced sample line, and heated head
pump used are not shown in Figure 3-1.
After passing through the filter assembly, a primary heat-traced PTFE sample line
transports the sample gas to the FTIR spectrometer maintained at approximately 177° C (350° F)
driven by a heated- head PTFE diaphragm sample pump maintained at approximately 204° C
(400° F). The sampling flow rate through the probe, filter, and sampling line is a nominal
20 standard liters per minute (LPM). Sample gas then enters an atmospheric pressure heated
PTFE distribution manifold where it is sent to the FTIR spectrometer via a slipstream flowing at
9 LPM. Other slipstreams can be sent to other instruments, if necessary. Excess sample gas not
used by instruments is vented to atmosphere.
A secondary heated-head PTFE diaphragm sample pump takes FTIR spectrometer sample
gas from the distribution manifold maintained at approximately 204° C (400° F) and directed
into the FTIR sample cell maintained at 185° C (365° F) for real-time analysis. The cell consists
of nickel-plated aluminum, with gold-plated glass substrate mirrors and potassium chloride
windows. Exhaust gas from the cell is vented to the atmosphere.
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Heat-traced line
Spike or QA/QC Gas
Sample
Gas In
Vaporization
block
I
QA/QC Gas Standard Manifold
Main Sample Pump
Heated Flow Meter
Legend
Bold text and lines = Heated
Normal text and lines = Unheated
Heat-traced line
( up to 100 feet)
QA/QC Gas Standards
Sample Distribution Manifold
FTIR
Sample (/
Pump/ I
irf
I I
To Other Instruments
Flowmeter'
FTIR Sample Cell
Spiking Solution
Excess sample to
atmosphere
Exhaust to atmosphere
Figure 3-1. FTIR Sampling and Measurement System
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Sample conditioning (when required) is achieved by passing raw sample gas through a
PermaPure® dryer and a series of impingers filled with sodium (or lithium) hydroxide pellets.
The PermaPure® drier selectively removes water vapor and the sodium hydroxide pellets remove
CO, and other acid gases. The sample conditioning apparatus is switched into the FTIR sample
path by a valving system. Lower detection limits for some compounds can be achieved with a
conditioned sample.
3.1.2 Preparation for Sampling
Before commencement of daily sampling operations, the following tasks were carried out:
• System leak check;
• Measurement of FTIR background spectrum;
• Instrumental QC; and
• Sampling and measurement system QC spike run.
Detailed descriptions of these tasks are described in the paragraphs below.
The heated sampling lines, probes, and a heated filter were positioned at the inlet and
outlet locations. All heated components were brought to operating temperature, and a leak check
of both inlet and outlet sampling systems were performed. The leak check was performed by
plugging the end of the probe and watching the main sample rotameter to observe the reading.
Positive leak check was confirmed when the rotameter reading was zero.
A background spectrum was measured using zero nitrogen through the cell. Next the QC
gases were measured. They agreed to within ±6 percent (±10 percent for HC1) of target value.
The QC gases used for this program include:
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Halocarbon 22 (H22), used to calibrate the pathlength. Halocarbon 22 is used for
its highly linear response due to the lack of sharp spectral features, and is an
extremely stable compound.
Carbon monoxide (CO) used for a frequency calibration. Carbon monoxide is
directly injected into the sample cell to measure photometric accuracy, validity of
the nonlinear correction algorithm and serve as a frequency (i.e., wavelength)
calibration. Acceptable limits for CO standard analysis are ±6 percent of certified
concentration;
Methane/nitric oxide/carbon dioxide mixture, used for overall system
performance check (calibration transfer standard) (acceptance limits are
±6 percent of the certified concentration); and
Hydrogen chloride standard, analyzed to verify the instrumental response of HC1,
a key target analyte (acceptance limits are ±10 percent of certified concentration).
The sampling and measurement system spike test was done to perform validation and
directly challenge the complete system and provide information on system accuracy and bias.
This test is conducted to satisfy the requirements set in EPA Draft Method 320 entitled
"Measurement of Vapor Phase Organic and Inorganic Emissions By Extractive Fourier
Transform Infrared Spectroscopy." Section B. 1 .C of Draft Method 320 gives a description of the
dynamic spiking apparatus.
The following FTIR spiking procedure was used:
• Measured native stack gas until system equilibrates - took two measurements
(i.e., two 1-minute samples);
• Started spike gas flow into sample stream, upstream of the heated filter;
• Let system equilibrate;
• Measured spiked sample stream for 2 minutes (i.e., two 1-minute samples);
• Turned off spike gas flow;
• Let system equilibrate with native stack gas; and
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• Repeated cycle, two more times.
The above procedure produced six spiked/unspiked sample pairs. Spike recovery for six
spiked/unspiked sample pairs were computed from the procedure given in Section 8.6.2 of EPA
Draft Method 320. The recovery was between 70-130 percent and allowed the system to be
considered acceptable for testing.
3.1.3 Sampling and Analysis
FTIR unconditioned sampling was performed simultaneously with the manual testing.
The start and stop times of the manual methods were coordinated with the FTIR operator, so that
FTIR data files can be coordinated with manual method start and stop times. FTIR inlet/outlet
sampling was accomplished using two heated transfer lines, and a valving system to switch from
inlet to outlet and vice versa.
Table 3-1 gives typical FTIR operating conditions. These parameters provide detection
limits of 0.1-1 ppm for typical FTIR analytes, while providing adequate dynamic range
(nominally 1-1,000 ppm). Some of these parameters are sample matrix dependent.
Table 3-1. Typical FTIR Operating Parameters
Parameter
Spectral Range (cm'1)
Spectral Resolution (cm'1)
Optical Cell Pathlength (m)
Optical Cell Temperature (° C)
Sample Flow Rate (liters/minute)
Integration Time (minutes)
Value
400 - 4,000
0.5
3.4
185
9 (3.0 optical cell volumes/minute)
1 (Average of 43 spectra)
Sample flow rate was determined by the data averaging interval and FTIR spectrometer
sample cell volume. A minimum of three sample cell volumes of gas must flow through the
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system to provide a representative sample during a single integration period. Typically, a
1 minute averaging period with a 3 liter volume sample cell gives a minimum flow rate of
9 LPM. Typically a flow rate of 20 standard LPM is used to accommodate the FTIR and other
instrumentation on-site, and to minimize sample residence time in the sampling system.
The temperature of all sampling system components were at a minimum of 177°C
(350 °F) to prevent condensation of water vapor or other analytes in the sampling system. Actual
sampling system operating temperatures were determined before the start of testing. The FTIR
sample cell temperature was maintained at 365° F (185° C) to minimize condensation of high-
boiling point analytes on the cell optics.
FTIR sample cell pressure was monitored in real-time to calculate analyte concentration
in parts-per-million. The cell was normally operated near atmospheric pressure with the cell
pressure continuously monitored.
Sampling probe location was determined by the requirements set in EPA Method 1 in
terms of duct diameters upstream and downstream of disturbances. Concurrent EPA Method 2
velocity measurements were not carried out at the same process stream location as the FTIR
sampling point to provide mass emission rate determination. The stack gas velocity and flow
rate were determined by the applicable manual test methods performed by PES. Velocity
information can be found from the report prepared by PES.
Sampling and analysis procedures are straightforward for a single-source measurement.
Once QA/QC procedures were completed at the beginning of the test day, the sample was
allowed to flow continuously through the FTIR spectrometer cell and the software was instructed
to start spectral data collection. The spectrometer collected one interferogram per second and
averaged a number of interferograms to form a time-integrated interferogram. The typical
averaging times range was approximately 1 minute. The interferogram was converted into a
spectrum and analyzed for the target analytes. After spectral analysis, the spectrum was stored
on the computer and later permanently archived. Spectral data collection was stopped after a
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predetermined time, corresponding to a "run." Typical runs were approximately 3 hours long,
giving approximately 180 1-minute average data points for each target analyte. The figure of
180 points were reduced by approximately 120 points due to elimination of data points per
switch between inlet/outlet samples and vice versa. At the end of the test day, the end-of-day
QA/QC procedures were conducted.
Before any testing was started at a given site, an initial "snapshot" of the stack gas was
taken with the FTIR measurement and analysis system to determine the true sample matrix.
Because sample conditioning was required for certain analytes, the FTIR spectrometer analyzed
these compounds after the unconditioned analysis. The order used during this program is shown
in the table below.
Sampling
Conditions
Unconditioned
Conditioned
Sampling Time
Synchronized with
dioxin sampling
1 hour (after
completion of
dioxin run)
Inlet
18 minute cell purge and
12 minute sample collection
2 minute cell purge and
28 minute sample collection
Outlet
23 minute cell purge
7 minute sample collection
2 minute cell purge and
28 minute sample collection
The sample being delivered to the FTIR cell alternated between the inlet and the outlet.
The switching valve, located just upstream of the common manifold, was manually activated
periodically to provide alternating inlet and outlet sample collections during each 3-hour period
(the estimated dioxin run duration). This procedure resulted in a set of data points collected for
the inlet and outlet, respectively. Five data points per set are discarded to eliminate analysis
results with combined inlet and outlet samples.
FTIR method performance was gauged from the results of the QA/QC procedures given
in Section B5 of EPA Draft Method 320. Acceptable spiking tests met acceptance for accuracy
within ± 30 percent. The acceptable instrument diagnostic and system response checked
KA0091 -02\002\003\REDLAND\REDLAND.NEW
3-8
-------
accuracy to be within ± 6 percent of target for all gas standards, and ± 10 percent for the HC1
standards. Acceptable system response check precision was 6 percent RSD.
Quantitative analysis was performed by a mathematical method called multi-variate least
squares (commonly known as Classical Least Squares or CLS). CLS constructs an optimized
linear combination (or 'fit') of the reference spectra to duplicate the sample spectrum, utilizing
the Beer-Lambert Law. The Beer-Lambert Law states that the absorbance of a particular spectral
feature due to a single analyte is proportional to its concentration. This relationship is the basis
of FTIR quantitative analysis. The coefficients of each compound in the linear fit yield the
concentration of that compound. If it is found that the quantitative analysis of a given compound
responds non-linearly to concentration, a calibration curve is developed by measuring a series of
reference spectra with differing optical depths (concentration times pathlength) and using them
in the linear fit. Low molecular weight species such as water vapor and carbon monoxide
require nonlinear correction, possibly even at levels as low as 100 ppm-meters (concentration
times pathlength). Analytes greater than 50-60 amu molecular weight usually does not require
nonlinear corrections. An experienced spectroscopist can determine whether nonlinear
corrections are necessary for an analyte in a given source testing scenario.
The ERG validated spectral database includes the compounds shown in Table 3-2. These
spectra were validated in the laboratory at a cell temperature of 185° C against certified gaseous
standards. Any compounds identified in the stack gas and not included in the ERG database can
be quantified if necessary after subsequent laboratory reference spectrum generation.
3.1.4 FTIR Method Data Review Procedures
The following procedure was conducted to review and validate the FTIR data.
KA0091-02\002\003\REDLAND\REDLAND.NEW 3-9
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Table 3-2. Compounds for Which Reference FTIR Spectra Are
Available in the ERG Spectral Library3
1-butene
1 ,3-butadiene
2-methylpropane
2-propanol
2-methoxyethanol
2-methyl-2-prop'anol
2-methylbutane
4-vinylcycIohexane
acetaldehyde
acetic acid
acetone
acetylene
acrolein
ammonia
benzene
carbon monoxide
carbon dioxide
carbonyl sulfide
chlorobenzene
cw-2-butene
cyclohexane
cyclopentane
cyclopropane
ethane
ethylbenzene
ethylene
formaldehyde
hydrogen fluoride
hydrogen chloride
isobutylene
m-xylene
/n-cresol
methane
methanol
methyl ethyl ketone
methylene chloride
n-butanol
n-butane
n-pentane
nitric oxide
nitrogen dioxide
nitrous oxide
o-cresol
o-xylene
p-cresol
/j-xylene
phenol
propane
propylene
styrene
sulfur dioxide
toluene
/ra«5-2-butene
water vapor
Spectra were collected at a cell temperature of 185° C.
KA0091 -02\002\003\REDLAND\REDLAND.NEW
3-10
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A. Post-test Data Review procedure (on-site)
1. Examine the concentration vs. time series plot for each compound of interest, and
identify regions with the following characteristics:
• sudden change in concentration;
• unrealistic concentration values;
• significant changes in 95 percent confidence intervals reported by
software; and
• sudden increase of noise in data.
2. Select representative spectra from the time periods indicated from Step 1.
3. Subtract from each representative spectrum chosen in Step 2 a spectrum taken
immediately prior in time to the indicated time region.
4. Manually quantitate (including any nonlinear corrections) for the species in
question and compare the result with the difference in software-computed
concentrations for respective spectra.
5. If concentration values in Step 4 do not agree to within 5 percent, determine
whether the difference is due to a recoverable or non-recoverable error.
6 (i). If the error is non-recoverable, the spectra in the indicated time region are
declared invalid.
7 (ii). If the error is recoverable, and time permits, determine possible source(s) of error
and attempt to correct. If time is critical, proceed with measurement. If
correction is achieved, conduct QA/QC checks before continuing.
8. Determine the peak-to-peak scatter or the root mean square (RMS) noise-
equivalent-absorbance (NEA) for the representative spectra.
9. If the NEA exceeds the limits required for acceptable detection limits, the spectra
in the time region are declared invalid (due to non-recoverable error).
10. Data found invalid are subject to re-measurement.
K.\009I-02\002\003\REDLAND\REDLAND.NEW 3-1 1
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B. Final Data Review (off-site)
The procedures for final data review include those given above; however, if a non-
recoverable error was found during this phase, the data are considered invalid. In addition, the
following procedures are carried out by the spectroscopist to perform a final data validation:
1. If any recoverable data errors are detected from the procedure, determine the
cause and perform any necessary corrections.
2. For analytes that were not detected or detected at low levels:
• estimate detection limits from validated data:
• check for measurement bias.
3. Verify spreadsheet calculations by independent calculation (results in
Appendix A).
3.1.5 FTIR QA/QC Procedures
The FTIR QA/QC apparatus will be used to perform two functions:
• Dynamic analyte spiking; and
• Instrumental performance checks.
Dynamic analyte spiking was used for quality control/quality assurance of the complete
sampling and analysis system. Dynamic spiking is continuous spiking of the sample gas to
provide information on system response, sample matrix effects, and potential sampling system
biases. Spiking is accomplished by either:
• Direct introduction of a certified gas standard; or
• Volatilization of a spiking solution.
K \0091 -02\002\003\REDLAND\REDLAND.NEW
3-12
-------
Certified gas standards are preferred due to simplicity of use, but many target analytes
cannot be obtained as certified gas standards, and must be spiked using standards generated by
volatilized solutions.
Gaseous spiking is carried out by metering the spike gas into the sample stream at a
known rate. Spike levels are calculated from mass balance principles. When certified gas
standards are used, a dilution tracer, such as sulfur hexafluoride, is used to directly measure the
fraction of spike gas spiked into the sample. This technique can be used instead of mass balance
calculations.
FTIR method performance is gauged from the results of the QA/QC. Acceptable spiking
tests will meet Draft Method 320 criteria (i.e., accuracy of within ± 30 percent) or a statistical
equivalent when less than 12 spiked/unspiked pairs are collected. The EPA Draft Method 320
instructs the user to determine the percent spike recovery of three pairs of spiked/unspiked
samples. The EPA Draft Method 320 acceptance criterion is 70 to 130 percent recovery for the
three pairs of samples. The acceptable instrument diagnostic and system response check
accuracy were within ± 6 percent of target (±10 percent for HC1 standards). Acceptable system
response check precision was 6 percent RSD.
KA0091 -02\002\003\REDLAND\REDLAND.NEW 3-13
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4.0 QUALITY ASSURANCE/QUALITY CONTROL
Specific QA/QC procedures were strictly followed during this test program to ensure the
production of useful and valid data throughout the project. A detailed presentation of QC
procedures for all sampling and analysis activities can be found in the Site Specific Test Plan and
Quality Assurance Project Plan for this project. This section reports all QC results so that the
data quality can be ascertained.
In summary, a high degree of data quality was maintained throughout the project. All
sampling system leak checks met the QC criteria as specified in Draft Method 320. Acceptable
spike recoveries and close agreement between duplicate analyses were shown for the sample
analyses. The data completeness was 100 percent, based on changes authorized by the Work
Assignment Manager.
4.1 FTIR Analytical Quality Control
Dynamic analyte spiking was used for quality control/quality assurance of the complete
sampling and analysis system. Dynamic spiking is continuous spiking of the sample gas to
provide information on system response, sample matrix effects, and potential sampling system
biases. Spiking was accomplished by direct introduction of a certified gas standard.
Gaseous spiking was carried out by metering the spike gas into the sample stream at a
known rate. A sulfur hexafluoride dilution tracer was used to directly measure the fraction of
spike gas spiked into the sample. The EPA Draft Method 320 limits the dilution of the sample
gas to 10 percent.
Before any testing was started at a given site, an initial "snapshot" of the stack gas is
taken with the FTIR measurement and analysis system to determine the true sample matrix. If
any target analytes are present at significantly higher levels than expected, adjustments were
K \009I-02\002\00.1\REDLAND\REDLAND.NEW 4- 1
-------
made to the cell pathlength and/or the spectral analysis regions used for quantitative analysis.
These adjustments minimized interferences due to unexpectedly high levels of detected analytes.
FTIR method performance is gauged from the results of the QA/QC. All spiking tests
met Draft Method 320 criteria. The acceptable instrument diagnostic and system response check
accuracy should be within ± 6 percent of target for all gas standards except HC1. The accuracy
for the HC1 standard should be within ±10 percent.
Analytical QC checks for the FTIR system consisted of the following:
• Dynamic spiking of HC1;
• Direct measurement of a HC1 gas standard:
j
• Direct measurement of a CO gas standard;
• Direct measurement of methane (CH4), nitrous oxide (NO2), and carbon dioxide
(C0:) standard; and
• Pathlength calibration using H22.
Dynamic spiking runs were conducted twice daily: before and after testing. Six spiked/unspiked
data points were collected. Statistical calculations consistent with EPA Method 301 were
performed on the data. Recovery of 70-130 percent was the acceptance criteria. Tables 4-1 and
4-2 summarize the dynamic spiking results. All dynamic spiking tests met the above acceptance
criteria. In all runs, sample gas was diluted 10 percent or less.
Direct instrumental measurement of HCl, CO, H22, and a CH4, NO2 and CO2 mixture
was conducted before and after daily testing activities. Acceptance criteria are normally
±6 percent of target, using EPA protocol gases. However, since the HCl standard was obtained
at a ±5 percent analytical tolerance, the acceptance criteria was set at ±10 percent. FTIR nitrogen
oxides (NOJ is measured as NO + NO;. Examination of Table 4-3 shows that all QC checks met
the above criteria.
KA0091 -02\002\003\REDLAND\REDLAND NEW
4-2
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Table 4-1. HCI QC Pre-Test Spike Results - Redland Stone Products
Outlet
Spike
Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
5.32
4.6 1
4.02
3.79
4.06
4.49
4.38
Spiked
(ppmv)
12.67
12.54
12.54
12.25
12.13
12.08
12.37
Corrected
Difference
(ppmv)
7.59
8.14
8.69
8.62
8.25
7.78
8.18
Spike
Level
(ppmv)
11.43
11.43
10.94
10.94
10.94
10.94
11.10
%
Recovery
iiiitii
73.68
SF6
Cone.
(ppmv)
0.23
0.23
0.22
0.22
0.22
0.22
0.223
Dilution
Ratio
0.045
0.045
0.043
0.043
0.043
0.043
0.044
Inlet
Spike
Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
7.29
6.46
6.82
7.84
7.02
6.13
6.93
Spiked
(ppmv)
21.02
21.62
22.37
23.36
23.41
22.45
22.37 j
Corrected
Difference
(ppmv)
14.35
15.71
16.13
16.17
16.97
16.84
16.03
Spike
Level
(ppmv)
21.42
21.42
21.42
20.92
20.92
21.42
21.25
%
Recovery
WM^^
75.42
SF6
Cone.
(ppmv)
0.43
0.43
0.43
0.42
0.42
0.43
0.427
Dilution
Ratio
0.085
0.085
0.085
0.083
0.083
0.085
0.084
NOTE: The spike runs were conducted before and after the test runs, therefore the minimum
and maximum values listed here may be different from those listed in the test runs. Section 2.
Sample gas dilution was held to 10 percent or less in all runs. Percent recovery is defined in
Draft Method 320.
(Stock spike gas values for HCI and SF6 values are 253 ppmv and 5.08 ppmv, respectively).
Recovery = 100 x
Corrected Difference
Spike level
Corrected Difference = Spiked - (1 - Dilution Ratio) X Unspiked
K.\009I-02\002\003\R£DLAND\REDLAND.NEW 4-3
-------
Table 4-2. HCI QC Post-Test Spike Results - Redland Stone Products
Outlet
Spike
Run
Number
1
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
4.24
4.27
4.23
4.39
4.03
4.73
4.32
Spiked
(ppmv)
17.34
17.97
18.06
18.25
18.31
18.59
18.09
Corrected
Difference
(ppmv)
13.37
13.97
14.10
14.14
14.53
14.16
14.04
Spike
Level
(ppmv)
15.94
15.94
15.94
15.44
15.44
15.44
15.69
%
Recovery
wss,
W^^M
89.48
SF6
Cone.
(ppmv)
0.320
0.320
0.320
0.310
0.310
0.310
0.315
Dilution
Ratio
0.063
0.063
0.063
0.061
0.061
0.061
0.062
Inlet
Spike
Run
Number
1
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
17.50
18.79
19.81
20.59
21.24
21.12
19.84
Spiked
(ppmv)
40.32
43.54
45.06
46.50
46.98
48.13
45.09
Corrected
Difference
(ppmv)
24.58
26.64
27.24
27.98
27.87
29.13
27.24
Spike
Level
(ppmv)
25.40
25.40
25.90
25.90
25.90
25.90
25.73
%
Recovery
WM!K
105.90
SF6
Cone.
(ppmv)
0.510
0.510
0.520
0.520
0.520
0.520
0.517
Dilution
Ratio
0.100
0.100
0.102
0.102
0.102
0.102
0.101
NOTE: The spike runs were conducted before and after the test runs, therefore the minimum
and maximum values listed here may be different from those listed in the test runs, Section 2.
Sample gas dilution was held to 10 percent or less in all runs. Percent recovery is defined in
Draft Method 320.
(Stock spike gas values for HCI and SF6 values are 253 ppmv and 5.08 ppmv. respectively).
% Recovery = 100 x
Corrected Difference
Spike level
Corrected Difference = Spiked - (1 - Dilution Ratio) X Unspiked
4-4
K \009I-02\002\003\REDLAND\REDLAND.NEW
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Table 4-3. Gas Standard Analysis Results
Date
6/28/98
6/28/98
Time
08:00 AM
02:45 PM
Compound
HC1
CO
CH4
NO
C02
H22
HC1
CO
CH4
NO
C02
H22
True
(ppm)*
253
102.3
491
503
4.99 %
253
102.3
491
503
4.99 %
Result
(ppm)*
253.4
102.8
489.9
506.3
5.06 %
3.45m
248.6
102.5
490.5
503.1
5.08%
3.41 m
%
Recovery
100.2
100.5
99.8
100.7
101.4
98.3
100.2
99.9
100
101.8
HC1 Gas Standard Accuracy: ±5 percent; Acceptance Criteria: ±10 percent of target.
CO Gas Standard Accuracy: ±1 percent; Acceptance Criteria: ±6 percent of target.
CH4 NO2 and CO2 Gas Standard Accuracy; ±1 percent; Acceptance Criteria: ±6 percent of target.
* All compounds are recorded in ppm except CO, in percent (%), and H22 in meters (m). The
Halocarbon 22 (H22) is used to calibrate the pa;hlength.
K:\0091 -02\002\003\REDLAND\REDLAND.NEW
4-5
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APPENDIX A
FTIR DATA SPREADSHEET CALCULATION
QA/QC SHEETS
K:\0091-02\002\003\REDLAND\REDLAND.NEW
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FTIR QA/QC REVIEW
Calculation and Methodology QA/QC Checklist
• For each facility tested, the reviewer will have:
1. Excel QA/QC workbook
2. Inlet and Outlet QA/QC information
Facility Name:
DATE:
Source Location (INLET or OUTLET)
TIME:
Run Description
Reviewer:
: flo.
Date:
1. Pollutants matches pollutants in both the
original and QA/QC data
2. Times for Inlet/Outlet samples match.
3. Number of data points match.
4. Column statistics match (i.e., Average,
Standard Deviation, Maximum, Minimum)
5. Verify that the QA/QC value is zero. This
indicated that both the original and the
QA/QC values are identical
1. No mathematical errors
2. No errors in the data macro
2.
Not able to determine
-------
FTIR QA/QC REVIEW
Calculation and Methodology QA/QC Checklist
• For each facility tested, the reviewer will have:
1. Excel QA/QC workbook
2. Inlet and Outlet QA/QC information
FacaityName:
DATE:
Source Location (INLETon OUTLET)
TIME:
/*: 20; 1 1
Run Description
Reviewer:
1. Pollutants matches pollutants in both the
original and QA/QC data
2. Times for Inlet/Outlet samples match.
I/
7
3. Number of data points match.
7
4. Column statistics match (i.e., Average,
Standard Deviation, Maximum, Minimum)
5. Verify that the QA/QC value is zero. This
indicated that both the original and the
^QA/QC values are identical.
1. No mathematical errors
2. No errors in the data macro
* Not able to determine
-------
FTIR QA/QC REVIEW
Calculation and Methodology QA/QC Checklist
For each facility tested, the reviewer will have:
1. Excel QA/QC workbook
2. Inlet and Outlet QA/QC information
Facility Name:
DATE:
Source Location (INLET or OUTLET)
TIME:
Run Description
0\ .
Reviewer:
Date:
1. Pollutants matches pollutants in both the
original and QA/QC data
V
2. Times for Inlet/Outlet samples match.
3. Number of data points match.
4. Column statistics match (i.e., Average,
Standard Deviation, Maximum, Minimum)
5. Verify that the QA/QC value is zero. This
indicated that both the original and the
QA/QC values are identical.
/
i. No mathematical errors
2. No errors in the data macro
-------
FTIR QA/QC REVIEW
Calculation and Methodology QA/QC Checklist
For each facility tested, the reviewer will have:
1. Excel QA/QC workbook
2. Inlet and Outlet QA/QC information
DATE:
Source Location (INLET or OUTLET)
XNUTT
TIME:
Run Description
(U°l
Reviewer:
Date:
1. Pollutants matches pollutants in both the
original and QA/QC data
2. Times for Inlet/Outlet samples match.
3. Number of data points match.
t/*
4. Column statistics match (i.e., Average,
Standard Deviation, Maximum, Minimum)
5. Verify that the QA/QC value is zero. This
indicated that both the original and the
v..,- .QA/QC values are identical.
V
i. No mathematical errors
2. No errors in the data macro
-------
Below are the results of the Draft Method 320 post-test calculations for this test program. The
calculations are organized by appendix as found in the FTIR Protocol. Since classical-least-
squares (CLS) is used for analysis, the CLS-equivalent calculations are used, since in some cases,
the FMU values using band-areas can differ as much as an order of magnitude compared to CLS-
derived results.
Appendix I
Determining Fractional Model Uncertainties:
These calculations determine the fractional error in the analysis for the analytes of interest (i.e.,
HC1). The results for HC1 are given in the table below for 1 spectrum selected from the inlet and
outlet test. In order to achieve results that are consistent with the CLS analysis approach, the CLS
equivalent of the calculation was performed. This is simply the reported analysis error divided
by the HC1 concentration.
TABLE 1. FMU CALCULATION FOR HCL -REDLANDS
Spectral File Name
RN010032.spa
RN010062.spa
Inlet/Outlet
Outlet
Inlet
Error (ppm)
0.15
0.19
Concentration (ppm)
6.62
17.4
FMU
0.023
0.011
Error is 95% confidence imervaJ reported by CLS software.
Appendix J
Overall Concentration Uncertainty
The CLS equivalent of overall concentration uncertainty is simply the error reported by the CLS
software. The results for this test program are found in Table 1, above.
K-\0091 -02\00/\iA);s\REDLAND\REDLAND.NEW
F-l
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APPENDIX F
POST-TEST CALCULATIONS
K:\0091 -02\002\003\REDLAND\REDLAND.NEW
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Appendix G
Measuring Noise Levels
The result of this calculation is given under the Appendix C heading.
Appendix H
Determining Sample Absorption Pathlength (Ls) and Fractional Analytical Uncertainty
Since the HCI reference spectrum used in this program were measured at the same pathlength to
be used during testing, these calculations are not required.
KA0091 -02\002\003\REDLAND\REDLAND.NEW E-3
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Appendix D
Estimating Minimum Concentration Measurement Uncertainties (MAU)
The result for HCI is:
MAU(HC1)= 0.4ppmv.
This value is computed using the formula given in Appendix D. However, this value is derived
using band area calculations. The FTIR spectral data in this field study are analyzed by classical
least squares (CLS), not band areas. CLS derived minimum measurement uncertainties for HCI
are on the order of 0.1-0.2 ppmv for this test program.
Appendix E
Determining Fractional Reproducibility Uncertainties (FRU)
This calculation estimates the uncertainty in analysis, using band areas, of two sequentially
measured CTS spectra collected immediately before and after the HCI reference spectrum. The
calculation is performed in the analysis region used for HCI. The result is:
FRU (HCI region) = 0.093.
The corresponding value using CLS is somewhat lower. For most analytes of interest, FRU
usually falls between 0.001 and 0.04 using CLS.
Appendix F
Determining Fractional Calibration Uncertainties (FCU)
This section determines the fractional calibration uncertainties when analyzing each reference
spectrum. These results will be applied to the compounds analyzed in the HCI analysis region.
The table below gives the results.
TABLE 2. FCU Determination
Analyte
H2O
HCI
CHd
ASC (ppm)
113000
253
491
ISC (H2O)
115000
-22.5
-23.0
ISC (HCI)
0.000
254
0.000
ISC (CH4)
0.000
0.000
493
FCU
-1.7%
-0.4%
-0.2%
AU
-
30%
-
K.\009I-02\002\003\REDLAND\REDLAND.NEW
E-2
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Below are the results of the Draft Method 320 pre-test calculations for this test program. The
calculations are organized by appendix as found in the FTIR Protocol. These calculations were
originally taken from the Secondary Aluminum HCI program from late 1997.
Appendix B
Potential Interferant Calculations:
These calculations determine potential spectral interferants for the analytes of interest (i.e., HCI).
The results for HCI are given in the table below. The analysis region for HCI is not given since it
is considered proprietary information.
TABLE 1. INTERFERANT CALCULATIONS
Analyte
Concentration
Band area
IAI/AAI
Average absorbance
HCI (target)
0.1 ppmv
0.0005436
0.00000322
H,O (potential interferant)
20%
0.2213
407
0.00131
CO2 (potential interferant)
20%
0.000002
0.0036
H,CO (potential interferant)
1 ppmv
0.0002100
0.386
CH4 (potential interferant)
20 ppmv
0.0105
19.3
0.00006213
AVT
0.00137
Note: compounds in bold are known interferants. AVT is computed from target and known
interferants.
Known interferant criteria is IAI/AAI > 0.5
From the Table, two potential interferants are identified: H2O and CH4.
Appendix C
Noise Level
This calculation determines instrumental noise level in the spectral analysis region for HCI. For
a 1 minute integration time, the RMS noise is found to be 0.00022 (absorbance units) in the HCI
spectral analysis region by the procedure given in Appendix G.
KA0091 -02\002\003\REDLANDVREDLAND.NEW
E-l
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APPENDIX E
PRE-TEST CALCULATIONS
KA009I-02\002\003\REDLAND\REDLAND.NEW
-------
Facility
Stack ID
Date
Run Number
Recorded By
Channel
FTIR Temperature Readout Sheet
Description
ir/r
K&0
*
Inlet Stack
Outlet Stack
o
n?
Inlet Probe
77*
i
Outlet Probe
72?
Inlet Filter
MB
tv*
Outlet Filter
Inlet HT
->**
10
Outlet HT
Inlet Pump
7,11
10
Outlet Pump
m
11
FTIR Pump
12
Pump Box
13
14
Extra HT
FTIR Jumper
15
Pump Jumper
16
Hot Box
3Z.
17
Hot Box
18
Extra HT
Z7Z
19
20
Electronics Box
4f
-------
FTIR Temperature Readout Sheet
-------
APPENDIX D
FTIR FIELD DATA SHEETS
KA0091 -02\002\003\REDLAND\REDLAND.NEW
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SR|SS8S8S8SJ8S8
SR
SR?assRt
3 grists
fill
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-------
APPENDIX C
RAW FTIR DATA
K \0091 -02\002\003\REDLAND\REDLAND.NEW
-------
APPENDIX B
GAS CYLINDER CERTIFICATION SHEETS
K:\0091 -02\002\003\REDLAND\REDLAND.NEW
-------
SPECTBfl GflSES
3434 Route 22 West • Branchburg, NJ 08876 USA Tel: (908) 252-9300 • (800) 932-0624 • Fax: (908) 252-0811
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Morrisville , NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 134942
ITEM*: 3
CERTIFICATION DATE: 8/10/98
P.O.#: 9101008011-R132
BLEND TYPE: CERTIFIED
CYLINDER #: 982153Y
CYLINDER PRES: 2000 psig
CYLINDER VALVE: CGA 330
ANALYTICAL ACCURACY: + / - 5%
COMPONENT
REQUESTED GAS
CONC
ANALYSIS
Hydrogen Chloride
Sulfur Hexafluoride
1,000 ppm
2.00 ppm
1,030 ppm
2.02 ppm
Nitrogen
Balance
Balance
Sulfur Hexafluoride is +/- 2%
ANALYST:
-
DATE:
8/10/98
Ted Neeme
USA • United Kingdom • Germany • Japan
-------
5b
SPECTRfl CBSES
277 Coit Street • Irvington, NJ 07111 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Morrisviile, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 132874
ITEM*: 1
CERTIFICATION DATE: 5/11/98
BLEND TYPE: CERTIFIED
CYLINDER*: 1757934Y
CYLINDER PRES: 2000 psig
P.OJ: 9101008004-R986
ANALYTICAL ACCURACY:
/- 2%*
COMPONENT
Hydrogen Chloride
Sulfur Hexafluoride
Nitrogen
REQUESTED GAS
CONG
500 ppm
5.00 ppm
Balance
ANALYSIS
516 ppm
5.09 ppm
Balance
* Analytical Accuracy of Hydrogen Chloride is +/- 5%
ANALYST:
Milje-Coyle
DATE: 5/11/98
USA • United Kingdom • Germam/ • .l
-------
SPECTRfl GRSES
3434 Route 22 West • Branchburg, NJ 08876 USA Tel: (908) 252-9300 • (800) 932-0624 • Fax: (908) 252-0811
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Morrisville, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 134942
ITEM*: 2
CERTIFICATION DATE: 8/10/98
P.O.#: 9101008011-R132
BLEND TYPE: CERTIFIED
CYLINDER*: 1015632Y
CYLINDER PRES: 2000 psig
CYLINDER VALVE: CGA 330
ANALYTICAL ACCURACY: + / - 5%
COMPONENT
REQUESTED GAS
CONC
ANALYSIS
Hydrogen Chloride
Sulfur Hexafluoride
250 ppm
2.00 ppm
260 ppm
2.00 ppm
Nitrogen
Balance
Balance
Sulfur Hexafluoride is +/- 2%
ANALYST:
Ted Neeme
DATE: 8/10/98
!!CA . ll-u-
-------
SPECTRH GflSES
RECD MAY 15 1998
^^M 277 Coit Street • Irvington, NJ 07111 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Morrisville, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER*: 132874
ITEM*: 2
CERTIFICATION DATE: 5/11/98
BLEND TYPE: CERTIFIED
CYLINDER*: 1370597Y
CYLINDER PRES: 2000 psig
P.O.*: 9101008004-R986
ANALYTICAL ACCURACY:
/- 2%*
COMPONENT
Hydrogen Chloride
Sulfur Hexafluoride
Nitrogen
REQUESTED GAS
CONG
250 ppm
5.00 ppm
Balance
ANALYSIS
253 ppm
5.08 ppm
Balance
* Analytical Accuracy of Hydrogen Chloride is +/- 5%
ANALYST:
DATE:
5/11/98
USA • United Kingdom • Germany • Japan
-------
EG
SPECTRfl GflSES
277 Coit Street • Irvington, NJ 07111 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Momsville, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER #: 128118
ITEM*: 1
CERTIFICATION DATE: 10/16/97
BLEND TYPE: CERTIFIED
CYLINDER # : 1757972Y
CYLINDER PRES: 2000 psig
P.O.*: 7904004005-R690
ANALYTICAL ACCURACY:
+1-2%
COMPONENT
Hydrogen Chloride**
Sulfur Hexafluoride
REQUESTED GAS
CONG
200 ppm
20.0 ppm
ANALYSIS
220 ppm
20.0 ppm
Nitrogen
Balance
Balance
' Analytical Accuracy of Hydrogen Chloride is +/- 5%
ANALYST:
Ted Neeme
DATE: 10/16/97
USA • United Kinadam
-------
SEP
SPECTRH GflSES
277 Coit Street • Irvington, NJ 07111 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Momsville, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 126876
ITEM*: 1
CERTIFICATION DATE: 8/29/97
BLEND TYPE: CERTIFIED
CYLINDER #: 1852209Y
CYLINDER PRES: 2000 PSIG
P.OJ: 7904004005-R562
ANALYTICAL ACCURACY:
+/- 5 %
COMPONENT
Hydrogen Chloride
Sulfur Hexafluoride
Nitrogen
REQUESTED GAS
CONG
200 ppm
20.0 ppm
Balance
ANALYSIS
210 ppm
20.2 ppm
Balance
ANALYST:
Ted Neeme
DATE: 8/29/97
USA • United Kingdom • Germany • Japan
-------
RECO AUG 141998
SPECTBH GflSES
^^M 3434 Route 22 West • Branchburg, NJ 08876 USA Tel: (908) 252-9300 • (800) 932-0624 • Fax: (908) 252-0811
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Morrisville , NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 134942
ITEM*: 1
CERTIFICATION DATE: 8/10/98
P.O,#: 9101008011-R132
BLEND TYPE: CERTIFIED
CYLINDER # : 1689487Y
CYLINDER PRES: 2000 psig
CYLINDER VALVE: CGA 330
ANALYTICAL ACCURACY: + / - 5%
COMPONENT
REQUESTED GAS
CONC
ANALYSIS
Hydrogen Chloride
Sulfur Hexafluonde
50.0 ppm
2.00 ppm
54.3 ppm
2.01 ppm
Nitrogen
Balance
Balance
Sulfur Hexafluoride is +/- 2%
ANALYST:
Ted Neeme
DATE: 8/10/98
USA • United Kingdom • Germany • Japan
-------
55
SPECTRA GASES
277 Coit St. • Irvington, NJ 07111 USA Tel.: (201) 372-2060 • (800) 932-0624 • Fax: (201) 372-8551
Shipped From: 80 Industrial Drive • Alpha, N.J. 08865
CERTIFICATE OF ANALYSIS
EPA PROTOCOL MIXTURE
PROCEDURE ft: G1
CUSTOMER:
SGI ORDER #:
ITEM*:
P.OJ:
Eastern Research Group Inc.
126876
5
7904004005-R562
CYLINDER #: CC79878
CYLINDER PRES: 2000 PSIG
CGA OUTLET: 660
CERTIFICATION DATE: 8/27/97
EXPIRATION DATE: 8/19/99
CERTIFICATION HISTORY
COMPONENT
Methane
Nitric Oxide
NOx
Carbon Dioxide
DATE OF
ASSAY
8/21/97
8/20/97
8/27/97
8/19/97
MEAN
CONCENTRATION
491 ppm
502.1 ppm
504.6 ppm
4.99 %
CERTIFIED
CONCENTRATION
491 ppm
503 ppm
503 ppm
4.99 %
ANALYTICAL
ACCURACY
+/- 1%
+/- 1%
Reference Value Only
+/- 1%
BALANCE
Nitrogen
REFERENCE STANDARDS
COMPONENT
Methane
Nitric Oxide
Carbon Dioxide
SRM/NTRM*
SRM-2751
NTRM-81687
SRM-1674b
CYLINDER*
CAL013479
CC57165
CLM007273
CONCENTRATION
98.6 ppm
1009 ppm
6.98%
INSTRUMENTATION
COMPONENT
Methane
Nitric Oxide
Carbon Dioxide
MAKE/MODEL
H. Packard-6890
Nicofet-760
Horiba-VIA-510
SERIAL #
US00001434
ADM9600121
571417045
DETECTOR
GC - FID
FTIR
NDIR
CALIBRATION
DATE(S)
8/21/97
8/27/97
7/25/97
THIS STANDARD WAS CERTIFIED ACCORDING TO THE EPA PROTOCOL PROCEDURES.
DO NOT USE THIS STANDARD IF THE CYLINDER PRESSURE IS LESS THAN 150 PSIG.
ANALYST:
DATE:
TED NEEME
8/27/97
-------
SEP 1 £ 1QQ?
SPECTRA GASES
277 Coit St. • Irvington, NJ 07111 USA Tel.: (201) 372-2060 • (800) 932-0624 • Fax: (201) 372-8551
Shipped From: 80 Industrial Drive • Alpha, NJ. 08865
r
CERTIFICATE OF ANALYSIS
EPA PROTOCOL MIXTURE
PROCEDURE #: G1
CUSTOMER:
SGI ORDER #:
ITEM#:
P.O.*:
Eastern Research Group Inc.
126876
3
7904004005-R562
CYLINDER #: CC80890
CYLINDER PRES: 2000 PSIG
CGA OUTLET: 350
CERTIFICATION DATE: 8/26/97
EXPIRATION DATE: 8/26/2000
CERTIFICATION HISTORY
COMPONENT
Carbon Monoxide
DATE OF
ASSAY
8/19/97
8/26/97
MEAN
CONCENTRATION
102.1 ppm
102.6 ppm
CERTIFIED
CONCENTRATION
102.3 ppm
ANALYTICAL
ACCURACY
+/- 1%
BALANCE
Nitrogen
REFERENCE STANDARDS
COMPONENT
Carbon Monoxide
SRM/NTRM*
SRM-1680b
CYLINDER*
CLM010013
CONCENTRATION
490.4 ppm
INSTRUMENTATION
COMPONENT
Carbon Monoxide
MAKE/MODEL
Horiba-VIA-510
SERIAL #
570423011
DETECTOR
NOIR
CALIBRATION
DATE(S)
8/26/97
THIS STANDARD WAS CERTIFIED ACCORDING TO THE EPA PROTOCOL PROCEDURES.
DO NOT USE THIS STANDARD IF THE CYLINDER PRESSURE IS LESS THAN 160 PSIG.
ANALYST:
DATE:
TED NEEME
8/26/97
-------
SEP 16 1997
SPECTRR BflSES
277 Coit Street • Irvington, NJ 071 1 1 USA Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-8551
SHIPPED FROM: 80 INDUSTRIAL DRIVE ALPHA, NJ. 08865 TEL: (908) 454-7455
SHIPPED TO:
Eastern Research Group Inc.
900 Perimeter Park
Momsvtlle, NC 27560
CERTIFICATE
OF
ANALYSIS
SGI ORDER # : 126876
ITEM*: 2
CERTIFICATION DATE: 8/29/97
BLEND TYPE: CERTIFIED
CYLINDER #: CC80877
CYLINDER PRES: 2000 PSIG
P.O.*: 7904004005-R562
ANALYTICAL ACCURACY: +/- 2 %
COMPONENT
Halocarbon 22
Nitrogen
REQUESTED GAS
CONG
40.0 ppm
Balance
ANALYSIS
40.3 ppm
Balance
ANALYST:
Ted Neeme
DATE: 8/29/97
» .-. ' V
USA • United Kinadom • Germanv • .
-------
TECHNICAL REPORT DATA
(Please read Instructions on reverse before completing)
1. REPORT NO.
EPA- 454/R-00-012
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Final Report of Lime Manufacturing Industry
Fourier Transform Infrared Spectroscopy
Redland Stone Products, San Antonio Texas
5. REPORT DATE
May 2000
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
EMAD
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, NC 27711
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-D7-0001
12. SPONSORING AGENCY NAME AND ADDRESS
Director
Office of Air Quality Planning and Standards
Office of Air and Radiation
U.S. Environmental Protection Agency
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Final Report
14. SPONSORING AGENCY CODE
EPA/200/04
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The United States Environmental protection Agency is investigating the lime manufacturing
industry source category to identify and quantify emissions of hazardous air pollutants (HAPs)
from rotary kilns. The primary objective of this test program was to obtain data on controlled and
uncontrolled emissions of hydrogen chloride (HCL) and gather screening data on other hazardous air
pollutants from lime production plants. EPA test Method 320 was used to collect the emission data.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b. IDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Hydrogen Chloride (HCL)
Hazardous Air Pollutants
Air Pollution control
Wet Scrubber
18. DISTRIBUTION STATEMENT
Release Unlimited
19. SECURITY CLASS (Report)
Unclassified
21. NO. OF PAGES
96
20. SECURITY CLASS (Page) „
- Unclassified
22?PRICE. '
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION IS OBSOLETE
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